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Sample records for rapid commun mass

  1. La Terre, notre bien commun

    Directory of Open Access Journals (Sweden)

    Arnaud Berthoud

    2008-03-01

    Full Text Available La Terre nous fait découvrir aujourd’hui une forme de responsabilité à l’égard de l’humanité toute entière. Quelle sorte de chose est donc la Terre lorsque nous usons de ce terme sous ses formes variées et que nous tentons de nous hisser au niveau de ce fait historique nouveau et de notre inquiétude à son sujet ? Je propose cette réponse générale : la Terre nous apparaît comme ce qui a été, est et sera toujours la chose la plus vaste à laquelle s’attache notre bien commun, parce qu’elle est le support, le fondement ou la base visible d’une vie que chacun éprouve intérieurement, selon un lien immédiat avec quelques semblables et comme le bien dont nous savons, comme le disait Maître Eckhart (1948, p.148, que « de tous les biens aucun ne nous est plus cher et plus désirable ». C’est cette réponse que je tente de développer en précisant successivement sous l’inspiration d’Aristote quelques traits relatifs au bien commun dont la Terre serait le support le plus vaste et sous l’inspiration biblique quelques remarques relatives au lien vivant qui nous attache à nos semblables et dont la Terre serait la base visible la plus claire. Je dirais alors que dans le premier cas la Terre est saisie comme un objet économique et que dans le second cas la Terre est saisie comme un objet religieux. J’essayerai dans la conclusion de rapporter ces deux types de propos l’un à l’autre.

  2. Gestion des communs et œconomie

    OpenAIRE

    Calame, Pierre

    2016-01-01

    Depuis le prix Nobel d’Elinor Ostrom, les communs sont à la mode et l’on ne compte plus les conférences, livres et réseaux consacrés aux communs et à leur renaissance. À juste titre : le concept même de commun renvoie à la prise de conscience des limites tant d’une régulation par le marché que par la gestion publique des biens et services. On en vient presque à oublier que les communs dont la prix Nobel a fait l’analyse étaient des communs de taille limitée gérée par des communautés fermées e...

  3. Rapid mass segregation in small stellar clusters

    Science.gov (United States)

    Spera, Mario; Capuzzo-Dolcetta, Roberto

    2017-12-01

    In this paper we focus our attention on small-to-intermediate N-body systems that are, initially, distributed uniformly in space and dynamically `cool' (virial ratios Q=2T/|Ω| below ˜0.3). In this work, we study the mass segregation that emerges after the initial violent dynamical evolution. At this scope, we ran a set of high precision N-body simulations of isolated clusters by means of HiGPUs, our direct summation N-body code. After the collapse, the system shows a clear mass segregation. This (quick) mass segregation occurs in two phases: the first shows up in clumps originated by sub-fragmentation before the deep overall collapse; this segregation is partly erased during the deep collapse to re-emerge, abruptly, during the second phase, that follows the first bounce of the system. In this second stage, the proper clock to measure the rate of segregation is the dynamical time after virialization, which (for cold and cool systems) may be significantly different from the crossing time evaluated from initial conditions. This result is obtained for isolated clusters composed of stars of two different masses (in the ratio mh/ml=2), at varying their number ratio, and is confirmed also in presence of a massive central object (simulating a black hole of stellar size). Actually, in stellar systems starting their dynamical evolution from cool conditions, the fast mass segregation adds to the following, slow, secular segregation which is collisionally induced. The violent mass segregation is an effect persistent over the whole range of N (128 ≤ N ≤1,024) investigated, and is an interesting feature on the astronomical-observational side, too. The semi-steady state reached after virialization corresponds to a mass segregated distribution function rather than that of equipartition of kinetic energy per unit mass as it should result from violent relaxation.

  4. In vitro rapid and mass multiplication of highly valuable medicinal ...

    African Journals Online (AJOL)

    In vitro rapid and mass multiplication of highly valuable medicinal plant Bacopa monnieri (L.) Wettst. Sudhir Sharma, Barkha Kamal, Neelima Rathi, Sudhir Chauhan, Vikas Jadon, Neha Vats, Ashok Gehlot, Sarita Arya ...

  5. Integrated database for rapid mass movements in Norway

    Directory of Open Access Journals (Sweden)

    C. Jaedicke

    2009-03-01

    Full Text Available Rapid gravitational slope mass movements include all kinds of short term relocation of geological material, snow or ice. Traditionally, information about such events is collected separately in different databases covering selected geographical regions and types of movement. In Norway the terrain is susceptible to all types of rapid gravitational slope mass movements ranging from single rocks hitting roads and houses to large snow avalanches and rock slides where entire mountainsides collapse into fjords creating flood waves and endangering large areas. In addition, quick clay slides occur in desalinated marine sediments in South Eastern and Mid Norway. For the authorities and inhabitants of endangered areas, the type of threat is of minor importance and mitigation measures have to consider several types of rapid mass movements simultaneously.

    An integrated national database for all types of rapid mass movements built around individual events has been established. Only three data entries are mandatory: time, location and type of movement. The remaining optional parameters enable recording of detailed information about the terrain, materials involved and damages caused. Pictures, movies and other documentation can be uploaded into the database. A web-based graphical user interface has been developed allowing new events to be entered, as well as editing and querying for all events. An integration of the database into a GIS system is currently under development.

    Datasets from various national sources like the road authorities and the Geological Survey of Norway were imported into the database. Today, the database contains 33 000 rapid mass movement events from the last five hundred years covering the entire country. A first analysis of the data shows that the most frequent type of recorded rapid mass movement is rock slides and snow avalanches followed by debris slides in third place. Most events are recorded in the steep fjord

  6. Integrated database for rapid mass movements in Norway

    Science.gov (United States)

    Jaedicke, C.; Lied, K.; Kronholm, K.

    2009-03-01

    Rapid gravitational slope mass movements include all kinds of short term relocation of geological material, snow or ice. Traditionally, information about such events is collected separately in different databases covering selected geographical regions and types of movement. In Norway the terrain is susceptible to all types of rapid gravitational slope mass movements ranging from single rocks hitting roads and houses to large snow avalanches and rock slides where entire mountainsides collapse into fjords creating flood waves and endangering large areas. In addition, quick clay slides occur in desalinated marine sediments in South Eastern and Mid Norway. For the authorities and inhabitants of endangered areas, the type of threat is of minor importance and mitigation measures have to consider several types of rapid mass movements simultaneously. An integrated national database for all types of rapid mass movements built around individual events has been established. Only three data entries are mandatory: time, location and type of movement. The remaining optional parameters enable recording of detailed information about the terrain, materials involved and damages caused. Pictures, movies and other documentation can be uploaded into the database. A web-based graphical user interface has been developed allowing new events to be entered, as well as editing and querying for all events. An integration of the database into a GIS system is currently under development. Datasets from various national sources like the road authorities and the Geological Survey of Norway were imported into the database. Today, the database contains 33 000 rapid mass movement events from the last five hundred years covering the entire country. A first analysis of the data shows that the most frequent type of recorded rapid mass movement is rock slides and snow avalanches followed by debris slides in third place. Most events are recorded in the steep fjord terrain of the Norwegian west coast, but

  7. Rapid identification of DNA-binding proteins by mass spectrometry

    DEFF Research Database (Denmark)

    Nordhoff, E; Krogsdam, A M; Jorgensen, H F

    1999-01-01

    We report a protocol for the rapid identification of DNA-binding proteins. Immobilized DNA probes harboring a specific sequence motif are incubated with cell or nuclear extract. Proteins are analyzed directly off the solid support by matrix-assisted laser desorption/ionization time-of-flight mass...... was validated by the identification of known prokaryotic and eukaryotic DNA-binding proteins, and its use provided evidence that poly(ADP-ribose) polymerase exhibits DNA sequence-specific binding to DNA....

  8. Michel François : le trait commun

    OpenAIRE

    Saudrais, Anthony

    2012-01-01

    Ce vingt-quatrième carnet d'études intitulé Trait commun est consacré à Michel François. Dans « The Drawing in my life » (pp. 9-16), Patrick Javault analyse les dessins de l'artiste au regard de lectures d'œuvres aussi variées que Contamination (pommes) (2006) ou A Black Vanity (2006-09). Pour le critique d’art, M.l François « ne cesse d'explorer le dessin dans toutes ses dimensions, de sembler parfois plonger à l'intérieur de la feuille et parfois de vouloir faire vivre la ligne » (p. 16). L...

  9. Differential Rapid Screening of Phytochemicals by Leaf Spray Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, Thomas; Graham Cooks, R. [Univ. of Innsbruck, Innsbruck (Austria)

    2014-03-15

    Ambient ionization can be achieved by generating an electrospray directly from plant tissue ('leaf spray'). The resulting mass spectra are characteristic of ionizable phytochemicals in the plant material. By subtracting the leaf spray spectra recorded from the petals of two hibiscus species H. moscheutos and H. syriacus one gains rapid access to the metabolites that differ most in the two petals. One such compound was identified as the sambubioside of quercitin (or delphinidin) while others are known flavones. Major interest centered on a C{sub 19}H{sub 29}NO{sub 5} compound that occurs only in the large H. moscheutos bloom. Attempts were made to characterize this compound by mass spectrometry alone as a test of such an approach. This showed that the compound is an alkaloid, assigned to the polyhydroxylated pyrrolidine class, and bound via a C{sub 3} hydrocarbon unit to a monoterpene.

  10. Detecting rapid mass movements using electrical self-potential measurements

    Science.gov (United States)

    Heinze, Thomas; Limbrock, Jonas; Pudasaini, Shiva P.; Kemna, Andreas

    2017-04-01

    Rapid mass movements are a latent danger for lives and infrastructure in almost any part of the world. Often such mass movements are caused by increasing pore pressure, for example, landslides after heavy rainfall or dam breaking after intrusion of water in the dam. Among several other geophysical methods used to observe water movement, the electrical self-potential method has been applied to a broad range of monitoring studies, especially focusing on volcanism and dam leakage but also during hydraulic fracturing and for earthquake prediction. Electrical self-potential signals may be caused by various mechanisms. Though, the most relevant source of the self-potential field in the given context is the streaming potential, caused by a flowing electrolyte through porous media with electrically charged internal surfaces. So far, existing models focus on monitoring water flow in non-deformable porous media. However, as the self-potential is sensitive to hydraulic parameters of the soil, any change in these parameters will cause an alteration of the electric signal. Mass movement will significantly influence the hydraulic parameters of the solid as well as the pressure field, assuming that fluid movement is faster than the pressure diffusion. We will present results of laboratory experiments under drained and undrained conditions with fluid triggered as well as manually triggered mass movements, monitored with self-potential measurements. For the undrained scenarios, we observe a clear correlation between the mass movements and signals in the electric potential, which clearly differ from the underlying potential variations due to increased saturation and fluid flow. In the drained experiments, we do not observe any measurable change in the electric potential. We therefore assume that change in fluid properties and release of the load causes disturbances in flow and streaming potential. We will discuss results of numerical simulations reproducing the observed effect. Our

  11. Modeling rapid mass movements using the shallow water equations

    Science.gov (United States)

    Hergarten, S.; Robl, J.

    2014-11-01

    We propose a new method to model rapid mass movements on complex topography using the shallow water equations in Cartesian coordinates. These equations are the widely used standard approximation for the flow of water in rivers and shallow lakes, but the main prerequisite for their application - an almost horizontal fluid table - is in general not satisfied for avalanches and debris flows in steep terrain. Therefore, we have developed appropriate correction terms for large topographic gradients. In this study we present the mathematical formulation of these correction terms and their implementation in the open source flow solver GERRIS. This novel approach is evaluated by simulating avalanches on synthetic and finally natural topographies and the widely used Voellmy flow resistance law. The results are tested against analytical solutions and the commercial avalanche model RAMMS. The overall results are in excellent agreement with the reference system RAMMS, and the deviations between the different models are far below the uncertainties in the determination of the relevant fluid parameters and involved avalanche volumes in reality. As this code is freely available and open source, it can be easily extended by additional fluid models or source areas, making this model suitable for simulating several types of rapid mass movements. It therefore provides a valuable tool assisting regional scale natural hazard studies.

  12. Rapidly progressive cryptogenic organising pneumonia presenting as a lung mass

    Science.gov (United States)

    Akram, Saeed; Irfan, Muhammad; Aftab, Kanwal

    2009-01-01

    A very rare case of a rapidly progressive variant of cryptogenic organising pneumonia (COP) presenting as a focal mass-like lesion with compression of the large airways leading to respiratory failure is described. A 60-year-old lady presented to the Aga Khan University Hospital Emergency Department in hypoxaemic respiratory failure with a 6-day history of dyspnoea, productive cough and fever. Chest x ray showed a right upper lobe mass-like lesion compressing the large airways and right pleural effusion. She deteriorated in the Emergency Department and was intubated due to worsening hypoxaemic respiratory failure. The pleural fluid and bronchoscopic specimens were negative on microbiological and cytological examination. CT-guided right lung biopsy revealed chronic non-specific inflammation without granuloma and malignancy. COP was diagnosed on video-assisted thoracoscopic (VATS) lung biopsy. She was successfully treated with high dose steroids and discharged in a stable condition; her 3-month follow-up chest x rays showed complete resolution of the lung lesion with some residual fibrosis. PMID:21686529

  13. [Rapid identification of microorganisms using MALDI-TOF mass spectrometry].

    Science.gov (United States)

    Sogawa, Kazuyuki; Watanabe, Masaharu; Nomura, Fumio

    2013-01-01

    In a clinical diagnostic microbiology laboratory, the current method of identifying bacterial isolates is based mainly on phenotypic characteristics, such as the growth pattern on different media, colony morphology, Gram stain, and various biochemical reactions. These techniques collectively allow high-level accuracy in identifying most bacterial isolates, but they are costly and time-consuming. In our clinical microbiology laboratory, we prospectively assessed the ability of matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) to identify bacterial strains that were routinely isolated from clinical samples. Bacterial colonies obtained from a total of 468 strains of 92 bacterial species isolated at the Department of Clinical Laboratory at Chiba University were directly placed on target MALDI plates, followed by the addition of CHCA matrix solution. The plates were then subjected to MALDI-TOF MS measurement, and the microorganisms were identified by pattern matching by the libraries in the BioTyper 2.0 software. The identification rates at species and genus levels were 91.7% (429/468) and 97.0% (454/468), respectively. MALDI-TOF MS is a rapid, simple, and high-throughput proteomic technique for the identification of a variety of bacterial species. Since colony to colony differences and the effects of culture duration on the results are minimal, it can be implemented in a conventional laboratory setting. Although for some pathogens, the preanalytic processes should be refined and current database should be improved to obtain more accurate results, the MALDI-TOF MS-based method generally performs as well as the conventional methods and is a promising technology in clinical laboratories.

  14. Santé et biens communs : un regard de juriste.

    Directory of Open Access Journals (Sweden)

    Isabelle Moine-Dupuis

    2010-11-01

    Full Text Available La santé constitue un domaine dans lequel les notions de bien commun ou de bien public mondial sont particulièrement pertinentes. Il faut cependant préciser de quels biens il est question. A titre d’exemple, le droit français comporte des notions susceptibles de qualifier le droit aux soins (comme droit inaliénable, ou le médicament, objet de propriété intellectuelle comme de propriété « traditionnelle ». Un droit international des biens de santé peut de la même manière être fondé sur un droit d’usage de chacun sur la molécule qui est la même dans le médicament générique et celui de marque. Une procédure d’accès équivalent aux produits, brevetés ou non, pourrait être mise en œuvre par principe dès la découverte, afin de parvenir rapidement à des prix équitables.Health is a field particularly suitable for notions as commons or public goods. It is necessary however to know which goods may be concerned. For instance, French lawyers use concepts which can be used in order to qualify right to care (as an inalienable right, or medicine as an object of intellectual property as well as “traditional” one. An international law for health goods could be also based on a right of use for each person on the molecule which is the same in the generic drug or in the patented one. A process of “equivalent access” to licensed or free products could be initiated, from the discovery itself to the use, in order to obtain rapidly fair prices.

  15. Rapid maxillary anterior teeth retraction en masse by bone compression: a canine model

    National Research Council Canada - National Science Library

    Liu, Chufeng; Cao, Yang; Liu, Conghua; Zhang, Jincai; Xu, Pingping

    2011-01-01

    The present study sought to establish an animal model to study the feasibility and safety of rapid retraction of maxillary anterior teeth en masse aided by alveolar surgery in order to reduce orthodontic treatment time...

  16. Rapid and generic identification of influenza A and other respiratory viruses with mass spectrometry

    NARCIS (Netherlands)

    Majchrzykiewicz-Koehorst, J.A.; Heikens, E.; Trip, H.; Hulst, A.G.; Jong, A.L. de; Viveen, M.C.; Sedee, N.J.A.; van der Plas, J.; Coenjaerts, F.E.J.; Paauw, A.

    2015-01-01

    The rapid identification of existing and emerging respiratory viruses is crucial in combating outbreaks and epidemics. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is a rapid and reliable identification method in bacterial diagnostics, but has not been

  17. A tendem mass spectrometric approach for determining the structure of molecular species of ceramide in the marine sponge, Haliclona cribricutis

    Digital Repository Service at National Institute of Oceanography (India)

    Tilvi, S.; Majik, M.; Naik, C.G.

    result from plasticizer contamination, most probably from the cap of a bottle of solvent or plastic washing bottles etc. 18 A comparison of signal intensities indicates that the mixture contains a substantial amount of ceramides with molecular..., “Identification and fragmentation study of plasticizers with post-source decay matrix-assisted laser desorption/ ionization mass spectrometry”, Rapid Commun. Mass Spectrom. 17, 783 (2003). 19. K. Mills, A. Johnson and B. Winchester, “Synthesis of novel internal...

  18. Rapid species specific identification and subtyping of Yersinia enterocolitica by MALDI-TOF mass spectrometry.

    Science.gov (United States)

    Stephan, Roger; Cernela, Nicole; Ziegler, Dominik; Pflüger, Valentin; Tonolla, Mauro; Ravasi, Damiana; Fredriksson-Ahomaa, Maria; Hächler, Herbert

    2011-11-01

    Yersinia enterocolitica are Gram-negative pathogens and known as important causes of foodborne infections. Rapid and reliable identification of strains of the species Y. enterocolitica within the genus Yersinia and the differentiation of the pathogenic from the non-pathogenic biotypes has become increasingly important. We evaluated here the application of matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) for rapid species identification and subtyping of Y. enterocolitica. To this end, we developed a reference MS database library including 19 Y. enterocolitica (non-pathogenic biotype 1A and pathogenic biotypes 2 and 4) as well as 24 non-Y. enterocolitica strains, belonging to eleven different other Yersinia spp. The strains provided reproducible and unique mass spectra profiles covering a wide molecular mass range (2000 to 30,000 Da). Species-specific and biotype-specific biomarker protein mass patterns were determined for Y. enterocolitica. The defined biomarker mass patterns (SARAMIS SuperSpectrum™) were validated using 117 strains from various Y. enterocolitica bioserotypes in a blind-test. All strains were correctly identified and for all strains the mass spectrometry-based identification scheme yielded identical results compared to a characterization by a combination of biotyping and serotyping. Our study demonstrates that MALDI-TOF-MS is a reliable and powerful tool for the rapid identification of Y. enterocolitica strains to the species level and allows subtyping of strains to the biotype level. Copyright © 2011 Elsevier B.V. All rights reserved.

  19. measles immunisation growing peri-urban area of a mass a rapidly ...

    African Journals Online (AJOL)

    A mass measles immunisation campaign, with a target coverage rate of 85 - 90%, was launched in Khayelitsha, a rapidly growing urban township in the Cape Town area. Cross-sectional surveys of the measles immunisation status of resident 6 - 23-month-old infants were conducted immediately before, immediately after, ...

  20. Collision-induced fragmentation accurate mass spectrometric analysis methods to rapidly characterize plant extracts

    Science.gov (United States)

    The rapid advances in analytical chromatography equipment have made the reliable and reproducible measurement of a wide range of plant chemical components possible. Full chemical characterization of a given plant material is possible with the new mass spectrometers currently available. For phytochem...

  1. Collision-induced fragmentation accurate mass spectrometric analysis methods to rapidly characterize phytochemicals in plant extracts

    Science.gov (United States)

    The rapid advances in analytical chromatography equipment have made the reliable and reproducible measurement of a wide range of plant chemical components possible. Full chemical characterization of a given plant material is possible with the new mass spectrometers currently available. New methods a...

  2. Rapid analysis of drug dissolution by paper spray ionization mass spectrometry.

    Science.gov (United States)

    Liu, Yang; Liu, Ning; Zhou, Ya-Nan; Lin, Lan; He, Lan

    2017-03-20

    With a great quantity of solid dosage tested by dissolution technology, developing a rapid and sensitive method to access the content of drug within dissolution media is highly desired by analysts and scientists. Traditionally, dissolution media is not compatible with mass spectrometry since the inorganic salts in the media might damage the mass spectrometer. Here, paper spray ionization mass spectrometry (PSI-MS), one of the ambient mass spectrometry technologies, is developed to characterize the content of drugs in dissolution media. The porous structure of paper can effectively retain salts from entering mass spectrometer. This makes the measurement of drug content within dissolution media by mass spectrometer possible. After the experimental parameters were optimized, calibration curves of model drugs - enalapril, quinapril and benazepril were established by using corresponding deuterated internal standards. PSI-MS was then deployed to characterize the content of enalapril from the dissolution testing of enalapril tablets. The results from PSI-MS are comparable to those from HPLC characterization. More importantly, the analysis time of 6 samples is shortened from 90min to 6min. Detection limit of enalapril maleate tablets by PSI-MS is 1/300 of LC. PSI-MS is rapid, sensitive and accurate in analyzing drug content from dissolution tests. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Biens communs, biens publics mondiaux et propriété. Introduction au dossier.

    Directory of Open Access Journals (Sweden)

    Bruno Boidin

    2008-03-01

    Full Text Available Nous proposons d’esquisser les différents enjeux liés au croisement des notions de biens communs et de propriété dans une économie mondialisée. Dans un premier temps un cadrage terminologique est présenté autour de termes juridiques qui font écho à des notions courantes dans l’analyse économique ; il s’agit de montrer l’intérêt d’articuler plusieurs disciplines autour de la question des liens entre biens communs et propriété. Dans un deuxième temps, quelques éclairages sont donnés sur les différentes conceptions des biens communs et des biens publics dits mondiaux ; on cherche ici à souligner à la fois la diversité, voire l’hétérogénéité des approches mais aussi les convergences entre celles-ci. Des perspectives sont ensuite initiées autour des contributions croisées que peuvent apporter les approches institutionnalistes, éthiques et d’économie politique.This article tackles the question of the links between the concepts of common goods and property in the context of globalisation. First we try to define theses different notions in the fields of law and economics. Our aim is to demonstrate the importance of pluridisciplinary approaches to analyse this links. Then we present various conceptions of common goods and public goods, to underline divergences and convergences. Finally we propose some perspectives offered by different heterodox approaches, in particular institutionalism, ethics and political economy.

  4. KariaNet : éclairages sur la mise en commun des connaissances ...

    International Development Research Centre (IDRC) Digital Library (Canada)

    KariaNet est un réseau régional qui cherche à améliorer la mise en commun des connaissances sur l'agriculture et le développement rural afin d'aider les ... était la plus réussie, a contribué à la diffusion des expériences auprès des regroupements d'agriculteurs au Maroc et dans le milieu de la gestion de l'eau en Égypte.

  5. Identification of the Species of Origin for Meat Products by Rapid Evaporative Ionization Mass Spectrometry.

    Science.gov (United States)

    Balog, Julia; Perenyi, Dora; Guallar-Hoyas, Cristina; Egri, Attila; Pringle, Steven D; Stead, Sara; Chevallier, Olivier P; Elliott, Chris T; Takats, Zoltan

    2016-06-15

    Increasingly abundant food fraud cases have brought food authenticity and safety into major focus. This study presents a fast and effective way to identify meat products using rapid evaporative ionization mass spectrometry (REIMS). The experimental setup was demonstrated to be able to record a mass spectrometric profile of meat specimens in a time frame of <5 s. A multivariate statistical algorithm was developed and successfully tested for the identification of animal tissue with different anatomical origin, breed, and species with 100% accuracy at species and 97% accuracy at breed level. Detection of the presence of meat originating from a different species (horse, cattle, and venison) has also been demonstrated with high accuracy using mixed patties with a 5% detection limit. REIMS technology was found to be a promising tool in food safety applications providing a reliable and simple method for the rapid characterization of food products.

  6. [A young man with rapidly progressing dyspnoea and a mediastinal mass].

    Science.gov (United States)

    van Spronsen, D J; van den Berkmortel, F W P J; Bootsma, G P; de Mulder, P H M

    2004-11-13

    An 18-year-old male presented with a 2-week history of rapid progressive dyspnoea and dry cough due to a large mediastinal mass with compression of the trachea. Based on the raised serum values of the tumour markers chorionogonadotrophin and alphafoetoprotein the diagnosis of germ-cell tumour was made. Because of the severity of his symptoms chemotherapy with bleomycin, etoposide and cisplatin was begun on the same day and before the results of the histology investigations were known. The next day the symptoms were diminished and after completing four courses of chemotherapy there was complete remission. The differential diagnosis of a rapid progressive mediastinal mass is limited and mainly relates to malignant lymphoma and germ-cell tumours. In emergency situations if tumour markers are raised then anti-tumour therapy may be begun before any histological confirmation is available.

  7. CONSTRAINTS ON THE MASS AND RADIUS OF THE ACCRETING NEUTRON STAR IN THE RAPID BURSTER

    Energy Technology Data Exchange (ETDEWEB)

    Sala, G.; Jose, J.; Parikh, A.; Longland, R. [Departament de Fisica i Enginyeria Nuclear, EUETIB, Universitat Politecnica de Catalunya, c/ Comte d' Urgell 187, E-08036 Barcelona (Spain); Haberl, F. [Max-Planck-Institut fuer extraterrestrische Physik, Giessenbachstrasse, D-85748 Garching (Germany); Pardo, L. C. [Grup de Caracteritzacio de Materials, Departament de Fisica i Enginyeria Nuclear, ETSEIB, Universitat Politecnica de Catalunya, Diagonal 647, E-08028 Barcelona, Catalonia (Spain); Andersen, M. [Research and Scientific Support Department, European Space Agency, ESTEC, Keplerlaan 1, NL-2200 AG Noordwijk (Netherlands)

    2012-06-20

    The Rapid Burster (MXB 1730-335) is a unique object, showing both type I and type II X-ray bursts. A type I burst of the Rapid Burster was observed with Swift/X-Ray Telescope on 2009 March 5, showing photospheric radius expansion (PRE) for the first time in this source. We report here on the mass and radius determination from this PRE burst using a Bayesian approach. After marginalization over the likely distance of the system (5.8-10 kpc), we obtain M = 1.1 {+-} 0.3 M{sub Sun} and R = 9.6 {+-} 1.5 km (1{sigma} uncertainties) for the compact object, ruling out the stiffest equations of state for the neutron star. We study the sensitivity of the results to the distance, the color correction factor, and the hydrogen mass fraction in the envelope. We find that only the distance plays a crucial role.

  8. The effects in humans of rapid loss of body mass on a boxing-related task.

    Science.gov (United States)

    Smith, M S; Dyson, R; Hale, T; Harrison, J H; McManus, P

    2000-09-01

    The physiological effects of strategies for a rapid loss of body mass immediately before weighing-in for competition in weight-governed sports are unclear. This study examined the effects of a 3%-4% loss in body mass on a boxing-related task. Seven novice amateur boxers completed three 3 min rounds of simulated boxing on a prototype boxing ergometer in an euhydrated state (E-trial) and after exercise-induced thermal dehydration (D-trial). All subjects lost body mass following dehydration-mean body mass fell 3.8 (SD +/- 0.3)% [77.3 (SD +/- 11.3) to 74.4 (SD +/- 10.7) kg, PPV) were inconsistent. Four subjects suffered reductions in PV between 15% and 30%, one subject maintained his E-trial value and two recorded an increase. The D-trial mean PV value was 8.0 (SD +/- 17.2)% lower but this fall was not statistically significant (P>0.05). Analysis of D-trial boxing performance showed one subject maintained his performance over the two trials and a second improved 17.8%. A two-way ANOVA (condition x time) with repeated measures on both factors showed no significant main effect differences for condition (F1,6 = 3.93 P>0.05), time (F1.83,48 = 1.12, P>0.05) or interaction between them (F1.93,48, P>0.05). Furthermore, neither heart rate nor blood lactate responses in the boxing task differed between trials. These data were affected by the small sample. Power and effect size analysis using eta(2) procedure and removing the outlier data produced a mean fall in boxing performance of 26.8%. However, some subjects appeared able to resist the deleterious effects of a rapid loss of body mass prior to competition and further research is needed to explain the mechanisms under-pinning this ability.

  9. Rapid Analysis of Corni fructus Using Paper Spray-Mass Spectrometry.

    Science.gov (United States)

    Guo, Yuan; Gu, Zhixin; Liu, Xuemei; Liu, Jingjing; Ma, Ming; Chen, Bo; Wang, Liping

    2017-07-01

    Paper spray-mass spectrometry (PS-MS) is a kind of ambient MS technique for the rapid analysis of samples. Corni fructus has been widely used in traditional Chinese compound preparations and healthy food. However, a number of counterfeits of Corni fructus, such as Crataegi fructus, Lycii fructus, and grape skin are illegally sold in crude herb markets. Therefore, the development of a rapid and high-throughput quality evaluation method is important for ensuring the effectiveness and safety of the crude materials of Corni fructus. To develop PS-MS chemical profiles and a semi-quantitative method of Corni fructus for quality assessment and control, and species distinction of Corni fructus. Both positive and negative ion PS-MS chemical profiles were constructed for species distinction. The statistical analysis of the chemical profiles was accomplished by principal component analysis (PCA). Rapid semi-quantitative analysis of loganin and morroniside in the extracts of Corni fructus were accomplished by PS-MS. The profiles of the Corni fructus and Crataegi fructus samples were clearly clustered into two categories. The limit of quantification (LOQ) in the semi-quantitative analysis was 6 μg/mL and 5.6 μg/mL for loganin and morroniside, respectively. PS-MS is a simple, rapid, and high-throughput method for the quality control and species distinction of Corni fructus. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  10. Elastic uplift in southeast Greenland due to rapid ice mass loss

    DEFF Research Database (Denmark)

    Khan, Shfaqat Abbas; Van dam, Tonie; Hamilton, Gordon S.

    2007-01-01

    , calculated from sequential digital elevation models, contributes about 16 mm of the observed uplift, with an additional 5 mm from volume loss of Kangerdlugssuaq Glacier. The remaining uplift signal is attributed to significant melt-induced ice volume loss from the ice sheet margin along the southeast coast......The rapid unloading of ice from the southeastern sector of the Greenland ice sheet between 2001 and 2006 caused an elastic uplift of 35 mm at a GPS site in Kulusuk. Most of the uplift results from ice dynamic-induced volume losses on two nearby outlet glaciers. Volume loss from Helheim Glacier...... between 62N and 66N. Citation: Khan, S. A., J. Wahr, L. A. Stearns, G. S. Hamilton, T. van Dam, K. M. Larson, and O. Francis (2007), Elastic uplift in southeast Greenland due to rapid ice mass loss....

  11. Coral mass spawning predicted by rapid seasonal rise in ocean temperature

    KAUST Repository

    Keith, Sally A.

    2016-05-11

    Coral spawning times have been linked to multiple environmental factors; however, to what extent these factors act as generalized cues across multiple species and large spatial scales is unknown. We used a unique dataset of coral spawning from 34 reefs in the Indian and Pacific Oceans to test if month of spawning and peak spawning month in assemblages of Acropora spp. can be predicted by sea surface temperature (SST), photosynthetically available radiation, wind speed, current speed, rainfall or sunset time. Contrary to the classic view that high mean SST initiates coral spawning, we found rapid increases in SST to be the best predictor in both cases (month of spawning: R2 = 0.73, peak: R2 = 0.62). Our findings suggest that a rapid increase in SST provides the dominant proximate cue for coral mass spawning over large geographical scales. We hypothesize that coral spawning is ultimately timed to ensure optimal fertilization success.

  12. Seed oil polyphenols: rapid and sensitive extraction method and high resolution-mass spectrometry identification.

    Science.gov (United States)

    Koubaa, Mohamed; Mhemdi, Houcine; Vorobiev, Eugène

    2015-05-01

    Phenolic content is a primary parameter for vegetables oil quality evaluation, and directly involved in the prevention of oxidation and oil preservation. Several methods have been reported in the literature for polyphenols extraction from seed oil but the approaches commonly used remain manually handled. In this work, we propose a rapid and sensitive method for seed oil polyphenols extraction and identification. For this purpose, polyphenols were extracted from Opuntia stricta Haw seed oil, using high frequency agitation, separated, and then identified using a liquid chromatography-high resolution mass spectrometry method. Our results showed good sensitivity and reproducibility of the developed methods. Copyright © 2015 Elsevier Inc. All rights reserved.

  13. [Rapid detection of antimicrobial resistance by MALDI-TOF mass spectrometry].

    Science.gov (United States)

    Oviaño, Marina; Dolores Rojo, María; Navarro Marí, José María; Bou, Germán

    2016-06-01

    In recent years, MALDI-TOF (matrix-assisted laser desorption ionization time-of-flight) mass spectrometry has become established as a first-line diagnostic tool in the identification of microorganisms, including those producing human infections. Rapid detection of antimicrobial resistance is one of the future applications of this technique with the greatest likelihood of success. This review describes the most important studies published in this field and discusses potential future challenges and the clinical application of this technique in the next few years. Copyright © 2016 Elsevier España, S.L.U. All rights reserved.

  14. Rapid detection of milk adulteration using intact protein flow injection mass spectrometric fingerprints combined with chemometrics.

    Science.gov (United States)

    Du, Lijuan; Lu, Weiying; Cai, Zhenzhen Julia; Bao, Lei; Hartmann, Christoph; Gao, Boyan; Yu, Liangli Lucy

    2018-02-01

    Flow injection mass spectrometry (FIMS) combined with chemometrics was evaluated for rapidly detecting economically motivated adulteration (EMA) of milk. Twenty-two pure milk and thirty-five counterparts adulterated with soybean, pea, and whey protein isolates at 0.5, 1, 3, 5, and 10% (w/w) levels were analyzed. The principal component analysis (PCA), partial least-squares-discriminant analysis (PLS-DA), and support vector machine (SVM) classification models indicated that the adulterated milks could successfully be classified from the pure milks. FIMS combined with chemometrics might be an effective method to detect possible EMA in milk. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Rapid and sensitive liquid chromatography-mass spectrometry method for determination of ropinirole in human plasma.

    Science.gov (United States)

    Bhatt, Jignesh; Jangid, Arvind; Shetty, Raghavendra; Shah, Bhavin; Kambli, Sandeep; Subbaiah, Gunta; Singh, Sadhana

    2006-03-18

    A rapid and robust liquid chromatography-mass spectrometry (LC-MS/MS) method was developed for non-ergoline dopamine D(2)-receptor agonist, ropinirole in human plasma using Es-citalopram oxalate as an internal standard. The method involves solid phase extraction from plasma, reversed-phase simple isocratic chromatographic conditions and mass spectrometric detection that enables a detection limit at picogram levels. The proposed method was validated with linear range of 20-1,200 pg/ml. The extraction recoveries for ropinirole and internal standard were 90.45 and 65.42%, respectively. The R.S.D.% of intra-day and inter-day assay was lower than 15%. For its sensitivity and reliability, the proposed method is particularly suitable for pharmacokinetic studies.

  16. Rapid discrimination of fatty acid composition in fats and oils by electrospray ionization mass spectrometry.

    Science.gov (United States)

    Kurata, Shoji; Yamaguchi, Kazutaka; Nagai, Masatoshi

    2005-12-01

    Fatty acids in 42 types of saponified vegetable and animal oils were analyzed by electrospray ionization mass spectrometry (ESI-MS) for the development of their rapid discrimination. The compositions were compared with those analyzed by gas chromatography-mass spectrometry (GC-MS), a more conventional method used in the discrimination of fats and oils. Fatty acids extracted with 2-propanol were-detected as deprotonated molecular ions ([M-H]-) in the ESI-MS spectra of the negative-ion mode. The composition obtained by ESI-MS corresponded to the data of the total ion chromatograms by GC-MS. The ESI-MS analysis discriminated the fats and oils within only one minute after starting the measurement. The detection limit for the analysis was approximately 10(-10) g as a sample amount analyzed for one minute. This result showed that the ESI-MS analysis discriminated the fats and oils much more rapidly and sensitively than the GC-MS analysis, which requires several tens of minutes and approximately 10(-9) g. Accordingly, the ESI-MS analysis was found to be suitable for a screening procedure for the discrimination of fats and oils.

  17. Modelling rapid mass movements using the shallow water equations in Cartesian coordinates

    Science.gov (United States)

    Hergarten, S.; Robl, J.

    2015-03-01

    We propose a new method to model rapid mass movements on complex topography using the shallow water equations in Cartesian coordinates. These equations are the widely used standard approximation for the flow of water in rivers and shallow lakes, but the main prerequisite for their application - an almost horizontal fluid table - is in general not satisfied for avalanches and debris flows in steep terrain. Therefore, we have developed appropriate correction terms for large topographic gradients. In this study we present the mathematical formulation of these correction terms and their implementation in the open-source flow solver GERRIS. This novel approach is evaluated by simulating avalanches on synthetic and finally natural topographies and the widely used Voellmy flow resistance law. Testing the results against analytical solutions and the proprietary avalanche model RAMMS, we found a very good agreement. As the GERRIS flow solver is freely available and open source, it can be easily extended by additional fluid models or source areas, making this model suitable for simulating several types of rapid mass movements. It therefore provides a valuable tool for assisting regional-scale natural hazard studies.

  18. Rapid and Concomitant Analysis of Pharmaceuticals in Treated Wastewater by Coated Blade Spray Mass Spectrometry.

    Science.gov (United States)

    Poole, Justen J; Gómez-Ríos, German A; Boyaci, Ezel; Reyes-Garcés, Nathaly; Pawliszyn, Janusz

    2017-11-07

    The widespread use of pharmaceuticals in both human and animal populations, and the resultant contamination of surface waters from the outflow of water treatment facilities is an issue of growing concern. This has raised the need for analytical methods that can both perform rapid sample analysis and overcome the limitations of conventional analysis procedures, such as multistep workflows and tedious procedures. Coated blade spray (CBS) is a solid-phase microextraction based technique that enables the direct-to-mass-spectrometry analysis of extracted compounds via the use of limited organic solvent to desorb analytes and perform electrospray ionization. This paper documents how CBS can be applied for the concomitant tandem mass spectrometric (MS/MS) analysis of nine pharmaceuticals in treated wastewater. The total analysis times of less than 11 min provided limits of detection lower than 50 ng L-1 for all target compounds in river water. The CBS methodology was then compared to a conventional solid-phase extraction technique for the analysis of the final effluent of six wastewater treatment facilities. The experimental results strongly suggest that CBS offers scientists a viable alternative method for analyzing water samples that is both rapid and relatively solvent-free.

  19. Rapid fingerprinting of lignin by ambient ionization high resolution mass spectrometry and simplified data mining.

    Science.gov (United States)

    Crawford, Elizabeth A; Gerbig, Stefanie; Spengler, Bernhard; Volmer, Dietrich A

    2017-11-22

    Ambient ionization techniques are typically used to analyze samples in their native states with minimal or no sample pretreatment prior to mass spectrometric (MS) analysis. Desorption electrospray ionization (DESI) and direct analysis in real time (DART) were systematically investigated in this work for direct solid analysis of depolymerized lignin samples, with the goal of rapidly fingerprinting these samples, to efficiently characterize the subunits of this renewable energy source. High resolution MS was required for enhanced selectivity in this study due to the inherent structural complexity of lignin. DESI provided results across a broader mass range (up to m/z 700) than DART and also ionized saturated compounds of low oxygen-to-carbon (O/C) ratios and low double bond equivalents (DBE). While DART detected the same core lignin monomeric and dimeric compounds as seen with DESI and electrospray ionization (ESI), results were restricted to a narrower mass range to m/z 500, due to thermal degradation and losses of methoxy groups. In contrast to DESI and ESI, the DART spectra were nearly void of saturated components. On a structural level, the core lignin compounds were visually fingerprinted and ionization method performances critically assessed by employing simplified Kendrick-based data mining approaches. A novel simplified data visualization approach was developed in this work based on modified Kendrick mass defect (KMD) filtering for lignin subunits and plotting the mass defect values against the degree of unsaturation. Direct visualization of monomeric, dimeric and trimeric lignin species was simplified by the KMD separation plots, easily allowing the core lignin compounds to be visually identified and compared. Modified KMD bases, namely methoxy and phenol bases, which represent monomer-specific lignin constituents, were successfully used to classify and group the complex mixture of lignin species. Further separation of methoxy-related lignin species was

  20. Rapid weight loss and the body fluid balance and hemoglobin mass of elite amateur boxers.

    Science.gov (United States)

    Reljic, Dejan; Hässler, Eike; Jost, Joachim; Friedmann-Bette, Birgit

    2013-01-01

    Dehydration is assumed to be a major adverse effect associated with rapid loss of body mass for competing in a lower weight class in combat sports. However, the effects of such weight cutting on body fluid balance in a real-life setting are unknown. To examine the effects of 5% or greater loss of body mass within a few days before competition on body water, blood volume, and plasma volume in elite amateur boxers. Case-control study. Sports medicine laboratory. Seventeen male boxers (age = 19.2 ± 2.9 years, height = 175.1 ± 7.0 cm, mass = 65.6 ± 9.2 kg) were assigned to the weight-loss group (WLG; n = 10) or the control group (CON; n = 7). The WLG reduced body mass by restricting fluid and food and inducing excessive sweat loss by adhering to individual methods. The CON participated in their usual precompetition training. During an ordinary training period (t-1), 2 days before competition (t-2), and 1 week after competition (t-3), we performed bioelectrical impedance measurements; calculated total body water, intracellular water, and extracellular water; and estimated total hemoglobin mass (tHbmass), blood volume, and plasma volume by the CO-rebreathing method. In the WLG, the loss of body mass (5.6% ± 1.7%) led to decreases in total body water (6.0% ± 0.9%), extracellular water (12.4% ± 7.6%), tHbmass (5.3% ± 3.8%), blood volume (7.6% ± 2.1%; P .05). At t-3, total body water, extracellular water, and plasma volume had returned to near baseline values, but tHbmass and blood volume still were less than baseline values (P .05). In a real-life setting, the loss of approximately 6% body mass within 5 days induced hypohydration, which became evident by the decreases in body water and plasma volume. The reduction in tHbmass was a surprising observation that needs further investigation.

  1. L'aiguillat commun (Squalus acanthias) dans le nord-est du Pacifique et histoire de son utilisation

    National Research Council Canada - National Science Library

    Ketchen, K. S

    1986-01-01

    ... présent rapport passe en revue la taxonomie, la distribution, les migrations, la définition des stocks et le cycle vital de l'aiguillat commun dans le contexte d'un compte rendu de son utilisation à travers les...

  2. Le paysage dans l’action publique : du patrimoine au bien commun

    Directory of Open Access Journals (Sweden)

    Anne Sgard

    2010-09-01

    Full Text Available Le paysage est dorénavant partie prenante des politiques publiques locales, souvent affiché au cœur même du projet de territoire. Cependant le débat reste largement ouvert dès lors qu’il s’agit de préciser à quoi « sert le paysage » et de lui associer une/des valeurs particulières, susceptibles de porter et de légitimer la problématique paysagère au cours du montage du projet. Ce texte part du constat que deux termes sont de manière récurrente associés au paysage, le patrimoine et, plus récemment, le bien commun, et se propose d’interroger cette orientation du discours sur le paysage. La pratique et le cadre juridique français, tendent à enfermer le paysage dans un registre avant tout patrimonial, privilégiant une logique de protection. L’expression de bien commun pose question : est-ce un équivalent de patrimoine, une facilité de langage portée par la mode, ou un apport innovant qui permet de réinterroger la place du paysage dans le débat et les méthodes d’intervention? Revenant sur les cadres théoriques de la réflexion sur les biens communs et sur sa diffusion actuelle dans l’ensemble des sciences sociales et environnementales, ce texte cherchera à identifier ce qu’elle peut apporter à la compréhension de la place du paysage dans les projets, en mettant notamment l’accent sur la question de l’accessibilité et de la négociation.The landscape is now part of local public policies, often displayed at the very heart of territorial projects. But the debate remains wide open when it comes to specifying what should be the use of “landscape" and to determine with which particular value, in order to legitimize the thematic of landscape in the building of the territorial project. This text is based on the observation that two notions are consistently associated with landscape: heritage and, more recently, common good. We propose to examine the effect of these notions on the contemporary discourses

  3. Rapid confirmatory analysis of avermectin residues in milk by liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Nurullah Ozdemir

    2016-01-01

    Full Text Available Our study developed a quick method for confirmatory analysis of avermectins (abamectin B1a, doramectin, ivermectin B1a, eprinomectin B1a, and moxidectin in bovine milk according to the European Commission Decision 2002/657/EC requirements. Avermectins were liquid–liquid extracted with acetonitrile, followed by an evaporation step, and then analyzed by liquid chromatography/electrospray ionization tandem mass spectrometry in the negative ion mode. An in-house method validation was performed and the data reported on specificity, linearity, recovery, limit of detection, limit of quantitation, decision limit, and detection capability. The advantage of this method is that low levels of avermectins are detectable and quantitatively confirmed at a rapid rate in milk.

  4. The Impacts of the Mass Rapid Transit System on Household Car Ownership in Taipei

    Directory of Open Access Journals (Sweden)

    Wen-Hsiu Huang

    2014-06-01

    Full Text Available This paper investigates the impacts of Taipei Mass Rapid Transit (MRT system on household car ownership and analyses how socioeconomic characteristics affect household car ownership. We employ a difference-in-difference (DID strategy integrated with generalized Poisson regression models to examine the effects of MRT. The results are as follows: first, the establishment of Taipei MRT significantly reduced the level of household car ownership. Expanding the network of MRT system can be a feasible policy to control car ownership. Second, the levels of household car ownership are related to household’s socioeconomic characteristics. Third, households with high dependence on public transport own fewer cars after Taipei MRT began operation. Hence, the traffic authority should adopt more effective methods to encourage public transit use in order to decrease household car ownership.

  5. Rapid maxillary anterior teeth retraction en masse by bone compression: a canine model.

    Directory of Open Access Journals (Sweden)

    Chufeng Liu

    Full Text Available OBJECTIVE: The present study sought to establish an animal model to study the feasibility and safety of rapid retraction of maxillary anterior teeth en masse aided by alveolar surgery in order to reduce orthodontic treatment time. METHOD: Extraction of the maxillary canine and alveolar surgery were performed on twelve adult beagle dogs. After that, the custom-made tooth-borne distraction devices were placed on beagles' teeth. Nine of the dogs were applied compression at 0.5 mm/d for 12 days continuously. The other three received no force as the control group. The animals were killed in 1, 14, and 28 days after the end of the application of compression. RESULTS: The tissue responses were assessed by craniometric measurement as well as histological examination. Gross alterations were evident in the experimental group, characterized by anterior teeth crossbite. The average total movements of incisors within 12 days were 4.63±0.10 mm and the average anchorage losses were 1.25±0.12 mm. Considerable root resorption extending into the dentine could be observed 1 and 14 days after the compression. But after consolidation of 28 days, there were regenerated cementum on the dentine. There was no apparent change in the control group. No obvious tooth loosening, gingival necrosis, pulp degeneration, or other adverse complications appeared in any of the dogs. CONCLUSIONS: This is the first experimental study for testing the technique of rapid anterior teeth retraction en masse aided by modified alveolar surgery. Despite a preliminary animal model study, the current findings pave the way for the potential clinical application that can accelerate orthodontic tooth movement without many adverse complications. CLINICAL RELEVANCE: It may become a novel method to shorten the clinical orthodontic treatment time in the future.

  6. Classification of Bacillus and Brevibacillus species using rapid analysis of lipids by mass spectrometry.

    Science.gov (United States)

    AlMasoud, Najla; Xu, Yun; Trivedi, Drupad K; Salivo, Simona; Abban, Tom; Rattray, Nicholas J W; Szula, Ewa; AlRabiah, Haitham; Sayqal, Ali; Goodacre, Royston

    2016-11-01

    Bacillus are aerobic spore-forming bacteria that are known to lead to specific diseases, such as anthrax and food poisoning. This study focuses on the characterization of these bacteria by the detection of lipids extracted from 33 well-characterized strains from the Bacillus and Brevibacillus genera, with the aim to discriminate between the different species. For the purpose of analysing the lipids extracted from these bacterial samples, two rapid physicochemical techniques were used: matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF-MS) and liquid chromatography in conjunction with mass spectrometry (LC-MS). The findings of this investigation confirmed that MALDI-TOF-MS could be used to identify different bacterial lipids and, in combination with appropriate chemometrics, allowed for the discrimination between these different bacterial species, which was supported by LC-MS. The average correct classification rates for the seven species of bacteria were 62.23 and 77.03 % based on MALDI-TOF-MS and LC-MS data, respectively. The Procrustes distance for the two datasets was 0.0699, indicating that the results from the two techniques were very similar. In addition, we also compared these bacterial lipid MALDI-TOF-MS profiles to protein profiles also collected by MALDI-TOF-MS on the same bacteria (Procrustes distance, 0.1006). The level of discrimination between lipids and proteins was equivalent, and this further indicated the potential of MALDI-TOF-MS analysis as a rapid, robust and reliable method for the classification of bacteria based on different bacterial chemical components. Graphical abstract MALDI-MS has been successfully developed for the characterization of bacteria at the subspecies level using lipids and benchmarked against HPLC.

  7. Rapid screening of Alternaria mycotoxins using MALDI-TOF mass spectrometry.

    Science.gov (United States)

    Sivagnanam, Kumaran; Komatsu, Emy; Rampitsch, Christoph; Perreault, Hélène; Gräfenhan, Tom

    2017-01-01

    Members of the Alternaria genus produce various toxins whose occurrence in agricultural commodities is a major concern for humans and the environment. The present study developed a simple and efficient matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) method for the rapid detection of Alternaria toxins. A new method for the detection of alternariol (AOH), alternariol monomethyl ether (AME) and tentoxin (TEN) by MALDI-TOF MS was developed. Different solid phase extraction (SPE) clean-up methods were tried to optimize the purification of wheat matrix, and an optimal extraction method was designed to recover the three Alternaria toxins. In addition, various MALDI matrices were examined and α-cyano-4-hydroxycinnamic acid (CHCA) matrix gave good repeatability for all three Alternaria toxins. This is the first study to report the detection of three important Alternaria toxins concurrently using MALDI-TOF MS and opens up the possibility of rapid screening of Alternaria toxins in several other cereals and food products. © 2016 Her Majesty the Queen in Right of Canada Journal of the Science of Food and Agriculture © 2016 Society of Chemical Industry. © 2016 Her Majesty the Queen in Right of Canada Journal of the Science of Food and Agriculture © 2016 Society of Chemical Industry.

  8. [Rapid determination of volatile organic compounds in workplace air by protable gas chromatography-mass spectrometer].

    Science.gov (United States)

    Zhu, H B; Su, C J; Tang, H F; Ruan, Z; Liu, D H; Wang, H; Qian, Y L

    2017-10-20

    Objective: To establish a method for rapid determination of 47 volatile organic compounds in the air of workplace using portable gas chromatography-mass spectrometer(GC-MS). Methods: The mixed standard gas with different concentration levels was made by using the static gas distribution method with the high purity nitrogen as dilution gas. The samples were injected into the GC-MS by a hand-held probe. Retention time and characteristic ion were used for qualitative analysis,and the internal standard method was usd for quantitation. Results: The 47 poisonous substances were separated and determined well. The linear range of this method was 0.2-16.0 mg/m(3),and the relative standard deviation of 45 volatile ovganic compounds was 3.8%-15.8%. The average recovery was 79.3%-119.0%. Conclusion: The method is simple,accurate,sensitive,has good separation effect,short analysis period, can be used for qualitative and quantitative analysis of volatile organic compounds in the workplace, and also supports the rapid identification and detection of occupational hazards.

  9. [Rapid identification of microorganisms by mass spectrometry in a blood culture system. Comparison of two procedures].

    Science.gov (United States)

    Cattani, María E; Posse, Tamara; Hermes, Ricardo L; Kaufman, Sara C

    2015-01-01

    Rapid identification of microorganisms is critical in hospitalized infected patients. Blood culture is currently the gold standard for detecting and identifying microorganisms causing bacteremia or sepsis. The introduction of mass spectrometry by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF MS) in microbiology laboratories, especially in microorganisms growing in blood culture bottles, provides rapid identification. This study evaluates the performance of the Maldi Sepsityper Biotyper procedure (hereinafter, MS) compared to that of an in-home method (hereinafter, HF). Eight hundred and forty (840) positive blood culture bottles were processed using the HF procedure, 542 of which were also processed using MS. The organisms were identified in 670 (79.76%) and 391 (72.14%) bottles respectively (p = 0,0013). This study demonstrates the effectiveness of both procedures for identifying microorganisms directly from positive blood culture bottles. However, the HF procedure proved to be more effective than MS, especially in the presence of Gram positive organisms. Copyright © 2015 Asociación Argentina de Microbiología. Publicado por Elsevier España, S.L.U. All rights reserved.

  10. Rapid determination of uranium isotopes in urine by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Shi, Y; Dai, X; Collins, R; Kramer-Tremblay, S

    2011-08-01

    Following a radiological or nuclear emergency involving uranium exposure, rapid analytical methods are needed to analyze the concentration of uranium isotopes in human urine samples for early dose assessment. The inductively coupled plasma mass spectrometry (ICP-MS) technique, with its high sample throughput and high sensitivity, has advantages over alpha spectrometry for uranium urinalysis after minimum sample preparation. In this work, a rapid sample preparation method using an anion exchange chromatographic column was developed to separate uranium from the urine matrix. A high-resolution sector field ICP-MS instrument, coupled with a high sensitivity desolvation sample introduction inlet, was used to determine uranium isotopes in the samples. The method can analyze up to 24 urine samples in two hours with the limits of detection of 0.0014, 0.10, and 2.0 pg mL(-1) for (234)U, (235)U, and (238)U, respectively, which meet the requirement for isotopic analysis of uranium in a radiation emergency.

  11. Rapid and reliable discrimination between Shigella species and Escherichia coli using MALDI-TOF mass spectrometry.

    Science.gov (United States)

    Paauw, Armand; Jonker, Debby; Roeselers, Guus; Heng, Jonathan M E; Mars-Groenendijk, Roos H; Trip, Hein; Molhoek, E Margo; Jansen, Hugo-Jan; van der Plas, Jan; de Jong, Ad L; Majchrzykiewicz-Koehorst, Joanna A; Speksnijder, Arjen G C L

    2015-01-01

    E. coli-Shigella species are a cryptic group of bacteria in which the Shigella species are distributed within the phylogenetic tree of E. coli. The nomenclature is historically based and the discrimination of these genera developed as a result of the epidemiological need to identify the cause of shigellosis, a severe disease caused by Shigella species. For these reasons, this incorrect classification of shigellae persists to date, and the ability to rapidly characterize E. coli and Shigella species remains highly desirable. Until recently, existing matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF MS) assays used to identify bacteria could not discriminate between E. coli and Shigella species. Here we present a rapid classification method for the E. coli-Shigella phylogroup based on MALDI-TOF MS which is supported by genetic analysis. E. coli and Shigella isolates were collected and genetically characterized by MLVA. A custom reference library for MALDI-TOF MS that represents the genetic diversity of E. coli and Shigella strains was developed. Characterization of E. coli and Shigella species is based on an approach with Biotyper software. Using this reference library it was possible to distinguish between Shigella species and E. coli. Of the 180 isolates tested, 94.4% were correctly classified as E. coli or shigellae. The results of four (2.2%) isolates could not be interpreted and six (3.3%) isolates were classified incorrectly. The custom library extends the existing MALDI-TOF MS method for species determination by enabling rapid and accurate discrimination between Shigella species and E. coli. Copyright © 2015 Elsevier GmbH. All rights reserved.

  12. Mass Spectral Profile for Rapid Differentiating Beta-Lactams from Their Ring-Opened Impurities

    Directory of Open Access Journals (Sweden)

    Hecheng Wang

    2015-01-01

    Full Text Available High performance liquid chromatography tandem mass spectrometry (HPLC MS has been widely used for β-lactam antibiotics determination. However, its application to identify impurities of these frequently used drugs is not sufficient at present. In this job, characteristic profiles of the collision induced dissociation (CID spectra of both β-lactams and ring-opened β-lactams were extracted from the MS data of six β-lactam antibiotics and their forty-five impurities, and were confirmed by the MS data reported in the literature. These characteristics have been successfully applied to rapid differentiation of β-lactam and ring-opened β-lactam impurities in cefixime, cefdinir, and cefaclor. However, these characteristic profiles can only be obtained under low activating voltage. They did not display in the high energy activated CID spectra. Diagnostic fragmentations for determining the localization of double bond and substituents on the thiazine ring and the side chain were also observed. In addition, several characteristic fragmentations are hopeful to be used to differentiate the configurations of C-2 on the thiazine ring of ring-opened impurities, which is generally disadvantageous of mass spectrometry. Taken together, forty-five impurities were identified from the capsules of cefixime, cefdinir, and cefaclor.

  13. The Formation of Rapidly Rotating Black Holes in High-mass X-Ray Binaries

    Science.gov (United States)

    Batta, Aldo; Ramirez-Ruiz, Enrico; Fryer, Chris

    2017-09-01

    High-mass X-ray binaries (HMXRBs), such as Cygnus X-1, host some of the most rapidly spinning black holes (BHs) known to date, reaching spin parameters a≳ 0.84. However, there are several effects that can severely limit the maximum BH spin parameter that could be obtained from direct collapse, such as tidal synchronization, magnetic core-envelope coupling, and mass loss. Here, we propose an alternative scenario where the BH is produced by a failed supernova (SN) explosion that is unable to unbind the stellar progenitor. A large amount of fallback material ensues, whose interaction with the secondary naturally increases its overall angular momentum content, and therefore the spin of the BH when accreted. Through SPH hydrodynamic simulations, we studied the unsuccessful explosion of an 8 {M}⊙ pre-SN star in a close binary with a 12 {M}⊙ companion with an orbital period of ≈1.2 days, finding that it is possible to obtain a BH with a high spin parameter a≳ 0.8 even when the expected spin parameter from direct collapse is a≲ 0.3. This scenario also naturally explains the atmospheric metal pollution observed in HMXRB stellar companions.

  14. Mass Housing Using GFRG Panels: A Sustainable, Rapid and Affordable Solution

    Science.gov (United States)

    Cherian, Philip; Paul, Shinto; Krishna, S. R. Gouri; Menon, Devdas; Meher Prasad, A.

    2017-06-01

    This work gives an overview of research and development carried out at IIT Madras, using glass fibre reinforced gypsum (GFRG) panels, to provide an innovative solution for rapid and affordable mass housing. The GFRG panels (124 mm thick), made from recycled industrial waste gypsum (from the fertilizer industry), are prefabricated in 3 m × 12 m sizes with cellular cavities inside, which can be filled with reinforced concrete wherever required and can be used as walls as well as floor slabs. The tests carried out (over the past 12 years) establish the performance of GFRG building systems to resist gravity and lateral loads as a load-bearing system (without beams and columns) in multi-storeyed buildings up to 8-10 storeys, with adequate strength, serviceability, durability and ductility. A two-storeyed four-apartment demonstration building has also been successfully constructed in the IIT Madras campus and presently a mass housing scheme (40 apartment units) using this technology is being demonstrated at Nellore. A structural design code has also been approved by the Bureau of Indian Standards, based on the extensive studies carried out on GFRG building systems.

  15. ACUTE EFFECTS OF SELF-SELECTED REGIMEN OF RAPID BODY MASS LOSS IN COMBAT SPORTS ATHLETES

    Directory of Open Access Journals (Sweden)

    Jaan Ereline

    2008-06-01

    Full Text Available The purpose of the study was to assess the acute effects of the self-selected regimen of rapid body mass loss (RBML on muscle performance and metabolic response to exercise in combat sports athletes. Seventeen male athletes (20.8 ± 1.0 years; mean ± SD reduced their body mass by 5.1 ± 1.1% within 3 days. The RBML was achieved by a gradual reduction of energy and fluid intake and mild sauna procedures. A battery of tests was performed before (Test 1 and immediately after (Test 2 RBML. The test battery included the measurement of the peak torque of knee extensors for three different speeds, assessment of total work (Wtot performed during a 3-min intermittent intensity knee extension exercise and measurements of blood metabolites (ammonia, lactate, glucose and urea. Absolute peak torque was lower in Test 2 compared with Test 1 at angular velocities of 1.57 rad·s-1 (218.6 ± 40.9 vs. 234.4 ± 42.2 N·m; p = 0.013 and 3.14 rad·s-1 (100.3 ± 27.8 vs. 111.7 ± 26.2 N·m; p = 0.008. The peak torque in relation to body mass remained unchanged for any speed. Absolute Wtot was lower in Test 2 compared with Test 1 (6359 ± 2326 vs. 7452 ± 3080 J; p = 0.003 as well as Wtot in relation to body mass (89.1 ± 29.9 vs. 98.6 ± 36.4 J·kg-1; p = 0.034, respectively. As a result of RBML, plasma urea concentration increased from 4.9 to 5.9 mmol·l-1 (p = 0.003. The concentration of ammonia in a post-test sample in Test 2 tended to be higher in comparison with Test 1 (80.9 ± 29.1 vs. 67.6 ± 26.5 mmol·l-1; p = 0.082. The plasma lactate and glucose responses to exercise were similar in Test 1 and Test 2. We conclude that the self-selected regimen of RBML impairs muscle performance in 3-min intermittent intensity exercise and induces an increase in blood urea concentration in experienced male combat sports athletes

  16. ADVANTAGES OF RAPID METHOD FOR DETERMINING SCALE MASS AND DECARBURIZED LAYER OF ROLLED COIL STEEL

    Directory of Open Access Journals (Sweden)

    E. V. Parusov

    2016-08-01

    Full Text Available Purpose. To determine the universal empirical relationships that allow for operational calculation of scale mass and decarbonized layer depth based on the parameters of the technological process for rolled coil steel production. Methodology. The research is carried out on the industrial batches of the rolled steel of SAE 1006 and SAE 1065 grades. Scale removability was determined in accordance with the procedure of «Bekaert» company by the specifi-cations: GA-03-16, GA-03-18, GS-03-02, GS-06-01. The depth of decarbonized layer was identified in accordance with GOST 1763-68 (M method. Findings. Analysis of experimental data allowed us to determine the rational temperature of coil formation of the investigated steel grades, which provide the best possible removal of scale from the metal surface, a minimal amount of scale, as well as compliance of the metal surface color with the require-ments of European consumers. Originality. The work allowed establishing correlation of the basic quality indicators of the rolled coil high carbon steel (scale mass, depth of decarbonized layer and inter-laminar distance in pearlite with one of the main parameters (coil formation temperature of the deformation and heat treatment mode. The re-sulting regression equations, without metallographic analysis, can be used to determine, with a minimum error, the quantitative values of the total scale mass, depth of decarbonized layer and the average inter-lamellar distance in pearlite of the rolled coil high carbon steel. Practical value. Based on the specifications of «Bekaert» company (GA-03-16, GA-03-18, GS-03-02 and GS-06-01 the method of testing descaling by mechanical means from the surface of the rolled coil steel of low- and high-carbon steel grades was developed and approved in the environment of PJSC «ArcelorMittal Kryvyi Rih». The work resulted in development of the rapid method for determination of total and remaining scale mass on the rolled coil steel

  17. Rapid quality assessment of Radix Aconiti Preparata using direct analysis in real time mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Hongbin; Wang Chunyan; Qi Yao [Changchun Center of Mass Spectrometry and Chemical Biology Laboratory, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); University of Chinese Academy of Sciences, Beijing 100039 (China); Song Fengrui, E-mail: songfr@ciac.jl.cn [Changchun Center of Mass Spectrometry and Chemical Biology Laboratory, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China); Liu Zhiqiang; Liu Shuying [Changchun Center of Mass Spectrometry and Chemical Biology Laboratory, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022 (China)

    2012-11-08

    Highlights: Black-Right-Pointing-Pointer DART MS combined with PCA and HCA was used to rapidly identify markers of Radix Aconiti. Black-Right-Pointing-Pointer The DART MS behavior of six aconitine-type alkaloids was investigated. Black-Right-Pointing-Pointer Chemical markers were recognized between the qualified and unqualified samples. Black-Right-Pointing-Pointer DART MS was shown to be an effective tool for quality control of Radix Aconiti Preparata. - Abstract: This study presents a novel and rapid method to identify chemical markers for the quality control of Radix Aconiti Preparata, a world widely used traditional herbal medicine. In the method, the samples with a fast extraction procedure were analyzed using direct analysis in real time mass spectrometry (DART MS) combined with multivariate data analysis. At present, the quality assessment approach of Radix Aconiti Preparata was based on the two processing methods recorded in Chinese Pharmacopoeia for the purpose of reducing the toxicity of Radix Aconiti and ensuring its clinical therapeutic efficacy. In order to ensure the safety and effectivity in clinical use, the processing degree of Radix Aconiti should be well controlled and assessed. In the paper, hierarchical cluster analysis and principal component analysis were performed to evaluate the DART MS data of Radix Aconiti Preparata samples in different processing times. The results showed that the well processed Radix Aconiti Preparata, unqualified processed and the raw Radix Aconiti could be clustered reasonably corresponding to their constituents. The loading plot shows that the main chemical markers having the most influence on the discrimination amongst the qualified and unqualified samples were mainly some monoester diterpenoid aconitines and diester diterpenoid aconitines, i.e. benzoylmesaconine, hypaconitine, mesaconitine, neoline, benzoylhypaconine, benzoylaconine, fuziline, aconitine and 10-OH-mesaconitine. The established DART MS approach in

  18. MALDI-TOF mass spectrometry for the rapid identification of aetiological agents of sepsis

    Directory of Open Access Journals (Sweden)

    Roberto Degl’Innocenti

    2013-04-01

    Full Text Available Introduction: The MALDI-TOF has recently become part of the methods of microbiological investigation in many laboratories of bacteriology with advantages both practical and economical.The use of this technique for the rapid identification of the causative agents of sepsis is of strategic importance to the ability to provide the clinician with useful information for a prompt and rapid establishment of an empirical antimicrobial “targeted” therapy. Methods: It was tested a total of 343 positive blood culture bottles from 211 patients. The samples after collection were incubated in the BACTEC FX (Becton Dickinson, USA. From these bottles were taken a few milliliters of broth culture and transferred into a vacutainer tube containing gel. This was centrifuged, the supernatant was decanted, and finally recovered the bacterial suspension on the gel. With micro-organisms recovered in this way, after several washes with distilled water, was prepared a slide for microscopic examination with Gram stain, and a plate for mass spectrometry (MS-Vitek, bioMérieux, France.Then, the same samples were inoculated on solid agar media according to the protocol in use in our laboratory.The next day was checked the possible bacterial growth on solid media; we then proceeded to the identification of the colonies by Vitek MS and / or with the system Vitek2 (bioMérieux, France. Results: 258 (75.2% positive vials show concordant results between direct identification and identification after growth on agar. For 83 (24.2% positive bottles there has been full compliance with the microscopic examination but not with culture. In particular, two bottles (0.6% have given complete discordance between the direct identification and that after growth. Conclusions: The protocol we use for the direct identification of organisms responsible for sepsis, directly on positive bottles, seems to be a quick and inexpensive procedure, which in less than 60 minutes can give valuable

  19. A real time metabolomic profiling approach to detecting fish fraud using rapid evaporative ionisation mass spectrometry.

    Science.gov (United States)

    Black, Connor; Chevallier, Olivier P; Haughey, Simon A; Balog, Julia; Stead, Sara; Pringle, Steven D; Riina, Maria V; Martucci, Francesca; Acutis, Pier L; Morris, Mike; Nikolopoulos, Dimitrios S; Takats, Zoltan; Elliott, Christopher T

    2017-01-01

    Fish fraud detection is mainly carried out using a genomic profiling approach requiring long and complex sample preparations and assay running times. Rapid evaporative ionisation mass spectrometry (REIMS) can circumvent these issues without sacrificing a loss in the quality of results. To demonstrate that REIMS can be used as a fast profiling technique capable of achieving accurate species identification without the need for any sample preparation. Additionally, we wanted to demonstrate that other aspects of fish fraud other than speciation are detectable using REIMS. 478 samples of five different white fish species were subjected to REIMS analysis using an electrosurgical knife. Each sample was cut 8-12 times with each one lasting 3-5 s and chemometric models were generated based on the mass range m/z 600-950 of each sample. The identification of 99 validation samples provided a 98.99% correct classification in which species identification was obtained near-instantaneously (≈ 2 s) unlike any other form of food fraud analysis. Significant time comparisons between REIMS and polymerase chain reaction (PCR) were observed when analysing 6 mislabelled samples demonstrating how REIMS can be used as a complimentary technique to detect fish fraud. Additionally, we have demonstrated that the catch method of fish products is capable of detection using REIMS, a concept never previously reported. REIMS has been proven to be an innovative technique to help aid the detection of fish fraud and has the potential to be utilised by fisheries to conduct their own quality control (QC) checks for fast accurate results.

  20. Rapid Mass Spectrometric Analysis of a Novel Fucoidan, Extracted from the Brown Alga Coccophora langsdorfii

    Directory of Open Access Journals (Sweden)

    Stanislav D. Anastyuk

    2014-01-01

    Full Text Available The novel highly sulfated (35% fucoidan fraction Cf2 , which contained, along with fucose, galactose and traces of xylose and uronic acids was purified from the brown alga Coccophora langsdorfii. Its structural features were predominantly determined (in comparison with fragments of known structure by a rapid mass spectrometric investigation of the low-molecular-weight fragments, obtained by “mild” (5 mg/mL and “exhaustive” (maximal concentration autohydrolysis. Tandem matrix-assisted laser desorption/ionization mass spectra (MALDI-TOF/TOFMS of fucooligosaccharides with even degree of polymerization (DP, obtained by “mild” autohydrolysis, were the same as that observed for fucoidan from Fucus evanescens, which have a backbone of alternating (1 → 3- and (1 → 4 linked sulfated at C-2 and sometimes at C-4 of 3-linked α-L-Fucp residues. Fragmentation patterns of oligosaccharides with odd DP indicated sulfation at C-2 and at C-4 of (1 → 3 linked α-L-Fucp residues on the reducing terminus. Minor sulfation at C-3 was also suggested. The “exhaustive” autohydrolysis allowed us to observe the “mixed” oligosaccharides, built up of fucose/xylose and fucose/galactose. Xylose residues were found to occupy both the reducing and nonreducing termini of FucXyl disaccharides. Nonreducing galactose residues as part of GalFuc disaccharides were found to be linked, possibly, by 2-type of linkage to fucose residues and were found to be sulfated, most likely, at position C-2.

  1. Rapid quantification of ionophores in feeds by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Huang, Min; Rumbeiha, Wilson K; Braselton, W Emmett; Johnson, Margaret

    2011-09-01

    Ionophores are widely used in veterinary medicine as coccidiostats and for improving nutrient utilization in livestock production. Because of widespread use, ionophores sometimes cause poisoning in livestock. Quantifying concentration of these compounds in feeds for diagnostic purposes is needed. A method with a single step of solvent extraction was developed for rapid simultaneous quantification of monensin, lasalocid, salinomycin, and narasin in feeds by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The ionophores were extracted using methanol:water (90:10). With the high specificity and high sensitivity of tandem mass spectrometry, the extract was introduced for measurement without further processing. The effect of particle size of feeds on extraction efficiency was also investigated. It was found that feeds passing through a 1-mm filter or sieve show better quantitative extraction. Nigericin was used as internal standard for the measurement. The method was validated by fortification of the selected ionophore compounds in horse feed at different concentrations. The typical recovery rate was 69-122%. Meanwhile, various interlaboratory proficiency test samples of different matrices were also quantified as part of the procedure for method validation. A good agreement was found between results and the suggested values. The method is very sensitive, with detection limits between 0.018 µg/g and 0.056 µg/g for the compounds tested. Results showed that the lower limit of quantification was 0.2 µg/g for the ionophore compounds, which is much lower than the contents of the ionophores in medicated feeds, which is generally approximately 10-100 µg/g feed.

  2. Rapid screening of clenbuterol in urine samples by desorption electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Lin, Ziqing; Zhang, Sichun; Zhao, Mengxia; Yang, Chengdui; Chen, Depu; Zhang, Xinrong

    2008-06-01

    Rapid screening of clenbuterol in urine was performed by combining desorption electrospray ionization (DESI) and tandem mass spectrometry (MS/MS). Optimization experiments were carried out including the selection of substrates, spray solutions, nebulizing gas pressures, high-voltage power supplies and flow rates of spray solution. The limit of detection (LOD), defined as the lowest quantity that can be detected, was 5.0 pg for the pure compound. Using DESI coupled with solid-phase extraction (SPE), the linear response range was from 10 to 400 ng/mL (R(2) = 0.993) and the concentration LOD for urine sample was 2.0 ng/mL. The analysis for one spiked urine sample was achieved within 4 min. In addition to the fast analysis speed, MS/MS provided structural information for the confirmation of clenbuterol. Urine samples from different people were investigated and the recoveries were within 100 +/- 20%. The developed method can potentially be used for screening of clenbuterol in doping control.

  3. Rapid and high-throughput pan-Orthopoxvirus detection and identification using PCR and mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Mark W Eshoo

    2009-07-01

    Full Text Available The genus Orthopoxvirus contains several species of related viruses, including the causative agent of smallpox (Variola virus. In addition to smallpox, several other members of the genus are capable of causing human infection, including monkeypox, cowpox, and other zoonotic rodent-borne poxviruses. Therefore, a single assay that can accurately identify all orthopoxviruses could provide a valuable tool for rapid broad orthopovirus identification. We have developed a pan-Orthopoxvirus assay for identification of all members of the genus based on four PCR reactions targeting Orthopoxvirus DNA and RNA helicase and polymerase genes. The amplicons are detected using electrospray ionization-mass spectrometry (PCR/ESI-MS on the Ibis T5000 system. We demonstrate that the assay can detect and identify a diverse collection of orthopoxviruses, provide sub-species information and characterize viruses from the blood of rabbitpox infected rabbits. The assay is sensitive at the stochastic limit of PCR and detected virus in blood containing approximately six plaque-forming units per milliliter from a rabbitpox virus-infected rabbit.

  4. Potential of short-column liquid chromatographia with tandem mass spectrometric detection for the rapid study of pesticide degradation

    NARCIS (Netherlands)

    Hogenboom, A.C.; Steen, R.J.C.A.; Niessen, W.M.A.; Brinkman, U.A.T.

    1998-01-01

    The applicability of solid-phase extraction-LC using two short columns (SPE-LC) and/or single-short-column liquid chromatography (SSC) combined on- line with tandem mass spectrometry (MS) was demonstrated for the rapid study of pesticide degradation. A fast analytical procedure was developed to

  5. Rapid detection of undesired cosmetic ingredients by matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Ouyang, Jie; An, Dongli; Chen, Tengteng; Lin, Zhiwei

    2017-10-01

    In recent years, cosmetic industry profits soared due to the widespread use of cosmetics, which resulted in illicit manufacturers and products of poor quality. Therefore, the rapid and accurate detection of the composition of cosmetics has become crucial. At present, numerous methods, such as gas chromatography and liquid chromatography-mass spectrometry, were available for the analysis of cosmetic ingredients. However, these methods present several limitations, such as failure to perform comprehensive and rapid analysis of the samples. Compared with other techniques, matrix-assisted laser desorption ionization time-of-flight mass spectrometry offered the advantages of wide detection range, fast speed and high accuracy. In this article, we briefly summarized how to select a suitable matrix and adjust the appropriate laser energy. We also discussed the rapid identification of undesired ingredients, focusing on antibiotics and hormones in cosmetics.

  6. Urban Air Pollution in Taiwan before and after the Installation of a Mass Rapid Transit System.

    Science.gov (United States)

    Ding, Pei-Hsiou; Wang, Gen-Shuh; Chen, Bing-Yu; Wan, Gwo-Hwa

    2016-09-01

    Urbanization causes air pollution in metropolitan areas, coupled with meteorological factors that affect air quality. Although previous studies focused on the relationships of urbanization, air pollution, and climate change in Western countries, this study evaluated long-term variations of air quality and meteorological factors in Taiwanese metropolitan areas (Taipei area, Taichung City, and Kaohsiung City) and a rural area (Hualien County) between 1993 and 2012. The influence of a mass rapid transit (MRT) system on air quality was also evaluated. Air pollutant concentrations and meteorology data were collected from Taiwan Environmental Protection Administration (TEPA) air monitoring stations and Central Weather Bureau stations in the surveyed areas, respectively. Analyses indicate that levels of air pollution in metropolitan areas were greater than in the rural area. Kaohsiung City had the highest levels of O, SO, and particulate matter 2.5 or 10 µm in diameter (PM and PM). Clear downward trends for CO, NO, PM, PM, and especially SO concentrations were found in the surveyed areas, whereas O showed no decrease. Both O and PM concentrations showed similar bimodal seasonal distributions. Taiwan's air quality has improved significantly since 1993, indicating the effectiveness of promoting air pollution strategies and policies by the TEPA. Air pollution had an obvious improvement in Taipei area after the MRT system began operations in 1996. Because global climate may potentially affect urban air pollution in Taiwan, further study to clarify the mechanisms by which air pollution may affect human health and other biological effects is warranted. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  7. Rapid High-throughput Species Identification of Botanical Material Using Direct Analysis in Real Time High Resolution Mass Spectrometry.

    Science.gov (United States)

    Lesiak, Ashton D; Musah, Rabi A

    2016-10-02

    We demonstrate that direct analysis in real time-high resolution mass spectrometry can be used to produce mass spectral profiles of botanical material, and that these chemical fingerprints can be used for plant species identification. The mass spectral data can be acquired rapidly and in a high throughput manner without the need for sample extraction, derivatization or pH adjustment steps. The use of this technique bypasses challenges presented by more conventional techniques including lengthy chromatography analysis times and resource intensive methods. The high throughput capabilities of the direct analysis in real time-high resolution mass spectrometry protocol, coupled with multivariate statistical analysis processing of the data, provide not only class characterization of plants, but also yield species and varietal information. Here, the technique is demonstrated with two psychoactive plant products, Mitragyna speciosa (Kratom) and Datura (Jimsonweed), which were subjected to direct analysis in real time-high resolution mass spectrometry followed by statistical analysis processing of the mass spectral data. The application of these tools in tandem enabled the plant materials to be rapidly identified at the level of variety and species.

  8. Rapid Evaporative Ionisation Mass Spectrometry (REIMS) Provides Accurate Direct from Culture Species Identification within the Genus Candida.

    Science.gov (United States)

    Cameron, Simon J S; Bolt, Frances; Perdones-Montero, Alvaro; Rickards, Tony; Hardiman, Kate; Abdolrasouli, Alireza; Burke, Adam; Bodai, Zsolt; Karancsi, Tamas; Simon, Daniel; Schaffer, Richard; Rebec, Monica; Balog, Julia; Takáts, Zoltan

    2016-11-14

    Members of the genus Candida, such as C. albicans and C. parapsilosis, are important human pathogens. Other members of this genus, previously believed to carry minimal disease risk, are increasingly recognised as important human pathogens, particularly because of variations in susceptibilities to widely used anti-fungal agents. Thus, rapid and accurate identification of clinical Candida isolates is fundamental in ensuring timely and effective treatments are delivered. Rapid Evaporative Ionisation Mass Spectrometry (REIMS) has previously been shown to provide a high-throughput platform for the rapid and accurate identification of bacterial and fungal isolates. In comparison to commercially available matrix assisted laser desorption ionisation time of flight mass spectrometry (MALDI-ToF), REIMS based methods require no preparative steps nor time-consuming cell extractions. Here, we report on the ability of REIMS-based analysis to rapidly and accurately identify 153 clinical Candida isolates to species level. Both handheld bipolar REIMS and high-throughput REIMS platforms showed high levels of species classification accuracy, with 96% and 100% of isolates classified correctly to species level respectively. In addition, significantly different (FDR corrected P value < 0.05) lipids within the 600 to 1000 m/z mass range were identified, which could act as species-specific biomarkers in complex microbial communities.

  9. Rapid Detection of OXA-48-Producing Enterobacteriaceae by Matrix-Assisted Laser Desorption Ionization−Time of Flight Mass Spectrometry

    Science.gov (United States)

    Oviaño, Marina; Barba, Maria José; Fernández, Begoña; Ortega, Adriana; Aracil, Belén; Oteo, Jesús; Campos, José

    2015-01-01

    A rapid and sensitive (100%) matrix-assisted laser desorption ionization−time of flight mass spectrometry (MALDI-TOF MS) assay was developed to detect OXA-48-type producers, using 161 previously characterized clinical isolates. Ertapenem was monitored to detect carbapenem resistance, and temocillin was included in the assay as a marker for OXA-48-producers. Structural analysis of temocillin is described. Data are obtained within 60 min. PMID:26677247

  10. Characterizing rapid, activity-linked conformational transitions in proteins via sub-second hydrogen deuterium exchange mass spectrometry.

    Science.gov (United States)

    Resetca, Diana; Wilson, Derek J

    2013-11-01

    This review outlines the application of time-resolved electrospray ionization mass spectrometry (TRESI-MS) and hydrogen-deuterium exchange (HDX) to study rapid, activity-linked conformational transitions in proteins. The method is implemented on a microfluidic chip which incorporates all sample-handling steps required for a 'bottom-up' HDX workflow: a capillary mixer for sub-second HDX labeling, a static mixer for HDX quenching, a microreactor for rapid protein digestion, and on-chip electrospray. By combining short HDX labeling pulses with rapid digestion, this approach provides a detailed characterization of the structural transitions that occur during protein folding, ligand binding, post-translational modification and catalytic turnover in enzymes. This broad spectrum of applications in areas largely inaccessible to conventional techniques means that microfluidics-enabled TRESI-MS/HDX is a unique and powerful approach for investigating the dynamic basis of protein function. © 2013 FEBS.

  11. Combination of SDS-PAGE and intact mass analysis for rapid determination of heterogeneities in monoclonal antibody therapeutics.

    Science.gov (United States)

    Yamada, Hideaki; Matsumura, Chiemi; Yamada, Keita; Teshima, Koichiro; Hiroshima, Takashi; Kinoshita, Mitsuhiro; Suzuki, Shigeo; Kakehi, Kazuaki

    2017-05-01

    mAbs are currently mainstream in biopharmaceuticals, and their market has been growing due to their high target specificity. Characterization of heterogeneities in mAbs is performed to secure their quality and safety by physicochemical analyses. However, they require time-consuming task, which often strain the resources of drug development in pharmaceuticals. Rapid and direct method to determine the heterogeneities should be a powerful tool for pharmaceutical analysis. Considering the advantages of electrophoresis and MS, this study addresses the combination of SDS-PAGE and intact mass analysis, which provides direct, rapid, and orthogonal determination of heterogeneities in mAb therapeutics. mAb therapeutics that migrated in SDS-PAGE were recovered from gel by treatment with SDC-containing buffer. Usage of SDC-containing buffer as extraction solvent and ethanol-based staining solution enhanced the recovery of intact IgG from SDS-PAGE gels. Recovery of mAbs reached more than 86% with 0.2% SD. The heterogeneities, especially N-glycan variants in the recovered mAb therapeutics, were clearly determined by intact mass analysis. We believe that the study is important in pharmaceuticals‧ perspective since orthogonal combination of gel electrophoresis and intact mass analysis should be pivotal role for rapid and precise characterization of mAbs. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Rapid comparison of a candidate biosimilar to an innovator monoclonal antibody with advanced liquid chromatography and mass spectrometry technologies.

    Science.gov (United States)

    Xie, Hongwei; Chakraborty, Asish; Ahn, Joomi; Yu, Ying Qing; Dakshinamoorthy, Deepalakshmi P; Gilar, Martin; Chen, Weibin; Skilton, St John; Mazzeo, Jeffery R

    2010-01-01

    This study shows that state-of-the-art liquid chromatography (LC) and mass spectrometry (MS) can be used for rapid verification of identity and characterization of sequence variants and posttranslational modifications (PTMs) for antibody products. A candidate biosimilar IgG1 monoclonal antibody (mAb) was compared in detail to a commercially available innovator product. Intact protein mass, primary sequence, PTMs, and the micro-differences between the two mAbs were identified and quantified simultaneously. Although very similar in terms of sequences and modifications, a mass difference observed by LC-MS intact mass measurements indicated that they were not identical. Peptide mapping, performed with data independent acquisition LC-MS using an alternating low and elevated collision energy scan mode (LC-MS(E)), located the mass difference between the biosimilar and the innovator to a two amino acid residue variance in the heavy chain sequences. The peptide mapping technique was also used to comprehensively catalogue and compare the differences in PTMs of the biosimilar and innovator mAbs. Comprehensive glycosylation profiling confirmed that the proportion of individual glycans was different between the biosimilar and the innovator, although the number and identity of glycans were the same. These results demonstrate that the combination of accurate intact mass measurement, released glycan profiling, and LC-MS(E) peptide mapping provides a set of routine tools that can be used to comprehensively compare a candidate biosimilar and an innovator mAb.

  13. Advanced Mass Spectrometric Methods for the Rapid and Quantitative Characterization of Proteomes

    Directory of Open Access Journals (Sweden)

    Richard D. Smith

    2006-04-01

    Full Text Available Progress is reviewed towards the development of a global strategy that aims to extend the sensitivity, dynamic range, comprehensiveness and throughput of proteomic measurements based upon the use of high performance separations and mass spectrometry. The approach uses high accuracy mass measurements from Fourier transform ion cyclotron resonance mass spectrometry (FTICR to validate peptide ‘accurate mass tags’ (AMTs produced by global protein enzymatic digestions for a specific organism, tissue or cell type from ‘potential mass tags’ tentatively identified using conventional tandem mass spectrometry (MS/MS. This provides the basis for subsequent measurements without the need for MS/ MS. High resolution capillary liquid chromatography separations combined with high sensitivity, and high resolution accurate FTICR measurements are shown to be capable of characterizing peptide mixtures of more than 105 components. The strategy has been initially demonstrated using the microorganisms Saccharomyces cerevisiae and Deinococcus radiodurans. Advantages of the approach include the high confidence of protein identification, its broad proteome coverage, high sensitivity, and the capability for stableisotope labeling methods for precise relative protein abundance measurements.

  14. Rapid tomato volatile profiling by using proton-transfer reaction mass spectrometry (PTS-MS)

    NARCIS (Netherlands)

    Farneti, B.; Cristescu, S.M.; Costa, G.; Harren, F.J.M.; Woltering, E.J.

    2012-01-01

    The availability of rapid and accurate methods to assess fruit flavor is of utmost importance to support quality control especially in the breeding phase. Breeders need more information and analytical tools to facilitate selection for complex multigenic traits such as flavor quality. In this study,

  15. Galaxy stellar mass functions from ZFOURGE/CANDELS: An excess of low-mass galaxies since z = 2 and the rapid buildup of quiescent galaxies

    Energy Technology Data Exchange (ETDEWEB)

    Tomczak, Adam R.; Tran, Kim-Vy H.; Papovich, Casey; Kawinwanichakij, Lalitwadee; Mehrtens, Nicola; Spitler, Lee R.; Tilvi, Vithal [George P. and Cynthia W. Mitchell Institute for Fundamental Physics and Astronomy, Department of Physics and Astronomy, Texas A and M University, College Station, TX 77843 (United States); Quadri, Ryan F.; Kelson, Daniel D.; McCarthy, Patrick J.; Monson, Andrew J.; Persson, S. Eric [Carnegie Observatories, Pasadena, CA 91101 (United States); Labbé, Ivo; Straatman, Caroline M. S. [Sterrewacht Leiden, Leiden University, NL-2300 RA Leiden (Netherlands); Glazebrook, Karl; Allen, Rebecca; Kacprzak, Glenn G. [Centre for Astrophysics and Supercomputing, Swinburne University, Hawthorn, VIC 3122 (Australia); Brammer, Gabriel B. [European Southern Observatory, Alonso de Córdova 3107, Casilla 19001, Vitacura, Santiago (Chile); Van Dokkum, Pieter, E-mail: tomczak@physics.tamu.edu [Department of Astronomy, Yale University, New Haven, CT 06520 (United States)

    2014-03-10

    Using observations from the FourStar Galaxy Evolution Survey (ZFOURGE), we obtain the deepest measurements to date of the galaxy stellar mass function (SMF) at 0.2 < z < 3. ZFOURGE provides well-constrained photometric redshifts made possible through deep medium-bandwidth imaging at 1-2 μm. We combine this with Hubble Space Telescope imaging from the Cosmic Assembly Near-IR Deep Extragalactic Legacy Survey, allowing for the efficient selection of both blue and red galaxies down to stellar masses of ∼10{sup 9.5} M {sub ☉} at z ∼ 2.5. The total surveyed area is 316 arcmin{sup 2} distributed over three independent fields. We supplement these data with the wider and shallower NEWFIRM Medium-Band Survey to provide stronger constraints at high masses. Several studies at z ≤ 1.5 have revealed a steepening of the slope at the low-mass end of the SMF, leading to an upturn at masses <10{sup 10} M {sub ☉} that is not well described by a standard single-Schechter function. We find evidence that this feature extends to at least z ∼ 2 and that it can be found in both the star-forming and quiescent populations individually. The characteristic mass (M*) and slope at the lowest masses (α) of a double-Schechter function fit to the SMF stay roughly constant at Log(M/M {sub ☉}) ∼ 10.65 and ∼ – 1.5, respectively. The SMF of star-forming galaxies has evolved primarily in normalization, while the change in shape is relatively minor. Our data allow us, for the first time, to observe a rapid buildup at the low-mass end of the quiescent SMF. Since z = 2.5, the total stellar mass density of quiescent galaxies (down to 10{sup 9} M {sub ☉}) has increased by a factor of ∼12, whereas the mass density of star-forming galaxies only increases by a factor of ∼2.2.

  16. Rapid confirmatory analysis of non-steroidal anti-inflammatory drugs in bovine milk by rapid resolution liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Dowling, Geraldine; Gallo, Pasquale; Malone, Edward; Regan, Liam

    2009-11-13

    A rapid method has been developed to analyse carprofen (CPF), diclofenac (DCF), mefenamic acid (MFN), niflumic acid (NIFLU), naproxen (NAP), oxyphenylbutazone (OXYPHEN), phenylbutazone (PBZ) and suxibuzone (SUXI) residues in bovine milk. Milk samples are extracted with acetonitrile and sample extracts were purified on Evolute ABN solid phase extraction cartridges. Aliquots were analysed by rapid resolution liquid chromatography tandem mass spectrometry (RRLC-MS/MS) with a runtime of 6.5 min. The method was validated in bovine milk, according to the criteria defined in Commission Decision 2002/657/EC. CCalpha values of 0.46, 1.08, 0.92, 1.26, 1.29, 2.12, 0.55 and 2.86 ng mL(-1) were determined for CPF, DCF, MFN, NIFLU, NAP, OXYPHEN, PBZ and SUXI, respectively. CCbeta values of 0.79, 1.85, 1.56, 2.15, 2.19, 3.62, 0.94 and 4.87 ng mL(-1) were determined for CPF, DCF, MFN, NIFLU, NAP, OXYPHEN, PBZ and SUXI, respectively. The measurement uncertainty of the method was estimated at 9, 28, 28, 45, 46, 45, 10 and 39% for CPF, DCF, MFN, NIFLU, NAP, OXYPHEN, PBZ and SUXI. Fortifying bovine milk samples (n=18) in three separate assays, show the accuracy of the method to be between 82 and 108%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (5, 7.5 and 10 ng mL(-1)) was less than 16%, respectively. The advantage of the method is that low ng mL(-1) levels can be detected and quantitatively confirmed rapidly in milk and that 3 batches of samples can be analysed within a single day using RRLC-MS/MS with a runtime of 6.5 min.

  17. Accurate Mass Fragment Library for Rapid Analysis of Pesticides on Produce Using Ambient Pressure Desorption Ionization with High-Resolution Mass Spectrometry

    Science.gov (United States)

    Kern, Sara E.; Lin, Lora A.; Fricke, Frederick L.

    2014-08-01

    U.S. food imports have been increasing steadily for decades, intensifying the need for a rapid and sensitive screening technique. A method has been developed that uses foam disks to sample the surface of incoming produce. This work provides complimentary information to the extensive amount of published pesticide fragmentation data collected using LCMS systems (Sack et al. Journal of Agricultural and Food Chemistry, 59, 6383-6411, 2011; Mol et al. Analytical and Bioanalytical Chemistry, 403, 2891-2908, 2012). The disks are directly analyzed using transmission-mode direct analysis in real time (DART) ambient pressure desorption ionization coupled to a high resolution accurate mass-mass spectrometer (HRAM-MS). In order to provide more certainty in the identification of the pesticides detected, a library of accurate mass fragments and isotopes of the protonated parent molecular ion (the [M+H]+) has been developed. The HRAM-MS is equipped with a quadrupole mass filter, providing the capability of "data-dependent" fragmentation, as opposed to "all -ion" fragmentation (where all of the ions enter a collision chamber and are fragmented at once). A temperature gradient for the DART helium stream and multiple collision energies were employed to detect and fragment 164 pesticides of varying chemical classes, sizes, and polarities. The accurate mass information of precursor ([M+H]+ ion) and fragment ions is essential in correctly identifying chemical contaminants on the surface of imported produce. Additionally, the inclusion of isotopes of the [M+H]+ in the database adds another metric to the confirmation process. The fragmentation data were collected using a Q-Exactive mass spectrometer and were added to a database used to process data collected with an Exactive mass spectrometer, an instrument that is more readily available for this screening application. The commodities investigated range from smooth-skinned produce such as apples to rougher surfaces like broccoli. The

  18. Rapid detection of cocaine, benzoylecgonine and methylecgonine in fingerprints using surface mass spectrometry.

    Science.gov (United States)

    Bailey, Melanie J; Bradshaw, Robert; Francese, Simona; Salter, Tara L; Costa, Catia; Ismail, Mahado; P Webb, Roger; Bosman, Ingrid; Wolff, Kim; de Puit, Marcel

    2015-09-21

    Latent fingerprints provide a potential route to the secure, high throughput and non-invasive detection of drugs of abuse. In this study we show for the first time that the excreted metabolites of drugs of abuse can be detected in fingerprints using ambient mass spectrometry. Fingerprints and oral fluid were taken from patients attending a drug and alcohol treatment service. Gas chromatography mass spectrometry (GC-MS) was used to test the oral fluid of patients for the presence of cocaine and benzoylecgonine. The corresponding fingerprints were analysed using Desorption Electrospray Ionization (DESI) which operates under ambient conditions and Ion Mobility Tandem Mass Spectrometry Matrix Assisted Laser Desorption Ionization (MALDI-IMS-MS/MS) and Secondary Ion Mass Spectrometry (SIMS). The detection of cocaine, benzoylecgonine (BZE) and methylecgonine (EME) in latent fingerprints using both DESI and MALDI showed good correlation with oral fluid testing. The sensitivity of SIMS was found to be insufficient for this application. These results provide exciting opportunities for the use of fingerprints as a new sampling medium for secure, non-invasive drug detection. The mass spectrometry techniques used here offer a high level of selectivity and consume only a small area of a single fingerprint, allowing repeat and high throughput analyses of a single sample.

  19. Rapid sample classification using an open port sampling interface coupled with liquid introduction atmospheric pressure ionization mass spectrometry.

    Science.gov (United States)

    Van Berkel, Gary J; Kertesz, Vilmos

    2017-02-15

    An "Open Access"-like mass spectrometric platform to fully utilize the simplicity of the manual open port sampling interface for rapid characterization of unprocessed samples by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The in-house developed integrated software with a simple, small and relatively low-cost mass spectrometry system introduced here fills this void. Software was developed to operate the mass spectrometer, to collect and process mass spectrometric data files, to build a database and to classify samples using such a database. These tasks were accomplished via the vendor-provided software libraries. Sample classification based on spectral comparison utilized the spectral contrast angle method. Using the developed software platform near real-time sample classification is exemplified using a series of commercially available blue ink rollerball pens and vegetable oils. In the case of the inks, full scan positive and negative ion ESI mass spectra were both used for database generation and sample classification. For the vegetable oils, full scan positive ion mode APCI mass spectra were recorded. The overall accuracy of the employed spectral contrast angle statistical model was 95.3% and 98% in case of the inks and oils, respectively, using leave-one-out cross-validation. This work illustrates that an open port sampling interface/mass spectrometer combination, with appropriate instrument control and data processing software, is a viable direct liquid extraction sampling and analysis system suitable for the non-expert user and near real-time sample classification via database matching. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

  20. Rapid development of adaptive, climate-driven clinal variation in seed mass in the invasive annual Forb Echium plantagineum L.

    Directory of Open Access Journals (Sweden)

    Tara K Konarzewski

    Full Text Available We examined adaptive clinal variation in seed mass among populations of an invasive annual species, Echium plantagineum, in response to climatic selection. We collected seeds from 34 field populations from a 1,000 km long temperature and rainfall gradient across the species' introduced range in south-eastern Australia. Seeds were germinated, grown to reproductive age under common glasshouse conditions, and progeny seeds were harvested and weighed. Analyses showed that seed mass was significantly related to climatic factors, with populations sourced from hotter, more arid sites producing heavier seeds than populations from cooler and wetter sites. Seed mass was not related to edaphic factors. We also found that seed mass was significantly related to both longitude and latitude with each degree of longitude west and latitude north increasing seed mass by around 2.5% and 4% on average. There was little evidence that within-population or between-population variation in seed mass varied in a systematic manner across the study region. Our findings provide compelling evidence for development of a strong cline in seed mass across the geographic range of a widespread and highly successful invasive annual forb. Since large seed mass is known to provide reproductive assurance for plants in arid environments, our results support the hypothesis that the fitness and range potential of invasive species can increase as a result of genetic divergence of populations along broad climatic gradients. In E. plantagineum population-level differentiation has occurred in 150 years or less, indicating that the adaptation process can be rapid.

  1. Mass Balance Evolution of Black Rapids Glacier, Alaska, 1980–2100, and Its Implications for Surge Recurrence

    Directory of Open Access Journals (Sweden)

    Christian Kienholz

    2017-07-01

    Full Text Available Surge-type Black Rapids Glacier, Alaska, has undergone strong retreat since it last surged in 1936–1937. To assess its evolution during the late Twentieth and Twenty-first centuries and determine potential implications for surge likelihood, we run a simplified glacier model over the periods 1980–2015 (hindcasting and 2015–2100 (forecasting. The model is forced by daily temperature and precipitation fields, with downscaled reanalysis data used for the hindcasting. A constant climate scenario and an RCP 8.5 scenario based on the GFDL-CM3 climate model are employed for the forecasting. Debris evolution is accounted for by a debris layer time series derived from satellite imagery (hindcasting and a parametrized debris evolution model (forecasting. A retreat model accounts for the evolution of the glacier geometry. Model calibration, validation and parametrization rely on an extensive set of in situ and remotely sensed observations. To explore uncertainties in our projections, we run the glacier model in a Monte Carlo fashion, varying key model parameters and input data within plausible ranges. Our results for the hindcasting period indicate a negative mass balance trend, caused by atmospheric warming in the summer, precipitation decrease in the winter and surface elevation lowering (climate-elevation feedback, which exceed the moderating effects from increasing debris cover and glacier retreat. Without the 2002 rockslide deposits on Black Rapids' lower reaches, the mass balances would be more negative, by ~20% between the 2003 and 2015 mass-balance years. Despite its retreat, Black Rapids Glacier is substantially out of balance with the current climate. By 2100, ~8% of Black Rapids' 1980 area are projected to vanish under the constant climate scenario and ~73% under the RCP 8.5 scenario. For both scenarios, the remaining glacier portions are out of balance, suggesting continued retreat after 2100. Due to mass starvation, a surge in the Twenty

  2. Mass balance evolution of Black Rapids Glacier, Alaska, 1980-2100, and its implications for surge recurrence

    Science.gov (United States)

    Kienholz, Christian; Hock, Regine; Truffer, Martin; Bieniek, Peter; Lader, Richard

    2017-07-01

    Surge-type Black Rapids Glacier, Alaska, has undergone strong retreat since it last surged in 1936-37. To assess its evolution during the late 20th and 21st centuries and determine potential implications for surge likelihood, we run a simplified glacier model over the periods 1980-2015 (hindcasting) and 2015-2100 (forecasting). The model is forced by daily temperature and precipitation fields, with downscaled reanalysis data used for the hindcasting. A constant climate scenario and an RCP 8.5 scenario based on the GFDL-CM3 climate model are employed for the forecasting. Debris evolution is accounted for by a debris layer time series derived from satellite imagery (hindcasting) and a parametrized debris evolution model (forecasting). A retreat model accounts for the evolution of the glacier geometry. Model calibration, validation and parametrization rely on an extensive set of in situ and remotely sensed observations. To explore uncertainties in our projections, we run the glacier model in a Monte Carlo fashion, varying key model parameters and input data within plausible ranges. Our results for the hindcasting period indicate a negative mass balance trend, caused by atmospheric warming in the summer, precipitation decrease in the winter and surface elevation lowering (climate-elevation feedback), which exceed the moderating effects from increasing debris cover and glacier retreat. Without the 2002 rockslide deposits on Black Rapids' lower reaches, the mass balances would be more negative, by 20% between the 2003 and 2015 mass-balance years. Despite its retreat, Black Rapids Glacier is substantially out of balance with the current climate. By 2100, 8% of Black Rapids' 1980 area are projected to vanish under the constant climate scenario and 73% under the RCP 8.5 scenario. For both scenarios, the remaining glacier portions are out of balance, suggesting continued retreat after 2100. Due to mass starvation, a surge in the 21st century is unlikely. The projected

  3. Mass fingerprint analysis of spider mites (Acari) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for rapid discrimination.

    Science.gov (United States)

    Kajiwara, Hideyuki; Hinomoto, Norihide; Gotoh, Tetsuo

    2016-04-30

    Discrimination of spider mite species is still performed using morphological information, although DNA and other biological approaches have been attempted for identification purposes. These techniques need much time, are expensive, and require specialist staff. As an alternative, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) analysis is applied for rapid discrimination of spider mite species. Spider mites were analyzed using MALDI-TOFMS after extraction with 70% formic acid and acetonitrile. A single spider mite was also analyzed directly on double-sided carbon tape. A dendrogram was compiled from the MS data. Evolutionarily close and morphologically similar spider mites, the Kanzawa (Tetranychus kanzawai) and the two-spotted (T. urticae) spider mites, as well as three other related species of spider mites, could be discriminated by mass fingerprints. Although female adults were mainly used in this report, male adults and nymphs showed almost the same mass fingerprints and were not considered to affect discrimination capability. A single spider mite on double-sided carbon tape was analyzed directly by MALDI-TOFMS. Spider mites could be analyzed directly by MALDI-TOFMS, with evolutionarily and morphologically closely related spider mites showing different mass fingerprints, allowing for their identification. Copyright © 2016 John Wiley & Sons, Ltd.

  4. Microstructural evolution in a rapidly solidified Al-4mass%Fe droplet

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seong-Gyoon (Department of Materials Science and Engineering, Kunsan National University, Kunsan 573-360 (Korea, Republic of)); Shin, Seong-Ho (Central Laboratory, Sammi Special Steel Company, Changwon 641-050 (Korea, Republic of)); Suzuki, Toshio (Engineering Research Institute, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113 (Japan)); Umeda, Takateru (Department of Metallurgy, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113 (Japan))

    1994-05-15

    A two-dimensional non-newtonian numerical analysis on the solidification of Al-4mass%Fe droplet was represented which includes the transition between the partitionless and partitioned solidification modes. It was shown that, instead of the banded-structure formation, a strong instability on the macroscopic solid-liquid interface occurs in the transition range. The patterns predicted as functions of the initial undercooling and the droplet size were compared with the microstructures of the gas-atomized Al-4mass%Fe powders. ((orig.))

  5. Process Modelling of Rapid Manufacturing Based Mass Customisation System for Fabrication of Custom Foot Orthoses: Review Paper

    Directory of Open Access Journals (Sweden)

    Saleh Jumani

    2013-04-01

    Full Text Available The need for custom-made devices, rehabilitation aids and treatments is explicit in the medical sector. Applications of rapid manufacturing techniques based on additive fabrication processes combined with medical digitising technologies can generate high quality solutions in situations where the need for custom-made devices and rehabilitation aids and low-lead times are very important factors. Foot orthoses are medical devices applied in the treatment of biomechanical foot disorders, foot injuries and foot diseases including rheumatoid arthritis and diabetes. The significant challenge in the treatment of foot related diseases is progressing pathological deterioration in the affected sites of the foot which requires quick provision of the orthoses. A process model is developed using the IDEF0 modelling technique in which a rapid manufacturing approach is integrated in the design and fabrication process of custom foot orthoses. The process model will be used in the development of rapid manufacturing based design and fabrication system for mass customisation of foot orthoses. The developed system is aimed at mass scale production of custom foot orthoses with the advantages of reduced cost, reduced lead-time and improved product in terms of increased fit, consistency and accuracy in the final product.

  6. Extra-uterine pregnancy with the bladder COmmunIcatIng

    African Journals Online (AJOL)

    A young woman presented 5 months after her last normal menstrual period with a history of having passed a macerated fetal limb during micturition. She had a pelvic mass which was found at laparo- tomy to be due to a ruptured infected extra-uterine pregnancy. This lay in the uterovesical pouch and communicated with t1~ ...

  7. Rapid mass spectrometric analysis of 15N-Leu incorporation fidelity during preparation of specifically labeled NMR samples

    DEFF Research Database (Denmark)

    Truhlar, Stephanie M E; Cervantes, Carla F; Torpey, Justin W

    2008-01-01

    . MALDI TOF-TOF MS/MS data provide additional information that shows where the "extra" (15)N labels are incorporated, which can be useful in confirming ambiguous assignments. The described procedure provides a rapid technique to monitor the fidelity of selective labeling that does not require a lot......Advances in NMR spectroscopy have enabled the study of larger proteins that typically have significant overlap in their spectra. Specific (15)N-amino acid incorporation is a powerful tool for reducing spectral overlap and attaining reliable sequential assignments. However, scrambling of the label...... during protein expression is a common problem. We describe a rapid method to evaluate the fidelity of specific (15)N-amino acid incorporation. The selectively labeled protein is proteolyzed, and the resulting peptides are analyzed using MALDI mass spectrometry. The (15)N incorporation is determined...

  8. A rapid and specific derivatization procedure to identify acyl-glucuronides by mass spectrometry.

    Science.gov (United States)

    Vaz, Alfin D N; Wang, Wei Wei; Bessire, Andrew J; Sharma, Raman; Hagen, Anne E

    2010-07-30

    A simple procedure is described to identify acyl-glucuronides by coupled liquid chromatography/mass spectrometry after derivatization to a hydroxamic acid with hydroxylamine. The reaction specificity obviates the need for isolation of the acyl-glucuronide from an extract. Glucuronides derived from carbamic acids, and alkyl- and aromatic amines, are inert to the derivatization reaction conditions, making the hydroxamic acid derivative a fingerprint for acyl-glucuronides. Copyright 2010 John Wiley & Sons, Ltd.

  9. Barrier Free Conditions of Mass Rapid Transit Stations in Hong Kong

    OpenAIRE

    OSAKAYA, Yoshiyuki; Aoyama, Takeshi; RATANAMART, Suphawadee

    2010-01-01

    In Hong Kong, it is estimated that aging will be rapidly going on after 2010. Increase of the elderly means increase of the disabled. In Hong Kong, there are 3 KCR lines(East Line, West Line and Ma On Shan Line) and 7 MTR lines(Kwun Tong Line, Tsuen Wan Line, Island Line, Tsueng Wan O Line,Tung Chung Line, Airport Line and Disneyland Line) in 2006. This study firstly made the actual conditions of barrier free at all 81 stations clear. It secondly made problems clear. It thirdly showed proposa...

  10. Human serum processing and analysis methods for rapid and reproducible N-glycan mass profiling.

    Science.gov (United States)

    Kronewitter, Scott R; de Leoz, Maria Lorna A; Peacock, Kyle S; McBride, Kelly R; An, Hyun Joo; Miyamoto, Suzanne; Leiserowitz, Gary S; Lebrilla, Carlito B

    2010-10-01

    Glycans constitute a new class of compounds for biomarker discovery. Glycosylation is a common post-translational modification and is often associated with transformation to malignancy. To analyze glycans, they are released from proteins, enriched, and measured with mass spectrometry. For biomarker discovery, repeatability at every step of the process is important. Locating and minimizing the process variability is key to establishing a robust platform stable enough for biomarker discovery. Understanding the variability of the measurement devices helps understand the variability associated with the chemical processing. This report explores the potential use of methods expediting the enzymatic release of glycans such as a microwave reactor and automation of the solid-phase extraction with a robotic liquid handler. The study employs matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry but would be suitable with any mass spectrometry method. Methods for system-wide data analysis are examined because proper metrics for evaluating the performance of glycan sample preparation procedures are not well established.

  11. Rapid analysis of urinary opiates using fast gas chromatography–mass spectrometry and hydrogen as a carrier gas

    Directory of Open Access Journals (Sweden)

    Sumandeep Rana

    2014-09-01

    Gas chromatographic–mass spectrometric analysis was performed in electron ionization mode by selective ion monitoring, using hydrogen as a carrier gas, a short narrow bore GC capillary column, and fast temperature program, allowing for a rapid analytical cycle to maximize the instrument time for high throughput laboratories. While maintaining specificity for these drugs, concentrations in human urine ranging from 50 to 5,000 ng/mL can be measured with intraday and interday imprecision, expressed as variation coefficients, of less than 2.3% for all analytes within a run time of less than 3.5 minutes.

  12. Des interactions indirectes entre les proies : Modélisation et influence du comportement du prédateur commun

    OpenAIRE

    Teixeira Alves, Mickaël

    2013-01-01

    Cette thèse a pour objet la modélisation de systèmes multi-proies–prédateurs. Elle s’intéresse particulièrement à l’influence du comportement d’un prédateur sur les interactions indirectes entre ses proies, i.e. l’effet de l’ajout d’une proie sur la densité des autres. La théorie classique prédit l’occurrence d’effets indirects négatifs entre les proies, ou compétition apparente, résultant de l’interaction avec un prédateur commun ; des résultats plus récents identifient certains mécanismes à...

  13. Rapid and Accurate Identification of Animal Species in Natural Leather Goods by Liquid Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Izuchi, Yukari; Takashima, Tsuneo; Hatano, Naoya

    2016-01-01

    The demand for leather goods has grown globally in recent years. Industry revenue is forecast to reach $91.2 billion by 2018. There is an ongoing labelling problem in the leather items market, in that it is currently impossible to identify the species that a given piece of leather is derived from. To address this issue, we developed a rapid and simple method for the specific identification of leather derived from cattle, horses, pigs, sheep, goats, and deer by analysing peptides produced by the trypsin-digestion of proteins contained in leather goods using liquid chromatography/mass spectrometry. We determined species-specific amino acid sequences by liquid chromatography/tandem mass spectrometry analysis using the Mascot software program and demonstrated that collagen α-1(I), collagen α-2(I), and collagen α-1(III) from the dermal layer of the skin are particularly useful in species identification.

  14. Precision mass measurements for studies of nucleosynthesis via the rapid neutron-capture process. Penning-trap mass measurements of neutron-rich cadmium and caesium isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Atanasov, Dinko

    2016-07-06

    Although the theory for the rapid neutron-capture process (r-process) was developed more than 55 years ago, the astrophysical site is still under a debate. Theoretical studies predict that the r-process path proceeds through very neutron-rich nuclei with very asymmetric proton-to-neutron ratios. Knowledge about the properties of neutron-rich isotopes found in similar regions of the nuclear chart and furthermore suitable for r-process studies is still little or even not existing. The basic nuclear properties such as binding energies, half-lives, neutron-induced or neutron-capture reaction cross-sections, play an important role in theoretical simulations and can vary or even drastically alternate results of these studies. Therefore, a considerable effort was put forward to access neutron-rich isotopes at radioactive ion-beam facilities like ISOLDE at CERN. The goal of this PhD thesis is to describe the experimental work done for the precision mass measurements of neutron-rich cadmium ({sup 129-131}Cd) and caesium ({sup 132,146-148}Cs) isotopes. Measurements were done at the on-line radioactive ion-beam facility ISOLDE by using the four-trap mass spectrometer ISOLTRAP. The cadmium isotopes are key nuclides for the synthesis of stable isotopes around the mass peak A = 130 in the Solar System abundance.

  15. Evaluation of methods of rapid mass killing of segregated early weaned piglets.

    Science.gov (United States)

    Whiting, Terry L; Steele, Gregory G; Wamnes, Steinar; Green, Chris

    2011-07-01

    The operational logistics of mass killing of healthy, surplus piglets by manual blunt force trauma, controlled blunt force trauma, intraperitoneal injection of barbiturate, and free bullet were recorded. Objective performance variables evaluated were, speed of application, human resource and input cost, animal restraint required, and failure rate. Subjective evaluation of esthetics and difficulty of application indicated manual blunt force trauma is an unacceptable technique. Under field conditions, physical methods of killing were superior to intraperitoneal injection of concentrated pentobarbital. Considering animal welfare metrics in isolation, controlled blunt force trauma was superior to all other techniques attempted.

  16. Rapid detection of economic adulterants in fresh milk by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Abernethy, Grant; Higgs, Kerianne

    2013-05-03

    A method to aid in the detection of the economically driven adulteration of fresh milk with a range of small, nitrogen containing compounds, including melamine, ammeline, ammelide, cyanuric acid, allantoin, thiourea, urea, biuret, triuret, semicarbazide, aminotriazine, 3- and 4-aminotriazole, cyanamide, dicyandiamide, guanidine, choline, hydroxyproline, nitrate, and a range of amino acids, has been developed. (15)N2-Urea is used as an internal standard. The adulteration of milk with exogenous urea has previously been difficult to detect because of the variation in the naturally occurring levels of urea in milk. However, by monitoring the contaminants biuret and triuret, which comprise up to 1% of synthetic urea, the adulteration of milk with urea-based fertilizer can be detected. We estimate that to be economically viable, adulteration of the order of 90-4000ppm of the above adulterants would need to be added to fresh milk. For most of the compounds, an arbitrary detection threshold of 2ppm is therefore more than sufficient. For biuret, a lower detection threshold, better than 0.5ppm, is desirable and the sensitivity for biuret and triuret can be improved by the post-column addition of lithium to create lithium adducts under electrospray ionisation. Sample handling involves a two-step solvent precipitation method that is deployed in a 96-well plate format, and the hydrophilic interaction liquid chromatography uses a rapid gradient (1.2min). Three separate injections, to detect the positively charged compounds, the negatively charged compounds and amino acids and finally the lithium adducts, are used. This rapid and qualitative survey method may be deployed as a second tier screening method to quickly reduce sample numbers indicated as irregular by an FTIR based screening system, and to direct analysis to appropriate quantification methods. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Rapid Preconcentration for Liquid Chromatography-Mass Spectrometry Assay of Trace Level Neuropeptides

    Science.gov (United States)

    Zhou, Ying; Mabrouk, Omar S.; Kennedy, Robert T.

    2013-11-01

    Measurement of neuropeptides in the brain through in vivo microdialysis sampling provides direct correlation between neuropeptide concentration and brain function. Capillary liquid chromatography-multistage mass spectrometry (CLC-MSn) has proven to be effective at measuring endogenous neuropeptides in microdialysis samples. In the method, microliter samples are concentrated onto nanoliter volume packed beds before ionization and mass spectrometry analysis. The long times required for extensive preconcentration present a barrier to routine use because of the many samples that must be analyzed and instability of neuropeptides. In this study, we evaluated the capacity of 75 μm inner diameter (i.d.) capillary column packed with 10 μm reversed phase particles for increasing the throughput in CLC-MSn based neuropeptide measurement. Coupling a high injection flow rate for fast sample loading/desalting with a low elution flow rate to maintain detection sensitivity, this column has reduced analysis time from ˜30 min to 3.8 min for 5 μL sample, with 3 pM limit of detection (LOD) for enkephalins and 10 pM LOD for dynorphin A1-8 in 5 μL sample. The use of isotope-labeled internal standard lowered peptide signal variation to less than 5 %. This method was validated for in vivo detection of Leu and Met enkephalin with microdialysate collected from rat globus pallidus. The improvement in speed and stability makes CLC-MSn measurement of neuropeptides in vivo more practical.

  18. Direct analysis in real time mass spectrometry for the rapid identification of four highly hazardous pesticides in agrochemicals.

    Science.gov (United States)

    Wang, Lei; Zhao, Pengyue; Zhang, Fengzu; Li, Yanjie; Pan, Canping

    2012-08-30

    Direct analysis in real time (DART) is a new ion source technique, which is conducted in the open air under ambient conditions, applied to the rapid and direct analysis of any material (gases, liquids, and solids) with minimal or no sample preparation. In order to take advantage of the capacity of DART mass spectrometry for the real-time analysis of hazardous ingredients in commercial agrochemicals, a pilot study of rapid qualitative determination of hazardous pesticides was performed. Highly hazardous pesticides were identified by DART ionization coupled to a single-quadrupole mass spectrometer (DART-MS). Acetonitrile was chosen for dissolving samples prior to the analysis. Samples were analyzed by this technique in as little as 5 s. Phorate, carbofuran, ethoprophos and fipronil were be detected directly from commercial agrochemicals. The ionization-related parameters (DART temperature, grid voltage and MS fragment) of these compounds were optimized to obtain highly response. Isotope patterns were taken into consideration for qualitative identification. Relative standard deviations (RSDs, n = 5) of 2.3-15.0% were obtained by measuring the relative abundance of selected isotopes. This study showed that DART-MS technology was able to qualitatively determine the existence of highly hazardous pesticides in commercial pesticide formulations. It is suggested that this technology should be applied for routine monitoring in the market. Copyright © 2012 John Wiley & Sons, Ltd.

  19. Rapid fingerprinting and classification of extra virgin olive oil by microjet sampling and extractive electrospray ionization mass spectrometry.

    Science.gov (United States)

    Law, Wai Siang; Chen, Huan Wen; Balabin, Roman; Berchtold, Christian; Meier, Lukas; Zenobi, Renato

    2010-04-01

    Microjet sampling in combination with extractive electrospray ionization (EESI) mass spectrometry (MS) was applied to the rapid characterization and classification of extra virgin olive oil (EVOO) without any sample pretreatment. When modifying the composition of the primary ESI spray solvent, mass spectra of an identical EVOO sample showed differences. This demonstrates the capability of this technique to extract molecules with varying polarities, hence generating rich molecular information of the EVOO. Moreover, with the aid of microjet sampling, compounds of different volatilities (e.g.E-2-hexenal, trans-trans-2,4-heptadienal, tyrosol and caffeic acid) could be sampled simultaneously. EVOO data was also compared with that of other edible oils. Principal Component Analysis (PCA) was performed to discriminate EVOO and EVOO adulterated with edible oils. Microjet sampling EESI-MS was found to be a simple, rapid (less than 2 min analysis time per sample) and powerful method to obtain MS fingerprints of EVOO without requiring any complicated sample pretreatment steps.

  20. Rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves by direct analysis in real time-mass spectrometry.

    Science.gov (United States)

    Huang, Zhongping; Xu, Yueting; Huang, Yilei; Liu, Charles; Jiang, Kezhi; Wang, Lili

    2017-11-14

    A novel method based on direct analysis in real time integrated with mass spectrometry was established and applied into rapid determination of ginkgolic acids in Ginkgo biloba kernels and leaves. Instrument parameter settings were optimized to obtain the sensitive and accurate determination of ginkgolic acids. At the sample introduction speed of 0.2 mm/s, high intensity of [M-H]- ions for ginkgolic acids were observed in the negative ion mode by utilization of high-purity helium gas at 450°C. Two microliters of methanol extract of G. biloba kernels or leaves dropped on the surface of Quick-Strip module was analyzed after solvent evaporated to dryness. A series of standard solutions of ginkgolic acid 13:0 in the range of 2-50 mg/L were analyzed with a correlation coefficient r = 0.9981 and relative standard deviation (n = 5) from 12.5 to 13.7%. The limit of detection was 0.5 mg/L. The results of direct analysis in real time-mass spectrometry were in agreement with those observed by thermochemolysis gas chromatography. The proposed method demonstrated significant potential in the application of the high-throughput screening and rapid analysis for ginkgolic acids in dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Rapid mass spectrometric analysis of 15N-Leu incorporation fidelity during preparation of specifically labeled NMR samples.

    Science.gov (United States)

    Truhlar, Stephanie M E; Cervantes, Carla F; Torpey, Justin W; Kjaergaard, Magnus; Komives, Elizabeth A

    2008-09-01

    Advances in NMR spectroscopy have enabled the study of larger proteins that typically have significant overlap in their spectra. Specific (15)N-amino acid incorporation is a powerful tool for reducing spectral overlap and attaining reliable sequential assignments. However, scrambling of the label during protein expression is a common problem. We describe a rapid method to evaluate the fidelity of specific (15)N-amino acid incorporation. The selectively labeled protein is proteolyzed, and the resulting peptides are analyzed using MALDI mass spectrometry. The (15)N incorporation is determined by analyzing the isotopic abundance of the peptides in the mass spectra using the program DEX. This analysis determined that expression with a 10-fold excess of unlabeled amino acids relative to the (15)N-amino acid prevents the scrambling of the (15)N label that is observed when equimolar amounts are used. MALDI TOF-TOF MS/MS data provide additional information that shows where the "extra" (15)N labels are incorporated, which can be useful in confirming ambiguous assignments. The described procedure provides a rapid technique to monitor the fidelity of selective labeling that does not require a lot of protein. These advantages make it an ideal way of determining optimal expression conditions for selectively labeled NMR samples.

  2. Rapid characterisation of Klebsiella oxytoca isolates from contaminated liquid hand soap using mass spectrometry, FTIR and Raman spectroscopy.

    Science.gov (United States)

    Dieckmann, Ralf; Hammerl, Jens Andre; Hahmann, Hartmut; Wicke, Amal; Kleta, Sylvia; Dabrowski, Piotr Wojciech; Nitsche, Andreas; Stämmler, Maren; Al Dahouk, Sascha; Lasch, Peter

    2016-06-23

    Microbiological monitoring of consumer products and the efficiency of early warning systems and outbreak investigations depend on the rapid identification and strain characterisation of pathogens posing risks to the health and safety of consumers. This study evaluates the potential of three rapid analytical techniques for identification and subtyping of bacterial isolates obtained from a liquid hand soap product, which has been recalled and reported through the EU RAPEX system due to its severe bacterial contamination. Ten isolates recovered from two bottles of the product were identified as Klebsiella oxytoca and subtyped using matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI TOF MS), near-infrared Fourier transform (NIR FT) Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. Comparison of the classification results obtained by these phenotype-based techniques with outcomes of the DNA-based methods pulsed-field gel electrophoresis (PFGE), multi-locus sequence typing (MLST) and single nucleotide polymorphism (SNP) analysis of whole-genome sequencing (WGS) data revealed a high level of concordance. In conclusion, a set of analytical techniques might be useful for rapid, reliable and cost-effective microbial typing to ensure safe consumer products and allow source tracking.

  3. A microfabricated silicon platform with 60 microfluidic chips for rapid mass spectrometric analysis.

    Science.gov (United States)

    Sainiemi, Lauri; Nissilä, Teemu; Kostiainen, Risto; Ketola, Raimo A; Franssila, Sami

    2011-09-07

    This work presents a way of using silicon microfabrication to take advantage of the rim of a silicon wafer in a novel manner. Our circular multichip platform, which is fabricated using only standard microfabrication techniques, has 60 identical miniaturized micropillar array electrospray ionization (μPESI) chips at the periphery of a silicon wafer. The fabricated platform is fixed on a computer controlled rotating table, in front of a mass spectrometer (MS). After each MS measurement an unused μPESI chip is aligned towards the MS by the programmable rotating table. Our wafer-scale platform enabled measurement of 60 samples in 8 minutes. The samples can also be stored on the platform for later analysis.

  4. Electrospray ionization mass spectrometry fingerprinting of perfumes: Rapid classification and counterfeit detection.

    Science.gov (United States)

    Marques, Lygia de Azevedo; Catharino, Rodrigo Ramos; Bruns, Roy E; Eberlin, Marcos N

    2006-01-01

    A fast procedure to classify perfumes and identify counterfeit samples is described. Dilution of a few microL of the sample in a 1:1 methanol/water solution is followed by detection of its major polar components via direct infusion electrospray ionization mass spectrometry (ESI-MS) in the positive ion mode. As proof-of-principle cases, three famous brands of perfumes were used. The ESI+-MS fingerprints of authentic samples were very characteristic, showing distinctive sets of polar markers for each sample. Principal component analysis (PCA) placed samples of the three perfume brands in well-defined groups. Counterfeit samples were also clearly detected owing to contrasting ESI-MS fingerprints, with PCA placing these samples far away from the authentic samples. Copyright 2006 John Wiley & Sons, Ltd.

  5. Rapid characterization of chemical compounds in liquid and solid states using thermal desorption electrospray ionization mass spectrometry.

    Science.gov (United States)

    Huang, Min-Zong; Zhou, Chi-Chang; Liu, De-Lin; Jhang, Siou-Sian; Cheng, Sy-Chyi; Shiea, Jentaie

    2013-10-01

    Rapid characterization of thermally stable chemical compounds in solid or liquid states is achieved through thermal desorption electrospray ionization mass spectrometry (TD-ESI/MS). A feature of this technique is that sampling, desorption, ionization, and mass spectrometric detection are four separate events with respect to time and location. A metal probe was used to sample analytes in their solid or liquid states. The probe was then inserted in a preheated oven to thermally desorb the analytes on the probe. The desorbed analytes were carried by a nitrogen gas stream into an ESI plume, where analyte ions were formed via interactions with charged solvent species generated in the ESI plume. The analyte ions were subsequently detected by a mass analyzer attached to the TD-ESI source. Quantification of acetaminophen in aqueous solutions using TD-ESI/MS was also performed in which a linear response for acetaminophen was obtained between 25 and 500 ppb (R(2) = 0.9978). The standard deviation for a reproducibility test for ten liquid samples was 9.6%. Since sample preparation for TD-ESI/MS is unnecessary, a typical analysis can be completed in less than 10 s. Analytes such as the active ingredients in over-the-counter drugs were rapidly characterized regardless of the different physical properties of said drugs, which included liquid eye drops, viscous cold syrup solution, ointment cream, and a drug tablet. This approach was also used to detect trace chemical compounds in illicit drugs and explosives, in which samples were obtained from the surfaces of a cell phone, piece of luggage made from hard plastic, business card, and wooden desk.

  6. Development of a Rapid Microbore Metabolic Profiling Ultraperformance Liquid Chromatography-Mass Spectrometry Approach for High-Throughput Phenotyping Studies.

    Science.gov (United States)

    Gray, Nicola; Adesina-Georgiadis, Kyrillos; Chekmeneva, Elena; Plumb, Robert S; Wilson, Ian D; Nicholson, Jeremy K

    2016-06-07

    A rapid gradient microbore ultraperformance liquid chromatography-mass spectrometry (UPLC-MS) method has been developed to provide a high-throughput analytical platform for the metabolic phenotyping of urine from large sample cohorts. The rapid microbore metabolic profiling (RAMMP) approach was based on scaling a conventional reversed-phase UPLC-MS method for urinary profiling from 2.1 mm × 100 mm columns to 1 mm × 50 mm columns, increasing the linear velocity of the solvent, and decreasing the gradient time to provide an analysis time of 2.5 min/sample. Comparison showed that conventional UPLC-MS and rapid gradient approaches provided peak capacities of 150 and 50, respectively, with the conventional method detecting approximately 19 000 features compared to the ∼6 000 found using the rapid gradient method. Similar levels of repeatability were seen for both methods. Despite the reduced peak capacity and the reduction in ions detected, the RAMMP method was able to achieve similar levels of group discrimination as conventional UPLC-MS when applied to rat urine samples obtained from investigative studies on the effects of acute 2-bromophenol and chronic acetaminophen administration. When compared to a direct infusion MS method of similar analysis time the RAMMP method provided superior selectivity. The RAMMP approach provides a robust and sensitive method that is well suited to high-throughput metabonomic analysis of complex mixtures such as urine combined with a 5-fold reduction in analysis time compared with the conventional UPLC-MS method.

  7. Rapid identification of regulated organic chemical compounds in toys using ambient ionization and a miniature mass spectrometry system.

    Science.gov (United States)

    Guo, Xiangyu; Bai, Hua; Lv, Yueguang; Xi, Guangcheng; Li, Junfang; Ma, Xiaoxiao; Ren, Yue; Ouyang, Zheng; Ma, Qiang

    2018-04-01

    Rapid, on-site analysis was achieved through significantly simplified operation procedures for a wide variety of toy samples (crayon, temporary tattoo sticker, finger paint, modeling clay, and bubble solution) using a miniature mass spectrometry system with ambient ionization capability. The labor-intensive analytical protocols involving sample workup and chemical separation, traditionally required for MS-based analysis, were replaced by direct sampling analysis using ambient ionization methods. A Mini β ion trap miniature mass spectrometer was coupled with versatile ambient ionization methods, e.g. paper spray, extraction spray and slug-flow microextraction nanoESI for direct identification of prohibited colorants, carcinogenic primary aromatic amines, allergenic fragrances, preservatives and plasticizers from raw toy samples. The use of paper substrates coated with Co 3 O 4 nanoparticles allowed a great increase in sensitivity for paper spray. Limits of detection as low as 5μgkg -1 were obtained for target analytes. The methods being developed based on the integration of ambient ionization with miniature mass spectrometer represent alternatives to current in-lab MS analysis operation, and would enable fast, outside-the-lab screening of toy products to ensure children's safety and health. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Rapid screening and characterisation of antioxidants of Cosmos caudatus using liquid chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Shui, Guanghou; Leong, Lai Peng; Wong, Shih Peng

    2005-11-15

    Ulam raja (Cosmos caudatus) is used traditionally for improving blood circulation. In this study, it was found that ulam raja had extremely high antioxidant capacity of about 2,400 mg l-ascorbic acid equivalent antioxidant capacity (AEAC) per 100 g of fresh sample. Antioxidant peaks in extract of ulam raja were firstly characterized using free radical spiking test through high performance liquid chromatography coupled with mass spectrometry (MS). Upon reaction with 2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) free radicals, intensities of antioxidant peaks will be significantly reduced. HPLC/MS(n) was further applied to elucidate the chemical structures of antioxidant peaks characterized in the spiking test. More than twenty antioxidants were identified in ulam raja, and their chemical structures were proposed. The major antioxidants in ulam raja were attributed to a number of proanthocyanidins that existed as dimers through hexamers, quercetin glycosides, chlorogenic, neo-chlorogenic, crypto-chlorogenic acid and (+)-catching. High content of antioxidants antioxidants contained in ulam raja could be partly responsible for its ability to reduce oxidative stress.

  9. Rapid characterization of biotherapeutic proteins by size-exclusion chromatography coupled to native mass spectrometry.

    Science.gov (United States)

    Haberger, Markus; Leiss, Michael; Heidenreich, Anna-Katharina; Pester, Oxana; Hafenmair, Georg; Hook, Michaela; Bonnington, Lea; Wegele, Harald; Haindl, Markus; Reusch, Dietmar; Bulau, Patrick

    2016-01-01

    High-molecular weight aggregates such as antibody dimers and other side products derived from incorrect light or heavy chain association typically represent critical product-related impurities for bispecific antibody formats. In this study, an approach employing ultra-pressure liquid chromatography size-exclusion separation combined with native electrospray ionization mass spectrometry for the simultaneous formation, identification and quantification of size variants in recombinant antibodies was developed. Samples exposed to storage and elevated temperature(s) enabled the identification of various bispecific antibody size variants. This test system hence allowed us to study the variants formed during formulation and bio-process development, and can thus be transferred to quality control units for routine in-process control and release analytics. In addition, native SEC-UV/MS not only facilitates the detailed analysis of low-abundant and non-covalent size variants during process characterization/validation studies, but is also essential for the SEC-UV method validation prior to admission to the market.

  10. A SIMPLE AND RAPID MATRIX-ASSISTED LASER DESORPTION/IONIZATION TIME OF FLIGHT MASS SPECTROMETRY METHOD TO SCREEN FISH PLASMA SAMPLES FOR ESTROGEN-RESPONSIVE BIOMARKERS

    Science.gov (United States)

    In this study, we describe and evaluate the performance of a simple and rapid mass spectral method for screening fish plasma for estrogen-responsive biomarkers using matrix assisted laster desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS) couopled with a short...

  11. Rapid Quadrupole-Time-of-Flight Mass Spectrometry Method Quantifies Oxygen-Rich Lignin Compound in Complex Mixtures

    Science.gov (United States)

    Boes, Kelsey S.; Roberts, Michael S.; Vinueza, Nelson R.

    2017-12-01

    Complex mixture analysis is a costly and time-consuming task facing researchers with foci as varied as food science and fuel analysis. When faced with the task of quantifying oxygen-rich bio-oil molecules in a complex diesel mixture, we asked whether complex mixtures could be qualitatively and quantitatively analyzed on a single mass spectrometer with mid-range resolving power without the use of lengthy separations. To answer this question, we developed and evaluated a quantitation method that eliminated chromatography steps and expanded the use of quadrupole-time-of-flight mass spectrometry from primarily qualitative to quantitative as well. To account for mixture complexity, the method employed an ionization dopant, targeted tandem mass spectrometry, and an internal standard. This combination of three techniques achieved reliable quantitation of oxygen-rich eugenol in diesel from 300 to 2500 ng/mL with sufficient linearity (R2 = 0.97 ± 0.01) and excellent accuracy (percent error = 0% ± 5). To understand the limitations of the method, it was compared to quantitation attained on a triple quadrupole mass spectrometer, the gold standard for quantitation. The triple quadrupole quantified eugenol from 50 to 2500 ng/mL with stronger linearity (R2 = 0.996 ± 0.003) than the quadrupole-time-of-flight and comparable accuracy (percent error = 4% ± 5). This demonstrates that a quadrupole-time-of-flight can be used for not only qualitative analysis but also targeted quantitation of oxygen-rich lignin molecules in complex mixtures without extensive sample preparation. The rapid and cost-effective method presented here offers new possibilities for bio-oil research, including: (1) allowing for bio-oil studies that demand repetitive analysis as process parameters are changed and (2) making this research accessible to more laboratories. [Figure not available: see fulltext.

  12. [Rapid determination of alkaloids in tobacco using gas chromatography-mass spectrometry with full scan-selected ion monitoring mode].

    Science.gov (United States)

    Wang, Baoxing; Yang, Shihua; Hou, Ying; Zeng, Xiaoying; Wu, Yi; Xu, Guowang

    2008-05-01

    Simultaneous full scan-selected ion monitoring mode (Scan-SIM) is a new improvement method of data acquisition of gas chromatography-mass spectrometry (GC-MS). A method of determing alkaloids in tobacco was established by GC-MS with Scan-SIM. Nicotine, nornicotine, anabasine and anatabine were determined with scan mode, and myosmine, nicotyrine, 2,3'-bipyridyl and cotinine were determined with SIM mode. The average recoveries of alkaloids ranged from 94.8% to 98.8%, and the relative standard deviations were less than 6.0% (n = 5). Therefore, it is a simple, rapid, accurate method. Tobacco samples picked in different years were determined using this method, and the results were satisfactory.

  13. Rapid identification of molecular changes in tulsi (Ocimum sanctum Linn) upon ageing using leaf spray ionization mass spectrometry.

    Science.gov (United States)

    Sarkar, Depanjan; Srimany, Amitava; Pradeep, T

    2012-10-07

    Tulsi or Holy Basil (Ocimum sanctum Linn) is a medicinally important plant. Ursolic acid (UA) and oleanolic acid (OA) are among its major constituents which account for many medicinal activities of the plant. In the present work, we deployed a new ambient ionization method, leaf spray ionization, for rapid detection of UA, OA and their oxidation products from tulsi leaves. Tandem electrospray ionization mass spectrometry (ESI-MS) has been performed on tulsi leaf extracts in methanol to establish the identity of the compounds. We probed changes occurring in the relative amounts of the parent compounds (UA and OA) with their oxidized products and the latter show an increasing trend upon ageing. The findings are verified by ESI-MS analysis of tulsi leaf extracts, which shows the same trend proving the reliability of the leaf spray method.

  14. Accessible surfaces of beta proteins increase with increasing protein molecular mass more rapidly than those of other proteins.

    Directory of Open Access Journals (Sweden)

    Anna V Glyakina

    Full Text Available Here we present a systematic analysis of accessible surface areas and hydrogen bonds of 2554 globular proteins from four structural classes (all-α, all-β, α/β and α+β proteins that is aimed to learn in which structural class the accessible surface area increases with increasing protein molecular mass more rapidly than in other classes, and what structural peculiarities are responsible for this effect. The beta structural class of proteins was found to be the leader, with the following possible explanations of this fact. First, in beta structural proteins, the fraction of residues not included in the regular secondary structure is the largest, and second, the accessible surface area of packaged elements of the beta-structure increases more rapidly with increasing molecular mass in comparison with the alpha-structure. Moreover, in the beta structure, the probability of formation of backbone hydrogen bonds is higher than that in the alpha helix for all residues of α+β proteins (the average probability is 0.73±0.01 for the beta-structure and 0.60±0.01 for the alpha-structure without proline and α/β proteins, except for asparagine, aspartic acid, glycine, threonine, and serine (0.70±0.01 for the beta-structure and 0.60±0.01 for the alpha-structure without the proline residue. There is a linear relationship between the number of hydrogen bonds and the number of amino acid residues in the protein (Number of hydrogen bonds=0.678·number of residues-3.350.

  15. Rapid Analysis of Bisphenol A and Its Analogues in Food Packaging Products by Paper Spray Ionization Mass Spectrometry.

    Science.gov (United States)

    Chen, Shuo; Chang, Quanying; Yin, Kai; He, Qunying; Deng, Yongxiu; Chen, Bo; Liu, Chengbin; Wang, Ying; Wang, Liping

    2017-06-14

    In this study, a paper spray ionization mass spectrometric (PS-MS) method was developed for the rapid in situ screening and simultaneous quantitative analysis of bisphenol A and its analogues, i.e., bisphenol S, bisphenol F, and bisphenol AF, in food packaging products. At the optimal PS-MS conditions, the calibration curves of bisphenols in the range of 1-100 μg/mL were linear. The correlation coefficients were higher than 0.998, and the LODs of the target compounds were 0.1-0.3 μg/mL. After a simple treatment by dichloromethane on the surface, the samples were analyzed by PS-MS in situ for rapid screening without a traditional sample pretreatment procedure, such as powdering, extraction, and enrichment steps. The analytical time of the PS-MS method was less than 1 min. In comparison with conventional HPLC-MS/MS, it was demonstrated that PS-MS was a more effective high-throughput screening and quantitative analysis method.

  16. A rapid quantitative method for the analysis of synthetic cannabinoids by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Freijo, Tom D; Harris, Steve E; Kala, Subbarao V

    2014-10-01

    Synthetic cannabinoids represent an emerging drug problem in the USA, as these compounds are constantly being modified and rapidly sold as soon as they become available. Laboratories around the world are constantly improving the analytical methods to detect and identify these newly available designer drugs. This study used a simple approach to detect and quantify a variety of synthetic cannabinoids (14 parent compounds and 15 metabolites including series XLR, AM, JWH, UR, RCS, PB, HU and AB-FUBINACA) using LC-MS-MS. Drug-free urine samples spiked with various synthetic cannabinoids and their metabolites were separated on a C18-Hypersil Gold column using an Agilent 1290 ultra-high performance liquid chromatography and detected by an AB Sciex API 4000 tandem mass spectrometer. Studies were carried out to determine limit of detection, limit of quantitation, upper limit of linearity, ion suppression, interference, precision and accuracy to validate the method. Urine samples from patients and known users were hydrolyzed with β-glucuronidase prior to the analysis by LC-MS-MS, and the data are presented. The method described here is rapid, highly sensitive and specific for the identification of a variety of synthetic cannabinoids. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  17. Rapid detection of sugar alcohol precursors and corresponding nitrate ester explosives using direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Sisco, Edward; Forbes, Thomas P

    2015-04-21

    This work highlights the rapid detection of nitrate ester explosives and their sugar alcohol precursors by direct analysis in real time mass spectrometry (DART-MS) using an off-axis geometry. Demonstration of the effect of various parameters, such as ion polarity and in-source collision induced dissociation (CID) on the detection of these compounds is presented. Sensitivity of sugar alcohols and nitrate ester explosives was found to be greatest in negative ion mode with sensitivities ranging from hundreds of picograms to hundreds of nanograms, depending on the characteristics of the particular molecule. Altering the in-source CID potential allowed for acquisition of characteristic molecular ion spectra as well as fragmentation spectra. Additional studies were completed to identify the role of different experimental parameters on the sensitivity for these compounds. Variables that were examined included the DART gas stream temperature, the presence of a related compound (i.e., the effect of a precursor on the detection of a nitrate ester explosive), incorporation of dopant species and the role of the analysis surface. It was determined that each variable affected the response and detection of both sugar alcohols and the corresponding nitrate ester explosives. From this work, a rapid and sensitive method for the detection of individual sugar alcohols and corresponding nitrate ester explosives, or mixtures of the two, has been developed, providing a useful tool in the real-world identification of homemade explosives.

  18. Optimization of Analytical Conditions for a Rapid Determination of Aniline in Environmental Water by Liquid Chromatography/Tandem Mass Spectrometry.

    Science.gov (United States)

    Furukawa, Koji; Hashimoto, Makoto; Kaneco, Satoshi

    2017-01-01

    A rapid determination of aniline in environmental water was examined based on liquid chromatography/tandem mass spectrometry (LC/MS/MS). Environmental water samples were diluted 20-fold with Mill-Q water and measured by LC/MS/MS after adding a surrogate substance (aniline-d5). In the results of the present study, the calibration curve of aniline showed good linearity in the range of 0.05 - 2.0 μg/L. Since the RSD (repeatability) by measuring repeatedly an aniline standard solution (0.05 μg/L, n = 7) was 3.2%, the repeatability of this work was very excellent. In addition, the recovery rate of aniline in environmental water was in the range of 99.0 - 102% with RSD 3.4 - 7.7%, and very good recovery test results were obtained. From these results, this analytical method was confirmed to be effective for aniline measurements of environmental water samples. Also, it is possible to conduct rapid analyses of aniline in environmental water without any solid-phase extraction process, compared to the solid-phase extraction-GC/MS method.

  19. Rapidly increasing body mass index among children, adolescents and young adults in a transitioning population, South Africa, 2008-15.

    Science.gov (United States)

    Sartorius, B; Sartorius, K; Taylor, M; Aagaard-Hansen, J; Dukhi, N; Day, C; Ndlovu, N; Slotow, R; Hofman, K

    2017-12-14

    There is a global epidemic of overweight and obesity; however, this rate of increase is even greater in some low- and middle-income countries (LMIC). South Africa (SA) is undergoing rapid socioeconomic and demographic changes that have triggered a rapid nutrition transition. The paper focuses on the recent rate of change of body mass index (BMI) among children, adolescents and young adults, further stratified by key sociodemographic factors. We analysed mean BMI of 28 247 individuals (including children) from 7301 households by age and year, from anthropometric data from four national cross-sectional (repeated panel) surveys using non-linear fitted curves and associated 95% confidence intervals. From 2008 to 2015, there was rapid rise in mean BMI in the 6-25 age band, with the highest risk (3-4+ BMI unit increase) among children aged 8-10 years. The increase was largely among females in urban areas and of middle-high socioeconomic standing. Prominent gains were also observed in certain rural areas, with extensive geographical heterogeneity across the country. We have demonstrated a major deviation from the current understanding of patterns of BMI increase, with a rate of increase substantially greater in the developing world context compared with the global pattern. This population-wide effect will have major consequences for national development as the epidemic of related non-communicable disease unfolds, and will overtax the national health care budget. Our refined understanding highlights that risks are further compounded for certain groups/places, and emphasizes that urgent geographical and population-targeted interventions are necessary. These interventions could include a sugar tax, clearer food labelling, revised school feeding programmes and mandatory bans on unhealthy food marketing to children.The scenario unfolding in South Africa will likely be followed in other LMICs.

  20. Fourier Transform Mass Spectrometry and Nuclear Magnetic Resonance Analysis for the Rapid and Accurate Characterization of Hexacosanoylceramide.

    Science.gov (United States)

    Ross, Charles W; Simonsick, William J; Bogusky, Michael J; Celikay, Recep W; Guare, James P; Newton, Randall C

    2016-06-28

    Ceramides are a central unit of all sphingolipids which have been identified as sites of biological recognition on cellular membranes mediating cell growth and differentiation. Several glycosphingolipids have been isolated, displaying immunomodulatory and anti-tumor activities. These molecules have generated considerable interest as potential vaccine adjuvants in humans. Accurate analyses of these and related sphingosine analogues are important for the characterization of structure, biological function, and metabolism. We report the complementary use of direct laser desorption ionization (DLDI), sheath flow electrospray ionization (ESI) Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS) and high-field nuclear magnetic resonance (NMR) analysis for the rapid, accurate identification of hexacosanoylceramide and starting materials. DLDI does not require stringent sample preparation and yields representative ions. Sheath-flow ESI yields ions of the product and byproducts and was significantly better than monospray ESI due to improved compound solubility. Negative ion sheath flow ESI provided data of starting materials and products all in one acquisition as hexacosanoic acid does not ionize efficiently when ceramides are present. NMR provided characterization of these lipid molecules complementing the results obtained from MS analyses. NMR data was able to differentiate straight chain versus branched chain alkyl groups not easily obtained from mass spectrometry.

  1. Rapid assignment of malting barley varieties by matrix-assisted laser desorption-ionisation - Time-of-flight mass spectrometry.

    Science.gov (United States)

    Šedo, Ondrej; Kořán, Michal; Jakešová, Michaela; Mikulíková, Renata; Boháč, Michal; Zdráhal, Zbyněk

    2016-09-01

    A method for discriminating malting barley varieties based on direct matrix-assisted laser desorption-ionisation - time-of-flight mass spectrometry (MALDI-TOF MS) fingerprinting of proteins was developed. Signals corresponding to hordeins were obtained by simple mixing of powdered barley grain with a MALDI matrix solution containing 12.5mgmL(-1) of ferulic acid in an acetonitrile:water:formic acid 50:33:17 v/v/v mixture. Compared to previous attempts at MALDI-TOF mass spectrometric analysis of barley proteins, the extraction and fractionation steps were practically omitted, resulting in a significant reduction in analytical time and costs. The discriminatory power was examined on twenty malting barley varieties and the practicability of the method was tested on sixty barley samples acquired from Pilsner Urquell Brewery. The method is proposed as a rapid tool for variety assignment and purity determination of malting barley that may replace gel electrophoresis currently used for this purpose. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Rapid and sensitive liquid chromatography tandem mass spectrometry method for the quantification of ambroxol in human plasma.

    Science.gov (United States)

    Hu, Wanqun; Xu, Yu; Liu, Fei; Liu, Aixiang; Guo, Qingxiang

    2008-10-01

    A sensitive, specific and rapid high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was described and validated for the quantification of ambroxol in human plasma using enalaprilat as the internal standard (IS). Chromatographic separation was performed on a Lichrospher CN column with a mobile phase of methanol and water (containing 0.1% formic acid) (70:30, v/v). The total run time was 5.0 min for each sample. The analytes was detected by mass spectrometry with electrospray ionization source in positive selected reaction monitoring mode. The precursor-fragment ion reaction for ambroxol was m/z 378.9 --> 263.8, and for IS was m/z 349.0 --> 205.9. The linearity was established over the concentration range of 1.56-400.00 ng/mL. The inter-day and the intra-day precisions were all within 10%. A simple protein precipitation with methanol was adopted for sample preparation. The extraction recoveries of ambroxol and IS were higher than 90.80%. The validated method was successfully applied in pharmacokinetic study after oral administration of 90 mg ambroxol to 24 healthy volunteers.

  3. Fourier Transform Mass Spectrometry and Nuclear Magnetic Resonance Analysis for the Rapid and Accurate Characterization of Hexacosanoylceramide

    Directory of Open Access Journals (Sweden)

    Charles W. Ross

    2016-06-01

    Full Text Available Ceramides are a central unit of all sphingolipids which have been identified as sites of biological recognition on cellular membranes mediating cell growth and differentiation. Several glycosphingolipids have been isolated, displaying immunomodulatory and anti-tumor activities. These molecules have generated considerable interest as potential vaccine adjuvants in humans. Accurate analyses of these and related sphingosine analogues are important for the characterization of structure, biological function, and metabolism. We report the complementary use of direct laser desorption ionization (DLDI, sheath flow electrospray ionization (ESI Fourier transform ion cyclotron resonance mass spectrometry (FTICR MS and high-field nuclear magnetic resonance (NMR analysis for the rapid, accurate identification of hexacosanoylceramide and starting materials. DLDI does not require stringent sample preparation and yields representative ions. Sheath-flow ESI yields ions of the product and byproducts and was significantly better than monospray ESI due to improved compound solubility. Negative ion sheath flow ESI provided data of starting materials and products all in one acquisition as hexacosanoic acid does not ionize efficiently when ceramides are present. NMR provided characterization of these lipid molecules complementing the results obtained from MS analyses. NMR data was able to differentiate straight chain versus branched chain alkyl groups not easily obtained from mass spectrometry.

  4. Extranodal NK/T-cell lymphoma, nasal type, manifesting as rapidly progressive dementia without any mass or enhancing brain lesion.

    Science.gov (United States)

    Shimatani, Yoshimitsu; Nakano, Yuta; Tsuyama, Naoko; Murayama, Shigeo; Oki, Ryosuke; Miyamoto, Ryosuke; Murakami, Nagahisa; Fujita, Koji; Watanabe, Syunsuke; Uehara, Hisanori; Abe, Takashi; Nodera, Hiroyuki; Kawarai, Toshitaka; Izumi, Yuishin; Kaji, Ryuji

    2016-10-01

    Among the many potential etiologies for rapidly progressive dementia (RPD), primary central nervous system extranodal NK/T-cell lymphoma, nasal-type (ENKL) is a rare entity. We present the first reported case of autopsy-proven RPD due to ENKL without any mass or enhancing lesion of the brain. A 54-year-old immunocompetent man presented with RPD, myoclonus and ataxia. The mini-mental state examination (MMSE) score was 22/30. His brain MRI revealed progressive brain atrophy without gadolinium enhancement or mass lesion. Five months after the initial evaluation, cognitive impairment further worsened with an MMSE score of 3/30. At the advanced stage, lumbar MRI showed swollen cauda equina with gadolinium enhancement. The number of Epstein-Barr virus (EBV) DNA in cerebrospinal fluid had gradually increased. Twelve months after onset, the patient died of respiratory failure. Pathological findings revealed that lymphoma cells had diffusely invaded the meninges, parenchyma of the brain, spinal cord and cauda equina. Cells were positive for CD3, CD56 and EBV-encoded small RNAs and negative for CD20. No evidence of malignancy was identified in the visceral organs. This report indicates that ENKL should be recognized as one of the rare causes of RPD. Early testing for EBV-DNA in cerebrospinal fluid and imaging of cauda equina would be useful diagnostic tools. © 2016 Japanese Society of Neuropathology.

  5. Desorption electrospray ionisation mass spectrometry: A rapid screening tool for veterinary drug preparations and forensic samples from hormone crime investigations

    Energy Technology Data Exchange (ETDEWEB)

    Nielen, M.W.F. [RIKILT Institute of Food Safety, P.O. Box 230, 6700 AE Wageningen (Netherlands); Wageningen University, Laboratory of Organic Chemistry, Dreijenplein 8, 6703 HB Wageningen (Netherlands)], E-mail: michel.nielen@wur.nl; Hooijerink, H. [RIKILT Institute of Food Safety, P.O. Box 230, 6700 AE Wageningen (Netherlands); Claassen, F.C. [Wageningen University, Laboratory of Organic Chemistry, Dreijenplein 8, 6703 HB Wageningen (Netherlands); Engelen, M.C. van [RIKILT Institute of Food Safety, P.O. Box 230, 6700 AE Wageningen (Netherlands); Beek, T.A. van [Wageningen University, Laboratory of Organic Chemistry, Dreijenplein 8, 6703 HB Wageningen (Netherlands)

    2009-04-01

    Hormone and veterinary drug screening and forensics can benefit from the recent developments in desorption electrospray ionisation (DESI) mass spectrometry (MS). In this work the feasibility of DESI application has been studied. Using a linear ion trap or quadrupole time-of-flight (TOF) MS instrument both full-scan and data-dependent collision-induced dissociation MS{sup n} spectra were acquired in seconds without sample preparation. Preliminary data are presented for the rapid screening of (pro)hormone supplement samples, an illegal steroid cocktail and forensic samples from veterinary drug investigations. The potential of this DESI approach is clearly demonstrated since compounds observed could be independently confirmed by liquid chromatography/TOFMS with accurate mass measurement, and/or proton nuclear magnetic resonance spectroscopy. Specific concerns related to false-positive and false-negative findings due to limitations in quantification and memory-effects are briefly discussed. It is envisaged that DESI will achieve a prominent role in hormone and veterinary drug analysis in the near future.

  6. Method Development for Rapid Analysis of Natural Radioactive Nuclides Using Sector Field Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lim, J.M.; Ji, Y.Y.; Lee, H.; Park, J.H.; Jang, M.; Chung, K.H.; Kang, M.J.; Choi, G.S. [Korea Atomic Energy Research Institute (Korea, Republic of)

    2014-07-01

    As an attempt to reduce the social costs and apprehension arising from radioactivity in the environment, an accurate and rapid assessment of radioactivity is highly desirable. Naturally occurring radioactive materials (NORM) are widely spread throughout the environment. The concern with radioactivity from these materials has therefore been growing for the last decade. In particular, radiation exposure in the industry when handling raw materials (e.g., coal mining and combustion, oil and gas production, metal mining and smelting, mineral sands (REE, Ti, Zr), fertilizer (phosphate), and building materials) has been brought to the public's attention. To decide the proper handling options, a rapid and accurate analytical method that can be used to evaluate the radioactivity of radionuclides (e.g., {sup 238}U, {sup 235}U, {sup 232}Th, {sup 226}Ra, and {sup 40}K) should be developed and validated. Direct measuring methods such as alpha spectrometry, a liquid scintillation counter (LSC), and mass-spectrometry are usually used for the measurement of radioactivity in NORM samples, and they encounter the most significant difficulties during pretreatment (e.g., purification, speciation, and dilution/enrichment). Since the pretreatment process consequently plays an important role in the measurement uncertainty, method development and validation should be performed. Furthermore, a-spectrometry has a major disadvantage of a long counting time, while it has a prominent measurement capability at a very low activity level of {sup 238}U, {sup 235}U, {sup 232}Th, and {sup 226}Ra. Contrary to the α-spectrometry method, a measurement technique using ICP-MS allow radioactivity in many samples to be measured in a short time period with a high degree of accuracy and precision. In this study, a method was developed for a rapid analysis of natural radioactive nuclides using ICP-MS. A sample digestion process was established using LiBO{sub 2} fusion and Fe co-precipitation. A magnetic

  7. Precision mass measurements for studies of nucleosynthesis via the rapid neutron-capture process Penning-trap mass measurements of neutron-rich cadmium and caesium isotopes

    CERN Document Server

    AUTHOR|(CDS)2085660; Litvinov, Yuri A.; Kreim, Susanne

    Although the theory for the rapid neutron-capture process (r-process) was developed more than 55 years ago, the astrophysical site is still under a debate. Theoretical studies predict that the r-process path proceeds through very neutron-rich nuclei with very asymmetric proton- to-neutron ratios. Knowledge about the properties of neutron-rich isotopes found in similar regions of the nuclear chart and furthermore suitable for r-process studies is still little or even not existing. The basic nuclear properties such as binding energies, half-lives, neutron-induced or neutron-capture reaction cross-sections, play an important role in theoretical simulations and can vary or even drastically alternate results of these studies. Therefore, a considerable effort was put forward to access neutron-rich isotopes at radioactive ion-beam facilities like ISOLDE at CERN. The goal of this PhD thesis is to describe the experimental work done for the precision mass measurements of neutron-rich cadmium (129−131 Cd) and caesium...

  8. Rapid detection of porins by matrix-assisted laser desorption/ionization-time of flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    Yanyan eHU

    2015-08-01

    Full Text Available The rapid and cost-efficient determination of carbapenem resistance is an important prerequisite for the choice of an adequate antibiotic therapy. A MALDI-TOF MS-based assay was set up to detect porins in the current study. A loss of the components of porin alone such as OmpK35/OmpK36 or together with the production of carbapenemases will augment the carbapenem resistance. Ten strains of E. coli and eight strains of K. pneumoniae were conducted for both SDS-PAGE and MALDI-TOF MS analysis. MALDI-TOF/TOF MS analysis was then performed to verify the corrospondence of proteins between SDS-PAGE and MALDI-TOF MS. The results indicated that the mass spectrum of ca. 35,000-m/z, 37,000-m/z and 38,000-m/z peaks of E. coli ATCC 25922 corresponded to OmpA, OmpC and OmpF with molecular weight of approximately ca. 38 kDa, 40 kDa and 41 kDa in SDS-PAGE gel, respectively. The band of OmpC and OmpF porins were unable to be distinguished by SDS-PAGE, whereas it was easy to be differentiated by MALDI-TOF MS. As for K. pneumoniae isolates, the mass spectrum of ca. 36,000-m/z and 38,600-m/z peaks was observed corresponding to OmpA and OmpK36 with molecular weight of approximately ca. 40 kDa and 42 kDa in SDS-PAGE gel, respectively. Porin OmpK35 was not observed in the current SDS-PAGE, while a 37,000-m/z peak was found in K. pneumoniae ATCC 13883 and carbapenem-susceptible strains by MALDI-TOF MS which was presumed to be the characteristic peak of the OmpK35 porin. Compared with SDS-PAGE, MALDI-TOF MS is able to rapidly identify the porin-deficient strains within half an hour with better sensitivity, less cost, and is easier to operate and has less interference.

  9. Plasmonic Thermal Decomposition/Digestion of Proteins: A Rapid On-Surface Protein Digestion Technique for Mass Spectrometry Imaging.

    Science.gov (United States)

    Zhou, Rong; Basile, Franco

    2017-09-05

    A method based on plasmon surface resonance absorption and heating was developed to perform a rapid on-surface protein thermal decomposition and digestion suitable for imaging mass spectrometry (MS) and/or profiling. This photothermal process or plasmonic thermal decomposition/digestion (plasmonic-TDD) method incorporates a continuous wave (CW) laser excitation and gold nanoparticles (Au-NPs) to induce known thermal decomposition reactions that cleave peptides and proteins specifically at the C-terminus of aspartic acid and at the N-terminus of cysteine. These thermal decomposition reactions are induced by heating a solid protein sample to temperatures between 200 and 270 °C for a short period of time (10-50 s per 200 μm segment) and are reagentless and solventless, and thus are devoid of sample product delocalization. In the plasmonic-TDD setup the sample is coated with Au-NPs and irradiated with 532 nm laser radiation to induce thermoplasmonic heating and bring about site-specific thermal decomposition on solid peptide/protein samples. In this manner the Au-NPs act as nanoheaters that result in a highly localized thermal decomposition and digestion of the protein sample that is independent of the absorption properties of the protein, making the method universally applicable to all types of proteinaceous samples (e.g., tissues or protein arrays). Several experimental variables were optimized to maximize product yield, and they include heating time, laser intensity, size of Au-NPs, and surface coverage of Au-NPs. Using optimized parameters, proof-of-principle experiments confirmed the ability of the plasmonic-TDD method to induce both C-cleavage and D-cleavage on several peptide standards and the protein lysozyme by detecting their thermal decomposition products with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). The high spatial specificity of the plasmonic-TDD method was demonstrated by using a mask to digest designated sections of

  10. Rapid Identification of the Foodborne Pathogen Trichinella spp. by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry.

    Science.gov (United States)

    Mayer-Scholl, Anne; Murugaiyan, Jayaseelan; Neumann, Jennifer; Bahn, Peter; Reckinger, Sabine; Nöckler, Karsten

    2016-01-01

    Human trichinellosis occurs through consumption of raw or inadequately processed meat or meat products containing larvae of the parasitic nematodes of the genus Trichinella. Currently, nine species and three genotypes are recognized, of which T. spiralis, T. britovi and T. pseudospiralis have the highest public health relevance. To date, the differentiation of the larvae to the species and genotype level is based primarily on molecular methods, which can be relatively time consuming and labor intensive. Due to its rapidness and ease of use a matrix assisted laser desorption / ionization time of flight mass spectrometry (MALDI-TOF MS) reference spectra database using Trichinella strains of all known species and genotypes was created. A formicacid/acetonitrile protein extraction was carried out after pooling 10 larvae of each Trichinella species and genotype. Each sample was spotted 9 times using α-cyano 4-hydoxy cinnamic acid matrix and a MicroFlex LT mass spectrometer was used to acquire 3 spectra (m/z 2000 to 20000 Da) from each spot resulting in 27 spectra/species or genotype. Following the spectra quality assessment, Biotyper software was used to create a main spectra library (MSP) representing nine species and three genotypes of Trichinella. The evaluation of the spectra generated by MALDI-TOF MS revealed a classification which was comparable to the results obtained by molecular methods. Also, each Trichinella species utilized in this study was distinct and distinguishable with a high confidence level. Further, different conservation methods such as freezing and conservation in alcohol and the host species origin of the isolated larvae did not have a significant influence on the generated spectra. Therefore, the described MALDI-TOF MS can successfully be implemented for both genus and species level identification and represents a major step forward in the use of this technique in foodborne parasitology.

  11. Rapid dereplication of estrogenic compounds in pomegranate (Punica granatum) using on-line biochemical detection coupled to mass spectrometry.

    Science.gov (United States)

    van Elswijk, Danny A; Schobel, Uwe P; Lansky, Ephraim P; Irth, Hubertus; van der Greef, Jan

    2004-01-01

    During recent years, phytoestrogens have been receiving an increasing amount of interest, as several lines of evidence suggest a possible role in preventing a range of diseases, including the hormonally dependent cancers. In this context, various parts of the pomegranate fruit (Punica granatum; Punicaceae), e.g. seed oil, juice, fermented juice and peel extract, have been shown to exert suppressive effects on human breast cancer cells in vitro. On-line biochemical detection coupled to mass spectrometry (LC-BCD-MS) was applied to rapidly profile the estrogenic activity in the pomegranate peel extract. The crude mixture was separated by HPLC, after which the presence of biologically active compounds, known or unknown, was detected by means of an on-line beta-estrogen receptor (ER) bioassay. Chemical information, such as molecular weight and MS/MS fingerprint, was obtained in real time by directing part of the HPLC effluent towards a mass spectrometer. Using this approach in total three estrogenic compounds, i.e. luteolin, quercetin and kaempferol, were detected and identified by comparing the obtained molecular weights and negative ion APCI MS/MS spectra with the data of an estrogenic compound library. Although well known in literature and widely distributed in nature, the presence of these phytoestrogenic compounds in pomegranate peel extract was not reported previously. Compared to traditional screening approaches of complex mixtures, often characterized by a repeating cycle of HPLC fractionation and biological screening, LC-BCD-MS was shown to profoundly accelerate the time required for compound description and identification.

  12. BREATHING FIRE: HOW STELLAR FEEDBACK DRIVES RADIAL MIGRATION, RAPID SIZE FLUCTUATIONS, AND POPULATION GRADIENTS IN LOW-MASS GALAXIES

    Energy Technology Data Exchange (ETDEWEB)

    El-Badry, Kareem; Geha, Marla [Department of Astronomy, Yale University, New Haven, CT (United States); Wetzel, Andrew; Hopkins, Philip F. [TAPIR, California Institute of Technology, Pasadena, CA USA (United States); Kereš, Dusan; Chan, T. K. [Department of Physics, Center for Astrophysics and Space Sciences, University of California at San Diego, La Jolla (United States); Faucher-Giguère, Claude-André, E-mail: kareem.el-badry@yale.edu [Department of Physics and Astronomy and CIERA, Northwestern University, Evanston, IL (United States)

    2016-04-01

    We examine the effects of stellar feedback and bursty star formation on low-mass galaxies (M{sub star} = 2 × 10{sup 6} − 5 × 10{sup 10} M{sub ⊙}) using the Feedback in Realistic Environments (FIRE) simulations. While previous studies emphasized the impact of feedback on dark matter profiles, we investigate the impact on the stellar component: kinematics, radial migration, size evolution, and population gradients. Feedback-driven outflows/inflows drive significant radial stellar migration over both short and long timescales via two processes: (1) outflowing/infalling gas can remain star-forming, producing young stars that migrate ∼1 kpc within their first 100 Myr, and (2) gas outflows/inflows drive strong fluctuations in the global potential, transferring energy to all stars. These processes produce several dramatic effects. First, galaxies’ effective radii can fluctuate by factors of >2 over ∼200 Myr, and these rapid size fluctuations can account for much of the observed scatter in the radius at fixed M{sub star}. Second, the cumulative effects of many outflow/infall episodes steadily heat stellar orbits, causing old stars to migrate outward most strongly. This age-dependent radial migration mixes—and even inverts—intrinsic age and metallicity gradients. Thus, the galactic-archaeology approach of calculating radial star formation histories from stellar populations at z = 0 can be severely biased. These effects are strongest at M{sub star} ≈ 10{sup 7–9.6} M{sub ⊙}, the same regime where feedback most efficiently cores galaxies. Thus, detailed measurements of stellar kinematics in low-mass galaxies can strongly constrain feedback models and test baryonic solutions to small-scale problems in ΛCDM.

  13. Rapid Identification of the Foodborne Pathogen Trichinella spp. by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry.

    Directory of Open Access Journals (Sweden)

    Anne Mayer-Scholl

    Full Text Available Human trichinellosis occurs through consumption of raw or inadequately processed meat or meat products containing larvae of the parasitic nematodes of the genus Trichinella. Currently, nine species and three genotypes are recognized, of which T. spiralis, T. britovi and T. pseudospiralis have the highest public health relevance. To date, the differentiation of the larvae to the species and genotype level is based primarily on molecular methods, which can be relatively time consuming and labor intensive. Due to its rapidness and ease of use a matrix assisted laser desorption / ionization time of flight mass spectrometry (MALDI-TOF MS reference spectra database using Trichinella strains of all known species and genotypes was created. A formicacid/acetonitrile protein extraction was carried out after pooling 10 larvae of each Trichinella species and genotype. Each sample was spotted 9 times using α-cyano 4-hydoxy cinnamic acid matrix and a MicroFlex LT mass spectrometer was used to acquire 3 spectra (m/z 2000 to 20000 Da from each spot resulting in 27 spectra/species or genotype. Following the spectra quality assessment, Biotyper software was used to create a main spectra library (MSP representing nine species and three genotypes of Trichinella. The evaluation of the spectra generated by MALDI-TOF MS revealed a classification which was comparable to the results obtained by molecular methods. Also, each Trichinella species utilized in this study was distinct and distinguishable with a high confidence level. Further, different conservation methods such as freezing and conservation in alcohol and the host species origin of the isolated larvae did not have a significant influence on the generated spectra. Therefore, the described MALDI-TOF MS can successfully be implemented for both genus and species level identification and represents a major step forward in the use of this technique in foodborne parasitology.

  14. Potential of fermentation profiling via rapid measurement of amino acid metabolism by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Dalluge, Joseph J; Smith, Sean; Sanchez-Riera, Fernando; McGuire, Chris; Hobson, Russell

    2004-07-16

    Monitoring amino acid metabolism during fermentation has significant potential from the standpoint of strain selection, optimizing growth and production in host strains, and profiling microbial metabolism and growth state. A method has been developed based on rapid quantification of underivatized amino acids using liquid chromatography-electrospray tandem mass spectrometry (LC-MS-MS) to monitor the metabolism of 20 amino acids during microbial fermentation. The use of a teicoplanin-based chiral stationary phase coupled with electrospray tandem mass spectrometry allows complete amino acid analyses in less than 4 min. Quantification is accomplished using five isotopically labeled amino acids as internal standards. Because comprehensive chromatographic separation and derivatization are not required, analysis time is significantly less than traditional reversed- or normal-phase LC-based amino acid assays. Intra-sample precisions for amino acid measurements in fermentation supernatants using this method average 4.9% (R.S.D.). Inter-day (inter-fermentation) precisions for individual amino acid measurements range from 4.2 to 129% (R.S.D.). Calibration curves are linear over the range 0-300 microg/ml, and detection limits are estimated at 50-450 ng/ml. Data visualization techniques for constructing semi-quantitative fermentation profiles of nitrogen source utilization have also been developed and implemented, and demonstrate that amino acid profiles generally correlate with observed growth profiles. Further, cellular growth events, such as lag-time and cell lysis can be detected using this methodology. Correlation coefficients for the time profiles of each amino acid measured illustrate that while several amino acids are differentially metabolized in similar fermentations, a select group of amino acids display strong correlations in these samples, indicating a sub-population of analytes that may be most useful for fermentation profiling.

  15. Rapid identification of Mycobacterium avium clinical isolates by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Lin, Chuan-Sheng; Su, Chih-Cheng; Hsieh, Shang-Chen; Lu, Chia-Chen; Wu, Tsu-Lan; Jia, Ju-Hsin; Wu, Ting-Shu; Han, Chau-Chung; Tsai, Wen-Cherng; Lu, Jang-Jih; Lai, Hsin-Chih

    2015-04-01

    Rapid and accurate discrimination of Mycobacterium avium from other mycobacteria is essential for appropriate therapeutic management and timely intervention for infection control. However, routine clinical identification methods for M. avium are both time consuming and labor intensive. In the present study, matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) was used to identify specific cellular protein pattern for rapid identification of M. avium isolates. A total of 40 clinically relevant Mycobacterium strains comprising 13 distinct species were enrolled for the MALDI-TOF MS identification. A 10-minute extraction-free examination procedure was set up to obtain mass spectral fingerprints from whole bacterial cells. The characteristic mass spectral peak patterns in the m/z (mass/charge ratio) range of 5-20 kDa can be obtained within 10 minutes. The species-specific mass spectra for M. avium is identified and can be differentiated from as Mycobacterium strains. This technique shortens and simplifies the identification procedure of MALDI-TOF MS and may further extend the mycobacterial MALDI-TOF MS database. Simplicity and rapidity of identification procedures make MALDI-TOF MS an attractive platform in routine identification of mycobacteria. MALDI-TOF MS is applicable for rapid discrimination of M. avium from other Mycobacterium species, and shows its potential for clinical application. Copyright © 2013. Published by Elsevier B.V.

  16. Establishment of an Efficient In Vitro Regeneration Protocol for Rapid and Mass Propagation of Dendrobium chrysotoxum Lindl. Using Seed Culture

    Science.gov (United States)

    2014-01-01

    An efficient in vitro regeneration protocol from seed culture has been established successfully for Dendrobium chrysotoxum, an epiphytic orchid having tremendous ornamental and medicinal values. Seed germination response was encouraging in Mitra (M) medium enriched with different combinations of auxins and cytokinins. Medium supplemented with 0.4% activated charcoal (AC), 2 mg/L 6-benzyl amino purine (BAP), and 2 mg/L indole-3-acetic acid (IAA) produced best seed germination percentage in 2 weeks of culture. Incorporation of higher concentration of kinetin (KN) or BAP in combination with low auxin in medium induced pronounced shooting and leaf formation. Reduction in leaf development was evident when cytokinins exist singly in medium indicating synergistic effect of auxin and cytokinin in leaf induction. Presence of elevated level of indole-3-butyric acid (IBA) or 1-naphthalene acetic acid (NAA) with low cytokinin content in medium generated more in vitro rooting, though IBA was found to be more effective in rooting induction as compared to NAA. The in vitro protocol for asymbiotic seed germination developed from the present investigation can be used for rapid mass propagation of this highly important Dendrobium orchid species. PMID:25401154

  17. Rapid Determination of L-carnitine in Infant and Toddler Formulas by Liquid Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    Ahn, Jang-Hyuk; Kwak, Byung-Man; Park, Jung-Min; Kim, Na-Kyeoung; Kim, Jin-Man

    2014-01-01

    A rapid and simple analytical method for L-carnitine was developed for infant and toddler formulas by liquid chromatography tandem mass spectrometry (LC-MS/MS). A 0.3 g of infant formula and toddler formula sample was mixed in a 50 mL conical tube with 9 mL water and 1 mL 0.1 M hydrochloric acid (HCl) to chemical extraction. Then, chloroform was used for removing a lipid fraction. After centrifuged, L-carnitine was separated and quantified using LC-MS/MS with electrospray ionization (ESI) mode. The precursor ion for L-carnitine was m/z 162, and product ions were m/z 103 (quantitative) and m/z 85 (qualitative), respectively. The results for spiked recovery test were in the range of 93.18-95.64% and the result for certified reference material (SRM 1849a) was within the range of the certificated values. This method could be implemented in many laboratories that require time and labor saving.

  18. Establishment of an efficient in vitro regeneration protocol for rapid and mass propagation of Dendrobium chrysotoxum Lindl. using seed culture.

    Science.gov (United States)

    Nongdam, Potshangbam; Tikendra, Leimapokpam

    2014-01-01

    An efficient in vitro regeneration protocol from seed culture has been established successfully for Dendrobium chrysotoxum, an epiphytic orchid having tremendous ornamental and medicinal values. Seed germination response was encouraging in Mitra (M) medium enriched with different combinations of auxins and cytokinins. Medium supplemented with 0.4% activated charcoal (AC), 2 mg/L 6-benzyl amino purine (BAP), and 2 mg/L indole-3-acetic acid (IAA) produced best seed germination percentage in 2 weeks of culture. Incorporation of higher concentration of kinetin (KN) or BAP in combination with low auxin in medium induced pronounced shooting and leaf formation. Reduction in leaf development was evident when cytokinins exist singly in medium indicating synergistic effect of auxin and cytokinin in leaf induction. Presence of elevated level of indole-3-butyric acid (IBA) or 1-naphthalene acetic acid (NAA) with low cytokinin content in medium generated more in vitro rooting, though IBA was found to be more effective in rooting induction as compared to NAA. The in vitro protocol for asymbiotic seed germination developed from the present investigation can be used for rapid mass propagation of this highly important Dendrobium orchid species.

  19. Rapid and reliable MALDI-TOF mass spectrometry identification of Candida non-albicans isolates from bloodstream infections.

    Science.gov (United States)

    Pulcrano, Giovanna; Iula, Dora Vita; Vollaro, Antonio; Tucci, Alessandra; Cerullo, Monica; Esposito, Matilde; Rossano, Fabio; Catania, Maria Rosaria

    2013-09-01

    Matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry (MS) fingerprinting has recently become an effective instrument for rapid microbiological diagnostics and in particular for identification of micro-organisms directly in a positive blood culture. The aim of the study was to evaluate a collection of 82 stored yeast isolates from bloodstream infection, by MALDI-TOF MS; 21 isolates were identified also directly from positive blood cultures and in the presence of other co-infecting micro-organisms. Of the 82 isolates grown on plates, 64 (76%) were correctly identified by the Vitek II system and 82 (100%) by MALDI-TOF MS; when the two methods gave different results, the isolate was identified by PCR. MALDI-TOF MS was unreliable in identifying two isolates (Candida glabrata and Candida parapsilosis) directly from blood culture; however, direct analysis from positive blood culture samples was fast and effective for the identification of yeast, which is of great importance for early and adequate treatment. © 2013. Published by Elsevier B.V. All rights reserved.

  20. Relationships between rapid isometric torque characteristics and vertical jump performance in division I collegiate American football players: influence of body mass normalization.

    Science.gov (United States)

    Thompson, Brennan J; Ryan, Eric D; Sobolewski, Eric J; Smith, Doug B; Akehi, Kazuma; Conchola, Eric C; Buckminster, Tyler

    2013-10-01

    The purpose of the present study was to examine the relationships between absolute and body mass-normalized rapid isometric torque variables and vertical jump (VJ) performance of the leg extensors and flexors in elite National Collegiate Athletic Association Division I Football Bowl Subdivision collegiate American football players. Thirty-one players performed isometric maximal voluntary contractions of the leg extensor and flexor muscle groups and a countermovement VJ. Rate of torque development (RTD) and the contractile impulse (IMPULSE) were determined from 0 to 30, 0 to 50, 0 to 100, and 0 to 200 milliseconds from the onset of muscular contraction. The relationships between absolute and normalized rapid torque variables and VJ performance were assessed using correlation coefficients (r). There were no significant correlations (p > 0.05) observed between the absolute rapid torque variables and VJ performance, except for leg flexion RTD at 0-200 milliseconds (p = 0.024). All normalized rapid torque variables of the leg extensors and flexors were significantly correlated to VJ performance (p ≤ 0.001-0.026). These findings indicated that normalizing rapid torque variables to body mass improves the relationships between isometric rapid torque variables and VJ performance and normalized leg extension and flexion are both similarly related to VJ performance. Strength and conditioning professionals may use these findings in an attempt to identify and monitor dynamic sport performance. Furthermore, future studies examining the relationship between dynamic on the field performances and laboratory-based isometric strength testing may consider including normalized rapid torque variables.

  1. Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Chen, Fangfang; Gong, Zhiyuan; Kelly, Barry C

    2015-02-27

    A sensitive analytical method based on liquid-liquid extraction (LLE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for rapid analysis of 11 pharmaceuticals and personal care products (PPCPs) in fish plasma micro-aliquots (∼20μL). Target PPCPs included, bisphenol A, carbamazepine, diclofenac, fluoxetine, gemfibrozil, ibuprofen, naproxen, risperidone, sertraline, simvastatin and triclosan. A relatively quicker and cheaper LLE procedure exhibited comparable analyte recoveries with solid-phase extraction. Rapid separation and analysis of target compounds in fish plasma extracts was achieved by employing a high efficiency C-18 HPLC column (Agilent Poroshell 120 SB-C18, 2.1mm×50mm, 2.7μm) and fast polarity switching, enabling effective monitoring of positive and negative ions in a single 9min run. With the exception of bisphenol A, which exhibited relatively high background contamination, method detection limits of individual PPCPs ranged between 0.15 and 0.69pg/μL, while method quantification limits were between 0.05 and 2.3pg/μL. Mean matrix effect (ME) values ranged between 65 and 156% for the various target analytes. Isotope dilution quantification using isotopically labelled internal surrogates was utilized to correct for signal suppression or enhancement and analyte losses during sample preparation. The method was evaluated by analysis of 20μL plasma micro-aliquots collected from zebrafish (Danio rerio) from a laboratory bioaccumulation study, which included control group fish (no exposure), as well as fish exposed to environmentally relevant concentrations of PPCPs. Using the developed LC-MS/MS based method, concentrations of the studied PPCPs were consistently detected in the low pg/μL (ppb) range. The method may be useful for investigations requiring fast, reliable concentration measurements of PPCPs in fish plasma. In particular, the method may be applicable for in situ contaminant biomonitoring, as well as

  2. Rapid screening of N-oxides of chemical warfare agents degradation products by ESI-tandem mass spectrometry.

    Science.gov (United States)

    Sridhar, L; Karthikraj, R; Lakshmi, V V S; Raju, N Prasada; Prabhakar, S

    2014-08-01

    Rapid detection and identification of chemical warfare agents and related precursors/degradation products in various environmental matrices is of paramount importance for verification of standards set by the chemical weapons convention (CWC). Nitrogen mustards, N,N-dialkylaminoethyl-2-chlorides, N,N-dialkylaminoethanols, N-alkyldiethanolamines, and triethanolamine, which are listed CWC scheduled chemicals, are prone to undergo N-oxidation in environmental matrices or during decontamination process. Thus, screening of the oxidized products of these compounds is also an important task in the verification process because the presence of these products reveals alleged use of nitrogen mustards or precursors of VX compounds. The N-oxides of aminoethanols and aminoethylchlorides easily produce [M + H](+) ions under electrospray ionization conditions, and their collision-induced dissociation spectra include a specific neutral loss of 48 u (OH + CH2OH) and 66 u (OH + CH2Cl), respectively. Based on this specific fragmentation, a rapid screening method was developed for screening of the N-oxides by applying neutral loss scan technique. The method was validated and the applicability of the method was demonstrated by analyzing positive and negative samples. The method was useful in the detection of N-oxides of aminoethanols and aminoethylchlorides in environmental matrices at trace levels (LOD, up to 500 ppb), even in the presence of complex masking agents, without the use of time-consuming sample preparation methods and chromatographic steps. This method is advantageous for the off-site verification program and also for participation in official proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons (OPCW), the Netherlands. The structure of N-oxides can be confirmed by the MS/MS experiments on the detected peaks. A liquid chromatography-mass spectrometry (LC-MS) method was developed for the separation of isomeric N-oxides of aminoethanols and

  3. A digital microfluidic system for the investigation of pre-steady-state enzyme kinetics using rapid quenching with MALDI-TOF mass spectrometry

    NARCIS (Netherlands)

    Nichols, K.P.F.; Gardeniers, Johannes G.E.

    2007-01-01

    A digital microfluidic system based on electrowetting has been developed to facilitate the investigation of pre-steady-state reaction kinetics using rapid quenching and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). The device consists of individually

  4. Proton Transfer Reaction Mass Spectrometry detects rapid changes in volatile metabolite emission by Mycobacterium smegmatis after the addition of specific antimicrobial agents

    NARCIS (Netherlands)

    Crespo, E.; Cristescu, S. M.; de Ronde, H.; Kuijper, S.; Kolk, A.H.J.; Anthony, R.M.; Harren, F. J. M.

    2011-01-01

    The metabolic activity of plants, animals or microbes can be monitored by gas headspace analysis. This can be achieved using Proton Transfer Reaction Mass Spectrometry (PTR-MS), a highly sensitive detection method for trace gas analysis. PTR-MS is rapid and can detect metabolic responses on-line as

  5. Rapid quantification of metabolic intermediates in blood by liquid chromatography-tandem mass spectrometry to investigate congenital lactic acidosis.

    Science.gov (United States)

    Peng, Minzhi; Cai, Yanna; Fang, Xiefan; Liu, Li

    2016-10-26

    A novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been established to quantify metabolic intermediates, including lactate (Lac), pyruvate (Pyr), acetoacetate (ACAC) and 3-hydroxybutyrate (3-HB) in blood. Samples were deproteinized with methanol-acetonitrile solution, and analytes were separated on an adamantyl group-bonded reverse phase column and detected in multiple reaction monitoring mode. Total analysis time was 4 min per sample. Method validation results displayed that limits of quantification were 10.0 μmol L(-1) for Lac and Pyr, and 5.0 μmol L(-1)for ACAC and 3-HB. The within- and between-run coefficients of variation were in the range of 1.2-6.4% for all analytes. The recoveries were ranged from 95.6 to 111.5%. The reference values of analytes were determined for the pediatric population. Duo to instability of Lac, Pyr and ACAC in vitro, a comprehensive stability assay was performed to determine optimal conditions for sample collection, pretreatment and storage. Results showed that precipitation of protein in blood at bedside combined with low storage temperature could effectively preserve the integrity of Lac, Pyr and 3-HB, but the precipitated protein accelerated degradation of ACAC. Isolation of supernatant fluid slowed degradation of ACAC. Supernatant samples could store at -20 °C for 10 days. The use of plasma or serum to determine these intermediates was not recommended. In this study, 450 samples from patients were analyzed, and 7 patients were diagnosed as congenital lactic acidosis. With the advantages of rapid, accurate and reliable, this method is very suitable for congenital lactic acidosis screening and researches related to energy metabolism. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Rapid detection and ruling out of neonatal sepsis by PCR coupled with Electrospray Ionization Mass Spectrometry (PCR/ESI-MS).

    Science.gov (United States)

    Delcò, Cristina; Karam, Oliver; Pfister, Riccardo; Gervaix, Alain; Renzi, Gesuele; Emonet, Stéphane; Schrenzel, Jacques; Posfay-Barbe, Klara M

    2017-05-01

    Sepsis is an important cause of morbidity and mortality in neonates and clinicians are typically required to administer empiric antibiotics while waiting for blood culture results. However, prolonged and inappropriate use of antibiotics is associated with various complications and adverse events. Better tools to rapidly rule out bacterial infections are therefore needed. We aimed to assess the negative predictive value of PCR coupled with Electrospray Ionization Mass Spectrometry (PCR/ESI-MS) compared to conventional blood cultures in neonatal sepsis. Prospective observational study. All consecutive neonates (PCR/ESI-MS analysis were collected at the same time as samples for the blood culture, before the initiation of antibiotics. Our primary objective was to evaluate the negative predictive value of PCR/ESI-MS for the detection of bacteria in the bloodstream of newborns with suspected sepsis. Our secondary objective was the evaluation of the sensitivity, specificity and positive predictive value of the PCR/ESI-MS in such a neonatal population. We analysed 114 samples over 14months. The median age and weight were 32weeks+3days and 1840g, respectively. Two patients had negative PCR/ESI-MS results, but positive blood cultures. Overall, the negative predictive value was 98% (95%CI: 92% to 100%). Based on these results, PCR/ESI-MS analysis of blood samples of neonates with suspected sepsis appears to have a very good negative predictive value when compared to blood cultures as gold standard. This novel test might allow for early reassessment of the need for antibiotics. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Rapid methods to determine procyanidins, anthocyanins, theobromine and caffeine in rat tissues by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Serra, Aida; Macià, Alba; Romero, Maria-Paz; Piñol, Carme; Motilva, Maria-José

    2011-06-01

    Rapid, selective and sensitive methods were developed and validated to determine procyanidins, anthocyanins and alkaloids in different biological tissues, such as liver, brain, the aorta vein and adipose tissue. For this purpose, standards of procyanidins (catechin, epicatechin, and dimer B(2)), anthocyanins (cyanidin-3-glucoside and malvidin-3-glucoside) and alkaloids (theobromine, caffeine and theophylline) were used. The methods included the extraction of homogenized tissues by off-line liquid-solid extraction, and then solid-phase extraction to analyze alkaloids, or microelution solid-phase extraction plate for the analysis of procyanidins and anthocyanins. The eluted extracts were then analyzed by ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry, using a triple quadrupole as the analyzer. The optimum extraction solution was water/methanol/phosphoric acid 4% (94/4.5/1.5, v/v/v). The extraction recoveries were higher than 81% for all the studied compounds in all the tissues, except the anthocyanins, which were between 50 and 65% in the liver and brain. In order to show the applicability of the developed methods, different rat tissues were analyzed to determine the procyanidins, anthocyanins and alkaloids and their generated metabolites. The rats had previously consumed 1g of a grape pomace extract (to analyze procyanidins and anthocyanins) or a cocoa extract (to analyze alkaloids) per kilogram of body weight. Different tissues were extracted 4h after administration of the respective extracts. The analysis of the metabolites revealed a hepatic metabolism of procyanidins. The liver was the tissue which produced a greater accumulation of these metabolites. Copyright © 2011 Elsevier B.V. All rights reserved.

  8. Carbachol induces a rapid and sustained hydrolysis of polyphosphoinositide in bovine tracheal smooth muscle measurements of the mass of polyphosphoinositides, 1,2-diacylglycerol, and phosphatidic acid.

    Science.gov (United States)

    Takuwa, Y; Takuwa, N; Rasmussen, H

    1986-11-05

    The effects of carbachol on polyphosphoinositides and 1,2-diacylglycerol metabolism were investigated in bovine tracheal smooth muscle by measuring both lipid mass and the turnover of [3H]inositol-labeled phosphoinositides. Carbachol induces a rapid reduction in the mass of phosphatidylinositol 4,5-bisphosphate and phosphatidylinositol 4-monophosphate and a rapid increase in the mass of 1,2-diacylglycerol and phosphatidic acid. These changes in lipid mass are sustained for at least 60 min. The level of phosphatidylinositol shows a delayed and progressive decrease during a 60-min period of carbachol stimulation. The addition of atropine reverses these responses completely. Carbachol stimulates a rapid loss in [3H]inositol radioactivity from phosphatidylinositol 4,5-bisphosphate and phosphatidylinositol 4-monophosphate associated with production of [3H]inositol trisphosphate. The carbachol-induced change in the mass of phosphoinositides and phosphatidic acid is not affected by removal of extracellular Ca2+ and does not appear to be secondary to an increase in intracellular Ca2+. These results indicate that carbachol causes phospholipase C-mediated polyphosphoinositide breakdown, resulting in the production of inositol trisphosphate and a sustained increase in the actual content of 1,2-diacylglycerol. These results strongly suggest that carbachol-induced contraction is mediated by the hydrolysis of polyphosphoinositides with the resulting generation of two messengers: inositol 1,4,5-trisphosphate and 1,2-diacylglycerol.

  9. Carbachol induces a rapid and sustained hydrolysis of polyphosphoinositide in bovine tracheal smooth muscle measurements of the mass of polyphosphoinositides, 1,2-diacylglycerol, and phosphatidic acid

    Energy Technology Data Exchange (ETDEWEB)

    Takuwa, Y.; Takuwa, N.; Rasmussen, H.

    1986-11-05

    The effects of carbachol on polyphosphoinositides and 1,2-diacylglycerol metabolism were investigated in bovine tracheal smooth muscle by measuring both lipid mass and the turnover of (/sup 3/H)inositol-labeled phosphoinositides. Carbachol induces a rapid reduction in the mass of phosphatidylinositol 4,5-bisphosphate and phosphatidylinositol 4-monophosphate and a rapid increase in the mass of 1,2-diacylglycerol and phosphatidic acid. These changes in lipid mass are sustained for at least 60 min. The level of phosphatidylinositol shows a delayed and progressive decrease during a 60-min period of carbachol stimulation. The addition of atropine reverses these responses completely. Carbachol stimulates a rapid loss in (/sup 3/H)inositol radioactivity from phosphatidylinositol 4,5-bisphosphate and phosphatidylinositol 4-monophosphate associated with production of (/sup 3/H)inositol trisphosphate. The carbachol-induced change in the mass of phosphoinositides and phosphatidic acid is not affected by removal of extracellular Ca/sup 2 +/ and does not appear to be secondary to an increase in intracellular Ca/sup 2 +/. These results indicate that carbachol causes phospholipase C-mediated polyphosphoinositide breakdown, resulting in the production of inositol trisphosphate and a sustained increase in the actual content of 1,2-diacylglycerol. These results strongly suggest that carbachol-induced contraction is mediated by the hydrolysis of polyphosphoinositides with the resulting generation of two messengers: inositol 1,4,5-trisphosphate and 1,2-diacylglycerol.

  10. Rapid determination of benzodiazepines, zolpidem and their metabolites in urine using direct injection liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Jeong, Yu-Dong; Kim, Min Kyung; Suh, Sung Ill; In, Moon Kyo; Kim, Jin Young; Paeng, Ki-Jung

    2015-12-01

    Benzodiazepines and zolpidem are generally prescribed as sedative, hypnotics, anxiolytics or anticonvulsants. These drugs, however, are frequently misused in drug-facilitated crime. Therefore, a rapid and simple liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for identification and quantification of benzodiazepines, zolpidem and their metabolites in urine using deuterium labeled internal standards (IS). Urine samples (120 μL) mixed with 80 μL of the IS solution were centrifuged. An aliquot (5 μL) of the sample solution was directly injected into the LC-MS/MS system for analysis. The mobile phases consisted of water and acetonitrile containing 2mM ammonium trifluoroacetate and 0.2% acetic acid. The analytical column was a Zorbax SB-C18 (100 mm × 2.1 mm i.d., 3.5 μm, Agilent). The separation and detection of 18 analytes were achieved within 10 min. Calibration curves were linear over the concentration ranges of 0.5-20 ng/mL (zolpidem), 1.0-40 ng/mL (flurazepam and temazepam), 2.5-100 ng/mL (7-aminoclonazepam, 1-hydroxymidazolam, midazolam, flunitrazepam and alprazolam), 5.0-200 ng/mL (zolpidem phenyl-4-carboxylic acid, α-hydroxyalprazolam, oxazepam, nordiazepam, triazolam, diazepam and α-hydroxytriazolam), 10-400 ng/mL (lorazepam and desalkylflurazepam) and 10-100 ng/mL (N-desmethylflunitrazepam) with the coefficients of determination (r(2)) above 0.9971. The dilution integrity of the analytes was examined for supplementation of short linear range. Dilution precision and accuracy were tested using two, four and ten-folds dilutions and they ranged from 3.7 to 14.4% and -12.8 to 12.5%, respectively. The process efficiency for this method was 63.0-104.6%. Intra- and inter-day precisions were less than 11.8% and 9.1%, while intra- and inter-day accuracies were less than -10.0 to 8.2%, respectively. The lower limits of quantification were lower than 10 ng/mL for each analyte. The applicability of the developed method was successfully

  11. Reverse transcription-PCR-electrospray ionization mass spectrometry for rapid detection of biothreat and common respiratory pathogens.

    Science.gov (United States)

    Jeng, Kevin; Hardick, Justin; Rothman, Richard; Yang, Samuel; Won, Helen; Peterson, Stephen; Hsieh, Yu-Hsiang; Masek, Billie Jo; Carroll, Karen C; Gaydos, Charlotte A

    2013-10-01

    Electrospray ionization mass spectrometry (ESI-MS) analysis of reverse transcription (RT)-PCR amplicons from human respiratory samples allows for broad pathogen identification approximately 8 h after collection. We investigated the performance characteristics of a high-throughput RT-PCR-coupled ESI-MS assay for distinguishing biothreat (BT) agents from common bacterial, fungal, and viral respiratory pathogens in bronchoalveolar lavage (BAL) fluid specimens from subjects with suspected respiratory infections. In a retrospective case series, 202 BAL fluid specimens were collected at the Johns Hopkins Hospital between August 2010 and February 2011 from patients with suspected acute respiratory infections. Samples were processed using standard bacterial, viral, and fungal testing in the clinical microbiology laboratory as part of routine care and then were blindly spiked with either water or nucleic acids from BT organisms (Bacillus anthracis, Yersinia pestis, Francisella tularensis, Brucella spp., Burkholderia spp., and Rickettsia prowazekii) and tested by RT-PCR-ESI-MS. The sensitivities and specificities of RT-PCR-ESI-MS versus standard clinical methods were as follows: for mock BT DNA, 98.5% sensitivity (95% confidence interval [CI], 94.2 to 99.7%) and 100% specificity (95% CI, 93.1 to 100.0%); for bacterial pathogens, 81.8% sensitivity (95% CI, 74.3 to 87.6%) and 73.6% specificity (95% CI, 64.2 to 81.4%); for viral pathogens, 93.3% sensitivity (95% CI, 66.0 to 99.7%) and 97.3% specificity (95% CI, 89.7 to 99.5%); for fungal pathogens, 42.6% sensitivity (95% CI, 29.5 to 56.7%) and 97.8% specificity (95% CI, 91.8 to 99.6%). Our data suggest that RT-PCR-ESI-MS is a useful adjunct to standard culture protocols for rapid detection of both BT and common respiratory pathogens; further study is required for assay validation, especially for fungal detection, and potential implementation.

  12. Reverse Transcription-PCR–Electrospray Ionization Mass Spectrometry for Rapid Detection of Biothreat and Common Respiratory Pathogens

    Science.gov (United States)

    Jeng, Kevin; Rothman, Richard; Yang, Samuel; Won, Helen; Peterson, Stephen; Hsieh, Yu-Hsiang; Masek, Billie Jo; Carroll, Karen C.; Gaydos, Charlotte A.

    2013-01-01

    Electrospray ionization mass spectrometry (ESI-MS) analysis of reverse transcription (RT)-PCR amplicons from human respiratory samples allows for broad pathogen identification approximately 8 h after collection. We investigated the performance characteristics of a high-throughput RT-PCR-coupled ESI-MS assay for distinguishing biothreat (BT) agents from common bacterial, fungal, and viral respiratory pathogens in bronchoalveolar lavage (BAL) fluid specimens from subjects with suspected respiratory infections. In a retrospective case series, 202 BAL fluid specimens were collected at the Johns Hopkins Hospital between August 2010 and February 2011 from patients with suspected acute respiratory infections. Samples were processed using standard bacterial, viral, and fungal testing in the clinical microbiology laboratory as part of routine care and then were blindly spiked with either water or nucleic acids from BT organisms (Bacillus anthracis, Yersinia pestis, Francisella tularensis, Brucella spp., Burkholderia spp., and Rickettsia prowazekii) and tested by RT-PCR–ESI-MS. The sensitivities and specificities of RT-PCR–ESI-MS versus standard clinical methods were as follows: for mock BT DNA, 98.5% sensitivity (95% confidence interval [CI], 94.2 to 99.7%) and 100% specificity (95% CI, 93.1 to 100.0%); for bacterial pathogens, 81.8% sensitivity (95% CI, 74.3 to 87.6%) and 73.6% specificity (95% CI, 64.2 to 81.4%); for viral pathogens, 93.3% sensitivity (95% CI, 66.0 to 99.7%) and 97.3% specificity (95% CI, 89.7 to 99.5%); for fungal pathogens, 42.6% sensitivity (95% CI, 29.5 to 56.7%) and 97.8% specificity (95% CI, 91.8 to 99.6%). Our data suggest that RT-PCR–ESI-MS is a useful adjunct to standard culture protocols for rapid detection of both BT and common respiratory pathogens; further study is required for assay validation, especially for fungal detection, and potential implementation. PMID:23903543

  13. Characterizing the Performance of a Proton-Transfer-Reaction Mass Spectrometer with a Rapid Cycling Tenax Preconcentrator

    Energy Technology Data Exchange (ETDEWEB)

    Garland, S.P.; Alexander, M.L.

    2006-01-01

    Volatile organic compounds (VOCs) are species of interest for atmospheric modeling, worker chemical exposure and medical studies. Sometimes the required detection limits for these compounds is below the capability of existing real-time instrumentation. Preconcentrators have been implemented as an inexpensive way to amplify chemical signals and improve detection limits. Proton-transfer-reaction mass spectrometry (PTR-MS) has been used as a tool for studying low concentrations of VOCs, but it lacks the capability to differentiate chemical signal contributions from isobaric compounds. In this work, behavior of a newly designed Tenax TA preconcentrator when coupled with a PTRMS is characterized. This novel preconcentrator design allows rapid temperature cycling, maintaining near real-time response. The preconcentrator was exposed to a sample gas of toluene in varying concentrations and loading times between and then thermally desorbed for analysis by PTR-MS. The effects of preconcentrating multiple analytes simultaneously were also investigated as well as the chromatographic effects of the preconcentrator. A linear behavior was observed when the integrated ion count rates (ICPS) from thermal desorption peaks were regressed against both varying loading times at a constant toluene concentration and varying concentrations with constant loading times. From these trends, it is possible to determine the concentration of a VOC by knowing its ICPS from thermal desorption peaks from a known preconcentration time. Peak height ion count rates representing ultimate detectability were amplified by factors up to 257 times the original signal, extending the range of the PTR-MS from 50pptv to nearly 250 parts per quadrillion. This corresponds to an ultimate sensitivity of 200 parts per quadrillion with 20 minute time resolution. Quantitative preconcentrator behavior was demonstrated using ICPS from these ion peaks and were amplified as much as 148 times their original signal. Results

  14. Health co-benefits in mortality avoidance from implementation of the mass rapid transit (MRT) system in Kuala Lumpur, Malaysia.

    Science.gov (United States)

    Kwan, Soo Chen; Tainio, Marko; Woodcock, James; Hashim, Jamal Hisham

    2016-03-01

    The mass rapid transit (MRT) is the largest transport infrastructure project under the national key economic area (NKEA) in Malaysia. As urban rail is anticipated to be the future spine of public transport network in the Greater Kuala Lumpur city, it is important to mainstream climate change mitigation and public health benefits in the local transport development. This study quantifies the health co-benefits in terms of mortality among the urbanites when the first line of the 150 km MRT system in Kuala Lumpur commences by 2017. Using comparative health risk assessment, we estimated the potential health co-benefits from the establishment of the MRT system. We estimated the reduced CO2 emissions and air pollution (PM2.5) exposure reduction among the general population from the reduced use of motorized vehicles. Mortality avoided from traffic incidents involving motorcycles and passenger cars, and from increased physical activity from walking while using the MRT system was also estimated. A total of 363,130 tonnes of CO2 emissions could be reduced annually from the modal shift from cars and motorcycles to the MRT system. Atmospheric PM2.5 concentration could be reduced 0.61 μg/m3 annually (2%). This could avoid a total of 12 deaths, mostly from cardio-respiratory diseases among the city residents. For traffic injuries, 37 deaths could be avoided annually from motorcycle and passenger cars accidents especially among the younger age categories (aged 15-30). One additional death was attributed to pedestrian walking. The additional daily physical activity to access the MRT system could avoid 21 deaths among its riders. Most of the mortality avoided comes from cardiovascular diseases. Overall, a total of 70 deaths could be avoided annually among both the general population and the MRT users in the city. The implementation of the MRT system in Greater Kuala Lumpur could bring substantial health co-benefits to both the general population and the MRT users mainly from the

  15. Volvulus du grêle sur mésentère commun incomplet - une redoutable complication rare chez l'adulte: à propos de 1 cas

    Science.gov (United States)

    Coulibaly, Mahamadoun; Boukatta, Brahim; Derkaoui, Ali; Sbai, Hicham; Ousadden, Abdelmalek; Kanjaa, Nabil

    2015-01-01

    Le mésentère commun résulte d'une anomalie de rotation du tube digestif. Il est caractérisé par la persistance d'une disposition anatomique embryonnaire secondaire à une anomalie de rotation de l'anse ombilicale primitive, constituant ainsi un méso commun à toute l'anse intestinale et une racine du mésentère extrêmement courte. Cette insuffisance de rotation est le plus souvent associée à un défaut d'accolement. Ces anomalies de rotation intestinale peuvent aboutir à des complications redoutables parfois mortelles, qui surviennent généralement au cours de la période néonatale où à l’âge pédiatrique. On estime que la prévalence de ces malformations congénitales à l’âge adulte est de l'ordre de 0,2% à 0,5% âge auquel elles demeurent très souvent asymptomatiques et donc non diagnostiquées. Le diagnostic de volvulus total du grêle peut se faire dans des circonstances très variées: en urgence devant un tableau d'occlusion intestinale aiguë, voire un état de choc pouvant conduire au décès, devant un tableau de douleurs abdominales répétées plus ou moins associées à des troubles du transit. Nous rapportons l'observation d'un patient de 18 ans admis pour volvulus total du grêle sur mésentère commun incomplet chez qui l’évolution était favorable. PMID:26113900

  16. The disk wind in the rapidly spinning stellar-mass black hole 4U 1630-472 observed with NuSTAR

    DEFF Research Database (Denmark)

    King, Ashley L.; Walton, Dominic J.; Miller, Jon M.

    2014-01-01

    We present an analysis of a short NuSTAR observation of the stellar-mass black hole and low-mass X-ray binary 4U 1630-472. Reflection from the inner accretion disk is clearly detected for the first time in this source, owing to the sensitivity of NuSTAR. With fits to the reflection spectrum, we...... find evidence for a rapidly spinning black hole, (1σ statistical errors). However, archival data show that the source has relatively low radio luminosity. Recently claimed relationships between jet power and black hole spin would predict either a lower spin or a higher peak radio luminosity. We also...

  17. Dynamic solid phase microextraction for sampling of airborne sarin with gas chromatography-mass spectrometry for rapid field detection and quantification.

    Science.gov (United States)

    Hook, Gary L; Jackson Lepage, Carmela; Miller, Stephen I; Smith, Philip A

    2004-08-01

    A portable dynamic air sampler and solid phase microextraction were used to simultaneously detect, identify, and quantify airborne sarin with immediate analysis of samples using a field portable gas chromatography-mass spectrometry system. A mathematical model was used with knowledge of the mass of sarin trapped, linear air velocity past the exposed sampling fiber, and sample duration allowing calculation of concentration estimates. For organizations with suitable field portable instrumentation, these methods are potentially useful for rapid onsite detection and quantification of high concern analytes, either through direct environmental sampling or through sampling of air collected in bags.

  18. Detection of Gelatin Adulteration in Traditional Chinese Medicine: Analysis of Deer-Horn Glue by Rapid-Resolution Liquid Chromatography-Triple Quadrupole Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jia Chen

    2015-01-01

    Full Text Available Simultaneous identification of donkey-hide gelatin and bovine-hide gelatin in deer-horn glue was established by rapid-resolution liquid chromatography-triple quadrupole mass spectrometry. Water containing 1% NH4HCO3 was used for sample dissolution and trypsin was used for hydrolysis of the gelatins. After separation by a SB-C18 reversed-phase analytical column, collagen marker peptides were detected by mass spectrometry in positive electrospray ionization mode with multiple reaction monitoring. The method was specific, precise and reliable, and suitable for detection of adulterants derived from donkey-hide gelatin and bovine-hide gelatin in deer-horn glue.

  19. Rapid Screening of Multiclass Syrup Adulterants in Honey by Ultrahigh-Performance Liquid Chromatography/Quadrupole Time of Flight Mass Spectrometry.

    Science.gov (United States)

    Du, Bing; Wu, Liming; Xue, Xiaofeng; Chen, Lanzhen; Li, Yi; Zhao, Jing; Cao, Wei

    2015-07-29

    Honey adulteration with sugar syrups is a widespread problem. Several types of syrups have been used in honey adulteration, and there is no available method that can simultaneously detect all of these adulterants. In this study, we generated a small-scale database containing the specific chromatographic and mass spectrometry information on sugar syrup markers and developed a simple, rapid, and effective ultrahigh-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF-MS) method for the detection of adulterated honey. Corn syrup, high-fructose corn syrup, inverted syrup, and rice syrup were used as honey adulterants; polysaccharides, difructose anhydrides, and 2-acetylfuran-3-glucopyranoside were used as detection markers. The presence of 10% sugar syrup in honey could be easily detected in <30 min using the developed method. The results revealed that UHPLC/Q-TOF-MS was simple and rapid.

  20. Rapid analysis of formic acid, acetic acid, and furfural in pretreated wheat straw hydrolysates and ethanol in a bioethanol fermentation using atmospheric pressure chemical ionisation mass spectrometry

    Science.gov (United States)

    2011-01-01

    Atmospheric pressure chemical ionisation mass spectrometry (APCI-MS) offers advantages as a rapid analytical technique for the quantification of three biomass degradation products (acetic acid, formic acid and furfural) within pretreated wheat straw hydrolysates and the analysis of ethanol during fermentation. The data we obtained using APCI-MS correlated significantly with high-performance liquid chromatography analysis whilst offering the analyst minimal sample preparation and faster sample throughput. PMID:21896164

  1. Rapid Characterization of Microalgae and Microalgae Mixtures Using Matrix-Assisted Laser Desorption Ionization Time-Of-Flight Mass Spectrometry (MALDI-TOF MS).

    Science.gov (United States)

    Barbano, Duane; Diaz, Regina; Zhang, Lin; Sandrin, Todd; Gerken, Henri; Dempster, Thomas

    2015-01-01

    Current molecular methods to characterize microalgae are time-intensive and expensive. Matrix Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (MALDI-TOF MS) may represent a rapid and economical alternative approach. The objectives of this study were to determine whether MALDI-TOF MS can be used to: 1) differentiate microalgae at the species and strain levels and 2) characterize simple microalgal mixtures. A common protein extraction sample preparation method was used to facilitate rapid mass spectrometry-based analysis of 31 microalgae. Each yielded spectra containing between 6 and 56 peaks in the m/z 2,000 to 20,000 range. The taxonomic resolution of this approach appeared higher than that of 18S rDNA sequence analysis. For example, two strains of Scenedesmus acutus differed only by two 18S rDNA nucleotides, but yielded distinct MALDI-TOF mass spectra. Mixtures of two and three microalgae yielded relatively complex spectra that contained peaks associated with members of each mixture. Interestingly, though, mixture-specific peaks were observed at m/z 11,048 and 11,230. Our results suggest that MALDI-TOF MS affords rapid characterization of individual microalgae and simple microalgal mixtures.

  2. Rapid Characterization of Microalgae and Microalgae Mixtures Using Matrix-Assisted Laser Desorption Ionization Time-Of-Flight Mass Spectrometry (MALDI-TOF MS)

    Science.gov (United States)

    Barbano, Duane; Diaz, Regina; Zhang, Lin; Sandrin, Todd; Gerken, Henri; Dempster, Thomas

    2015-01-01

    Current molecular methods to characterize microalgae are time-intensive and expensive. Matrix Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry (MALDI-TOF MS) may represent a rapid and economical alternative approach. The objectives of this study were to determine whether MALDI-TOF MS can be used to: 1) differentiate microalgae at the species and strain levels and 2) characterize simple microalgal mixtures. A common protein extraction sample preparation method was used to facilitate rapid mass spectrometry-based analysis of 31 microalgae. Each yielded spectra containing between 6 and 56 peaks in the m/z 2,000 to 20,000 range. The taxonomic resolution of this approach appeared higher than that of 18S rDNA sequence analysis. For example, two strains of Scenedesmus acutus differed only by two 18S rDNA nucleotides, but yielded distinct MALDI-TOF mass spectra. Mixtures of two and three microalgae yielded relatively complex spectra that contained peaks associated with members of each mixture. Interestingly, though, mixture-specific peaks were observed at m/z 11,048 and 11,230. Our results suggest that MALDI-TOF MS affords rapid characterization of individual microalgae and simple microalgal mixtures. PMID:26271045

  3. Using MALDI-TOF mass spectrometry as a rapid and accurate diagnostic tool in infective endocarditis: a case report of a patient with mitral valve infective endocarditis caused by Abiotrophia defectiva

    DEFF Research Database (Denmark)

    Holler, Jon Gitz; Pedersen, Line; Calum, Henrik

    2011-01-01

    A case of infective endocarditis caused by Abiotrophia defectiva is presented. The use of MALDI-TOF mass spectrometry as a rapid and accurate diagnostic tool in infective endocarditis is discussed.......A case of infective endocarditis caused by Abiotrophia defectiva is presented. The use of MALDI-TOF mass spectrometry as a rapid and accurate diagnostic tool in infective endocarditis is discussed....

  4. Evaluation of Flow-Injection Tandem Mass Spectrometry for Rapid and High-Throughput Quantitative Determination of B-Vitamins in Nutritional Supplements

    Energy Technology Data Exchange (ETDEWEB)

    Bhandari, Deepak [ORNL; Van Berkel, Gary J [ORNL

    2012-01-01

    The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B-vitamins, viz. B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed by adding extraction solvent to a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Automated flow injection introduced 1 L of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s representing significant improvement over conventional liquid chromatography approaches which typically require 25-45 min, and often require more significant sample preparation procedures. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and NIST standard reference material (SRM 3280) multivitamin/multielement tablets. The quantity determined for each B-vitamin in SRM 3280 was within the statistical range provided for the respective certified values. The same sample preparation and analysis approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B-vitamins as evidenced by an agreement with the labels values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.

  5. Rapid profiling of polymeric phenolic acids in Salvia miltiorrhiza by hybrid data-dependent/targeted multistage mass spectrometry acquisition based on expected compounds prediction and fragment ion searching.

    Science.gov (United States)

    Shen, Yao; Feng, Zijin; Yang, Min; Zhou, Zhe; Han, Sumei; Hou, Jinjun; Li, Zhenwei; Wu, Wanying; Guo, De-An

    2018-01-15

    Phenolic acids are the major water-soluble components in Salvia miltiorrhiza (> 5%). According to previous studies, many of them contribute to the cardiovascular effects and antioxidant effects of S. miltiorrhiza. Polymeric phenolic acids can be considered as the tanshinol derived metabolites, e.g., dimmers, trimers and tetramers. A strategy combined with tanshinol-based expected compounds prediction, total ion chromatogram filtering, Fragment Ion Searching and parent list-based multistage mass spectrometry acquisition by Linear Trap Quadropole-orbitrap Velos Mass Spectrometry was proposed to rapid profile polymeric phenolic acids in S. miltiorrhiza. More than 480 potential polymeric phenolic acids could be screened out by this strategy. Based on the fragment information obtained by parent list-activated data dependent multistage mass spectrometry acquisition, 190 polymeric phenolic acids were characterized by comparing their mass information with literature data, and 18 of them were firstly detected from S. miltiorrhiza. Seven potential compounds were tentatively characterized as new polymeric phenolic acids from S. miltiorrhiza. This strategy facilitates identification of polymeric phenolic acids in complex matrix with both selectivity and sensitivity, which could be expanded for rapid discovery and identification of compounds from complex matrix. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  6. Rapid Detection of Gas Hazards and Leaks with an Atmospheric Sampling, High Resolution, Mass Spectrometer with Low Pumping Requirements Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Miniaturization of mass spectrometers is restricted almost exclusively by the ability of small vacuum pumps to remove gas loads during operation of the instrument....

  7. Rapid and Deep Proteomes by Faster Sequencing on a Benchtop Quadrupole Ultra-High-Field Orbitrap Mass Spectrometer

    DEFF Research Database (Denmark)

    Kelstrup, Christian D; Jersie-Christensen, Rosa R; Batth, Tanveer Singh

    2014-01-01

    Shotgun proteomics is a powerful technology for global analysis of proteins and their post-translational modifications. Here, we investigate faster sequencing speed of the latest Q Exactive HF mass spectrometer, which features an ultra-high-field Orbitrap mass analyzer. Proteome coverage is evalu......Shotgun proteomics is a powerful technology for global analysis of proteins and their post-translational modifications. Here, we investigate faster sequencing speed of the latest Q Exactive HF mass spectrometer, which features an ultra-high-field Orbitrap mass analyzer. Proteome coverage...... in less than 24 hours of analysis time by offline high pH reversed-phase peptide fractionation from which we identify more than 140,000 unique peptide sequences. This is comparable to state-of-the-art multi-day, multi-enzyme efforts. Finally the acquisition methods are evaluated for single-shot...

  8. Rapid and Deep Proteomes by Faster Sequencing on a Benchtop Quadrupole Ultra-High-Field Orbitrap Mass Spectrometer

    DEFF Research Database (Denmark)

    Kelstrup, Christian D; Jersie-Christensen, Rosa R; Batth, Tanveer Singh

    2014-01-01

    Shotgun proteomics is a powerful technology for global analysis of proteins and their post-translational modifications. Here, we investigate faster sequencing speed of the latest Q Exactive HF mass spectrometer, which features an ultra-high-field Orbitrap mass analyzer. Proteome coverage is evalu......Shotgun proteomics is a powerful technology for global analysis of proteins and their post-translational modifications. Here, we investigate faster sequencing speed of the latest Q Exactive HF mass spectrometer, which features an ultra-high-field Orbitrap mass analyzer. Proteome coverage...... per second or up to 600 new peptides sequenced per gradient minute. We identify 4400 proteins from one microgram of HeLa digest using a one hour gradient, which is an approximately 30% improvement compared to previous instrumentation. In addition, we show very deep proteome coverage can be achieved...

  9. Direct Infusion Electrospray Ionization - Ion Mobility - High Resolution Mass Spectrometry (DIESI-IM-HRMS) for Rapid Characterization of Potential Bioprocess Streams

    Science.gov (United States)

    Munisamy, Sharon M.; Chambliss, C. Kevin; Becker, Christopher

    2012-07-01

    Direct infusion electrospray ionization - ion mobility - high resolution mass spectrometry (DIESI-IM-HRMS) has been utilized as a rapid technique for the characterization of total molecular composition in "whole-sample" biomass hydrolysates and extracts. IM-HRMS data reveal a broad molecular weight distribution of sample components (up to 1100 m/z) and provide trendline isolation of feedstock components from those introduced "in process." Chemical formulas were obtained from HRMS exact mass measurements (with typical mass error less than 5 ppm) and were consistent with structural carbohydrates and other lignocellulosic degradation products. Analyte assignments are supported via IM-MS collision-cross-section measurements and trendline analysis (e.g., all carbohydrate oligomers identified in a corn stover hydrolysate were found to fall within 6 % of an average trendline). These data represent the first report of collision cross sections for several negatively charged carbohydrates and other acidic species occurring natively in biomass hydrolysates.

  10. Rapid enzymatic hydrolysis of masked deoxynivalenol and zearalenone prior to liquid chromatography mass spectrometry or immuniassay analysis

    NARCIS (Netherlands)

    Nielen, M.W.F.; Weijers, C.A.G.M.; Peters, J.; Weignerová, L.; Zuilhof, H.; Franssen, M.C.R.

    2014-01-01

    Recently it has been shown that conjugates (‘masked mycotoxins’) may contribute to the total daily intake of hazardous mycotoxins. Therefore, there is an urgent need for rapid analysis methods that assess the level of both free and masked mycotoxins in food and feed. However, the analysis of masked

  11. Rapid screening of chemical warfare nerve agent metabolites in urine by atmospheric solids analysis probe-mass spectroscopy (ASAP-MS).

    Science.gov (United States)

    Zydel, Frank; Smith, J Richard; Pagnotti, Vincent S; Lawrence, Richard J; McEwen, Charles N; Capacio, Benedict R

    2012-01-01

    Exposures to organophosphorus nerve agents (OPNA) remain a threat to both civilian and military populations. Verification of exposures typically involves determinations of urinary metabolites or adducted proteins in blood. Urinary alkyl methylphosphonic acid metabolites resulting from hydrolysis of OPNAs provide a convenient marker for OPNA exposure. In a military setting, urine is a relatively easy sample to obtain, and a rapid turnaround for analyses for the identification of metabolites is critical for field commanders. Timely information on use and identity of OPNAs facilitates decisions regarding employment of personal protective equipment and additional strategies to mitigate additional exposure(s). Herein, we report the development of a rapid mass spectrometric (MS) method to identify OPNA metabolites directly from urine with no sample preparation. Synthetic urine spiked with multiple OPNA metabolites was analyzed using an atmospheric solids analysis probe (ASAP) attached to a high resolution mass spectrometer. The alkyl methylphosphonic acid metabolites resulting from hydrolysis of sarin, cyclosarin, soman, and Russian VX were clearly detectable down to a level of 1.0 ng/ml. The ability to rapidly detect OPNA metabolites in unprepared urine allows for the design of a field-deployable device that could afford field personnel the ability to rapidly screen individuals for specific OPNA exposure. In addition, this provides proof-of-concept evidence that a fieldable ASAP-MS device could afford personnel the ability to rapidly detect OPNAs on skin, equipment, and other porous surfaces. Published 2012. This article is a US Government work and is in the public domain in the USA. Copyright © 2012 John Wiley & Sons, Ltd.

  12. Equipment and methods for rapid analysis of PWO full-sized scintillation crystal radiation hardness during mass production

    CERN Document Server

    Drobychev, G Yu; Fedorov, A; Korzhik, M V; Lecoq, P; Lopatik, A; Missevitch, O V; Peigneux, J P; Singovsky, A V; Zouevski, R F

    2001-01-01

    The mass production of lead tungstate crystals (PWO) for the Compact Muon Solenoid (CMS) Project at CERN began at the Bogoroditsk Techno- Chemical Plant (BTCP, Tula Region, Russia) in 2000. Mass production technology, developed in recent years, is based on a set of methods and instrumentation for crystal growth and machining, as well as quality control and certification of crystals. One of the most crucial categories of tolerances is the radiation hardness of crystals. Control of the PWO radiation hardness during the mass production phase requires a reliable, easy-to-use measuring tool with high productivity. A semiautomatic spectrometric setup for PWO radiation hardness monitoring was developed and tested at CERN. After final crosschecks, the setup was put into operation at BTCP. (13 refs).

  13. Precision Mass Measurements of 129-131Cd and Their Impact on Stellar Nucleosynthesis via the Rapid Neutron Capture Process

    CERN Document Server

    Atanasov, D.; Blaum, K.; Cakirli, R.B.; Cocolios, T.E.; George, S.; Herfurth, F.; Kisler, D.; Janka, H.T.; Just, O.; Kowalska, M.; Kreim, S.; Kisler, D.; Litvinov, Yu. A.; Lunney, D.; Manea, V.; Neidherr, D.; Rosenbusch, M.; Schweikhard, L.; Welker, A.; Wienholtz, F.; Wolf, R. N.; Zuber, K.

    2015-01-01

    Masses adjacent to the classical waiting-point nuclide 130Cd have been measured by using the Penning- trap spectrometer ISOLTRAP at ISOLDE/CERN. We find a significant deviation of over 400 keV from earlier values evaluated by using nuclear beta-decay data. The new measurements show the reduction of the N = 82 shell gap below the doubly magic 132Sn. The nucleosynthesis associated with the ejected wind from type-II supernovae as well as from compact object binary mergers is studied, by using state-of-the-art hydrodynamic simulations. We find a consistent and direct impact of the newly measured masses on the calculated abundances in the A = 128 - 132 region and a reduction of the uncertainties from the precision mass input data.

  14. Endocytic pathway rapidly delivers internalized molecules to lysosomes: an analysis of vesicle trafficking, clustering and mass transfer.

    Science.gov (United States)

    Pangarkar, Chinmay; Dinh, Anh-Tuan; Mitragotri, Samir

    2012-08-20

    Lysosomes play a critical role in intracellular drug delivery. For enzyme-based therapies, they represent a potential target site whereas for nucleic acid or many protein drugs, they represent the potential degradation site. Either way, understanding the mechanisms and processes involved in routing of materials to lysosomes after cellular entry is of high interest to the field of drug delivery. Most therapeutic cargoes other than small hydrophobic molecules enter the cells through endocytosis. Endocytosed cargoes are routed to lysosomes via microtubule-based transport and are ultimately shared by various lysosomes via tethering and clustering of endocytic vesicles followed by exchange of their contents. Using a combined experimental and numerical approach, here we studied the rates of mass transfer into and among the endocytic vesicles in a model cell line, 3T3 fibroblasts. In order to understand the relationship of mass transfer with microtubular transport and vesicle clustering, we varied both properties through various pharmacological agents. At the same time, microtubular transport and vesicle clustering were modeled through diffusion-advection equations and the Smoluchowski equations, respectively. Our analysis revealed that the rate of mass transfer is optimally related to microtubular transport and clustering properties of vesicles. Further, the rate of mass transfer is highest in the innate state of the cell. Any perturbation to either microtubular transport or vesicle aggregation led to reduced mass transfer to lysosome. These results suggest that in the absence of an external intervention the endocytic pathway appears to maximize molecular delivery to lysosomes. Strategies are discussed to reduce mass transfer to lysosomes so as to extend the residence time of molecules in endosomes or late endosomes, thus potentially increasing the likelihood of their escape before disposition in the lysosomes. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. A drop in the pond: the effect of rapid mass-loss on the dynamics and interaction rate of collisionless particles

    Science.gov (United States)

    Penoyre, Zephyr; Haiman, Zoltán

    2018-01-01

    In symmetric gravitating systems experiencing rapid mass-loss, particle orbits change almost instantaneously, which can lead to the development of a sharply contoured density profile, including singular caustics for collisionless systems. This framework can be used to model a variety of dynamical systems, such as accretion discs following a massive black hole merger and dwarf galaxies following violent early star formation feedback. Particle interactions in the high-density peaks seem a promising source of observable signatures of these mass-loss events (i.e. a possible EM counterpart for black hole mergers or strong gamma-ray emission from dark matter annihilation around young galaxies), because the interaction rate depends on the square of the density. We study post-mass-loss density profiles, both analytic and numerical, in idealized cases and present arguments and methods to extend to any general system. An analytic derivation is presented for particles on Keplerian orbits responding to a drop in the central mass. We argue that this case, with initially circular orbits, gives the most sharply contoured profile possible. We find that despite the presence of a set of singular caustics, the total particle interaction rate is reduced compared to the unperturbed system; this is a result of the overall expansion of the system dominating over the steep caustics. Finally, we argue that this result holds more generally, and the loss of central mass decreases the particle interaction rate in any physical system.

  16. Multicomponent mixed dopant optimization for rapid screening of polycyclic aromatic hydrocarbons using ultra high performance liquid chromatography coupled to atmospheric pressure photoionization high-resolution mass spectrometry

    KAUST Repository

    Sioud, Salim

    2012-05-04

    RATIONALE To enhance the ionization efficiencies in atmospheric pressure photoionization mass spectrometry a dopant with favorable ionization energy such as chlorobenzene is typically used. These dopants are typically toxic and difficult to mix with water-soluble organic solvents. In order to achieve a more efficient and less toxic dopant, a multicomponent mixed dopant was explored. METHODS A multicomponent mixed dopant for non-targeted rapid screening of polycyclic aromatic hydrocarbons (PAHs) was developed and optimized using ultra high performance liquid chromatography (UPLC) coupled to atmospheric pressure photoionization high-resolution mass spectrometry. Various single and multicomponent mixed dopants consisting of ethanol, chlorobenzene, bromobenzene, anisole and toluene were evaluated. RESULTS Fourteen out of eighteen PAHs were successfully separated and detected at low pg/μL levels within 5 min with high mass accuracy ≤4 ppm. The optimal mixed multicomponent dopant consisted of ethanol/chlorobenzene/bromobenzene/anisole (98.975:0.1:0.9:0.025, v/v %) and it improved the limit of detection (LOD) by 2- to 10-fold for the tested PAHs compared to those obtained with pure chlorobenzene. CONCLUSIONS A novel multicomponent dopant that contains 99% ethanol and 1% mixture of chlorobenzene, bromobenzene and anisole was found to be an effective dopant mixture to ionize PAHs. The developed UPLC multicomponent dopant assisted atmospheric pressure photoionization high-resolution mass spectrometry offered a rapid non targeted screening method for detecting the PAHs at low pg/;μL levels within a 5 min run time with high mass accuracy a;circ4 ppm. Copyright © 2012 John Wiley & Sons, Ltd.

  17. Multicomponent mixed dopant optimization for rapid screening of polycyclic aromatic hydrocarbons using ultra high performance liquid chromatography coupled to atmospheric pressure photoionization high-resolution mass spectrometry.

    Science.gov (United States)

    Sioud, Salim; Amad, Ma'an; Al-Talla, Zeyad A

    2012-06-30

    To enhance the ionization efficiencies in atmospheric pressure photoionization mass spectrometry a dopant with favorable ionization energy such as chlorobenzene is typically used. These dopants are typically toxic and difficult to mix with water-soluble organic solvents. In order to achieve a more efficient and less toxic dopant, a multicomponent mixed dopant was explored. A multicomponent mixed dopant for non-targeted rapid screening of polycyclic aromatic hydrocarbons (PAHs) was developed and optimized using ultra high performance liquid chromatography (UPLC) coupled to atmospheric pressure photoionization high-resolution mass spectrometry. Various single and multicomponent mixed dopants consisting of ethanol, chlorobenzene, bromobenzene, anisole and toluene were evaluated. Fourteen out of eighteen PAHs were successfully separated and detected at low pg/μL levels within 5 min with high mass accuracy ≤4 ppm. The optimal mixed multicomponent dopant consisted of ethanol/chlorobenzene/bromobenzene/anisole (98.975:0.1:0.9:0.025, v/v %) and it improved the limit of detection (LOD) by 2- to 10-fold for the tested PAHs compared to those obtained with pure chlorobenzene. A novel multicomponent dopant that contains 99% ethanol and 1% mixture of chlorobenzene, bromobenzene and anisole was found to be an effective dopant mixture to ionize PAHs. The developed UPLC multicomponent dopant assisted atmospheric pressure photoionization high-resolution mass spectrometry offered a rapid non targeted screening method for detecting the PAHs at low pg/μL levels within a 5 min run time with high mass accuracy ≤4 ppm. Copyright © 2012 John Wiley & Sons, Ltd.

  18. [Rapid screening and identification of 22 allergenic disperse dyes in ecological textiles by high performance liquid chromatography-linear ion trap/orbitrap mass spectrometry].

    Science.gov (United States)

    Niu, Zengyuan; Luo, Xin; Ye, Xiwen; Xiu, Xiaoli; Zhang, Li; Wang, Xin; Chen, Jing

    2015-10-01

    A rapid screening method based on high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry (HPLC-LTQ/Orbitrap MS) for 22 disperse dyes in ecological textiles has been established. The target compounds were extracted by pyridine/water (1:1, v/v) by shaking extraction in 90 degrees C water bath. The extracts were then separated by a CAPCELL PAK C18 column (100 mm x 2.0 mm, 5 μm) using gradient elution with acetonitrile-5 mmol/L ammonium acetate containing 0.01% (v/v) formic acid as mobile phases, and finally analyzed by HPLC-LTQ/Orbitrap in positive and negative ESI modes. The retention time and accurate mass of parent ion were used for fast screening of 22 disperse dyes, while the confirmatory analysis was obtained by fragments generated by collision-induced dissociation (CID) MS/MS. Target analysis exhibited high mass accuracy (textiles, and Disperse Orange 37/76 was detected in one of them. With high selectivity and strong anti-jamming ability, this method is simple, rapid, accurate, and it can be used for the inspection of disperse dyes in textiles.

  19. [Rapid screening and confirming carcinogenic banned azo colorants in textiles by high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry].

    Science.gov (United States)

    Yun, Huan; Liu, Xin; Wang, Jing; Yan, Hua; Cui, Fengyun; Zhang, Zhaohui

    2013-09-01

    A method of high performance liquid chromatography-linear ion trap/orbitrap highresolution mass spectrometry (HPLC-LTP/Orbitrap MS) was ued to screen and confirm-banned azo colorants in textiles rapidly. The analytes were reduced to carcinogenic aromatic amines with sodium dithionite in citrate buffer solution. The reduced solution was extracted bydiatomite, and loadd onto an Acquity UPLC BEH C18 column (50 mm x 2.1 MM. 1.7 microm) with a gradient elution of methanol and 0.1% (v/v) methane acid aqueous solution, and finally detected by linear ion trap/orbitrap high-resolution mass spectrometry in positive ESI mode. In mass spectrometry method, the MS spectrum of high-resolution and the collision induced dissociation (CID) spectrum of data-dependent scan mode were used for screening analysis and conformation, respectively. The calibration curves showed a good linearity in the range of 0.05 -2.00 mg/b, and the correlation coefficients (r) were higher than 0.99. By detecting spiked samples, the limits of quantification were 0.08 mg/kg for all the residues and the recoveries were in the range of 65.5% - 111.5% with the relative standard deviations (RSDs) between 0.87% and 2.49%. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analysis of carcinogenic aromatic amines in textiles.

  20. Rapid Patient Discharge Contribution to Bed Surge Capacity During a Mass Casualty Incident: Findings From an Exercise With New York City Hospitals.

    Science.gov (United States)

    Jacobs-Wingo, Jasmine L; Cook, Heather A; Lang, William H

    Mass casualty incidents may increase patient volume suddenly and dramatically, requiring hospitals to expeditiously manage bed inventories to release acute care beds for disaster victims. Electronic patient tracking systems combined with unit walk-throughs can identify patients for rapid discharge. The New York City (NYC) Department of Health and Mental Hygiene's 2013 Rapid Patient Discharge Assessment (RPDA) aimed to determine the maximum number of beds NYC hospitals could make available through rapid patient discharge and to characterize discharge barriers. Unit representatives identified discharge candidates within normal operations in round 1 and additional discharge candidates during a disaster scenario in round 2. Descriptive statistics were performed. Fifty-five NYC hospitals participated in the RPDA exercise; 45 provided discharge candidate counts in both rounds. Representatives identified 4225 patients through the RPDA: among these, 1138 (26.9%) were already confirmed for discharge; 1854 (43.9%) were round 1 discharge candidates; and 1233 (29.2%) were round 2 discharge candidates. These 4225 patients represented 21.4% of total bed capacity. Frequently reported barriers included missing prescriptions for aftercare or discharge orders. The NYC hospitals could implement rapid patient discharge to clear one-fifth of occupied inpatient beds for disaster victims, given they address barriers affecting patients' safe and efficient discharge.

  1. Low-mass vector-meson production at forward rapidity in $p$$+$$p$ collisions at $\\sqrt{s}=200$ GeV

    CERN Document Server

    Adare, A; Ajitanand, N N; Akiba, Y; Akimoto, R; Al-Ta'ani, H; Alexander, J; Alfred, M; Andrews, K R; Angerami, A; Aoki, K; Apadula, N; Appelt, E; Aramaki, Y; Armendariz, R; Asano, H; Aschenauer, E C; Atomssa, E T; Awes, T C; Azmoun, B; Babintsev, V; Bai, M; Bandara, N S; Bannier, B; Barish, K N; Bassalleck, B; Basye, A T; Bathe, S; Baublis, V; Baumann, C; Bazilevsky, A; Beaumier, M; Beckman, S; Belmont, R; Ben-Benjamin, J; Bennett, R; Berdnikov, A; Berdnikov, Y; Black, D; Blau, D S; Bok, J; Bok, J S; Boyle, K; Brooks, M L; Broxmeyer, D; Bryslawskyj, J; Buesching, H; Bumazhnov, V; Bunce, G; Butsyk, S; Campbell, S; Castera, P; Chen, C -H; Chi, C Y; Chiu, M; Choi, I J; Choi, J B; Choudhury, R K; Christiansen, P; Chujo, T; Chvala, O; Cianciolo, V; Citron, Z; Cole, B A; del Valle, Z Conesa; Connors, M; Csanád, M; Csörgő, T; Dairaku, S; Datta, A; Daugherity, M S; David, G; Dayananda, M K; DeBlasio, K; Dehmelt, K; Denisov, A; Deshpande, A; Desmond, E J; Dharmawardane, K V; Dietzsch, O; Ding, L; Dion, A; Do, J H; Donadelli, M; Drapier, O; Drees, A; Drees, K A; Durham, J M; Durum, A; D'Orazio, L; Efremenko, Y V; Engelmore, T; Enokizono, A; En'yo, H; Esumi, S; Fadem, B; Feege, N; Fields, D E; Finger, M; Jr., \\,; Fleuret, F; Fokin, S L; Frantz, J E; Franz, A; Frawley, A D; Fukao, Y; Fusayasu, T; Gal, C; Gallus, P; Garg, P; Garishvili, I; Ge, H; Giordano, F; Glenn, A; Gong, X; Gonin, M; Goto, Y; de Cassagnac, R Granier; Grau, N; Greene, S V; Perdekamp, M Grosse; Gu, Y; Gunji, T; Guo, L; Guragain, H; Gustafsson, H -Å; Hachiya, T; Haggerty, J S; Hahn, K I; Hamagaki, H; Hamblen, J; Han, R; Han, S Y; Hanks, J; Harper, C; Hasegawa, S; Hashimoto, K; Haslum, E; Hayano, R; He, X; Hemmick, T K; Hester, T; Hill, J C; Hollis, R S; Holzmann, W; Homma, K; Hong, B; Horaguchi, T; Hori, Y; Hornback, D; Hoshino, T; Huang, S; Ichihara, T; Ichimiya, R; Iinuma, H; Ikeda, Y; Imai, K; Imazu, Y; Inaba, M; Iordanova, A; Isenhower, D; Ishihara, M; Issah, M; Ivanischev, D; Ivanishchev, D; Iwanaga, Y; Jacak, B V; Jeon, S J; Jezghani, M; Jia, J; Jiang, X; John, D; Johnson, B M; Jones, T; Joo, E; Joo, K S; Jouan, D; Jumper, D S; Kamin, J; Kaneti, S; Kang, B H; Kang, J H; Kang, J S; Kapustinsky, J; Karatsu, K; Kasai, M; Kawall, D; Kazantsev, A V; Kempel, T; Key, J A; Khachatryan, V; Khanzadeev, A; Kihara, K; Kijima, K M; Kim, B I; Kim, C; Kim, D H; Kim, D J; Kim, E -J; Kim, H -J; Kim, M; Kim, Y -J; Kim, Y K; Kinney, E; Kiss, Á; Kistenev, E; Klatsky, J; Kleinjan, D; Kline, P; Koblesky, T; Kochenda, L; Kofarago, M; Komkov, B; Konno, M; Koster, J; Kotov, D; Král, A; Kunde, G J; Kurita, K; Kurosawa, M; Kwon, Y; Kyle, G S; Lacey, R; Lai, Y S; Lajoie, J G; Lebedev, A; Lee, D M; Lee, J; Lee, K B; Lee, K S; Lee, S H; Lee, S R; Leitch, M J; Leite, M A L; Leitgab, M; Li, X; Lim, S H; Levy, L A Linden; Liu, H; Liu, M X; Love, B; Lynch, D; Maguire, C F; Makdisi, Y I; Makek, M; Manion, A; Manko, V I; Mannel, E; Mao, Y; Masui, H; McCumber, M; McGaughey, P L; McGlinchey, D; McKinney, C; Means, N; Meles, A; Mendoza, M; Meredith, B; Miake, Y; Mibe, T; Mignerey, A C; Miki, K; Miller, A J; Milov, A; Mishra, D K; Mitchell, J T; Miyachi, Y; Miyasaka, S; Mizuno, S; Mohanty, A K; Montuenga, P; Moon, H J; Moon, T; Morino, Y; Morreale, A; Morrison, D P; Motschwiller, S; Moukhanova, T V; Murakami, T; Murata, J; Mwai, A; Nagamiya, S; Nagle, J L; Naglis, M; Nagy, M I; Nakagawa, I; Nakagomi, H; Nakamiya, Y; Nakamura, K R; Nakamura, T; Nakano, K; Nattrass, C; Netrakanti, P K; Newby, J; Nguyen, M; Nihashi, M; Niida, T; Nouicer, R; Novitzky, N; Nyanin, A S; Oakley, C; O'Brien, E; Ogilvie, C A; Oka, M; Okada, K; Koop, J D Orjuela; Oskarsson, A; Ouchida, M; Ozaki, H; Ozawa, K; Pak, R; Pantuev, V; Papavassiliou, V; Park, B H; Park, I H; Park, S; Park, S K; Pate, S F; Patel, L; Patel, M; Pei, H; Peng, J -C; Pereira, H; Perepelitsa, D V; Perera, G D N; Peressounko, D Yu; Perry, J; Petti, R; Pinkenburg, C; Pinson, R; Pisani, R P; Proissl, M; Purschke, M L; Qu, H; Rak, J; Ravinovich, I; Read, K F; Reygers, K; Reynolds, D; Riabov, V; Riabov, Y; Richardson, E; Riveli, N; Roach, D; Roche, G; Rolnick, S D; Rosati, M; Rosendahl, S S E; Rowan, Z; Rubin, J G; Sahlmueller, B; Saito, N; Sakaguchi, T; Sako, H; Samsonov, V; Sano, S; Sarsour, M; Sato, S; Sato, T; Savastio, M; Sawada, S; Schaefer, B; Schmoll, B K; Sedgwick, K; Seele, J; Seidl, R; Sen, A; Seto, R; Sett, P; Sexton, A; Sharma, D; Shein, I; Shibata, T -A; Shigaki, K; Shim, H H; Shimomura, M; Shoji, K; Shukla, P; Sickles, A; Silva, C L; Silvermyr, D; Silvestre, C; Sim, K S; Singh, B K; Singh, C P; Singh, V; Slunečka, M; Sodre, T; Soltz, R A; Sondheim, W E; Sorensen, S P; Sourikova, I V; Stankus, P W; Stenlund, E; Stepanov, M; Stoll, S P; Sugitate, T; Sukhanov, A; Sumita, T; Sun, J; Sziklai, J; Takagui, E M; Takahara, A; Taketani, A; Tanabe, R; Tanaka, Y; Taneja, S; Tanida, K; Tannenbaum, M J; Tarafdar, S; Taranenko, A; Tennant, E; Themann, H; Thomas, D; Tieulent, R; Timilsina, A; Todoroki, T; Togawa, M; Tomášek, L; Tomášek, M; Torii, H; Towell, M; Towell, R; Towell, R S; Tserruya, I; Tsuchimoto, Y; Utsunomiya, K; Vale, C; van Hecke, H W; Vargyas, M; Vazquez-Zambrano, E; Veicht, A; Velkovska, J; Vértesi, R; Virius, M; Vossen, A; Vrba, V; Vznuzdaev, E; Wang, X R; Watanabe, D; Watanabe, K; Watanabe, Y; Watanabe, Y S; Wei, F; Wei, R; Wessels, J; Whitaker, S; White, S N; Winter, D; Wolin, S; Woody, C L; Wright, R M; Wysocki, M; Xia, B; Xue, L; Yalcin, S; Yamaguchi, Y L; Yang, R; Yanovich, A; Ying, J; Yokkaichi, S; Yoo, J S; Yoon, I; You, Z; Young, G R; Younus, I; Yushmanov, I E; Zajc, W A; Zelenski, A; Zhou, S

    2014-01-01

    The PHENIX experiment at the Relativistic Heavy Ion Collider has measured low mass vector meson, $\\omega$, $\\rho$, and $\\phi$, production through the dimuon decay channel at forward rapidity ($1.2<|y|<2.2$) in $p$$+$$p$ collisions at $\\sqrt{s}=200$ GeV. The differential cross sections for these mesons are measured as a function of both $p_T$ and rapidity. We also report the integrated differential cross sections over $1

  2. Rapid characterization of dry cured ham produced following different PDOs by proton transfer reaction time of flight mass spectrometry (PTR-ToF-MS).

    Science.gov (United States)

    Del Pulgar, José Sánchez; Soukoulis, Christos; Biasioli, Franco; Cappellin, Luca; García, Carmen; Gasperi, Flavia; Granitto, Pablo; Märk, Tilmann D; Piasentier, Edi; Schuhfried, Erna

    2011-07-15

    In the present study, the recently developed proton transfer reaction time of flight mass spectrometry (PTR-ToF-MS) technique was used for the rapid characterization of dry cured hams produced according to 4 of the most important Protected Designations of Origin (PDOs): an Iberian one (Dehesa de Extremadura) and three Italian ones (Prosciutto di San Daniele, Prosciutto di Parma and Prosciutto Toscano). In total, the headspace composition and respective concentration for nine Spanish and 37 Italian dry cured ham samples were analyzed by direct injection without any pre-treatment or pre-concentration. Firstly, we show that the rapid PTR-ToF-MS fingerprinting in conjunction with chemometrics (Principal Components Analysis) indicates a good separation of the dry cured ham samples according to their production process and that it is possible to set up, using data mining methods, classification models with a high success rate in cross validation. Secondly, we exploited the higher mass resolution of the new PTR-ToF-MS, as compared with standard quadrupole based versions, for the identification of the exact sum formula of the mass spectrometric peaks providing analytical information on the observed differences. The work indicates that PTR-ToF-MS can be used as a rapid method for the identification of differences among dry cured hams produced following the indications of different PDOs and that it provides information on some of the major volatile compounds and their link with the implemented manufacturing practices such as rearing system, salting and curing process, manufacturing practices that seem to strongly affect the final volatile organic profile and thus the perceived quality of dry cured ham. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Rapid metabolic profiling of Nicotiana tabacum defence responses against Phytophthora nicotianae using direct infrared laser desorption ionization mass spectrometry and principal component analysis.

    Science.gov (United States)

    Ibáñez, Alfredo J; Scharte, Judith; Bones, Philipp; Pirkl, Alexander; Meldau, Stefan; Baldwin, Ian T; Hillenkamp, Franz; Weis, Engelbert; Dreisewerd, Klaus

    2010-06-09

    Successful defence of tobacco plants against attack from the oomycete Phytophthora nicotianae includes a type of local programmed cell death called the hypersensitive response. Complex and not completely understood signaling processes are required to mediate the development of this defence in the infected tissue. Here, we demonstrate that different families of metabolites can be monitored in small pieces of infected, mechanically-stressed, and healthy tobacco leaves using direct infrared laser desorption ionization orthogonal time-of-flight mass spectrometry. The defence response was monitored for 1 - 9 hours post infection. Infrared laser desorption ionization orthogonal time-of-flight mass spectrometry allows rapid and simultaneous detection in both negative and positive ion mode of a wide range of naturally occurring primary and secondary metabolites. An unsupervised principal component analysis was employed to identify correlations between changes in metabolite expression (obtained at different times and sample treatment conditions) and the overall defence response.A one-dimensional projection of the principal components 1 and 2 obtained from positive ion mode spectra was used to generate a Biological Response Index (BRI). The BRI obtained for each sample treatment was compared with the number of dead cells found in the respective tissue. The high correlation between these two values suggested that the BRI provides a rapid assessment of the plant response against the pathogen infection. Evaluation of the loading plots of the principal components (1 and 2) reveals a correlation among three metabolic cascades and the defence response generated in infected leaves. Analysis of selected phytohormones by liquid chromatography electrospray ionization mass spectrometry verified our findings. The described methodology allows for rapid assessment of infection-specific changes in the plant metabolism, in particular of phenolics, alkaloids, oxylipins, and carbohydrates

  4. Rapid metabolic profiling of Nicotiana tabacum defence responses against Phytophthora nicotianae using direct infrared laser desorption ionization mass spectrometry and principal component analysis

    Directory of Open Access Journals (Sweden)

    Weis Engelbert

    2010-06-01

    Full Text Available Abstract Background Successful defence of tobacco plants against attack from the oomycete Phytophthora nicotianae includes a type of local programmed cell death called the hypersensitive response. Complex and not completely understood signaling processes are required to mediate the development of this defence in the infected tissue. Here, we demonstrate that different families of metabolites can be monitored in small pieces of infected, mechanically-stressed, and healthy tobacco leaves using direct infrared laser desorption ionization orthogonal time-of-flight mass spectrometry. The defence response was monitored for 1 - 9 hours post infection. Results Infrared laser desorption ionization orthogonal time-of-flight mass spectrometry allows rapid and simultaneous detection in both negative and positive ion mode of a wide range of naturally occurring primary and secondary metabolites. An unsupervised principal component analysis was employed to identify correlations between changes in metabolite expression (obtained at different times and sample treatment conditions and the overall defence response. A one-dimensional projection of the principal components 1 and 2 obtained from positive ion mode spectra was used to generate a Biological Response Index (BRI. The BRI obtained for each sample treatment was compared with the number of dead cells found in the respective tissue. The high correlation between these two values suggested that the BRI provides a rapid assessment of the plant response against the pathogen infection. Evaluation of the loading plots of the principal components (1 and 2 reveals a correlation among three metabolic cascades and the defence response generated in infected leaves. Analysis of selected phytohormones by liquid chromatography electrospray ionization mass spectrometry verified our findings. Conclusion The described methodology allows for rapid assessment of infection-specific changes in the plant metabolism, in particular

  5. Accretion turnoff and rapid evaporation of very light secondaries in low-mass X-ray binaries

    Energy Technology Data Exchange (ETDEWEB)

    Ruderman, M.; Shaham, J.; Tavani, M.

    1989-01-01

    The illumination of companion stars in very low mass X-ray binaries by various kinds of radiation from the neighborhood of the neutron star after accretion has terminated or during accretion is considered. If a neutron star's spun-up period approaches 0.001 s, pulsar kHz radiation can quench accretion by pushing surrounding plasma away from the neutron star, and may leave the companion to be evaporated by the high-energy radiation component expected from an isolated millisecond radiopulsar. Expected accretion-powered MeV gamma-rays and e(+ or -) winds may also be effective in evaporating dwarf companions. Neutron star spin-down energy release may sustain the power in these radiation mechanisms even while accretion falls. Accretion-powered soft X-rays may speed the mass loss of highly evolved dwarf companions, particularly those with a large fraction of carbon and oxygen. 30 references.

  6. Rapid Species-level Identification of Salvias by Chemometric Processing of Ambient Ionisation Mass Spectrometry-derived Chemical Profiles.

    Science.gov (United States)

    Giffen, Justine E; Lesiak, Ashton D; Dane, A John; Cody, Robert B; Musah, Rabi A

    2017-01-01

    The Salvia genus contains numerous economically important plants that have horticultural, culinary and nutraceutical uses. They are often similar in appearance, making species determination difficult. Species identification of dried Salvia products is also challenging since distinguishing plant morphological features are no longer present. The development of a simple high-throughput method of analysis of fresh and dried Salvia leaves that would permit rapid species-level identification and detection of diagnostic biomarkers. Plant leaves were analysed in their native form by DART-MS without the need for any sample preparation steps. This furnished chemical fingerprints characteristic of each species. In the same experiment, in-source collision-induced dissociation was used to identify biomarkers. Biomarker presence was also independently confirmed by GC-MS. Chemometric processing of DART-MS profiles was performed by kernel discriminant analysis (KDA) and soft independent modelling of class analogy (SIMCA) to classify the fingerprints according to species. The approach was successful despite the occurrence of diurnal cycle and plant-age related chemical profile variations within species. In a single rapid experiment, the presence of essential oil biomarkers such as 3-carene, α-pinene, β-pinene, β-thujone, β-caryophyllene, camphor and borneol could be confirmed. The method was applied to rapid identification and differentiation of Salvia apiana, S. dominica, S. elegans, S. officinalis, S. farinacea and S. patens. Species-level identification of Salvia plant material could be accomplished by chemometric processing of DART-HRMS-derived chemical profiles of both fresh and dried Salvia material. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  7. [Utility of rapid on-site cytology in endoscopic ultrasonography-guided fine needle aspiration of pancreatic masses].

    Science.gov (United States)

    Furuhata, Ayako; Shirahase, Hiroyuki; Shirai, Takao; Hirata, Masahiro; Yoshizawa, Akihiko; Haga, Hironori; Nakaizumi, Akihiko

    2012-05-01

    Endoscopic ultrasonography-guided fine needle aspiration (EUS-FNA) is a safe and effective method for obtaining samples for cytological diagnosis. Pancreatic cancer is extremely serious and often extremely aggressive, so early detection and diagnosis is important. Therefore, we actively perform EUS FNA for pathological diagnosis of cancer of digestive organs, especially the pancreas. EUS-FNA was performed in 67 patients (39 male, 28 female, median age 63.3 years) from January 2007 to December 2010 in Kyoto University Hospital. To eliminate both quantitatively and qualitatively inadequate samples, we performed EUS-FNA with rapid on-site cytology. Two squash preparations of the collected cells from biopsy were retrieved. One was stained on-site with Giemsa for rapid cytology to evaluate the quantity and quality of the cell collection. If necessary, second or third trials were carried out to obtain appropriate samples for final cytology diagnosis. The other was wet-fixed and used for Papanicolaou staining. All 11 cases of inflammatory disease were diagnosed as negative on cytology. Solid-pseudopapillary neoplasm (1 case) and Endocrine neoplasms (3 cases) were correctly diagnosed on cytology. In pancreatic cancer, 49 of 52 cases (94%) were diagnosed as positive, but 3 cases (6%) were false-negative on cytology. The number of centesis for sampling was once in 21 cases, twice in 26 cases and more than twice in 20 cases. In this study of EUS-FNA, sensitivity was 94% and specificity was 100%. Results of our examination suggest that the combination of EUS-FNA and rapid on-site cytology is a highly specific and sensitive test for detection of pancreatic cancer, and may contribute to reduce excessive centesis.

  8. Direct identification of bacteria in positive blood cultures: comparison of two rapid methods, FilmArray and mass spectrometry.

    Science.gov (United States)

    Rand, Kenneth H; Delano, John P

    2014-07-01

    We evaluated the accuracy and performance of the FilmArray Direct from Positive Blood Culture system (BCID) (BioFire Diagnostics, Salt Lake City, UT, USA) and the VITEK Mass Spectrometry System (Vitek MS; bioMerieux, Durham, NC, USA) to identify bacterial isolates from 161 positive blood culture bottles. The BCID uses multiplex PCR to identify 90-95% of common isolates to the genus or species/complex level as well as mecA, Van A/B, and bla(KPC) genes in approximately 1 hour. Of 151 monomicrobic isolates, the FilmArray correctly identified 48/49 (98%) to the genus and 84/84 (100%) to the species/complex level, while 18/151 (12%) gave no identification, as expected from the database. Mass spectrometry correctly identified 142/151 (94%) monomicrobic cultures to the genus level, 137/151 (91%) to the species level, with only 8/151(5%) giving no identification. Although mass spectrometry has a much larger database, the filtration system was cumbersome in contrast to the 3-5 minutes hands-on-time for the BCID. Copyright © 2014 Elsevier Inc. All rights reserved.

  9. Rapid MALDI-TOF Mass Spectrometry Strain Typing during a Large Outbreak of Shiga-Toxigenic Escherichia coli

    Science.gov (United States)

    Christner, Martin; Trusch, Maria; Rohde, Holger; Kwiatkowski, Marcel; Schlüter, Hartmut; Wolters, Manuel; Aepfelbacher, Martin; Hentschke, Moritz

    2014-01-01

    Background In 2011 northern Germany experienced a large outbreak of Shiga-Toxigenic Escherichia coli O104:H4. The large amount of samples sent to microbiology laboratories for epidemiological assessment highlighted the importance of fast and inexpensive typing procedures. We have therefore evaluated the applicability of a MALDI-TOF mass spectrometry based strategy for outbreak strain identification. Methods Specific peaks in the outbreak strain’s spectrum were identified by comparative analysis of archived pre-outbreak spectra that had been acquired for routine species-level identification. Proteins underlying these discriminatory peaks were identified by liquid chromatography tandem mass spectrometry and validated against publicly available databases. The resulting typing scheme was evaluated against PCR genotyping with 294 E. coli isolates from clinical samples collected during the outbreak. Results Comparative spectrum analysis revealed two characteristic peaks at m/z 6711 and m/z 10883. The underlying proteins were found to be of low prevalence among genome sequenced E. coli strains. Marker peak detection correctly classified 292 of 293 study isolates, including all 104 outbreak isolates. Conclusions MALDI-TOF mass spectrometry allowed for reliable outbreak strain identification during a large outbreak of Shiga-Toxigenic E. coli. The applied typing strategy could probably be adapted to other typing tasks and might facilitate epidemiological surveys as part of the routine pathogen identification workflow. PMID:25003758

  10. A rapid screening method to monitor expression of various recombinant proteins from prokaryotic and eukaryotic expression systems using MALDI-TOF mass spectrometry

    DEFF Research Database (Denmark)

    Jebanathirajah, J.A.; Andersen, S.; Blagoev, B.

    2002-01-01

    Rapid methods using matrix-assisted laser desorption ionization-time-of-flight mass spectrometry to monitor recombinant protein expression from various prokaryotic and eukaryotic cell culture systems were devised. Intracellular as well as secreted proteins from both induced and constitutive...... expression systems were measured and monitored from whole cells and growth media, thus providing an alternative to time-consuming traditional methods for screening and monitoring of protein expression. The methods described here involve minimal processing of samples and are therefore relevant to high...

  11. Isocratic Solid Phase Extraction-Liquid Chromatography (SPE-LC) Interfaced to High-Performance Tandem Mass Spectrometry for Rapid Protein Identification

    DEFF Research Database (Denmark)

    Hørning, Ole B; Kjeldsen, Frank; Theodorsen, Søren

    2008-01-01

    Reversed-phase liquid chromatography interfaced to electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) allows analysis of very complex peptide mixtures at great sensitivity, but it can be very time-consuming, typically using 60 min, or more, per sample analysis. We recently introduced...... the isocratic solid phase extraction-liquid chromatography (SPE-LC) technology for rapid separation ( approximately 8 min) of simple peptide samples. We now extend these studies to demonstrate the potential of SPE-LC separation in combination with a hybrid linear ion trap-Orbitrap tandem mass spectrometer...... for efficient analysis of peptide samples in proteomics research. The system performance of SPE-LC-MS/MS was evaluated in terms of sensitivity and efficiency for the analysis of tryptic peptide digests obtained from samples consisting of up to 12 standard proteins. The practical utility of the analytical setup...

  12. Rapid Discrimination of Closely Related Seed Herbs (Cumin, Caraway, and Fennel) by Direct Analysis in Real Time Mass Spectrometry (DART-MS).

    Science.gov (United States)

    Antal, Borbála; Kuki, Ákos; Nagy, Lajos; Nagy, Tibor; Zsuga, Miklós; M-Hamvas, Márta; Vasas, Gábor; Kéki, Sándor

    2016-01-01

    Direct analysis in real time mass spectrometry (DART-MS) was applied as a rapid method for the discrimination of the spices and traditional medicines cumin (Cuminum cyminum L.), caraway (Carum carvi L.), and fennel (Foeniculum vulgare Mill.). The seeds of these plants were analyzed without sample preparation by DART ion source coupled with quadrupole time-of-flight (QTOF) tandem mass spectrometry. The relatively clean DART spectra showed characteristic patterns, fingerprints, for each herb. It was found that a marker compound can be assigned to each species that can identify unambiguously these plants. Principal component analysis has also been used to analyze the DART-MS data of these seed herbs. Crispanone, carvone, and fenchone are the dominant compounds in the positive DART spectra of cumin, caraway, and fennel, respectively. Crispanone was first time identified as a constituent of cumin. Furthermore, the collision-induced dissociation (CID) behavior of the [M+NH4](+) ion of crispanone was also described.

  13. Early Paleocene landbird supports rapid phylogenetic and morphological diversification of crown birds after the K-Pg mass extinction

    Science.gov (United States)

    Ksepka, Daniel T.; Stidham, Thomas A.; Williamson, Thomas E.

    2017-07-01

    Evidence is accumulating for a rapid diversification of birds following the K-Pg extinction. Recent molecular divergence dating studies suggest that birds radiated explosively during the first few million years of the Paleocene; however, fossils from this interval remain poorly represented, hindering our understanding of morphological and ecological specialization in early neoavian birds. Here we report a small fossil bird from the Nacimiento Formation of New Mexico, constrained to 62.221-62.517 Ma. This partial skeleton represents the oldest arboreal crown group bird known. Phylogenetic analyses recovered Tsidiiyazhi abini gen. et sp. nov. as a member of the Sandcoleidae, an extinct basal clade of stem mousebirds (Coliiformes). The discovery of Tsidiiyazhi pushes the minimum divergence ages of as many as nine additional major neoavian lineages into the earliest Paleocene, compressing the duration of the proposed explosive post-K-Pg radiation of modern birds into a very narrow temporal window parallel to that suggested for placental mammals. Simultaneously, Tsidiiyazhi provides evidence for the rapid morphological (and likely ecological) diversification of crown birds. Features of the foot indicate semizygodactyly (the ability to facultatively reverse the fourth pedal digit), and the arcuate arrangement of the pedal trochleae bears a striking resemblance to the conformation in owls (Strigiformes). Inclusion of fossil taxa and branch length estimates impacts ancestral state reconstructions, revealing support for the independent evolution of semizygodactyly in Coliiformes, Leptosomiformes, and Strigiformes, none of which is closely related to extant clades exhibiting full zygodactyly.

  14. Solid-phase microextraction low temperature plasma mass spectrometry for the direct and rapid analysis of chemical warfare simulants in complex mixtures.

    Science.gov (United States)

    Dumlao, Morphy C; Jeffress, Laura E; Gooding, J Justin; Donald, William A

    2016-06-21

    Solid-phase microextraction (SPME) is directly integrated with low temperature plasma ionisation mass spectrometry to rapidly detect organophosphate chemical warfare agent simulants and their hydrolysis products in chemical mixtures, including urine. In this sampling and ionization method, the fibre serves: (i) to extract molecules from their native environment, and (ii) as the ionization electrode that is used to desorb and ionize molecules directly from the SPME surface. By use of a custom fabricated SPME fibre consisting of a stainless steel needle coated with a Linde Type A (LTA) zeolitic microporous material and low temperature plasma mass spectrometry, protonated dimethyl methylphosphonate (DMMP), diethyl ethylphosphonate (DEEP) and pinacolyl methylphosphonic acid (PinMPA) can be detected at less than 100 ppb directly in water and urine. Organophosphates were not readily detected by this approach using an uncoated needle in negative control experiments. The use of the LTA coating significantly outperformed the use of a high alumina Zeolite Socony Mobil-5 (ZSM-5) coating of comparable thickness that is significantly less polar than LTA. By conditioning the LTA probe by immersion in an aqueous CuSO4 solution, the ion abundance for protonated DMMP increased by more than 300% compared to that obtained without any conditioning. Sample recovery values were between 96 and 100% for each analyte. The detection of chemical warfare agent analogues and hydrolysis products required less than 2 min per sample. A key advantage of this sampling and ionization method is that analyte ions can be directly and rapidly sampled from chemical mixtures, such as urine and seawater, without sample preparation or chromatography for sensitive detection by mass spectrometry. This ion source should prove beneficial for portable mass spectrometry applications because relatively low detection limits can be obtained without the use of compressed gases, fluid pumps, and lasers. Moreover, the

  15. Rapid Screening and Identification of Daidzein Metabolites in Rats Based on UHPLC-LTQ-Orbitrap Mass Spectrometry Coupled with Data-Mining Technologies

    Directory of Open Access Journals (Sweden)

    Wenjing Zhao

    2018-01-01

    Full Text Available Daidzein, the main bioactive soy isoflavone in Nature, has been found to possess many biological functions. It has been investigated in particular as a phytoestrogen owing to the similarity of its structure with that of the human hormone estrogen. Due to the lack of comprehensive studies on daidzein metabolism, further research is still required to clarify its in vivo metabolic fate and intermediate processes. In this study, an efficient strategy was established using UHPLC-LTQ-Orbitrap mass spectrometry to profile the metabolism of daidzein in rats. Meanwhile, multiple data-mining methods including high-resolution extracted ion chromatogram (HREIC, multiple mass defect filtering (MMDF, neutral loss fragment (NLF, and diagnostic product ion (DPI were utilized to investigate daidzein metabolites from the HR-ESI-MS1 to ESI-MSn stage in both positive and negative ion modes. Consequently, 59 metabolites, including prototype compounds, were positively or tentatively elucidated based on reference standards, accurate mass measurements, mass fragmentation behaviors, chromatographic retention times, and corresponding calculated ClogP values. As a result, dehydration, hydrogenation, methylation, dimethylation, glucuronidation, glucosylation, sulfonation, ring-cleavage, and their composite reactions were ascertained to interpret its in vivo biotransformation. Overall, our results not only revealed the potential pharmacodynamics forms of daidzein, but also aid in establishing a practical strategy for rapid screening and identifying metabolites of natural compounds.

  16. Rapid Screening and Identification of Daidzein Metabolites in Rats Based on UHPLC-LTQ-Orbitrap Mass Spectrometry Coupled with Data-Mining Technologies.

    Science.gov (United States)

    Zhao, Wenjing; Shang, Zhanpeng; Li, Qinqing; Huang, Moran; He, Wenbin; Wang, Zhibin; Zhang, Jiayu

    2018-01-12

    Daidzein, the main bioactive soy isoflavone in Nature, has been found to possess many biological functions. It has been investigated in particular as a phytoestrogen owing to the similarity of its structure with that of the human hormone estrogen. Due to the lack of comprehensive studies on daidzein metabolism, further research is still required to clarify its in vivo metabolic fate and intermediate processes. In this study, an efficient strategy was established using UHPLC-LTQ-Orbitrap mass spectrometry to profile the metabolism of daidzein in rats. Meanwhile, multiple data-mining methods including high-resolution extracted ion chromatogram (HREIC), multiple mass defect filtering (MMDF), neutral loss fragment (NLF), and diagnostic product ion (DPI) were utilized to investigate daidzein metabolites from the HR-ESI-MS¹ to ESI-MSn stage in both positive and negative ion modes. Consequently, 59 metabolites, including prototype compounds, were positively or tentatively elucidated based on reference standards, accurate mass measurements, mass fragmentation behaviors, chromatographic retention times, and corresponding calculated ClogP values. As a result, dehydration, hydrogenation, methylation, dimethylation, glucuronidation, glucosylation, sulfonation, ring-cleavage, and their composite reactions were ascertained to interpret its in vivo biotransformation. Overall, our results not only revealed the potential pharmacodynamics forms of daidzein, but also aid in establishing a practical strategy for rapid screening and identifying metabolites of natural compounds.

  17. Detection and mapping of Cannabinoids in single hair samples through rapid derivatization- Matrix-Assisted Laser Desorption Ionization Mass Spectrometry

    OpenAIRE

    Beasley, Emma; Francese, Simona; Bassindale, Thomas

    2016-01-01

    The sample preparation method reported in this work has permitted for the first time the application of Matrix Assisted Laser Desorption Ionization Mass Spectrometry Profiling and Imaging (MALDI-MSP and MALDI-MSI) for the detection and mapping of cannabinoids in a single hair sample. MALDI-MSI analysis of hair samples has recently been suggested as an alternative technique to traditional methods of GC-MS and LC-MS due to simpler sample preparation, the ability to detect a narrower time frame ...

  18. Surprising Rapid Collapse of Sirius B from Red Giant to White Dwarf Through Mass Transfer to Sirius a

    Science.gov (United States)

    Yousef, Shahinaz; Ali, Ola

    2013-03-01

    Sirius was observed in antiquity as a red star. In his famous astronomy textbook the Almagest written 140 AD, Ptolemy described the star Sirius as fiery red. He curiously depicted it as one of six red-colored stars. The other five are class M and K stars, such as Arcturus and Betelgeuse. Apparent confirmation in ancient Greek and Roman sources are found and Sirius was also reported red in Europe about 1400 years ago. Sirius must have changed to a white dwarf in the night of Ascension. The star chapter in the Quran started with "by the star as it collapsed (1) your companion have not gone astray nor being misled (2), and in verse 49 which is the rotation period of the companion Sirius B around Sirius A, it is said" He is the Lord of Sirius (49). If Sirius actually was red what could have caused it to change into the brilliant bluish-white star we see today? What the naked eye perceives as a single star is actually a binary star system, consisting of a white main sequence star of spectral type A1V, termed Sirius A, and a faint white dwarf companion of spectral type DA2, termed Sirius B. The red color indicates that the star seen then was a red giant. It looks that what they have seen in antiquity was Sirius B which was then a red giant and it collapsed to form a white dwarf. Since there is no evidence of a planetary nebula, then the red Sirius paradox can be solved in terms of stellar evolution with mass transfer. Sirius B was the most massive star which evolved to a red giant and filled the Roche lobe. Mass transfer to Sirius A occurred through the Lagrangian point. Sirius A then became more massive while Sirius B lost mass and shrank. Sirius B then collapsed abruptly into a white dwarf. In the case of Algol, Ptolmy observed it as white star but it was red at the time of El sufi. At present it is white. The rate of mass transfer from Sirius B to Sirius A, and from Algol B to A is estimated from observational data of colour change from red to bullish white to be 0

  19. Rapid and sensitive liquid chromatography-tandem mass spectrometry method for the quantitation of levodropropizine in human plasma.

    Science.gov (United States)

    Tang, Yunbiao; Zhao, Limei; Wang, Yingwu; Fawcett, J Paul; Gu, Jingkai

    2005-05-05

    A rapid and sensitive LC-MS-MS method for quantifying levodropropizine in human plasma after oral administration of a single-dose (60 mg/day) was developed and validated. The sample preparation used liquid-liquid extraction with a mixture of dichloromethane-diethyl ether (2:3, v/v) in a basic environment. The retention time of levodropropizne and zolmitriptan (used as internal standard) was 1.6 and 1.4 min, respectively. The assay was linear over the range 0.25-500 ng/mL with a LOQ of 0.25 ng/mL. The intra- and inter-day precision were levodropropizine concentration profile in human plasma was determined.

  20. Rapid and sensitive hormonal profiling of complex plant samples by liquid chromatography coupled to electrospray ionization tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Müller Maren

    2011-11-01

    Full Text Available Abstract Background Plant hormones play a pivotal role in several physiological processes during a plant's life cycle, from germination to senescence, and the determination of endogenous concentrations of hormones is essential to elucidate the role of a particular hormone in any physiological process. Availability of a sensitive and rapid method to quantify multiple classes of hormones simultaneously will greatly facilitate the investigation of signaling networks in controlling specific developmental pathways and physiological responses. Due to the presence of hormones at very low concentrations in plant tissues (10-9 M to 10-6 M and their different chemistries, the development of a high-throughput and comprehensive method for the determination of hormones is challenging. Results The present work reports a rapid, specific and sensitive method using ultrahigh-performance liquid chromatography coupled to electrospray ionization tandem spectrometry (UPLC/ESI-MS/MS to analyze quantitatively the major hormones found in plant tissues within six minutes, including auxins, cytokinins, gibberellins, abscisic acid, 1-amino-cyclopropane-1-carboxyic acid (the ethylene precursor, jasmonic acid and salicylic acid. Sample preparation, extraction procedures and UPLC-MS/MS conditions were optimized for the determination of all plant hormones and are summarized in a schematic extraction diagram for the analysis of small amounts of plant material without time-consuming additional steps such as purification, sample drying or re-suspension. Conclusions This new method is applicable to the analysis of dynamic changes in endogenous concentrations of hormones to study plant developmental processes or plant responses to biotic and abiotic stresses in complex tissues. An example is shown in which a hormone profiling is obtained from leaves of plants exposed to salt stress in the aromatic plant, Rosmarinus officinalis.

  1. Equipment and methods for rapid analysis of PWO full size scintillation crystals radiation hardness at mass production

    CERN Document Server

    Annenkov, A N; Drobychev, G Yu; Fedorov, A; Ivankin, P; Korzhik, M V; Lecoq, P; Ligun, V; Lopatik, A; Matveev, L; Missevitch, O V; Zouevski, R F; Peigneux, J P; Sigovski, A

    2000-01-01

    This year an extensive R&D on lead tungstate crystals has entered into the pre-production phase at the Bogoroditsk Techno-Chemical Plant (BTCP). Laboratory small-scale PWO crystal growth technology, which has been tuned and optimised over the last years, is transforming now into an industrial technology of mass production. This mass production technology is based on a set of methods and instrumentation for crystal growth, machining, crystal quality control and certification. According to the specification on lead tungstate pre-production crystals, one of the most important categories of tolerance is the radiation hardness. Control of the PWO radiation hardness at the pre-production phase requires reliability and an easy to use measuring tool with a high productivity. A semi- automatic spectrometric setup for PWO radiation hardness monitoring has been developed and tested at the X5 CERN irradiation facility. After final crosschecks the setup was set into operation at the BTCP. Together with several other m...

  2. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  3. Rapid disaster victim identification in mass fatality incidents: decision-support tool to facilitate human remains identification.

    Science.gov (United States)

    de Cosmo, Sergio; Barbera, Joseph A

    2012-10-01

    A quantitative decision-support tool (DST), using a combination of selected human physical attributes as identification elements, was developed to facilitate body identification in mass fatality incidents, particularly in settings with limited availability of technological resources and forensic expertise. To construct the DST, the external biological attributes of interest were first selected. A process was then developed to guide collection of the selected categories of attributes and record them into objective antemortem (AM) and postmortem (PM) records. Finally, a framework for assessing the similarity between confronting PM-AM attribute records was established. The DST evaluates the similarities between each set of like attributes in the AM and PM records being compared. It then computes an overall similarity score for each evaluated AM record that was compared to a selected PM record. The AM record with the highest score represents the highest probable match, with the PM file selected for the comparison. Multiple simulations across a range of mass fatality situations demonstrated the effectiveness of the DST in the experimental setting. The developed DST may provide authorities with a method for expediting body identification without completely eliminating any missing person file from consideration. Under specific circumstances, this method may reduce the need for technologically sophisticated forensic identification techniques (eg, dental records, fingerprints, and DNA). At a minimum, it should facilitate the efficiency of the current technological matching process.

  4. Applying characteristic fragment filtering for rapid detection and identification of ingredients in rhubarb by HPLC coupled with linear ion trap-Orbitrap mass spectrometry.

    Science.gov (United States)

    Wang, Qing; Lu, Zhiwei; Zhang, Li; Zhang, Qingqing; Wang, Meiling; Zhao, Huizhen; Liu, Yuehong; Fu, Shuang; Huang, Zhenghai; Xie, Ziye; Yu, Honghong; Zhang, Zhixin; Gao, Xiaoyan

    2017-07-01

    Chemical characteristic fragment filtering in MSn chromatograms was proposed to detect and identify the components in rhubarb rapidly using high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry. Characteristic fragments consist of diagnostic ions and neutral loss fragments. Characteristic fragment filtering is a postacquisition data mining method for the targeted screening of groups with specific structures, including three steps: first, in order to comprehensively summarize characteristic fragments for global identification of the ingredients in rhubarb, representative authentic standards of dominant chemical categories contained in rhubarb were chosen, from which fragmentation rules and a characteristic fragments schedule were proposed; second, characteristic fragment filtering was used to rapidly recognize analogous skeletons; finally, combined with retention time, accurate mass, characteristic fragments, and previous literature, the structures of the filtered compounds were identified or tentatively characterized. As a result, a total of 271 compounds were detected and identified in rhubarb, including 34 anthraquinones, 83 anthrones, 46 tannins, 17 stilbenes, 24 phenylbutanones, 26 acylglucosides, 26 chromones, and 15 other compounds, 69 of which are potentially new compounds. The proposed characteristic fragment filtering strategy would be a reference for the large-scale detection and identification of the ingredients of herbal medicines. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Diagnosis of congenital adrenal hyperplasia by rapid determination of 17alpha-hydroxyprogesterone in dried blood spots by gas chromatography/mass spectrometry following microwave-assisted silylation.

    Science.gov (United States)

    Deng, Chunhui; Ji, Jie; Zhang, Lijuan; Zhang, Xiangmin

    2005-01-01

    17alpha-Hydroxyprogesterone (17OHP) is considered to be the biomarker of congential adrenal hyperplasia (CAH). Screening for CAH in newborns by measuring levels of the biomarker of 17OHP has become routine. In the work, a rapid, simple and sensitive technique was developed for the diagnosis of neonatal CAH by the quantitative analysis of 17OHP in neonatal blood spots. The technique was based on microwave-assisted silylation (MAS) followed by gas chromatography/mass spectrometry (GC/MS). In the method, fast derivatization of 17OHP with N,O-bis(trimethylsilyl)trifluoroacetamide was performed by using microwave irradiation, and the trimethylsilyl derivative thus formed was analyzed by GC/MS. The results of the experiment indicate that MAS followed by GC/MS analysis is a rapid, simple and sensitive method for the determination of 17OHP in blood samples. The proposed technique has been shown to have potential as a powerful tool for the rapid diagnosis of neonatal CAH. (c) 2005 John Wiley & Sons, Ltd.

  6. Simultaneous detection of perchlorate and bromate using rapid high-performance ion exchange chromatography-tandem mass spectrometry and perchlorate removal in drinking water.

    Science.gov (United States)

    West, Danielle M; Mu, Ruipu; Gamagedara, Sanjeewa; Ma, Yinfa; Adams, Craig; Eichholz, Todd; Burken, Joel G; Shi, Honglan

    2015-06-01

    Perchlorate and bromate occurrence in drinking water causes health concerns due to their effects on thyroid function and carcinogenicity, respectively. The purpose of this study was threefold: (1) to advance a sensitive method for simultaneous rapid detection of perchlorate and bromate in drinking water system, (2) to systematically study the occurrence of these two contaminants in Missouri drinking water treatment systems, and (3) to examine effective sorbents for minimizing perchlorate in drinking water. A rapid high-performance ion exchange chromatography-tandem mass spectrometry (HPIC-MS/MS) method was advanced for simultaneous detection of perchlorate and bromate in drinking water. The HPIC-MS/MS method was rapid, required no preconcentration of the water samples, and had detection limits for perchlorate and bromate of 0.04 and 0.01 μg/L, respectively. The method was applied to determine perchlorate and bromate concentrations in total of 23 selected Missouri drinking water treatment systems during differing seasons. The water systems selected include different source waters: groundwater, lake water, river water, and groundwater influenced by surface water. The concentrations of perchlorate and bromate were lower than or near to method detection limits in most of the drinking water samples monitored. The removal of perchlorate by various adsorbents was studied. A cationic organoclay (TC-99) exhibited effective removal of perchlorate from drinking water matrices.

  7. Rapid detection of GM1 ganglioside in cerebrospinal fluid in dogs with GM1 gangliosidosis using matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Satoh, Hiroyuki; Yamauchi, Toyofumi; Yamasaki, Masahiro; Maede, Yoshimitsu; Yabuki, Akira; Chang, Hye-Sook; Asanuma, Taketoshi; Yamato, Osamu

    2011-11-01

    The concentration of GM1 (monosialotetrahexosyl ganglioside) in cerebrospinal fluid (CSF) is markedly increased in dogs with GM1 gangliosidosis due to GM1 accumulation in the central nervous system and leakage to the CSF. The present study established a rapid and simple method for detection of accumulated GM1 in the CSF in dogs with GM1 gangliosidosis using matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI TOF MS) and discusses the usefulness of this method for the rapid diagnosis and/or high-risk screening of this disease in domestic animals. Cerebrospinal fluid was collected from normal dogs and 4- to 11-month-old Shiba dogs with GM1 gangliosidosis. The MALDI TOF MS analysis was carried out in combination with a special sample plate and a simple desalting step on the plate. Specific signs of GM1 could be detected in the standard GM1 solutions at concentrations of 50 nmol/l or more. The signs were also clearly detected in CSF (131-618 nmol/l) in affected dogs, but not in normal canine CSF (12 ± 5 nmol/l, mean ± standard deviation). The results demonstrated that MALDI TOF MS can detect GM1 accumulated in canine CSF even in the early stage of the disease. In conclusion, the rapid detection of increased CSF GM1 using MALDI TOF MS is a useful method for diagnosis and/or screening for canine GM1 gangliosidosis.

  8. Rapid and simultaneous in situ assessment of aflatoxins and stilbenes using silica plate imprinting mass spectrometry imaging.

    Directory of Open Access Journals (Sweden)

    Diogo N de Oliveira

    Full Text Available A fast and direct combination of techniques for simultaneous mycotoxin and phytoalexin identification in peanut skin and kernel is described. Silica Plate Imprinting Laser Desorption/Ionization Mass Spectrometry Imaging (SPILDI-MSI is a powerful technique that exhibits great advantages, such as solvent-free and matrix-free characteristics, as well as no sample preparation or separation steps. It also permits accurate identification of mycotoxins and phytoalexins with unique fingerprint profiles in just a few seconds. Results are expressed as chemical images of the 4 identified types of aflatoxins (B1, B2, G1 and G2 and a stilbenoid (resveratrol. Also, SPILDI-MSI allows the comparison between the spatial distribution of aflatoxins and resveratrol found in kernel and skin. This novel application has proven to be useful for instantaneous qualitative assessment of aflatoxins and stilbenoids both in the peanut skin and kernel and offers precise tracking of fungal contamination in nuts and other foodstuffs.

  9. A novel method to rapidly distinguish the geographical origin of traditional fermented-salted vegetables by mass fingerprinting

    Science.gov (United States)

    Yoon, So-Ra; Kim, Sung Hyun; Lee, Hae-Won

    2017-01-01

    The geographical origin of kimchi is of interest to consumers and producers because the prices of commercial kimchi products can vary significantly according to the geographical origin. Hence, social issues related to the geographical origin of kimchi in Korea have emerged as a major problem. In this study, the geographical origin of kimchi was determined by comparing the mass fingerprints obtained for Korean and Chinese kimchi samples by MALDI-TOF MS with multivariate analysis. The results obtained herein provide an accurate, powerful tool to clearly discriminate kimchi samples based on their geographical origin within a short time and to ensure food authenticity, which is of significance in the kimchi industry. Furthermore, our MALDI-TOF MS method could be applied to determining the geographical origin of other fermented-salted vegetables at a reduced cost in shorter times. PMID:29149220

  10. A novel method to rapidly distinguish the geographical origin of traditional fermented-salted vegetables by mass fingerprinting.

    Directory of Open Access Journals (Sweden)

    So-Ra Yoon

    Full Text Available The geographical origin of kimchi is of interest to consumers and producers because the prices of commercial kimchi products can vary significantly according to the geographical origin. Hence, social issues related to the geographical origin of kimchi in Korea have emerged as a major problem. In this study, the geographical origin of kimchi was determined by comparing the mass fingerprints obtained for Korean and Chinese kimchi samples by MALDI-TOF MS with multivariate analysis. The results obtained herein provide an accurate, powerful tool to clearly discriminate kimchi samples based on their geographical origin within a short time and to ensure food authenticity, which is of significance in the kimchi industry. Furthermore, our MALDI-TOF MS method could be applied to determining the geographical origin of other fermented-salted vegetables at a reduced cost in shorter times.

  11. Rapid discrimination of environmental Vibrio by matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Eddabra, Rkia; Prévost, Gilles; Scheftel, Jean-Michel

    2012-04-20

    The aim of this study was to discriminate 30 Vibrio strains isolated from two wastewater treatment plants from Agadir, Morocco by two molecular typing methods, pulsed-field gel electrophoresis (PFGE) and matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS). Out of the 30 strains of Vibrio examined in this study, 5 isolates could not be typed by PFGE and consistently appeared as a smear on the gel. In general, high genetic biodiversity among the Vibrio strains was found regardless to the isolation source. The results of MALDI TOF analysis show a high congruence of strain grouping demonstrating the accuracy and reliability of MALDI-TOF MS. Copyright © 2011 Elsevier GmbH. All rights reserved.

  12. Rapid and simultaneous in situ assessment of aflatoxins and stilbenes using silica plate imprinting mass spectrometry imaging.

    Science.gov (United States)

    de Oliveira, Diogo N; Ferreira, Mônica S; Catharino, Rodrigo R

    2014-01-01

    A fast and direct combination of techniques for simultaneous mycotoxin and phytoalexin identification in peanut skin and kernel is described. Silica Plate Imprinting Laser Desorption/Ionization Mass Spectrometry Imaging (SPILDI-MSI) is a powerful technique that exhibits great advantages, such as solvent-free and matrix-free characteristics, as well as no sample preparation or separation steps. It also permits accurate identification of mycotoxins and phytoalexins with unique fingerprint profiles in just a few seconds. Results are expressed as chemical images of the 4 identified types of aflatoxins (B1, B2, G1 and G2) and a stilbenoid (resveratrol). Also, SPILDI-MSI allows the comparison between the spatial distribution of aflatoxins and resveratrol found in kernel and skin. This novel application has proven to be useful for instantaneous qualitative assessment of aflatoxins and stilbenoids both in the peanut skin and kernel and offers precise tracking of fungal contamination in nuts and other foodstuffs.

  13. Trypsin immobilization on an ethylenediamine-based monolithic minidisk for rapid on-line peptide mass fingerprinting studies.

    Science.gov (United States)

    Nicoli, R; Rudaz, S; Stella, C; Veuthey, J-L

    2009-03-27

    The aim of this work was to develop a trypsin-based micro-immobilized enzyme reactor prepared on a monolithic ethylenediamine BIA Separations CIM (convective interaction media) minidisk. The micro-immobilized enzyme reactor (IMER) was integrated in a liquid chromatography system hyphenated to electrospray ionization tandem mass spectrometry to carry out on-line protein digestion and identification. The performance of this IMER was compared with that obtained using a previously developed bioreactor prepared on a conventional CIM ethylenediamine disk and with that of the commercially available Poroszyme immobilized trypsin cartridge. In this work, we showed how different proteins were identified with good recoveries using a digestion time of 10 min only.

  14. Rapid simultaneous determination of organophosphorus pesticides in human serum and urine by liquid chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Zlatković Milica

    2010-01-01

    Full Text Available Background/Aim. Analysis of organophosphosphorus compounds and their metabolites in a biological material includes the use of numerous methods, covering both preparation of samples for analysis and their identification that is considered to be very complex. Low concentrations monitoring requires implementation of highly sensitive analytical techniques. The aim of this study was to develop and validate an original and sensitive method for the detection and quantitation of organophosphorus pesticides (dimethoate, diazinon, malathion and malaoxon in human biological matrices (serum, urine. Methods. This method was based on a solid-phase extraction procedure, a chromatographic separation using an ACQUITY UPLC ® HSST3 column and mass spectrometric detection in the positve ion mode. Mobile phase: was consited of Solvent A (5 mM ammonium formate pH 3.0 and Solvent B (0.1% acetic formate in methanol, in a linear gradient (constant flow-rate 0.3 mL/min. Results. The standard curve was linear in the range of 0.05-5.00 mg/L for malathion and malaoxon, 0.10-5.00 mg/L for dimethoate and 0.05-2.50 mg/L for diazinon. The correlation coefficient was r ≥ 0.99. Extraction recoveries were satisfactory and ranged between 90-99%. The limits of detection (LOD was between 0.007- 0.07 mg/L and the limits of quantitation (LOQ ranged between 0.022-0.085 mg/L. Intra- and interassay precision and accuracy were satisfactory for all of the pesticides analyzed. Conclusion. The method of liquid chromatography - mass spectrometry is simple, accurate, and useful for the determination of organophosphorus pesticides in both clinical and forensic toxicology.

  15. Rapid and reliable steroid hormone profiling in Tursiops truncatus blubber using liquid chromatography tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Boggs, Ashley S P; Schock, Tracey B; Schwacke, Lori H; Galligan, Thomas M; Morey, Jeanine S; McFee, Wayne E; Kucklick, John R

    2017-08-01

    Monitoring of marine mammal steroid hormone status using matrices alternative to blood is desirable due to the ability to remotely collect samples, which minimizes stress to the animal. However, measurement techniques in alternative matrices such as blubber described to date are limited in the number and types of hormones measured. Therefore, a new method using bead homogenization to QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction, C18 post extraction cleanup and analysis by liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed and applied to the measurement of hormone suites in bottlenose dolphin blubber. Validations were conducted in blubber from fresh dead stranded bottlenose dolphin. The final method consisting of two LC separations and garnet bead homogenization was tested for extraction efficiencies. Steroids were separated using a biphenyl column for reproductive hormones and C18 column for corticosteroids. Three hormones previously noted in blubber, testosterone, progesterone, and cortisol, were quantified in addition to previously unmeasured androstenedione, 17-hydroxyprogesterone, 11-deoxycortisol, 11-deoxycorticosterone, and cortisone in a single sample (0.4 g blubber). Extraction efficiencies of all hormones from blubber ranged from 84% to 112% and all RSDs were comparable to those reported using immunoassay methods (< 15%). The method was successfully applied to remote biopsied blubber samples to measure baseline hormone concentrations. Through this method, increased coverage of steroid hormone pathways from a single remotely collected sample potentially enhances the ability to interpret biological phenomena such as reproduction and stress in wild dolphin populations. Graphical abstract The steroid hormone profile is quantifiable from a single sample of bottlenose dolphin blubber using liquid chromatography tandem mass spectrometry. This profile can be applied to remotely collected dart biopsies and be used to

  16. Rapid identification of siderophores by combined thin-layer chromatography/matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Hayen, Heiko; Volmer, Dietrich A

    2005-01-01

    The investigation of a combined thin-layer chromatography/matrix-assisted laser desorption/ionization mass spectrometry (TLC/MALDI-MS) method for the analysis of siderophores from microbial samples is described. The investigated siderophores were enterobactin, ferrioxamine B, ferrichrome, ferrirhodin, rhodotorulic acid and coprogen. Solid-phase extraction was employed to recover the siderophores from the microbial samples. After visualization of the spots via spraying with ferric chloride or chrome azurol sulfonate assay solution, the MALDI matrix was applied to the gel surface. Several TLC/MALDI experimental parameters were optimized, such as type and concentration of MALDI matrix, as well as the type and composition of solvent to facilitate analyte transport from the inside of the TLC gel to the surface. The impact of these parameters on sensitivity, precision and ion formation of the various siderophores was studied. The detection limits for the investigated siderophores were in the range 1-4 pmol. These values were about 4-24 times higher than the detection limits obtained directly from stainless steel MALDI targets. The differences were most likely due to incomplete transport of the 'trapped' analyte molecules from the deeper layers of the TLC gel to the surface and into the matrix layer. In addition, chromatographic band broadening spread the analyte further in TLC as compared with the steel plates, resulting in less analyte per surface area. The identification of the siderophores was aided by concurrently applying a Ga(III) nitrate solution to the TLC plate during the visualization step. The resulting formation of Ga(III) complexes lead to distinctive (69)Ga/(71)Ga isotope patterns in the mass spectra. The versatility of the TLC/MALDI-MS assay was demonstrated by using it to analyze siderophores in a Pseudomonas aeruginosa sample. An iron-binding compound was identified in the sample, namely pyochelin (2-(2-o-hydroxyphenyl-2-thiazolin-4-yl)-3

  17. Rapid X-ray variability properties during the unusual very hard state in neutron-star low-mass X-ray binaries

    Science.gov (United States)

    Wijnands, R.; Parikh, A. S.; Altamirano, D.; Homan, J.; Degenaar, N.

    2017-11-01

    Here, we study the rapid X-ray variability (using XMM-Newton observations) of three neutron-star low-mass X-ray binaries (1RXS J180408.9-342058, EXO 1745-248 and IGR J18245-2452) during their recently proposed very hard spectral state. All our systems exhibit a strong to very strong noise component in their power density spectra (rms amplitudes ranging from 34 per cent to 102 per cent) with very low characteristic frequencies (as low as 0.01 Hz). These properties are more extreme than what is commonly observed in the canonical hard state of neutron-star low-mass X-ray binaries observed at X-ray luminosities similar to those we observe from our sources. This suggests that indeed the very hard state is a spectral-timing state distinct from the hard state, although we argue that the variability behaviour of IGR J18245-2452 is very extreme and possibly this source was in a very unusual state. We also compare our results with the rapid X-ray variability of the accreting millisecond X-ray pulsars IGR J00291+5934 and Swift J0911.9-6452 (also using XMM-Newton data) for which previously similar variability phenomena were observed. Although their energy spectra (as observed using the Swift X-ray telescope) were not necessarily as hard (i.e. for Swift J0911.9-6452) as for our other three sources, we conclude that likely both sources were also in very similar state during their XMM-Newton observations. This suggests that different sources that are found in this new state might exhibit different spectral hardness and one has to study both the spectral and the rapid variability to identify this unusual state.

  18. Rapid, non-destructive selection of peanuts for high aflatoxin content by soaking and tandem mass spectrometry.

    Science.gov (United States)

    Schatzki, Thomas F; Haddon, William F

    2002-05-08

    Peanut lots are subject to aflatoxin levels high enough to cause concern to health agencies and trade channels. A possible solution would be to mechanically sort out high aflatoxin nuts from the process stream. Only highly contaminated nuts would need to be removed. However, there exists at present no sorting mechanism which meets commercial needs of adequate reduction and product preservation. To build such a sorter requires knowledge of the properties that can be used for sorting. The first step in the design is to select on the order of one hundred undamaged contaminated nuts which can be compared with noncontaminated ones. Because contaminated nuts are rare, a very large number of nuts needs to be examined nondestructively. We present a method to rapidly carry out such a selection. The method is based on dipping nuts into extraction fluid and examining the resulting fluid by tandem MS without preliminary cleanup. This method has been applied to examine over 65,000 nuts, yielding approximately 120 nuts, each containing more than 250-43000 ng/g aflatoxin (depending on process stream).

  19. Use of Molecular Methods for the Rapid Mass Detection of Schistosoma mansoni (Platyhelminthes: Trematoda) in Biomphalaria spp. (Gastropoda: Planorbidae).

    Science.gov (United States)

    Caldeira, Roberta Lima; Jannotti-Passos, Liana Konovaloffi; Dos Santos Carvalho, Omar

    2017-01-01

    The low stringency-polymerase chain reaction (LS-PCR) and loop-mediated isothermal amplification (LAMP) assays were used to detect the presence of S. mansoni DNA in (1) Brazilian intermediate hosts (Biomphalaria glabrata, B. straminea, and B. tenagophila) with patent S. mansoni infections, (2) B. glabrata snails with prepatent S. mansoni infections, (3) various mixtures of infected and noninfected snails; and (4) snails infected with other trematode species. The assays showed high sensitivity and specificity and could detect S. mansoni DNA when one positive snail was included in a pool of 1,000 negative specimens of Biomphalaria. These molecular approaches can provide a low-cost, effective, and rapid method for detecting the presence of S. mansoni in pooled samples of field-collected Biomphalaria. These assays should aid mapping of transmission sites in endemic areas, especially in low prevalence regions and improve schistosomiasis surveillance. It will be a useful tool to monitor low infection rates of snails in areas where control interventions are leading towards the elimination of schistosomiasis.

  20. Determining the masses and radii of rapidly rotating, oblate neutron stars using energy-resolved waveforms of their X-ray burst oscillations

    Science.gov (United States)

    Lamb, Frederick K.; Miller, M. Coleman

    2014-08-01

    We have developed new, more sophisticated, and much faster Bayesian analysis methods that enable us to estimate the masses and radii of rapidly rotating, oblate neutron stars using the energy-resolved waveforms of their X-ray burst oscillations and to determine the uncertainties in these mass and radius estimates. We first generate the energy-resolved burst oscillation waveforms that would be produced by a hot spot on various rapidly rotating, oblate stars, using the oblate-star Schwarzschild-spacetime (OS) approximation. In generating these synthetic data, we assume that 1 million counts have been collected from the hot spot and that the background is 9 million counts. This produces a realistic modulation amplitude and a total number of counts comparable to the number that could be obtained by a future space mission such as the proposed LOFT or AXTAR missions or the accepted NICER mission by combining data from many bursts from a given star. We then compute the joint posterior distribution of the mass M and radius R in standard models, for each synthetic waveform, and use these posterior distributions to determine the 1-, 2-, and 3-sigma confidence regions in the M-R plane for each synthetic waveform and model. We report here the confidence regions obtained when Schwarzschild+Doppler (S+D) and OS waveform models are used, including results obtained when the properties of the star used to generate the synthetic waveform data differ from the properties of the star used in modeling the waveform. These results are based on research supported by NSF grant AST0709015 at the University of Illinois and NSF grant AST0708424 at the University of Maryland.

  1. Rapid profiling and structural characterization of bioactive compounds and their distribution in different parts of Berberis petiolaris Wall. ex G. Don applying hyphenated mass spectrometric techniques.

    Science.gov (United States)

    Singh, A; Bajpai, V; Srivastava, M; Arya, K R; Kumar, B

    2014-10-15

    Berberis petiolaris Wall. is a lesser known medicinal plant, belonging to the family Berberidaceae. The genus Berberis is known for many biological activities such as anti-microbial, anti-inflammatory and anti-diarrheal, etc. There are not many reports of the isolation of components from Berberis petiolaris. This study aims to seek identification, characterization and quantification of components. A method was developed for rapid screening of phytochemicals using high-pressure liquid chromatography hyphenated with quadrupole time-of-flight mass spectrometry (HPLC/ESI-QTOF-MS/MS). Suitable collision-induced dissociation mass spectrometry (CID-MS/MS) methods were developed for structural investigation of alkaloids, flavanoids and other classes of compounds using nine reference standards for authentication. Multiple reaction monitoring (MRM) methods were developed for quantitative study of five constituents using triple quadrupole-linear ion trap mass spectrometry (UPLC/QqLIT-MS/MS). On the basis of HPLC retention behavior and fragmentation pathways obtained by high-resolution MS and MS/MS, 32 compounds were identified and characterized in different parts of Berberis petiolaris. Quantitative studies of chlorogenic acid, magnoflorine, jatrorrhizine, palmatine and berberine were also completed successfully. Rapid and accurate HPLC/ESI-QTOF-MS/MS and UPLC/ESI-QqLIT-MS/MS methods were established for identification, characterization and quantification of phytochemicals in the ethanolic extract of Berberis petiolaris. These methods, therefore, can be used for studies on phytochemical variation in different parts of the plant. Principle components analysis (PCA) may be used for plant part discrimination. Copyright © 2014 John Wiley & Sons, Ltd.

  2. Magnetic solid phase extraction coupled with desorption corona beam ionization-mass spectrometry for rapid analysis of antidepressants in human body fluids.

    Science.gov (United States)

    Chen, Di; Zheng, Hao-Bo; Huang, Yun-Qing; Hu, Yu-Ning; Yu, Qiong-Wei; Yuan, Bi-Feng; Feng, Yu-Qi

    2015-08-21

    Ambient ionization techniques show good potential in rapid analysis of target compounds. However, a direct application of these ambient ionization techniques for the determination of analytes in a complex matrix is difficult due to the matrix interference and ion suppression. To resolve this problem, here we developed a strategy by coupling magnetic solid phase extraction (MSPE) with desorption corona beam ionization (DCBI)-mass spectrometry (MS). As a proof of concept, the pyrrole-coated Fe3O4 magnetic nanoparticles (Fe3O4@Ppy) were prepared and used for the extraction of antidepressants. After extraction, the Fe3O4@Ppy with trapped antidepressants was then directly subjected to DCBI-MS analysis with the aid of a homemade magnetic glass capillary. As the MSPE process is rapid and the direct DCBI-MS analysis does not need solvent desorption or chromatographic separation processes, the overall analysis can be completed within 3 min. The proposed MSPE-DCBI-MS method was then successfully used to determine antidepressants in human urine and plasma. The calibration curves were obtained in the range of 0.005-0.5 μg mL(-1) for urine and 0.02-1 μg mL(-1) for plasma with reasonable linearity (R(2) > 0.951). The limits of detection of three antidepressants were in the range of 0.2-1 ng mL(-1) for urine and 2-5 ng mL(-1) for plasma. Acceptable reproducibility for rapid analysis was achieved with relative standard deviations less than 19.1% and the relative recoveries were 85.2-118.7%. Taken together, the developed MSPE-DCBI-MS strategy offers a powerful capacity for rapid analysis of target compounds in a complex matrix, which would greatly expand the applications of ambient ionization techniques with plentiful magnetic sorbents.

  3. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

    2013-12-04

    A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography-mass spectrometry (GC-MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C2mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78°C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Use of a cholera rapid diagnostic test during a mass vaccination campaign in response to an epidemic in Guinea, 2012.

    Directory of Open Access Journals (Sweden)

    Isabel Martinez-Pino

    Full Text Available BACKGROUND: During the 2012 cholera outbreak in the Republic of Guinea, the Ministry of Health, supported by Médecins Sans Frontières - Operational Center Geneva, used the oral cholera vaccine Shanchol as a part of the emergency response. The rapid diagnostic test (RDT Crystal VC, widely used during outbreaks, detects lipopolysaccharide antigens of Vibrio cholerae O1 and O139, both included in Shanchol. In the context of reactive use of a whole-cell cholera vaccine in a region where cholera cases have been reported, it is essential to know what proportion of vaccinated individuals would be reactive to the RDT and for how long after vaccination. METHODOLOGY/PRINCIPAL FINDINGS: A total of 108 vaccinated individuals, selected systematically among all persons older than one year, were included at vaccination sites and 106 were included in the analysis. Stools samples of this cohort of vaccinated participants were collected and tested with the RDT every day until the test was negative for two consecutive visits or for a maximum of 7 days. A total of 94.3% of cholera vaccine recipients had a positive test after vaccination; all except one of these positive results were reactive only with the O139 antigen. The mean time to become negative in those with an initial positive result after vaccination was 3.8 days, standard deviation 1.1 days. CONCLUSIONS/SIGNIFICANCE: The RDT Crystal VC becomes positive in persons recently vaccinated against cholera, although almost exclusively to the O139 antigen. This reactivity largely disappeared within five days after vaccination. These results suggest that the test can be used normally as soon as 24 hours after vaccination in a context of O1 epidemics, which represent the vast majority of cases, and after a period of five days in areas where V. cholerae O139 is present. The reason why only O139 test line became positive remains to be investigated.

  5. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for rapid identification of fungal rhinosinusitis pathogens.

    Science.gov (United States)

    Huang, Yanfei; Wang, Jinglin; Zhang, Mingxin; Zhu, Min; Wang, Mei; Sun, Yufeng; Gu, Haitong; Cao, Jingjing; Li, Xue; Zhang, Shaoya; Lu, Xinxin

    2017-03-01

    Filamentous fungi are among the most important pathogens, causing fungal rhinosinusitis (FRS). Current laboratory diagnosis of FRS pathogens mainly relies on phenotypic identification by culture and microscopic examination, which is time consuming and expertise dependent. Although matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) MS has been employed to identify various fungi, its efficacy in the identification of FRS fungi is less clear. A total of 153 FRS isolates obtained from patients were analysed at the Clinical Laboratory at the Beijing Tongren Hospital affiliated to the Capital Medical University, between January 2014 and December 2015. They were identified by traditional phenotypic methods and Bruker MALDI-TOF MS (Bruker, Biotyper version 3.1), respectively. Discrepancies between the two methods were further validated by sequencing. Among the 153 isolates, 151 had correct species identification using MALDI-TOF MS (Bruker, Biot 3.1, score ≥2.0 or 2.3). MALDI-TOF MS enabled identification of some very closely related species that were indistinguishable by conventional phenotypic methods, including 1/10 Aspergillus versicolor, 3/20 Aspergillus flavus, 2/30 Aspergillus fumigatus and 1/20 Aspergillus terreus, which were misidentified by conventional phenotypic methods as Aspergillus nidulans, Aspergillus oryzae, Aspergillus japonicus and Aspergillus nidulans, respectively. In addition, 2/2 Rhizopus oryzae and 1/1 Rhizopus stolonifer that were identified only to the genus level by the phenotypic method were correctly identified by MALDI-TOF MS. MALDI-TOF MS is a rapid and accurate technique, and could replace the conventional phenotypic method for routine identification of FRS fungi in clinical microbiology laboratories.

  6. Rapid Quantification of Major Volatile Metabolites in Fermented Food and Beverages Using Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Farhana R. Pinu

    2017-07-01

    Full Text Available Here we present a method for the accurate quantification of major volatile metabolites found in different food and beverages, including ethanol, acetic acid and other aroma compounds, using gas chromatography coupled to mass spectrometry (GC-MS. The method is combined with a simple sample preparation procedure using sodium chloride and anhydrous ethyl acetate. The GC-MS analysis was accomplished within 4.75 min, and over 80 features were detected, of which 40 were positively identified using an in-house and a commercialmass spectrometry (MS library. We determined different analytical parameters of these metabolites including the limit of detection (LOD, limit of quantitation (LOQ and range of quantification. In order to validate the method, we also determined detailed analytical characteristics of five major fermentation end products including ethanol, acetic acid, isoamyl alcohol, ethyl-L-lactate and, acetoin. The method showed very low technical variability for the measurements of these metabolites in different matrices (<3% with an excellent accuracy (100% ± 5%, recovery (100% ± 10%, reproducibility and repeatability [Coefficient of variation (CV 1–10%]. To demonstrate the applicability of the method, we analysed different fermented products including balsamic vinegars, sourdough, distilled (whisky and non-distilled beverages (wine and beer.

  7. Rapid and sensitive detection of carbapenemase activity in Acinetobacter baumannii using superficially porous liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lin, Huei-Ru; Hu, Anren; Lai, Meng-Jiun; Chiang, Chih-Wei; Liao, Chao-Chuan; Chang, Kai-Chih

    2016-12-01

    The emergence and spread of carbapenem-resistant Acinetobacter baumannii poses a challenge for optimizing antibiotic therapies and preventing outbreaks. Traditional phenotypic assays such as the modified Hodge test (MHT) or polymerase chain reaction (PCR)-based detection of the carbapenemase genes are time-consuming and complicated. Therefore, new approaches for the efficient detection of carbapenemase-producing A. baumannii are urgently required. In this study, we used the superficially porous liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay to measure carbapenem hydrolysis in a solution spiked with test strains of A. baumannii. The rate of carbapenem hydrolysis during incubation was expressed as the ratio of the carbapenem peak area of the test A. baumannii strains to the noncarbapenemase-producing A. baumannii ATCC 17978. This method can accurately measure the carbapenem hydrolysis rate and, therefore, can effectively identify carbapenemase-producing strains within 75 minutes. A total of 112 A. baumannii strains were used in this study, including 103 clinical isolates with 68 carbapenem-resistant strains and 35 carbapenem-susceptible strains, seven ATCC strains and two selected mutants. The results of the superficially porous LC-MS/MS assay showed higher detection sensitivity compared to the results of the MHT. Our results demonstrate the ability of the former method to routinely detect carbapenemase-producing A. baumannii. Copyright © 2015. Published by Elsevier B.V.

  8. Liquid Chromatography-Mass Spectrometry-Based Rapid Secondary-Metabolite Profiling of Marine Pseudoalteromonas sp. M2

    Directory of Open Access Journals (Sweden)

    Woo Jung Kim

    2016-01-01

    Full Text Available The ocean is a rich resource of flora, fauna, and food. A wild-type bacterial strain showing confluent growth on marine agar with antibacterial activity was isolated from marine water, identified using 16S rDNA sequence analysis as Pseudoalteromonas sp., and designated as strain M2. This strain was found to produce various secondary metabolites including quinolone alkaloids. Using high-resolution mass spectrometry (MS and nuclear magnetic resonance (NMR analysis, we identified nine secondary metabolites of 4-hydroxy-2-alkylquinoline (pseudane-III, IV, V, VI, VII, VIII, IX, X, and XI. Additionally, this strain produced two novel, closely related compounds, 2-isopentylqunoline-4-one and 2-(2,3-dimetylbutylqunoline-4-(1H-one, which have not been previously reported from marine bacteria. From the metabolites produced by Pseudoalteromonas sp. M2, 2-(2,3-dimethylbutylquinolin-4-one, pseudane-VI, and pseudane-VII inhibited melanin synthesis in Melan-A cells by 23.0%, 28.2%, and 42.7%, respectively, wherein pseudane-VII showed the highest inhibition at 8 µg/mL. The results of this study suggest that liquid chromatography (LC-MS/MS-based metabolite screening effectively improves the efficiency of novel metabolite discovery. Additionally, these compounds are promising candidates for further bioactivity development.

  9. Development of a loop-mediated isothermal amplification method for rapid mass-screening of sand flies for Leishmania infection.

    Science.gov (United States)

    Nzelu, Chukwunonso O; Gomez, Eduardo A; Cáceres, Abraham G; Sakurai, Tatsuya; Martini-Robles, Luiggi; Uezato, Hiroshi; Mimori, Tatsuyuki; Katakura, Ken; Hashiguchi, Yoshihisa; Kato, Hirotomo

    2014-04-01

    Entomological monitoring of Leishmania infection in leishmaniasis endemic areas offers epidemiologic advantages for predicting the risk and expansion of the disease, as well as evaluation of the effectiveness of control programs. In this study, we developed a highly sensitive loop-mediated isothermal amplification (LAMP) method for the mass screening of sand flies for Leishmania infection based on the 18S rRNA gene. The LAMP technique could detect 0.01 parasites, which was more sensitive than classical PCR. The method was robust and could amplify the target DNA within 1h from a crude sand fly template without DNA purification. Amplicon detection could be accomplished by the newly developed colorimetric malachite green (MG)--mediated naked eye visualization. Pre-addition of MG to the LAMP reaction solution did not inhibit amplification efficiency. The field applicability of the colorimetric MG-based LAMP assay was demonstrated with 397 field-caught samples from the endemic areas of Ecuador and eight positive sand flies were detected. The robustness, superior sensitivity, and ability to produce better visual discriminatory reaction products than existing LAMP fluorescence and turbidity assays indicated the field potential usefulness of this new method for surveillance and epidemiological studies of leishmaniasis in developing countries. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. [Rapid determination of 6 pesticide residues in tomato paste by ultra performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Su, Min; Li, Shiyu; Li, Fengge; Gong, Zhiguo; Wang, Jinhua

    2011-11-01

    An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) was established for the simultaneous determination of imidacloprid, carbendazim, thiophanate-methyl, propamocarb, methomyl and dimethomorph residues in tomato paste. The samples were extracted by methanol-water (1: 1, v/v) containing 0.1% (v/v) acetic acid. The separation was performed on a Waters Acquity UPLC system with a BEH C18 column with the gradient elution of methanol and water (containing 10 mmol/L ammonium acetate). The six pesticides were determined in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched standard solution, and the calibration curves showed good linearity within the concentrations of 0.005 to 0.2 mg/L and the correlation coefficients (r) were more than 0.995. The average recoveries of the six pesticides ranged from 66.8% to 102.9% in the three spiked levels of 0.02, 0.05 and 0.2 mg/kg. The relative standard deviations (RSDs) were all less than 15%. The limits of quantification (LOQ, S/N > 10) were 0.02 mg/kg for the all analytes. The results indicate that the method is easier, faster, more sensitive, and suitable for the qualitative and quantitative confirmation of the six pesticide residues from tomato paste.

  11. A rapid liquid chromatography tandem mass spectrometry-based method for measuring propranolol on dried blood spots.

    Science.gov (United States)

    Della Bona, Maria Luisa; Malvagia, Sabrina; Villanelli, Fabio; Giocaliere, Elisa; Ombrone, Daniela; Funghini, Silvia; Filippi, Luca; Cavallaro, Giacomo; Bagnoli, Paola; Guerrini, Renzo; la Marca, Giancarlo

    2013-05-05

    Propranolol, a non-selective beta blocker drug, is used in young infants and newborns for treating several heart diseases; its pharmacokinetics has been extensively evaluated in adult patients using extrapolation to treat pediatric population. The purpose of the present study was to develop and validate a method to measure propranolol levels in dried blood spots. The analysis was performed by using liquid chromatography/tandem mass spectrometry operating in multiple reaction monitoring mode. The calibration curve in matrix was linear in the concentration range of 2.5-200 μg/L with correlation coefficient r=0.9996. Intra-day and inter-day precisions and biases were less than 8.0% (n=10) and 11.5% (n=10) respectively. The recoveries ranged from 94 to 100% and the matrix effect did not result in a severe signal suppression. Propranolol on dried blood spot showed a good stability at three different temperatures for one month. This paper describes a micromethod for measuring propranolol levels on dried blood spot, which determines a great advantage in neonates or young infants during pharmacokinetic studies because of less invasive sampling and small blood volume required. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Rapid Quantification of Major Volatile Metabolites in Fermented Food and Beverages Using Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Pinu, Farhana R; Villas-Boas, Silas G

    2017-07-26

    Here we present a method for the accurate quantification of major volatile metabolites found in different food and beverages, including ethanol, acetic acid and other aroma compounds, using gas chromatography coupled to mass spectrometry (GC-MS). The method is combined with a simple sample preparation procedure using sodium chloride and anhydrous ethyl acetate. The GC-MS analysis was accomplished within 4.75 min, and over 80 features were detected, of which 40 were positively identified using an in-house and a commercialmass spectrometry (MS) library. We determined different analytical parameters of these metabolites including the limit of detection (LOD), limit of quantitation (LOQ) and range of quantification. In order to validate the method, we also determined detailed analytical characteristics of five major fermentation end products including ethanol, acetic acid, isoamyl alcohol, ethyl-L-lactate and, acetoin. The method showed very low technical variability for the measurements of these metabolites in different matrices (<3%) with an excellent accuracy (100% ± 5%), recovery (100% ± 10%), reproducibility and repeatability [Coefficient of variation (CV) 1-10%)]. To demonstrate the applicability of the method, we analysed different fermented products including balsamic vinegars, sourdough, distilled (whisky) and non-distilled beverages (wine and beer).

  13. A rapid method for simultaneous determination of arsenic, cadmium and lead in drinking water by inductively coupled plasma mass spectrometry

    Directory of Open Access Journals (Sweden)

    Joshua Rey P. Torres

    Full Text Available The raw water source of drinking water in most areas in the Philippines is typically river water and in some cases groundwater. These sources are prone to elevated levels of metals and metalloids that may cause exposure of the general population when the treatment of the water is inadequate. This work presents a simple method based on EPA Method 200.8 for the determination of total concentrations of arsenic (As, cadmium (Cd and lead (Pb in drinking water using inductively coupled plasma-mass spectrometry (ICP-MS as the element-selective detector. This was applied in the determination of these elements in the water supply in Metro Manila, Philippines. The method detection limits were 0.095 μg L-1, 0.043 μg L-1, and 0.114 μg L-1 for total As, Cd and Pb, respectively.The method was validated using National Institute of Standards and Technology (NIST 1643e certified reference material for trace elements in water and determined values were 60.4 ± 0.5 μg L-1, 6.7 ± 0.1 μg L-1, and 19.6 ± 0.5 μg L-1 for As, Cd and Pb, respectively. These determined values were in good agreement with the certified values in the reference material. Analysis of actual drinking water samples showed that most samples did not exceed the limit of the Philippine drinking water standard for the elements.

  14. [Rapid determination of benzene series in seawater by gas chromatography-mass spectrometry with static headspace extraction].

    Science.gov (United States)

    Bai, Hongyan; Han, Bin; Chen, Junhui; Zheng, Li; Yang, Dongfang; Wang, Xiaoru

    2012-05-01

    A method for the simultaneous determination of 13 benzene series (BTEX) in seawater using gas chromatography-mass spectrometry with static headspace extraction (HS-GC/MS) was developed. To carefully characterize the performance of this method, several factors affecting parameters were studied in detail, such as the type of column, heating procedure, equilibrium temperature, equilibrium time and the volume ratio of gas phase to liquid phase. The optimized conditions were as follows: the polar column of DB-WAX; heating procedure, 40 degrees C kept for 4 min, then raised to 120 degrees C at 10 degrees C/min, to 180 degrees C at 25 degrees C/min; equilibrium temperature, 80 degrees C; equilibrium time, 10 min; and the volume ratio of gas phase to liquid phase, 1:1. Under the optimized conditions, the linear equations were obtained in the concentration range of 0.16-320 microg/L with correlation coefficients greater than 0.999. The limits of detection (S/N = 3) were 0.019-0.033 microg/L. The recoveries at the three spiked levels of 1.6, 16 and 160 microg/L ranged from 81. 25% to 103.73% with the relative standard deviations (RSD, n=6) from 0.3% to 4.4%. The analytical results of the practical seawater samples from Shanghai Huangpu District were satisfactory. The determination of the 13 benzene series can be finished in 12 min. The method is simple, accurate, reliable, efficient and environmental-friendly.

  15. Rapid identification of Burkholderia mallei and Burkholderia pseudomallei by intact cell Matrix-assisted Laser Desorption/Ionisation mass spectrometric typing

    Science.gov (United States)

    2012-01-01

    Background Burkholderia (B.) pseudomallei and B. mallei are genetically closely related species. B. pseudomallei causes melioidosis in humans and animals, whereas B. mallei is the causative agent of glanders in equines and rarely also in humans. Both agents have been classified by the CDC as priority category B biological agents. Rapid identification is crucial, because both agents are intrinsically resistant to many antibiotics. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-TOF MS) has the potential of rapid and reliable identification of pathogens, but is limited by the availability of a database containing validated reference spectra. The aim of this study was to evaluate the use of MALDI-TOF MS for the rapid and reliable identification and differentiation of B. pseudomallei and B. mallei and to build up a reliable reference database for both organisms. Results A collection of ten B. pseudomallei and seventeen B. mallei strains was used to generate a library of reference spectra. Samples of both species could be identified by MALDI-TOF MS, if a dedicated subset of the reference spectra library was used. In comparison with samples representing B. mallei, higher genetic diversity among B. pseudomallei was reflected in the higher average Eucledian distances between the mass spectra and a broader range of identification score values obtained with commercial software for the identification of microorganisms. The type strain of B. pseudomallei (ATCC 23343) was isolated decades ago and is outstanding in the spectrum-based dendrograms probably due to massive methylations as indicated by two intensive series of mass increments of 14 Da specifically and reproducibly found in the spectra of this strain. Conclusions Handling of pathogens under BSL 3 conditions is dangerous and cumbersome but can be minimized by inactivation of bacteria with ethanol, subsequent protein extraction under BSL 1 conditions and MALDI-TOF MS analysis being faster than

  16. Rapid identification of Burkholderia mallei and Burkholderia pseudomallei by intact cell Matrix-assisted Laser Desorption/Ionisation mass spectrometric typing.

    Science.gov (United States)

    Karger, Axel; Stock, Rüdiger; Ziller, Mario; Elschner, Mandy C; Bettin, Barbara; Melzer, Falk; Maier, Thomas; Kostrzewa, Markus; Scholz, Holger C; Neubauer, Heinrich; Tomaso, Herbert

    2012-10-10

    Burkholderia (B.) pseudomallei and B. mallei are genetically closely related species. B. pseudomallei causes melioidosis in humans and animals, whereas B. mallei is the causative agent of glanders in equines and rarely also in humans. Both agents have been classified by the CDC as priority category B biological agents. Rapid identification is crucial, because both agents are intrinsically resistant to many antibiotics. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-TOF MS) has the potential of rapid and reliable identification of pathogens, but is limited by the availability of a database containing validated reference spectra. The aim of this study was to evaluate the use of MALDI-TOF MS for the rapid and reliable identification and differentiation of B. pseudomallei and B. mallei and to build up a reliable reference database for both organisms. A collection of ten B. pseudomallei and seventeen B. mallei strains was used to generate a library of reference spectra. Samples of both species could be identified by MALDI-TOF MS, if a dedicated subset of the reference spectra library was used. In comparison with samples representing B. mallei, higher genetic diversity among B. pseudomallei was reflected in the higher average Eucledian distances between the mass spectra and a broader range of identification score values obtained with commercial software for the identification of microorganisms. The type strain of B. pseudomallei (ATCC 23343) was isolated decades ago and is outstanding in the spectrum-based dendrograms probably due to massive methylations as indicated by two intensive series of mass increments of 14 Da specifically and reproducibly found in the spectra of this strain. Handling of pathogens under BSL 3 conditions is dangerous and cumbersome but can be minimized by inactivation of bacteria with ethanol, subsequent protein extraction under BSL 1 conditions and MALDI-TOF MS analysis being faster than nucleic amplification methods. Our

  17. Rapid identification of Burkholderia mallei and Burkholderia pseudomallei by intact cell Matrix-assisted Laser Desorption/Ionisation mass spectrometric typing

    Directory of Open Access Journals (Sweden)

    Karger Axel

    2012-10-01

    Full Text Available Abstract Background Burkholderia (B. pseudomallei and B. mallei are genetically closely related species. B. pseudomallei causes melioidosis in humans and animals, whereas B. mallei is the causative agent of glanders in equines and rarely also in humans. Both agents have been classified by the CDC as priority category B biological agents. Rapid identification is crucial, because both agents are intrinsically resistant to many antibiotics. Matrix-assisted laser desorption/ionisation mass spectrometry (MALDI-TOF MS has the potential of rapid and reliable identification of pathogens, but is limited by the availability of a database containing validated reference spectra. The aim of this study was to evaluate the use of MALDI-TOF MS for the rapid and reliable identification and differentiation of B. pseudomallei and B. mallei and to build up a reliable reference database for both organisms. Results A collection of ten B. pseudomallei and seventeen B. mallei strains was used to generate a library of reference spectra. Samples of both species could be identified by MALDI-TOF MS, if a dedicated subset of the reference spectra library was used. In comparison with samples representing B. mallei, higher genetic diversity among B. pseudomallei was reflected in the higher average Eucledian distances between the mass spectra and a broader range of identification score values obtained with commercial software for the identification of microorganisms. The type strain of B. pseudomallei (ATCC 23343 was isolated decades ago and is outstanding in the spectrum-based dendrograms probably due to massive methylations as indicated by two intensive series of mass increments of 14 Da specifically and reproducibly found in the spectra of this strain. Conclusions Handling of pathogens under BSL 3 conditions is dangerous and cumbersome but can be minimized by inactivation of bacteria with ethanol, subsequent protein extraction under BSL 1 conditions and MALDI-TOF MS

  18. Rapid evaporative ionisation mass spectrometry of electrosurgical vapours for the identification of breast pathology: towards an intelligent knife for breast cancer surgery.

    Science.gov (United States)

    St John, Edward R; Balog, Julia; McKenzie, James S; Rossi, Merja; Covington, April; Muirhead, Laura; Bodai, Zsolt; Rosini, Francesca; Speller, Abigail V M; Shousha, Sami; Ramakrishnan, Rathi; Darzi, Ara; Takats, Zoltan; Leff, Daniel R

    2017-05-23

    Re-operation for positive resection margins following breast-conserving surgery occurs frequently (average = 20-25%), is cost-inefficient, and leads to physical and psychological morbidity. Current margin assessment techniques are slow and labour intensive. Rapid evaporative ionisation mass spectrometry (REIMS) rapidly identifies dissected tissues by determination of tissue structural lipid profiles through on-line chemical analysis of electrosurgical aerosol toward real-time margin assessment. Electrosurgical aerosol produced from ex-vivo and in-vivo breast samples was aspirated into a mass spectrometer (MS) using a monopolar hand-piece. Tissue identification results obtained by multivariate statistical analysis of MS data were validated by histopathology. Ex-vivo classification models were constructed from a mass spectral database of normal and tumour breast samples. Univariate and tandem MS analysis of significant peaks was conducted to identify biochemical differences between normal and cancerous tissues. An ex-vivo classification model was used in combination with bespoke recognition software, as an intelligent knife (iKnife), to predict the diagnosis for an ex-vivo validation set. Intraoperative REIMS data were acquired during breast surgery and time-synchronized to operative videos. A classification model using histologically validated spectral data acquired from 932 sampling points in normal tissue and 226 in tumour tissue provided 93.4% sensitivity and 94.9% specificity. Tandem MS identified 63 phospholipids and 6 triglyceride species responsible for 24 spectral differences between tissue types. iKnife recognition accuracy with 260 newly acquired fresh and frozen breast tissue specimens (normal n = 161, tumour n = 99) provided sensitivity of 90.9% and specificity of 98.8%. The ex-vivo and intra-operative method produced visually comparable high intensity spectra. iKnife interpretation of intra-operative electrosurgical vapours, including data

  19. Rapid Screening Technique To Identify Sudan Dyes (I to IV) in Adulterated Tomato Sauce, Chilli Powder, and Palm Oil by Innovative High-Resolution Mass Spectrometry.

    Science.gov (United States)

    Sciuto, Simona; Esposito, Giovanna; Dell'Atti, Luana; Guglielmetti, Chiara; Acutis, Pier Luigi; Martucci, Francesca

    2017-04-01

    Sudan dyes are synthetic azo dyes used by industry in a variety of applications. Classified as carcinogenic, they are not allowed in foodstuffs; however, their presence as adulterants in food products has been regularly reported. Here, we describe an innovative screening method to detect Sudan I, II, III, and IV in tomato sauce, palm oil, and chilli powder. The method entails minimal sample preparation, completely avoiding the liquid chromatography phase, followed by detection and identification through atmospheric pressure chemical ionization time-of-flight mass spectrometry, in positive ionization mode. Analytes were efficiently identified and detected in samples, fortified both with individual analytes and with their mixture, with an error in mass identification less than 5 ppm. Limits of identification of the analytes in the fortified samples were 0.5 to 1 mg/kg, depending on the dye and matrix. The method had a linear range of 0.05 to 5 mg/kg and good linear relationships (R2 > 0.98). Repeatability was satisfactory, with a coefficient of variation lower than 20%. The method was applied to detect the dyes in real adulterated chilli samples, previously found positive by confirmatory high-performance liquid chromatography-mass spectrometry and ELISA, and in commercial products purchased from supermarkets. In all positive samples, analytes were correctly identified with an error in mass identification lower than 5 ppm, while none of the 45 commercial samples analyzed were found to be contaminated. The proposed new assay is sensitive, with a limit of identification, for all the three matrices, complying with the limits defined by the European Union (0.5 to 1 mg/kg) for analytical methods. Compared with conventional methods, the new assay is rapid and inexpensive and characterized by a high throughput; thus, it could be suitable as screening technique to identify Sudan dyes in adulterated food products.

  20. Rapid Profiling of Bovine and Human Milk Gangliosides by Matrix-Assisted Laser Desorption/Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry.

    Science.gov (United States)

    Lee, Hyeyoung; An, Hyun Joo; Lerno, Larry A; German, J Bruce; Lebrilla, Carlito B

    2011-08-15

    Gangliosides are anionic glycosphingolipids widely distributed in vertebrate tissues and fluids. Their structural and quantitative expression patterns depend on phylogeny and are distinct down to the species level. In milk, gangliosides are exclusively associated with the milk fat globule membrane. They may participate in diverse biological processes but more specifically to host-pathogen interactions. However, due to the molecular complexities, the analysis needs extensive sample preparation, chromatographic separation, and even chemical reaction, which makes the process very complex and time-consuming. Here, we describe a rapid profiling method for bovine and human milk gangliosides employing matrix-assisted desorption/ionization (MALDI) Fourier transform ion cyclotron resonance (FTICR) mass spectrometry (MS). Prior to the analyses of biological samples, milk ganglioside standards GM3 and GD3 fractions were first analyzed in order to validate this method. High mass accuracy and high resolution obtained from MALDI FTICR MS allow for the confident assignment of chain length and degree of unsaturation of the ceramide. For the structural elucidation, tandem mass spectrometry (MS/MS), specifically as collision-induced dissociation (CID) and infrared multiphoton dissociation (IRMPD) were employed. Complex ganglioside mixtures from bovine and human milk were further analyzed with this method. The samples were prepared by two consecutive chloroform/methanol extraction and solid phase extraction. We observed a number of differences between bovine milk and human milk. The common gangliosides in bovine and human milk are NeuAc-NeuAc-Hex-Hex-Cer (GD3) and NeuAc-Hex-Hex-Cer (GM3); whereas, the ion intensities of ganglioside species are different between two milk samples. Kendrick mass defect plot yields grouping of ganglioside peaks according to their structural similarities. Gangliosides were further probed by tandem MS to confirm the compositional and structural assignments

  1. Rapid "breath-print" of liver cirrhosis by proton transfer reaction time-of-flight mass spectrometry. A pilot study.

    Directory of Open Access Journals (Sweden)

    Filomena Morisco

    Full Text Available UNLABELLED: The aim of the present work was to test the potential of Proton Transfer Reaction Time-of-Flight Mass Spectrometry (PTR-ToF-MS in the diagnosis of liver cirrhosis and the assessment of disease severity by direct analysis of exhaled breath. Twenty-six volunteers have been enrolled in this study: 12 patients (M/F 8/4, mean age 70.5 years, min-max 42-80 years with liver cirrhosis of different etiologies and at different severity of disease and 14 healthy subjects (M/F 5/9, mean age 52.3 years, min-max 35-77 years. Real time breath analysis was performed on fasting subjects using a buffered end-tidal on-line sampler directly coupled to a PTR-ToF-MS. Twelve volatile organic compounds (VOCs resulted significantly differently in cirrhotic patients (CP compared to healthy controls (CTRL: four ketones (2-butanone, 2- or 3- pentanone, C8-ketone, C9-ketone, two terpenes (monoterpene, monoterpene related, four sulphur or nitrogen compounds (sulfoxide-compound, S-compound, NS-compound, N-compound and two alcohols (heptadienol, methanol. Seven VOCs (2-butanone, C8-ketone, a monoterpene, 2,4-heptadienol and three compounds containing N, S or NS resulted significantly differently in compensate cirrhotic patients (Child-Pugh A; CP-A and decompensated cirrhotic subjects (Child-Pugh B+C; CP-B+C. ROC (Receiver Operating Characteristic analysis was performed considering three contrast groups: CP vs CTRL, CP-A vs CTRL and CP-A vs CP-B+C. In these comparisons monoterpene and N-compound showed the best diagnostic performance. CONCLUSIONS: Breath analysis by PTR-ToF-MS was able to distinguish cirrhotic patients from healthy subjects and to discriminate those with well compensated liver disease from those at more advanced severity stage. A breath-print of liver cirrhosis was assessed for the first time.

  2. Rapid characterisation and identification of compounds in Saposhnikoviae Radix by high-performance liquid chromatography coupled with electrospray ionisation quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Chen, Luxiao; Chen, Xiangyang; Su, Lei; Jiang, Yanyan; Liu, Bin

    2017-08-18

    Saposhnikoviae Radix (SR), the dried root of Saposhnikovia divaricata (Turcz.) Schischk. (Umbelliferae), is commonly used as a traditional Chinese medicine. In this study, a rapid and accurate method was firstly, developed for the qualitative analysis of SR by high-performance liquid chromatography coupled with electrospray ionisation quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF-MS/MS). A total of 45 compounds were identified or tentatively characterised, including 13 chromones, 28 coumarins and four others. Among them, 16 compounds were identified from SR for the first time. In addition, six chromones reference standards, including two isolated compounds of 3'-O-angeloylhamaudol and norcimifugin from the extraction of SR, were used to study the fragmentation pathways of chromones. The developed method was effective for characterising the compounds of SR, and the results of the study enriched the understanding of the chemical connotation.

  3. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after.......319 ± 0.004 g, n=5). The chemical yields of plutonium were averagely better than 90% under the optimal experimental conditions and the entire analytical procedure could be accomplished within a short timeframe (

  4. Rapid determination of the binding affinity and specificity of the mushroom Polyporus squamosus lectin using frontal affinity chromatography coupled to electrospray mass spectrometry.

    Science.gov (United States)

    Zhang, B; Palcic, M M; Mo, H; Goldstein, I J; Hindsgaul, O

    2001-02-01

    The binding affinity and specificity of the mushroom Polyporus squamosus lectin has been determined by the recently developed method of frontal affinity chromatography coupled to electrospray mass spectrometry (FAC/MS). A micro-scale affinity column was prepared by immobilizing the lectin ( approximately 25 microg) onto porous glass beads in a tubing column (9.8 microl column volume). The column was then used to screen several oligosaccharide mixtures. The dissociation constants of 22 sialylated or sulfated oligosaccharides were evaluated against the immobilized lectin. The lectin was found to be highly specific for Neu5Acalpha2-6Galbeta1-4Glc/GlcNAc containing oligosaccharides with K(d) values near 10 microM. The FAC/MS assay permits the rapid determination of the dissociation constants of ligands as well as a higher throughput screening of compound mixtures, making it a valuable tool for affinity studies, especially for testing large numbers of compounds.

  5. Rapid development of sensitive, high-throughput, quantitative and highly selective mass spectrometric targeted immunoassays for clinically important proteins in human plasma and serum

    Science.gov (United States)

    Krastins, Bryan; Prakash, Amol; Sarracino, David A.; Nedelkov, Dobrin; Niederkofler, Eric E.; Kiernan, Urban A.; Nelson, Randall; Vogelsang, Maryann S.; Vadali, Gouri; Garces, Alejandra; Sutton, Jennifer N.; Peterman, Scott; Byram, Gregory; Darbouret, Bruno; Pérusse, Joëlle R.; Seidah, Nabil G.; Coulombe, Benoit; Gobom, Johan; Portelius, Erik; Pannee, Josef; Blennow, Kaj; Kulasingam, Vathany; Couchman, Lewis; Moniz, Caje; Lopez, Mary F.

    2013-01-01

    Objectives The aim of this study was to develop high-throughput, quantitative and highly selective mass spectrometric, targeted immunoassays for clinically important proteins in human plasma or serum. Design and methods The described method coupled mass spectrometric immunoassay (MSIA), a previously developed technique for immunoenrichment on a monolithic microcolumn activated with an anti-protein antibody and fixed in a pipette tip, to selected reaction monitoring (SRM) detection and accurate quantification of targeted peptides, including clinically relevant sequence or truncated variants. Results In this report, we demonstrate the rapid development of MSIA-SRM assays for sixteen different target proteins spanning seven different clinically important areas (including neurological, Alzheimer's, cardiovascular, endocrine function, cancer and other diseases) and ranging in concentration from pg/mL to mg/mL. The reported MSIA-SRM assays demonstrated high sensitivity (within published clinical ranges), precision, robustness and high-throughput as well as specific detection of clinically relevant isoforms for many of the target proteins. Most of the assays were tested with bona-fide clinical samples. In addition, positive correlations, (R2 0.67–0.87, depending on the target peptide), were demonstrated for MSIA-SRM assay data with clinical analyzer measurements of parathyroid hormone (PTH) and insulin growth factor 1 (IGF1) in clinical sample cohorts. Conclusions We have presented a practical and scalable method for rapid development and deployment of MS-based SRM assays for clinically relevant proteins and measured levels of the target analytes in bona fide clinical samples. The method permits the specific quantification of individual protein isoforms and addresses the difficult problem of protein heterogeneity in clinical proteomics applications. PMID:23313081

  6. A novel tandem mass spectrometry method for rapid confirmation of medium- and very long-chain acyl-CoA dehydrogenase deficiency in newborns.

    Directory of Open Access Journals (Sweden)

    Frank ter Veld

    Full Text Available BACKGROUND: Newborn screening for medium- and very long-chain acyl-CoA dehydrogenase (MCAD and VLCAD, respectively deficiency, using acylcarnitine profiling with tandem mass spectrometry, has increased the number of patients with fatty acid oxidation disorders due to the identification of additional milder, and so far silent, phenotypes. However, especially for VLCADD, the acylcarnitine profile can not constitute the sole parameter in order to reliably confirm disease. Therefore, we developed a new liquid chromatography tandem mass spectrometry (LC-MS/MS method to rapidly determine both MCAD- and/or VLCAD-activity in human lymphocytes in order to confirm diagnosis. METHODOLOGY: LC-MS/MS was used to measure MCAD- or VLCAD-catalyzed production of enoyl-CoA and hydroxyacyl-CoA, in human lymphocytes. PRINCIPAL FINDINGS: VLCAD activity in controls was 6.95+/-0.42 mU/mg (range 1.95 to 11.91 mU/mg. Residual VLCAD activity of 4 patients with confirmed VLCAD-deficiency was between 0.3 and 1.1%. Heterozygous ACADVL mutation carriers showed residual VLCAD activities of 23.7 to 54.2%. MCAD activity in controls was 2.38+/-0.18 mU/mg. In total, 28 patients with suspected MCAD-deficiency were assayed. Nearly all patients with residual MCAD activities below 2.5% were homozygous 985A>G carriers. MCAD-deficient patients with one other than the 985A>G mutation had higher MCAD residual activities, ranging from 5.7 to 13.9%. All patients with the 199T>C mutation had residual activities above 10%. CONCLUSIONS: Our newly developed LC-MS/MS method is able to provide ample sensitivity to correctly and rapidly determine MCAD and VLCAD residual activity in human lymphocytes. Importantly, based on measured MCAD residual activities in correlation with genotype, new insights were obtained on the expected clinical phenotype.

  7. [Rapid screening of fipronil and its metabolites in egg and egg products by solid phase extraction-liquid chromatography-quadrupole time-of-flight mass spectrometry].

    Science.gov (United States)

    Guo, Dehua; Shi, Yiyin; Li, You; Yi, Xionghai; Deng, Xiaojun; Xiao, Wenqing; Wang, Jian; Li, Xiao; Liu, Han; Shen, Weijian

    2017-12-08

    A method for rapid screening of fipronil and its metabolites in egg and egg products was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF MS). The samples were extracted by acid-acetonitrile, cleaned up by PRiME HLB SPE. The separation was performed on a Poroshell 120 EC C18 column (150 mm×3 mm, 2.7 μm) with gradient elution using water and acetonitrile as mobile phases. The target compounds were monitored under negative ionization mode with electrospray ionization (ESI) source and two databases of accurate mass and fragment ions were created. The matrix effects in four kinds of egg and egg products were considered and the quantification was carried out by internal standard method. The results demonstrated that the linear ranges were from 0.1 to 5 μg/L with good correlation coefficients (r2>0.99). The limits of detection (LODs, S/N>3) and limits of quantitation (LOQs, S/N>10) were 0.2 μg/kg and 1 μg/kg, respectively. The recoveries of fipronil and its metabolites in different matrixes spiked with 1, 2 and 5 μg/kg varied from 82.6%-98.1%, and the relative standard deviations (RSDs) were between 3.8%-9.9% (n=6). The method can effectively correct the ionization suppression. It is sensitive, accurate and suitable for the rapid screening of fipronil, fipronil sulfide, fipronil sulfone and fipronil desulfinyl in egg, egg noodle, cake and mayonnaise.

  8. Rapid and High-Throughput Detection and Quantitation of Radiation Biomarkers in Human and Nonhuman Primates by Differential Mobility Spectrometry-Mass Spectrometry.

    Science.gov (United States)

    Chen, Zhidan; Coy, Stephen L; Pannkuk, Evan L; Laiakis, Evagelia C; Hall, Adam B; Fornace, Albert J; Vouros, Paul

    2016-10-01

    Radiation exposure is an important public health issue due to a range of accidental and intentional threats. Prompt and effective large-scale screening and appropriate use of medical countermeasures (MCM) to mitigate radiation injury requires rapid methods for determining the radiation dose. In a number of studies, metabolomics has identified small-molecule biomarkers responding to the radiation dose. Differential mobility spectrometry-mass spectrometry (DMS-MS) has been used for similar compounds for high-throughput small-molecule detection and quantitation. In this study, we show that DMS-MS can detect and quantify two radiation biomarkers, trimethyl-L-lysine (TML) and hypoxanthine. Hypoxanthine is a human and nonhuman primate (NHP) radiation biomarker and metabolic intermediate, whereas TML is a radiation biomarker in humans but not in NHP, which is involved in carnitine synthesis. They have been analyzed by DMS-MS from urine samples after a simple strong cation exchange-solid phase extraction (SCX-SPE). The dramatic suppression of background and chemical noise provided by DMS-MS results in an approximately 10-fold reduction in time, including sample pretreatment time, compared with liquid chromatography-mass spectrometry (LC-MS). DMS-MS quantitation accuracy has been verified by validation testing for each biomarker. Human samples are not yet available, but for hypoxanthine, selected NHP urine samples (pre- and 7-d-post 10 Gy exposure) were analyzed, resulting in a mean change in concentration essentially identical to that obtained by LC-MS (fold-change 2.76 versus 2.59). These results confirm the potential of DMS-MS for field or clinical first-level rapid screening for radiation exposure. Graphical Abstract ᅟ.

  9. A simple method for rapid microbial identification from positive monomicrobial blood culture bottles through matrix-assisted laser desorption ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Lin, Jung-Fu; Ge, Mao-Cheng; Liu, Tsui-Ping; Chang, Shih-Cheng; Lu, Jang-Jih

    2017-06-30

    Rapid identification of microbes in the bloodstream is crucial in managing septicemia because of its high disease severity, and direct identification from positive blood culture bottles through matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) can shorten the turnaround time. Therefore, we developed a simple method for rapid microbiological identification from positive blood cultures by using MALDI-TOF MS. We modified previously developed methods to propose a faster, simpler and more economical method, which includes centrifugation and hemolysis. Specifically, our method comprises two-stage centrifugation with gravitational acceleration (g) at 600g and 3000g, followed by the addition of a lysis buffer and another 3000g centrifugation. In total, 324 monomicrobial bacterial cultures were identified. The success rate of species identification was 81.8%, which is comparable with other complex methods. The identification success rate was the highest for Gram-negative aerobes (85%), followed by Gram-positive aerobes (78.2%) and anaerobes (67%). The proposed method requires less than 10 min, costs less than US$0.2 per usage, and facilitates batch processing. We conclude that this method is feasible for clinical use in microbiology laboratories, and can serve as a reference for treatments or further complementary diagnostic testing. Copyright © 2017. Published by Elsevier B.V.

  10. Rapid identification of Enterobacteriaceae in milk and dairy products with the Matrix-Assisted Laser Desorption Ionization–Time of Flight Mass Spectrometry (MALDI-TOF MS

    Directory of Open Access Journals (Sweden)

    Miroslava Kačániová

    2017-11-01

    Full Text Available Identification of microorganisms by MALDI-TOF MS Biotyper has been demonstrated to be accurate, rapid and lower cost than conventional food investigation methods. Rapid identification of pathogenic and spoilage microorganisms is crucial for dairy industry to ensure the quality and safety of milk and milk products. In this study, the bacterial species representing the Enterobacteriaceae family were identified in raw milk and milk products using the MALDI-TOF MS mass spectrometry. Altogether, 20 samples of Slovak milk and milk products were examined. Samples were cultured on VRBG agar at 37 °C for 24-48 h. Typical bacterial colonies were selected for identification with MALDI-TOF MS Biotyper. Escherichia coli and Enterobacter sp. were the most abundant  Enterobacteriaceae family representatives identified. E. coli was found in nine  and Enterobacter sp. in eight samples. Enterobacter sp. comprised 49 % and Escherichia coli 23 % of all bacterial isolates. The study shows that MALDI-TOF MS Biotyper was reliable identification method of Enterobacteriaceae in milk and dairy products. This method was helpful in evaluation of bacterial contamination of milk.

  11. Rapid determination of yunaconitine and related alkaloids in aconites and aconite-containing drugs by ultra high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Song, Long; Zhang, Hong; Liu, Xin; Zhao, Zhi-Li; Chen, Shi-Lin; Wang, Zheng-Tao; Xu, Hong-Xi

    2012-12-01

    Yunaconitine (YAC) is a toxic aconite alkaloid that is considered to be a hidden aconite poison since it is frequently found in body fluids from aconite poisoning patients, but has not been well studied in commonly used herbal drugs. In this paper, a rapid and sensitive ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) detection combined with microwave-assisted extraction (MAE) was developed for high throughput simultaneous determination of YAC and six other toxic aconite alkaloids in 31 samples of crude, processed aconites and aconite-containing drugs. The optimized method showed excellent linearity, precision, accuracy and recovery for all target compounds with short run time. YAC was detected in some samples with contents from 0.015 to 10.41 mg/g. This is the first report on the determination of YAC in Radix Aconiti, Radix Aconiti Kusnezoffii and aconite-containing drugs. This newly developed method facilitates the rapid screening of YAC and related toxic aconite alkaloids and allows YAC to be used as a chemical marker for the quality control of aconites and aconite-containing drugs. Copyright © 2012 John Wiley & Sons, Ltd.

  12. Rapid detection by direct analysis in real time-mass spectrometry (DART-MS) of psychoactive plant drugs of abuse: the case of Mitragyna speciosa aka "Kratom".

    Science.gov (United States)

    Lesiak, Ashton D; Cody, Robert B; Dane, A John; Musah, Rabi A

    2014-09-01

    Mitragyna speciosa, also known commonly as "Kratom" or "Ketum", is a plant with psychoactive properties that have been attributed to the presence of various indole alkaloids such as mitragynine and 7-hydroxymitragynine. M. speciosa use is gaining popularity internationally as a natural and legal alternative to narcotics. As a drug of abuse, its detection and identification are not straightforward, since M. speciosa plant material is not particularly distinctive. Here, we show that direct analysis in real time-mass spectrometry (DART-MS) can be used not only to rapidly identify M. speciosa plant material and distinguish it from other plants, but also to distinguish between M. speciosa plant varieties, based on differences between their chemical profiles. The method is rapid and the analysis expeditious. Plant material such as that found at a crime scene can be analyzed directly with no sample pre-preparation steps. Furthermore, we show that the basis set of principal components that permit characterization of the plant material can be used to positively identify M. speciosa. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  13. Rapid speciation of iron by on-line coupling of short column capillary electrophoresis and inductively coupled plasma mass spectrometry with the collision cell technique.

    Science.gov (United States)

    Li, Bao-Hui; Yan, Xiu-Ping

    2007-04-01

    A method for rapid speciation analysis of iron was developed by on-line coupling of short column capillary electrophoresis and inductively coupled plasma mass spectrometry. The collision cell technique was used to eliminate argon-based polyatomic interferences and a Micromist nebulizer was employed to increase the nebulization efficiency. Rapid speciation analysis of Fe(II) and Fe(III) was achieved within 1 min by short column capillary electrophoresis in a 14 cm x 50 microm id capillary at 28 kV voltage with a mixture of 15 mmol/L tris(hydroxymethyl)aminomethane + 1 mmol/L 1,10-phenanthroline + 1 mmol/L EDTA (pH 8.6) as running electrolyte. The precisions (RSD, n = 5) of migration time and peak area for Fe(II) and Fe(III) were in the range of 1.0 - 2.6 and 1.9 - 3.9%, respectively. The limits of detection (3sigma) of Fe(II) and Fe(III) were 10.0 and 8.3 microg/L, respectively.

  14. Rapid determination of 4-aminobutyric acid and L-glutamic acid in biological decarboxylation process by capillary electrophoresis-mass spectrometry.

    Science.gov (United States)

    Takeda, Sahori; Yamano, Naoko; Kawasaki, Norioki; Ando, Hisanori; Nakayama, Atsuyoshi

    2012-01-01

    4-Aminobutylic acid (GABA) is a monomer of plastic polyamide 4. Bio-based polyamide 4 can be produced by using GABA obtained from biomass. The production of L-glutamic acid (Glu) from biomass has been established. GABA is produced by decarboxylation of Glu in biological process. High-performance liquid chromatography (HPLC) with derivatization is generally used to determine the concentration of GABA and Glu in reacted solution samples for the efficient production of GABA. In this study, we have investigated the rapid determination of GABA and Glu by capillary electrophoresis-mass spectrometry (CE-MS) without derivatization. The determination was achieved with the use of a shortened capillary, a new internal standard for GABA, and optimization of sheath liquid composition. Determined concentrations of GABA and Glu by CE-MS were compared with those by pre-column derivatization HPLC with phenylisothiocyanate. The determined values by CE-MS were close to those by HPLC with pre-column derivatization. These results suggest that the determination of GABA and Glu in reacted solution is rapid and simplified by the use of CE-MS. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Rapid identification of clinical mycobacterial isolates by protein profiling using matrix assisted laser desorption ionization-time of flight mass spectrometry.

    Science.gov (United States)

    Panda, A; Kurapati, S; Samantaray, J C; Myneedu, V P; Verma, A; Srinivasan, A; Ahmad, H; Behera, D; Singh, U B

    2013-01-01

    The purpose of this study was to evaluate the identification of Mycobacterium tuberculosis which is often plagued with ambiguity. It is a time consuming process requiring 4-8 weeks after culture positivity, thereby delaying therapeutic intervention. For a successful treatment and disease management, timely diagnosis is imperative. We evaluated a rapid, proteomic based technique for identification of clinical mycobacterial isolates by protein profiling using matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). Freshly grown mycobacterial isolates were used. Acetonitrile/trifluoroacetic acid extraction procedure was carried out, following which cinnamic acid charged plates were subjected to identification by MALDI-TOF MS. A comparative analysis of 42 clinical mycobacterial isolates using the MALDI-TOF MS and conventional techniques was carried out. Among these, 97.61% were found to corroborate with the standard methods at genus level and 85.36% were accurate till the species level. One out of 42 was not in accord with the conventional assays because MALDI-TOF MS established it as Mycobacterium tuberculosis (log (score)>2.0) and conventional methods established it to be non-tuberculous Mycobacterium. MALDI-TOF MS was found to be an accurate, rapid, cost effective and robust system for identification of mycobacterial species. This innovative approach holds promise for early therapeutic intervention leading to better patient care.

  16. Assessing direct analysis in real-time-mass spectrometry (DART-MS) for the rapid identification of additives in food packaging.

    Science.gov (United States)

    Ackerman, L K; Noonan, G O; Begley, T H

    2009-12-01

    The ambient ionization technique direct analysis in real time (DART) was characterized and evaluated for the screening of food packaging for the presence of packaging additives using a benchtop mass spectrometer (MS). Approximate optimum conditions were determined for 13 common food-packaging additives, including plasticizers, anti-oxidants, colorants, grease-proofers, and ultraviolet light stabilizers. Method sensitivity and linearity were evaluated using solutions and characterized polymer samples. Additionally, the response of a model additive (di-ethyl-hexyl-phthalate) was examined across a range of sample positions, DART, and MS conditions (temperature, voltage and helium flow). Under optimal conditions, molecular ion (M+H+) was the major ion for most additives. Additive responses were highly sensitive to sample and DART source orientation, as well as to DART flow rates, temperatures, and MS inlet voltages, respectively. DART-MS response was neither consistently linear nor quantitative in this setting, and sensitivity varied by additive. All additives studied were rapidly identified in multiple food-packaging materials by DART-MS/MS, suggesting this technique can be used to screen food packaging rapidly. However, method sensitivity and quantitation requires further study and improvement.

  17. Rapid screening and quantification of residual pesticides and illegal adulterants in red wine by direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Guo, Tianyang; Fang, Pingping; Jiang, Juanjuan; Zhang, Feng; Yong, Wei; Liu, Jiahui; Dong, Yiyang

    2016-11-04

    A rapid method to screen and quantify multi-class analytic targets in red wine has been developed by direct analysis in real time (DART) coupled with triple quadruple tandem mass spectrometry (QqQ-MS). A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for increasing analytical speed and reducing matrix effect, and the multiple reaction monitoring (MRM) in DART-MS/MS ensured accurate analysis. One bottle of wine containing 50 pesticides and 12 adulterants, i.e., preservatives, antioxidant, sweeteners, and azo dyes, could be totally determined less than 12min. This method exhibited proper linearity (R2≥0.99) in the range of 1-1000ng/mL for pesticides and 10-5000ng/mL for adulterants. The limits of detection (LODs) were obtained in a 0.5-50ng/mL range for pesticides and 5-50ng/mL range for adulterants, and the limits of quantification (LOQs) were in a 1-100ng/mL range for pesticides and 10-250ng/mL range for adulterants. Three spiked levels for each analyte in wine were evaluated, and the recoveries were in a scope of 75-120%. The results demonstrated DART-MS/MS was a rapid and simple method, and could be applied to rapid analyze residual pesticides and illegal adulterants in a large quantities of red wine. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Propriété, biens publics mondiaux, bien(s commun(s : Une lecture des concepts économiques

    Directory of Open Access Journals (Sweden)

    Jérôme Ballet

    2008-03-01

    Full Text Available La notion de bien public mondial s’est développée ces dernières années. Elle renvoie à un dépassement ambigu de la notion usuelle dans la théorie économique de bien public. A cette occasion elle ouvre le débat sur l’équité en complément de l’efficience. De ce fait, la confrontation de cette nouvelle notion avec l’analyse de l’efficience des régimes de propriété s’impose. Par ailleurs, la confrontation avec la notion de bien commun, notion elle aussi en développement, éclaire l’enjeu autour de l’équité.Property, Global Public Goods, Common Good(s : A Lecture. The concept of global public good emerged these last years. It proposes, in an ambiguous way, to go beyond the usual concept of public good. Then, added to usual questions on efficiency, the debate on fairness becomes a stake. Confrontation with analysis on property rights command attention, Furthermore, confrontation with the concept of common good, also a developing concept, highlight stake around fairness.

  19. Principle component analysis combined with matrix-assisted laser desorption ionization mass spectrometry for rapid diagnosing the sera of patients with major depression.

    Science.gov (United States)

    Huang, Tiao-Lai; Cho, Yi-Tzu; Su, Hong; Shiea, Jentaie

    2013-09-23

    Previously, we demonstrated that 6M HCl hydrolysis followed by matrix-assisted laser desorption/ionization (MALDI-TOF) mass spectrometry is a useful technique to detect potential protein biomarkers in the sera collected from major depression (MD) patients and from healthy controls. In this study, the effects of various organic acids in hydrolyzing proteins in serum were first examined. The organic matrixes commonly used in MALDI analysis were also examined for characterizing the hydrolyzed peptides. Finally, principle component analysis (PCA) was used to analyze the MALDI mass spectra of acid-hydrolyzed serum samples. It was found that 20% TFA and sinapinic acid were the optimal reagents for hydrolysis and MALDI matrix. Samples collected from MD patients and healthy controls were readily classified through PCA analysis. A receiver operating characteristic (ROC) curve based on the ratio of the intensities of the two fragment ions (m/z 8606 and 9287) indicated by PCA plot was also constructed. The area under the curve was 0.845; the sensitivity and specificity were both 80%. An analytical platform employing trifluoroacetic acid to hydrolyze serum proteins followed by MALDI-TOF/MS and PCA analysis was developed to rapidly differentiate the sera between MD patients and healthy controls. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Rapid Spread of Zika Virus in The Americas - Implications for Public Health Preparedness for Mass Gatherings at the 2016 Brazil Olympic Games

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    Eskild Petersen

    2016-03-01

    Full Text Available Mass gatherings at major international sporting events put millions of international travelers and local host-country residents at risk of acquiring infectious diseases, including locally endemic infectious diseases. The mosquito-borne Zika virus (ZIKV has recently aroused global attention due to its rapid spread since its first detection in May 2015 in Brazil to 22 other countries and other territories in the Americas. The ZIKV outbreak in Brazil, has also been associated with a significant rise in the number of babies born with microcephaly and neurological disorders, and has been declared a ‘Global Emergency by the World Health Organization. This explosive spread of ZIKV in Brazil poses challenges for public health preparedness and surveillance for the Olympics and Paralympics which are due to be held in Rio De Janeiro in August, 2016. We review the epidemiology and clinical features of the current ZIKV outbreak in Brazil, highlight knowledge gaps, and review the public health implications of the current ZIKV outbreak in the Americas. We highlight the urgent need for a coordinated collaborative response for prevention and spread of infectious diseases with epidemic potential at mass gatherings events.

  1. A rapid and sensitive liquid chromatography–tandem mass spectrometric method for the determination of hederasaponin B in rat plasma: Application to a pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Jiaxin Liu

    2017-07-01

    Full Text Available A rapid, simple and sensitive ultra-high performance liquid chromatography–tandem mass spectrometric (UPLC–MS/MS method was developed and validated for the determination of hederasaponin B, an active triterpenoid saponin widely existed in Hedera helix L. Plasma samples were processed by protein precipitation with acetonitrile and separated on a Thermo Hypersil GOLD C18 (2.1 mm × 50 mm,1.9 µm at flow rate of 0.3 ml/min, with a gradient elution consisting of acetonitrile and water containing 0.1% (v/v formic acid at 30 °C and detected by electrospray ionization mass spectrometry in the positive multiple reaction monitoring (MRM mode. The linearity was found to be within the concentration range of 0.5–5000 ng/ml with a lower limit of quantification of 0.5 ng/ml. The absolute oral bioavailability of hederasaponin B was 0.24 ± 0.49%. This indicated that the concentration-time course of the hederasaponin B existed a double-peak phenomenon. This method was further applied to the determination of hederasaponin B in rat plasma and showed good practicability, for the first time, after intragastric (25 mg/kg and intravenous (2 mg/kg administration in rats.

  2. Rapid determination of amino acids in fruits of Ziziphus jujuba by hydrophilic interaction ultra-high-performance liquid chromatography coupled with triple-quadrupole mass spectrometry.

    Science.gov (United States)

    Guo, Sheng; Duan, Jin-ao; Qian, Dawei; Tang, Yuping; Qian, Yefei; Wu, Dawei; Su, Shulan; Shang, Erxin

    2013-03-20

    In this study, a sensitive and rapid method for the simultaneous determination of free amino acids without derivatization using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry (HILIC-MS/MS) was developed. The method was performed on an ultra-high-performance liquid chromatography (UHPLC) separation system coupled with a triple-quadrupole mass spectrometry (TQ-MS) instrument. Sufficient separation of 23 underivatized amino acids was achieved on an Acquity BEH Amide column (2.1 mm × 100 mm, 1.7 μm) in a single run of 12 min. Then the method was applied for the analysis of the free amino acids in 46 batches of Ziziphus jujuba fruits which comprised 39 cultivars from 26 cultivation regions. Multivariate statistical analysis was also used to investigate the differences in free amino acid profiles among the samples. This study showed that HILIC-UHPLC-TQ-MS is an effective technique to analyze underivatized amino acids in the food samples.

  3. Development of a rapid screening method to determine primary aromatic amines in kitchen utensils using direct analysis in real time mass spectrometry (DART-MS).

    Science.gov (United States)

    Paseiro-Cerrato, R; Noonan, G O; Begley, T H

    2014-01-01

    Primary aromatic amines (PAAs) are a group of substances with undesirable health effects, that are used in a variety of commercial products. Several recent studies, using a number of screening and confirmatory methods, have reported the migration of PAAs from some kitchen utensils into acetic acid 3% (w/v). Many of these methods require significant sample preparation, therefore the aim of this work was to determine if direct analysis in real time mass spectrometry (DART-MS) could be utilised as a rapid screening tool for the determination of PAAs in kitchen utensils. DART-MS results from direct analysis of the utensil have been compared with results of PAA migration by ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method. The UPLC-MS/MS method had excellent linearity, appropriate sensitivity (LOD ≤ 1.5 µg L(-1); LOQ ≤ 4.5 µg L(-1)), repeatability from 2.4 to 13.2% and acceptable recoveries. DART-MS results were in good agreement with UPLC-MS/MS data, with 100% of non-compliant (PAA positive) samples successfully identified by DART-MS.

  4. An integrated strategy for rapid discovery and identification of the sequential piperine metabolites in rats using ultra high-performance liquid chromatography/high resolution mass spectrometery.

    Science.gov (United States)

    Shang, Zhanpeng; Cai, Wei; Cao, Yanfeng; Wang, Fei; Wang, Zhibin; Lu, Jianqiu; Zhang, Jiayu

    2017-11-30

    Piperine, one of the major bioactive constituents isolated from natural flavorings and medicinal-culinary herbs, possesses various biological activities. In the present study, an integrated strategy based on ultra high-performance liquid chromatography/high resolution mass spectrometry was established to reveal piperine metabolism in rats. First of all, post-acquisition data-mining methods, including high resolution extracted ion chromatograms (HREICs) and multiple mass defect filtering (MMDF), were used to screen piperine metabolite candidates in a full-scan HRMS(1) level. Then, parent ion list-dynamic exclusion coupled with data-dependent data-acquisition method was utilized to acquire MS(n) datasets. In addition, the established reverse molecular assembly (RMA) approach based on paired diagnostic product ions (pDPIs) coupled with neutral loss fragments (NLFs) was used to ascertain and identify the major-to-trace piperine metabolites efficiently. And then, the calculated ClogP values were utilized to distinguish the positional isomers. As a result, a total of 148 piperine metabolites were detected and characterized tentatively. The results demonstrated that piperine mainly underwent hydrogenation, dehydrogenation, hydroxylation, glucuronide conjugation, sulfate conjugation, ring-cleavage, and their composite reactions. Our results not only provided novel and useful data to better understand the safety, toxicity and efficacy of this potential therapeutic agent, but also indicated that the proposed strategy was reliable for a rapid discovery and identification drug-related constituents in vivo. Copyright © 2017. Published by Elsevier B.V.

  5. A differential mobility spectrometry/mass spectrometry platform for the rapid detection and quantitation of DNA adduct dG-ABP.

    Science.gov (United States)

    Kafle, Amol; Klaene, Joshua; Hall, Adam B; Glick, James; Coy, Stephen L; Vouros, Paul

    2013-07-15

    There is continued interest in exploring new analytical technologies for the detection and quantitation of DNA adducts, biomarkers which provide direct evidence of exposure and genetic damage in cells. With the goal of reducing clean-up steps and improving sample throughput, a Differential Mobility Spectrometry/Mass Spectrometry (DMS/MS) platform has been introduced for adduct analysis. A DMS/MS platform has been utilized for the analysis of dG-ABP, the deoxyguanosine adduct of the bladder carcinogen 4-aminobiphenyl (4-ABP). After optimization of the DMS parameters, each sample was analyzed in just 30 s following a simple protein precipitation step of the digested DNA. A detection limit of one modification in 10^6 nucleosides has been achieved using only 2 µg of DNA. A brief comparison (quantitative and qualitative) with liquid chromatography/mass spectrometry is also presented highlighting the advantages of using the DMS/MS method as a high-throughput platform. The data presented demonstrate the successful application of a DMS/MS/MS platform for the rapid quantitation of DNA adducts using, as a model analyte, the deoxyguanosine adduct of the bladder carcinogen 4-aminobiphenyl. Copyright © 2013 John Wiley & Sons, Ltd.

  6. Rapid separation and identification of phenolics in crude red grape skin extracts by high performance liquid chromatography coupled to diode array detection and tandem mass spectrometry.

    Science.gov (United States)

    Ji, Mei; Li, Chen; Li, Qiang

    2015-10-02

    A rapid and efficient method was established for the simultaneous determination of structures and configurations for 45 phenolics isolated from crude red grape skin extracts without extensive sample preparation. Separation and compound assignments were achieved using high performance liquid chromatography coupled to diode array detection and tandem mass spectrometry (HPLC-DAD-MS(2)). A Poroshell 120 EC-C18 (100mm×3.0mm, 2.7μm) column was employed to separate the phenolics, which were eluted using a gradient of acetonitrile and water acidified with 0.2% formic acid. Phenolics were identified by comparison of their UV-vis spectra, mass spectra and MS(2) data with those in the literature. Using this procedure, five compounds were detected for the first time in Vitis amurensis. Good separation of most phenolics was achieved in 26min. The methods described here can be used for the characterization of phenolics in a variety of grapes and grape products. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Rapid comprehensive amino acid analysis by liquid chromatography/tandem mass spectrometry: comparison to cation exchange with post-column ninhydrin detection.

    Science.gov (United States)

    Dietzen, Dennis J; Weindel, Annette L; Carayannopoulos, Mary O; Landt, Michael; Normansell, Ellen T; Reimschisel, Tyler E; Smith, Carl H

    2008-11-01

    Ion-exchange chromatography with ninhydrin detection remains the gold standard for detecting inborn errors of amino acid catabolism and transport. Disadvantages of such analysis include long chromatography times and interference from other ninhydrin-positive compounds. The aim of this project was to develop a more rapid and specific technique using liquid chromatography/tandem mass spectrometry (LC/MS/MS). Optimal fragmentation patterns for 32 amino acids were determined on a triple quadrupole mass spectrometer following butylation. Chromatographic characteristics of each of the amino acids were determined using C8 reversed-phase chromatography with 20% acetonitrile/0.1% formic acid as isocratic mobile phase. Quantitation using eleven deuterated internal standards was compared to cation exchange and ninhydrin detection on a Beckman 7300 system. Following methanol extraction and butylation, determination of 32 amino acids required 20 min. The dynamic range of each amino acid was generally 1-1000 micromol/L. Imprecision ranged from 7 to 23% (CV) over 6 months and recovery ranged from 88-125%. Deming regression with the Beckman 7300 yielded slopes from 0.4-1.2, intercepts from -21 to 65 micromol/L, correlation coefficients from 0.84-0.99 and Syx from 2-125 micromol/L. Isobaric amino acids were separated by chromatography (e.g. leucine, isoleucine) or by unique fragmentation (e.g., alanine, beta-alanine). LC/MS/MS is comparable to traditional LC-ninhydrin detection. Mass spectral detection shortens analysis times and reduces potential for interference in detecting inborn metabolic errors.

  8. Rapid screening and identification of chemical hazards in surface and drinking water using high resolution mass spectrometry and a case-control filter.

    Science.gov (United States)

    Kaserzon, Sarit L; Heffernan, Amy L; Thompson, Kristie; Mueller, Jochen F; Gomez Ramos, Maria Jose

    2017-09-01

    Access to clean, safe drinking water poses a serious challenge to regulators, and requires analytical strategies capable of rapid screening and identification of potentially hazardous chemicals, specifically in situations when threats to water quality or security require rapid investigations and potential response. This study describes a fast and efficient chemical hazard screening strategy for characterising trace levels of polar organic contaminants in water matrices, based on liquid chromatography high resolution mass spectrometry with post-acquisition 'case-control' data processing. This method allowed for a rapid response time of less than 24 h for the screening of target, suspect and non-target unknown chemicals via direct injection analysis, and a second, more sensitive analysis option requiring sample pre-concentration. The method was validated by fortifying samples with a range of pesticides, pharmaceuticals and personal care products (n = 46); with >90% of target compounds positively screened in samples at 1 ng mL-1, and 46% at 0.1 ng mL-1 when analysed via direct injection. To simulate a contamination event samples were fortified with compounds not present in the commercial library (designated 'non-target compounds'; fipronil and fenitrothion), tentatively identified at 0.2 and 1 ng mL-1, respectively; and a compound not included in any known commercial library or public database (designated 'unknown' compounds; 8Cl- perfluorooctanesulfonic acid), at 0.8 ng mL-1. The method was applied to two 'real-case' scenarios: (1) the assessment of drinking water safety during a high-profile event in Brisbane, Australia; and (2) to screen treated, re-circulated drinking water and pre-treated (raw) water. The validated workflow was effective for rapid prioritisation and screening of suspect and non-target potential hazards at trace levels, and could be applied to a wide range of matrices and investigations where comparison of organic contaminants between

  9. Rapid measurement of 8-oxo-7,8-dihydro-2'-deoxyguanosine in human biological matrices using ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lam, Patricia M W; Mistry, Vilas; Marczylo, Timothy H; Konje, Justin C; Evans, Mark D; Cooke, Marcus S

    2012-05-15

    Interaction of reactive oxygen species with DNA results in a variety of modifications, including 8-oxo-7,8-dihydro-2'-deoxyguanosine (8-oxodG), which has been extensively studied as a biomarker of oxidative stress. Oxidative stress is implicated in a number of pathophysiological processes relevant to obstetrics and gynecology; however, there is a lack of understanding as to the precise role of oxidative stress in these processes. We aimed to develop a rapid, validated assay for the accurate quantification of 8-oxodG in human urine using solid-phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and then investigate the levels of 8-oxodG in several fluids of interest to obstetrics and gynecology. Using UHPLC-MS/MS, 8-oxodG eluted after 3.94 min with an RSD for 15 injections of 0.07%. The method was linear between 0.95 and 95 nmol/L with LOD and LOQ of 5 and 25 fmol on-column, respectively. Accuracy and precision were 98.7-101.0 and seminal plasma>amniotic fluid>plasma>serum>peritoneal fluid, and it was not detected in saliva. Urine concentrations normalized to creatinine (n=15) ranged between 0.55 and 1.95 pmol/μmol creatinine. We describe, for the first time, 8-oxodG concentrations in human seminal plasma, peritoneal fluid, amniotic fluid, and breast milk, as well as in urine, plasma, and serum, using a rapid UHPLC-MS/MS method that will further facilitate biomonitoring of oxidative stress. Copyright © 2012 Elsevier Inc. All rights reserved.

  10. Identification by mass spectrometry and automated susceptibility testing from positive bottles: a simple, rapid, and standardized approach to reduce the turnaround time in the management of blood cultures.

    Science.gov (United States)

    Mauri, Carola; Principe, Luigi; Bracco, Silvia; Meroni, Elisa; Corbo, Nicoletta; Pini, Beatrice; Luzzaro, Francesco

    2017-12-06

    Speeding up identification and antimicrobial susceptibility testing (AST) is of foremost importance in the management of blood cultures. Here, we describe a simple, rapid, and standardized approach based on a very short-term incubation on solid medium from positive blood cultures followed by MALDI-TOF mass spectrometry identification and automated AST. The aim of the study was to evaluate the impact in the laboratory practice of this new procedure with respect to that previously used (standard method) by comparing TAT and cumulative percentage of final reports to clinicians. Compared with the standard method, the new procedure gave correct organism identification at genus or species level in 98.4% of monomicrobial samples. AST resulted in 97.7% essential agreement and 98.1% categorical agreement, with 0.9% minor errors, 1.0% major error, and 1.5% very major errors. The mean turnaround time to identification and AST was 61.4 h by using the new method compared to 83.1 h by using standard procedure. Concerning cumulative percentages of final reports, approximately a third of results were available at 48 h from the check-in of the sample when using the new procedure, whereas no final reports were ready at the same time with the standard method. The new procedure allows faster and reliable results using a simple and standardized approach. Thus, it represents an important tool for a more rapid management of blood cultures when molecular methods are not available in the laboratory.

  11. Validation and comparison of a rapid liquid chromatography tandem mass spectrometry method for serum 25OHD with the efficiency of separating 3-epi 25OHD3.

    Science.gov (United States)

    Yu, Songlin; Zhou, Weiyan; Zhang, Ruiping; Cheng, Xinqi; Fang, Huiling; Han, Jianhua; Cheng, Qian; Su, Wei; Qiu, Ling

    2016-09-01

    To develop a rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method with ability to separate 3-epi 25OHD3 (EPI-LC-MS/MS) from 25OHD3, and evaluate the effects of 3-epi 25OHD3 on routine LC-MS/MS that cannot separate 3-epi 25OHD3 (NEPI-LC-MS/MS). Performance of the newly built EPI-LC-MS/MS was validated, and 982 samples were analyzed and compared by the two methods. Both methods showed a linearity coefficient correlation exceeding 0.999 in the 6.25-500nmol/L range for 25OHD2 and 25OHD3. Moreover, they showed a between run coefficient variation (CV) and total CV of epi 25OHD3. Comparison of the 25OHD results obtained by the two methods for 982 patients (age 1-100years) revealed excellent clinical agreement (Cohen's kappa=0.875) and correlation (R2=0.973). Among the 982patients, only 73patients had 3-epi 25OHD3 (>6.25nmol/L); out of these 73patients, the 3-epi 25OHD3 level in 58patients was between 6.25 and 12.5nmol/L. In patients with epi 25OHD3 levels exceeding 12.5nmol/L (range: 13.3 - 27.5nmol/L). Among samples containing 3-epi 25OHD3, only three were separated into different 25OHD-deficiency groups using the above methods. A rapid and precise EPI-LC-MS/MS method for measuring 25OHD with efficient separation of 3-epi 25OHD3 was developed. Our results showed that 3-epi 25OHD3 had little effect on the routinely used NEPI-LC-MS/MS. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  12. Sequential determination of fat- and water-soluble vitamins in Rhodiola imbricata root from trans-Himalaya with rapid resolution liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Tayade, Amol B; Dhar, Priyanka; Kumar, Jatinder; Sharma, Manu; Chaurasia, Om P; Srivastava, Ravi B

    2013-07-30

    A rapid method was developed to determine both types of vitamins in Rhodiola imbricata root for the accurate quantification of free vitamin forms. Rapid resolution liquid chromatography/tandem mass spectrometry (RRLC-MS/MS) with electrospray ionization (ESI) source operating in multiple reactions monitoring (MRM) mode was optimized for the sequential analysis of nine water-soluble vitamins (B1, B2, two B3 vitamins, B5, B6, B7, B9, and B12) and six fat-soluble vitamins (A, E, D2, D3, K1, and K2). Both types of vitamins were separated by ion-suppression reversed-phase liquid chromatography with gradient elution within 30 min and detected in positive ion mode. Deviations in the intra- and inter-day precision were always below 0.6% and 0.3% for recoveries and retention time. Intra- and inter-day relative standard deviation (RSD) values of retention time for water- and fat-soluble vitamin were ranged between 0.02-0.20% and 0.01-0.15%, respectively. The mean recoveries were ranged between 88.95 and 107.07%. Sensitivity and specificity of this method allowed the limits of detection (LOD) and limits of quantitation (LOQ) of the analytes at ppb levels. The linear range was achieved for fat- and water-soluble vitamins at 100-1000 ppb and 10-100 ppb. Vitamin B-complex and vitamin E were detected as the principle vitamins in the root of this adaptogen which would be of great interest to develop novel foods from the Indian trans-Himalaya. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Matrix-assisted laser desorption/ionisation-time of flight mass spectrometry: rapid identification of bacteria isolated from patients with cystic fibrosis.

    Science.gov (United States)

    Baillie, S; Ireland, K; Warwick, S; Wareham, D; Wilks, M

    2013-01-01

    Despite extensive research into the diagnosis and management of cystic fibrosis (CF) over the past decades, sufferers still have a median life expectancy of less than 37 years. Respiratory tract infections have a significant role in increasing the morbidity and mortality of patients with CF via a progressive decline in lung function. Rapid identification of organisms recovered from CF sputum is necessary for effective management of respiratory tract infections; however, standard techniques of identification are slow, technically demanding and expensive. The aim of this study is to asses the suitability of matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF MS) in identifying bacteria isolated from the respiratory tract of patients with CF, and is assessed by testing the accuracy of MALDI-TOF MS in identifying samples from a reference collection of rare CF strains in conjunction with comparing MALDI-TOF MS and standard techniques in identifying clinical isolates from sputum samples of CF patients. MALDI-TOF MS accurately identified 100% of isolates from the reference collection of rare CF pathogens (EuroCare CF collection). The isolate identification given by MALDI-TOF MS agreed with that given by standard techniques for 479/481 (99.6%) clinical isolates obtained from respiratory samples provided by patients with CE In two (0.4%) of 481 samples there was a discrepancy in identification between MALDI-TOF MS and standard techniques. One organism was identified as Pseudomonas aeruginosa by MALDI-TOF but could only be identified by the laboratory's standard methods as of the Pseudomonas genus. The second organism was identified as P. beteli by MALDI-TOF MS and Stenotrophomonas maltophilia by standard methods. This study shows that MALDI-TOF MS is superior to standard techniques in providing cheap, rapid and accurate identification of CF sputum isolates.

  14. Rapid and scalable plant-based production of a cholera toxin B subunit variant to aid in mass vaccination against cholera outbreaks.

    Directory of Open Access Journals (Sweden)

    Krystal Teasley Hamorsky

    Full Text Available INTRODUCTION: Cholera toxin B subunit (CTB is a component of an internationally licensed oral cholera vaccine. The protein induces neutralizing antibodies against the holotoxin, the virulence factor responsible for severe diarrhea. A field clinical trial has suggested that the addition of CTB to killed whole-cell bacteria provides superior short-term protection to whole-cell-only vaccines; however, challenges in CTB biomanufacturing (i.e., cost and scale hamper its implementation to mass vaccination in developing countries. To provide a potential solution to this issue, we developed a rapid, robust, and scalable CTB production system in plants. METHODOLOGY/PRINCIPAL FINDINGS: In a preliminary study of expressing original CTB in transgenic Nicotiana benthamiana, the protein was N-glycosylated with plant-specific glycans. Thus, an aglycosylated CTB variant (pCTB was created and overexpressed via a plant virus vector. Upon additional transgene engineering for retention in the endoplasmic reticulum and optimization of a secretory signal, the yield of pCTB was dramatically improved, reaching >1 g per kg of fresh leaf material. The protein was efficiently purified by simple two-step chromatography. The GM1-ganglioside binding capacity and conformational stability of pCTB were virtually identical to the bacteria-derived original B subunit, as demonstrated in competitive enzyme-linked immunosorbent assay, surface plasmon resonance, and fluorescence-based thermal shift assay. Mammalian cell surface-binding was corroborated by immunofluorescence and flow cytometry. pCTB exhibited strong oral immunogenicity in mice, inducing significant levels of CTB-specific intestinal antibodies that persisted over 6 months. Moreover, these antibodies effectively neutralized the cholera holotoxin in vitro. CONCLUSIONS/SIGNIFICANCE: Taken together, these results demonstrated that pCTB has robust producibility in Nicotiana plants and retains most, if not all, of major

  15. Analyse de discours et inégalités sociales: de l’empathie pour les invisibles à l’engagement pour le commun

    Directory of Open Access Journals (Sweden)

    Alain Rabatel

    2016-12-01

    Full Text Available L’article analyse le lien entre inégalités sociales et invisibilité puis étudie quelques exemples de luttes de reconnaissance. Il interroge ensuite les précautions à prendre pour que l’analyse de discours rende compte de l’invisibilité sociale lorsqu’elle est redoublée par l’invisibilité médiatique et linguistique – avec des phénomènes d’effacement énonciatif, de naturalisation, de prise en compte énonciative qui ne vont pas jusqu’à la prise en charge. À cette fin, il liste des conditions épistémologiques, méthodologiques et théoriques faisant système concernant: l’articulation entre linguistique et réalité extralinguistique; la problématisation de la notion de représentation; le rapport des corpus marginaux à la norme; l’interprétation de la dualité marqué/non marqué en termes de continuums; la prise en compte des stratégies de communication formatées par les situations, par les choix discursifs révélateurs des intentions des locuteurs; une analyse de discours critique (aux antipodes des postures de dénonciation en appui sur des vérités monologiques; le choix de l’interdisciplinarité; l’analyse empathique – non seulement envers différents acteurs, mais envers des groupes, des façons de penser conflictuelles –, afin de pouvoir mieux penser la place et la contribution des uns et des autres dans la co-construction d’un (bien commun partagé.

  16. Fully validated method for rapid and simultaneous measurement of six antiepileptic drugs in serum and plasma using ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Kuhn, Joachim; Knabbe, Cornelius

    2013-06-15

    Therapeutic drug monitoring (TDM) may be very useful in the clinical management of antiepileptic drug therapy for multiple reasons, such as individual variability, metabolism, genetic factors or drug-drug or drug-food interactions. In addition, TDM is helpful to study the variation in pharmacokinetics that occurs between individuals. Here, we describe a rapid assay using ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry to measure the antiepileptic drugs lacosamide, lamotrigine, levetiracetam, primidone, topiramate, and zonisamide. After the addition of internal standards (ISs) and protein precipitation of serum or plasma, 1 μl of sample was separated on a 2.1×50 mm reverse phase column (Waters, Acquity UPLC BEH Phenyl, 1.7 μm). Analytes were then ionized and detected by electrospray ionization mass spectrometry with multiple reaction monitoring. Runtime was 2.5 min per injection. Matrix effects were investigated by systematical ion suppression and in-source fragmentation experiments. The calibration curves of the 6 antiepileptic drugs were linear over the working range between 0.05 and 50 mg/L (r>0.99). The limit of detection (LOD) was measured in the assay. The intraassay and interassay coefficients of variation for all compounds were 1.0 mg/L). Mean recoveries were between 87.8 and 98.6% for all drugs. There were no significant ion suppressions detected at the elution times of the analytes. The mean differences between serum and heparinized plasma values were less than 6% for the 6 antiepileptic drugs. All drugs were stable in serum at -20°C, 4°C, and even at RT for at least 1 month. In summary, a specific and sensitive stable isotope dilution UPLC-MS/MS method was developed and validated for routine clinical monitoring of lacosamide, lamotrigine, levetiracetam, primidone, topiramate, and zonisamide. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Rapid simultaneous determination of paracetamol, amantadine hydrochloride, caffeine and chlorpheniramine maleate in human plasma by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Feng, Shudan; Tian, Yuan; Zhang, Zunjian; Zhang, Jingjing; Huang, Meihua; Chen, Yun

    2009-01-01

    A rapid, simple and sensitive high performance liquid chromatography with positive ion electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) was first developed and validated to simultaneously determine paracetamol (PAR, CAS 103-90-2), amantadine hydrochloride (ATH, CAS 665-66-7), caffeine (CAF, CAS 58-08-2) and chlorpheniramine maleate (CPM, CAS 113-92-8) in human plasma using tramadol hydrochloride (TMH, CAS 22204-88-2) as internal standard (IS). Following methanol-induced protein precipitation, the analytes were separated using a mobile phase comprised of methanol:water (0.5% formic acid) = 20:80 (v/v) on a commercially available column (150 mm x 2.1 mm I.D., 5 microm) and analyzed by electrospray ionization tandem mass spectrometry in the selected reaction monitoring (SRM) mode with the precursor to product ion transitions m/z 152.3-->110.2 for PAR, 152.3-->135.3 for ATH, 195.1-->138.3 for CAF, 275.2-->230.3 for CPM and 264.2-->58.2 for TMH. The standard curves were linear (r2 > 0.99) over the concentration range of 0.2-20 microg/mL for PAR, 20-2000 ng/mL for ATH and CAF, 0.1-10 ng/mL for CPM and had good accuracy and precision, respectively. The within- and between-batch precisions were less than 15% in terms of relative standard deviation (RSD). The lower limit of quantitation (LLOQ) were 0.2 microg/mL, 20 ng/mL, 20 ng/mL and 0.1 ng/mL for PAR, ATH, CAF and CPM, respectively. The described method has been successfully applied to study the pharmacokinetics of paracetamol-amantadine hydrochloride tablets in Chinese healthy male volunteers with great precision and sensitivity.

  18. Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

    2017-01-27

    A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Rapid determination of cocamidopropyl betaine impurities in cosmetic products by core-shell hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wang, Perry G; Zhou, Wanlong

    2016-08-26

    Cocamidopropyl betaine (CAPB) is a common surfactant widely used in personal care products. Dimethylaminopropylamine (DMAPA) and lauramidopropyldimethylamine (LAPDMA) are two chemicals present as impurities in CAPB and have been reported as skin sensitizers. A rapid and sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method, using a core shell hydrophilic interaction liquid chromatography (HILIC) column, has been developed to quantify DMAPA and LAPDMA in cosmetic products. Corresponding stable isotopically labeled analogues of the above native compounds were used as internal standards to compensate for matrix effect and for loss of recovery. Each sample was first screened to determine whether the sample needed to be diluted to minimize matrix effects as well as to fit the calibration range. The concept of matrix effect factor (MEF) was introduced to quantitatively evaluate each sample with a unique matrix using the internal standards. Recoveries at three spiking levels of low, medium, and high concentrations ranged from 98.4 to 112% with RSDs less than 5%. This method has been validated and is the first UHPLC-MS/MS method, which uses core shell HILIC column and stable isotopically labeled internal standards to simultaneously determine these two CAPB impurities in cosmetic products. Published by Elsevier B.V.

  20. Rapid shotgun proteomic liquid chromatography-electrospray ionization-tandem mass spectrometry-based method for the lupin ( Lupinus albus L.) multi-allergen determination in foods.

    Science.gov (United States)

    Mattarozzi, Monica; Bignardi, Chiara; Elviri, Lisa; Careri, Maria

    2012-06-13

    Allergy to lupin is a growing food safety problem because this legume, increasingly exploited in the food industry, is one of the allergens that, according to law, must be declared on the labels of food products in the European Union. In this context, a rapid targeted proteomic approach based on liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analysis was proposed and aimed to unequivocal confirmation and reliable determination of the major lupin allergens, i.e., conglutins, in pasta and biscuits. Detected concentrations were around 1 mg of lupin/kg of pasta and biscuits, proving the capabilities of the MS-based method in terms of the sensitive allergen screening method. Good precision was observed in terms of both intra- and interday repeatability, with relative standard deviation (RSD) lower than 23%. Recoveries from 95 ± 10 to 118 ± 12% and from 103 ± 1 to 110 ± 12% ranges were calculated for biscuits and pasta, respectively. Finally, the applicability of the devised method was investigated by analyzing market samples containing lupin and samples that may possibly contain traces of lupin deriving from cross-contamination between products and production lines.

  1. Matrix-assisted laser desorption ionisation time-of-flight mass spectrometry rapid detection of carbapenamase activity in Acinetobacter baumannii isolates.

    Science.gov (United States)

    Abouseada, Noha; Raouf, May; El-Attar, Eman; Moez, Pacinte

    2017-01-01

    Carbapenamase-producing Acinetobacter baumannii are an increasing threat in hospitals and Intensive Care Units. Accurate and rapid detection of carbapenamase producers has a great impact on patient improvement and aids in implementation of infection control measures. In this study, we describe the use of matrix-assisted laser desorption ionisation time-of-flight mass spectrometry (MALDI TOF MS) to identify carbapenamase-producing A. baumannii isolates in up to 3 h. Isolates and Methods: A total of 50 A. baumannii isolates (of which 39 were carabapenamase producers) were tested using MALDI TOF MS. Isolates were incubated for 3 h with 0.25 mg/ml up to 2 mg/ml of imipenem (IMP) at 37°C. Supernatants were analysed by MALDI TOF to analyse peaks corresponding to IMP (300 Da) and an IMP metabolite (254 Da) using UltrafleXtreme (Bruker Daltonics, Bremen, Germany). All carbapenamase-producing isolates were evidenced by the disappearance or reduction in intensity of the 300 Da peak of IPM and the appearance of a 254 Da peak of the IPM metabolite. In isolates that did not produce carbapenamase, the IPM 300 Da peak remained intact. MALDI TOF is a promising tool in the field of diagnostic microbiology that has the ability to transfer identification and antimicrobial susceptibility testing time from days to hours.

  2. Soil transmitted helminths and scabies in Zanzibar, Tanzania following mass drug administration for lymphatic filariasis - a rapid assessment methodology to assess impact

    Directory of Open Access Journals (Sweden)

    Mohammed Khalfan A

    2012-12-01

    Full Text Available Abstract Background Ivermectin and albendazole are used in annual mass drug administration (MDA for the lymphatic filariasis elimination programmes in African countries co-endemic for onchocerciasis, but have additional impact on soil transmitted helminths and the ectoparasitic mite which causes scabies. Assessing these collateral impacts at scale is difficult due to the insensitivity of available parasite detection techniques. Methods The numbers of cases diagnosed with intestinal helminths and scabies and who received prescriptions for treatment were evaluated in 50 health centres in Zanzibar. Records were examined from 2000, prior to the initiation of MDA to 2005, after six rounds of MDA for lymphatic filariasis had taken place. Results Health centre records showed a consistent decline in the number of cases of intestinal helminths and scabies diagnosed by community health workers in Zanzibar and the number of prescriptions issued across five age groups. A 90-98% decline in soil transmitted helminths and 68-98% decline in scabies infections were recorded. Poisson regression models aggregated to both the island-level and district-level indicated that the decline was statistically significant. Conclusions The described method of examining health centre records has the potential for use on a large scale, despite limitations, as a rapid method to evaluate the impacts resulting from both lymphatic filariasis and onchocerciasis MDA. This would result in a reduction in the need for parasitological evaluations to determine prevalence and intensity.

  3. Validation of a rapid method of analysis using ultrahigh-performance liquid chromatography - tandem mass spectrometry for nitrogen-rich adulterants in nutritional food ingredients.

    Science.gov (United States)

    Draher, Jon; Pound, Vickie; Reddy, Todime M

    2014-12-19

    A method for the rapid quantification of 9 potential nitrogen-rich economic adulterants (dicyandiamide, urea, biuret, cyromazine, amidinourea, ammeline, amidinourea, melamine, and cyanuric acid) in five milk and soy derived nutritional ingredients, i.e. whole milk powder, nonfat dry milk, milk protein concentrate, sodium caseinate, and soy protein isolate has been developed and validated for routine use. The samples were diluted tenfold with water followed by treatment with 2% formic acid and acetonitrile to precipitate proteins. Sample extracts were analyzed using hydrophilic interaction chromatography and tandem mass spectrometry (HILIC-MS/MS) under both positive and negative modes. Stable isotope labeled internal standards were used to ensure accurate quantification. In multi-day validation experiments, the average accuracies, relative standard deviations (RSD), and method detection limits (MDL) for all analytes in whole milk powder were 82-101%, 6-13%, and 0.1mg/kg-7 mg/kg, respectively. The retention times of the analytes in matrix spiked controls were within ± 0.06 min of the average retention times of the corresponding analytes in calibration standards. The validated method was proven to be rugged for routine use to quantify the presence of 9 nitrogen-rich compounds in milk and soy derived ingredients and to provide a defense from economically motivated adulteration. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Rapid determination of pesticide residues in Chinese materia medica using QuEChERS sample preparation followed by gas chromatography–mass spectrometry

    Directory of Open Access Journals (Sweden)

    Yichen Hu

    2012-06-01

    Full Text Available Pesticide residue analysis plays an important role in the quality control of Chinese materia medica. This paper reports the development and validation of an analytical method for the quantitative determination of the residues of 39 pesticides in 12 different matrices of Chinese materia medica. Sample preparation utilized the QuEChERS method with acetonitrile:1% aqueous acetic acid (9:1, v/v as extraction solvent followed by sample clean-up by dispersive solid phase extraction using primary secondary amine sorbent and graphitized carbon black. Extracts were then analysed by gas chromatography coupled with electron impact mass spectrometry in the selected ion monitoring mode. Limit of detection (LOD and limit of quantitation (LOQ values were in the ranges 0.5–50 ng/g and 1–100 ng/g, respectively. The recoveries of the 39 pesticides were in the range 75–112% with precision (as relative standard deviation, RSD <15%. The results show that the modified QuEChERS method allows rapid and sensitive analysis of multiple pesticide residues in Chinese materia medica.

  5. Rapid gas chromatographic analysis of less abundant compounds in distilled spirits by direct injection with ethanol-water venting and mass spectrometric data deconvolution.

    Science.gov (United States)

    Macnamara, Kevin; Lee, Michelle; Robbat, Albert

    2010-01-01

    The principal trace secondary compounds common to fermentation-derived distilled spirits can be rapidly quantified by directly injecting 5muL of spirit without sample preparation to a narrow-bore 0.15mm internal diameter capillary column. The ethanol-water is removed in an initial solvent venting step using a programmed temperature vapourization injector, followed by splitless transfer of the target analytes to the column. The larger injection facilitates trace analysis and ethanol-water removal extends column lifetime. Problems of coelution between analytes or with sample matrix were surmounted by using mass spectral deconvolution software for quantification. All operations in the analysis from injection with solvent venting to data reduction are fully automated for unattended sequential sample analysis. The synergy of the various contributory steps combines to offer an effective novel solution for this analysis. Applications include quantification of low ppm amounts of acids and esters and sub-ppm profiling of trace compounds from both the raw material malt and the ageing in wood barrels. Copyright 2009 Elsevier B.V. All rights reserved.

  6. Direct analysis in real time-mass spectrometry (DART-MS) for rapid qualitative screening of toxic glycols in glycerin-containing products.

    Science.gov (United States)

    Self, Randy L

    2013-06-01

    In 2007, the United States Food and Drug Administration released guidance recommending testing of glycerin used in regulated consumer products, such as cough syrup preparations, toothpaste, and other pharmaceutical and food products, for the toxic compounds ethylene glycol and diethylene glycol. Regulatory laboratories routinely test glycerin, and products containing glycerin or related compounds for these toxic glycols, using an official gas chromatographic method, to ensure the safety of these products. The current work describes a companion technique to compliment this GC-FID method utilizing Orbitrap mass spectrometry with direct analysis in real time ionization to rapidly screen these samples qualitatively, with results in as little as five seconds, with no sample preparation required. This allows the more time and resource intensive method to be reserved for those rare cases when these compounds are detected, potentially greatly improving laboratory efficiency. The technique was evaluated for qualitative sensitivity and repeatability, and compared against the GC-FID method. The method appears to perform well against these metrics. Published by Elsevier B.V.

  7. Rapid determination of endogenous cytokinins in plant samples by combination of magnetic solid phase extraction with hydrophilic interaction chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Liu, Zhao; Cai, Bao-Dong; Feng, Yu-Qi

    2012-04-01

    A 2-acrylamido-2-methyl-1-propanesulfonic acid-co-ethylene glycol dimethacrylate (Fe₃O₄/SiO₂/P(AMPS-co-EGDMA)) copolymer was prepared and used as a magnetic solid phase extraction (MSPE) medium for recovery of endogenous cytokinins (CKs) from plant extracts. This magnetic porous polymer was characterized by electron microscopy, nitrogen sorption experiments, elemental analysis and Fourier-transformed infrared spectroscopy. It was demonstrated to have high extraction capacity toward CKs in plants due to its specificity, surface area and porous structure. Coupled with hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS/MS), a rapid, simple, and effective MSPE-HILIC-MS/MS analytical method for the quantitative analysis of endogenous CKs in Oryza sativa (O. sativa) roots was successfully established. Good linearities were obtained for all CKs investigated with correlation coefficients (R²>0.9975. The results showed that LODs (S/N=3) were ranged from 0.18 to 3.65 pg mL⁻¹. Reproducibility of the method was obtained with intra-day and inter-day relative standard deviations (RSDs) less than 16.1% and the recoveries in plant samples ranged from 72.8% to 115.5%. Finally, the MSPE-HILIC-MS/MS method was applied to several plant samples, and the amounts of endogenous CKs in O. sativa roots, leaves and Arabidopsis thaliana (A. thaliana) were successfully determined. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. A new membrane inlet interface of a vacuum ultraviolet lamp ionization miniature mass spectrometer for on-line rapid measurement of volatile organic compounds in air.

    Science.gov (United States)

    Hou, Keyong; Wang, Junde; Li, Haiyang

    2007-01-01

    A novel membrane inlet interface coupled to a single-photon ionization (SPI) miniature time-of-flight mass spectrometer has been developed for on-line rapid measurement of volatile organic compounds (VOCs). The vacuum ultraviolet (VUV) light source for SPI was a commercial krypton discharge lamp with photon energy of 10.6 eV and photon flux of 10(10) photons/s. The experimental results showed that the sensitivity was 5 times as high as obtained with the traditional membrane inlet. The enrichment efficiency could be adjusted in the range of 10 to 20 times for different VOCs when a buffer cell was added to the inlet interface, and the memory effect was effectively eliminated. A detection limit as low as 25 parts-per-billion by volume (ppbv) for benzene has been achieved, with a linear dynamic range of three orders of magnitude. The rise times were 6 s, 10 s and 15 s for benzene, toluene and p-xylene, respectively, and the fall time was only 6 s for all of these compounds. The analytical capacity of this system was demonstrated by the on-line analysis of VOCs in single puff mainstream cigarette smoke, in which more than 50 compounds were detected in 2 s. Copyright 2007 John Wiley & Sons, Ltd.

  9. Rapid determination of caffeine in one drop of beverages and foods using drop-to-drop solvent microextraction with gas chromatography/mass spectrometry.

    Science.gov (United States)

    Shrivas, Kamlesh; Wu, Hui-Fen

    2007-11-02

    A simple and rapid sample cleanup and preconcentration method for the quantitative determination of caffeine in one drop of beverages and foods by gas chromatography/mass spectrometry (GC/MS) has been proposed using drop-to-drop solvent microextraction (DDSME). The best optimum experimental conditions for DDSME were: chloroform as the extraction solvent, 5 min extraction time, 0.5 microL exposure volume of the extraction phase and no salt addition at room temperature. The optimized methodology exhibited good linearity between 0.05 and 5.0 microg/mL with correlation coefficient of 0.980. The relative standard deviation (RSD) and limits of detection (LOD) of the DDSME/GC/MS method were 4.4% and 4.0 ng/mL, respectively. Relative recovery of caffeine in beverages and foods were found to be 96.6-101%, which showing good reliability of this method. This DDSME excludes the major disadvantages of conventional method of caffeine extraction, like large amount of organic solvent and sample consumption and long sample pre-treatment process. So, this approach proves that the DDSME/GC/MS technique can be applied as a simple, fast and feasible diagnosis tool for environmental, food and biological application for extremely small amount of real sample analysis.

  10. Integration of Affinity Selection-Mass Spectrometry and Functional Cell-Based Assays to Rapidly Triage Druggable Target Space within the NF-κB Pathway.

    Science.gov (United States)

    Kutilek, Victoria D; Andrews, Christine L; Richards, Matthew P; Xu, Zangwei; Sun, Tianxiao; Chen, Yiping; Hashke, Andrew; Smotrov, Nadya; Fernandez, Rafael; Nickbarg, Elliott B; Chamberlin, Chad; Sauvagnat, Berengere; Curran, Patrick J; Boinay, Ryan; Saradjian, Peter; Allen, Samantha J; Byrne, Noel; Elsen, Nathaniel L; Ford, Rachael E; Hall, Dawn L; Kornienko, Maria; Rickert, Keith W; Sharma, Sujata; Shipman, Jennifer M; Lumb, Kevin J; Coleman, Kevin; Dandliker, Peter J; Kariv, Ilona; Beutel, Bruce

    2016-07-01

    The primary objective of early drug discovery is to associate druggable target space with a desired phenotype. The inability to efficiently associate these often leads to failure early in the drug discovery process. In this proof-of-concept study, the most tractable starting points for drug discovery within the NF-κB pathway model system were identified by integrating affinity selection-mass spectrometry (AS-MS) with functional cellular assays. The AS-MS platform Automated Ligand Identification System (ALIS) was used to rapidly screen 15 NF-κB proteins in parallel against large-compound libraries. ALIS identified 382 target-selective compounds binding to 14 of the 15 proteins. Without any chemical optimization, 22 of the 382 target-selective compounds exhibited a cellular phenotype consistent with the respective target associated in ALIS. Further studies on structurally related compounds distinguished two chemical series that exhibited a preliminary structure-activity relationship and confirmed target-driven cellular activity to NF-κB1/p105 and TRAF5, respectively. These two series represent new drug discovery opportunities for chemical optimization. The results described herein demonstrate the power of combining ALIS with cell functional assays in a high-throughput, target-based approach to determine the most tractable drug discovery opportunities within a pathway. © 2016 Society for Laboratory Automation and Screening.

  11. Rapid and selective determination of free chlorine in aqueous solution using electrophilic addition to styrene by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Wakigawa, Kengo; Gohda, Akinaga; Fukushima, Sunao; Mori, Takeshi; Niidome, Takuro; Katayama, Yoshiki

    2013-01-15

    We developed a rapid and selective method for determination of free chlorine in aqueous solution by gas chromatography/mass spectrometry for the first time. Free chlorine was converted to styrene chlorohydrin using electrophilic addition to styrene in sodium acetate buffer solution (pH 5). The chlorine derivative obtained was extracted with chloroform, and then analyzed by GC/MS. The calibration curve showed good linearity from 0.2-100 μg/mL (as available chlorine). The detection limit was 0.1 μg/mL, and the intra- and interday accuracy were measured at concentrations of 10, 50, and 75 μg/mL to be -1.3 to 6.9% (intraday) and 3.8-8.0% (interday) as % Bias. The precision was between 1.4 and 4.5% as % RSD. These results indicate that this method is a superior technique for the identification of free chlorine. This method was successfully applied to quantification in commercial samples and in samples of a criminal case. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. A rapid gas chromatographic injection-port derivatization method for the tandem mass spectrometric determination of patulin and 5-hydroxymethylfurfural in fruit juices.

    Science.gov (United States)

    Marsol-Vall, Alexis; Balcells, Mercè; Eras, Jordi; Canela-Garayoa, Ramon

    2016-07-01

    A novel method consisting of injection-port derivatization coupled to gas chromatography-tandem mass spectrometry is described. The method allows the rapid assessment of 5-hydroxymethylfurfural (HMF) and patulin content in apple and pear derivatives. The chromatographic separation of the compounds was achieved in a short chromatographic run (12.2min) suitable for routine controls of these compounds in the fruit juice industry. The optimal conditions for the injection-port derivatization were at 270°C, 0.5min purge-off, and a 1:2 sample:derivatization reagent ratio (v/v). These conditions represent an important saving in terms of derivatization reagent consumption and sample preparation time. Quality parameters were assessed for the target compounds, giving LOD of 0.7 and 1.6μg/kg and LOQ of 2 and 5μg/kg for patulin and HMF, respectively. These values are below the maximum patulin concentration in food products intended for infants and young children. Repeatability (%RSD n=5) was below 12% for both compounds. In addition, the method linearity ranged between 25 and 1000μg/kg and between 5 and 192μg/kg for HMF and patulin, respectively. Finally, the method was applied to study HMF and patulin content in various fruit juice samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Capillary electrophoresis coupled with inductively coupled mass spectrometry as an alternative to cloud point extraction based methods for rapid quantification of silver ions and surface coated silver nanoparticles.

    Science.gov (United States)

    Qu, Haiou; Mudalige, Thilak K; Linder, Sean W

    2016-01-15

    Speciation and accurate quantification of ionic silver and metallic silver nanoparticles are critical to investigate silver toxicity and to determine the shelf-life of products that contain nano silver under various storage conditions. We developed a rapid method for quantification of silver ions and silver nanoparticles using capillary electrophoresis (CE) interfaced with inductively-coupled plasma mass spectrometry (ICPMS). The addition of 2-mercaptopropionylglycine (tiopronin) to the background electrolyte was used to facilitate the chromatographic separation of ionic silver and maintain the oxidation state of silver. The obtained limits of detection were 0.05 μg kg(-1) of silver nanoparticles and 0.03 μg kg(-1) of ionic silver. Nanoparticles of varied sizes (10-110 nm) with different surface coating, including citrate acid, lipoic acid, polyvinylpyrrolidone and bovine serum albumin (BSA) were successfully analyzed. Particularly good recoveries (>93%) were obtained for both ionic silver and silver nanoparticle in the presence of excess amount of BSA. The method was further tested with six commercially available dietary supplements which varied in concentration and matrix components. The summed values of silver ions and silver nanoparticles correlated well with the total silver concentration determined by ICPMS after acid digestion. This method can serve as an alternative to cloud point extraction technique when the extraction efficiency for protein coated nanoparticles is low. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Rapid identification viruses from nasal pharyngeal aspirates in acute viral respiratory infections by RT-PCR and electrospray ionization mass spectrometry.

    Science.gov (United States)

    Chen, Kuan-Fu; Rothman, Richard E; Ramachandran, Padmini; Blyn, Lawrence; Sampath, Rangarajan; Ecker, David J; Valsamakis, Alexandra; Gaydos, Charlotte A

    2011-04-01

    Diagnosis of the etiologic agent of respiratory viral infection relies traditionally on culture or antigen detection. This pilot evaluation compared performance characteristics of the RT-PCR and electrospray ionization mass spectrometry (RT-PCR/ESI-MS) platform to conventional virologic methods for identifying multiple clinically relevant respiratory viruses in nasopharyngeal aspirates. The RT-PCR/ESI-MS respiratory virus surveillance kit was designed to detect respiratory syncytial virus, influenza A and B, parainfluenza types 1-4, adenoviridae types A-F, coronaviridae, human bocavirus, and human metapneumovirus. Patients (N=192) attending an emergency department during the 2007-2008 respiratory season consented, and "excess" frozen archived nasopharyngeal aspirates were analysed; 46 were positive by conventional virology and 69 by RT-PCR/ESI-MS, among which there were six samples with multiple viral pathogens detected. The sensitivity and specificity of the assay were 89.1% and 80.3%, respectively. Additional viruses that were not identified by conventional virology assays were detected (4 human bocaviruses and 7 coronaviruses). Samples in which the RT-PCR/ESI-MS results disagreed with conventional virology were sent for analysis by a third method using a commercial RT-PCR-based assay, which can identify viruses not detectable by conventional virologic procedures. Time to first result of RT-PCR/ESI-MS was 8h. RT-PCR/ESI-MS demonstrated capacity to detect respiratory viruses identifiable and unidentifiable by conventional methods rapidly. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. A simple and rapid ultra-high-performance liquid chromatography-tandem mass spectrometry method to determine plasma biotin in hemodialysis patients.

    Science.gov (United States)

    Yagi, Shigeaki; Nishizawa, Manabu; Ando, Itiro; Oguma, Shiro; Sato, Emiko; Imai, Yutaka; Fujiwara, Masako

    2016-08-01

    A simple, rapid, and selective method for determination of plasma biotin was developed using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). After single-step protein precipitation with methanol, biotin and stable isotope-labeled biotin as an internal standard (IS) were chromatographed on a pentafluorophenyl stationary-phase column (2.1 × 100 mm, 2.7 μm) under isocratic conditions using 10 mm ammonium formate-acetonitrile (93:7, v/v) at a flow rate of 0.6 mL/min. The total chromatographic runtime was 5 min for each injection. Detection was performed in a positive electrospray ionization mode by monitoring selected ion transitions at m/z 245.1/227.0 and 249.1/231.0 for biotin and the IS, respectively. The calibration curve was linear in the range of 0.05-2 ng/mL using 300 μL of plasma. The intra- and inter-day precisions were all biotin concentrations in hemodialysis patients. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  16. Rapid determination of acetone in human blood by derivatization with pentafluorobenzyl hydroxylamine followed by headspace liquid-phase microextraction and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Deng, Chunhui; Li, Ning; Wang, Xiaochuan; Zhang, Xiangmin; Zeng, Jia

    2005-01-01

    In the current work, a simple, rapid, accurate and inexpensive method was developed for the determination of acetone in human blood. The proposed method is based on derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), followed by headspace liquid-phase microextraction (HS-LPME) and gas chromatography/mass spectrometry (GC/MS). In the present method, acetone in blood samples was derivatized with PFBHA and acetone oxime formed in several seconds. The formed oxime was enriched by HS-LPME using the organic solvent film (OSF) formed in a microsyringe barrel as extraction interface. Finally, the enriched oxime was analyzed by GC/MS in electron ionization (EI) mode. HS-LPME parameters including solvent, syringe plunger withdrawal rate, sampling volume, and extraction cycle were optimized and the method reproducibility, linearity, recovery and detection limit were studied. The proposed method was applied to determination of acetone in diabetes blood and normal blood. It has been shown that derivatization with HS-LPME and GC/MS is an alternative method for determination of the diabetes biomarker, acetone, in blood samples.

  17. Rapid and precise measurement of serum branched-chain and aromatic amino acids by isotope dilution liquid chromatography tandem mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Ruiyue Yang

    Full Text Available BACKGROUND: Serum branched-chain and aromatic amino acids (BCAAs and AAAs have emerged as predictors for the future development of diabetes and may aid in diabetes risk assessment. However, the current methods for the analysis of such amino acids in biological samples are time consuming. METHODS: An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS method for serum BCAAs and AAAs was developed. The serum was mixed with isotope-labeled BCAA and AAA internal standards and the amino acids were extracted with acetonitrile, followed by analysis using LC/MS/MS. The LC separation was performed on a reversed-phase C18 column, and the MS/MS detection was performed via the positive electronic spray ionization in multiple reaction monitoring mode. RESULTS: Specific analysis of the amino acids was achieved within 2 min. Intra-run and total CVs for the amino acids were less than 2% and 4%, respectively, and the analytical recoveries ranged from 99.6 to 103.6%. CONCLUSION: A rapid and precise method for the measurement of serum BCAAs and AAAs was developed and may serve as a quick tool for screening serum BCAAs and AAAs in studies assessing diabetes risk.

  18. Comments on “Synchronization and anti-synchronization of new uncertain fractional-order modified unified chaotic systems via novel active pinning control” [Commun Nonlinear Sci Numer Simulat 2010;15:3754-3762

    Science.gov (United States)

    Asheghan, Mohammad Mostafa; Beheshti, Mohammad Taghi Hamidi; Tavazoei, Mohammad Saleh

    2011-06-01

    In this note some points to paper [L. Pan, W. Zhou, J. Fang, D. Li, Synchronization and anti-synchronization of new uncertain fractional-order modified unified chaotic systems via novel active pinning control, Commun Nonlinear Sci Numer Simulat 2010;15:3754-3762] are presented. Hereby, we illustrate that the way that authors in [1] treat with fractional version of Lyapunov stability theorem suffers lack of a correct justification.

  19. Rapid and reliable species identification of wild mushrooms by matrix assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF MS).

    Science.gov (United States)

    Sugawara, Ryota; Yamada, Sayumi; Tu, Zhihao; Sugawara, Akiko; Suzuki, Kousuke; Hoshiba, Toshihiro; Eisaka, Sadao; Yamaguchi, Akihiro

    2016-08-31

    Mushrooms are a favourite natural food in many countries. However, some wild species cause food poisoning, sometimes lethal, due to misidentification caused by confusing fruiting bodies similar to those of edible species. The morphological inspection of mycelia, spores and fruiting bodies have been traditionally used for the identification of mushrooms. More recently, DNA sequencing analysis has been successfully applied to mushrooms and to many other species. This study focuses on a simpler and more rapid methodology for the identification of wild mushrooms via protein profiling based on matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS). A preliminary study using 6 commercially available cultivated mushrooms suggested that a more reproducible spectrum was obtained from a portion of the cap than from the stem of a fruiting body by the extraction of proteins with a formic acid-acetonitrile mixture (1 + 1). We used 157 wild mushroom-fruiting bodies collected in the centre of Hokkaido from June to November 2014. Sequencing analysis of a portion of the ribosomal RNA gene provided 134 identifications of mushrooms by genus or species, however 23 samples containing 10 unknown species that had lower concordance rate of the nucleotide sequences in a BLAST search (less than 97%) and 13 samples that had unidentifiable poor or mixed sequencing signals remained unknown. MALDI-TOF MS analysis yielded a reproducible spectrum (frequency of matching score ≥ 2.0 was ≥6 spectra from 12 spectra measurements) for 114 of 157 samples. Profiling scores that matched each other within the database gave correct species identification (with scores of ≥2.0) for 110 samples (96%). An in-house prepared database was constructed from 106 independent species, except for overlapping identifications. We used 48 wild mushrooms that were collected in autumn 2015 to validate the in-house database. As a result, 21 mushrooms were identified at the species level with

  20. Savoirs disciplinaires scolaires et savoirs de sens commun ou pourquoi des « idées vraies » ne prennent pas, tandis que des « idées fausses » ont la vie dure

    Directory of Open Access Journals (Sweden)

    David Lefrançois

    2011-05-01

    Full Text Available Les savoirs de sens commun sont solidement ancrés dans les usages, notamment grâce à l’habitude et à la sécurité ontologique qu’ils engendrent. Cet article examinera d’abord pourquoi les savoirs disciplinaires appris à l’école ne sont pas automatiquement réinvestis dans des contextes de nature extrascolaire et pourquoi les savoirs de sens commun résistent à leur déconstruction. La première partie de l’analyse sera marquée par le croisement de discours épistémologiques concernant la nature et la place des savoirs de sens commun dans les conceptions familières de la science. Cet article explorera ensuite les dynamiques qui marquent les relations qu’entretiennent les savoirs disciplinaires scolaires et les savoirs de sens commun en contexte scolaire. Le langage propre à la seconde partie se rattachera davantage aux débats en éducation sur l’importance prépondérante des savoirs de sens commun dans l’apprentissage disciplinaire par concepts. Enfin, nous montrerons qu’il existe des stratégies d’enseignement qui peuvent optimiser l’appropriation intellectuelle des savoirs disciplinaires scolaires et leur transfert dans les interactions quotidiennes.Common sense knowledge is firmly anchored in everyday practices, notably as a result of habit and also for the ontological security it provides. This article will first examine why disciplinary knowledge learned in school is not automatically reinvested in non-school contexts, as well as why common sense knowledge persists in the face of its own deconstruction. The first part of this analysis juxtaposes various epistemological discourses relating to the nature of common sense knowledge and its position in familiar conceptions of science. The article then explores how disciplinary knowledge taught in school and common sense knowledge interact in an educational context. This section of the article will focus mainly on educational debates pertaining to the

  1. A temperature programmed reaction/single-photon ionization time-of-flight mass spectrometry system for rapid investigation of gas-solid heterogeneous catalytic reactions under realistic reaction conditions

    NARCIS (Netherlands)

    He, Songbo; Cui, Huapeng; Lai, Yulong; Sun, Chenglin; Luo, Sha; Li, Haiyang; Seshan, Kulathuiyer

    2015-01-01

    A Temperature-Programmed Reaction (TPRn)/Single-Photon Ionization Time-of-Flight Mass Spectrometry (SPI-TOF-MS) system is described. The TPRn/SPI-TOF-MS system allows rapid characterization of heterogeneous catalytic reactions under realistic reaction conditions and at the same time allows for the

  2. On-line solid-phase extraction-short-column liquid chromatography combined with various tandem mass spectrometric scanning strategies for the rapid study of transformation of pesticides in surface water.

    NARCIS (Netherlands)

    Hogenboom, A.C.; Niessen, W.M.A.; Brinkman, U.A.T.

    1999-01-01

    The applicability of solid-phase extraction-short-column liquid chromatography using two short columns (i.e., 10 and 20 mm long) coupled on-line with tandem mass spectrometric detection is demonstrated for the rapid degradation study of pesticides and their transformation products in water at the

  3. Rapid identification and quantification of methamphetamine and amphetamine in hair by gas chromatography/mass spectrometry coupled with micropulverized extraction, aqueous acetylation and microextraction by packed sorbent.

    Science.gov (United States)

    Miyaguchi, Hajime; Iwata, Yuko T; Kanamori, Tatsuyuki; Tsujikawa, Kenji; Kuwayama, Kenji; Inoue, Hiroyuki

    2009-05-01

    We developed a rapid identification and quantification method for the toxicological analysis of methamphetamine and amphetamine in human hair by gas chromatography/mass spectrometry coupled with a novel combination of micropulverized extraction, aqueous acetylation and microextraction by packed sorbent (MEPS) named MiAMi-GC/MS. A washed hair sample (1-5 mg) was micropulverized for 5 min in a 2 mL plastic tube with 250 microL of water. An anion-exchange sorbent was added to adsorb anionic interferences. After removing the residue with a membrane-filter unit, sodium carbonate and acetic anhydride was admixed in turn. Acetylation was completed in approximately 20 min at room temperature. The acetylated analytes in the reaction liquid were concentrated to an octadecylsilica sorbent packed in the needle of a syringe by a CombiPAL autosampler. Elution was carried out with 50 microL of methanol, and the entire eluate injected into a gas chromatograph using a programmable temperature vaporizing (PTV) technique. The time required for sample preparation and GC/MS analysis was approximately 1 h from a washed hair sample, and an evaporation process was not required. Ranges for quantification were 0.20-50 (ng/mg) each for methamphetamine and amphetamine using 1 mg of hair. Accuracy and relative standard deviation (RSD) were evaluated intraday and interday at three concentrations, and the results were within the limit of a guidance issued by U.S. Food and Drug Administration. For identification, full-scan mass spectra of methamphetamine and amphetamine were obtained using 5 mg of fortified hair samples at 0.2 ng/mg. The extraction device of MEPS was durable for at least 300 extractions, whereas the liner of the gas chromatograph should be replaced after 20-30 times use. The carry over was estimated to be about 1-2%. This sample-preparation method coupled with GC/MS is fast and labor-saving in comparison with conventional methods.

  4. Rapid whole monoclonal antibody analysis by mass spectrometry: An ultra scale-down study of the effect of harvesting by centrifugation on the post-translational modification profile.

    Science.gov (United States)

    Reid, C Q; Tait, A; Baldascini, H; Mohindra, A; Racher, A; Bilsborough, S; Smales, C M; Hoare, M

    2010-09-01

    With the trend towards the generation and production of increasing numbers of complex biopharmaceutical (protein based) products, there is an increased need and requirement to characterize both the product and production process in terms of robustness and reproducibility. This is of particular importance for products from mammalian cell culture which have large molecular structures and more often than not complex post-translational modifications (PTMs) that can impact the efficacy, stability and ultimately the safety of the final product. It is therefore vital to understand how the operating conditions of a bioprocess affect the distribution and make up of these PTMs to ensure a consistent quality and activity in the final product. Here we have characterized a typical bioprocess and determined (a) how the time of harvest from a mammalian cell culture and, (b) through the use of an ultra scale-down mimic how the nature of the primary recovery stages, affect the distribution and make up of the PTMs observed on a recombinant IgG(4) monoclonal antibody. In particular we describe the use of rapid whole antibody analysis by mass spectrometry to analyze simultaneously the changes that occur to the cleavage of heavy chain C-terminal lysine residues and the glycosylation pattern, as well as the presence of HL dimers. The time of harvest was found to have a large impact upon the range of glycosylation patterns observed, but not upon C-terminal lysine cleavage. The culture age had a profound impact on the ratio of different glycan moieties found on antibody molecules. The proportion of short glycans increased (e.g., (G0F)(2) 20-35%), with an associated decrease in the proportion of long glycans with culture age (e.g., (G2F)(2) 7-4%, and G1F/G2F from 15.2% to 7.8%). Ultra scale-down mimics showed that subsequent processing of these cultures did not change the post-translational modifications investigated, but did increase the proportion of half antibodies present in the

  5. Development of a rapid method for the analysis of synthetic growth promoters in bovine muscle using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Malone, E M; Elliott, C T; Kennedy, D G; Regan, L

    2009-04-01

    A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous identification, confirmation and quantitation of thirteen synthetic growth promoters in bovine muscle. The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC. A value of 1mugkg(-1) was chosen as the required performance level (RPL) for all analytes. The growth promoters investigated were alpha and beta trenbolone, 16-beta-OH stanozolol, methylboldenone, fluoxymesterone, methyltestosterone, medroxyprogesterone acetate, megestrol acetate, melengestrol acetate, dexamethasone, flumethasone, dienestrol and hexestrol. The method involved enzymatic hydrolysis, purification by solid phase extraction followed by analysis by UPLC-MS/MS using electrospray ionization operated in both positive and negative polarities with a total run time of 14 min. The decision limit (CCalpha) values obtained, ranged from 0.09 to 0.19 microgkg(-1) and the detection capability (CCbeta) values obtained, ranged from 0.15 to 0.32 microgkg(-1). The results of the inter-assay study, which was performed by fortifying bovine muscle samples (n=18) on three separate days, show the accuracy calculated for the various analytes to range between 98% and 102%. The precision of the method, expressed as R.S.D. values for the inter-assay variation of each analyte at the three levels of fortification (1, 1.5 and 2.0 microgkg(-1)), ranged between 3.1% and 5.8%. A Day 4 assay was carried out to examine variations due to different animals and different muscle types.

  6. Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) for rapid identification of micro-organisms in the routine clinical microbiology laboratory.

    Science.gov (United States)

    Wattal, C; Oberoi, J K; Goel, N; Raveendran, R; Khanna, S

    2017-05-01

    The study evaluates the utility of matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF MS) Vitek MS for identification of microorganisms in the routine clinical microbiology laboratory. From May 2013 to April 2014, microbial isolates recovered from various clinical samples were identified by Vitek MS. In case of failure to identify by Vitek MS, the isolate was identified using the Vitek 2 system (bioMerieux, France) and serotyping wherever applicable or otherwise by nucleic acid-mediated methods. All the moulds were identified by Lactophenol blue mounts, and mycobacterial isolates were identified by molecular identification systems including AccuProbe (bioMerieux, France) or GenoType Mycobacterium CM (Hain Lifescience, Germany). Out of the 12,003 isolates, the Vitek MS gave a good overall ID at the genus and or species level up to 97.7% for bacterial isolates, 92.8% for yeasts and 80% for filamentous fungi. Of the 26 mycobacteria tested, only 42.3% could be identified using the Saramis RUO (Research Use Only) database. VITEK MS could not identify 34 of the 35 yeast isolates identified as C. haemulonii by Vitek 2. Subsequently, 17 of these isolates were identified as Candida auris (not present in the Vitek MS database) by 18S rRNA sequencing. Using these strains, an in-house superspectrum of C. auris was created in the VITEK MS database. Use of MALDI-TOF MS allows a rapid identification of aerobic bacteria and yeasts in clinical practice. However, improved sample extraction protocols and database upgrades with inclusion of locally representative strains is required, especially for moulds.

  7. Rapid and simple analysis of disease-associated biomarkers of Taiwanese patients with schizophrenia using matrix-assisted laser desorption ionization mass spectrometry.

    Science.gov (United States)

    Huang, Tiao-Lai; Lo, Li-Hua; Shiea, Jentaie; Su, Hung

    2017-10-01

    Matrix-assisted laser desorption ionization/time-of-flight mass spectrometry (MALDI-TOF MS) is an extremely sensitive analytical tool for characterizing biological compounds in bio samples. In this study, we applied MALDI-TOF MS to assess potential protein biomarkers in the peripheral blood mononuclear cells (PBMCs) of patients with schizophrenia in the acute phase, recovery phase and healthy controls in Taiwan. We recruited 40 participants, including 20 pairs of patients diagnosed with schizophrenia in the acute phase, after four-week treatment with drug in the recovery phase, and 20 healthy controls. The schizophrenic patients were diagnosed using Structured Clinical Interview for DSM-IV Axis I Disorders (SCID), and severity was assessed by a positive and negative symptom scale at baseline and at endpoint following four-week treatment with drug. The patients' PBMCs biomarkers were rapidly measured using a technique that combines MALDI-TOF MS and principle component analysis. A receiver operating characteristic curve was created for the evaluated biomarker. Significant differences in α-defensins 1-3 were found between the patients in acute phase with schizophrenia and the healthy controls, but not between the schizophrenic patients in recovery phase and healthy controls or between the schizophrenic patients in acute phase and in recovery phase. α-Defensins can be biomarkers of Taiwanese patients with schizophrenia, thus supporting the hypothesis that the inflammatory response and immunity system is correlated with the pathophysiology of schizophrenia. Moreover, the result also implies that α-defensins may be related in schizophrenia-associated disease not in efficacy of drug-treatment. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Rapid and sensitive serum glucose determination using chemical labeling coupled with black phosphorus-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Wang, Qing; Yu, Lei; Qi, Chu-Bo; Ding, Jun; He, Xiao-Mei; Wang, Ren-Qi; Feng, Yu-Qi

    2018-01-01

    Monitoring the concentration of blood glucose in patients is a key component of good medical diagnoses. Therefore, developing an accurate, rapid and sensitive strategy for monitoring blood glucose is of vital importance. We proposed a strategy for serum glucose determination combining 2-(4-boronobenzyl) isoquinolin-2-ium bromide chemical labeling with black phosphorus assisted laser desorption ionization-time of flight mass spectrometry (CL-BP/ALDI-TOF MS). The entire analytical process consisted of 1min of protein precipitation and 3min of chemical labeling in a microwave oven prior to the BP/ALDI-TOF MS analysis. The analysis can be completed in 5min with high throughput and extremely low sample consumption. Good linearity for glucose was obtained with a correlation coefficient (R) of 0.9986. The limit of detection (LOD) and limit of quantification (LOQ) were 11.5 fmol and 37.5 fmol, respectively. Satisfied reproducibility and reliability were gained by evaluation of the intra- and inter-day precisions with relative standard deviations (RSDs) less than 7.2% and relative recoveries ranging from 87.1% to 108.1%, respectively. The proposed strategy was also applied for the analysis of endogenous glucose in various serum samples and the results were consistent with those obtained using the hexokinase method in a clinical laboratory. Considering the results, the proposed CL-BP/ALDI-TOF MS strategy has proven to be reliable, fast, and sensitive for quantitative analysis of serum glucose. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Rapid enrichment of (homo)acetogenic consortia from animal feces using a high mass-transfer gas-lift reactor fed with syngas.

    Science.gov (United States)

    Park, Shinyoung; Yasin, Muhammad; Kim, Daehee; Park, Hee-Deung; Kang, Chang Min; Kim, Duk Jin; Chang, In Seop

    2013-09-01

    A gas-lift reactor having a high mass transfer coefficient (k(L)a = 80.28 h(-1)) for a relatively insoluble gas (carbon monoxide; CO) was used to enrich (homo)acetogens from animal feces. Samples of fecal matter from cow, rabbit, chicken, and goat were used as sources of inoculum for the enrichment of CO and H(2) utilizing microbial consortia. To confirm the successful enrichment, the Hungate roll tube technique was employed to count and then isolate putative CO utilizers. The results of this work showed that CO and H(2) utilizing consortia were established for each inoculum source after 8 days. The number of colony-forming units in cow, rabbit, chicken, and goat fecal samples were 3.83 × 10(9), 1.03 × 10(9), 8.3 × 10(8), and 3.25 × 10(8) cells/ml, respectively. Forty-two colonies from the animal fecal samples were screened for the ability to utilize CO/H(2). Ten of these 42 colonies were capable of utilizing CO/H(2). Five isolates from cow feces (samples 5, 6, 8, 16, and 22) were highly similar to previously unknown (homo)acetogen, while cow-7 has shown 99 % similarity with Acetobacterium sp. as acetogens. On the other hand, four isolates from chicken feces (samples 3, 8, 10, and 11) have also shown high CO/H(2) utilizing activity. Hence, it is expected that this research could be used as the basis for the rapid enrichment of (homo)acetogenic consortia from various environmental sources.

  10. Rapid in vivo determination of fluoroquinolones in cultured puffer fish (Takifugu obscurus) muscle by solid-phase microextraction coupled with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tang, Yijia; Xu, Jianqiao; Chen, Le; Qiu, Junlang; Liu, Yuan; Ouyang, Gangfeng

    2017-12-01

    Fluoroquinolones (FQs) are a group of antimicrobial agents that have been widely used for therapeutic purposes in clinical medicine for human and veterinary diseases, as well as in aquaculture production. Their residues, however, may survive in foods of animal origin, thus causing health risks for human. In this study, a rapid and sensitive method based on in vivo solid-phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to detect the residues of five FQs in cultured puffer fish (Takifugu obscurus). In vitro fiber evaluation experiment demonstrated that, compared with the thicker polydimethylsiloxane (PDMS) coating (165µm), the custom-made biocompatible C18-PAN fibers (45µm) exhibited much higher extraction efficiencies towards FQs (approximately 9-31 times). The custom-made C18-PAN coating also possessed excellent reproducibility in fish muscle with the intra-fiber relative standard deviations (RSDs) ranging from 11.2% to 14.3% (n = 6) and inter-fiber RSDs ranging from 13.1% to 16.1% (n = 6), which was suitable for in vivo sampling. The custom-made SPME fibers were subsequently applied to determine fluoroquinolones in dorsal-epaxial muscle of living puffer fish. The accuracies were verified through the comparison with traditional liquid extraction (LE) method, and the sensitivities were demonstrated to be satisfying with the limits of detection (LODs) ranging from 0.3ngg -1 to 1.5ngg -1 . In general, this study presented a convenient and high-efficient method to determine fluoroquinolones in puffer fish by in vivo sampling. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Coupling frontal elution paper chromatography with desorption corona beam ionization mass spectrometry for rapid analysis of chlorphenamine in herbal medicines and dietary supplements.

    Science.gov (United States)

    Huang, Yun-Qing; You, Jing-Qing; Zhang, Junsheng; Sun, Wenjian; Ding, Li; Feng, Yu-Qi

    2011-10-14

    We developed a convenient method by coupling frontal elution paper chromatography with desorption corona beam ionization mass spectrometry (DCBI-MS) for rapid determination of chlorphenamine added in herbal medicines or dietary supplements. In this method, the ethanol extract of the herbal products was spotted directly onto an isosceles triangular filter paper sheet, and then the paper sheet was developed under strong elution condition with the sample zone migrating at the solvent front. The analyte was finally condensed at the V-shaped tip which could then be placed under the visible plasma beam of DCBI for ionization. The overall procedure took less than 5 min. The frontal elution paper chromatography on a triangular plate used in this work improved the signal intensity of chlorphenamine by 30-fold due to the analyte condensing at the tip and the reduction of the background suppression. Furthermore, the paper sheet also functioned as a filter in the analysis of solid or powder samples, which can increase the analytical throughput by omitting the step of centrifugation. The proposed method in current study was successfully applied in the determination of chlorphenamine in herbal medicines. Chlorphenamine was detected in four of the twelve types of herbal medicines examined in this study. The limit of detection was 200 ng/mL (2.0 ng absolute) in full-scan positive-ion mode and the linear range was from 5.0 μg/mL to 50 μg/mL with satisfactory linear coefficient (R(2) (the square of the correlation coefficient)=0.895). Good reproducibility was achieved with relative standard deviations (RSDs) less than 15.0% and the recoveries of chlorphenamine ranged from 84.3 to 90.6%. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Rapid Quantitation of Ascorbic and Folic Acids in SRM 3280 Multivitamin/Multielement Tablets using Flow-Injection Tandem Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bhandari, Deepak [ORNL; Kertesz, Vilmos [ORNL; Van Berkel, Gary J [ORNL

    2013-01-01

    RATIONALE: Ascorbic acid (AA) and folic acid (FA) are water-soluble vitamins and are usually fortified in food and dietary supplements. For the safety of human health, proper intake of these vitamins is recommended. Improvement in the analysis time required for the quantitative determination of these vitamins in food and nutritional formulations is desired. METHODS: A simple and fast (~5 min) in-tube sample preparation was performed, independently for FA and AA, by mixing extraction solvent with a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Quantitative detection was achieved by flow-injection (1 L injection volume) electrospray ionization tandem mass spectrometry (ESI-MS/MS) in negative ion mode using the method of standard addition. RESULTS: Method of standard addition was employed for the quantitative estimation of each vitamin in a sample extract. At least 2 spiked and 1 non-spiked sample extract were injected in triplicate for each quantitative analysis. Given an injection-to-injection interval of approximately 2 min, about 18 min was required to complete the quantitative estimation of each vitamin. The concentration values obtained for the respective vitamins in the standard reference material (SRM) 3280 using this approach were within the statistical range of the certified values provided in the NIST Certificate of Analysis. The estimated limit of detections of FA and AA were 13 and 5.9 ng/g, respectively. CONCLUSIONS: Flow-injection ESI-MS/MS was successfully applied for the rapid quantitation of FA and AA in SRM 3280 multivitamin/multielement tablets.

  13. Reliable and reproducible method for rapid identification of Nocardia species by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Toyokawa, Masahiro; Kimura, Keigo; Nishi, Isao; Sunada, Atsuko; Ueda, Akiko; Sakata, Tomomi; Asari, Seishi

    2013-01-01

    Recently, matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been challenged for the identification of Nocardia species. However, the standard ethanol-formic acid extraction alone is insufficient in allowing the membrane proteins of Nocardia species to be ionized by the matrix. We therefore aimed to establish our new extraction method for the MALDI-TOF MS-based identification of Nocardia species isolates. Our modified extraction procedure is through dissociation in 0.5% Tween-20 followed by bacterial heat-inactivation, mechanical breaking of the cell wall by acid-washed glass beads and protein extraction with formic acid and acetonitrile. As reference methods for species identification, full-length 16S rRNA gene sequencing and some phenotypical tests were used. In a first step, we made our own Nocardia database by analyzing 13 strains (13 different species including N. elegans, N. otitidiscaviarum, N. asiatica, N. abscessus, N. brasiliensis, N. thailandica, N. farcinica, N. nova, N. mikamii, N. cyriacigeorgica, N. asteroids, Nocardiopsis alba, and Micromonospora sp.) and registered to the MALDI BioTyper database. Then we established our database. The analysis of 12 challenge strains using the our database gave a 100% correct identification, including 8 strains identified to the species level and 4 strains to the genus level (N. elegans, N. nova, N. farcinica, Micromonospora sp.) according to the manufacture's log score specifications. In the estimation of reproducibility of our method intended for 4 strains, both within-run and between-run reproducibility were excellent. These data indicates that our method for rapid identification of Nocardia species is with reliability, reproducibility and cost effective.

  14. Development of new efficient method for isolation of phenolics from sea algae prior to their rapid resolution liquid chromatographic-tandem mass spectrometric determination.

    Science.gov (United States)

    Klejdus, Bořivoj; Plaza, Merichel; Šnóblová, Marie; Lojková, Lea

    2017-02-20

    The extraction of phenolic compounds from 4 different sea algae samples, three brown algae (Cystoseira abies-marina, C. abies-marina grinded under cryogenic conditions with liquid nitrogen, Undaria pinnatifida and Sargassum muticum) and one red algae (Chondrus crispus) via solid phase extraction using micro-elution solid-phase extraction (μ-SPE) plate method was studied. Prior to μ-SPE, 50mg of algae with 80% methanol mixture was extracted in hyphenated series by various extraction techniques, such as pressurized liquid extraction and Ika Ultra-Turrax® Tube Drive, in combination with ultrasound assisted extraction. The μ-SPE plate technique reduced the time of sample pre-treatment thanks to higher sensitivity and pre-concentration effect. Selected groups of benzoic acid derivatives (p-hydroxybenzoic, protocatechuic, gallic, vanillic, and syringic acids), hydroxybenzaldehydes (4-hydroxybenzaldehyde, and 3,4-dihydroxybenzaldehyde), and cinnamic acid derivatives (p-coumaric, caffeic, ferulic, sinapic, and chlorogenic acids) were determined using rapid resolution liquid chromatography coupled to mass spectrometry detection with negative ion electrospray ionization (RRLC-ESI-MS) using multiple reactions monitoring. LOQs of measured samples varied in the range 0.23-1.68ng/mL and LODs in the range 0.07-0.52ng/mL. The applied method allowed a simultaneous determination of phenolics (i.e. free, esters soluble in methanol, glycosides, and esters insoluble in methanol) in less than 5min (including alkaline or acidic hydrolysis of raw extracts) from sea algae extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Impact of rapid microbial identification directly from positive blood cultures using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry on patient management.

    Science.gov (United States)

    Martiny, D; Debaugnies, F; Gateff, D; Gérard, M; Aoun, M; Martin, C; Konopnicki, D; Loizidou, A; Georgala, A; Hainaut, M; Chantrenne, M; Dediste, A; Vandenberg, O; Van Praet, S

    2013-12-01

    For septic patients, delaying the initiation of antimicrobial therapy or choosing an inappropriate antibiotic can considerably worsen their prognosis. This study evaluated the impact of rapid microbial identification (RMI) from positive blood cultures on the management of patients with suspected sepsis. During a 6-month period, RMI by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was performed for all new episodes of bacteraemia. For each patient, the infectious disease specialist was contacted and questioned about his therapeutic decisions made based on the Gram staining and the RMI. This information was collected to evaluate the number of RMIs that led to a therapeutic change or to a modification of the patient's general management (e.g. fast removal of infected catheters). During the study period, 277 new episodes of bacteraemia were recorded. In 71.12% of the cases, MALDI-TOF MS resulted in a successful RMI (197/277). For adult and paediatric patients, 13.38% (21/157) and 2.50% (1/40) of the RMIs, respectively, resulted in modification of the treatment regimen, according to the survey. In many other cases, the MALDI-TOF MS was a helpful tool for infectious disease specialists because it confirmed suspected cases of contamination, especially in the paediatric population (15/40 RMIs, 37.50%), or suggested complementary diagnostic testing. This study emphasizes the benefits of RMI from positive blood cultures. Although the use of this technique represents an extra cost for the laboratory, RMI using MALDI-TOF MS has been implemented in our daily practice. © 2013 The Authors Clinical Microbiology and Infection © 2013 European Society of Clinical Microbiology and Infectious Diseases.

  16. Rapid determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction and ultraperformance convergence chromatography tandem mass spectrometry.

    Science.gov (United States)

    Deng, Huimin; Yang, Fei; Li, Zhonghao; Bian, Zhaoyang; Fan, Ziyan; Wang, Ying; Liu, Shanshan; Tang, Gangling

    2017-07-21

    Aromatic amines in mainstream cigarette smoke have long been monitored due to their carcinogenic toxicity. In this work, a reliable and rapid method was developed for the simultaneous determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction (DLLME) and ultraperformance convergence chromatography tandem mass spectrometry (UPC2-MS/MS). Briefly, the particulate phase of the cigarette smoke was captured by a Cambridge filter pad, and diluted hydrogen chloride aqueous solution is employed to extract the aromatic amines under mechanical shaking. After alkalization with sodium hydroxide solution, small amount of toluene was introduced to further extract and enrich aromatic amines by modified DLLME under vortexing. After centrifugation, toluene phase was purified by a universal QuEChERS cleanup kit and was finally analyzed by UPC2-MS/MS. Attributing to the superior performance of UPC2-MS/MS, this novel approach allowed the separation and determination of 9 aromatic amines within 5.0min with satisfactory resolution and sensitivity. The proposed method was finally validated using Kentucky reference cigarette 3R4F, and emission levels of targeted aromatic amines determined were comparable to previously reported methods At three different spiked levels, the recoveries of most analytes were ranged from 74.01% to 120.50% with relative standard deviation (RSD) less than 12%, except that the recovery of p-toluidine at low spiked level and 3-aminobiphenyl at medium spiked level was 62.77% and 69.37% respectively. Thus, this work provides a novel alternative method for the simultaneous analysis of 9 aromatic amines in mainstream cigarette smoke. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Rapid in vivo determination of tetrodotoxin in pufferfish (Fugu) muscle by solid-phase microextraction coupled to high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Chen, Le; Qiu, Junlang; Tang, Yijia; Xu, Jianqiao; Huang, Shuyao; Liu, Yuan; Ouyang, Gangfeng

    2017-08-15

    Tetrodotoxin (TTX) is one of the most toxic substances of non-protein in nature. In present study, a rapid and sensitive method based on in vivo solid-phase microextraction (SPME) coupled to liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed to detect the endogenous TTX in pufferfish (Fugu). Fiber evaluation experiments demonstrated that, compared with the commercial PDMS and PA fibers, the home-made electrospun PS@PDA-GA fibers exhibited much better extraction performance towards to TTX in water (120 times and 20 times, respectively), under the optimized conditions. Then, the home-made SPME fibers were employed to extract TTX in spiked homogeneous fish muscle samples, and a LC-MS-MS was used for the analysis. The reproducibilities (RSDs of inter and intra fiber were 12.1%, and 7.9% respectively), linear range (10-1000ngg-1, R2=0.9963) and sensitivity (the LOD was 2.3ngg-1) of the method were found to be excellent and satisfactory for further in vivo experiments. Especially the LOD of the established method is lower than the National Standard Method of China (GB/T 23217-2008, LOD 50ngg-1). Subsequently, the method was successfully applied to detect the TTX in the dorsal muscle of living pufferfish, and the accuracy was verified with traditional liquid extraction (LE) method. In general, this is the first study to detect TTX in pufferfish by in vivo sampling method, which provided a promising alternative method for the studies of TTX, and also advanced the implementation of SPME for more in vivo studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Mass spectrometry

    DEFF Research Database (Denmark)

    Nyvang Hartmeyer, Gitte; Jensen, Anne Kvistholm; Böcher, Sidsel

    2010-01-01

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) is currently being introduced for the rapid and accurate identification of bacteria. We describe 2 MALDI-TOF MS identification cases - 1 directly on spinal fluid and 1 on grown bacteria. Rapidly obtained r...

  19. Rapid identification of bacillus anthracis spores in suspicious powder samples by using matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS)

    NARCIS (Netherlands)

    Dybwad, M.; Laaken, A.L. van der; Blatny, J.M.; Paauw, A.

    2013-01-01

    Rapid and reliable identification of Bacillus anthracis spores in suspicious powders is important to mitigate the safety risks and economic burdens associated with such incidents. The aim of this study was to develop and validate a rapid and reliable laboratory- based matrix-assisted laser

  20. Rapid identification of microorganisms from positive blood cultures by MALDI-TOF mass spectrometry subsequent to very short-term incubation on solid medium.

    Science.gov (United States)

    Idelevich, E A; Schüle, I; Grünastel, B; Wüllenweber, J; Peters, G; Becker, K

    2014-10-01

    Rapid identification of the causative microorganism is important for appropriate antimicrobial therapy of bloodstream infections. Bacteria from positive blood culture (BC) bottles are not readily available for identification by matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). Lysis and centrifugation procedures suggested for direct MALDI-TOF MS from positive BCs without previous culture are associated with additional hands-on processing time and costs. Here, we describe an alternative approach applying MALDI-TOF MS from bacterial cultures incubated very briefly on solid medium. After plating of positive BC broth on Columbia blood agar (n = 165), MALDI-TOF MS was performed after 1.5, 2, 3, 4, 5, 6, 7, 8, 12 and (for control) 24 h of incubation until reliable identification to the species level was achieved (score ≥2.0). Mean incubation time needed to achieve species-level identification was 5.9 and 2.0 h for Gram-positive aerobic cocci (GPC, n = 86) and Gram-negative aerobic rods (GNR, n = 42), respectively. Short agar cultures with incubation times ≤2, ≤4, ≤6, ≤8 and ≤12 h yielded species identification in 1.2%, 18.6%, 64.0%, 96.5%, 98.8% of GPC, and in 76.2%, 95.2%, 97.6%, 97.6%, 97.6% of GNR, respectively. Control species identification at 24 h was achieved in 100% of GPC and 97.6% of GNR. Ethanol/formic acid protein extraction performed for an additional 34 GPC isolates cultivated from positive BCs showed further reduction in time to species identification (3.1 h). MALDI-TOF MS using biomass subsequent to very short-term incubation on solid medium allows very early and reliable bacterial identification from positive BCs without additional time and cost expenditure. © 2014 The Authors Clinical Microbiology and Infection © 2014 European Society of Clinical Microbiology and Infectious Diseases.

  1. Rapid Quantitative Chiral Amphetamines Liquid Chromatography-Tandem Mass Spectrometry Method in Plasma and Oral Fluid with a Cost-effective Chiral Derivatizing Reagent

    Science.gov (United States)

    Newmeyer, Matthew N.; Concheiro, Marta; Huestis, Marilyn A.

    2014-01-01

    Methamphetamine is a widely abused psychostimulant containing a chiral center. Consumption of over-the-counter and prescription medications may yield positive amphetamines results, but chiral separation of l- and d- methamphetamine and its metabolite amphetamine can help determine whether the source was licit or illicit. We present the first LC-MS/MS method with precolumn derivatization for methamphetamine and amphetamine chiral resolution in plasma and oral fluid collected with the Oral-Eze® and Quantisal™ devices. To 0.5 mL plasma, 0.75 mL Oral-Eze, or 1 mL Quantisal specimen racemic d11-methamphetamine and amphetamine internal standards were added, followed by protein precipitation. Samples were centrifuged and supernatants loaded onto pre-conditioned Phenomenex® Strata™-XC Polymeric Strong Cation solid phase extraction columns. After washing, analytes were eluted with 5% ammonium hydroxide in methanol. The eluate was evaporated to dryness and reconstituted in water. Derivatization was performed with 1-fluoro-2,4-dinitrophenyl-5-l-alanineamide (Marfey's reagent) and heating at 45°C for 1 h. Derivatized enantiomer separations were performed under isocratic conditions (methanol:water, 60:40) with a Phenomenex® Kinetex® 2.6 μm C18 column. Analytes were identified and quantified by two MRM transitions and their ratio on a 3200 QTrap (AB Sciex) mass spectrometer in ESI negative mode. In all three matrices, the method was linear for all enantiomers from 1-500 μg/L, with imprecision and accuracy of ≤11.3% and 85.3-108%, respectively. Extraction efficiencies ranged from 67.4-117% and matrix effects from -17.0-468%, with variation always ≤19.1%. Authentic plasma and OF specimens were collected from an IRB-approved study that included controlled Vicks® VapoInhaler™ administration. The present method is sensitive, selective, economic and rapid (separations accomplished in <10 min), and improves methamphetamine result interpretation. PMID:25065924

  2. Rapid quantitative chiral amphetamines liquid chromatography-tandem mass spectrometry: method in plasma and oral fluid with a cost-effective chiral derivatizing reagent.

    Science.gov (United States)

    Newmeyer, Matthew N; Concheiro, Marta; Huestis, Marilyn A

    2014-09-05

    Methamphetamine is a widely abused psychostimulant containing a chiral center. Consumption of over-the-counter and prescription medications may yield positive amphetamines results, but chiral separation of l- and d-methamphetamine and its metabolite amphetamine can help determine whether the source was licit or illicit. We present the first LC-MS/MS method with precolumn derivatization for methamphetamine and amphetamine chiral resolution in plasma and oral fluid collected with the Oral-Eze(®) and Quantisal™ devices. To 0.5mL plasma, 0.75mL Oral-Eze, or 1mL Quantisal specimen racemic d11-methamphetamine and amphetamine internal standards were added, followed by protein precipitation. Samples were centrifuged and supernatants loaded onto pre-conditioned Phenomenex(®) Strata™-XC Polymeric Strong Cation solid phase extraction columns. After washing, analytes were eluted with 5% ammonium hydroxide in methanol. The eluate was evaporated to dryness and reconstituted in water. Derivatization was performed with 1-fluoro-2,4-dinitrophenyl-5-l-alanineamide (Marfey's reagent) and heating at 45°C for 1h. Derivatized enantiomer separations were performed under isocratic conditions (methanol:water, 60:40) with a Phenomenex(®) Kinetex(®) 2.6μm C18 column. Analytes were identified and quantified by two MRM transitions and their ratio on a 3200 QTrap (AB Sciex) mass spectrometer in ESI negative mode. In all three matrices, the method was linear for all enantiomers from 1 to 500μg/L, with imprecision and accuracy of ≤11.3% and 85.3-108%, respectively. Extraction efficiencies ranged from 67.4 to 117% and matrix effects from -17.0 to 468%, with variation always ≤19.1%. Authentic plasma and OF specimens were collected from an IRB-approved study that included controlled Vicks(®) VapoInhaler™ administration. The present method is sensitive, selective, economic and rapid (separations accomplished in <10min), and improves methamphetamine result interpretation. Published

  3. Gram-stain plus MALDI-TOF MS (Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry for a rapid diagnosis of urinary tract infection.

    Directory of Open Access Journals (Sweden)

    Almudena Burillo

    Full Text Available Microbiological confirmation of a urinary tract infection (UTI takes 24-48 h. In the meantime, patients are usually given empirical antibiotics, sometimes inappropriately. We assessed the feasibility of sequentially performing a Gram stain and MALDI-TOF MS mass spectrometry (MS on urine samples to anticipate clinically useful information. In May-June 2012, we randomly selected 1000 urine samples from patients with suspected UTI. All were Gram stained and those yielding bacteria of a single morphotype were processed for MALDI-TOF MS. Our sequential algorithm was correlated with the standard semiquantitative urine culture result as follows: Match, the information provided was anticipative of culture result; Minor error, the information provided was partially anticipative of culture result; Major error, the information provided was incorrect, potentially leading to inappropriate changes in antimicrobial therapy. A positive culture was obtained in 242/1000 samples. The Gram stain revealed a single morphotype in 207 samples, which were subjected to MALDI-TOF MS. The diagnostic performance of the Gram stain was: sensitivity (Se 81.3%, specificity (Sp 93.2%, positive predictive value (PPV 81.3%, negative predictive value (NPV 93.2%, positive likelihood ratio (+LR 11.91, negative likelihood ratio (-LR 0.20 and accuracy 90.0% while that of MALDI-TOF MS was: Se 79.2%, Sp 73.5, +LR 2.99, -LR 0.28 and accuracy 78.3%. The use of both techniques provided information anticipative of the culture result in 82.7% of cases, information with minor errors in 13.4% and information with major errors in 3.9%. Results were available within 1 h. Our serial algorithm provided information that was consistent or showed minor errors for 96.1% of urine samples from patients with suspected UTI. The clinical impacts of this rapid UTI diagnosis strategy need to be assessed through indicators of adequacy of treatment such as a reduced time to appropriate empirical treatment or

  4. Hannah Arendt : la part de l’art dans la constitution d’un monde commun d’apparence

    Directory of Open Access Journals (Sweden)

    Alain Cambier

    2007-05-01

    Full Text Available Que l’art puisse participer à l’édification d’un monde humain est une idée qu’Hannah Arendt a repensée dans Condition de l’homme moderne. S’il est vrai que l’apparence comme manifestation est la seule voie d’accès à l’Être, l’art nous y initie puisqu’il a vocation à déployer entre l’artiste et son public un espace commun d’apparence. L’éclat des œuvres d’art contribue à garantir l’objectivité de notre monde parce qu’elles sont destinées traditionnellement à se maintenir durablement dans l’espace public. Mais certains ont cru s’autoriser d’Hannah Arendt pour condamner l’art contemporain au motif qu’il se fourvoierait dans l’éphémère. C’est oublier que l’art ne se réduit pas à une poiésis artisanale : loin de se présenter comme l’accomplissement d’une fin, il se manifeste davantage comme commencement. En mettant en évidence la capacité proprement humaine de commencer quelque chose, l’art contemporain relève d’une expérience de liberté, au même titre que la praxis politique ou éthique. Il nous révèle aussi que si l’œuvre d’art est chose du monde, elle ne vaut pourtant que dans la mesure où elle ouvre le public à un champ de possibles insoupçonnés qui renouvelle sa perception du monde.That Art can participate in the formation of a human world is an idea rethought by Hannah Arendt in « The Human Condition ». If it’s true that appearance in itself is the only way of access to being, art initiates us since it is known for opening a common ground of appearance between the artist and the public. The splendour of works of art contributes to the worldly reality since they are traditionally destined to last in a public place. Some have used Hannah Arendt’s authority to condemn contempory art giving as a pretext it loses itself in momentariness. That means forgetting that art cannot be reduced to « handmade »: far from presenting itself as an

  5. Neutral fragment filtering for rapid identification of new diester-diterpenoid alkaloids in roots of Aconitum carmichaeli by ultra-high-pressure liquid chromatography coupled with linear ion trap-orbitrap mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Jing Zhang

    Full Text Available A rapid and effective method was developed for separation and identification of diester-diterpenoid alkaloids (DDA in the roots of Aconitum carmichaeli by ultra-high-pressure liquid chromatography coupled with high resolution LTQ-Orbitrap tandem mass spectrometry (UHPLC-LTQ-Orbitrap-MS(n. According to accurate mass measurement and the characteristic neutral loss filtering strategy, a total of 42 diester-diterpenoid alkaloids (DDA were rapidly detected and characterized or tentatively identified. Meanwhile, the proposed fragmentation pathways and the major diagnostic fragment ions of aconitine, mesaconitine and hypaconitine were investigated to trace DDA derivatives in crude plant extracts. 23 potential new compounds were successfully screened and characterized in Aconitum carmichaeli, including 16 short chain fatty acyls DDA, 4 N-dealkyl DDA and several isomers of aconitine, mesaconitine and hypaconitine.

  6. An Ultra-Performance Liquid Chromatoghraphy-Tandem Mass Spectrometry (UPLC-MS/MS) Method for the Rapid and Sensitive Determination of Sulforaphane and Sulforaphane Nitrile in Brassica Vegetables

    OpenAIRE

    Alvarez Jubete, Laura; Smyth, Thomas J.; Valverde, Juan; Rai, Dilip K.; Barry-Ryan, Catherine

    2013-01-01

    A rapid UPLC-MS/MS method has been developed and validated for the simultaneous analysis of sulforaphane and sulforaphane nitrile from Brassica Oleracea L. This method was developed utilising an Acquity BEH C8 column with gradient elution combined with tandem mass spectrometry detection, using positive ion electrospray ionisation in multiple reaction monitoring (MRM) mode. The method was validated for linearity, sensitivity, precision, accuracy, matrix effects and recovery. The retention time...

  7. Rapid and sensitive method for quantification of gestodene in human plasma as the oxime derivative by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and its application to bioequivalence study.

    Science.gov (United States)

    Saxena, Ashish; Gupta, Arun; Kasibhatta, Ravisekhar; Bob, Manoj; Kumar, V Praveen; Purwar, Bipin

    2014-01-15

    A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the estimation of gestodene in human plasma. Gestodene was extracted from human plasma by using solid-phase extraction technique. Gestodene D6 was used as the internal standard. An Acquity HSS-T3 column provided chromatographic separation of analytes followed by detection with mass spectrometry. The mass transition ion-pair was followed as m/z 326.2→124.1 for gestodene and m/z 332.3→129.1 for gestodene D6. The method involves a solid phase extraction from plasma, rapid derivatization with hydroxylamine to form oxime, simple gradient chromatographic conditions and mass spectrometric detection that enables detection at sub-picogram levels. The proposed method has been validated for a linear range of 50-11957pg/ml with a correlation coefficient≥0.9994. The intra-run and inter-run precision and accuracy were within 10%. The overall recoveries for gestodene and gestodene D6 were 62.02% and 67.57% respectively. The total run time was 4.0min. The developed method was applied for the determination of the pharmacokinetic parameters of gestodene following a single oral administration of a 2×0.06mg gestodene tablets in 10 healthy female volunteers. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Rapid Determination of Plutonium Isotopes in Environmental Samples Using Sequential Injection Extraction Chromatography and Detection by Inductively Coupled Plasma Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2009-01-01

    This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed by det...

  9. Rapid Quantitative Analysis of Multiple Explosive-Compound Classes on a Single Instrument via Flow-Injection Analysis Tandem Mass Spectrometry

    Science.gov (United States)

    2017-03-20

    criminal  forensics,  [11]  rapid  sample screening, [12,13,14,15] and trace‐evidence chem‐ ical  imaging [16,17,18]. Explosives detection has also  pro ...date,  FIA‐ MS/MS  has  been  used  for  rapid  quantitative  analysis  of  pharmaceuticals  [33],  pesticides   [34], environmental con‐ taminants...the literature reference listed  in the reference section of this paper.    As shown  in the Table 3 FIA ESI/APCI MSMS  pro ‐ vides quick and sensitive

  10. Rapid activity-directed screening of estrogens by parallel coupling of liquid chromatography with a functional gene reporter assay and mass spectrometry

    NARCIS (Netherlands)

    Jonker, W.; Lamoree, M.H.; Houtman, C.J.; Hamers, T.; Somsen, G.W.; Kool, J.

    2015-01-01

    In this study we developed a new LC nanofractionation platform that combines a human cell (BG1.Luc) gene reporter assay with a high resolution mass spectrometer for the detection and identification of estrogenic and anti-estrogenic compounds in environmental waters. The selection of this assay was

  11. Energy dependence of acceptance-corrected dielectron excess mass spectrum at mid-rapidity in Au+Au collisions at sNN=19.6 and 200 GeV

    Directory of Open Access Journals (Sweden)

    L. Adamczyk

    2015-11-01

    Full Text Available The acceptance-corrected dielectron excess mass spectra, where the known hadronic sources have been subtracted from the inclusive dielectron mass spectra, are reported for the first time at mid-rapidity |yee|<1 in minimum-bias Au+Au collisions at sNN=19.6 and 200 GeV. The excess mass spectra are consistently described by a model calculation with a broadened ρ spectral function for Mee<1.1 GeV/c2. The integrated dielectron excess yield at sNN=19.6 GeV for 0.4rapidity, has a value similar to that in In+In collisions at sNN=17.3 GeV. For sNN=200 GeV, the normalized excess yield in central collisions is higher than that at sNN=17.3 GeV and increases from peripheral to central collisions. These measurements indicate that the lifetime of the hot, dense medium created in central Au+Au collisions at sNN=200 GeV is longer than those in peripheral collisions and at lower energies.

  12. Les accidents du travail dans le transport urbain en commun de la ville province de Kinshasa, République Démocratique du Congo: une étude transversale descriptive

    Science.gov (United States)

    Wangata, Jemima; Elenge, Myriam; De Brouwer, Christophe

    2014-01-01

    Introduction Le transport en commun urbain constitue un secteur où les travailleurs sont très exposés aux accidents du travail. Cette étude visait une description épidémiologique des accidents du travail dans le secteur informel du transport en commun à Kinshasa en vue d'apporter les pistes d'amélioration de la sécurité des travailleurs dans cette activité. Méthodes Un questionnaire sur les accidents du travail, administré en Décembre 2012 a permis d'explorer les tendances significatives entre les accidents et leurs circonstances, leurs facteurs associés, leurs conséquences au sein d'une population des travailleurs (n = 472) du transport en commun à Kinshasa. Résultats Durant les 12 derniers précédant l’étude 76.5% des travailleurs ont connu au moins un accident du travail, 54,8% ont connu un arrêt d'au moins 1jour. Les accidents liés à la circulation routière étaient plus important suivis des chutes. Les facteurs ayant montré des différences significatives étaient le travail sous l'influence de l'alcool et le port des équipements de protection individuelle. Les plaies (46,3%) et les contusions (39,4%) étaient les lésions les plus courantes. Les membres supérieurs (51,3%) et inférieurs (30,7%) étaient les plus atteints. 76,6% des travailleurs ont assumé seuls leur prise en charge médicale. Conclusion L'incidence des accidents du travail dans ce secteur est très élevée. La mise en place d'une politique de prévention et gestion de différents facteurs associés ainsi qu'un système de déclaration d'accidents est nécessaire dans ce secteur. Les patrons ainsi que les politiques devraient veiller à une prise en charge médicale correcte pour des travailleurs accidentés. PMID:25667703

  13. Development of a Rapid and Accurate Identification Method for Citrobacter Species Isolated from Pork Products Using a Matrix-Assisted Laser-Desorption Ionization Time-of-Flight Mass Spectrometry (MALDI-TOF MS).

    Science.gov (United States)

    Kwak, Hye-Lim; Han, Sun-Kyung; Park, Sunghoon; Park, Si Hong; Shim, Jae-Yong; Oh, Mihwa; Ricke, Steven C; Kim, Hae-Yeong

    2015-09-01

    Previous detection methods for Citrobacter are considered time consuming and laborious. In this study, we have developed a rapid and accurate detection method for Citrobacter species in pork products, using matrix-assisted laser desorption ionization time-of-flight (MALDI-TOF) mass spectrometry (MS). A total of 35 Citrobacter strains were isolated from 30 pork products and identified by both MALDI-TOF MS and 16S rRNA gene sequencing approaches. All isolates were identified to the species level by the MALDI-TOF MS, while 16S rRNA gene sequencing results could not discriminate them clearly. These results confirmed that MALDI-TOF MS is a more accurate and rapid detection method for the identification of Citrobacter species.

  14. Rapid Differentiation of Haemophilus influenzae and Haemophilus haemolyticus by Use of Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry with ClinProTools Mass Spectrum Analysis.

    Science.gov (United States)

    Chen, Jonathan H K; Cheng, Vincent C C; Wong, Chun-Pong; Wong, Sally C Y; Yam, Wing-Cheong; Yuen, Kwok-Yung

    2017-09-01

    Haemophilus influenzae is associated with severe invasive disease, while Haemophilus haemolyticus is considered part of the commensal flora in the human respiratory tract. Although the addition of a custom mass spectrum library into the matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) system could improve identification of these two species, the establishment of such a custom database is technically complicated and requires a large amount of resources, which most clinical laboratories cannot afford. In this study, we developed a mass spectrum analysis model with 7 mass peak biomarkers for the identification of H. influenzae and H. haemolyticus using the ClinProTools software. We evaluated the diagnostic performance of this model using 408 H. influenzae and H. haemolyticus isolates from clinical respiratory specimens from 363 hospitalized patients and compared the identification results with those obtained with the Bruker IVD MALDI Biotyper. The IVD MALDI Biotyper identified only 86.9% of H. influenzae (311/358) and 98.0% of H. haemolyticus (49/50) clinical isolates to the species level. In comparison, the ClinProTools mass spectrum model could identify 100% of H. influenzae (358/358) and H. haemolyticus (50/50) clinical strains to the species level and significantly improved the species identification rate (McNemar's test, P mass spectrometry to handle closely related bacterial species when the proprietary spectrum library failed. This approach should be useful for the differentiation of other closely related bacterial species. Copyright © 2017 American Society for Microbiology.

  15. Rapid fingerprinting of sterols and related compounds in vegetable and animal oils and phytosterol enriched- margarines by transmission mode direct analysis in real time mass spectrometry.

    Science.gov (United States)

    Alberici, Rosana M; Fernandes, Gabriel D; Porcari, Andréia M; Eberlin, Marcos N; Barrera-Arellano, Daniel; Fernández, Facundo M

    2016-11-15

    Plant-derived sterols, often referred to as phytosterols, are important constituents of plant membranes where they assist in maintaining phospholipid bilayer stability. Consumption of phytosterols has been suggested to positively affect human health by reducing cholesterol levels in blood via inhibition of its absorption in the small intestine, thus protecting against heart attack and stroke. Sterols are challenging analytes for mass spectrometry, since their low polarity makes them difficult to ionize by both electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI), typically requiring derivatization steps to overcome their low ionization efficiencies. We present a fast and reliable method to characterize the composition of phytosterols in vegetable oils and enriched margarines. The method requires no derivatization steps or sample extraction procedures thanks to the use of transmission mode direct analysis in real time mass spectrometry (TM-DART-MS). Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. A multiple-dimension liquid chromatography coupled with mass spectrometry data strategy for the rapid discovery and identification of unknown compounds from a Chinese herbal formula (Er-xian decoction).

    Science.gov (United States)

    Wang, Caihong; Zhang, Jinlan; Wu, Caisheng; Wang, Zhe

    2017-10-06

    It is very important to rapidly discover and identify the multiple components of traditional Chinese medicine (TCM) formula. High performance liquid chromatography with high resolution tandem mass spectrometry (HPLC-HRMS/MS) has been widely used to analyze TCM formula and contains multiple-dimension data including retention time (RT), high resolution mass (HRMS), multiple-stage mass spectrometric (MSn), and isotope intensity distribution (IID) data. So it is very necessary to exploit a useful strategy to utilize multiple-dimension data to rapidly probe structural information and identify chemical compounds. In this study, a new strategy to initiatively use the multiple-dimension LC-MS data has been developed to discover and identify unknown compounds of TCM in many styles. The strategy guarantees the fast discovery of candidate structural information and provides efficient structure clues for identification. The strategy contains four steps in sequence: (1) to discover potential compounds and obtain sub-structure information by the mass spectral tree similarity filter (MTSF) technique, based on HRMS and MSn data; (2) to classify potential compounds into known chemical classes by discriminant analysis (DA) on the basis of RT and HRMS data; (3) to hit the candidate structural information of compounds by intersection sub-structure between MTSF and DA (M,D-INSS); (4) to annotate and confirm candidate structures by IID data. This strategy allowed for the high exclusion efficiency (greater than 41%) of irrelevant ions in er-xian decoction (EXD) while providing accurate structural information of 553 potential compounds and identifying 66 candidates, therefore accelerating and simplifying the discovery and identification of unknown compounds in TCM formula. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Determination of red blood cell fatty acid profiles: Rapid and high-confident analysis by chemical ionization-gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Schober, Yvonne; Wahl, Hans Günther; Renz, Harald; Nockher, Wolfgang Andreas

    2017-01-01

    Cellular fatty acid (FA) profiles have been acknowledged as biomarkers in various human diseases. Nevertheless, common FA analysis by gas chromatography mass spectrometry (GC-MS) requires long analysis time. Hence, there is a need for feasible methods for high throughput analysis in clinical studies. FA was extracted from red blood cells (RBC) and derivatized to fatty acid methyl esters (FAME). A method using gas chromatography tandem mass spectrometry (GC-MS/MS) with ammonia-induced chemical ionization (CI) was developed for the analysis of FA profiles in human RBC. We compared this method with classical single GC-MS using electron impact ionization (EI). The FA profiles of 703 RBC samples were determined by GC-MS/MS. In contrast to EI ammonia-induced CI resulted in adequate amounts of molecular ions for further fragmentation of FAME. Specific fragments for confident quantification and fragmentation were determined for 45 FA. The GC-MS/MS method has a total run time of 9min compared to typical analysis times of up to 60min in conventional GC-MS. Intra and inter assay variations were Analysis of RBC FA composition revealed an age-dependent increase of the omega-3 eicosapentaenoic and docosahexaenoic acid, and a decline of the omega-6 linoleic acid with a corresponding rise of the omega-3 index. The combination of ammonia-induced CI and tandem mass spectrometry after GC separation allows for high-throughput, robust and confident analysis of FA profiles in the clinical laboratory. Copyright © 2016. Published by Elsevier B.V.

  18. Matrix-assisted laser desorption/ionization mass spectrometric imaging for the rapid segmental analysis of methamphetamine in a single hair using umbelliferone as a matrix.

    Science.gov (United States)

    Wang, Hang; Wang, Ying

    2017-07-04

    Segmental hair analysis offers a longer period for retrospective drug detection than blood or urine. Hair is a keratinous fiber and is strongly hydrophobic. The embedding of drugs in hydrophobic hair at low concentrations makes it difficult for extraction and detection with matrix-assisted laser desorption/ionization (MALDI) coupled with mass spectrometric imaging (MSI). In this study, a single scalp hair was longitudinally cut with a cryostat section to a length of 4 mm and fixed onto a stainless steel MALDI plate. Umbelliferone was used as a new hydrophobic matrix to enrich and assist the ionization efficiency of methamphetamine in the hair sample. MALDI-Fourier transform ion cyclotron resonance (FTICR)-MS profiling and imaging were performed for direct detection and mapping of methamphetamine on the longitudinal sections of the single hair sample in positive ion mode. Using MALDI-MSI, the distribution of methamphetamine was observed throughout five longitudinally sectioned hair samples from a drug abuser. The changes of methamphetamine were also semi-quantified by comparing the ratios of methamphetamine/internal standard (I.S). This method improves the detection sensitivity of target drugs embedded in a hair matrix for imaging with mass spectrometry. The method could provide a detection level of methamphetamine down to a nanogram per milligram incorporated into hair. The results were also compared with the conventional high performance liquid chromatography -tandem mass spectrometry (HPLC-MS/MS) method. Changes in the imaging results over time by the MSI method showed good semi-quantitative correlation to the results from the HPLC-MS/MS method. This study provides a powerful tool for drug abuse control and forensic medicine analysis in a narrow time frame, and a reduction in the sample amount required. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. An electrospray/inductively coupled plasma dual-source time-of-flight mass spectrometer for rapid metallomic and speciation analysis. Part 1. Molecular channel characterization.

    Science.gov (United States)

    Rogers, Duane A; Ray, Steven J; Hieftje, Gary M

    2010-04-01

    A new time-of-flight mass spectrometer has been developed that uses an electrospray source and an inductively coupled plasma to extract molecular, atomic, and isotopic information simultaneously from a single sample. This paper will focus on characterization of the ESI channel. Sensitivities are reported for hexadecyltrimethylammonium, tetrahexylammonium, tetraoctylammonium, myoglobin, insulin, cyanocobalamin, leucine enkephalin, and alcohol dehydrogenase. Skimmer-nozzle collisionally induced dissociation is explored for adduct removal and analyte fragmentation on the ESI channel for tetraoctylammonium ion and leucine enkephalin. Long-term and short-term spray stability is also examined.

  20. Desorption Electrospray Ionization Mass Spectrometry (DESI-MS) Analysis of Organophosphorus Chemical Warfare Agents: Rapid Acquisition of Time-Aligned Parallel (TAP) Fragmentation Data

    Science.gov (United States)

    2010-06-01

    Résumé …..... On a appliqué la méthode désorption - ionisation par électronébulisation - spectrométrie de masse (DESI-SM) pour l’analyse...2010-047, R & D pour la défense Canada – Suffield; Juin 2010. Introduction : On a appliqué la méthode désorption – ionisation par...132, 868-875. DRDC Suffield TM 2010-047 29 [26] Williams, J.P. and Scrivens, J.H. (2008). Coupling desorption electrospray ionisation with

  1. Rapid identification of positive blood cultures by matrix-assisted laser desorption ionization-time of flight mass spectrometry using prewarmed agar plates.

    Science.gov (United States)

    Bhatti, M M; Boonlayangoor, S; Beavis, K G; Tesic, V

    2014-12-01

    This study describes an inexpensive and straightforward method for identifying bacteria by matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) directly from positive blood cultures using prewarmed agar plates. Different inoculation methods and incubation times were evaluated to determine the optimal conditions. The two methods using pelleted material from positive culture bottles performed best. In particular, the pellet streak method correctly identified 94% of the Gram negatives following 4 h of incubation and 98% of the Gram positives following 6 h of incubation. Copyright © 2014, American Society for Microbiology. All Rights Reserved.

  2. Rapid and simultaneous determination of neptunium and plutonium in environmental samples using anion exchange chromatographic and sequential injection setup combined with inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jixin Qiao; Hou, X.; Roos, P. (Technical Univ. of Denmark, Risoe National Lab. for Sustainable Energy. Radiation Research Div., Roskilde (Denmark)); Miro, M. (Univ. of the Balearic Islands, Dept. of Chemistry, Faculty of Sciences, Palma de Mallorca (Spain))

    2010-03-15

    Full text: This paper presents an automated analytical method for the rapid and simultaneous determination of Pu and Np in the environmental samples. Anion exchange chromatographic column was incorporated in a sequential injection system to actualize the automated separation of Pu isotpes along with 237Np from the matrix elements and interfering radionuclides. K{sub 2}S{sub 2}O{sub 5}-conc. HNO{sub 3} was applied as redox reagents for the valence adjustment and stabilization of Pu(IV) and Np(IV). 242Pu preformed well as a tracer for both Pu isotopes and 237Np. It was observed that the cross-link and particle size of the resins had significant effluence on the separation efficiency and anion exchange resin Bio-Rad AG 1 x 4 with the particle size of 100-200 mesh was chosen as the optimum. The investigation on the capacity showed small-sized column packed with 2mL resin sufficed up to 50g of soil sample, which provides an advantage of low consumption of the resin and low generation of acid waste after the column washing. The analytical results for Pu and Np in three reference materials showed good agreement with the certified or reference values at the 0.05 significance level. Chemical yields of Pu and Np equally range from 80% to 100%, and the decontamination factors for uranium, thorium and lead were in the range of 103 to 104. The total time of separation for a single sample was < 2.5 hours, which extremely improve the analysis efficiency and reduces the labor intensity, as well as enables a rapid determination of Pu and Np in emergency situations. (author)

  3. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples

    Directory of Open Access Journals (Sweden)

    E. Gerace

    2012-02-01

    Full Text Available A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid–liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration. Keywords: Anti-estrogens, Fast-GC/MS, Urine screening, Validation, Breast cancer

  4. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples

    Science.gov (United States)

    Gerace, E.; Salomone, A.; Abbadessa, G.; Racca, S.; Vincenti, M.

    2011-01-01

    A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid–liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

  5. Rapid identification of Vibrio parahaemolyticus isolated from shellfish, sea water and sediments of the Khnifiss lagoon, Morocco, by MALDI-TOF mass spectrometry.

    Science.gov (United States)

    Malainine, S M; Moussaoui, W; Prévost, G; Scheftel, J-M; Mimouni, R

    2013-05-01

    We establish the presence of Vibrio parahaemolyticus and deepen the comparison of isolates using MALDI-TOF MS for the typing of isolates originating from the Khnifiss lagoon (Morocco). Amongst 48 samples from sea water, sediment and shellfish isolated from different sites of Khnifiss lagoon, Morocco, we obtained 22 isolates of V. parahaemolyticus identified by Vitek 2™ System (bioMérieux) and MALDI Biotyper™ (Bruker Daltonics). All isolates were highly resistant to ampicillin and ticarcillin, moderately resistant to cefalotin, but sensitive to 16 other antimicrobials tested. MALDI-TOF MS was used to discriminate between closely related environmental strains of V. parahaemolyticus. A clustering and distribution based on MALDI-TOF spectra were generated using the BioTyper 1.1™ software. Despite low diversity in regard to the biochemical characteristics and antimicrobial resistance, the isolates evoke a larger biodiversity when analysed through mass spectra of abundant proteins. Different evaluations of a cut-off value showed that, when placed at a 10% threshold of the whole diversity, isolates differed by at least three mass peaks. © 2013 The Society for Applied Microbiology.

  6. Early Holocene (8.6 ka) rock avalanche deposits, Obernberg valley (Eastern Alps): Landform interpretation and kinematics of rapid mass movement.

    Science.gov (United States)

    Ostermann, Marc; Sanders, Diethard; Ivy-Ochs, Susan; Alfimov, Vasily; Rockenschaub, Manfred; Römer, Alexander

    2012-10-15

    In the Obernberg valley, the Eastern Alps, landforms recently interpreted as moraines are re-interpreted as rock avalanche deposits. The catastrophic slope failure involved an initial rock volume of about 45 million m³, with a runout of 7.2 km over a total vertical distance of 1330 m (fahrböschung 10°). 36Cl surface-exposure dating of boulders of the avalanche mass indicates an event age of 8.6 ± 0.6 ka. A 14C age of 7785 ± 190 cal yr BP of a palaeosoil within an alluvial fan downlapping the rock avalanche is consistent with the event age. The distal 2 km of the rock-avalanche deposit is characterized by a highly regular array of transverse ridges that were previously interpreted as terminal moraines of Late-Glacial. 'Jigsaw-puzzle structure' of gravel to boulder-size clasts in the ridges and a matrix of cataclastic gouge indicate a rock avalanche origin. For a wide altitude range the avalanche deposit is preserved, and the event age of mass-wasting precludes both runout over glacial ice and subsequent glacial overprint. The regularly arrayed transverse ridges thus were formed during freezing of the rock avalanche deposits.

  7. Ultra-high performance liquid chromatography with linear ion trap-Orbitrap hybrid mass spectrometry combined with a systematic strategy based on fragment ions for the rapid separation and characterization of components in Stellera chamaejasme extracts.

    Science.gov (United States)

    Wang, Zhixin; Qu, Yang; Wang, Li; Zhang, Xiaozhe; Xiao, Hongbin

    2016-04-01

    Stellera chamaejasme, a famous toxic herb, has been used in traditional Chinese medicine to treat various diseases. For decades, increasing attention in modern pharmacological studies has been drawn to S. chamaejasme because of its potential anti-tumor, anti-virus, and anti-fungus activities. However, due to the intrinsic complexity of chemical constitutes, hardly any investigations formed an overall recognition for the chemical profiles of this herb. In this study, a rapid and sensitive ultra-high performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry method was developed to characterize the chemical components of S. chamaejasme extracts. Based on optimized ultra-high performance liquid chromatography and mass spectrometry conditions and systematic fragment ions-based strategy, a total of 47 components including flavones, diterpenes, coumarins, and lignans were simultaneously detected and identified or tentatively identified for the first time. The MS(n) fragmentation patterns of all the characterized compounds in positive or negative electrospray ionization modes were also explored and summarized. These results provided essential data for further pharmacological research on S. chamaejasme. Moreover, the method was demonstrated to be an efficient tool for rapid qualitative analysis of secondary metabolites from natural resources. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Rapid Screening for Potential Epitopes Reactive with a Polycolonal Antibody by Solution-Phase H/D Exchange Monitored by FT-ICR Mass Spectrometry

    Science.gov (United States)

    Zhang, Qian; Noble, Kyle A.; Mao, Yuan; Young, Nicolas L.; Sathe, Shridhar K.; Roux, Kenneth H.; Marshall, Alan G.

    2013-07-01

    The potential epitopes of a recombinant food allergen protein, cashew Ana o 2, reactive to polyclonal antibodies, were mapped by solution-phase amide backbone H/D exchange (HDX) coupled with Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS). Ana o 2 polyclonal antibodies were purified in the serum from a goat immunized with cashew nut extract. Antibodies were incubated with recombinant Ana o 2 (rAna o 2) to form antigen:polyclonal antibody (Ag:pAb) complexes. Complexed and uncomplexed (free) rAna o 2 were then subjected to HDX-MS analysis. Four regions protected from H/D exchange upon pAb binding are identified as potential epitopes and mapped onto a homologous model.

  9. Orbital and physical parameters of eclipsing binaries from the All-Sky Automated Survey catalogue. III. Two new low-mass systems with rapidly evolving spots

    Science.gov (United States)

    Hełminiak, K. G.; Konacki, M.; Złoczewski, K.; Ratajczak, M.; Reichart, D. E.; Ivarsen, K. M.; Haislip, J. B.; Crain, J. A.; Foster, A. C.; Nysewander, M. C.; Lacluyze, A. P.

    2011-03-01

    Aims: We present the results of our spectroscopic and photometric analysis of two newly discovered low-mass detached eclipsing binaries found in the All-Sky Automated Survey (ASAS) catalogue: ASAS J093814-0104.4 and ASAS J212954-5620.1. Methods: Using the Grating Instrument for Radiation Analysis with a Fibre-Fed Echelle (GIRAFFE) on the 1.9-m Radcliffe telescope at the South African Astronomical Observatory (SAAO) and the University College London Echelle Spectrograph (UCLES) on the 3.9-m Anglo-Australian Telescope, we obtained high-resolution spectra of both objects and derived their radial velocities (RVs) at various orbital phases. The RVs of both objects were measured with the two-dimensional cross-correlation technique (TODCOR) using synthetic template spectra as references. We also obtained V and I band photometry using the 1.0-m Elizabeth telescope at SAAO and the 0.4-m Panchromatic Robotic Optical Monitoring and Polarimetry Telescopes (PROMPT) located at the Cerro Tololo Inter-American Observatory (CTIO). The orbital and physical parameters of the systems were derived with PHOEBE and JKTEBOP codes. We compared our results with several sets of widely-used isochrones. Results: Our multi-epoch photometric observations demonstrate that both objects show significant out-of-eclipse modulations, which vary in time. We believe that this effect is caused by stellar spots, which evolve on time scales of tens of days. For this reason, we constructed our models on the basis of photometric observations spanning short time scales (less than a month). Our modeling indicates that (1) ASAS J093814-0104.04 is a main sequence active system with nearly-twin components with masses of M1 = 0.771 ± 0.033 M⊙, M2 = 0.768 ± 0.021 M⊙ and radii of R1 = 0.772 ± 0.012 R⊙ and R2 = 0.769 ± 0.013 R⊙. (2) ASAS J212954-5620.1 is a main sequence active binary with component masses of M1 = 0.833 ± 0.017 M⊙, M2 = 0.703 ± 0.013 M⊙ and radii of R1 = 0.845 ± 0.012 R⊙ and R2

  10. Reagent Precoated Targets for Rapid In-Tissue Derivatization of the Anti-Tuberculosis Drug Isoniazid Followed by MALDI Imaging Mass Spectrometry

    Science.gov (United States)

    Manier, M. Lisa; Reyzer, Michelle L.; Goh, Anne; Dartois, Veronique; Via, Laura E.; Barry, Clifton E.; Caprioli, Richard M.

    2011-08-01

    Isoniazid (INH) is an important component of front-line anti-tuberculosis therapy with good serum pharmacokinetics but unknown ability to penetrate tuberculous lesions. However, endogenous background interferences hinder our ability to directly analyze INH in tissues. Chemical derivatization has been successfully used to measure isoniazid directly from tissue samples using matrix-assisted laser desorption/ionization (MALDI) imaging mass spectrometry (IMS). MALDI targets were pretreated with trans-cinnamaldehyde (CA) prior to mounting tissue slices. Isoniazid present in the tissues was efficiently derivatized and the INH-CA product measured by MS/MS. Precoating of MALDI targets allows the tissues to be directly thaw-mounted and derivatized, thus simplifying the preparation. A time-course series of tissues from tuberculosis infected/INH dosed animals were assayed and the MALDI MS/MS response correlates well with the amount of INH determined to be in the tissues by high-performance liquid chromatography (HPLC)-MS/MS.

  11. Early Holocene (8.6 ka) rock avalanche deposits, Obernberg valley (Eastern Alps): Landform interpretation and kinematics of rapid mass movement

    OpenAIRE

    Ostermann, Marc; Sanders, Diethard; Ivy-Ochs, Susan; Alfimov, Vasily; Rockenschaub, Manfred; Römer, Alexander

    2012-01-01

    In the Obernberg valley, the Eastern Alps, landforms recently interpreted as moraines are re-interpreted as rock avalanche deposits. The catastrophic slope failure involved an initial rock volume of about 45 million m³, with a runout of 7.2 km over a total vertical distance of 1330 m (fahrböschung 10°). 36Cl surface-exposure dating of boulders of the avalanche mass indicates an event age of 8.6 ± 0.6 ka. A 14C age of 7785 ± 190 cal yr BP of a palaeosoil within an alluvial fan downlapping the ...

  12. Rapid liquid chromatography/tandem mass spectrometer (LCMS) method for clozapine and its metabolite N-desmethyl clozapine (norclozapine) in human serum.

    Science.gov (United States)

    Rao, L V; Snyder, M L; Vallaro, G M

    2009-01-01

    Clozapine is indicated for the treatment of schizophrenia and related psychotic disorders. Several methods have been developed for monitoring Clozapine levels; however, they possess limited specificity and are often laborious. This study describes a simple liquid chromatography/tandem mass spectrometer (LCMS) method in human serum. The ion transitions monitored were m/z 327, 270, 296 for Clozapine, m/z 313, 192, 227 for Norclozapine and m/z 328, 271 for Loxapine. The assay is linear (25-1000 ng/ml) and showed a good correlation (r=0.98) within the analytical range of 79-1210 ng/ml in human serum. This assay is highly specific and sensitive for the simultaneous measurements of Clozapine and Norclozapine. The simplification of this assay makes it ideal for high throughput analyses of the patient samples in a routine clinical laboratory staffed with general medical technologists.

  13. Rapid screening and identification of multi-class substances of very high concern in textiles using liquid chromatography-hybrid linear ion trap orbitrap mass spectrometry.

    Science.gov (United States)

    Zhang, Li; Luo, Xin; Niu, Zengyuan; Ye, Xiwen; Tang, Zhixu; Yao, Peng

    2015-03-20

    A new analytical method was established and validated for the analysis of 19 substances of very high concern (SVHCs) in textiles, including phthalic acid esters (PAEs), organotins (OTs), perfluorochemicals (PFCs) and flame retardants (FRs). After ultrasonic extraction in methanol, the textile samples were analyzed by high performance liquid chromatography-hybrid linear ion trap Orbitrap high resolution mass spectrometry (HPLC-LTQ/Orbitrap). The values of LOQ were in the range of 2-200mg/kg. Recoveries at two levels (at the LOQ and at half the limit of regulation) ranged from 68% to 120%, and the repeatability was lower than 13%. This method was successfully applied to the screening of SVHCs in commercial textile samples and is useful for the fast screening of various SVHCs. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. APPLICATION METHOD OF ANTIMICROBIAL SUB -STANCES FOR THE CONTROL OF schiZophyllum commuN e FR. CAUSING BROWN GERM AND SEED ROT OF OIL PALM

    Directory of Open Access Journals (Sweden)

    ANTARIO DIKIN

    2008-01-01

    Full Text Available Biological seed treatment promotes to save the environment from toxic chemicals in the agricultural practices. Schizophyllum commune is one of the important seedborne pathogenic fungi causing brown germ and seed rot of oil palm which required effective and efficient treat -ment based on environmental friendly approaches. Anti-microbial substances are extracted from antagonistic bacteria of B. multivorans and M. testaceum after mass production in the liquid media. Application method of anti-microbial substances for the control of Schizophylllum commune was done by seed dipping for 30 minutes and vacuum infiltration at 400 mm Hg. vac. for 2 min. in supernatant of anti-microbial substances diluted in sterilized distilled water with concentra -tion ratio of 1:4. Application method using anti-microbial substances from antagonistic bacteria inhibited the growth of pathogenic fungus, enhanced seed germination, and without causing any abnormal growth of oil palm seedlings.

  15. Stability evaluation and sensitive determination of antiviral drug, valacyclovir and its metabolite acyclovir in human plasma by a rapid liquid chromatography-tandem mass spectrometry method.

    Science.gov (United States)

    Yadav, Manish; Upadhyay, Vivek; Singhal, Puran; Goswami, Sailendra; Shrivastav, Pranav S

    2009-03-15

    A simple, sensitive and high throughput liquid chromatography/positive-ion electrospray ionization mass spectrometry (LC-ESI-MS/MS) method has been developed for the simultaneous determination of valacyclovir and acyclovir in human plasma using fluconazole as internal standard (IS). The method involved solid phase extraction of the analytes and IS from 0.5 mL human plasma with no reconstitution and drying steps (direct injection of eluate). The chromatographic separation was achieved on a Gemini C18 analytical column using isocratic mobile phase, consisting of 0.1% formic acid and methanol (30:70 v/v), at a flow-rate of 0.8 mL/min. The precursor-->product ion transition for valacyclovir (m/z 325.2-->152.2), acyclovir (m/z 226.2-->152.2) and IS (m/z 307.1-->220.3) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) mode. The method was validated over the concentration range 5.0-1075 ng/mL and 47.6-10225 ng/mL for valacyclovir and acyclovir respectively. The mean recovery of valacyclovir (92.2%), acyclovir (84.2%) and IS (103.7%) from spiked plasma samples was consistent and reproducible. The bench top stability of valacyclovir and acyclovir was extensively evaluated in buffered and unbuffered plasma. It was successfully applied to a bioequivalence study in 41 healthy human subjects after oral administration of 1000 mg valacyclovir tablet formulation under fasting condition.

  16. MALDI-ToF mass spectrometry coupled with multivariate pattern recognition analysis for the rapid biomarker profiling of Escherichia coli in different growth phases.

    Science.gov (United States)

    Momo, Remi A; Povey, Jane F; Smales, C Mark; O'Malley, Christopher J; Montague, Gary A; Martin, Elaine B

    2013-10-01

    Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-ToF MS) has been exploited extensively in the field of microbiology for the characterisation of bacterial species, the detection of biomarkers for early disease diagnosis and bacterial identification. Here, the multivariate data analysis technique of partial least squares-discriminant analysis (PLS-DA) was applied to 'intact cell' MALDI-ToF MS data obtained from Escherichia coli cell samples to determine if such an approach could be used to distinguish between, and characterise, different growth phases. PLS-DA is a technique that has the potential to extract systematic variation from large and noisy data sets by identifying a lower-dimensional subspace that contains latent information. The application of PLS-DA to the MALDI-ToF data obtained from cells at different stages of growth resulted in the successful classification of the samples according to the growth phase of the bacteria cultures. A further outcome of the analysis was that it was possible to identify the mass-to-charge (m/z) ratio peaks or ion signals that contributed to the classification of the samples. The Swiss-Prot/TrEMBL database and primary literature were then used to provisionally assign a small number of these m/z ion signals to proteins, and these tentative assignments revealed that the major contributors from the exponential phase were ribosomal proteins. Additional assignments were possible for the stationary phase and the decline phase cultures where the proteins identified were consistent with previously observed biological interpretation. In summary, the results show that MALDI-ToF MS, PLS-DA and a protein database search can be used in combination to discriminate between 'intact cell' E. coli cell samples in different growth phases and thus could potentially be used as a tool in process development in the bioprocessing industry to enhance cell growth and cell engineering strategies.

  17. Rapid identification of microorganisms by mass spectrometry: improved performance by incorporation of in-house spectral data into a commercial database.

    Science.gov (United States)

    Sogawa, Kazuyuki; Watanabe, Masaharu; Sato, Kenichi; Segawa, Syunsuke; Miyabe, Akiko; Murata, Syota; Saito, Tomoko; Nomura, Fumio

    2012-06-01

    Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is increasingly used as a microbial diagnostic method for species identification of pathogens. However, MALDI-TOF identification of bacteria at the species level remains unsatisfactory, with the major problem being an incomplete database that still needs refinement and expansion. Augmentation of the original MALDI BioTyper 2.0 (Bruker) database by incorporating mass spectra obtained in-house from clinical isolates may increase the identification rate at the species level. We conducted a prospective study to assess whether the augmented database can improve the performance of MALDI-TOF MS for routine identification of species. Cluster analyses revealed distinct differences in MS spectral profiles of clinical isolates obtained in our hospital and those of ATCC strains in the Bruker database. In the first part of the study, which was performed over 3 weeks, 259 bacterial isolates were subjected to analysis by MALDI-TOF MS, and MS spectra of 229 successfully identified isolates (49 species) were incorporated into the original database to give the augmented Bruker-Chiba database. In a second separate analysis, the concordance of identification of 498 clinical isolates of the 49 species with conventional methods was 87.1% (434/498) with the commercial Bruker database and 98.0% (488/498) using the Bruker-Chiba database. These results indicate that refinement of a commercial database can be achieved relatively easy and effectively by incorporating MS spectra of clinical isolates obtained in a clinical laboratory.

  18. Development and validation of a rapid liquid chromatography isotope dilution tandem mass spectrometry (LC-IDMS/MS) method for serum creatinine.

    Science.gov (United States)

    Hétu, Pierre-Olivier; Gingras, Marie-Eve; Vinet, Bernard

    2010-09-01

    To develop an isotope dilution liquid chromatography tandem mass spectrometry (LC-IDMS/MS) method for the standardization of serum creatinine. Supernatants obtained by protein precipitation were injected into a LC-MS/MS. Chromatography was performed on a cation exchanger pre-column in normal phase isocratic mode. Creatinine and creatinine-D(3) were quantified using ion transitions of m/z 114-->44 and 117-->47, respectively. The method was calibrated with the NIST Standard Reference Material 914a and was found to be exact in analyzing the certified reference material SRM 967 from NIST (97.1+/-0.9% and 102.1+/-0.9% of target value for levels 1 and 2, respectively) and by calculating recuperation of spiked creatinine in 10 different patient samples (103.6+/-4.1%). Intra-assay imprecision was 0.9% at both 64.6 and 354 micromol/L creatinine, while inter-assay imprecisions were 1.9% and 1.8%. Absence of ion suppression was confirmed by spiking experiments. The method was shown to be free of carryover. A good correlation was obtained between the LC-MS/MS method and a Jaffe method run on an automated analyzer (r=0.999). We have developed a fast and simple method for the quantification of serum creatinine by isotope dilution tandem mass spectrometry (IDMS/MS) and we propose that this method can be used as a reference method by laboratories that wish to validate their serum creatinine automated assay. Published by Elsevier Inc.

  19. Rapid on-site detection of explosives on surfaces by ambient pressure laser desorption and direct inlet single photon ionization or chemical ionization mass spectrometry.

    Science.gov (United States)

    Ehlert, S; Hölzer, J; Rittgen, J; Pütz, M; Schulte-Ladbeck, R; Zimmermann, R

    2013-09-01

    Considering current security issues, powerful tools for detection of security-relevant substances such as traces of explosives and drugs/drug precursors related to clandestine laboratories are required. Especially in the field of detection of explosives and improvised explosive devices, several relevant compounds exhibit a very low vapor pressure. Ambient pressure laser desorption is proposed to make these substances available in the gas phase for the detection by adapted mass spectrometers or in the future with ion-mobility spectrometry as well. In contrast to the state-of-the-art thermal desorption approach, by which the sample surface is probed for explosive traces by a wipe pad being transferred to a thermal desorber unit, by the ambient pressure laser desorption approach presented here, the sample is directly shockwave ablated from the surface. The laser-dispersed molecules are sampled by a heated sniffing capillary located in the vicinity of the ablation spot into the mass analyzer. This approach has the advantage that the target molecules are dispersed more gently than in a thermal desorber unit where the analyte molecules may be decomposed by the thermal intake. In the technical realization, the sampling capillary as well as the laser desorption optics are integrated in the tip of an endoscopic probe or a handheld sampling module. Laboratory as well as field test scenarios were performed, partially in cooperation with the Federal Criminal Police Office (Bundeskriminalamt, BKA, Wiesbaden, Germany), in order to demonstrate the applicability for various explosives, drugs, and drug precursors. In this work, we concentrate on the detection of explosives. A wide range of samples and matrices have been investigated successfully.

  20. Rapid non-invasive quality control of semi-finished products for the food industry by direct injection mass spectrometry headspace analysis: the case of milk powder, whey powder and anhydrous milk fat.

    Science.gov (United States)

    Makhoul, Salim; Yener, Sine; Khomenko, Iuliia; Capozzi, Vittorio; Cappellin, Luca; Aprea, Eugenio; Scampicchio, Matteo; Gasperi, Flavia; Biasioli, Franco

    2016-09-01

    In this study, we demonstrated the suitability of direct injection mass spectrometry headspace analysis for rapid non-invasive quality control of semi-finished dairy ingredients, such as skim milk powder (SMP), whole milk powder (WMP), whey powder (WP) and anhydrous milk fat (AMF), which are widely used as ingredients in the food industry. In this work, for the first time, we applied proton transfer reaction-mass spectrometry (PTR-MS) with a time-of-flight (ToF) analyzer for the rapid and non-invasive analysis of volatile compounds in different samples of SMP, WMP, WP and AMF. We selected different dairy ingredients in various concrete situations (e.g. same producer and different expiration times, different producers and same days of storage, different producers) based on their sensory evaluation. PTR-ToF-MS allowed the separation and characterization of different samples based on the volatile organic compound (VOC) profiles. Statistically significant differences in VOC content were generally coherent with differences in sensory evaluation, particularly for SMP, WMP and WP. The good separation of SMP samples from WMP samples suggested the possible application of PTR-ToF-MS to detect possible cases of adulteration of dairy ingredients for the food industry. Our findings demonstrate the efficient and rapid differentiation of dairy ingredients on the basis of the released VOCs via PTR-ToF-MS analysis and suggest this method as a versatile tool (1) for the facilitation/optimization of the selection of dairy ingredients in the food industry and (2) and for the prompt innovation in the production of dairy ingredients. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  1. Rapid methodology via mass spectrometry to quantify addition of soybean oil in extra virgin olive oil: A comparison with traditional methods adopted by food industry to identify fraud.

    Science.gov (United States)

    da Silveira, Roberta; Vágula, Julianna Matias; de Lima Figueiredo, Ingrid; Claus, Thiago; Galuch, Marilia Bellanda; Santos Junior, Oscar Oliveira; Visentainer, Jesui Vergilio

    2017-12-01

    Fast and innovative methodology to monitors the addition of soybean oil in extra virgin olive oil was developed employing ESI-MS with ionization operating in positive mode. A certified extra virgin olive oil and refined soybean oil samples were analyzed by direct infusion, the identification of a natural lipid marker present only in soybean oil (m/z 886.68 [TAG+NH4]+) was possible. The certified extra virgin olive oil was purposely adulterated with soybean oil in different levels (1, 5, 10, 20, 50, 70, 90%) being possible to observe that the new methodology is able to detect even small fraud concentration, such as 1% (v/v). Additionally, commercial samples were analyzed and were observed the addition of soybean oil as a common fraud in this segment. This powerful analytical method proposed could be applied as routine analysis by control organization, as well as food industries, considering its pronounced advantages; simplicity, rapidity, elevated detectability and minor amounts of sample and solvent consumed. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Rapid isolation of plutonium in environmental solid samples using sequential injection anion exchange chromatography followed by detection with inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Qiao Jixin, E-mail: jixin.qiao@risoe.d [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Hou Xiaolin; Roos, Per [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Miro, Manuel [Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, Carretera de Valldemossa km. 7.5, E-07122 Palma de Mallorca, Illes Balears (Spain)

    2011-01-31

    This paper reports an automated analytical method for rapid determination of plutonium isotopes ({sup 239}Pu and {sup 240}Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-x4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 10{sup 3} to 10{sup 4}. The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials.

  3. Early gamma oscillations during rapid auditory processing in children with a language-learning impairment: changes in neural mass activity after training.

    Science.gov (United States)

    Heim, Sabine; Keil, Andreas; Choudhury, Naseem; Thomas Friedman, Jennifer; Benasich, April A

    2013-04-01

    Children with language-learning impairment (LLI) have consistently shown difficulty with tasks requiring precise, rapid auditory processing. Remediation based on neural plasticity assumes that the temporal precision of neural coding can be improved by intensive training protocols. Here, we examined the extent to which early oscillatory responses in auditory cortex change after audio-visual training, using combined source modeling and time-frequency analysis of the human electroencephalogram (EEG). Twenty-one elementary school students diagnosed with LLI underwent the intervention for an average of 32 days. Pre- and post-training assessments included standardized language/literacy tests and EEG recordings in response to fast-rate tone doublets. Twelve children with typical language development were also tested twice, with no intervention given. Behaviorally, improvements on measures of language were observed in the LLI group following completion of training. During the first EEG assessment, we found reduced amplitude and phase-locking of early (45-75 ms) oscillations in the gamma-band range (29-52 Hz), specifically in the LLI group, for the second stimulus of the tone doublet. Amplitude reduction for the second tone was no longer evident for the LLI children post-intervention, although these children still exhibited attenuated phase-locking. Our findings suggest that specific aspects of inefficient sensory cortical processing in LLI are ameliorated after training. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Rapid Analysis of Ingredients in Cream Using Ultrasonic Mist-Direct Analysis in Real-Time Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Shimada, Haruo; Maeno, Katsuyuki; Kinoshita, Kazumasa; Shida, Yasuo

    2017-07-01

    A novel method for the simultaneous detection of ingredients in pharmaceutical applications such as creams and lotions was developed. An ultrasonic atomizer has been used to produce a mist containing ingredients. The analyte molecules in the mist can be ionized by using direct analysis in real time (DART) at lower temperature than traditionally used, and we thus solved the problem of normal DART-MS measurement using a high-temperature gas. Thereby, molecular-related ions of heat-unstable components and nonvolatile components became detectable. The deprotonated molecular ion of glycyrrhizic acid (m/z 821), which is unstable at high temperatures, was detected without pyrolysis by ultrasonic mist-DART-MS using unheated helium gas, although it was not detected by normal DART-MS using heated helium gas. The cationized molecular ions of derivatives of polyethylene glycol fatty acid monoesters, which are nonvolatile compounds, were also detected as m/z peaks observed from 800 to 2300. Although the protonated molecular ion of tocopherol acetate was not detected in ionization by ultrasonic mist, it was detected by ultrasonic mist-DART-MS even in the emulsion. It was not necessary to dissolve a sample completely to detect its ions. This method enabled us to obtain the composition of pharmaceutical applications simply and rapidly.

  5. Rapid freeze-drying cycle optimization using computer programs developed based on heat and mass transfer models and facilitated by tunable diode laser absorption spectroscopy (TDLAS).

    Science.gov (United States)

    Kuu, Wei Y; Nail, Steven L

    2009-09-01

    Computer programs in FORTRAN were developed to rapidly determine the optimal shelf temperature, T(f), and chamber pressure, P(c), to achieve the shortest primary drying time. The constraint for the optimization is to ensure that the product temperature profile, T(b), is below the target temperature, T(target). Five percent mannitol was chosen as the model formulation. After obtaining the optimal sets of T(f) and P(c), each cycle was assigned with a cycle rank number in terms of the length of drying time. Further optimization was achieved by dividing the drying time into a series of ramping steps for T(f), in a cascading manner (termed the cascading T(f) cycle), to further shorten the cycle time. For the purpose of demonstrating the validity of the optimized T(f) and P(c), four cycles with different predicted lengths of drying time, along with the cascading T(f) cycle, were chosen for experimental cycle runs. Tunable diode laser absorption spectroscopy (TDLAS) was used to continuously measure the sublimation rate. As predicted, maximum product temperatures were controlled slightly below the target temperature of -25 degrees C, and the cascading T(f)-ramping cycle is the most efficient cycle design. In addition, the experimental cycle rank order closely matches with that determined by modeling.

  6. Rapid and Efficient Desulfonation Method for the Analysis of Glucosinolates by High-Resolution Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Singh, Jashbir; Jayaprakasha, Guddadarangavvanahally K; Patil, Bhimanagouda S

    2017-12-20

    The goal of our present research was to develop a simple and rapid method for the quantitation of desulfoglucosinolates (desulfoGLS) without using column chromatography. The proposed method involves extraction, concentration, incubation of glucosinolates with a sulfatase enzyme, and HPLC analysis. Identification of desulfoGLS in green kohlrabi was performed by LC-HR-ESI-QTOF-MS in positive-ionization mode. A total of 11 desulfoGLS were identified with neoglucobrassicin (3.32 ± 0.05 μmol/g DW) as the predominant indolyl, whereas progoitrin and sinigrin were the major aliphatic desulfoGLS. The levels of the aliphatic desulfoGLS glucoiberin, progoitrin, and glucoerucin at 7 h were found to be 3.6-, 1.9-, and 1.6-fold higher, respectively, than those produced through the conventional method. This technique was successfully applied in the identification of desulfoGLS from cabbage. The developed method has fewer unit operations, has maximum recovery, and is reproducible in the determination of desulfoGLS in a large number of Brassicaceae samples in a short time.

  7. Rapid screening of anabolic steroids in horse urine with ultra-high-performance liquid chromatography/tandem mass spectrometry after chemical derivatisation.

    Science.gov (United States)

    Wong, Colton H F; Leung, David K K; Tang, Francis P W; Wong, Jenny K Y; Yu, Nola H; Wan, Terence S M

    2012-04-06

    Liquid chromatography/mass spectrometry (LC/MS) has been successfully applied to the detection of anabolic steroids in biological samples. However, the sensitive detection of saturated hydroxysteroids, such as androstanediols, by electrospray ionisation (ESI) is difficult because of their poor ability to ionise. In view of this, chemical derivatisation has been used to enhance the detection sensitivity of hydroxysteroids by LC/MS. This paper describes the development of a sensitive ultra-high-performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) method for the screening of anabolic steroids in horse urine by incorporating a chemical derivatisation step, using picolinic acid as the derivatisation reagent. The method involved solid-phase extraction (SPE) of both free and conjugated anabolic steroids in horse urine using a polymer-based SPE cartridge (Abs Elut Nexus). The conjugated steroids in the eluate were hydrolysed by methanolysis and the resulting extract was further cleaned up by liquid-liquid extraction. The resulting free steroids in the extract were derivatised with picolinic acid to form the corresponding picolinoyl esters and analysed by UHPLC/MS/MS in the positive ESI mode with selected-reaction-monitoring. Separation of the targeted steroids was performed on a C18 UHPLC column. The instrument turnaround time was 10.5 min inclusive of post-run equilibration. A total of thirty-three anabolic steroids (including 17β-estradiol, 5(10)-estrene-3β,17α-diol, 5α-estrane-3β,17α-diol, 17α-ethyl-5α-estran-3α,17β-diol, 17α-methyl-5α-androstan-3,17β-diols, androstanediols, nandrolone and testosterone) spiked in negative horse urine at the QC levels (ranging from 0.75 to 30 ng/mL) could be consistently detected. The intra-day and inter-day precisions (% RSD) for the peak area ratios were around 7-51% and around 1-72%, respectively. The intra-day and inter-day precisions (% RSD) for the relative retention times were both less than 1% for

  8. Rapid and sensitive on-line monitoring 6 different kinds of volatile organic compounds in aqueous samples by spray inlet proton transfer reaction mass spectrometry (SI-PTR-MS).

    Science.gov (United States)

    Zou, Xue; Kang, Meng; Wang, Hongmei; Huang, Chaoqun; Shen, Chengyin; Chu, Yannan

    2017-06-01

    Rapid and sensitive monitoring of volatile organic compounds (VOCs) in aqueous samples is very important to human health and environmental protection. In this study, an on-line spray inlet proton transfer reaction mass spectrometry (SI-PTR-MS) method was developed for the rapid and sensitive monitoring of 6 different kinds of VOCs, namely acetonitrile, acetaldehyde, ethanol, acetone, aether, and methylbenzene, in aqueous samples. The response time, limit of detection (LOD), and repeatability of the SI-PTR-MS system were evaluated. The response of the SI-PTR-MS was quite rapid with response times of 31-88 s. The LODs for all these VOCs were below 10 μg/L. The LOD of methylbenzene was 0.9 μg/L, much lower than the maximum contaminant level (MCL) in drinking water. The repeatability of this method was evaluated with 5 replicate determinations. The relative standard deviations (RSDs) were in the range of 0.8-3.1%, indicating good repeatability. To evaluate the matrix effects, the SI-PTR-MS system was employed for on-line monitoring of these 6 VOCs in different aqueous matrices, including lake water, tap water, and waste water. The relative recoveries were in the range of 94.6-106.0% for the lake water, 96.3-105.6% for the tap water, and 95.6-102.9% for the waste water. The results indicate that the SI-PTR-MS method has important application values in the rapid and sensitive monitoring of VOCs in these aqueous samples. In addition, the effect of salt concentration on the extracting efficiency was evaluated. The results showed that the LOD of the SI-PTR-MS could be further decreased by changing the salt concentration. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Quasi-simultaneous acquisition of hard electron ionization and soft single-photon ionization mass spectra during GC/MS analysis by rapid switching between both ionization methods: analytical concept, setup, and application on diesel fuel.

    Science.gov (United States)

    Eschner, Markus S; Gröger, Thomas M; Horvath, Thomas; Gonin, Marc; Zimmermann, Ralf

    2011-05-15

    This work describes the realization of rapid switching between hard electron ionization (EI) and soft single-photon ionization (SPI) integrated in a compact orthogonal acceleration time-of-flight mass spectrometer. Vacuum-ultraviolet (VUV) photons of 9.8 eV (126 nm) emitted from the innovative electron-beam-pumped rare-gas excimer light source (EBEL) filled with argon are focused into the ion chamber by an ellipsoidal mirror optic for accomplishing of SPI. This novel orthogonal acceleration time-of-flight mass spectrometer with switching capability was hyphenated to one-dimensional gas chromatography (GC) and comprehensive two-dimensional (2D) gas chromatography (GC × GC) for the first time. Within this demonstration study, a maximum switching frequency of 80 Hz was applied for investigation of a mineral-oil-type diesel sample. This approach allows the quasi-simultaneous acquisition of complementary information about the fragmentation pattern (EI) as well as the molecular mass (SPI) of compounds within a single analysis. Furthermore, by application of a polar GC column for separation, the SPI data can be displayed in a 2D contour plot, leading to a comprehensive 2D characterization (GC × MS), whereas the typical group-type assignment for diesel is also met.

  10. Rapid quantitative analysis of ormeloxifene and its active metabolite, 7-desmethyl ormeloxifene, in rat plasma using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Sharma, Abhisheak; Jaiswal, Swati; Shukla, Mahendra; Malik, Mohd Yaseen; Lal, Jawahar

    2015-08-01

    Ormeloxifene (ORM) is a non-steroidal, selective estrogen receptor modulator used as a once a week oral contraceptive and is intended for long-term clinical use by females. Therefore, a simple, sensitive and rapid LC-MS/MS method was developed and validated for simultaneous quantification of ORM and its active metabolite (7-desmethyl ormeloxifene, 7-DMO) in rat plasma. Also, the method was partially validated in human plasma. Chromatographic separation was achieved on Discovery HS C-18 column (5μm, 50×4.6mm) with mobile phase [acetonitrile: aqueous ammonium acetate (0.01M) buffer (85: 15, %v/v)] at a flow rate of 0.8mL/min. The calibration curve was linear (r≥0.99) for a concentration range of 0.78-100ng/mL for both the analytes. The precision (%RSD; ORM, 1.3 to 13.4; 7-DMO, 3.1 to 15.0) and accuracy (%bias; ORM, -13.8 to 12.5; 7-DMO, -10.6 to 6.8) in both rat and human plasma were within the acceptable limits. The recovery for ORM and 7-DMO was always >79.1% and >72.9%, respectively. Both the analytes were found stable in rat plasma even after 30 days of storage at -80°C and on being subjected to three freeze-thaw cycles. The method has not only short run time (3.5min) but requires a low plasma sample volume (20μL) and is the first reported LC-MS/MS method for simultaneous quantification of the marketed drug known as centchroman (INN: ormeloxifene) and the metabolite 7-DMO in plasma. The method was applied to evaluate drug-drug interaction of ORM with the commonly prescribed antidepressant drug sertraline using serial sampling in rats. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Rapid multi-residue method for the quantitative determination and confirmation of glucocorticosteroids in bovine milk using liquid chromatography-electrospray ionization-tandem mass spectrometry.

    Science.gov (United States)

    McDonald, Mark; Granelli, Kristina; Sjöberg, Pernilla

    2007-04-04

    Dexamethasone, betamethasone and prednisolone are synthetic glucocorticosteroids authorized for therapeutic use in bovine animals within the European Union. Dexamethasone and betamethasone are used mainly for the treatment of metabolic and inflammatory diseases. Prednisolone is used to treat bovine mastitis. Maximum residue limits (MRLs) of 0.3 microg kg(-1) for both dexamethasone and betamethasone and 6.0 microg kg(-1) for prednisolone in bovine milk have been established. 6alpha-Methylprednisolone and flumethasone are not authorized for use in bovine animals and are completely banned in bovine milk. The proposed method is based on deprotenisation of milk using 20% (w/v) trichloroacetic acid. Samples are filtered using glass microfiber filters and subject to clean-up using OASIS HLB solid phase extraction. Separation was achieved on a Hypercarb 100 mm x 2.1 mm x 5 microm column. Mobile phase was: 90/10 acetonitrile/0.1% formic acid in water; flow rate was 600 microL min(-1). The method allowed the rapid identification and confirmation of the five glucocorticosteroids according to the criteria laid down in Commission Decision 2002/657/EC. Matrix calibration curves for all compounds were linear in the interval 0.0 MRL to 2.0 MRL with a correlation coefficient (r(2)) higher than 0.96. Relative recoveries ranged from 97% for betamethasone to 111% for prednisolone. Precision at the MRL ranged from 3.8% for prednisolone to 13.8% for betamethasone. Decision limits, CCalpha, and detection capability, CCbeta have been calculated for all compounds.

  12. [Application of a rapid and simple multi-residue method for determination of pesticide residues in drinking water and beverages using liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Fukui, Naoki; Takatori, Satoshi; Kitagawa, Yoko; Okihashi, Masahiro; Osakada, Masakazu; Nakatsuji, Naoto; Nakayama, Yukiko; Kakimoto, You; Obana, Hirotaka

    2012-01-01

    A rapid and simple multi-residue method for determination of pesticides has been applied to drinking water and beverages. To a disposable polypropylene tube containing 10.0 g sample, 20 mL acetonitrile was added and the mixture was shaken vigorously for 1 min to extract pesticides. Then, 1 g sodium chloride and 4 g magnesium sulfate anhydrous were added, followed by vigorous shaking for 1 min and centrifugation to obtain the organic phase. The organic phase was processed with a graphite carbon black/PSA solid phase column. After concentration and reconstitution with 25% methanol containing aqueous solution, the test solution was analyzed with LC-MS/MS. Recovery tests of 91 pesticides fortified (0.02 μg/g) in 35 kinds of drinking water and beverages were conducted. The decline of recoveries in alcoholic beverages is considered to be due to the increase of organic phase volume owing to ethanol included in the alcoholic beverages. A simulation study was carried out with simulated alcoholic beverages, which consisted of 50% grape juice, with various amounts of ethanol and water, to examine pesticides recoveries and volume of the organic phase. The results suggested this method would be applicable both to alcoholic beverages containing less than 10% ethanol and to alcoholic beverages containing over 10% ethanol after dilution with water to below 10% ethanol prior to the addition of acetonitrile. A sample could be processed and analyzed by LC-MS/MS within 2 h. Thus, this method should be useful for monitoring and screening pesticide residues in drinking water and various beverages.

  13. Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) for Rapid Determination of Microbial Cell Lipid Content: Correlation with Gas Chromatography-Mass Spectrometry (GC-MS).

    Science.gov (United States)

    Millan-Oropeza, Aaron; Rebois, Rolando; David, Michelle; Moussa, Fathi; Dazzi, Alexandre; Bleton, Jean; Virolle, Marie-Joelle; Deniset-Besseau, Ariane

    2017-10-01

    There is a growing interest worldwide for the production of renewable oil without mobilizing agriculture lands; fast and reliable methods are needed to identify highly oleaginous microorganisms of potential industrial interest. The aim of this study was to demonstrate the relevance of attenuated total reflection (ATR) spectroscopy to achieve this goal. To do so, the total lipid content of lyophilized samples of five Streptomyces strains with varying lipid content was assessed with two classical quantitative but time-consuming methods, gas chromatography-mass spectrometry (GC-MS) and ATR Fourier transform infrared (ATR FT-IR) spectroscopy in transmission mode with KBr pellets and the fast ATR method, often questioned for its lack of reliability. A linear correlation between these three methods was demonstrated allowing the establishment of equations to convert ATR values expressed as CO/amide I ratio, into micrograms of lipid per milligram of biomass. The ATR method proved to be as reliable and quantitative as the classical GC-MS and FT-IR in transmission mode methods but faster and more reproducible than the latter since it involves far less manipulation for sample preparation than the two others. Attenuated total reflection could be regarded as an efficient fast screening method to identify natural or genetically modified oleaginous microorganisms by the scientific community working in the field of bio-lipids.

  14. Rapid and simultaneous determination of polychlorinated biphenyls and their main metabolites (hydroxylated and methyl sulfonyl) by gas chromatography coupled to mass spectrometry: comparison of different ionisation modes.

    Science.gov (United States)

    Castro-Puyana, M; Herrero, L; González, M J; Gómara, B

    2013-07-17

    Instrumental methods based on gas chromatography coupled to mass spectrometry (GC-MS) have been developed and compared using two different MS ionisation modes, electron impact (EI) and electron capture negative ionisation (ECNI), for the fast, quantitative and simultaneous determination of polychlorinated biphenyls (PCBs) and their main metabolites (hydroxylated PCBs, OH-PCBs, and methyl sulfone PCBs, MeSO2-PCBs). Parameters affecting chromatographic separation and MS detection were evaluated in order to achieve the highest selectivity and sensitivity for both operation modes. The analytical characteristics of the developed methods were studied and compared in terms of linear range, limits of detection (LODs), limits of quantification (LOQs), and instrumental precision (repeatability and intermediate precision). Both ionisation methods showed similar precision, being relative standard deviations (RSD, %) lower than 9% and 14% for repeatability and intermediate precision, respectively. However, better LODs (from 0.01 to 0.14 pg injected for the three families of congeners studied) were achieved using ECNI-MS as ionisation mode. The suitability of the developed method was demonstrated through their application to fish liver oil samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Rapid determination of rivaroxaban in human urine and serum using colloidal palladium surface-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Cheng, Yu-Han; Chen, Wen-Chi; Chang, Sarah Y

    2015-11-15

    Rivaroxaban is a new anticoagulant drug that has recently been introduced for clinical applications. To ensure optimum efficacy while minimizing the risk of toxicity and other adverse effects, a simple and sensitive analytical procedure for monitoring the concentration of rivaroxaban in biological fluids is required. Rivaroxaban was extracted from aqueous solutions by dispersive liquid-liquid microextraction (DLLME). Detection of rivaroxaban was achieved through surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) using colloidal palladium as the SALDI matrix. The calibration curve for rivaroxaban in aqueous solutions was linear over the concentration range from 5 to 500 nM. The limit of detection (LOD) for rivaroxaban at a signal-to-noise ratio of 3 was 2 nM. With a sample-to-extract volume ratio of 200, the enrichment factors were calculated to be 141. This method was successfully applied for the determination of rivaroxaban in human urine and serum samples. The LODs for rivaroxaban in urine and serum were calculated to be 6 nM and 60 nM, respectively. The analysis speed, together with the ease of operation and high sensitivity, allows SALDI-MS method to be particularly suitable for the high-throughput screening of rivaroxaban levels in human urine and serum samples. Copyright © 2015 John Wiley & Sons, Ltd.

  16. Pipette tip solid-phase extraction and ultra-performance liquid chromatography/mass spectrometry based rapid analysis of picrosides from Picrorhiza scrophulariiflora.

    Science.gov (United States)

    Shen, Qing; Dong, Wei; Wang, Yixuan; Gong, Like; Dai, Zhiyuan; Cheung, Hon-Yeung

    2013-06-01

    Pipette tip solid-phase extraction (PT-SPE) is a technique popular in sample preparation of biological fluids and protein hydrolysates. In this study, we developed a microtechnic using a pipette tip packed with C18 as sorbent for extraction and purification of bioactive compounds, picroside-I, II and III, in crude herbal extracts from Picrorhiza scrophulariiflora (P. scrophulariiflora). Compared to conventional SPE, PT-SPE is fast, easy to operate, and the tools are very accessible (pipette tip and tube, without expensive SPE set-up). Moreover, it is also cost-effective because significant amount of sorbent and solvents can be saved. The eluate was analyzed by ultra-performance liquid chromatography and tandem mass spectrometry (UPLC-MS/MS). Afterwards, the method was fully validated and the results demonstrated that the PT-SPE-UPLC-MS/MS method is an excellent technique for analysis of the herbal medicine. Finally, this PT-SPE-UPLC-MS/MS strategy was successfully applied to analyze the crude extracts from P. scrophulariiflora samples within 10min (2min for PT-SPE and 8min for UPLC), 3.5mL solvents (including water, 0.3mL for PT-SPE and 3.2mL for UPLC), and 2mg C18 sorbent for each sample. We believe this method to be very practical and, in particular, to be suitable for widespread herbal medicine analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Acute incident rapid response at a mass-gathering event through comprehensive planning systems: a case report from the 2013 Shamrock Shuffle.

    Science.gov (United States)

    Başdere, Mehmet; Ross, Colleen; Chan, Jennifer L; Mehrotra, Sanjay; Smilowitz, Karen; Chiampas, George

    2014-06-01

    Planning and execution of mass-gathering events involves various challenges. In this case report, the Chicago Model (CM), which was designed to organize and operate such events and to maintain the health and wellbeing of both runners and the public in a more effective way, is described. The Chicago Model also was designed to prepare for unexpected incidents, including disasters, during the marathon event. The model has been used successfully in the planning and execution stages of the Bank of America Shamrock Shuffle and the Bank of America Chicago Marathon since 2008. The key components of the CM are organizational structure, information systems, and communication. This case report describes how the organizers at the 2013 Shamrock Shuffle used the key components of the CM approach in order to respond to an acute incident caused by a man who was threatening to jump off the State Street Bridge. The course route was changed to accommodate this unexpected event, while maintaining access to key health care facilities. The lessons learned from the incident are presented and further improvements to the existing model are proposed.

  18. Rapid and specific detection of urea nitrate and ammonium nitrate by electrospray ionization time-of-flight mass spectrometry using infusion with crown ethers.

    Science.gov (United States)

    de Perre, Chloé; Prado, Adelheid; McCord, Bruce R

    2012-01-30

    Urea nitrate (UN) and ammonium nitrate (AN) are fertilizer-based explosives that are commonly used in improvised munitions and can have highly destructive effects. Because they are in the form of salts, their relatively low volatility makes them difficult to detect at trace levels. In addition, these salts readily undergo metathetic reactions in water to form urea, ammonium and nitrate, which are ubiquitous in the environment. Thus, selective methods are needed for their detection. In this study, a procedure was developed to detect UN and AN in non-aqueous environments by positive ion electrospray ionization mass spectrometry through the addition of 18-crown-6. The method is sensitive, with detection limits under 2 μM, and selective. The procedure is capable of differentiating urea from uronium ions (protonated urea) and a mixture of urea and AN did not interfere with the UN signal. The procedure is quite versatile and the addition of crown ethers to the sample matrix does not interfere with the detection of high explosives in the negative ionization mode. Experimental results are presented on the utilization of the method in the detection of UN and AN on various surfaces. Semi-quantitative studies showed that AN and UN can be detected at trace levels following finger transfer and a series of studies were performed to demonstrate the effect of various interferences. The results show the method to be a quick and robust procedure for trace detection. Copyright © 2011 John Wiley & Sons, Ltd.

  19. A simple and rapid method to identify and quantitatively analyze triterpenoid saponins in Ardisia crenata using ultrafast liquid chromatography coupled with electrospray ionization quadrupole mass spectrometry.

    Science.gov (United States)

    Ma, Ling; Li, Wei; Wang, Hanqing; Kuang, Xinzhu; Li, Qin; Wang, Yinghua; Xie, Peng; Koike, Kazuo

    2015-01-01

    Ardisia plant species have been used in traditional medicines, and their bioactive constituents of 13,28-epoxy triterpenoid saponins have excellent biological activities for new drug development. In this study, a fast and simple method based on ultrafast liquid chromatography coupled to electrospray ionization mass spectrometry (UFLC-MS) was developed to simultaneously identify and quantitatively analyze triterpenoid saponins in Ardisia crenata extracts. In total, 22 triterpenoid saponins, including two new compounds, were identified from A. crenata. The method exhibited good linearity, precision and recovery for the quantitative analysis of eight marker saponins. A relative quantitative method was also developed using one major saponin (ardisiacrispin B) as the standard to break through the choke-point of the lack of standards in phytochemical analysis. The method was successfully applied to quantitatively analyze saponins in commercially available plant samples. This study describes the first systematic analysis of 13,28-epoxy-oleanane-type triterpenoid saponins in the genus Ardisia using LC-ESI-MS. The results can provide the chemical support for further biological studies, phytochemotaxonomical studies and quality control of triterpenoid saponins in medicinal plants of the genus Ardisia. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Rapid determination of four short-chain alkyl mercapturic acids in human urine by column-switching liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Eckert, Elisabeth; Göen, Thomas

    2014-08-15

    We developed and validated an analytical method for the simultaneous determination of methyl mercapturic acid (MeMA), ethyl mercapturic acid (EtMA), n-propyl mercapturic acid (PrMA) and iso-propyl mercapturic acid (iPrMA) in human urine. These alkyl mercapturic acids are known or presumed biomarkers of exposure to several alkylating agents including methyl bromide, dimethyl sulfate, ethyl bromide, 1-bromopropane and 2-bromopropane. The method involves a column switching arrangement for online solid phase extraction of the analytes with subsequent analytical separation and detection using liquid chromatography and tandem mass spectrometry. Within day and day-to-day imprecision was determined to range from 4.5 to 12.2%. The analytical method is distinguished by its wide linear working range of up to 2,500 μg/L with detection limits ranging from 2.0 μg/L (for PrMA) to 5.1 μg/L (for MeMA) that render possible the application in various biomonitoring studies regarding exposure to alkylating agents. The results of a pilot study on urine samples of 30 individuals occupationally non-exposed to alkylating agents using the new procedure confirmed the background excretion of MeMA (<5.1-35.6 μg/L) and PrMA (<2.0-95.7 μg/L). Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tagiri-Endo, Misako; Suzuki, Shigeru; Nakamura, Tomoyuki; Hatakeyama, Takashi; Kawamukai, Kazuo

    2009-02-01

    A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 microl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01-0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.

  2. Rapidly differentiating grape seeds from different sources based on characteristic fingerprints using direct analysis in real time coupled with time-of-flight mass spectrometry combined with chemometrics.

    Science.gov (United States)

    Song, Yuqiao; Liao, Jie; Dong, Junxing; Chen, Li

    2015-09-01

    The seeds of grapevine (Vitis vinifera) are a byproduct of wine production. To examine the potential value of grape seeds, grape seeds from seven sources were subjected to fingerprinting using direct analysis in real time coupled with time-of-flight mass spectrometry combined with chemometrics. Firstly, we listed all reported components (56 components) from grape seeds and calculated the precise m/z values of the deprotonated ions [M-H](-) . Secondly, the experimental conditions were systematically optimized based on the peak areas of total ion chromatograms of the samples. Thirdly, the seven grape seed samples were examined using the optimized method. Information about 20 grape seed components was utilized to represent characteristic fingerprints. Finally, hierarchical clustering analysis and principal component analysis were performed to analyze the data. Grape seeds from seven different sources were classified into two clusters; hierarchical clustering analysis and principal component analysis yielded similar results. The results of this study lay the foundation for appropriate utilization and exploitation of grape seed samples. Due to the absence of complicated sample preparation methods and chromatographic separation, the method developed in this study represents one of the simplest and least time-consuming methods for grape seed fingerprinting. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Rapid and Green Separation of Mono- and Diesters of Monochloropropanediols by Ultrahigh Performance Supercritical Fluid Chromatography-Mass Spectrometry Using Neat Carbon Dioxide as a Mobile Phase.

    Science.gov (United States)

    Jumaah, Firas; Jędrkiewicz, Renata; Gromadzka, Justyna; Namieśnik, Jacek; Essén, Sofia; Turner, Charlotta; Sandahl, Margareta

    2017-09-20

    This study demonstrates the effect of column selectivity and density of supercritical carbon dioxide (SC-CO 2 ) on the separation of monochloropropanediol (MCPD) esters, known as food toxicants, using SC-CO 2 without addition of cosolvent in ultrahigh performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS). This study shows that over 20 2-monochloropropanediol (2-MCPD) and 3-monochloropropanediol (3-MCPD) mono- and diesters are separated on a 2-picolylamine column in less than 12 min. The presence and position of a hydroxyl group in the structure, the number of unsaturated bonds, and the acyl chain length play a significant role in the separation of MCPD esters. The flow rate, backpressure, and column oven temperature, which affect the density of the mobile phase, were shown to have a substantial impact on retention, efficiency, and selectivity. The developed method was successfully applied for the determination of MCPD esters in refined oils and showed a close to excellent green analysis score using the Analytical Eco-Scale.

  4. A Rapid Magnetic Solid Phase Extraction Method Followed by Liquid Chromatography-Tandem Mass Spectrometry Analysis for the Determination of Mycotoxins in Cereals

    Directory of Open Access Journals (Sweden)

    Giorgia La Barbera

    2017-04-01

    Full Text Available Mycotoxins can contaminate various food commodities, including cereals. Moreover, mycotoxins of different classes can co-contaminate food, increasing human health risk. Several analytical methods have been published in the literature dealing with mycotoxins determination in cereals. Nevertheless, in the present work, the aim was to propose an easy and effective system for the extraction of six of the main mycotoxins from corn meal and durum wheat flour, i.e., the main four aflatoxins, ochratoxin A, and the mycoestrogen zearalenone. The developed method exploited magnetic solid phase extraction (SPE, a technique that is attracting an increasing interest as an alternative to classical SPE. Therefore, the use of magnetic graphitized carbon black as a suitable extracting material was tested. The same magnetic material proved to be effective in the extraction of mycoestrogens from milk, but has never been applied to complex matrices as cereals. Ultra high–performance liquid chromatography tandem mass spectrometry was used for detection. Recoveries were >60% in both cereals, even if the matrix effects were not negligible. The limits of quantification of the method results were comparable to those obtained by other two magnetic SPE-based methods applied to cereals, which were limited to one or two mycotoxins, whereas in this work the investigated mycotoxins belonged to three different chemical classes.

  5. Rapid identification of pathogens directly from blood culture bottles by Bruker matrix-assisted laser desorption laser ionization-time of flight mass spectrometry versus routine methods.

    Science.gov (United States)

    Jamal, Wafaa; Saleem, Rola; Rotimi, Vincent O

    2013-08-01

    The use of matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) for identification of microorganisms directly from blood culture is an exciting dimension to the microbiologists. We evaluated the performance of Bruker SepsiTyper kit™ (STK) for direct identification of bacteria from positive blood culture. This was done in parallel with conventional methods. Nonrepetitive positive blood cultures from 160 consecutive patients were prospectively evaluated by both methods. Of 160 positive blood cultures, the STK identified 114 (75.6%) isolates and routine conventional method 150 (93%). Thirty-six isolates were misidentified or not identified by the kit. Of these, 5 had score of >2.000 and 31 had an unreliable low score of time using the STK was 35 min, including extraction steps and 30:12 to 36:12 h with routine method. The STK holds promise for timely management of bacteremic patients. Copyright © 2013 Elsevier Inc. All rights reserved.

  6. Hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry for highly rapid and sensitive analysis of underivatized amino acids in functional foods.

    Science.gov (United States)

    Zhou, Guisheng; Pang, Hanqing; Tang, Yuping; Yao, Xin; Mo, Xuan; Zhu, Shaoqing; Guo, Sheng; Qian, Dawei; Qian, Yefei; Su, Shulan; Zhang, Li; Jin, Chun; Qin, Yong; Duan, Jin-ao

    2013-05-01

    This work presented a new analytical methodology based on hydrophilic interaction ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry in multiple-reaction monitoring mode for analysis of 24 underivatized free amino acids (FAAs) in functional foods. The proposed method was first reported and validated by assessing the matrix effects, linearity, limit of detections and limit of quantifications, precision, repeatability, stability and recovery of all target compounds, and it was used to determine the nutritional substances of FAAs in ginkgo seeds and further elucidate the nutritional value of this functional food. The result showed that ginkgo seed turned out to be a good source of FAAs with high levels of several essential FAAs and to have a good nutritional value. Furthermore, the principal component analysis was performed to classify the ginkgo seed samples on the basis of 24 FAAs. As a result, the samples could be mainly clustered into three groups, which were similar to areas classification. Overall, the presented method would be useful for the investigation of amino acids in edible plants and agricultural products.

  7. Rapid determination of acetone in human plasma by gas chromatography-mass spectrometry and solid-phase microextraction with on-fiber derivatization.

    Science.gov (United States)

    Deng, Chunhui; Zhang, Wei; Zhang, Jie; Zhang, Xiangmin

    2004-06-15

    Acetone is an important volatile disease marker. Due to its nature of activity and volatility, it is a difficult task to measure the concentration of acetone in biological samples with accuracy. In this paper, we developed a novel method for determination of trace amount acetone in human plasma by solid-phase microextraction technique with on-fiber derivatization. In this method, the poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) fiber was used and O-2,3,4,5,6-(pentafluorobenzyl) hydroxylamine hydrochloride (PFBHA) was first loaded on the fiber. Acetone in plasma sample was agitated into headspace and extracted by solid-phase microextraction (SPME) fiber and subsequently derivatized with PFBHA on the fiber. Acetone oxime was analyzed by gas chromatography-mass spectrometry (GC-MS). Quantitative analysis of acetone in plasma was carried out by using external standard method. The SPME conditions (extraction temperature and time) and the method validation were studied. The present method was tested by determination of acetone in diabetes plasma and normal plasma. Acetone concentration in diabetes plasma was found to be higher than 1.8mM, while in normal plasma was lower than 0.017 mM. The results show that the present method is a potential tool for diagnosis of diabetes.

  8. Rapid and sensitive gas chromatography ion-trap mass spectrometry method for the determination of tobacco specific N-nitrosamines in secondhand smoke

    Energy Technology Data Exchange (ETDEWEB)

    SLEIMAN, Mohamad; MADDALENA, Randy L.; GUNDEL, Lara A.; DESTAILLATS, Hugo

    2009-07-01

    Tobacco-specific nitrosamines (TSNAs) are some of the most potent carcinogens in tobacco and cigarette smoke. Accurate quantification of these chemicals is needed to help assess public health risks. We developed and validated a specific and sensitive method to measure four TSNAs in both the gas- and particle-phase of secondhand smoke (SHS) using gas chromatography and ion-trap tandem mass spectrometry,. A smoking machine in an 18-m3 room-sized chamber generated relevant concentrations of SHS that were actively sampled on Teflon coated fiber glass (TCFG) filters, and passively sampled on cellulose substrates. A simple solid-liquid extraction protocol using methanol as solvent was successfully applied to both filters with high recoveries ranging from 85 to 115percent. Tandem MS parameters were optimized to obtain the best sensitivity in terms of signal to-noise ratio (S/N) for the target compounds. For each TSNA, the major fragmentation pathways as well as ion structures were elucidated and compared with previously published data. The method showed excellent performances with a linear dynamic range between 2 and 1000 ng mL-1, low detection limits (S/N> 3) of 30-300 pg.ml-1 and precision with experimental errors below 10percent for all compounds. Moreover, no interfering peaks were observed indicating a high selectivity of MS/MS without the need for a sample clean up step. The sampling and analysis method provides a sensitive and accurate tool to detect and quantify traces of TSNA in SHS polluted indoor environments.

  9. Development of an extraction method based on new porous organogel materials coupled with liquid chromatography-mass spectrometry for the rapid quantification of bisphenol A in urine.

    Science.gov (United States)

    ter Halle, Alexandra; Claparols, Catherine; Garrigues, Jean Christophe; Franceschi-Messant, Sophie; Perez, Emile

    2015-10-02

    A new method based on the use of porous organogel materials in combination with liquid chromatography-tandem mass spectrometry (LC-MS-MS) was assessed for the quantification of trace contaminants in complex matrices. As a demonstration of the use of these new materials, the contaminant chosen as a model was bisphenol A (BPA) and its extraction was investigated in urine. Organogel materials consist of an organic solvent immobilized by an organogelator. The composition of the organogel materials was optimized in terms of extraction efficiency and compatibility with LC-MS-MS. Porosity was introduced into the organogel by means of the particulate leaching method using sugar crystals. This new absorbing material is simple to use; the extraction method is reduced to a few steps. The originality of the method lies in the complete dissolution of the material for analysis by LC-MS-MS. The matrix effect of the organogel components was studied and was found to be minimal in atmospheric-pressure chemical ionization (APCI) compared to electrospray ionization (ESI) in negative mode. The influence of matrix components on the extraction was investigated by working with different media (acidified water, synthetic urine, horse urine and human urine). The partition coefficient was not affected within the margin of error (±0.1). After optimization, bisphenol A recoveries from urine samples reached 80%. The actual concentration factor was 10. The relative standard deviation (RSD, n=6) for the extraction and determination of BPA in horse urine spiked at 10ngmL(-1) was 9%. Tests with spiked human urine showed that the extraction performances were the same as with the solutions tested previously. The use of porous organogel allowed a fast, simple, sensitive, robust, green method to be developed for the determination of trace contaminants in complex matrices. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Rapid screening and confirmation of drugs and toxic compounds in biological specimens using liquid chromatography/ion trap tandem mass spectrometry and automated library search.

    Science.gov (United States)

    Liu, Hsiu-Chuan; Liu, Ray H; Lin, Dong-Liang; Ho, Hsiu-O

    2010-01-01

    Recent advances in liquid chromatography/tandem mass spectrometry (LC/MS/MS) technology have provided an opportunity for the development of more specific approaches to achieve the 'screen' and 'confirmation' goals in a single analytical step. For this purpose, this study adapts the electrospray ionization ion trap LC/MS/MS instrumentation (LC/ESI-MS/MS) for the screening and confirmation of over 800 drugs and toxic compounds in biological specimens. Liquid-liquid and solid-phase extraction protocols were coupled to LC/ESI-MS/MS using a 1.8-microm particle size analytical column operated at 50 degrees C. Gradient elution of the analytes was conducted using a solvent system composed of methanol and water containing 0.1% formic acid. Positive-ion ESI-MS/MS spectra and retention times for each of the 800 drugs and toxic compounds were first established using 1-10 microg/mL standard solutions. This spectra and retention time information was then transferred to the library and searched by the identification algorithm for the confirmation of compounds found in test specimens - based on retention time matches and scores of fit, reverse fit, and purity resulting from the searching process. The established method was found highly effective when applied to the analyses of postmortem specimens (blood, urine, and hair) and external proficiency test samples provided by the College of American Pathology (CAP). The development of this approach has significantly improved the efficiency of our routine laboratory operation that was based on a two-step (immunoassay and GC/MS) approach in the past. Copyright 2009 John Wiley & Sons, Ltd.

  11. Development and validation of an ultra-performance liquid chromatography quadrupole time of flight mass spectrometry method for rapid quantification of free amino acids in human urine.

    Science.gov (United States)

    Joyce, Richard; Kuziene, Viktorija; Zou, Xin; Wang, Xueting; Pullen, Frank; Loo, Ruey Leng

    2016-01-01

    An ultra-performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-qTOF-MS) method using hydrophilic interaction liquid chromatography was developed and validated for simultaneous quantification of 18 free amino acids in urine with a total acquisition time including the column re-equilibration of less than 18 min per sample. This method involves simple sample preparation steps which consisted of 15 times dilution with acetonitrile to give a final composition of 25 % aqueous and 75 % acetonitrile without the need of any derivatization. The dynamic range for our calibration curve is approximately two orders of magnitude (120-fold from the lowest calibration curve point) with good linearity (r (2) ≥ 0.995 for all amino acids). Good separation of all amino acids as well as good intra- and inter-day accuracy (amino acids in the prepared urine samples was found to be stable for 72 h at 4 °C, after one freeze thaw cycle and for up to 4 weeks at -80 °C. We have applied this method to quantify the content of 18 free amino acids in 646 urine samples from a dietary intervention study. We were able to quantify all 18 free amino acids in these urine samples, if they were present at a level above the LOD. We found our method to be reproducible (accuracy and precision were typically <10 % for QCL, QCM and QCH) and the relatively high sample throughput nature of this method potentially makes it a suitable alternative for the analysis of urine samples in clinical setting.

  12. A rapid profiling of gallotannins and flavonoids of the aqueous extract of Rhus coriaria L. by flow injection analysis with high-resolution mass spectrometry assisted with database searching.

    Science.gov (United States)

    Regazzoni, Luca; Arlandini, Emanuele; Garzon, Davide; Santagati, Natale Alfredo; Beretta, Giangiacomo; Maffei Facino, Roberto

    2013-01-01

    Hydrolysable tannins appear to have some extremely important biological roles including antioxidant, antibacterial, anti-inflammatory, anti-hypoglycemic, anti-angiogenic, and anticancer activities. The aim of this work was to set up a flow injection high-resolution mass spectrometric approach combined with database searching to obtain rapidly a profiling of gallotannins and other phenolics in a crude extract from plant tissue. The flow injection analysis (FIA) takes place in an electrospray ionization source of an hybrid orbitrap high resolution mass spectrometry system (ESI-HR-MS/MS(2), resolution 100,000, negative ion mode) and polyphenols are tentatively identified by matching the monoisotopic masses of the spectra with those of polyphenols databases. This leads to the most probable molecular formulas and to the possible structures among those reported in the database. The structures confirmation occurs by the compliance of MS(2) fragments with those of a prediction fragment commercial database. With this method we identified in the aqueous extract of sumac leaves, with a maximum error of 1.7 ppm, a group of ten gallotannins from mono- to deca-galloyl glycosides of the class of hydrolysable tannins and a set of coextracted flavonoid derivatives including myricetin, quercetin-3-O-rhamnoside, myricetin-3-O-glucoside, myricetin-3-O-glucuronide, and myricetin-3-O-rhamnoglucoside. The separation of isomers of gallotannins and flavonoids present in the same extract occurred by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry (HPLC/ESI-HR-MS(2)); this approach allowed the structure resolution of the isobaric flavonoids quercetin-3-O-glucoside and myricetin-3-O-rhamnoside. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Rapid method for the determination of tranquilizers and a beta-blocker in porcine and bovine kidney by liquid chromatography with tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mitrowska, Kamila [National Veterinary Research Institute, Department of Pharmacology and Toxicology, al. Partyzantow 57, 24-100 Pulawy (Poland)], E-mail: kamitro@piwet.pulawy.pl; Posyniak, Andrzej; Zmudzki, Jan [National Veterinary Research Institute, Department of Pharmacology and Toxicology, al. Partyzantow 57, 24-100 Pulawy (Poland)

    2009-04-01

    A fast and simple liquid chromatography with tandem mass spectrometry method for detection and confirmation of tranquilizers (chlorpromazine, propionylpromazine, acepromazine, triflupromazine, promazine, azaperone and its metabolite, azaperol) and beta-blocker (carazolol) in porcine and bovine kidney has been presented. The method relies on the extraction with acetonitrile followed by centrifugation. After evaporation of acetonitrile, the residue was reconstituted in a mobile phase and filtrated. The separation of analytes was performed on a C18 column using a mobile phase of acetonitrile and ammonium formate buffer (0.05 M, pH 4.5) with gradient elution. The electrospray ionization was used to obtain the protonated molecules [M+H]{sup +} and two product ions were monitored for each compound. For quantification deutered internal standards were used. The whole method has been validated according to the European Union requirements. Specificity, decision limit (CC{alpha}), detection capability (CC{beta}), trueness and precision were determined. The results showed good trueness ranged from 73.2% to 110.6% with a good R.S.D., less than 13.0% under within-laboratory reproducibility conditions. The calculated critical concentrations of CC{alpha} for phenothiazines were between 5.8 and 6.6 {mu}g kg{sup -1} while for azaperone CC{alpha} was 105.5 {mu}g kg{sup -1} and for azaperol was 121.4 {mu}g kg{sup -1}. CC{alpha} for carazolol was 16.7 {mu}g kg{sup -1} in bovine and 21.9 {mu}g kg{sup -1} in porcine kidney. CC{beta} for phenothiazines were between 6.3 and 7.6 {mu}g kg{sup -1}, for azaperone was 119.0 {mu}g kg{sup -1} and for azaperol was 140.0 {mu}g kg{sup -1}. For carazolol in bovine kidney CC{beta} was 18.6 {mu}g kg{sup -1} whereas in porcine kidney was 24.4 {mu}g kg{sup -1}.

  14. Rapid ultra-trace analysis of sucralose in multiple-origin aqueous samples by online solid-phase extraction coupled to high-resolution mass spectrometry.

    Science.gov (United States)

    Batchu, Sudha Rani; Ramirez, Cesar E; Gardinali, Piero R

    2015-05-01

    Because of its widespread consumption and its persistence during wastewater treatment, the artificial sweetener sucralose has gained considerable interest as a proxy to detect wastewater intrusion into usable water resources. The molecular resilience of this compound dictates that coastal and oceanic waters are the final recipient of this compound with unknown effects on ecosystems. Furthermore, no suitable methodologies have been reported for routine, ultra-trace detection of sucralose in seawater as the sensitivity of traditional liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis is limited by a low yield of product ions upon collision-induced dissociation (CID). In this work, we report the development and field test of an alternative analysis tool for sucralose in environmental waters, with enough sensitivity for the proper quantitation and confirmation of this analyte in seawater. The methodology is based on automated online solid-phase extraction (SPE) and high-resolving-power orbitrap MS detection. Operating in full scan (no CID), detection of the unique isotopic pattern (100:96:31 for [M-H](-), [M-H+2](-), and [M-H+4](-), respectively) was used for ultra-trace quantitation and analyte identification. The method offers fast analysis (14 min per run) and low sample consumption (10 mL per sample) with method detection and confirmation limits (MDLs and MCLs) of 1.4 and 5.7 ng/L in seawater, respectively. The methodology involves low operating costs due to virtually no sample preparation steps or consumables. As an application example, samples were collected from 17 oceanic and estuarine sites in Broward County, FL, with varying salinity (6-40 PSU). Samples included the ocean outfall of the Southern Regional Wastewater Treatment Plant (WWTP) that serves Hollywood, FL. Sucralose was detected above MCL in 78% of the samples at concentrations ranging from 8 to 148 ng/L, with the exception of the WWTP ocean outfall (at pipe end, 28 m below the surface

  15. Rapid determination of polycyclic aromatic hydrocarbons (PAHs) in tea using two-dimensional gas chromatography coupled with time of flight mass spectrometry.

    Science.gov (United States)

    Drabova, Lucie; Pulkrabova, Jana; Kalachova, Kamila; Tomaniova, Monika; Kocourek, Vladimir; Hajslova, Jana

    2012-10-15

    A simple, fast, and cost effective sample preparation procedure has been developed and validated for the determination of 15+1 European Union Polycyclic Aromatic Hydrocarbons (15+1 EU PAHs) in dried tea leave samples. Based on a critical assessment of several sample extraction/clean-up approaches, the method based on the ethyl acetate extraction followed by the use of PAHs dedicated cartridges with molecularly imprinted polymers (MIPs) has been found as an optimal alternative in terms of time demands and obtained good extract purity. For the final identification/quantification of target PAHs, two dimensional gas chromatography coupled to a time-of-flight mass spectrometry (GC×GC-TOFMS) was used. The performance characteristics of the overall analytical method for individual PAHs determined at three spiking levels (0.5, 2.5 and 5 μg kg(-1)) were in following ranges: limits of quantitation (LOQs) 0.05-0.2 μg kg(-1), repeatabilities 2-9%, and recoveries 73-103%. The recoveries achieved by the newly developed sample preparation procedure when employed for naturally contaminated sample ("incurred" PAHs) were comparable to those obtained by other routinely used approaches employing sonication and/or pressurised liquid extraction for sample analytes isolation. The validated method was subsequently used for the determination of selected genotoxic PAHs in 36 samples of black and green tea obtained from the Czech retail market. The levels of ΣPAH4 (sum of benzo[a]anthracene (BaA), chrysene (CHR), benzo[b]fluoranthene (BbFA) and benzo[a]pyrene (BaP)) in black and green tea leaves ranged from 7.4 to 700 μg kg(-1) and from 4.5 to 102 μg kg(-1), respectively. Contamination of tested tea samples by BaP was in the range of 0.2-152 μg kg(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF) mass spectrometry as a tool for rapid diagnosis of potentially toxigenic Corynebacterium species in the laboratory management of diphtheria-associated bacteria.

    Science.gov (United States)

    Konrad, R; Berger, A; Huber, I; Boschert, V; Hörmansdorfer, S; Busch, U; Hogardt, M; Schubert, S; Sing, A

    2010-10-28

    The rapid identification of the potentially toxigenic Corynebacterium species, C. diphtheriae, C. ulcerans and C. pseudotuberculosis is essential for diagnosis and treatment of diphtheria and diphtheria-like diseases. We used matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDIT-OF MS) in comparison with classical microbiological and molecular methods on 116 Corynebacterium strains. All 90 potentially toxigenic Corynebacterium strains collected by the German National Consiliary Laboratory on Diphtheria in a period of more than ten years were correctly identified by MALDI-TOF MS. We propose an algorithm for fast and reliable diagnosis of diphtheria incorporating MALDI-TOF MS, real-time tox PCR and Elek testing.

  17. Rapid wide-scope screening of drugs of abuse, prescription drugs with potential for abuse and their metabolites in influent and effluent urban wastewater by ultrahigh pressure liquid chromatography-quadrupole-time-of-flight-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez, Felix, E-mail: felix.hernandez@qfa.uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellon (Spain); Bijlsma, Lubertus, E-mail: bijlsma@guest.uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellon (Spain); Sancho, Juan V.; Diaz, Ramon; Ibanez, Maria [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellon (Spain)

    2011-01-17

    This work illustrates the potential of hybrid quadrupole-time-of-flight mass spectrometry (QTOF MS) coupled to ultrahigh pressure liquid chromatography (UHPLC) to investigate the presence of drugs of abuse in wastewater. After solid-phase extraction with Oasis MCX cartridges, seventy-six illicit drugs, prescription drugs with potential for abuse, and metabolites were investigated in the samples by TOF MS using electrospray interface under positive ionization mode, with MS data acquired over an m/z range of 50-1000 Da. For 11 compounds, reference standards were available, and experimental data (e.g., retention time and fragmentation data) could be obtained, facilitating a more confident identification. The use of a QTOF instrument enabled the simultaneous application of two acquisition functions with different collision energies: a low energy (LE) function, where none or poor fragmentation took place, and a high energy (HE) function, where fragmentation in the collision cell was promoted. This approach, known as MS{sup E}, enabled the simultaneous acquisition of full-spectrum accurate mass data of both protonated molecules and fragment ions in a single injection, providing relevant information that facilitates the rapid detection and reliable identification of these emerging contaminants in the sample matrices analyzed. In addition, isomeric compounds, like the opiates, morphine and norcodeine, could be discriminated by their specific fragments observed in HE TOF MS spectra, without the need of reference standards. UHPLC-QTOF MS was proven to be a powerful and efficient technique for rapid wide-scope screening and identification of many relevant drugs in complex matrices, such as influent and effluent urban wastewater.

  18. Evaluation of repetitive-PCR and matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) for rapid strain typing of Bacillus coagulans.

    Science.gov (United States)

    Sato, Jun; Nakayama, Motokazu; Tomita, Ayumi; Sonoda, Takumi; Hasumi, Motomitsu; Miyamoto, Takahisa

    2017-01-01

    In order to establish rapid and accurate typing method for Bacillus coagulans strains which is important for controlling in some canned foods and tea-based beverages manufacturing because of the high-heat resistance of the spores and high tolerance of the vegetative cells to catechins and chemicals, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) and repetitive-PCR (rep-PCR) were evaluated. For this purpose, 28 strains of B. coagulans obtained from various culture collections were tested. DNA sequence analyses of the genes encoding 16S rRNA and DNA gyrase classified the test strains into two and three groups, respectively, regardless of their phenotypes. Both MALDI-TOF MS and rep-PCR methods classified the test strains in great detail. Strains classified in each group showed similar phenotypes, such as carbohydrate utilization determined using API 50CH. In particular, the respective two pairs of strains which showed the same metabolic characteristic were classified into the same group by both MALDI-TOF MS and rep-PCR methods separating from the other strains. On the other hand, the other strains which have the different profiles of carbohydrate utilization were separated into different groups by these methods. These results suggested that the combination of MALDI-TOF MS and rep-PCR analyses was advantageous for the rapid and detailed typing of bacterial strains in respect to both phenotype and genotype.

  19. Evaluation of repetitive-PCR and matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS for rapid strain typing of Bacillus coagulans.

    Directory of Open Access Journals (Sweden)

    Jun Sato

    Full Text Available In order to establish rapid and accurate typing method for Bacillus coagulans strains which is important for controlling in some canned foods and tea-based beverages manufacturing because of the high-heat resistance of the spores and high tolerance of the vegetative cells to catechins and chemicals, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS and repetitive-PCR (rep-PCR were evaluated. For this purpose, 28 strains of B. coagulans obtained from various culture collections were tested. DNA sequence analyses of the genes encoding 16S rRNA and DNA gyrase classified the test strains into two and three groups, respectively, regardless of their phenotypes. Both MALDI-TOF MS and rep-PCR methods classified the test strains in great detail. Strains classified in each group showed similar phenotypes, such as carbohydrate utilization determined using API 50CH. In particular, the respective two pairs of strains which showed the same metabolic characteristic were classified into the same group by both MALDI-TOF MS and rep-PCR methods separating from the other strains. On the other hand, the other strains which have the different profiles of carbohydrate utilization were separated into different groups by these methods. These results suggested that the combination of MALDI-TOF MS and rep-PCR analyses was advantageous for the rapid and detailed typing of bacterial strains in respect to both phenotype and genotype.

  20. Integrated rapid resolution liquid chromatography-tandem mass spectrometric approach for screening and identification of metabolites of the potential anticancer agent 3,6,7-trimethoxyphenanthroindolizidine in rat urine.

    Science.gov (United States)

    Tian, Yaping; He, Jiuming; Zhang, Ruiping; Lv, Haining; Ma, Shuanggang; Chen, Yanhua; Yu, Shishan; Chen, Xiaoguang; Wu, Yan; He, Wenyi; Abliz, Zeper

    2012-06-20

    An integrated approach combining data acquisition using MS(E) and multi-period product ion scan (mpMS/MS), with high-resolution characteristic extracted ion chromatograms (hcXIC) as a data mining method, was developed for in vivo drug metabolites screening and identification. This approach is illustrated by analyzing metabolites of a potential anticancer agent, 3,6,7-trimethoxyphenanthroindolizidine (CAT) in rat urine based on rapid resolution liquid chromatography combined with tandem mass spectrometry (RRLC-MS/MS). Untargeted full-scan MS(E) enabled the high-throughput acquisition of potential metabolites, and targeted mpMS/MS contributed to the sensitivity and specificity of the acquisition of molecules of interest. The data processing method hcXIC, based on the structure of CAT, was shown to be highly effective for the metabolite discovery. Through the double-filtering effect of the characteristic ion and accurate mass, conventional extracted ion chromatograms that contained a substantial number of false-positive peaks were simplified into chromatograms essentially free of endogenous interferences. As a result, 21 metabolites were detected in rat urine after oral administration of CAT. Based on the characteristic fragmentation patterns of the phenanthroindolizidine alkaloid, the structures of 9 metabolites were identified. Furthermore, the interpretation of the MS/MS spectra of these metabolites enabled the determination of demethylation position as well as the differentiation between N-oxidized and hydroxylated metabolites. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. A rapid method for the determination of perfluoroalkyl substances including structural isomers of perfluorooctane sulfonic acid in human serum using 96-well plates and column-switching ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Salihovic, Samira; Kärrman, Anna; Lindström, Gunilla; Lind, P Monica; Lind, Lars; van Bavel, Bert

    2013-08-30

    To facilitate high-throughput analysis suitable for large epidemiological studies we developed an automated column-switching ultra-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determination of perfluorocarboxylic acids (PFCAs; C5, C6, C7, C8, C9, C10, C11, C12, and C13), perfluoroalkyl sulfonic acids (PFSAs; C4, C6, C8, and C10), perfluorooctane sulfonamide (PFOSA), and five groups of structural perfluorooctane sulfonic acid (PFOS) isomers in human serum or plasma. The analytical procedure involves rapid protein precipitation using 96-well plates followed by an automated sample clean-up using an on-line trap column removing many potentially interfering sample components while through the mobile phase gradient the target analytes are eluted onto the analytical column for further separation and subsequent mass detection. The method was linear (R(2)determination of perfluoroalkyl substances including structural PFOS isomers in human plasma from an epidemiological study. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. A rapid method for the simultaneous determination of L-ascorbic acid and acetylsalicylic acid in aspirin C effervescent tablet by ultra performance liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    Wabaidur, Saikh Mohammad; Alothman, Zeid Abdullah; Khan, Mohammad Rizwan

    2013-05-01

    In present study, a rapid and sensitive method using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of L-ascorbic acid and acetylsalicylic acid in aspirin C effervescent tablet. The optimum chromatographic separation was carried out on a reversed phase Waters® Acquity UPLC BEH C18 column (1.7 μm particle size, 100 mm × 2.1 mm ID) with an isocratic elution profile and mobile phase consisting of 0.1% formic acid in water and acetonitrile (75:25, v/v, pH 3.5) at flow rate of 0.5 mL min-1. The influences of mobile phase composition, flow rate and pH on chromatographic resolution were investigated. The total chromatographic analysis time was as short as 2 min with excellent resolution. Detection and quantification of the target compounds were carried out with a triple quadrupole mass spectrometer using negative electrospray ionization (ESI) and multiple reaction monitoring (MRM) modes. The performance of the method was evaluated and very low limits of detection less than 0.09 μg g-1, excellent coefficient correlation (r2 > 0.999) with liner range over a concentration range of 0.1-1.0 μg g-1 for both L-ascorbic acid and acetylsalicylic acid, and good intraday and interday precisions (relative standard deviations (R.S.D.) effervescent tablet.

  3. The New Panacea in Metabolomics, Proteomics and Genomics - Electrochemistry/Mass Spectrometry

    Science.gov (United States)

    Kraj, A.; Chervet, J.P.; Purkerson, J.; Eysberg, M.

    2010-01-01

    RP-65 Combining Electrochemistry (EC) with Mass Spectrometry (MS) has shown great potential for the investigation of drug metabolism1,2,3. Recently, the use of EC/MS has been extended towards new applications such as: 1. Fast synthesis of metabolites in micro preparative mode to generate sufficient amounts for the characterization by NMR and/or use as reference material. A specially designed μ-preparative electrochemical flow cell will be presented. 2. Rapid risk assessments of drug-protein binding. Investigation of drug-protein adducts by conventionally used techniques (microsomal incubation, in-vivo studies) are very laborious and have often low efficiency. With the application of EC, it is possible to activate proteins and drugs within seconds to undergo covalent drug-protein binding. 3. Signal enhancement in MS Proteomics. EC/LC/MS can enhance the signal intensity in MS by using electroactive derivatizing agent (e.g. N-(2-Ferroceneethyl)maleimide (FEM) for stabilizing thiol groups in proteins) or directly improving ionization efficiency. 4. Oxidative damage of DNA. On-line EC/ESI-MS is novel tool to study oxidative processes of nucleic acids, as well as to create covalent drug adducts with nucleic acids. All these applications illustrate the tremendous power and broad applicability of electrochemistry as a promising tool to mimic nature's Redox reactions, including oxidative damage of DNA, protein stress, lipid oxidation, etc. [1] Jurva U., Wikstrom H. V., Weidolf L., Bruins A.P., Comparison between electrochemistry/mass spectrometry and cytochrome P450 catalyzed oxidation reactions, Rapid Commun. Mass Spectrom. 17 (2003) 800–810. [2] Baumann A., Lohmann W., Schubert B., Oberacher H., Karst U., Metabolic studies of tetrazepam based on electrochemical simulation incomparison to in vivo and in vitro methods, J. Chromatogr. A 1216 (2009) 3192–3198. [3] Lohmann W., Hayen H., Karst U.,Covalent Protein Modification by Reactive Drug Metabolites Using Online

  4. Analytical strategy for rapid identification and quantification of lubricant additives in mineral oil by high-performance thin-layer chromatography with UV absorption and fluorescence detection combined with mass spectrometry and infrared spectroscopy.

    Science.gov (United States)

    Dytkiewitz, Elisabeth; Morlock, Gertrud E

    2008-01-01

    A simple strategy for identification and quantification of lubricant additives in mineral oil was demonstrated by high-performance thin-layer chromatography with UV absorption and fluorescence detection using various coupling options, e.g., with attenuated total reflectance infrared (ATR-IR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, electrospray ionization mass spectrometry (ESI-MS), and direct analysis in real-time mass spectrometry (DART-MS). For the additives zinc bis(O,O'-diisobutyl dithiophosphate), zinc bis(O,O'-didodecyl dithiophosphate), and Anglamol 99, 2 chromatographic systems were developed, i.e., a reversed-phase (RP) system on RP2 plates using an acetonitrile-based mobile phase and a normal-phase system on silica gel 60 plates using a toluene-based gradient. Densitometry was performed by absorption measurement at 220 nm. Repeatabilities (relative standard deviation, n = 6) between 2.2 and 5.5% and correlation coefficients >0.9973 were highly satisfactory for the analysis of these additives in the mineral oil. Primuline reagent was used to improve the detection limit of the lipophilic additives by a factor of 2, followed by fluorescence measurement at UV 366/>400 nm. For rapid identification by ATR-IR and FTIR, the respective additive zones on the plate were online extracted by an interface called ChromeXtract, concentrated, and directly applied for measurements in the wave number range of 4000-400 cm(-1). Identification was confirmed by online ESI-MS within a minute using ChromeXtract and by DART-MS within seconds.

  5. Determination of unbound vismodegib (GDC-0449) concentration in human plasma using rapid equilibrium dialysis followed by solid phase extraction and high-performance liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Deng, Yuzhong; Wong, Harvey; Graham, Richard A; Liu, Wenbin; Shen, Heuy-shin; Shi, Yao; Wang, Laixin; Meng, Min; Malhi, Vikram; Ding, Xiao; Dean, Brian

    2011-07-15

    A rapid equilibrium dialysis (RED) assay followed by a solid phase extraction (SPE) high-performance liquid chromatography tandem mass spectrometry (LC-MS/MS) assay for the quantitative determination of unbound vismodegib in human plasma was developed and validated. The equilibrium dialysis was carried out using 0.3 mL plasma samples in the single-use plate RED system at 37°C for 6h. The dialysis samples (0.1 mL) were extracted using a Strata-X-C 33u Polymeric Strong Cation SPE plate and the resulting extracts were analyzed using reverse-phase chromatography and positive electrospray ionization (ESI) mass spectrometry. The standard curve, which ranged from 0.100 to 100 ng/mL for vismodegib, was fitted to a 1/x(2) weighted linear regression model. The lower limit of quantitation (LLOQ, 0.100 ng/mL) was sufficient to quantify unbound concentrations of vismodegib after dialysis. The intra-assay precision of the LC-MS/MS assay, based on the four analytical QC levels (LLOQ, low, medium and high), was within 7.7% CV and inter-assay precision was within 5.5% CV. The assay accuracy, expressed as %Bias, was within ±4.0% of the nominal concentration values. Extraction recovery of vismodegib was between 77.9 and 84.0%. The assay provides a means for accurate assessment of unbound vismodegib plasma concentrations in clinical studies. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. High-throughput ultra high performance liquid chromatography combined with mass spectrometry approach for the rapid analysis and characterization of multiple constituents of the fruit of Acanthopanax senticosus (Rupr. et Maxim.) Harms.

    Science.gov (United States)

    Han, Yue; Zhang, Aihua; Sun, Hui; Zhang, Yingzhi; Meng, Xiangcai; Yan, Guangli; Liu, Liang; Wang, Xijun

    2017-05-01

    Acanthopanax senticosus (Rupr. et Maxim.) Harms, a traditional Chinese medicine, has been widely used to improve the function of skeleton, heart, spleen and kidney. This fruit is rich in nutrients, but the chemical constituents of Acanthopanax senticosus fruit are still unclear. A rapid method based on ultra high performance liquid chromatography with time-of-flight mass spectrometry was developed for the compound analysis of Acanthopanax senticosus fruit in vitro and in vivo. In this study, the Acanthopanax senticosus fruit could significantly increase the weight of immune organs, promote the proliferation of lymphatic T cells, regulate the lymphatic B cell function, and decrease the ability of natural killer cells. A total of 104 compounds of Acanthopanax senticosus fruit including lignans, flavones, triterpenoidsaponins, phenolic acids, and other constituents were identified. Among them, seven chemical compounds were reported for the first time in the Acanthopanax senticosus fruit. Compared with the serum sample of blank and dosed samples, 24 prototype compositions were characterized. The results of our experiment could be helpful to understand the complex compounds of Acanthopanax senticosus fruit in vitro and in vivo for further pharmacological activity studies. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. The Profiling and Identification of the Absorbed Constituents and Metabolites of Guizhi Decoction in Rat Plasma and Urine by Rapid Resolution Liquid Chromatography Combined with Quadrupole-Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Hongjun Xiang

    2016-09-01

    Full Text Available Guizhi decoction (GZD, a well-known traditional Chinese medicine (TCM prescription consisting of Ramulus Cinnamomi, Radix Paeoniae Alba, Radix Glycyrrhizae, Fructus Jujubae and Rhizoma Zingiberis Recens, is usually used for the treatment of common colds, influenza, and other pyretic conditions in the clinic. However, the absorbed ingredients and metabolic compounds of GZD have not been reported. In this paper, a method incorporating rapid resolution liquid chromatography (RRLC with quadrupole-time-of-flight mass spectrometry (Q-TOF-MS was used to identify ingredients after oral administration of GZD. Identification of the primary components in GZD, drug-containing serum and urine samples was carried out in order to investigate the assimilation and metabolites of the decoction in vivo. By comparing the total ion chromatograms (TICs of GZD, a total of 71 constituents were detected or characterized. By comparing TICs of blank and dosed rat plasma, a total of 15 constituents were detected and identified as prototypes according to their retention time (tR and MS, MS/MS data. Based on this, neutral loss scans of 80 and 176 Da in samples of rat plasma and urine helped us to identify most of the metabolites. Results showed that the predominant metabolic pathways of (epi catechin and gallic acid were sulfation, methylation, glucuronidation and dehydroxylation; the major metabolic pathways of flavone were hydrolysis, sulfation and glucuronidation. Furthermore, degradation, oxidation and ring fission were found to often occur in the metabolism process of GZD in vivo.

  8. Rapid high-performance liquid chromatography-tandem mass spectrometry method for simultaneous measurement of venlafaxine and O-desmethylvenlafaxine in human plasma and its application in comparative bioavailability study.

    Science.gov (United States)

    Rajasekhar, D; Kumar, I Jaswanth; Venkateswarlu, P

    2009-12-01

    A rapid high-performance liquid chromatography-tandem mass spectrometry method has been developed and validated for simultaneous measurement of venlafaxine and O-desmethylvenlafaxine in human plasma using fluoxetine as an internal standard. In the liquid-liquid extraction method, compounds and internal standard were extracted from plasma using methyl tertiary butyl ether as an extraction solvent. The HPLC separation of the analytes was performed on a Zorbax SB-C(18), 50 x 4.6 mm, 5 microm column, using a isocratic elution program using a mobile phase consisting of HPLC-grade methanol: 5 mm ammonium acetate (80:20 v/v) at a flow-rate of 1.0 mL/min with a total runtime of 3.0 min. The proposed method has been validated with a linear range of 4-400 ng/mL for venlafaxine and 5-500 ng/mL for O-desmethyl venlafaxine. The method was applied for a bio-equivalence study of 75 mg tablets formulation in 32 Indian male healthy subjects under fasting conditions.

  9. Rapid Determination of 30 Polyphenols in Tongmai Formula, a Combination of Puerariae Lobatae Radix, Salviae Miltiorrhizae Radix et Rhizoma, and Chuanxiong Rhizoma, via Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Wang, Fu-Rong; Zhang, Ying; Yang, Xin-Bao; Liu, Chun-Xu; Yang, Xiu-Wei; Xu, Wei; Liu, Jian-Xun

    2017-03-29

    Tongmai formula (TMF) is a herbal preparation composed of three traditional Chinese medicinal materials: Puerariae Lobatae Radix (Gegen), Salviae Miltiorrhizae Radix et Rhizoma (Danshen) and Chuanxiong Rhizoma (Chuanxiong). It has been used to treat cardiovascular diseases for decades. To develop a reliable and convenient analytical method for a comprehensive determination of polyphenols in TMF and the ascertainment of their chemical correlations with its herbal components, a method combining high-performance liquid chromatography with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) was developed and validated for rapid determination of 30 polyphenols in TMF and its three herbal components. The chromatographic separation was carried out on a Chromolith Fastgradient RP-18 endcapped 50-2 column using an optimized gradient elution. Statistical analysis of obtained data demonstrated that the method had a desirable linearity, precision, and accuracy, as well as excellent sensitivity. The obtained results indicated that, among the 30 polyphenols in TMF, 22 originated from Gegen, 6 originated from Danshen, and 2 originated from Chuanxiong. The major polyphenols in TMF have been identified as puerarin, mirificin, salvianolic acid B, salvianic acid A, 3'-hydroxypuerarin, 3'-methoxypuerarin, and salvianolic acid A, with a combined contribution of 19.2% of the preparation. The development and validation of this method will greatly facilitate future pharmacological studies of TMF and its herbal components, as well as polyphenols in cardiovascular therapies.

  10. Gas chromatography-mass spectrometry method for rapid identification and differentiation of Burkholderia pseudomallei and Burkholderia mallei from each other, Burkholderia thailandensis and several members of the Burkholderia cepacia complex.

    Science.gov (United States)

    Li, D; March, J K; Bills, T M; Holt, B C; Wilson, C E; Lowe, W; Tolley, H D; Lee, M L; Robison, R A

    2013-11-01

    To develop a simple gas chromatography-mass spectrometry (GC-MS) method for the detection and differentiation of Burkholderia pseudomallei and Burkholderia mallei from each other, Burkholderia thailandensis and several members of the Burkholderia cepacia complex. Biomarkers were generated by one-step thermochemolysis (TCM) and analysed using a GC-MS system. Fragments of poly-3-hydroxybutyrate-co-hydroxyvalerate [poly(3HBA-co-3HVA)] produced by TCM were useful biomarkers. Several cellular fatty acid methyl esters were important in differentiating the various Burkholderia species. A statistical discrimination algorithm was constructed using a combination of biomarkers. The identities of four B. pseudomallei strains, four B. mallei strains and one strain of each near neighbour were confirmed in a statistically designed test using the algorithm. The detection limit for this method was found to be approximately 4000 cells. The method is fast, accurate and easy to use. The algorithm is robust against different growth conditions (medium and temperature). This assay may prove beneficial in a clinical diagnostic setting, where the rapid identification of B. pseudomallei is essential to effective treatment. This method could also be easily employed after a biological attack to confirm the presence of either B. pseudomallei or B. mallei. © 2013 The Society for Applied Microbiology.

  11. Rapid and sensitive analysis of phthalate metabolites, bisphenol A, and endogenous steroid hormones in human urine by mixed-mode solid-phase extraction, dansylation, and ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Wang, He-xing; Wang, Bin; Zhou, Ying; Jiang, Qing-wu

    2013-05-01

    Steroid hormone levels in human urine are convenient and sensitive indicators for the impact of phthalates and/or bisphenol A (BPA) exposure on the human steroid hormone endocrine system. In this study, a rapid and sensitive method for determination of 14 phthalate metabolites, BPA, and ten endogenous steroid hormones in urine was developed and validated on the basis of ultra-performance liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry. The optimized mixed-mode solid phase-extraction separated the weakly acidic or neutral BPA and steroid hormones from acidic phthalate metabolites in urine: the former were determined in positive ion mode with a methanol/water mobile phase containing 10 mM ammonium formate; the latter were determined in negative ion mode with a acetonitrile/water mobile phase containing 0.1 % acetic acid, which significantly alleviated matrix effects for the analysis of BPA and steroid hormones. Dansylation of estrogens and BPA realized simultaneous and sensitive analysis of the endogenous steroid hormones and BPA in a single chromatographic run. The limits of detection were less than 0.84 ng/mL for phthalate metabolites and less than 0.22 ng/mL for endogenous steroid hormones and BPA. This proposed method had satisfactory precision and accuracy, and was successfully applied to the analyses of human urine samples. This method could be valuable when investigating the associations among endocrine-disrupting chemicals, endogenous steroid hormones, and relevant adverse outcomes in epidemiological studies.

  12. Preconcentration and sensitive determination of hexabromocyclododecane diastereomers in environmental water samples using solid phase extraction with bamboo charcoal cartridge prior to rapid resolution liquid chromatography-electrospray tandem mass spectrometry.

    Science.gov (United States)

    Zhao, Ru-Song; Hu, Cong; Zhou, Jia-Bin; Yuan, Jin-Peng; Wang, Shan-Shan; Wang, Xia

    2011-05-01

    In this paper, a simple and cheap method for the simultaneous preconcentration and sensitive determination of three hexabromocyclododecane (HBCD) diastereomers (α-, β-, and γ-HBCD) in environmental water samples has been developed. It was based on solid phase extraction (SPE) and rapid resolution liquid chromatography-electrospray tandem mass spectrometry. Bamboo charcoal, one kind of cheap material, was investigated and used as SPE adsorbent for the enrichment and determination of HBCD diastereomers. Related important parameters affecting extraction efficiencies, including type and volume of eluant, amount of sorbent, sample pH, flow rate, and sample volume, were investigated and optimized in detail. Under the optimum conditions, experimental data exhibited excellent linear relationships between peak area and concentrations over the range 0.1-10 μg L(-1). The limits of detection and precision were in the range of 0.005-0.015 μg L(-1) and 4.59-7.47%, respectively. The proposed method has been successfully applied for the trace analysis of HBCD diastereomers in real-world environmental water samples.

  13. Rapid Prototyping

    Science.gov (United States)

    1999-01-01

    Javelin, a Lone Peak Engineering Inc. Company has introduced the SteamRoller(TM) System as a commercial product. The system was designed by Javelin during a Phase II NASA funded small commercial product. The purpose of the invention was to allow automated-feed of flexible ceramic tapes to the Laminated Object Manufacturing rapid prototyping equipment. The ceramic material that Javelin was working with during the Phase II project is silicon nitride. This engineered ceramic material is of interest for space-based component.

  14. Adiabatic Betatron deceleration of ionospheric charged particles: a new explanation for (i) the rapid outflow of ionospheric O ions, and for (ii) the increase of plasma mass density observed in magnetospheric flux tubes during main phases of geomagnetic s

    Science.gov (United States)

    Lemaire, Joseph; Pierrard, Viviane; Darrouzet, Fabien

    2013-04-01

    Using European arrays of magnetometers and the cross-phase analysis to determine magnetic field line resonance frequencies, it has been found by Kale et al. (2009) that the plasma mass density within plasmaspheric flux tubes increased rapidly after the SSC of the Hallowe'en 2003 geomagnetic storms. These observations tend to confirm other independent experimental results, suggesting that heavy ion up-flow from the ionosphere is responsible for the observed plasma density increases during main phases of geomagnetic storms. The aim of our contribution is to point out that, during main phases, reversible Betatron effect induced by the increase of the southward Dst-magnetic field component (|Δ Bz|), diminishes slightly the perpendicular kinetic energy (W?) of charged particles spiraling along field lines. Furthermore, due to the conservation of the first adiabatic invariant (μ = Wm/ Bm) the mirror points of all ionospheric ions and electrons are lifted up to higher altitudes i.e. where the mirror point magnetic field (Bm) is slightly smaller. Note that the change of the mirror point altitude is given by: Δ hm = -1/3 (RE + hm) Δ Bm / Bm. It is independent of the ion species and it does not depend of their kinetic energy. The change of kinetic energy is determined by: Δ Wm = Wm Δ Bm / Bm. Both of these equations have been verified numerically by Lemaire et al. (2005; doi: 10.1016/S0273-1177(03)00099-1) using trajectory calculations in a simple time-dependant B-field model: i.e. the Earth's magnetic dipole, plus an increasing southward B-field component: i.e. the Dst magnetic field whose intensity becomes more and more negative during the main phase of magnetic storms. They showed that a variation of Bz (or Dst) by more than - 50 nT significantly increases the mirror point altitudes by more than 100 km which is about equal to scale height of the plasma density in the topside ionosphere where particles are almost collisionless (see Fig. 2 in Lemaire et al., 2005

  15. Multi-class, multi-residue analysis of trace veterinary drugs in milk by rapid screening and quantification using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Yaqian; Li, Xiang; Liu, Xiaomao; Zhang, Jinjie; Cao, Yanzhong; Shi, Zhihong; Sun, Hanwen

    2015-12-01

    A simple and rapid multi-class multi-residue analytical method was developed for the screening and quantification of veterinary drugs in milk by ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS). A total of 90 veterinary drugs investigated belonged to almost 20 classes including lincomycins, macrolides, sulfonamides, quinolones, tetracyclines, β-agonists, β-lactams, sedatives, β-receptor antagonists, sex hormones, glucocorticoids, nitroimidazoles, benzimidazoles, nitrofurans, and some others. A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure was developed for the sample preparation without the solid-phase extraction step. The linearity, sensitivity, accuracy, repeatability, and reproducibility of the method were fully validated. The response of the detector was linear for each target compound in a wide concentration range with a correlation coefficient (R(2)) of 0.9973 to 0.9999 (among them R(2)>0.999 for 73 of 90 analytes). The range of the limit of quantification for these compounds in the milk ranged from 0.10 to 17.30μg/kg. The repeatability and reproducibility were in the range of 2.11 to 9.62% and 2.76 to 13.9%, respectively. The average recoveries ranged from 72.62 to 122.2% with the RSD (n=6) of 1.30 to 9.61% at 3 concentration levels. For the screening method, the data of the precursor and product ions of the target analytes were simultaneously acquired under the all ions MS/MS mode in a single run. An accurate mass database for the confirmation and identification of the target compounds was established. The applicability of the screening method was verified by applying to real milk samples. The proposed analytical method allows the identification and confirmation of the target veterinary drugs at trace levels employing quick analysis time. Certain veterinary drugs were detected in some cases. Copyright © 2015 American Dairy Science Association. Published by

  16. A rapid and high-precision method for sulfur isotope δ(34)S determination with a multiple-collector inductively coupled plasma mass spectrometer: matrix effect correction and applications for water samples without chemical purification.

    Science.gov (United States)

    Lin, An-Jun; Yang, Tao; Jiang, Shao-Yong

    2014-04-15

    Previous studies have indicated that prior chemical purification of samples, although complex and time-consuming, is essential in obtaining precise and accurate results for sulfur isotope ratios using multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). In this study, we introduce a new, rapid and precise MC-ICP-MS method for sulfur isotope determination from water samples without chemical purification. The analytical work was performed on an MC-ICP-MS instrument with medium mass resolution (m/Δm ~ 3000). Standard-sample bracketing (SSB) was used to correct samples throughout the analytical sessions. Reference materials included an Alfa-S (ammonium sulfate) standard solution, ammonium sulfate provided by the lab of the authors and fresh seawater from the South China Sea. A range of matrix-matched Alfa-S standard solutions and ammonium sulfate solutions was used to investigate the matrix (salinity) effect (matrix was added in the form of NaCl). A seawater sample was used to confirm the reliability of the method. Using matrix-matched (salinity-matched) Alfa-S as the working standard, the measured δ(34)S value of AS (-6.73 ± 0.09‰) was consistent with the reference value (-6.78 ± 0.07‰) within the uncertainty, suggesting that this method could be recommended for the measurement of water samples without prior chemical purification. The δ(34)S value determination for the unpurified seawater also yielded excellent results (21.03 ± 0.18‰) that are consistent with the reference value (20.99‰), thus confirming the feasibility of the technique. The data and the results indicate that it is feasible to use MC-ICP-MS and matrix-matched working standards to measure the sulfur isotopic compositions of water samples directly without chemical purification. In comparison with the existing MC-ICP-MS techniques, the new method is better for directly measuring δ(34)S values in water samples with complex matrices; therefore, it can

  17. Comparison of ZnS semiconductor nanoparticles capped with various functional groups as the matrix and affinity probes for rapid analysis of cyclodextrins and proteins in surface-assisted laser desorption/ionization time-of-flight mass spectrometry.

    Science.gov (United States)

    Kailasa, Suresh Kumar; Kiran, Kamatam; Wu, Hui-Fen

    2008-12-15

    Zinc sulfide (ZnS) semiconductor nanoparticles (NPs) capped with a variety of functional groups including bare ZnS NPs, 3-mercaptopropanoic acid (ZnS-3-MPA), sodium citrate (ZnS-citrate), cysteamine (ZnS-Cys), and 2-mercaptoethane sulfonate (ZnS-2-MES) have been investigated as the matrix and affinity probes for analysis of alpha-, beta-, and gamma-cyclodextrins (CDs), ubiquitin, and insulin in biological samples by using surface-assisted laser desorption/ionization time-of-flight mass spectrometry (SALDI-TOF-MS). Various parameters that would influence the ionization efficiency and sensitivity of these ZnS NPs in SALDI-TOF-MS were examined including the effect of capping agents, sample pH, ion abundance, and concentration of ZnS NPs. Among these ZnS NPs, our results have demonstrated that ZnS-3-MPA exhibited the highest efficiency toward CDs, ubiquitin, and insulin for high-sensitivity detection in SALDI-TOF-MS. The detection limits were 20-55 nM for CDs, 91 nM for ubiquitin, and 85 nM for insulin. The applicability of the present method is demonstrated by detection of ubiquitin-like proteins in oyster mushroom and also in the analysis of analytes in biological samples such as human urine and plasma. To our best knowledge, this is the first time semiconductor NPs were used as the matrix and affinity probes for high-sensitivity detection of organic and biomolecules in SALDI-TOF-MS. This approach exhibits the advantages of being simple, rapid, efficient, and straightforward for direct analysis of organic and biological samples in SALDI-TOF-MS without the need for time-consuming separation processes, tedious washing steps, or further laborious purification. In addition, it also can provide a sensitive and reliable quantitative assay for small- and large-molecule analysis with the detectable mass up to 8500 Da. We believe that this novel ZnS nanoprobe is simple, efficient, lower cost (compared with Au, Ag, and Pt NPs), fast, and with the potential for high

  18. Ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride as a novel matrix for rapid quantitative and qualitative determination of serum free fatty acids by matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yaping [Department of Biophysics and Structural Biology, Institute of Basic Medical Sciences, Chinese Academy of Medical Sciences and School of Basic Medicine, Peking Union Medical College, 5 Dongdan San Tiao, Beijing 100005 (China); Wang, Yanmin [Department of Clinical Laboratory, Heze Municipal Hospital, Shandong (China); Guo, Shuai; Guo, Yumei; Liu, Hui [Department of Biophysics and Structural Biology, Institute of Basic Medical Sciences, Chinese Academy of Medical Sciences and School of Basic Medicine, Peking Union Medical College, 5 Dongdan San Tiao, Beijing 100005 (China); Li, Zhili, E-mail: lizhili@ibms.pumc.edu.cn [Department of Biophysics and Structural Biology, Institute of Basic Medical Sciences, Chinese Academy of Medical Sciences and School of Basic Medicine, Peking Union Medical College, 5 Dongdan San Tiao, Beijing 100005 (China)

    2013-09-10

    Graphical abstract: -- Highlights: •A novel MALDI matrix for the detection of serum free fatty acids is ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride. •Multiple point internal standard calibration curves were constructed for nine FFAs, respectively, with excellent correlation coefficients between 0.991 and 0.999. •The MALDI-MS approach was used to rapidly differentiate the patients with and without hyperglycemia and healthy controls. -- Abstract: The blood free fatty acids (FFAs), which provide energy to the cell and act as substrates in the synthesis of fats, lipoproteins, liposaccharides, and eicosanoids, involve in a number of important physiological processes. In the present study, matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR MS) with ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride (ATNEDC) as a novel MALDI matrix in a negative ion mode was employed to directly quantify serum FFAs. Multiple point internal standard calibration curves between the concentration ratios of individual fatty acids to internal standard (IS, C{sub 17:0}) versus their corresponding intensity ratios were constructed for C{sub 14:0}, C{sub 16:1}, C{sub 16:0}, C{sub 18:0}, C{sub 18:1}, C{sub 18:2}, C{sub 18:3}, C{sub 20:4}, and C{sub 22:6}, respectively, in their mixture, with correlation coefficients between 0.991 and 0.999 and limits of detection (LODs) between 0.2 and 5.4 μM, along with the linear dynamic range of more than two orders of magnitude. The results indicate that the multiple point internal standard calibration could reduce the impact of ion suppression and improve quantification accuracy in the MALDI mode. The quantitative results of nine FFAs from 339 serum samples, including 161 healthy controls, 118 patients with hyperglycemia and 60 patients without hyperglycemia show that FFAs levels in hyperglycemic patient sera are significantly higher than those in healthy

  19. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF) directly from positive blood culture flasks allows rapid identification of bloodstream infections in immunosuppressed hosts.

    Science.gov (United States)

    Egli, A; Osthoff, M; Goldenberger, D; Halter, J; Schaub, S; Steiger, J; Weisser, M; Frei, R

    2015-06-01

    In immunosuppressed hosts, rapid identification of microorganisms of bloodstream infections is crucial to ensuring effective antimicrobial therapy. Conventional culture requires up to 72 h from sample collection to pathogen identification. We used the SepsiTyper Kit and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF; Microflex, Bruker) directly from positive blood culture (BacT/ALERT 3D, FN/FA vials; bioMérieux) in comparison to standard culture methodology (VITEK 2; bioMérieux) for species identification. A total of 62 consecutive positive blood cultures from immunosuppressed patients (solid organ or hematopoietic transplant recipients, or with febrile neutropenia) were analyzed. Culture yielded gram-negative bacteria (GNB) in 27/62 (43.5%) and gram-positive (GPB) in 35/62 (56.5%) vials. For GNB, the predominant species identified by MALDI-TOF and confirmed by VITEK were Escherichia coli (16/16 correctly identified) and Enterobacter cloacae (4/4), with a sensitivity and specificity of 92.6% and 100%, respectively. For GPB, predominant species were Staphylococcus aureus (3/3), coagulase-negative staphylococci (12/24), and Enterococcus faecium (6/6) with a sensitivity of 100%, 60%, and 100%, respectively. The median time from blood collection to species identification was 27.4 h with MALDI-TOF identification and 46.6 h with conventional methodology. Using MALDI-TOF directly from positive blood cultures allowed a shorter time to identification with high sensitivity and specificity in immunosuppressed patients. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  20. Universal protocol for the rapid automated detection of carbapenem-resistant Gram-negative bacilli directly from blood cultures by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF/MS).

    Science.gov (United States)

    Oviaño, Marina; Sparbier, Katrin; Barba, Maria José; Kostrzewa, Markus; Bou, Germán

    2016-12-01

    Detection of carbapenemase-producing bacteria directly from blood cultures is a major challenge, as patients with bacteraemia are critically ill. Early detection can be helpful for selection of the most appropriate antibiotic therapy as well as adequate control of outbreaks. In the current study, a novel matrix-assisted laser desorption/ionisation time-of-flight (MALDI-TOF)-based method was developed for the rapid, automated detection of carbapenemase-producing Enterobacteriaceae, Pseudomonas aeruginosa and Acinetobacter baumannii directly from blood cultures. Carbapenemase activity was determined in 30 min by measuring hydrolysis of imipenem (0.31 mg/mL) in blood cultures spiked with a series of 119 previously characterised isolates, 81 of which carried a carbapenemase enzyme (10 blaKPC, 10 blaVIM, 10 blaNDM, 10 blaIMP, 26 blaOXA-48-type, 9 blaOXA-23, 1 blaOXA-237, 3 blaOXA-24 and 2 blaOXA-58). Twenty blood cultures obtained from bacteraemic patients carrying blaOXA-48-producing isolates were also analysed using the same protocol. Analysis was performed using MALDI-TOF Biotyper® Compass software, which automatically provides a result of sensitivity or resistance, calculated as the logRQ or ratio of hydrolysis of the antibiotic. This assay is simple to perform, inexpensive, time saving, universal for Gram-negative bacilli, and highly reliable (overall sensitivity and specificity of 98% and 100%, respectively). Moreover, the protocol could be established as a standardised method in clinical laboratories as it does not require specialised training in mass spectrometry. Copyright © 2016 Elsevier B.V. and International Society of Chemotherapy. All rights reserved.

  1. A rapid method for simultaneous determination of zearalenone, α-zearalenol, β-zearalenol, zearalanone, α-zearalanol and β-zearalanol in traditional Chinese medicines by ultra-high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Han, Zheng; Ren, Yiping; Zhou, Hailong; Luan, Lianjun; Cai, Zengxuan; Wu, Yongjiang

    2011-02-15

    A rapid and reliable ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous determination of zearalenone (ZEN), α-zearalenol (α-ZOL), β-zearalenol (β-ZOL), zearalanone (ZAN), α-zearalanol (α-ZAL) and β-zearalanol (β-ZAL) in traditional Chinese medicines (TCMs) was developed. The development of the method and investigations of the matrix influence were described in particular. After evaluation of the matrix effects of different TCMs, i.e., rhizomes and roots, seeds, flowers, grasses and leaves, by the post-extraction spiked method, a reliable sample clean-up method based on home-made clean-up cartridges, a suitable internal standard and the matrix calibration were combined using to minimize the matrix effects to ensure the accuracy of the method. The established method was further validated by determining the linearity (R(2)≥0.9990), sensitivity (limit of quantitation 0.11-0.99 ng mL(-1)), average recovery (86.6-113.5%) and precision (relative standard deviation ≤13.5%). It was shown to be a suitable method for simultaneous determination of ZEN, α-ZOL, β-ZOL, ZAN, α-ZAL and β-ZAL in different TCMs. Finally, the established method was successfully applied to the determination of the six mycotoxins in various TCMs and the results were presented to provide relevant insights to researchers in TCM analysis. Copyright © 2010 Elsevier B.V. All rights reserved.

  2. Diagnostic Accuracy of Loop-mediated Isothermal Amplifica-tion Assay as a Field Molecular Tool for Rapid Mass Screening of Old World Leishmania Infections in Sand Flies and In Vitro Culture

    Directory of Open Access Journals (Sweden)

    Mehdi GHODRATI

    2017-12-01

    Full Text Available AbstractBackground: We employed a highly sensitive loop-mediated isothermal amplification (LAMP by targeting 18S rRNA gene to identify the rapid mass screening of Leishmania infections in captured sand flies of southwest Iran and In vitro culture. Methods: One hundred fifty sand flies were collected from 11 sites adjacent to Iraqi’s borders in southern parts of Khuzestan Province by using sticky sheets of paper and CDC miniature light traps during late May 2014 to Nov 2015. Following morphological identification of sand flies species, the DNA of infected samples was extracted and amplified by PCR and LAMP assays by targeting ITS-rDNA and 18S rRNA genes. The PCR amplicons were directly sequenced to conduct the phylogenetic analysis Results: Ten (6.6% Leishmania infections were identified by LAMP assay (detection limit 0.01 parasites DNA among infected Sergentomyia baghdadis, S. sintoni and Phlebotomus papatasi sand flies that was more sensitive than PCR (n=6.4%; (detection limit 101parasites DNA. LAMP can identify 101-106promastigotes/100 µl RPMI 1640 while PCR recognized104-106 promastigotes. The majority infection rate of sand flies was confirmed to L. major inferred by phylogenetic analysis. Conclusion: This is the first exploration characterized the Old World Leishmania infections by LAMP technique in both infected sand flies and In vitro conditions. The LAMP method because of its shorter reaction time, robustness, more sensitivity, lack of requirement of complicated equipment and visual discriminatory of positivity can be appeared a promising tool instead of PCR to identify low Leishmania loads and entomological monitoring of leishmaniasis in resource-limited endemic of the world.

  3. Development and Validation of a Rapid 13C6-Glucose Isotope Dilution UPLC-MRM Mass Spectrometry Method for Use in Determining System Accuracy and Performance of Blood Glucose Monitoring Devices

    Science.gov (United States)

    Matsunami, Risë K.; Angelides, Kimon; Engler, David A.

    2015-01-01

    Background: There is currently considerable discussion about the accuracy of blood glucose concentrations determined by personal blood glucose monitoring systems (BGMS). To date, the FDA has allowed new BGMS to demonstrate accuracy in reference to other glucose measurement systems that use the same or similar enzymatic-based methods to determine glucose concentration. These types of reference measurement procedures are only comparative in nature and are subject to the same potential sources of error in measurement and system perturbations as the device under evaluation. It would be ideal to have a completely orthogonal primary method that could serve as a true standard reference measurement procedure for establishing the accuracy of new BGMS. Methods: An isotope-dilution liquid chromatography/mass spectrometry (ID-UPLC-MRM) assay was developed using 13C6-glucose as a stable isotope analogue to specifically measure glucose concentration in human plasma, and validated for use against NIST standard reference materials, and against fresh isolates of whole blood and plasma into which exogenous glucose had been spiked. Assay performance was quantified to NIST-traceable dry weight measures for both glucose and 13C6-glucose. Results: The newly developed assay method was shown to be rapid, highly specific, sensitive, accurate, and precise for measuring plasma glucose levels. The assay displayed sufficient dynamic range and linearity to measure across the range of both normal and diabetic blood glucose levels. Assay performance was measured to within the same uncertainty levels (glucose measurement in human serum. Conclusions: The newly developed ID UPLC-MRM assay can serve as a validated reference measurement procedure to which new BGMS can be assessed for glucose measurement performance. PMID:25986627

  4. Development and Validation of a Rapid (13)C6-Glucose Isotope Dilution UPLC-MRM Mass Spectrometry Method for Use in Determining System Accuracy and Performance of Blood Glucose Monitoring Devices.

    Science.gov (United States)

    Matsunami, Risë K; Angelides, Kimon; Engler, David A

    2015-05-18

    There is currently considerable discussion about the accuracy of blood glucose concentrations determined by personal blood glucose monitoring systems (BGMS). To date, the FDA has allowed new BGMS to demonstrate accuracy in reference to other glucose measurement systems that use the same or similar enzymatic-based methods to determine glucose concentration. These types of reference measurement procedures are only comparative in nature and are subject to the same potential sources of error in measurement and system perturbations as the device under evaluation. It would be ideal to have a completely orthogonal primary method that could serve as a true standard reference measurement procedure for establishing the accuracy of new BGMS. An isotope-dilution liquid chromatography/mass spectrometry (ID-UPLC-MRM) assay was developed using (13)C6-glucose as a stable isotope analogue to specifically measure glucose concentration in human plasma, and validated for use against NIST standard reference materials, and against fresh isolates of whole blood and plasma into which exogenous glucose had been spiked. Assay performance was quantified to NIST-traceable dry weight measures for both glucose and (13)C6-glucose. The newly developed assay method was shown to be rapid, highly specific, sensitive, accurate, and precise for measuring plasma glucose levels. The assay displayed sufficient dynamic range and linearity to measure across the range of both normal and diabetic blood glucose levels. Assay performance was measured to within the same uncertainty levels (glucose measurement in human serum. The newly developed ID UPLC-MRM assay can serve as a validated reference measurement procedure to which new BGMS can be assessed for glucose measurement performance. © 2015 Diabetes Technology Society.

  5. Rapid collection and identification of a novel component from Clausena lansium Skeels leaves by means of three-dimensional preparative gas chromatography and nuclear magnetic resonance/infrared/mass spectrometric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Sciarrone, Danilo [Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina (Italy); Chromaleont s.r.l. A start-up of the University of Messina, c/o University of Messina, Viale Annunziata, 98168 Messina (Italy); Pantò, Sebastiano [Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina (Italy); Rotondo, Archimede [Dipartimento di Scienze Chimiche, Università di Messina, Via D’Alcontres 31, 98166 Messina (Italy); Tedone, Laura; Tranchida, Peter Quinto [Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina (Italy); Dugo, Paola [Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus Bio-Medico, Via Álvaro del Portillo, 21 - 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus Bio-Medico, Via Álvaro del Portillo, 21 - 00128 Roma (Italy)

    2013-06-27

    Graphical abstract: -- Highlights: •A recently-developed three-dimensional prep-GC system has been applied to wampee essential oil. •The prep GC system enables the rapid collection of pure compounds from complex samples. •An isolated unknown solute was identified through NMR, IR and MS data. •The structure of an oxygenated sesquiterpene is here reported for the first time. -- Abstract: The present research reports the use of a three-dimensional preparative gas chromatography (prep GC) system, equipped with three Deans-switch devices and 5%diphenyl/wax/mid-polarity ionic liquid stationary phases, for the isolation of volatile components from a complex natural source, namely wampee essential oil (derived from Clausena lansium Skeels leaves). Collection was performed by using a simple and effective lab-constructed trapping device. Initially, an unknown (and abundant) wampee oil constituent was erroneously identified as α-sinensal, through an MS database search (a low similarity match was attained), performed after a GC-quadMS experiment., The unknown compound was then the isolated by using the novel prep GC system, in a highly pure form (at the mg level), and was correctly identified by using nuclear magnetic resonance (NMR), Fourier transform infrared spectroscopy (FTIR) and mass spectrometry (MS). Both FTIR and MS data were used to confirm the NMR information. The name given to the molecule was (2E,6E)-2-methyl-6-(4-methylcyclohex-3-enylidene)hept-2-enal. The results herein described will demonstrate the need for a high-resolution GC step, prior to analyte collection, in the prep GC analysis of complex samples.

  6. A simple and rapid analytical method based on solid-phase extraction and liquid chromatography-tandem mass spectrometry for the simultaneous determination of free catecholamines and metanephrines in urine and its application to routine clinical analysis.

    Science.gov (United States)

    Woo, Hye In; Yang, Jeong Soo; Oh, Hyeon Ju; Cho, Yoon Young; Kim, Jae Hyeon; Park, Hyung-Doo; Lee, Soo-Youn

    2016-05-01

    Urinary catecholamines and metanephrines are biochemical indicators of pheochromocytoma. We developed and validated a rapid and precise analytical method based on solid-phase extraction (SPE) and liquid chromatography separation coupled to tandem mass spectrometry (LC-MS/MS) for measuring urinary free catecholamines and metanephrines in a clinical setting. Following SPE purification of catecholamines and metanephrines from urine specimens, chromatographic separation and quantitative detection were performed using LC-MS/MS. The developed method for simultaneous measurement of urinary free catecholamines and metanephrines was validated with clinical urine specimens and was compared with other clinical and biochemical results, including urinary total metanephrines, vanillylmandelic acid (VMA), and plasma free metanephrines. The performance of our newly developed method for measuring urinary free epinephrine (EPI), norepinephrine (NE), dopamine (DA), metanephrine (MN), and normetanephrine (NMN), was acceptable. The recoveries and matrix effects of analytes were 61-107% and 84.5-130.7%. The linear ranges of each analyte were 3.8-2163μg/L, 7.4-2,359μg/L, 5.4-2,825μg/L, 3.5-2,466μg/L, and 3.7-2,569μg/L, and the coefficients of variation (CV) were less than 10% with respect to imprecision. Carryover and sample stability were also validated. Validation using clinical urine specimens by comparison with various biochemical results showed that urinary free metanephrines had comparable sensitivity (100%) and superior specificity (97.1%) to urinary total and plasma free metanephrines. The facile and reliable simultaneous measurement method for urinary free catecholamines and metanephrines using LC-MS/MS developed in this study is helpful in obtaining information about multiple metabolites and is applicable to routine clinical settings for the screening of pheochromocytoma. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights

  7. Evaluation of repetitive-PCR and matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) for rapid strain typing of Bacillus coagulans

    National Research Council Canada - National Science Library

    Jun Sato; Motokazu Nakayama; Ayumi Tomita; Takumi Sonoda; Motomitsu Hasumi; Takahisa Miyamoto

    2017-01-01

    In order to establish rapid and accurate typing method for Bacillus coagulans strains which is important for controlling in some canned foods and tea-based beverages manufacturing because of the high...

  8. Rapid chemical separations

    CERN Document Server

    Trautmann, N

    1976-01-01

    A survey is given on the progress of fast chemical separation procedures during the last few years. Fast, discontinuous separation techniques are illustrated by a procedure for niobium. The use of such techniques for the chemical characterization of the heaviest known elements is described. Other rapid separation methods from aqueous solutions are summarized. The application of the high speed liquid chromatography to the separation of chemically similar elements is outlined. The use of the gas jet recoil transport method for nuclear reaction products and its combination with a continuous solvent extraction technique and with a thermochromatographic separation is presented. Different separation methods in the gas phase are briefly discussed and the attachment of a thermochromatographic technique to an on-line mass separator is shown. (45 refs).

  9. Rapid response manufacturing (RRM)

    Energy Technology Data Exchange (ETDEWEB)

    Cain, W.D. [Lockheed Martin Energy Systems, Inc., Oak Ridge, TN (United States); Waddell, W.L. [National Centers for Manufacturing Sciences, Ann Arbor, MI (United States)

    1997-02-18

    US industry is fighting to maintain its competitive edge in the global market place. Today markets fluctuate rapidly. Companies, to survive, have to be able to respond with quick-to-market, improved, high quality, cost efficient products. The way products are developed and brought to market can be improved and made more efficient through the proper incorporation of emerging technologies. The RRM project was established to leverage the expertise and resources of US private industries and federal agencies to develop, integrate, and deploy new technologies that meet critical needs for effective product realization. The RRM program addressed a needed change in the US Manufacturing infrastructure that will ensure US competitiveness in world market typified by mass customization. This project provided the effort needed to define, develop and establish a customizable infrastructure for rapid response product development design and manufacturing. A major project achievement was the development of a broad-based framework for automating and integrating the product and process design and manufacturing activities involved with machined parts. This was accomplished by coordinating and extending the application of feature-based product modeling, knowledge-based systems, integrated data management, and direct manufacturing technologies in a cooperative integrated computing environment. Key technological advancements include a product model that integrates product and process data in a consistent, minimally redundant manner, an advanced computer-aided engineering environment, knowledge-based software aids for design and process planning, and new production technologies to make products directly from design application software.

  10. Bacterial rapid identification with matrix assisted laser desorption/ionization time-of-flight mass spectrometry: development of an 'in-house method' and comparison with Bruker Sepsityper(®) kit.

    Science.gov (United States)

    Frédéric Ric, S; Antoine, M; Bodson, A; Lissoir, B

    2015-10-01

    The objective of this study was to compare an in-house matrix-assisted laser desorption ionization with time of flight (MALDI-TOF) method and a commercial MALDI-TOF kit (Sepsityper(®) kit) for direct bacterial identification in positive blood cultures. We also evaluated the time saved and the cost associated with the rapid identification techniques. We used the BACTEC(®) automated system for detecting positive blood cultures. Direct identification using Sepsityper kit and the in-house method were compared with conventional identification by MALDI-TOF using pure bacterial culture on the solid phase. We also evaluated different cut-off scores for rapid bacterial identification. In total, 127 positive blood vials were selected. The rate of rapid identification with the MALDI Sepsityper kit was 25.2% with the standard cut-off and 33.9% with the enlarged cut-off, while the results for the in-house method were 44.1 and 61.4%, respectively. Error rates with the enlarged cut-off were 6.98 (n = 3) and 2.56% (n = 2) for Sepsityper and the in-house method, respectively. Identification rates were higher for gram-negative bacteria. Direct bacterial identification succeeded in supplying rapid identification of the causative organism in cases of sepsis. The time taken to obtain a result was nearly 24  hours shorter for the direct bacterial identification methods than for conventional MALDI-TOF on solid phase culture. Compared with the Sepsityper kit, the in-house method offered better results and fewer errors, was more cost-effective and easier to use.

  11. Rapid detection of carbapenemase-producing Klebsiella pneumoniae strains derived from blood cultures by Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry (MALDI-TOF MS).

    Science.gov (United States)

    Sakarikou, Christina; Ciotti, Marco; Dolfa, Camilla; Angeletti, Silvia; Favalli, Cartesio

    2017-03-08

    Carbapenemase-producing Enterobacteriaceae (CPE), particularly carbapenemase-producing Klebsiella pneumoniae isolates, are important causative agents of nosocomial infections associated with significant mortality rates mostly in critical wards. The rapid detection and typing of these strains is critical either for surveillance purposes and to prevent outbreaks and optimize antibiotic therapy. In this study, the MALDI-TOF MS method was used to detect rapidly these isolates from blood cultures (BCs) and to obtain proteomic profiles enable to discriminate between carbapenemase-producing and non-carbapenemase-producing strains. Fifty-five K. pneumoniae strains were tested. Identification and carbapenemase-production detection assay using Ertapenem were performed both from bacterial pellets extracted directly from BCs flasks and from subcultures of these strains. For all isolates, a complete antimicrobial susceptibility testing and a genotypic characterization were performed. We found 100% agreement between the carbapenemase-producing profile generated by MALDI TOF MS and that obtained using conventional methods. The assay detected and discriminated different carbapenemase-producing K. pneumoniae isolates within 30 min to 3 h after incubation with Ertapenem. MALDI-TOF MS is a promising, rapid and economical method for the detection of carbapenemase-producing K. pneumoniae strains that could be successfully introduced into the routine diagnostic workflow of clinical microbiology laboratories.

  12. Rapid simultaneous determination of eperisone, tolperisone, and tizanidine in human serum by using a MonoSpin® C18 extraction column and liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Miura, Naoya; Saito, Takeshi; Taira, Takayuki; Yamagiwa, Takeshi; Morita, Sein; Inokuchi, Sadaki

    2014-01-01

    A method was developed for rapid toxicological analysis of eperisone, tolperisone, and tizanidine in human serum using a MonoSpin® C18 extraction column and LC/MS/MS. The method was validated for LOD, linearity, precision, and extraction recovery. This method was rapid with an LOD of 0.5 ng/mL, linearity range 1-500.0 ng/mL (r2 = 0.999), and RSD value below 14.6%. Extraction recovery from the sample was greater than 98.6, 98.8, and 88.5% for eperisone, tolperisone, and tizanidine, respectively. Results showed that combination of the MonoSpin C18 extraction column and LC/MS/MS is a simple and rapid method for the analysis of these three analytes, and a method is described for simultaneous quantitative determination of the analytes in human serum by LC/MSIMS. This method was used to determine the serum levels of eperisone in a patient with eperisone poisoning, and could be successfully applied for screening analyses in clinical cases other than poisoning.

  13. Rapidity Dependence of the Single Inclusive Jet Cross-Section in $p\\bar{p}$ Collisions at the Center-of-Mass Energy of 18-TeV with the D0 Detector

    Energy Technology Data Exchange (ETDEWEB)

    Babukhadia, Levan R. [Arizona U.

    1999-01-01

    We have made a precise measurement of the rapidity dependence of inclusive single jet production cross section $d^2\\sigma/(dE_T d\\eta)$ in $p\\overline{p}$ collisions at $\\sqrt{s}$ = 1.8 TeV. The measurement is based on integrated luminosity of 92 $pb^{-1}$ data collected by the D0 detector at the Tevatron Collider, Fermi National Accelerator Laboratory. The cross sections are reported as a function of jet transverse energy in five pseudorapidity $(\\eta)$ intervals up to $\\eta$ = 3:0. The experimental results are in good agreement with the theoretical predictions from next-to-leading order perturbative quantum chromodynamics.

  14. Investigation of the fission yields of the fast neutron-induced fission of {sup 233}U; Mesure de la distribution en masse et en charge des produits de la fission rapide de l'{sup 233}U

    Energy Technology Data Exchange (ETDEWEB)

    Galy, J

    1999-09-01

    As a stars, a survey of the different methods of investigations of the fission product yields and the experimental data status have been studied, showing advantages and shortcomings for the different approaches. An overview of the existing models for the fission product distributions has been as well intended. The main part of this thesis was the measurement of the independent yields of the fast neutron-induced fission of{sup 233}U, never investigated before this work. The experiment has been carried out using the mass separator OSIRIS (Isotope Separator On-Line). Its integrated ion-source and its specific properties required an analysis of the delay-parameter and ionisation efficiency for each chemical species. On the other hand, this technique allows measurement of independent yields and cumulative yields for elements from Cu to Ba, covering most of the fission yield distribution. Thus, we measured about 180 independent yields from Zn (Z=30) to Sr (Z=38) in the mass range A=74-99 and from Pd (Z=46) to Ba (Z=56) in the mass range A=113-147, including many isomeric states. An additional experiment using direct {gamma}-spectroscopy of aggregates of fission products was used to determine more than 50 cumulative yields of element with half-life from 15 min to a several days. All experimental data have been compared to estimates from a semi-empirical model, to calculated values and to evaluated values from the European library JEF 2.2. Furthermore, a study of both thermal and fast neutron-induced fission of {sup 233}U measured at Studsvik, the comparison of the OSIRIS and LOHENGRIN facilities and the trends in new data for the Reactors Physics have been discussed. (author)

  15. Development of a lipid profiling system using reverse-phase liquid chromatography coupled to high-resolution mass spectrometry with rapid polarity switching and an automated lipid identification software.

    Science.gov (United States)

    Yamada, Takayuki; Uchikata, Takato; Sakamoto, Shigeru; Yokoi, Yasuto; Fukusaki, Eiichiro; Bamba, Takeshi

    2013-05-31

    Lipidomics requires accurate lipid profiling, which until recently has been challenging at best. In the present study, we developed a practical workflow for high-throughput and exhaustive lipid profiling by combining reverse-phase liquid chromatography coupled to quadrupole orbitrap Fourier transform mass spectrometry, with an automated lipid identification software. This validated method enables highly sensitive and simultaneous analysis of lipids with varying polarities such as glycerophospholipids and sphingophospholipids, by switching the acquisition polarities in mass spectrometry. In addition, it facilitates data-dependent MS(2) analysis targeting the lipid molecular species without any influence from other ions by setting the inclusion list, the target m/z list for the product ion scanning. The m/z values of the target lipid molecular species, stored in the database of Lipid Search software, are added to the inclusion list. Moreover, optimizing the identification conditions of the software for the LC/MS system enables high-throughput and accurate identification of lipid molecular species existing in biological samples. Specifically, LC separation is essential for accurate identification of lipid molecular species that possess some fatty acid chains, because it can be difficult to determine fatty acid chain composition of detected molecular species especially in triacylglycerol compounds in direct infusion mass spectrometry. This method has high reproducibility and can be used for structural analysis even for low-abundance compounds. Using this method, over 400 lipid compounds targeted in this research were detected and identified from a sample of mouse plasma. This result indicates that the LC/MS method in the present study enables efficient lipid profiling. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Rapid Detection and Identification of Candidemia by Direct Blood Culturing on Solid Medium by Use of Lysis-Centrifugation Method Combined with Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry (MALDI-TOF MS).

    Science.gov (United States)

    Idelevich, Evgeny A; Grünastel, Barbara; Becker, Karsten

    2017-01-01

    Candida sepsis is a life-threatening condition with increasing prevalence. In this study, direct blood culturing on solid medium using a lysis-centrifugation procedure enabled successful Candida species identification by matrix-assisted laser desorption-ionization time of flight mass spectrometry on average 3.8 h (Sabouraud agar) or 7.4 h (chocolate agar) before the positivity signal for control samples in Bactec mycosis-IC/F or Bactec Plus aerobic/F bottles, respectively. Direct culturing on solid medium accelerated candidemia diagnostics compared to that with automated broth-based systems. Copyright © 2016 American Society for Microbiology.

  17. Spatial localisation of curcumin and rapid screening of the chemical compositions of turmeric rhizomes (Curcuma longa Linn.) using Direct Analysis in Real Time-Mass Spectrometry (DART-MS).

    Science.gov (United States)

    Rahman, A F M Motiur; Angawi, Rihab F; Kadi, Adnan A

    2015-04-15

    Curcumin is a potent antioxidant agent having versatile biological activities is present in turmeric rhizomes (Curcuma longa Linn.). Powder of turmeric rhizomes is consumes as curry spicy worldwide, especially in Asia. In this study, we demonstrate that, bioactive curcumin and its analog demethoxycurcumin are chiefly concentrated in the pith rather than the other parts of the turmeric rhizomes and it was discovered using modern atmospheric ionisation source 'Direct Analysis in Real Time' (DART) connected with an Ion Trap Mass Spectrometry. In addition, all the major components present in turmeric rhizomes were detected in positive and/or in negative ion mode using DART. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. The mass spectrometry technology MALDI-TOF (Matrix-Assisted Laser Desorption/Ionization Time- Of-Flight for a more rapid and economic workflow in the clinical microbiology laboratory

    Directory of Open Access Journals (Sweden)

    Simona Barnini

    2012-12-01

    Full Text Available Introduction: In order to improve the outcome of patients, reduce length of stay, costs and resources engaged in diagnostics, more rapid reports are requested to the clinical microbiologists.The purpose of this study is to assess the impact on workflow of MALDI-TOF technology, recently made available for use in routine diagnostics. Methods:The work list by the management information system is sent to the instrument MALDI-TOF, where are held at least three successive analytic sessions: the first includes bacteria isolated from CSF, blood cultures, and cases already reported as serious/urgent, the second includes all other germs isolated, the third, microorganisms that require extraction with trifluoroacetic acid (TFA or formic acid (FA for identification.The results of each session direct to the execution of different types of susceptibility testing. Results:The times of microbial identifications are reduced by 24 or 48 hours and made available to the clinician for the rational empirical therapy.The reagent costs are reduced by 40%.The subcultures were reduced by 80%, and microscopic examinations by 50%.The antibiotic susceptibility tests were immediately performed with the most appropriate method, based on the knowledge of local epidemiology and microbial species. Conclusion:The bacteriology is the less automated discipline among the clinical laboratory activities and results of diagnostic tests are poorly well-timed. The new interpretative algorithms of MALDI-TOF spectra, now available, allow the correct identification of bacteria in near real time, completely eliminating the wait is necessary for biochemical identification and guiding the operator in selecting the most appropriate antibiotic susceptibility tests. This technology makes work more rapid, economic and efficient, eliminating errors and, together with effective computerization of data, transforms the information content of the microbiological report, making it much more effective

  19. Ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride as a novel matrix for rapid quantitative and qualitative determination of serum free fatty acids by matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry.

    Science.gov (United States)

    Zhang, Yaping; Wang, Yanmin; Guo, Shuai; Guo, Yumei; Liu, Hui; Li, Zhili

    2013-09-10

    The blood free fatty acids (FFAs), which provide energy to the cell and act as substrates in the synthesis of fats, lipoproteins, liposaccharides, and eicosanoids, involve in a number of important physiological processes. In the present study, matrix-assisted laser desorption/ionization-Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR MS) with ammonia-treated N-(1-naphthyl) ethylenediamine dihydrochloride (ATNEDC) as a novel MALDI matrix in a negative ion mode was employed to directly quantify serum FFAs. Multiple point internal standard calibration curves between the concentration ratios of individual fatty acids to internal standard (IS, C17:0) versus their corresponding intensity ratios were constructed for C14:0, C16:1, C16:0, C18:0, C18:1, C18:2, C18:3, C20:4, and C22:6, respectively, in their mixture, with correlation coefficients between 0.991 and 0.999 and limits of detection (LODs) between 0.2 and 5.4μM, along with the linear dynamic range of more than two orders of magnitude. The results indicate that the multiple point internal standard calibration could reduce the impact of ion suppression and improve quantification accuracy in the MALDI mode. The quantitative results of nine FFAs from 339 serum samples, including 161 healthy controls, 118 patients with hyperglycemia and 60 patients without hyperglycemia show that FFAs levels in hyperglycemic patient sera are significantly higher than those in healthy controls and patients without hyperglycemia, and elevated FFA levels are also associated with increased levels of fasting blood glucose (FBG) in hyperglycemic patient sera. Serum FFAs were identified on the basis of the observed accurate molecular masses and reliable isotope distributions obtained by MALDI-FTICR MS. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. A high performance liquid chromatography fingerprinting and ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry chemical profiling approach to rapidly find characteristic chemical markers for quality evaluation of dispensing granules, a case study on Chuanxiong Rhizoma.

    Science.gov (United States)

    Zhang, Xiao-Lin; Liu, Li-Fang; Zhu, Ling-Ying; Bai, Ying-Jia; Mao, Qian; Li, Song-Lin; Chen, Shi-Lin; Xu, Hong-Xi

    2014-01-01

    A high performance liquid chromatography-photodiode array detector (HPLC-PDA) fingerprinting and ultra high performance liquid chromatography-photodiode array detector coupled with quadrupole time-of-flight mass spectrometry (UHPLC-PDA-QTOF-MS/MS) based chemical profiling approach was developed to rapidly find characteristic chemical markers for quality control of dispensing granules, taking Chuanxiong Rhizoma (CR) as a model herb. Firstly, CR crude drugs, their traditional decoctions and CR dispensing granules were analyzed by HPLC-PDA to rapidly establish the fingerprints and thereby generate the simulative median chromatograms of CR crude drugs, decoctions and dispensing granules, and by comparing the simulative median chromatograms, major characteristic peaks of CR decoctions and dispensing granules could be determined. Secondary, UHPLC-PDA-QTOF-MS/MS was used to identify the major characteristic peaks of CR decoctions and dispensing granules. The identities of three major peaks were elucidated and confirmed to be ferulic acid (1), senkyunolide I (2) and senkyunolide H (3) by comparing the mass/UV spectra and retention times with that of the reference compounds. Thirdly, an HPLC-PDA method was validated to quantify the three characteristic components in commercial CR dispensing granules. The average contents of ferulic acid and senkyunolide H were found to be less than 1.0mg/g, whereas that of senkyunolide I was 4.40mg/g in CR dispensing granules, which indicated that senkyunolide I might be chosen as a suitable quantitative marker, while ferulic acid and senkyunolide H as qualitative markers for the quality evaluation of CR dispensing granules. It is suggested that this newly established approach could be used to practically and rapidly find suitable marker compounds for quality control of dispensing granules derived from other medicinal herbs. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Nominal Mass?

    Science.gov (United States)

    Attygalle, Athula B.; Pavlov, Julius

    2017-08-01

    The current IUPAC-recommended definition of the term "nominal mass," based on the most abundant naturally occurring stable isotope of an element, is flawed. We propose that Nominal mass should be defined as the sum of integer masses of protons and neutrons in any chemical species. In this way, all isotopes and isotopologues can be assigned a definitive identifier.

  2. Validation of a rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) assay for the simultaneous determination of existing and new antiretroviral compounds.

    Science.gov (United States)

    Else, Laura; Watson, Victoria; Tjia, John; Hughes, Andrew; Siccardi, Marco; Khoo, Saye; Back, David

    2010-06-01

    Clinical pharmacokinetic studies of antiretrovirals require accurate and precise measurement of plasma drug concentrations. Here we describe a simple, fast and sensitive HPLC-MS/MS method for determination of the commonly used protease inhibitors (PI) amprenavir, atazanavir, darunavir, lopinavir, ritonavir, saquinavir and the non-nucleoside reverse transcriptase inhibitor (NNRTI) nevirapine, as well as the more recent antiretrovirals, the CCR5 antagonist maraviroc and the "second generation" NNRTI etravirine and rilpivirine. An internal standard (quinoxalone; QX) was added to plasma aliquots (100 microl) prior to protein precipitation with acetonitrile (500 microl) followed by centrifugation and addition of 0.05% formic acid (200 microl) to the supernatant. Chromatographic separation was achieved using a gradient (acetonitrile and 0.05% formic acid) mobile phase on a reverse-phase C18 column. Detection was via selective reaction monitoring (SRM) operating in positive ionization mode on a triple-quadrupole mass spectrometer. All compounds eluted within a 5 min run time. Calibration curves were validated over concentration ranges reflecting therapeutic concentrations observed in HIV-infected patients from pharmacokinetic data reported in the literature. Correlation coefficients (r2) exceeded 0.998. Inter- and intra-assay variation ranged between 1% and 10% and % recovery exceeded 90% for all analytes. The method described is being successfully applied to measure plasma antiretroviral concentrations from samples obtained from clinical pharmacokinetic studies. Copyright 2010 Elsevier B.V. All rights reserved.

  3. Rapid determination of capsaicinoids by colorimetric method

    OpenAIRE

    Ryu, Wang-Kyun; Kim, Hee-Woong; Kim, Geun-Dong; Rhee, Hae-Ik

    2016-01-01

    Capsaicinoids, the pungent component of chili peppers, are generally analyzed by precise analytical techniques, such as gas chromatography and high-performance liquid chromatography (HPLC), but these are not practical for the mass analyses of samples. To analyze mass samples rapidly, a colorimetric method was suggested. In this work, pigments and capsaicinoids were efficiently separated from chili pepper extract by sequential solid–liquid extraction and liquid–liquid extraction in test tubes ...

  4. Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry.

    Science.gov (United States)

    Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca

    2016-01-08

    This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1. Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSDmilk and dairy products studied. The proposed method improves the performance of AFM1 analysis in milk samples as AFM1 determination is performed with a degree of accuracy higher than the conventional methods. Other advantages are the reduction of sample preparation procedure, time and cost of the analysis, enabling high sample throughput that meet the current concerns of food safety and the public health protection. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Rapid discrimination of Haemophilus influenzae, H. parainfluenzae, and H. haemolyticus by fluorescence in situ hybridization (FISH) and two matrix-assisted laser-desorption-ionization time-of-flight mass spectrometry (MALDI-TOF-MS) platforms.

    Science.gov (United States)

    Frickmann, Hagen; Christner, Martin; Donat, Martina; Berger, Anja; Essig, Andreas; Podbielski, Andreas; Hagen, Ralf Matthias; Poppert, Sven

    2013-01-01

    Due to considerable differences in pathogenicity, Haemophilus influenzae, H. parainfluenzae and H. haemolyticus have to be reliably discriminated in routine diagnostics. Retrospective analyses suggest frequent misidentifications of commensal H. haemolyticus as H. influenzae. In a multi-center approach, we assessed the suitability of fluorescence in situ hybridization (FISH) and matrix-assisted laser-desorption-ionization time-of-flight mass-spectrometry (MALDI-TOF-MS) for the identification of H. influenzae, H. parainfluenzae and H. haemolyticus to species level. A strain collection of 84 Haemophilus spp. comprising 50 H. influenzae, 25 H. parainfluenzae, 7 H. haemolyticus, and 2 H. parahaemolyticus including 77 clinical isolates was analyzed by FISH with newly designed DNA probes, and two different MALDI-TOF-MS systems (Bruker, Shimadzu) with and without prior formic acid extraction. Among the 84 Haemophilus strains analyzed, FISH led to 71 correct results (85%), 13 uninterpretable results (15%), and no misidentifications. Shimadzu MALDI-TOF-MS resulted in 59 correct identifications (70%), 19 uninterpretable results (23%), and 6 misidentifications (7%), using colony material applied directly. Bruker MALDI-TOF-MS with prior formic acid extraction led to 74 correct results (88%), 4 uninterpretable results (5%) and 6 misidentifications (7%). The Bruker MALDI-TOF-MS misidentifications could be resolved by the addition of a suitable H. haemolyticus reference spectrum to the system's database. In conclusion, no analyzed diagnostic procedure was free of errors. Diagnostic results have to be interpreted carefully and alternative tests should be applied in case of ambiguous test results on isolates from seriously ill patients.

  6. Rapid headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric method for qualitative profiling of ice wine volatile fraction. II: Classification of Canadian and Czech ice wines using statistical evaluation of the data.

    Science.gov (United States)

    Setkova, Lucie; Risticevic, Sanja; Pawliszyn, Janusz

    2007-04-20

    The previously developed and optimized headspace solid-phase microextraction (HS-SPME)-GC-time-of-flight (TOF) MS analytical method for the determination of compounds with a wide range of polarities and volatilities was successfully used in this study to characterize and classify a large set of ice wines according to their origin, grape variety and oak or stainless steel fermentation/ageing conditions, based on a statistical evaluation (principal component analysis (PCA)) of the measured data. More than 130 ice wine samples collected directly from Canadian and Czech wine producers were analyzed in this study. The SPME step was beneficially carried out utilizing the new-generation super elastic divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50 microm/30 microm fiber assembly. One fiber was used for the whole sequence of ice wine samples, control and blank experiments, which consisted of more than 600 individual extraction/injection cycles. Utilizing the high-speed TOF analyzer, full spectral information within the range of 35-450 u was collected for the entire GC run (as short as 4.5 min) without compromising in the detection sensitivity, as compared to other scanning mass analyzers operated in selected ion monitoring or MS(n) mode to achieve similar sensitivity. The identification of analytes was performed by a combination of the linear temperature-programmed retention index (LTPRI) approach with the comparison of the obtained spectra with three libraries included in the ChromaTOF software. A total of 201 peaks were tentatively assigned as ice wine aroma components and 58 of those compounds were evaluated in all of the examined samples.

  7. Rapid and effective sample cleanup based on graphene oxide-encapsulated core–shell magnetic microspheres for determination of fifteen trace environmental phenols in seafood by liquid chromatography–tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Sheng-Dong; Chen, Xiao-Hong [Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang 315010 (China); Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010 (China); Shen, Hao-Yu [Ningbo Institute of Technology, Zhejiang University, Ningbo, Zhejiang 315100 (China); Li, Xiao-Ping [Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang 315010 (China); Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010 (China); Cai, Mei-Qiang [School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310018 (China); Zhao, Yong-Gang [Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang 315010 (China); Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010 (China); Jin, Mi-Cong, E-mail: jmcjc@163.com [Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang 315010 (China); Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010 (China)

    2016-05-05

    In this study, graphene oxide-encapsulated core–shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach between positive charged poly(diallyldimethylammonium) chloride (PDDA)-modified Fe{sub 3}O{sub 4}@SiO{sub 2} and negative charged GO sheets via electrostatic interaction. The as-prepared GOE-CS-MM was carefully characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer analysis (VSM), and X-ray photoelectron spectroscopy (XPS), and was used as a cleanup adsorbent in magnetic solid-phase extraction (MSPE) for determination of 15 trace-level environmental phenols in seafood coupled to liquid chromatography–tandem mass spectrometry (LC–MS/MS). The obtained results showed that the GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect. The cleanup mechanisms were investigated and referred to π–π stacking interaction and hydrogen bond between GOE-CS-MM and impurities in the extracts. Moreover, the extraction and cleanup conditions of GOE-CS-MM toward phenols were optimized in detail. Under the optimized conditions, the limits of detection (LODs) were found to be 0.003–0.06 μg kg{sup −1}, and satisfactory recovery values of 84.8–103.1% were obtained for the tested seafood samples. It was confirmed that the developed method is simple, fast, sensitive, and accurate for the determination of 15 trace environmental phenols in seafood samples. - Highlights: • Novel graphene oxide-encapsulated core-shell magnetic microspheres (GOE-CS-MM) were fabricated by a self-assemble approach. • The as-prepared material GOE-CS-MM exhibited excellent cleanup efficiency and could availably reduce the matrix effect. • The cleanup mechanisms refer to π–π stacking interaction and hydrogen bond. • The developed MSPE–LC–MS/MS method was simple, fast, sensitive and accurate.

  8. Nutritional interventions to preserve skeletal muscle mass

    NARCIS (Netherlands)

    Backx, Evelien M.P.

    2016-01-01

    Muscle mass is the main predictor for muscle strength and physical function. The amount of muscle mass can decline rapidly during periods of reduced physical activity or during periods of energy intake restriction. For athletes, it is important to maintain muscle mass, since the loss of muscle is

  9. Rapid Prototyping Laboratory

    Data.gov (United States)

    Federal Laboratory Consortium — The ARDEC Rapid Prototyping (RP) Laboratory was established in December 1992 to provide low cost RP capabilities to the ARDEC engineering community. The Stratasys,...

  10. Neutrino masses

    CERN Document Server

    Gelmini, Graciela B; Gelmini, Graciela; Roulet, Esteban

    1995-01-01

    This is a review for Reports of Progress in Physics. After an introduction we start by explaining the different neutrino masses corresponding to different types of neutrinos, Dirac or Majorana, in section 2. In section 3 we discuss the main elementary particle models for neutrino masses and their distinctive phenomenological consequences. In section 4 we describe the status of direct mass searches and Majorana mass searches in neutrinoless double beta decays. In section 5 we go over the many cosmological implications of, and constraints on, neutrino properties, mainly masses and lifetimes. Sections 6, 7 and 8 review neutrino oscillations, the solar neutrino problem and the atmospheric neutrino problem, their implications and the current and future experiments. In particular, we explain oscillations in vacuum in section 6 and oscillations in matter in section 7. Section 9 summarizes the main bounds imposed by stars, mainly SN1987A. A few concluding remarks follow.

  11. Mass Society

    DEFF Research Database (Denmark)

    Borch, Christian

    2017-01-01

    the negative features usually ascribed by late nineteenth-century crowd psychology to spontaneous crowds, and attributes these to the entire social fabric. However, in contrast to crowd psychology, theorists of mass society often place greater emphasis on how capitalism, technological advances, or demographic......Mass society is a societal diagnosis that emphasizes – usually in a pejorative, modernity critical manner – a series of traits allegedly associated with modern society, such as the leveling of individuality, moral decay, alienation, and isolation. As such, the notion of mass society generalizes...... developments condition such negative features, and some theorists argue that mass society produces a propensity to totalitarianism. Discussions of mass society culminated in the early and mid-twentieth century....

  12. Implementation of rapid diagnostics with antimicrobial stewardship.

    Science.gov (United States)

    Minejima, Emi; Wong-Beringer, Annie

    2016-11-01

    Antimicrobial stewardship (ASP) is an intervention-based program to improve patient outcomes to infection while limiting spread of resistance and unintended consequences. Many rapid diagnostic tools are now FDA cleared for clinical use, with three evaluated across multiple settings: Matrix Assisted Laser Desorption Ionization Time-of-Flight Mass Spectrometry, Verigene, and FilmArray. Areas covered: This review will focus on studies published that evaluated ASP intervention with rapid diagnostic implementation on outcomes of infection. A description of the key ASP personnel, rapid diagnostic notification methods, hours of notification, and scope of ASP intervention is summarized. Expert commentary: It is critical that ASPs continually re-evaluate and evolve with technological advances. Rapid diagnostic tools are powerful in their ability to identify organisms quickly. A trained clinician is needed to evaluate the results and interact with the providers to educate them on result interpretation and optimal antimicrobial selection to maximize treatment success.

  13. Rapid Airplane Parametric Input Design (RAPID)

    Science.gov (United States)

    Smith, Robert E.

    1995-01-01

    RAPID is a methodology and software system to define a class of airplane configurations and directly evaluate surface grids, volume grids, and grid sensitivity on and about the configurations. A distinguishing characteristic which separates RAPID from other airplane surface modellers is that the output grids and grid sensitivity are directly applicable in CFD analysis. A small set of design parameters and grid control parameters govern the process which is incorporated into interactive software for 'real time' visual analysis and into batch software for the application of optimization technology. The computed surface grids and volume grids are suitable for a wide range of Computational Fluid Dynamics (CFD) simulation. The general airplane configuration has wing, fuselage, horizontal tail, and vertical tail components. The double-delta wing and tail components are manifested by solving a fourth order partial differential equation (PDE) subject to Dirichlet and Neumann boundary conditions. The design parameters are incorporated into the boundary conditions and therefore govern the shapes of the surfaces. The PDE solution yields a smooth transition between boundaries. Surface grids suitable for CFD calculation are created by establishing an H-type topology about the configuration and incorporating grid spacing functions in the PDE equation for the lifting components and the fuselage definition equations. User specified grid parameters govern the location and degree of grid concentration. A two-block volume grid about a configuration is calculated using the Control Point Form (CPF) technique. The interactive software, which runs on Silicon Graphics IRIS workstations, allows design parameters to be continuously varied and the resulting surface grid to be observed in real time. The batch software computes both the surface and volume grids and also computes the sensitivity of the output grid with respect to the input design parameters by applying the precompiler tool

  14. Risk Informed Design Using Integrated Vehicle Rapid Assessment Tools Project

    Data.gov (United States)

    National Aeronautics and Space Administration — A successful proof of concept was performed in FY 2012 integrating the Envision tool for parametric estimates of vehicle mass and the Rapid Response Risk Assessment...

  15. Masses of noble gases

    CERN Multimedia

    Marx, G H; Herfurth, F; Stora, T; Blaum, K; Beck, D; Audi, G; Rosenbusch, M

    The so-called magic numbers, cornerstones of the quantum nuclear ensemble, are now known to lose their supernatural powers