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Sample records for bead-injection lab-on-valve hyphenated

  1. Hyphenating multisyringe flow injection lab-on-valve analysis with atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of trace levels of hydride-forming elements in environmental samples

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    of the functional moieties, so that maximum benefit can be taken from the application of the bead renewal strategy. The proposed procedure is characterized by a high tolerance to metal species and interfering hydride forming elements. In fact, ratios of Se(IV) to As ≤ 5000 and Sb(V) to As ≤ 500 are tolerated...... for the bead-injection mode whenever the loading sample volume was affixed at 3.0 mL. The reliability and accuracy of the automated procedure was ascertained by determining total inorganic arsenic in both spiked environmental waters and certified reference materials of variable matrix complexity (TMDA-54...

  2. 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

    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......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...

  3. Automated on-line renewable solid-phase extraction-liquid chromatography exploiting multisyringe flow injection-bead injection lab-on-valve analysis.

    Science.gov (United States)

    Quintana, José Benito; Miró, Manuel; Estela, José Manuel; Cerdà, Víctor

    2006-04-15

    In this paper, the third generation of flow injection analysis, also named the lab-on-valve (LOV) approach, is proposed for the first time as a front end to high-performance liquid chromatography (HPLC) for on-line solid-phase extraction (SPE) sample processing by exploiting the bead injection (BI) concept. The proposed microanalytical system based on discontinuous programmable flow features automated packing (and withdrawal after single use) of a small amount of sorbent (residues (viz., ketoprofen, naproxen, bezafibrate, diclofenac, and ibuprofen) and one metabolite (viz., salicylic acid) in surface water, urban wastewater, and urine. To this end, the copolymeric divinylbenzene-co-n-vinylpyrrolidone beads (Oasis HLB) were utilized as renewable sorptive entities in the micromachined unit. The automated analytical method features relative recovery percentages of >88%, limits of detection within the range 0.02-0.67 ng mL(-1), and coefficients of variation <11% for the column renewable mode and gives rise to a drastic reduction in operation costs ( approximately 25-fold) as compared to on-line column switching systems.

  4. A Universal Approach for Selective Trace Metal Determinations via Sequential Injection-Bead Injection-Lab-on-Valve (SI-BI-LOV) Using Renewable Reagent-loaded Hydrophobic Beads

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    -Lab-on-Valve (SI-LOV) mode. The methodology uses poly(styrene-divinylbenzene) beads containing pendant octadecyl moieties (C18-PS/DVB), which are pre-impregnated with a selective organic metal chelating agent prior to the automatic manipulation of the beads in the microbore conduits of the LOV unit. By adapting......A new sample pretreatment approach is presented for selective and sensitive determination of trace metals via electrothermal atomic absorption spectrometry (ETAAS) based on the principle of bead injection (BI) with renewable reagent-loaded hydrophobic beads in a Sequential Injection...... in selecting the most favourable elution mode in order to attain the highest sensitivity. Cr(VI) is used as model analyte to demonstrate the potential of the SI-BI-LOV scheme, in which 1,5-diphenylcarbazide (DPC) is pre-impregnated on the beads, the surface of which serves as the active microzone. It is shown...

  5. An automatic micro-sequential injection bead injection lab-on-valve (muSI-BI-LOV) assembly for speciation analysis of ultra trace levels of Cr(III) and Cr(VI) incorporating on-line chemical reduction and employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    A novel, miniaturized micro-sequential injection Lab-on-Valve (muSI-LOV) system hyphenated with electrothermal atomic absorption spectrometry (ETAAS) is proposed for the automatic preconcentration and speciation analysis of Cr(III) and Cr(VI) utilizing solid-phase extraction on hydrophilic...

  6. Multisyringe flow injection lab-on-valve systems coupled to hydride generation atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of total inorganic arsenic in environmental waters

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    stream network is assembled for accurate handling of solutions and on-line post column derivatization of the eluate for the generation of the volatile species. The potential of the new hyphenated technique for environmental assays was ascertained via the determination of ultratrace levels of total...... and 10% KI. The eluate merges downstream with a defined plug of sodium tetrahydroborate (0.3% w/v) for generation of arsine, which is subsequently quantified by AFS. An oxidation agent, namely 2x10-6 M potassium permanganate, was employed for the quantitative oxidation of As(III) to As(V) in the samples...

  7. Exploiting the bead-injection approach in the integrated sequential injection Lab-on-Valve format using hydrophobic packing materials for on-line matrix removal and preconcentration of trace levels of cadmium in environmental and biological samples via formation of non-charged chelates prior

    DEFF Research Database (Denmark)

    Miró, Manuel; Jonczyk, Sylwia; Wang, Jianhua

    2003-01-01

    The concept of renewable microcolumns within the conduits of an automated single injection lab-on-valve system was exploited in a sorption/elution fashion using sorbents of hydrophobic nature. The scheme's practical applicability was demonstrated for the electrothermal atomic absorption spectrome...... spectrometry determination of trace level concentrations of cadmium in complex matrices. Statistical comparisons between the proposed procedure and certified values revealed no significant differences at the 95% confidence level....

  8. On-line dynamic extraction and automated determination of readily bioavailable hexavalent chromium in solid substrates using micro-sequential injection bead-injection lab-on-valve hyphenated with electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    ). The effect of simulated acidic rain on the accessibility of chromate forms for plant uptake was also investigated. The proposed approach offers several advantages over conventional speciation/fractionation protocols in the batch mode, including immediate separation with concomitant preconcentration...

  9. On-line dynamic extraction and automated determination of readily bioavailable hexavalent chromium in solid substrates using micro-sequential injection bead-injection lab-on-valve hyphenated with electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    leached from the matrix constituents onto a Q Sepharose strong anion-exchanger freshly packed into the microconduits of the μSI-assembly; air-segmented elution of the sorbed species by a 40 μL plug of 0.5 mol L-1 NH4NO3 (pH 8) eluent; and detection by electrothermal atomic absorption spectrometry (ETAAS...

  10. Fully automated lab-on-valve-multisyringe flow injection analysis-ICP-MS system: An effective tool for fast, sensitive and selective determination of thorium and uranium at environmental levels exploiting solid phase extraction

    OpenAIRE

    Avivar, Jessica; Ferrer, Laura; Casas, Montserrat; Cerdà, Víctor

    2012-01-01

    An on-line solid-phase extraction method linked to inductively coupled mass spectrometry (ICP-MS) has been developed for the determination of low levels of uranium and thorium in environmental samples. The hyphenation of lab-on-valve (LOV) and multisyringe flow injection analysis (MSFIA), coupled to an ICP-MS, allows the simultaneous determination of thorium and uranium in different types of environmental sample matrices achieving high selectivity and sensitivity levels. On-line separation an...

  11. Bead injection ELISA for the determination of antibodies implicated in type 1 diabetes mellitus.

    Science.gov (United States)

    Carroll, Andrea D; Scampavia, Louis; Luo, Dong; Lernmark, Ake; Ruzicka, Jaromir

    2003-09-01

    This work introduces a novel analytical method for the detection and study of GAD65 autoantibodies, which have been implicated in the onset of type 1 diabetes. There is a clinical need for a rapid and automated assay for GAD65 autoantibodies. Therefore, this method was designed to exploit the advantages of bead injection (BI) analysis for enzyme-linked immunosorbent assays (ELISA). BI ELISA is a microscale technique that uses enzyme labeled secondary antibodies to detect the capture of target antibodies on immobilized antigen in the flow cell of the lab-on-valve (LOV) manifold. A detection limit of 20 ng mL(-1) of GAD65 monoclonal antibody 144 compares favorably with the sensitivity and precision of a standard ELISA currently employed to detect GAD65 autoantibodies. Compared to the standard ELISA protocol, BI ELISA offers a significantly reduced assay time and complete automation of solution handling and detection.

  12. Lab on valve-multisyringe flow injection system (LOV-MSFIA) for fully automated uranium determination in environmental samples.

    Science.gov (United States)

    Avivar, Jessica; Ferrer, Laura; Casas, Montserrat; Cerdà, Víctor

    2011-06-15

    The hyphenation of lab-on-valve (LOV) and multisyringe flow analysis (MSFIA), coupled to a long path length liquid waveguide capillary cell (LWCC), allows the spectrophotometric determination of uranium in different types of environmental sample matrices, without any manual pre-treatment, and achieving high selectivity and sensitivity levels. On-line separation and preconcentration of uranium is carried out by means of UTEVA resin. The potential of the LOV-MSFIA makes possible the fully automation of the system by the in-line regeneration of the column. After elution, uranium(VI) is spectrophotometrically detected after reaction with arsenazo-III. The determination of levels of uranium present in environmental samples is required in order to establish an environmental control. Thus, we propose a rapid, cheap and fully automated method to determine uranium(VI) in environmental samples. The limit of detection reached is 1.9 ηg of uranium and depending on the preconcentrated volume; it results in ppt levels (10.3 ηg L(-1)). Different water sample matrices (seawater, well water, freshwater, tap water and mineral water) and a phosphogypsum sample (with natural uranium content) were satisfactorily analyzed. Copyright © 2010 Elsevier B.V. All rights reserved.

  13. Universal approach for selective trace metal determinations via sequential injection-bead injection-lab-on-valve using renewable hydrophobic bead surfaces as reagent carriers

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    that the bead material exhibits excellent chemical stability at low pH values. On-line pH sample adjustment prevents alteration of the original distribution of chromium species while assuring fast rates for the DPC-Cr(VI) reaction. The proposed procedure was successfully applied to the determination of trace...... levels of Cr(VI) in natural waters containing high levels of dissolved salts (such as seawater and hard tap water) without requiring any dilution step. Method validation was performed by determination of total chromium in an NIST standard reference material (NIST 1640, natural water) after Cr...... favourable elution mode in order to attain the highest sensitivity. The potential of the SI-BI-LOV scheme is demonstrated by taking Cr(VI) as a model analyte, using a 1,5-diphenylcarbazide (DPC)-loaded bead column as the active microzone. As this reaction requires the use of high acidity, it is also shown...

  14. Sequential injection lab-on-valve: the third generation of flow injection analysis

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2003-01-01

    Termed the third generation of flow injection analysis, sequential injection (SI)-lab-on-valve (LOV) has specific advantages and allows novel, unique applications - not least as a versatile front end to a variety of detection techniques. This review presents snd discusses progress to date of the ...

  15. Towards an automatic lab-on-valve-ion mobility spectrometric system for detection of cocaine abuse.

    Science.gov (United States)

    Cocovi-Solberg, David J; Esteve-Turrillas, Francesc A; Armenta, Sergio; de la Guardia, Miguel; Miró, Manuel

    2017-08-25

    A lab-on-valve miniaturized system integrating on-line disposable micro-solid phase extraction has been interfaced with ion mobility spectrometry for the accurate and sensitive determination of cocaine and ecgonine methyl ester in oral fluids. The method is based on the automatic loading of 500μL of oral fluid along with the retention of target analytes and matrix clean-up by mixed-mode cationic/reversed-phase solid phase beads, followed by elution with 100μL of 2-propanol containing (3% v/v) ammonia, which are online injected into the IMS. The sorptive particles are automatically discarded after every individual assay inasmuch as the sorptive capacity of the sorbent material is proven to be dramatically deteriorated with reuse. The method provided a limit of detection of 0.3 and 0.14μgL -1 for cocaine and ecgonine methyl ester, respectively, with relative standard deviation values from 8 till 14% with a total analysis time per sample of 7.5min. Method trueness was evaluated by analyzing oral fluid samples spiked with cocaine at different concentration levels (1, 5 and 25μgL -1 ) affording relative recoveries within the range of 85±24%. Fifteen saliva samples were collected from volunteers and analysed following the proposed automatic procedure, showing a 40% cocaine occurrence with concentrations ranging from 1.3 to 97μgL -1 . Field saliva samples were also analysed by reference methods based on lateral flow immunoassay and gas chromatography-mass spectrometry. The application of this procedure to the control of oral fluids of cocaine consumers represents a step forward towards the development of a point-of-care cocaine abuse sensing system. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Sequential injection/bead injection lab-on-valve schemes for on-line solid phase extraction and preconcentration of ultra-trace levels of heavy metals with determination by ETAAS and ICPMS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Miró, Manuel

    2003-01-01

    -to-handle hydrophilic renewable reactors hold the features of improved R.S.D.s and LODs as compared to those operated in the conventional, permanent mode, in addition to the elimination of flow resistance. The hydrophobic columns fall into two categories, that is, the renewable one packed with C18-PS/DVB beads entails...

  17. Determination of Low Level Concentrations of Metals by Means of Sequential Injection (SI) and Lab-on-Valve (LOV) Methodologies

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel; Petersen, Roongrat

    In recent years sequential injection (SI) analysis and Lab-on-Valve (LOV) approaches have proven themselves as powerful and versatile front ends to implement suitable pre-treatment procedures (separation and pre-concentration) for the assay of low concentrations of metals, as amply reflected...... in the substantial number of papers that have emerged in the scientific literature. These novel generations of flow injection analysis have demonstrated themselves as attractive substitutes for labour-intensive, manual sample pre-treatment and solution handling methods prior to analyte detection by atomic absorption....../emission spectrometry (FAAS, ETAAS, ICP-AES, ICP-MS). The lecture will initially give an overview of various automated alternatives for facilitating appropriate SI/LOV-separation and pre-concentration schemes of metals in liquid samples, including examples of solid-phase extraction with permanent columns or renewable...

  18. Determination of Low Level Concentrations of Metals by Means of Sequential Injection (SI) and Lab-on-Valve (LOV) Methodologies

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    In recent years sequential injection (SI) analysis and Lab-on-Valve (LOV) approaches have proven themselves as powerful and versatile front ends to implement suitable pre-treatment procedures (separation and pre-concentration) for the assay of low concentrations of metals, as amply reflected...... in the increasing number of papers appearing in the scientific literature. These novel generations of flow injection analysis have demonstrated themselves as attractive substitutes for labour-intensive, manual sample pre-treatment and solution handling methods prior to analyte detection by atomic absorption....../emission spectrometric devices such as FAAS, ETAAS, AFS, ICP-AES, and ICP-MS. While earlier separation and pre-concentration schemes of metals in liquid samples primarily have been centred on the use solvent extraction, or precipitate/(co)-precipitate collection in incorporated knotted reactors, or permanent columns...

  19. Recent developments in automated determinations of trace level concentrations of elements and on-line fractionations schemes exploiting the micro-sequential injection - lab-on-valve approach

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel; Long, Xiangbao

    2006-01-01

    . In this context sequential injection (SI) and lab-on-valve (LOV) schemes have proven themselves as superb vehicles to act as front-end microanalytical methodologies, particularly when employing solid-phase extraction (SPE) procedures. In this communication, selected SPE-procedures in a bead-renewable fashion...... are presented as based on the exploitation of micro-sequential injection (μSI-LOV) using hydrophobic as well as hydrophilic bead materials. The examples given comprise the presentation of a universal approach for SPE-assays, front-end speciation of Cr(III) and Cr(VI) in a fully automated and enclosed set...

  20. Exploiting the Lab-on-Valve Concept for Determination of Trace Levels of Metals in Complex Matrices with Detection by ETAAS and ICPMS

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    Termed the third generation of flow injection analysis, the Sequential Injection (SI)-Lab-on-Valve (LOV) concept has proven to entail specific advantages and to allow novel and unique applications. Both in term of its use in the automation and micro-miniaturization of suitable on-line sample...... approach [1,2]. Coupled to detection by ETAAS and ICPMS, and illustrated by recent exploits in the authors’ laboratory, it is shown that this methodology eliminates the problems encountered in conventional on-line column preconcentration systems and at the same time improves the overall operational...

  1. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  2. Online Coupling of Lab-on-Valve Format to Amperometry Based on Polyvinylpyrrolidone-Doped Carbon Paste Electrode and Its Application to the Analysis of Morin

    Directory of Open Access Journals (Sweden)

    Yang Wang

    2012-01-01

    Full Text Available The potential capabilities and analytical performance of lab-on-valve (LOV manifold as a front end to amperometry have been explored for the on-line determination of morin. Meanwhile, the electrochemical behaviors of morin were investigated based on polyvinylpyrrolidone- (PVP- doped carbon paste electrode (CPE, which found that PVP can significantly improve its oxidation peak current. The excellent amperometric current response was achieved when the potential difference (ΔE of 0.6 V was implemented in pH 6.5 phosphate buffer solution (PBS that served as the supporting electrolyte. A well-defined oxidation peak has been obtained in studies using PVP as a modifier of CPE based on the oxidation of morin. The present work introduces the LOV technique as a useful tool for amperometric measurement, documents advantages of using programmable flow, and outlines means for miniaturization of assays on the basis of PVP modified CPE. The proposed method was applied successfully to the determination of morin in real samples, and the spiked recoveries were satisfactory.

  3. Determination of trace zinc in seawater by coupling solid phase extraction and fluorescence detection in the Lab-On-Valve format.

    Science.gov (United States)

    Grand, Maxime M; Chocholouš, Petr; Růžička, Jarda; Solich, Petr; Measures, Christopher I

    2016-06-07

    By virtue of their compactness, long-term stability, minimal reagent consumption and robustness, miniaturized sequential injection instruments are well suited for automation of assays onboard research ships. However, in order to reach the sensitivity and limit of detection required for open-ocean determinations of trace elements, it is necessary to preconcentrate the analyte prior its derivatization and subsequent detection by fluorescence. In this work, a novel method for the determination of dissolved zinc (Zn) at subnanomolar levels in seawater is described. The proposed method combines, for the first time, automated matrix removal, extraction of the target element, and fluorescence detection within a miniaturized flow manifold, based on the Lab-On-Valve (LOV) concept. The key feature of the microfluidic manipulation of the sample is flow programming, designed to pass sample through a mini-column where the target analyte and other complexable cations are retained, while the seawater matrix is washed out. Next, zinc is eluted and merged with a Zn selective fluorescent probe (FluoZin-3) at the confluence point of the LOV central channel using two high-precision stepper motor driven pumps that are operated in concert. Finally, the thus formed Zn complex is transported to the LOV flow cell for selective fluorescence measurement. This work describes the characterization and optimization of the method including Solid Phase Extraction using the Toyopearl AF-Chelate-650M resin, and detailed assay protocol controlled by a commercially available software and instrument. The proposed method features a LOD of 0.02 nM, high precision (seawater reference standards and comparison with ICP-MS determinations on seawater samples collected in the upper 1300 m of the subtropical south Indian Ocean. This work confirms that integration of sample pretreatment with optical detection in the LOV format offers a widely applicable approach to trace analysis of seawater. Copyright © 2016

  4. A LabVIEW®-based software for the control of the AUTORAD platform. A fully automated multisequential flow injection analysis Lab-on-Valve (MSFIA-LOV) system for radiochemical analysis

    International Nuclear Information System (INIS)

    Barbesi, Donato; Vilas, Victor Vicente; Millet, Sylvain; Sandow, Miguel; Colle, Jean-Yves; Heras, Laura Aldave de las

    2017-01-01

    A LabVIEW®-based software for the control of the fully automated multi-sequential flow injection analysis Lab-on-Valve (MSFIA-LOV) platform AutoRAD performing radiochemical analysis is described. The analytical platform interfaces an Arduino®-based device triggering multiple detectors providing a flexible and fit for purpose choice of detection systems. The different analytical devices are interfaced to the PC running LabVIEW®VI software using USB and RS232 interfaces, both for sending commands and receiving confirmation or error responses. The AUTORAD platform has been successfully applied for the chemical separation and determination of Sr, an important fission product pertinent to nuclear waste. (author)

  5. A LabVIEW®-based software for the control of the AUTORAD platform: a fully automated multisequential flow injection analysis Lab-on-Valve (MSFIA-LOV) system for radiochemical analysis.

    Science.gov (United States)

    Barbesi, Donato; Vicente Vilas, Víctor; Millet, Sylvain; Sandow, Miguel; Colle, Jean-Yves; Aldave de Las Heras, Laura

    2017-01-01

    A LabVIEW ® -based software for the control of the fully automated multi-sequential flow injection analysis Lab-on-Valve (MSFIA-LOV) platform AutoRAD performing radiochemical analysis is described. The analytical platform interfaces an Arduino ® -based device triggering multiple detectors providing a flexible and fit for purpose choice of detection systems. The different analytical devices are interfaced to the PC running LabVIEW ® VI software using USB and RS232 interfaces, both for sending commands and receiving confirmation or error responses. The AUTORAD platform has been successfully applied for the chemical separation and determination of Sr, an important fission product pertinent to nuclear waste.

  6. Evaluation of a novel PTFE material for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems interfaced with detection by ETAAS

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr

    The operational characteristics of a novel PTFE bead material, granular Algoflon®, used for separation and preconcentration of metal ions via adsorption of on-line generated non-charged metal complexes, were evaluated in a sequential injection (SI) system furnished with an external packed column...... and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used material, Aldrich PTFE, which had...... demonstrated that PTFE was the most promising for solid-state pretreatments. By comparing the two materials, the Algoflon® beads exhibited much higher sensitivity (1.6107 versus 0.2956 μg l-1 per integrated absorbance (s)), and better retention efficiency (82% versus 74%) and enrichment factor (20.8 versus 17...

  7. Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald

    2004-01-01

    with an external packed column and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used...

  8. Hyphenated history: Osgood-Schlatter disease.

    Science.gov (United States)

    Nowinski, R J; Mehlman, C T

    1998-08-01

    The language of orthopedics is rather interesting in that it often credits the original describers or those who popularized a disease process by attaching their names to the disease process in question. These so-called "eponyms" have become quite commonplace in our literature and offer important orthopedic historical insight. Often throughout history, the simultaneous discovery of a disorder is described by two independent researchers, resulting in a hyphenated eponym. Such is the case in the observations made by two physicians, Robert Bayley Osgood and Carl Schlatter, concerning overuse injuries of the tibial tubercle in adolescents. This disorder subsequently became known as "Osgood-Schlatter disease, and aspects of its hyphenated history are the focus of this paper.

  9. 'Transnationalism and the Hyphen: Randolph Bourne and Raphael Hawaweeny'

    DEFF Research Database (Denmark)

    Lock, Charles

    2016-01-01

    On the political controversy around the use of the hyphen in labelling Americans identity (Irish-American, German-American) at the time of the First World War.......On the political controversy around the use of the hyphen in labelling Americans identity (Irish-American, German-American) at the time of the First World War....

  10. Hyphenated analytical techniques for materials characterisation

    Science.gov (United States)

    Armstrong, Gordon; Kailas, Lekshmi

    2017-09-01

    This topical review will provide a survey of the current state of the art in ‘hyphenated’ techniques for characterisation of bulk materials, surface, and interfaces, whereby two or more analytical methods investigating different properties are applied simultaneously to the same sample to better characterise the sample than can be achieved by conducting separate analyses in series using different instruments. It is intended for final year undergraduates and recent graduates, who may have some background knowledge of standard analytical techniques, but are not familiar with ‘hyphenated’ techniques or hybrid instrumentation. The review will begin by defining ‘complementary’, ‘hybrid’ and ‘hyphenated’ techniques, as there is not a broad consensus among analytical scientists as to what each term means. The motivating factors driving increased development of hyphenated analytical methods will also be discussed. This introduction will conclude with a brief discussion of gas chromatography-mass spectroscopy and energy dispersive x-ray analysis in electron microscopy as two examples, in the context that combining complementary techniques for chemical analysis were among the earliest examples of hyphenated characterisation methods. The emphasis of the main review will be on techniques which are sufficiently well-established that the instrumentation is commercially available, to examine physical properties including physical, mechanical, electrical and thermal, in addition to variations in composition, rather than methods solely to identify and quantify chemical species. Therefore, the proposed topical review will address three broad categories of techniques that the reader may expect to encounter in a well-equipped materials characterisation laboratory: microscopy based techniques, scanning probe-based techniques, and thermal analysis based techniques. Examples drawn from recent literature, and a concluding case study, will be used to explain the

  11. Direct 13C NMR Detection in HPLC Hyphenation Mode

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Johansen, Kenneth; Nyberg, Nils

    2012-01-01

    is indubitable in simplifying structural elucidations. In the current study, we demonstrated direct (13)C NMR detection of triterpenoids from a Ganoderma lucidum extract in hyphenation mode. The combined advantage of a cryogenically cooled probe, miniaturization, and multiple trapping enabled the first reported...

  12. Screening for triterpenoid saponins in plants using hyphenated analytical platforms

    DEFF Research Database (Denmark)

    Khakimov, Bekzod; Tseng, Li Hong; Godejohann, Markus

    2016-01-01

    of sugar moieties attached to the aglycone. A total of 49 peaks were tentatively identified as saponins from both plants; they are derived from eight types of aglycones and with 2-5 sugar moieties. Identification of two previously known insect-deterrent saponins, hederagenin cellobioside and oleanolic acid...... saponins consist of a triterpene aglycone with one or more sugar moieties attached to it. However, due to similar physico-chemical properties, isolation and identification of a large diversity of triterpenoid saponins remain challenging. This study demonstrates a methodology to screen saponins using...... hyphenated analytical platforms, GC-MS, LC-MS/MS, and LC-SPE-NMR/MS, in the example of two different phenotypes of the model plant Barbarea vulgaris (winter cress), glabrous (G) and pubescent (P) type that are known to differ by their insect resistance. The proposed methodology allows for detailed comparison...

  13. Advantages and disadvantages of nuclear magnetic resonance spectroscopy as a hyphenated technique

    International Nuclear Information System (INIS)

    Silva Elipe, Maria Victoria

    2003-01-01

    A general overview of the advancements and applications of nuclear magnetic resonance (NMR) hyphenated with other analytical techniques is given from a practical point of view. Details on the advantages and disadvantages of the hyphenation of NMR with liquid chromatography as LC-NMR and also with mass spectrometry as LC-MS-NMR are demonstrated with two examples. Current developments of NMR with other analytical separation techniques, especially with capillary liquid chromatography (capLC) are discussed

  14. Editor's intervention in the register of compounds in archaic Portuguese texts: some reflections on the use of hyphen

    Directory of Open Access Journals (Sweden)

    Antonia Vieira dos Santos

    2014-07-01

    Full Text Available The use of hyphen within compounds was not built up before the nineteenth century. Thus, compounds spelled with hyphen in archaic Portuguese texts are a result of editing criteria adopted by editors. From this type of intervention, the relationship between hyphen use – result of a spelling convention – and the definition of compound adopted by the editor are discussed. Its absence is significant to the history of the language.

  15. Screening for Triterpenoid Saponins in Plants Using Hyphenated Analytical Platforms

    Directory of Open Access Journals (Sweden)

    Bekzod Khakimov

    2016-11-01

    Full Text Available Recently the number of studies investigating triterpenoid saponins has drastically increased due to their diverse and potentially attractive biological activities. Currently the literature contains chemical structures of few hundreds of triterpenoid saponins of plant and animal origin. Triterpenoid saponins consist of a triterpene aglycone with one or more sugar moieties attached to it. However, due to similar physico-chemical properties, isolation and identification of a large diversity of triterpenoid saponins remain challenging. This study demonstrates a methodology to screen saponins using hyphenated analytical platforms, GC-MS, LC-MS/MS, and LC-SPE-NMR/MS, in the example of two different phenotypes of the model plant Barbarea vulgaris (winter cress, glabrous (G and pubescent (P type that are known to differ by their insect resistance. The proposed methodology allows for detailed comparison of saponin profiles from intact plant extracts as well as saponin aglycone profiles from hydrolysed samples. Continuously measured 1D proton NMR data during LC separation along with mass spectrometry data revealed significant differences, including contents of saponins, types of aglycones and numbers of sugar moieties attached to the aglycone. A total of 49 peaks were tentatively identified as saponins from both plants; they are derived from eight types of aglycones and with 2–5 sugar moieties. Identification of two previously known insect-deterrent saponins, hederagenin cellobioside and oleanolic acid cellobioside, demonstrated the applicability of the methodology for relatively rapid screening of bioactive compounds.

  16. New Trends in Flow Injection Analysis: Exploitation of Sequential and Lab-on-Valve Schemes

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    which are difficult or, in fact, otherwise impossible to do, thereby opening new and novel avenues for analytical methods relying on concepts such as kinetic discriminations schemes, exploitation of metastable constituents of attractive analytical characteristics, or utilisation of detection by bio...

  17. Hyphenation of optimized microfluidic sample preparation with nano liquid chromatography for faster and greener alkaloid analysis

    NARCIS (Netherlands)

    Shen, Y.; Beek, van T.A.; Zuilhof, H.; Chen, B.

    2013-01-01

    A glass liquid–liquid extraction (LLE) microchip with three parallel 3.5 cm long and 100 µm wide interconnecting channels was optimized in terms of more environmentally friendly (greener) solvents and extraction efficiency. In addition, the optimized chip was successfully hyphenated with nano-liquid

  18. Application of Hyphenated Techniques in Speciation Analysis of Arsenic, Antimony, and Thallium

    Directory of Open Access Journals (Sweden)

    Rajmund Michalski

    2012-01-01

    Full Text Available Due to the fact that metals and metalloids have a strong impact on the environment, the methods of their determination and speciation have received special attention in recent years. Arsenic, antimony, and thallium are important examples of such toxic elements. Their speciation is especially important in the environmental and biomedical fields because of their toxicity, bioavailability, and reactivity. Recently, speciation analytics has been playing a unique role in the studies of biogeochemical cycles of chemical compounds, determination of toxicity and ecotoxicity of selected elements, quality control of food products, control of medicines and pharmaceutical products, technological process control, research on the impact of technological installation on the environment, examination of occupational exposure, and clinical analysis. Conventional methods are usually labor intensive, time consuming, and susceptible to interferences. The hyphenated techniques, in which separation method is coupled with multidimensional detectors, have become useful alternatives. The main advantages of those techniques consist in extremely low detection and quantification limits, insignificant interference, influence as well as high precision and repeatability of the determinations. In view of their importance, the present work overviews and discusses different hyphenated techniques used for arsenic, antimony, and thallium species analysis, in different clinical, environmental and food matrices.

  19. Application of Hyphenated Techniques in Speciation Analysis of Arsenic, Antimony, and Thallium

    Science.gov (United States)

    Michalski, Rajmund; Szopa, Sebastian; Jabłońska, Magdalena; Łyko, Aleksandra

    2012-01-01

    Due to the fact that metals and metalloids have a strong impact on the environment, the methods of their determination and speciation have received special attention in recent years. Arsenic, antimony, and thallium are important examples of such toxic elements. Their speciation is especially important in the environmental and biomedical fields because of their toxicity, bioavailability, and reactivity. Recently, speciation analytics has been playing a unique role in the studies of biogeochemical cycles of chemical compounds, determination of toxicity and ecotoxicity of selected elements, quality control of food products, control of medicines and pharmaceutical products, technological process control, research on the impact of technological installation on the environment, examination of occupational exposure, and clinical analysis. Conventional methods are usually labor intensive, time consuming, and susceptible to interferences. The hyphenated techniques, in which separation method is coupled with multidimensional detectors, have become useful alternatives. The main advantages of those techniques consist in extremely low detection and quantification limits, insignificant interference, influence as well as high precision and repeatability of the determinations. In view of their importance, the present work overviews and discusses different hyphenated techniques used for arsenic, antimony, and thallium species analysis, in different clinical, environmental and food matrices. PMID:22654649

  20. Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

    Science.gov (United States)

    Marcinkowska, Monika; Barałkiewicz, Danuta

    2016-12-01

    Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Electrophoretic separation techniques and their hyphenation to mass spectrometry in biological inorganic chemistry.

    Science.gov (United States)

    Holtkamp, Hannah; Grabmann, Gerlinde; Hartinger, Christian G

    2016-04-01

    Electrophoretic methods have been widely applied in research on the roles of metal complexes in biological systems. In particular, CE, often hyphenated to a sensitive MS detector, has provided valuable information on the modes of action of metal-based pharmaceuticals, and more recently new methods have been added to the electrophoretic toolbox. The range of applications continues to expand as a result of enhanced CE-to-MS interfacing, with sensitivity often at picomolar level, and evolved separation modes allowing for innovative sample analysis. This article is a followup to previous reviews about CE methods in metallodrug research (Electrophoresis, 2003, 24, 2023-2037; Electrophoresis, 2007, 28, 3436-3446; Electrophoresis, 2012, 33, 622-634), also providing a comprehensive overview of metal species studied by electrophoretic methods hyphenated to MS. It highlights the latest CE developments, takes a sneak peek into gel electrophoresis, traces biomolecule labeling, and focuses on the importance of early-stage drug development. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Metabolite profiling of human amniotic fluid by hyphenated nuclear magnetic resonance spectroscopy.

    Science.gov (United States)

    Graça, Gonçalo; Duarte, Iola F; J Goodfellow, Brian; Carreira, Isabel M; Couceiro, Ana Bela; Domingues, Maria do Rosário; Spraul, Manfred; Tseng, Li-Hong; Gil, Ana M

    2008-08-01

    The metabolic profiling of human amniotic fluid (HAF) is of potential interest for the diagnosis of disorders in the mother or the fetus. In order to build a comprehensive metabolite database for HAF, hyphenated NMR has been used, for the first time, for systematic HAF profiling. Experiments were carried out using reverse-phase (RP) and ion-exchange liquid chromatography (LC), in order to detect less and more polar compounds, respectively. RP-LC conditions achieved good separation of amino acids, some sugars, and xanthines. Subsequent NMR and MS analysis enabled the rapid identification of 30 compounds, including 3-methyl-2-oxovalerate and 4-aminohippurate identified in HAF for the first time, to our knowledge. Under ion-exchange LC conditions, a different set of 30 compounds was detected, including sugars, organic acids, several derivatives of organic acids, and amino acids. In this experiment, five compounds were identified for the first time in HAF: D-xylitol, amino acid derivatives (N-acetylalanine, N-acetylglycine, 2-oxoleucine), and isovalerate. The nonendogenous nature of some metabolites (caffeine, paraxanthine, D-xylitol, sorbitol) is discussed. Hyphenated NMR has allowed the rapid detection of approximately 60 metabolites in HAF, some of which are not detectable by standard NMR due to low abundance (microM) and signal overlap thus enabling an extended metabolite database to be built for HAF.

  3. The re-emergence of hyphenated history-and-philosophy-of-science and the testing of theories of scientific change.

    Science.gov (United States)

    Laudan, Larry; Laudan, Rachel

    2016-10-01

    A basic premise of hyphenated history-and-philosophy-of-science is that theories of scientific change have to be based on empirical evidence derived from carefully constructed historical case studies. This paper analyses one such systematic attempt to test philosophical claims, describing its historical context, rationale, execution, and limited impact. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. MetAlign: Interface-Driven, Versatile Metabolomics Tool for Hyphenated Full-Scan Mass Spectrometry Data Preprocessing

    NARCIS (Netherlands)

    Lommen, A.

    2009-01-01

    Hyphenated full-scan MS technology creates large amounts of data. A versatile easy to handle automation tool aiding in the data analysis is very important in handling such a data stream. MetAlign software-as described in this manuscript-handles a broad range of accurate mass and nominal mass GC/MS

  5. HPTLC Hyphenated with FTIR: Principles, Instrumentation and Qualitative Analysis and Quantitation

    Science.gov (United States)

    Cimpoiu, Claudia

    In recent years, much effort has been devoted to the coupling of high-performance thin-layer chromatography (HPTLC) with spectrometric methods because of the robustness and simplicity of HPTLC and the need for detection techniques that provide identification and determination of sample constituents. IR is one of the spectroscopic methods that have been coupled with HPTLC. IR spectroscopy has a high potential for the elucidation of molecular structures, and the characteristic absorption bands can be used for compound-specific detection. HPTLC-FTIR coupled method has been widely used in the modern laboratories for the qualitative and quantitative analysis. The potential of this method is demonstrated by its application in different fields of analysis such as drug analysis, forensic analysis, food analysis, environmental analysis, biological analysis, etc. The hyphenated HPTLC-FTIR technique will be developed in the future with the aim of taking full advantage of this method.

  6. Brief on -Hyphenated Methods of HPLC for Determining the Presence of Solutes.

    Directory of Open Access Journals (Sweden)

    Mohamad Taleuzzaman

    2017-02-01

    Full Text Available HPLC is the tool in liquid chromatography is unique because of particle size, smaller particle in the stationary phase, increase efficiency of a separation. However, if the particles are made smaller, capillary action increases and it becomes more difficult to drain the column under gravity. For quantitative analysis different types of detector is used in conjunction with HPLC which give precise and accurate result and it is apply according to the nature of the substance. Various types of detectors used in HPLC are mass spectrometry, infrared spectroscopy, visible spectroscopy, ultraviolet spectroscopy, fluorescence spectroscopy, nuclear magnetic resonance, conductivity measurement, and refractive index measurement. Each detector has its assets, limitations and sample types for which it is most effective. The recent development of the so-called hyphenated techniques has improved the ability to separate and identify multiple entities within a mixture.

  7. Speaking the Unspeakable - The Hyphenated in the Irish-Caribbean Dialogue

    Directory of Open Access Journals (Sweden)

    Mahmoud Gewaily

    2014-12-01

    Full Text Available Speaking the unspeakable is to see how far the creative acts of cultural translation in the conflict between history and memory sharpen a natural native knack to converge in a polyphonic way. I pay special attention to the influence that the archetypal theme of speaking the unspeakable in the novel through the initiation experience of the subaltern develops and exerts in the context of increased intercultural awareness. This awareness of the cultural dilemma seems especially important because, in my observation, there is as much alienation and chaos among individuals in the daily contexts of speech communication as among heroes in the imagined communities of literary texts. The hyphenated Irish-Caribbean dialogue of this article aims to bridge cultures in the literary thought of the many writers. Padraic O Conaire and George Lamming, in the two works of Exile (E and The Pleasures of Exile (PE, respectively, are given as examples of the dialogic interlocution.

  8. Interfacing microfluidic handling with spectroscopic detection for real-life applications via the lab-on-valve platform: A review

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel

    2008-01-01

    with syringe pump propelling devices as a front end to a plethora of spectroscopic detection schemes including UV-Vis spectroscopy, spectrofluorimetry, chemiluminescence, AAS, AFS and ICP-AES/MS. In contrast to lab-on-a-chip units, the versatile configuration of the micromachined LOV readily facilitates...

  9. Trying to detect gas-phase ions? Understanding Ion Mobility Spectrometry: Part 2: Hyphenated Methods and Effects of Experimental Parameters

    OpenAIRE

    Cumeras, R.; Figueras, E.; Davis, C.E.; Baumbach, J.I.; Gràcia, I.

    2015-01-01

    Ion Mobility Spectrometry (IMS) is a widely used and ‘well-known’ technique of ion separation in gaseous phase based on the differences of ion mobilities under an electric field. This technique has received increased interest over the last several decades as evidenced by the pace and advances of new IMS devices available. In this review we explore the hyphenated techniques that are used with IMS, especially mass spectrometry as identification approach and multi-capillary column as pre-separat...

  10. Identification and characterization of related substances in EVT-401 by hyphenated LC–MS techniques

    Directory of Open Access Journals (Sweden)

    Binan Zhu

    2017-08-01

    Full Text Available A sensitive and selective method was developed for the separation and characterization of related substances (RSs in EVT-401 by hyphenated LC–MS techniques. Complete separation of the RSs was achieved with an Inertsil ODS-SP column (250 mm×4.6 mm, 5 µm by linear gradient elution using a mobile phase consisting of 0.2% formic acid solution, methanol and acetonitrile. EVT-401 was found to be susceptible to acid, alkaline and oxidative stresses, while relatively stable under photolytic and thermal dry stress conditions. Fourteen RSs including six process-related substances and eight degradation products were detected and identified in EVT-401 with positive ESI high-resolution TOF-MS analysis of their parent ions and the corresponding product mass spectra elucidation, and some of them were further verified by chemical synthesis and NMR spectroscopy. The specific LC–MS method developed for separation, identification and characterization of RSs is valuable for EVT-401 manufacturing process optimization and quality control.

  11. Rice starch granule characterization by flow cytometry scattering techniques hyphenated with sedimentation field-flow fractionation.

    Science.gov (United States)

    Clédat, Dominique; Battu, Serge; Mokrini, Redouane; Cardot, Philippe J P

    2004-09-17

    Sedimentation field-flow fractionation (SdFFF) elution mode of micron sized particle is described generically as "Hyperlayer" and involves particle size, density, shape and rigidity. It requires the use of specific detectors of mass, size, surface, or of other characteristics of the eluted particles. Correlation of FFF retention data with such signals gives hyphenated information about particle properties. Flow cytometry (FC) is a multi dimensional particle counter, which permits specific particle property characterization using light scattering and fluorescence principles. It appears therefore as a powerful technique for micron sized species description. FC is mostly known for cell analyses, while its potential is much broader once proper calibration performed. In this report, forward angle signal (FS) is calibrated in size by using standard latex beads and produces, for a given particle sample, a number versus size histogram, describing particle size distribution. These histograms can be an alternative to Coulter counting. That methodology is tested with rice starch population (RSP) fractions obtained from FFF separation.

  12. Solvent exchange module for LC-NMR hyphenation using machine vision-controlled droplet evaporation.

    Science.gov (United States)

    Schoonen, Jan-Willem; Vulto, Paul; de Roo, Niels; van Duynhoven, John; van der Linden, Heiko; Hankemeier, Thomas

    2013-06-18

    We report the use of pendant droplet evaporation for exchange of eluents for (1)H nuclear magnetic resonance ((1)H NMR) purposes. Analytes are fed and retained in 500 nL droplets, which are concentrated by evaporation and subsequently redissolved in deuterated solvent. Droplet size is monitored by machine vision (MV), and heating rates are adjusted concordingly to maintain a stable droplet volume. Evaporation control is independent of solvent properties, and the setup handles feed rates up to 7 μL min(-1). The interface is capable of exchanging up to 90% of solvent for deuterated solvent, with a good recovery and repeatability for tomato extracts (Solanum lycopersicum). The system was capable of handling both polar and nonpolar analytes in one run. Volatiles such as formate, acetate, and lactate and the thermosensitive compound epigallocatechin gallate were recovered without significant losses. Ethanol and propionate were recovered with significant losses due to the formation of a minimum boiling azeotrope. The current setup is ideally suited for on- and off-line hyphenation of liquid chromatography and NMR, as it is comprehensive, fully automated, and easy to operate.

  13. Review on ion mobility spectrometry. Part 2: hyphenated methods and effects of experimental parameters.

    Science.gov (United States)

    Cumeras, R; Figueras, E; Davis, C E; Baumbach, J I; Gràcia, I

    2015-03-07

    Ion Mobility Spectrometry (IMS) is a widely used and 'well-known' technique of ion separation in the gaseous phase based on the differences of ion mobilities under an electric field. This technique has received increased interest over the last several decades as evidenced by the pace and advances of new IMS devices available. In this review we explore the hyphenated techniques that are used with IMS, specifically mass spectrometry as an identification approach and a multi-capillary column as a pre-separation approach. Also, we will pay special attention to the key figures of merit of the ion mobility spectrum and how data sets are treated, and the influences of the experimental parameters on both conventional drift time IMS (DTIMS) and miniaturized IMS also known as high Field Asymmetric IMS (FAIMS) in the planar configuration. The present review article is preceded by a companion review article which details the current instrumentation and contains the sections that configure both conventional DTIMS and FAIMS devices. These reviews will give the reader an insightful view of the main characteristics and aspects of the IMS technique.

  14. Microfluidic high performance liquid chromatography-chip hyphenation to inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Bishop, David P; Blanes, Lucas; Wilson, Alexander B; Wilbanks, Thor; Killeen, Kevin; Grimm, Rudolf; Wenzel, Ross; Major, Derek; Macka, Mirek; Clarke, David; Schmid, Robin; Cole, Nerida; Doble, Philip A

    2017-05-12

    The Agilent Chip Cube Interface is a microfluidic chip-based technology originally designed for nanospray molecular mass spectrometry in which the sample enrichment, nano-column, tubing, connectors and spray tip were integrated into a single biocompatible chip. Here we describe the hyphenation of the Chip Cube Interface to ICP-MS via modification of the standard HPLC chip design and a new total consumption nebuliser suitable for flow rates as low as 300nLmin -1 . The potential of the instrument to eliminate common nanoLC - ICP-MS shortcomings such as leaks, blockages and band-broadening was demonstrated via analysis of cyanocobalamin in equine plasma. The method was linear over three orders of magnitude with an r 2 of 0.9999, the peak area repeatability was 1.9% (n=7), and the detection limit was 14ngmL -1 . This novel configuration of the Chip Cube Interface coupled to ICP-MS is a suitable platform for the analysis of biomolecules associated with trace metals and speciation applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Chemometric profile of root extracts of Rhodiola imbricata Edgew. with hyphenated gas chromatography mass spectrometric technique.

    Directory of Open Access Journals (Sweden)

    Amol B Tayade

    Full Text Available Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo, belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S; 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl; α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful

  16. Bioprofiling of Salicaceae bud extracts through high-performance thin-layer chromatography hyphenated to biochemical, microbiological and chemical detections.

    Science.gov (United States)

    Hage, Salim; Morlock, Gertrud E

    2017-03-24

    The buds of poplars (Populus L.) and willows (Salix L.), both from the same family (Salicaceae Mirbel), are increasingly used in gemmotherapy and importantly contribute to the production of the physiologically active propolis by European bee Apis mellifera L. In order to study their phenolic profiles, polar extracts of buds from P. nigra L. were compared to those of P. alba L. and S. alba L. through high-performance thin-layer chromatography (HPTLC). Five chemotypical patterns were distinguished after derivatisation with the Natural Product reagent and confirmed by principal component analysis. The HPTLC analysis was directly hyphenated to various microbiological and biochemical assays as well as spectrometric techniques, directly linking to active molecules in the chromatograms. At a glance, polyvalent compounds were evident when all derivatisation and activity assays, to which HPTLC was hyphenated at ease, were combined together. In Populus buds, at least three antimicrobial compound zones were detected using Aliivibrio fischeri and Bacillus subtilis bioassays, and one phyto-œstrogen with the planar yeast œstrogen screen. In all samples, several inhibitors of acetyl- and butyrylcholinesterase and rabbit liver esterase were detected. Hyphenation to high resolution mass spectrometry supported the assignment of bioactive compounds, as shown for chrysin as selective cholinesterase inhibitor as well as caffeic acid and galangin as antimicrobials in P. nigra and P. alba. This fast and cost-efficient method can be appropriately extended and applied to the botanical origin determination and quality control of bud extracts and propolis samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Hyphenation of infrared spectroscopy to liquid chromatography for qualitative and quantitative polymer analysis: Degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.; Hankemeier, T.

    2006-01-01

    Hyphenation of infrared spectroscopy (IR) to liquid chromatography (LC) has been applied to study chemical changes in poly(bisphenol A)carbonate (PC) as a result of degradation. Especially coupling of LC to FTIR through solvent elimination is a sensitive approach to identify changes in functionality

  18. Development of a microfluidic confocal fluorescence detection system for the hyphenation of nano-LC to on-line biochemical assays

    NARCIS (Netherlands)

    Heus, F.; Giera, M.A.; de Kloe, G.E.; van Iperen, D.; Buijs, J.B.; Nahar, T.T.; Smit, A.B.; Lingeman, H.; de Esch, I.J.P.; Niessen, W.M.A.; Irth, H.; Kool, J.

    2010-01-01

    One way to profile complex mixtures for receptor affinity is to couple liquid chromatography (LC) on-line to biochemical detection (BCD). A drawback of this hyphenated screening approach is the relatively high consumption of sample, receptor protein and (fluorescently labeled) tracer ligand. Here,

  19. Current status of hyphenated mass spectrometry in studies of the metabolism of drugs of abuse, including doping agents.

    Science.gov (United States)

    Meyer, Markus R; Maurer, Hans H

    2012-01-01

    This paper reviews scientific contributions on the identification and/or quantification of metabolites of drugs of abuse in in vitro assays or various body samples using hyphenated mass spectrometry. Gas chromatography-mass spectrometry (GC-MS) as well as liquid chromatography-mass spectrometry (LC-MS) approaches are considered and discussed if they have been reported in the last five years and are relevant to clinical and forensic toxicology or doping control. Workup and artifact formation are discussed, and typical examples of studies of the metabolism of designer drugs, doping agents, herbal drugs, and synthetic cannabinoids are provided. Procedures for quantifying metabolites in body samples for pharmacokinetic studies or in enzyme incubations for enzyme kinetic studies are also reviewed. In conclusion, the reviewed papers showed that both GC-MS and LC-MS still have important roles to play in research into the metabolism of drugs of abuse, including doping agents.

  20. Hyphenation of two simultaneously employed soft photo ionization mass spectrometers with thermal analysis of biomass and biochar

    International Nuclear Information System (INIS)

    Fendt, Alois; Geissler, Robert; Streibel, Thorsten

    2013-01-01

    Highlights: ► First simultaneous hyphenation of two time-of-flight mass spectrometers with different soft photo ionization techniques (SPI and REMPI) to Thermal Analysis using a newly developed prototype for EGA is presented. ► Resonance enhanced multi-photon ionization (REMPI) enables sensitive and selective analysis of aromatic species. ► Single photon ionization (SPI) using VUV light supplied by an innovative electron-beam pumped excimer light source (EBEL) comprehensively ionizes (nearly) all organic molecules. ► The resulting mass spectra show distinct patterns for the evolved gases of the miscellaneous biomasses and chars thereof. ► The potential for detailed kinetic studies is apparent on account of the complex pyrolysis gas compositions. - Abstract: Evolved gas analysis (EGA) is a powerful and complementary tool for Thermal Analysis. In this context, two time-of-flight mass spectrometers with different soft photo-ionization techniques are simultaneously hyphenated to a thermo balance and applied in form of a newly developed prototype for EGA of pyrolysis gases from biomass and biochar. Resonance enhanced multi-photon ionization (REMPI) is applied for selective analysis of aromatic species. Furthermore, single photon ionization (SPI) using VUV light supplied by an electron-beam pumped excimer light source (EBEL) was used to comprehensively ionize (nearly) all organic molecules. The soft ionization capability of photo-ionization techniques allows direct and on-line analysis of the evolved pyrolysis gases. Characteristic mass spectra with specific patterns could be obtained for the miscellaneous biomass feeds used. Temperature profiles of the biochars reveal a desorption step, followed by pyrolysis as observed for the biomasses. Furthermore, the potential for kinetic studies is apparent for this instrumental setup.

  1. TLC-UV hyphenated with MALDI-TOFMS for the screening of invertase substrates in plant extracts.

    Science.gov (United States)

    Ferey, Justine; Da Silva, David; Lafite, Pierre; Daniellou, Richard; Maunit, Benoît

    2017-08-01

    In this study, thin-layer chromatography (TLC) hyphenated with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) was developed for the screening of invertase substrates in complex matrices. BfrA, a specific β-D-fructofuranosidase from Leishmania major, was chosen as a model enzyme to screen biological activity in plant extracts due to its capacity to hydrolyze specific carbohydrates. TLC was considered to be a reliable technique for screening substrates (bioactive molecules) in plant extracts due to its quantitative capabilities whereas MALDI-TOFMS was particularly useful for rapid identification. The first part of this approach consisted of a differential analysis by TLC-densitometry to highlight band under- and over-expressions in plant extract between blank and enzymatic reaction. Zones of interest were then immediately analyzed by TLC-MALDI-TOFMS coupling to identify bioactive molecules. Development of the method presented various challenges: the separation and analysis of isomers (such as glucose and fructose), the high matrix effect (demonstrated by the analysis of products with invertase enzyme naturally present in plant extract), and the analysis of polar molecules with low molecular mass (sugars). Thanks to the separative technique, the specificity of detection, and the high precision of the characterization, this method was shown to be feasible for the analysis of bioactive molecules in complex mixtures containing interfering compounds (e.g. proteins, salts). Overall, this study demonstrates that Thin-layer chromatography hyphenated with Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry is a simple, rapid, precise and efficient method for the analysis of suitable substrates in raw samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Development of a method to extract and purify target compounds from medicinal plants in a single step: online hyphenation of expanded bed adsorption chromatography and countercurrent chromatography

    Science.gov (United States)

    Li, Yang; Wang, Nan; Zhang, Min; Ito, Yoichiro; Zhang, Hongyang; Wang, Yuerong; Guo, Xin; Hu, Ping

    2014-01-01

    Pure compounds extracted and purified from natural sources are crucial to lead discovery and drug screening. This study presents a novel two-dimensional hyphenation of expanded bed adsorption chromatography (EBAC) and high-speed countercurrent chromatography (HSCCC) for extraction and purification of target compounds from medicinal plants in a single step. The EBAC and HSCCC were hyphenated via a six-port injection valve as an interface. Fractionation of ingredients of Salvia miltiorrhiza and Rhizoma coptidis was performed on the hyphenated system to verify its efficacy. An amount each of 52.9 mg of salvianolic acid B and 2.1 mg of rosmarinic acid was obtained from Salvia miltiorrhiza by the two-dimensional system in a single step. The purities of the targets were over 96% of salvianolic acid B and 74% of rosmarinic acid. An amount each of 4.6 mg of coptisine and 4.1 mg of berberine was obtained from Rhizoma coptidis each with 98% and 82% purity, respectively. The processing time was nearly 50% that of the multi-step method. These results indicate that the present method is a rapid and green way to harvest targets from medicinal plants in a single step. PMID:24588208

  3. Capillary Electrophoresis Hyphenated with Mass Spectrometry for Determination of Inflammatory Bowel Disease Drugs in Clinical Urine Samples

    Directory of Open Access Journals (Sweden)

    Katarína Maráková

    2017-11-01

    Full Text Available Azathioprine is the main thiopurine drug used in the treatment of immune-based inflammations of gastrointestinal tract. For the purpose of therapy control and optimization, effective and reliable analytical methods for a rapid drug monitoring in biological fluids are essential. Here, we developed a separation method based on the capillary electrophoresis (CE hyphenated with tandem mass spectrometry (MS/MS for the simultaneous determination of azathioprine and its selected metabolites (6-thioguanine, 6-mercaptopurine, and 6-methylmercaptopurine as well as other co-medicated drugs (mesalazine, prednisone, and allopurinol. The optimized CE-MS/MS conditions provided a very efficient and stable system for the separation and sensitive detection of these drugs in human urine matrices. The developed method was successfully applied for the assay of the targeted drugs and their selected metabolites in urine samples collected from patients suffering from inflammatory bowel disease (IBD and receiving azathioprine therapy. The developed CE-MS/MS method, due to its reliability, short analysis time, production of complex clinical profiles, and favorable performance parameters, evaluated according to FDA guidelines for bioanalytical method validation, is proposed for routine clinical laboratories to optimize thiopurine therapy, estimate enzymatic activity, and control patient compliance with medication and co-medication.

  4. A Hyphenated Technique based on High-Performance Thin Layer Chromatography for Determining Neutral Sphingolipids: A Proof of Concept

    Directory of Open Access Journals (Sweden)

    Andrés Domínguez

    2015-04-01

    Full Text Available Hyphenated HPTLC has been used to analyze several neutral sphingolipids acting as lysosomal storage disease (LSD biomarkers. Automated multiple development (AMD provides separation of lipid peaks, which are detected and quantified using fluorescence detection by intensity changes (FDIC after primuline post-impregnation. A final online transfer to a mass spectrometer by means of an elution-based interface allows their identification using electrospray ionization (ESI and atmospheric pressure chemical ionization (APCI.Given that the increases in fluorescent emission detected by FDIC are produced by non-specific, electrostatic interactions between the primuline and hydrocarbon chains in the ceramide backbones of sphingolipids, it is a non-destructive detection technique, allowing the precise location and transfer of biomarker peaks to a mass spectrometer using an elution interface. By using primuline as a fluorophore, the technique is also compatible with ESI-APCI and does not interfere with the MS of sphingolipids. APCI provides useful and complementary structural information to the ESI for sphingolipid identification. Moreover, FDIC emission can be used for quantitative purposes. Results include the determination of sphingomyelin (SM in human-plasma samples (RSD < 6% by means of a standard addition method with non-linear calibration, and the identification of globotriaosylceramide (Gb3 in the plasma of a Fabry patient. Only one HPTLC plate is needed to perform the analysis.

  5. Lab-on-Valve Micro Sequential Injection: A Versatile Approach for Implementing Integrated Sample Pre-preparations and Executing (Bio)Chemical Assays

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    by bio- and chemiluminescence. In recent years, FIA has been supplemented by Sequential Injection Analysis (SIA), which, although it inherently entails some limitations as compared to FIA, offers specific advantages, notably in terms of significantly reduced sample and reagent(s) consumption and hence...... of applications. Particular focus will be placed on its use as a vehicle for pretreatment of complex sample matrices for determination of trace-level concentrations of metal ions by electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) via exploitation...... of the renewable microcolumn concept. Despite their excellent analytical chemical capabilities, ETAAS as well as ICPMS often require that the samples are subjected to suitable pretreatment in order to obtain the necessary sensitivity and selectivity. Either in order to separate the analyte from potentially...

  6. Lab-on-Valve Micro Sequential Injection: A Versatile Approach for Implementing Integrated Sample Pre-preparations and Executing (Bio)Chemical Assays

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    In the last decade, Flow Injection Analysis (FIA) became supplemented by Sequential Injection Analysis (SIA), which, although it inherently entails some limitations as compared to FIA, offers specific advantages, notably in terms of significantly reduced sample and reagent(s) consumption and hence...... will be directed towards its use as a vehicle for on-line pretreatment of complex sample matrices for determination of trace-level concentrations of metal ions by electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS) via exploitation of the renewable solid......-phase microcolumn concept utilising hydrophobic as well as hydrophilic bead materials. Although ETAAS and ICPMS both are characterised by excellent analytical chemical capabilities, they nevertheless often require that the samples be subjected to suitable pretreatment in order to obtain the necessary sensitivity...

  7. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters.

    Science.gov (United States)

    Santos, Inês C; Mesquita, Raquel B R; Rangel, António O S S

    2015-09-03

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60-160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11-21 for the metal ions. A LOD of 0.23 μg L(-1) for cadmium, 2.39 μg L(-1) for zinc, and 0.11 μg L(-1) for copper and a sampling rate of 12, 13, and 15 h(-1) for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters

    International Nuclear Information System (INIS)

    Santos, Inês C.; Mesquita, Raquel B.R.; Rangel, António O.S.S.

    2015-01-01

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60–160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11–21 for the metal ions. A LOD of 0.23 μg L −1 for cadmium, 2.39 μg L −1 for zinc, and 0.11 μg L −1 for copper and a sampling rate of 12, 13, and 15 h −1 for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. - Highlights: • Multi-parametric determination of cadmium, zinc, and copper at the μg L −1 level. • In-line metal ions preconcentration using NTA resin. • Minimization of matrix interferences by performing solid phase spectrometry in a SI-LOV platform. • Successful application to metal ions determination in freshwaters.

  9. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Inês C. [CBQF–Centro de Biotecnologia e Química Fina – Laboratório Associado, Escola Superior de Biotecnologia, Universidade Católica Portuguesa/Porto, Rua Arquiteto Lobão Vital, Apartado 2511, 4202-401 Porto (Portugal); Mesquita, Raquel B.R. [CBQF–Centro de Biotecnologia e Química Fina – Laboratório Associado, Escola Superior de Biotecnologia, Universidade Católica Portuguesa/Porto, Rua Arquiteto Lobão Vital, Apartado 2511, 4202-401 Porto (Portugal); Laboratório de Hidrobiologia, Instituto de Ciências Biomédicas Abel Salazar (ICBAS), Universidade do Porto, Rua de Jorge Viterbo Ferreira no. 228, 4050-313 Porto (Portugal); Rangel, António O.S.S., E-mail: arangel@porto.ucp.pt [CBQF–Centro de Biotecnologia e Química Fina – Laboratório Associado, Escola Superior de Biotecnologia, Universidade Católica Portuguesa/Porto, Rua Arquiteto Lobão Vital, Apartado 2511, 4202-401 Porto (Portugal)

    2015-09-03

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60–160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11–21 for the metal ions. A LOD of 0.23 μg L{sup −1} for cadmium, 2.39 μg L{sup −1} for zinc, and 0.11 μg L{sup −1} for copper and a sampling rate of 12, 13, and 15 h{sup −1} for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. - Highlights: • Multi-parametric determination of cadmium, zinc, and copper at the μg L{sup −1} level. • In-line metal ions preconcentration using NTA resin. • Minimization of matrix interferences by performing solid phase spectrometry in a SI-LOV platform. • Successful application to metal ions determination in freshwaters.

  10. At-line hyphenation of high-speed countercurrent chromatography with Sephadex LH-20 column chromatography for bioassay-guided separation of antioxidants from vine tea (Ampelopsis grossedentata).

    Science.gov (United States)

    Ma, Ruyi; Zhou, Rongrong; Tong, Runna; Shi, Shuyun; Chen, Xiaoqing

    2017-01-01

    Vine tea (Ampelopsis grossedentata), a widely used healthy tea, beverage and herbal medicine, exhibited strong antioxidant activity. However, systematic purification of antioxidants, especially for those with similar structures or polarities, is a challenging work. Here, we present a novel at-line hyphenation of high-speed countercurrent chromatography with Sephadex LH-20 column chromatography (HSCCC-Sephadex LH-20 CC) for rapid and efficient separation of antioxidants from vine tea target-guided by 1,1-diphenyl-2-picryl-hydrazyl radical-high performance liquid chromatography (DPPH-HPLC) experiment. A makeup pump, a six-port switching valve and a trapping column were served as interface. The configuration had no operational time and mobile phase limitations between two dimensional chromatography and showed great flexibility without tedious sample-handling procedure. Seven targeted antioxidants were firstly separated by stepwise HSCCC using petroleum ether-ethyl acetate-methanol-water (4:9:4:9, v/v/v/v) and (4:9:5:8, v/v/v/v) as solvent systems, and then co-eluted antioxidants were on-line trapped, concentrated and desorbed to Sephadex LH-20 column for further off-line purification by methanol. It is noted that six elucidated antioxidants with purity over 95% exhibited stronger activity than ascorbic acid (VC). More importantly, this at-line hyphenated strategy could sever as a rapid and efficient pathway for systematic purification of bioactive components from complex matrix. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Inline roasting hyphenated with gas chromatography-mass spectrometry as an innovative approach for assessment of cocoa fermentation quality and aroma formation potential.

    Science.gov (United States)

    Van Durme, Jim; Ingels, Isabel; De Winne, Ann

    2016-08-15

    Today, the cocoa industry is in great need of faster and robust analytical techniques to objectively assess incoming cocoa quality. In this work, inline roasting hyphenated with a cooled injection system coupled to a gas chromatograph-mass spectrometer (ILR-CIS-GC-MS) has been explored for the first time to assess fermentation quality and/or overall aroma formation potential of cocoa. This innovative approach resulted in the in-situ formation of relevant cocoa aroma compounds. After comparison with data obtained by headspace solid phase micro extraction (HS-SPME-GC-MS) on conventional roasted cocoa beans, ILR-CIS-GC-MS data on unroasted cocoa beans showed similar formation trends of important cocoa aroma markers as a function of fermentation quality. The latter approach only requires small aliquots of unroasted cocoa beans, can be automatated, requires no sample preparation, needs relatively short analytical times (<1h) and is highly reproducible. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Extraction and separation of lactate dehydrogenase inhibitors from Poria cocos (Schw.) Wolf based on a hyphenated technique and in vitro methods.

    Science.gov (United States)

    Li, Sainan; Zhang, Jianxu; Li, Senlin; Liu, Chunming; Liu, Shu; Liu, Zhiqiang

    2017-04-01

    Stroke is one of the most common diseases worldwide. Lactate dehydrogenase inhibitors are widely used in the treatment of ischemic stroke, with natural products considered a promising source of lactate dehydrogenase inhibitors. In this study, ultrafiltration liquid chromatography coupled with mass spectrometry was used for the screening and identification of lactate dehydrogenase inhibitors from Poria cocos. Five lactate dehydrogenase inhibitors were selected: dehydropachymic acid, pachymic acid, dehydrotrametenolic acid, trametenolic acid, and eburicoic acid. The inhibitors were extracted and isolated with purities of 96.75, 98.15, 97.25, 95.46, and 94.88%, respectively, by using a new "hyphenated" strategy of microwave-assisted extraction coupled with counter-current chromatography and centrifugal partition chromatography by a two-phase solvent system of n-hexane/ethyl acetate/ethanol/water at the volume ratio 0.965:1.000:0.936:0.826 v/v/v/v. The bioactivity of the isolated compounds was assessed using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay in PC12 cells. The results also showed that the hyphenated technique of microwave-assisted extraction coupled with counter-current chromatography and centrifugal partition chromatography was an efficient method for the continuous extraction and online isolation of chemical constituents from medicinal herbs. Furthermore, the research route based on the activity screening, extraction, separation, and activity verification of the compounds offered advantages of efficiency, orientation, and objectivity. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Online hyphenation of extraction, Sephadex LH-20 column chromatography, and high-speed countercurrent chromatography: A highly efficient strategy for the preparative separation of andrographolide from Andrographis paniculata in a single step.

    Science.gov (United States)

    Zhang, Ying-Qi; Wang, Shan-Shan; Han, Chao; Xu, Jin-Fang; Luo, Jian-Guang; Kong, Ling-Yi

    2017-12-01

    A novel isolation strategy, online hyphenation of ultrasonic extraction, Sephadex LH-20 column chromatography combined with high-speed countercurrent chromatography, was developed for pure compounds extraction and purification. Andrographolide from Andrographis paniculata was achieved only in a single step purification protocol via the present strategy. The crude powder was ultrasonic extracted and extraction was pumped into Sephadex LH-20 column directly to cut the nontarget fractions followed by the second-dimensional high-speed countercurrent chromatography, hyphenated by a six-port valve equipped at the post-end of Sephadex LH-20 column, for the final purification. The results yielded andrographolide with the amount of 1.02 mg and a purity of 98.5% in a single step, indicating that the present method is effective to harvest target compound from medicinal plant. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Mass spectrometry and NMR spectroscopy: modern high-end detectors for high resolution separation techniques--state of the art in natural product HPLC-MS, HPLC-NMR, and CE-MS hyphenations.

    Science.gov (United States)

    Seger, Christoph; Sturm, Sonja; Stuppner, Hermann

    2013-07-01

    Current natural product research is unthinkable without the use of high resolution separation techniques as high performance liquid chromatography or capillary electrophoresis (HPLC or CE respectively) combined with mass spectrometers (MS) or nuclear magnetic resonance (NMR) spectrometers. These hyphenated instrumental analysis platforms (CE-MS, HPLC-MS or HPLC-NMR) are valuable tools for natural product de novo identification, as well as the authentication, distribution, and quantification of constituents in biogenic raw materials, natural medicines and biological materials obtained from model organisms, animals and humans. Moreover, metabolic profiling and metabolic fingerprinting applications can be addressed as well as pharmacodynamic and pharmacokinetic issues. This review provides an overview of latest technological developments, discusses the assets and drawbacks of the available hyphenation techniques, and describes typical analytical workflows.

  15. On-line hyphenation of centrifugal partition chromatography and high pressure liquid chromatography for the fractionation of flavonoids from Hippophaë rhamnoides L. berries.

    Science.gov (United States)

    Michel, Thomas; Destandau, Emilie; Elfakir, Claire

    2011-09-09

    Centrifugal Partition Chromatography (CPC), a liquid-liquid preparative chromatography using two immiscible solvent systems, benefits from numerous advantages for the separation or purification of synthetic or natural products. This study presents the on-line hyphenation of CPC-Evaporative Light Scattering Detector (CPC-ELSD) with High Performance Liquid Chromatography-UV (HPLC-UV) for the fractionation of flavonols from a solvent-free microwave extract of sea buckthorn (Hippophaë rhamnoides L., Elaeagnaceae) berries. An Arizona G system was used for the fractionation of flavonoids by CPC and a fused core Halo C18 column allowed the on-line analyses of collected fractions by HPLC. The on-line CPC/HPLC procedure allowed the simultaneous fractionation step at preparative scale combined with the HPLC analyses which provide direct fingerprint of collected fractions. Thus the crude extract was simplified and immediate information on the composition of fractions could be obtained. Furthermore, this methodology reduced the time of post-fractionation steps and facilitated identification of main molecules by Mass Spectrometry (MS). Rutin, isorhamnetin-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin-3-O-glucoside, isorhamnetin-rhamnoside, quercetin and isorhamnetin were identified. CPC-ELSD/HPLC-UV could be considered as a high-throughput technique for the guided fractionation of bioactive natural products from complex crude extracts. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Open-Source Assisted Laboratory Automation through Graphical User Interfaces and 3D Printers: Application to Equipment Hyphenation for Higher-Order Data Generation.

    Science.gov (United States)

    Siano, Gabriel G; Montemurro, Milagros; Alcaráz, Mirta R; Goicoechea, Héctor C

    2017-10-17

    Higher-order data generation implies some automation challenges, which are mainly related to the hidden programming languages and electronic details of the equipment. When techniques and/or equipment hyphenation are the key to obtaining higher-order data, the required simultaneous control of them demands funds for new hardware, software, and licenses, in addition to very skilled operators. In this work, we present Design of Inputs-Outputs with Sikuli (DIOS), a free and open-source code program that provides a general framework for the design of automated experimental procedures without prior knowledge of programming or electronics. Basically, instruments and devices are considered as nodes in a network, and every node is associated both with physical and virtual inputs and outputs. Virtual components, such as graphical user interfaces (GUIs) of equipment, are handled by means of image recognition tools provided by Sikuli scripting language, while handling of their physical counterparts is achieved using an adapted open-source three-dimensional (3D) printer. Two previously reported experiments of our research group, related to fluorescence matrices derived from kinetics and high-performance liquid chromatography, were adapted to be carried out in a more automated fashion. Satisfactory results, in terms of analytical performance, were obtained. Similarly, advantages derived from open-source tools assistance could be appreciated, mainly in terms of lesser intervention of operators and cost savings.

  17. Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Romaris-Hortas, Vanessa; Bermejo-Barrera, Pilar [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n. 15782 - Santiago de Compostela (Spain); Moreda-Pineiro, Jorge [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira, s/n. 15071, A Coruna (Spain); Moreda-Pineiro, Antonio, E-mail: antonio.moreda@usc.es [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n. 15782 - Santiago de Compostela (Spain)

    2012-10-01

    Highlights: Black-Right-Pointing-Pointer Bioavailable iodine and bromine speciation in edible seaweed were developed. Black-Right-Pointing-Pointer In vitro dialyzability was used to assess the bioavailable fractions. Black-Right-Pointing-Pointer AEC hyphenated with inductively coupled plasma-mass spectrometry was used. Black-Right-Pointing-Pointer Iodide, MIT, DIT, bromide and bromate were found in dialyzates from edible seaweed. Black-Right-Pointing-Pointer Positive correlation between bioavailability and protein contents was found. - Abstract: A bioavailability study based on an in vitro dialyzability approach has been applied to assess the bio-available fractions of iodine and bromine species from edible seaweed. Iodide, iodate, 3-iodo-tyrosine (MIT), 3,5-diiodo-tyrosine (DIT), bromide and bromate were separated by anion exchange chromatography under a gradient elution mode (175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase, and flow rates within the 0.5-1.5 mL min{sup -1} range). Inductively coupled plasma-mass spectrometry (ICP-MS) was used as a selective detector for iodine ({sup 127}I) and bromine ({sup 79}Br). Low dialyzability ratios (within the 2.0-18% range) were found for iodine species; whereas, moderate dialyzability percentages (from 9.0 to 40%) were obtained for bromine species. Iodide and bromide were the major species found in the dialyzates from seaweed, although MIT and bromate were also found in the dialyzates from most of the seaweed samples analysed. However, DIT was only found in dialyzates from Wakame, Kombu, and NIES 09 (Sargasso) certified reference material; whereas, iodate was not found in any dialyzate. Iodine dialyzability was found to be dependent on the protein content (negative correlation), and on the carbohydrate and dietary fibre levels (positive correlation). However, bromine dialyzability was only dependent on the protein amount in seaweed (negative correlation).

  18. Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Jorge; Moreda-Piñeiro, Antonio

    2012-01-01

    Highlights: ► Bioavailable iodine and bromine speciation in edible seaweed were developed. ► In vitro dialyzability was used to assess the bioavailable fractions. ► AEC hyphenated with inductively coupled plasma-mass spectrometry was used. ► Iodide, MIT, DIT, bromide and bromate were found in dialyzates from edible seaweed. ► Positive correlation between bioavailability and protein contents was found. - Abstract: A bioavailability study based on an in vitro dialyzability approach has been applied to assess the bio-available fractions of iodine and bromine species from edible seaweed. Iodide, iodate, 3-iodo-tyrosine (MIT), 3,5-diiodo-tyrosine (DIT), bromide and bromate were separated by anion exchange chromatography under a gradient elution mode (175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase, and flow rates within the 0.5–1.5 mL min −1 range). Inductively coupled plasma-mass spectrometry (ICP-MS) was used as a selective detector for iodine ( 127 I) and bromine ( 79 Br). Low dialyzability ratios (within the 2.0–18% range) were found for iodine species; whereas, moderate dialyzability percentages (from 9.0 to 40%) were obtained for bromine species. Iodide and bromide were the major species found in the dialyzates from seaweed, although MIT and bromate were also found in the dialyzates from most of the seaweed samples analysed. However, DIT was only found in dialyzates from Wakame, Kombu, and NIES 09 (Sargasso) certified reference material; whereas, iodate was not found in any dialyzate. Iodine dialyzability was found to be dependent on the protein content (negative correlation), and on the carbohydrate and dietary fibre levels (positive correlation). However, bromine dialyzability was only dependent on the protein amount in seaweed (negative correlation).

  19. Hyphenation of solid-phase extraction with liquid chromatography and nuclear magnetic resonance: application of HPLC-DAD-SPE-NMR to identification of constituents of Kanahia laniflora.

    Science.gov (United States)

    Clarkson, Cailean; Staerk, Dan; Hansen, Steen Honoré; Jaroszewski, Jerzy W

    2005-06-01

    The introduction of on-line solid-phase extraction (SPE) in HPLC-NMR has dramatically enhanced the sensitivity of this technique by concentration of the analytes in a small-volume NMR flow cell and by increasing the amount of the analyte by multiple peak trapping. In this study, the potential of HPLC-DAD-SPE-NMR hyphenation was demonstrated by structure determination of complex constituents of flower, leaf, root, and stem extracts of an African medicinal plant Kanahia laniflora. The technique was shown to allow acquisition of high-quality homo- and heteronuclear 2D NMR data following analytical-scale HPLC separation of extract constituents. Four flavonol glycosides [kaempferol 3-O-(6-O-alpha-l-rhamnopyranosyl)-beta-d-glucopyranoside; kaempferol 3-O-(2,6-di-O-alpha-l-rhamnopyranosyl)-beta-d-glucopyranoside; quercetin 3-O-(2,6-di-O-alpha-l-rhamnopyranosyl)-beta-d-glucopyranoside (rutin); and isorhamnetin, 3-O-(6-O-alpha-l-rhamnopyranosyl)-beta-d-glucopyranoside] and three 5alpha-cardenolides [coroglaucigenin 3-O-6-deoxy-beta-d-allopyranoside; coroglaucigenin 3-O-(4-O-beta-d-glucopyranosyl)-6-deoxy-beta-d-glucopyranoside; 3'-O-acetyl-3'-epiafroside] were identified, with complete assignments of 1H and 13C resonances based on HSQC and HMBC spectra whenever required. Confirmation of the structures was provided by HPLC-MS data. The HPLC-DAD-SPE-NMR technique therefore speeds up the dereplication of complex mixtures of natural origin significantly, by characterization of individual extract components prior to preparative isolation work.

  20. Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

    Science.gov (United States)

    Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

    2016-03-18

    Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Hyphenation of Thermal Analysis to Ultrahigh-Resolution Mass Spectrometry (Fourier Transform Ion Cyclotron Resonance Mass Spectrometry) Using Atmospheric Pressure Chemical Ionization For Studying Composition and Thermal Degradation of Complex Materials.

    Science.gov (United States)

    Rüger, Christopher P; Miersch, Toni; Schwemer, Theo; Sklorz, Martin; Zimmermann, Ralf

    2015-07-07

    In this study, the hyphenation of a thermobalance to an ultrahigh-resolution Fourier transform ion cyclotron resonance mass spectrometer (UHR FTICR MS) is presented. Atmospheric pressure chemical ionization (APCI) is used for efficient ionization. The evolved gas analysis (EGA), using high-resolution mass spectrometry allows the time-resolved molecular characterization of thermally induced processes in complex materials or mixtures, such as biomass or crude oil. The most crucial part of the setup is the hyphenation between the thermobalance and the APCI source. Evolved gases are forced to enter the atmospheric pressure ionization interface of the MS by applying a slight overpressure at the thermobalance side of the hyphenation. Using the FTICR exact mass data, detailed chemical information is gained by calculation of elemental compositions from the organic species, enabling a time and temperature resolved, highly selective detection of the evolved species. An additional selectivity is gained by the APCI ionization, which is particularly sensitive toward polar compounds. This selectivity on the one hand misses bulk components of petroleum samples such as alkanes and does not deliver a comprehensive view but on the other hand focuses particularly on typical evolved components from biomass samples. As proof of principle, the thermal behavior of different fossil fuels: heavy fuel oil, light fuel oil, and a crude oil, and different lignocellulosic biomass, namely, beech, birch, spruce, ash, oak, and pine as well as commercial available softwood and birch-bark pellets were investigated. The results clearly show the capability to distinguish between certain wood types through their molecular patterns and compound classes. Additionally, typical literature known pyrolysis biomass marker were confirmed by their elemental composition, such as coniferyl aldehyde (C10H10O3), sinapyl aldehyde (C11H12O4), retene (C18H18), and abietic acid (C20H30O2).

  2. Highly selective micro-sequential injection lab-on-valve (μSI-LOV) method for determination of ultra trace concentrations of nickel in saline matrices using detection by electrothermal atomic absorption spectrometr

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Jensen, Rikard

    2006-01-01

    by electrothermal atomic absorption spectrometry (ETAAS). Based on the dimethylglyoxime (DMG) gravimetric procedure used for nickel analysis, the sample, as contained in pH 9.0 buffer, is, after on-line merging with the chelating reagent, transported to a reaction coil attached to one of the external ports...

  3. On-line ion exchange preconcentration in a sequential injection lab-on-valve microsystem incorporating a renewable column with ETAAS for the trace-level determination of bismuth in urine and river sediment

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2001-01-01

    with the preconcentration process of the ensuing sample. The performance of the system is demonstrated for the determination of bismuth. With 2.4 ml sample loading, an enrichment factor of 33.4, a detection limit of 27 ng /l, along with a sampling frequency of 10 was obtained. The relative standard deviation was 2.......3% for the determination of 2.0 mug/l Bi (n = 7). The procedure was validated by determination of bismuth in a certified reference material CRM 320 (river sediment), and by bismuth spike recoveries in two human urine samples....

  4. Screening for illicit drugs in pooled human urine and urinated soil samples and studies on the stability of urinary excretion products of cocaine, MDMA, and MDEA in wastewater by hyphenated mass spectrometry techniques

    DEFF Research Database (Denmark)

    Mardal, Marie; Kinyua, Juliet; Ramin, Pedram

    2017-01-01

    ) is useful to detect consumed drugs and identify targets of illicit drugs use. The aims of the study were (1) to screen PU and urinated soil (US) samples collected at festivals for illicit drug excretion products using hyphenated techniques; (2) to develop and validate a hydrophilic interaction liquid...... chromatography – mass spectrometry / mass spectrometry (HILIC-MS/MS) method of quantifying urinary targets of identified drugs in wastewater; and (3) to conduct a 24 h stability study, using PU and US to better reflect the chemical environment for targets in wastewater. Cocaine (COC) and ecstasy-like compounds....... The results suggest HMMA as analytical target for MDMA consumption in WBE, due to its stability in wastewater and its excretion as the main phase I metabolite of MDMA. Copyright © 2016 John Wiley & Sons, Ltd....

  5. A high-throughput microdialysis-parallel solid phase extraction-inductively coupled plasma mass spectrometry hyphenated system for continuous monitoring of extracellular metal ions in living rat brain.

    Science.gov (United States)

    Su, Cheng-Kuan; Hsia, Sheng-Chieh; Sun, Yuh-Chang

    2014-01-24

    To significantly improve the temporal resolving power of in vivo trace brain metal monitoring system, in this paper we describe a novel analytical configuration combining the dual functions of online segmentation of the rat brain microdialysate and parallel solid phase extraction (SPE) of multiple segmented samples. In contrast to traditional SPE procedures, in this study the three pumped media-the buffered rat brain microdialysate, the eluent, and the air stream-were converted to a series of segmented streams through the manipulation of a flow-through stream selector. After optimizing this online automatic MD/parallel poly(vinyl chloride) SPE/inductively coupled plasma mass spectrometry hyphenated system for the analysis of ultra-trace metal ions, the sample volume of the microdialysate was set at 0.83μL, the analytical sequence was repeatable every 20s, and the detection limits were in the range 0.03-0.24μgL(-1), with spike analyses of Mn, Co, Ni, Cu, and Zn in a rat brain ECF sample agreeing well with expected values (88-107%). To further examine the system's practicability, we also performed (i) in vivo dynamic monitoring of these trace metal ions in living rat brain extracellular fluid post-probe implantation (the basal values for Mn, Co, Ni, Cu, and Zn were 1.17±0.18, 1.27±0.36, 2.46±0.62, 0.86±0.37, and 2.35±0.55μgL(-1), respectively) and (ii) real-time visualization of the physiological response to acute neural depolarization elicited upon perfusing a high-K(+) medium through the MD probe. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Screening for illicit drugs in pooled human urine and urinated soil samples and studies on the stability of urinary excretion products of cocaine, MDMA, and MDEA in wastewater by hyphenated mass spectrometry techniques.

    Science.gov (United States)

    Mardal, Marie; Kinyua, Juliet; Ramin, Pedram; Miserez, Bram; Van Nuijs, Alexander L N; Covaci, Adrian; Meyer, Markus R

    2017-01-01

    Monitoring population drug use through wastewater-based epidemiology (WBE) is a useful method to quantitatively follow trends and estimate total drug consumption in communities. Concentrations of drug biomarkers might be low in wastewater due to dilution; and therefore analysis of pooled urine (PU) is useful to detect consumed drugs and identify targets of illicit drugs use. The aims of the study were (1) to screen PU and urinated soil (US) samples collected at festivals for illicit drug excretion products using hyphenated techniques; (2) to develop and validate a hydrophilic interaction liquid chromatography - mass spectrometry / mass spectrometry (HILIC-MS/MS) method of quantifying urinary targets of identified drugs in wastewater; and (3) to conduct a 24 h stability study, using PU and US to better reflect the chemical environment for targets in wastewater. Cocaine (COC) and ecstasy-like compounds were the most frequently detected illicit drugs; an analytical method was developed to quantify their excretion products. Hydroxymethoxymethamphetamine (HMMA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), HMMA sulfate (HMMA-S), benzoylecgonine (BE), and cocaethylene (CE) had 85-102% of initial concentration after 8 h of incubation, whereas COC and ecgonine methyl ester (EME) had 74 and 67% after 8 h, respectively. HMMA showed a net increase during 24 h of incubation (107% ± 27, n = 8), possibly due to the cleavage of HMMA conjugates, and biotransformation of MDMA. The results suggest HMMA as analytical target for MDMA consumption in WBE, due to its stability in wastewater and its excretion as the main phase I metabolite of MDMA. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  7. Comparison of hydrodynamically closed isotachophoresis-capillary zone electrophoresis with hydrodynamically open capillary zone electrophoresis hyphenated with tandem mass spectrometry in drug analysis: pheniramine, its metabolite and phenylephrine in human urine.

    Science.gov (United States)

    Piešťanský, Juraj; Maráková, Katarína; Kovaľ, Marián; Mikuš, Peter

    2014-09-05

    The advanced two dimensional isotachophoresis (ITP)-capillary zone electrophoresis (CZE) hyphenated with tandem mass spectrometry (MS/MS, here triple quadrupole, QqQ) was developed in this work to demonstrate analytical potentialities of this approach in the analysis of drugs in multicomponent ionic matrices. Pheniramine (PHM), phenylephrine (PHE), paracetamol (PCM) and their potential metabolic products were taken for the analysis by the ITP-CZE-ESI-QqQ technique working in hydrodynamically closed CE separation system and then a comparison with the conventional (hydrodynamically open) CZE-ESI-QqQ technique was made. The ITP-CZE-ESI-QqQ method was favorable in terms of obtainable selectivity (due to highly effective heart-cut analysis), concentration limits of detection (LOD at pgmL(-1) levels due to enhanced sample load capacity and ITP preconcentration), sample handling (on-line sample pretreatment, i.e. clean-up, preconcentration, preseparation), and, by that, possibilities for future automation and miniaturization. On the other hand, this experimental arrangement, in contrast to the CZE-ESI-QqQ arrangement supported by an electroosmotic flow, is principally limited to the analysis of uniformly (i.e. positively or negatively) charged analytes in one run without any possibilities to analyze neutral compounds (here, PCM and neutral or acidic metabolites of the drugs had to be excluded from the analysis). Hence, these general characteristics should be considered when choosing a proper analytical CE-MS approach for a given biomedical application. Here, the analytical potential of the ITP-CZE-ESI-QqQ method was demonstrated showing the real time profiles of excreted targeted drugs and metabolite (PHM, PHE, M-PHM) in human urine after the administration of one dose of Theraflu(®) to the volunteers. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Separation and preconcentration of ultratrace levels of cadmium(II) in a sequential injection (SI) system with a PTFE packed column as a mimic sequential injection lab-on-valve (SI-LOV) system with renewable column employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr

    of cadmium(II) by detection with electrothermal atomic absorption spectrometry (ETAAS). The non-charged complex formed between the analyste and the chelating reagent diethyldithiophosphate (DDPA) was selectively adsorbed on the surface of the PTFE beads and eluted by ethanol before being directed...

  9. Hyphenated hydrology: Interdisciplinary evolution of water resource science

    Science.gov (United States)

    McCurley, Kathryn L.; Jawitz, James W.

    2017-04-01

    Hydrology has advanced considerably as a scientific discipline since its recognized inception in the mid-twentieth century. Modern water resource related questions have forced adaptation from exclusively physical or engineering science viewpoints toward a deliberate interdisciplinary context. Over the past few decades, many of the eventual manifestations of this evolution were foreseen by prominent expert hydrologists. However, their narrative descriptions have lacked substantial quantification. This study addressed that gap by measuring the prevalence of and analyzing the relationships between the terms most frequently used by hydrologists to define and describe their research. We analyzed 16,591 journal article titles from 1965-2015 in Water Resources Research, through which the scientific dialogue and its time-sensitive progression emerged. Our word frequency and term cooccurrence network results revealed the dynamic timing of the lateral movement of hydrology across multiple disciplines as well as the deepening of scientific discourse with respect to traditional hydrologic questions. The conversation among water resource scientists surrounding the hydrologic subdisciplines of catchment-hydrology, hydro-meteorology, socio-hydrology, hydro-climatology, and eco-hydrology gained statistically significant momentum in the analyzed time period, while that of hydro-geology and contaminant-hydrology experienced periods of increase followed by significant decline. This study concludes that formerly exotic disciplines can potentially modify hydrology, prompting new insights and inspiring unconventional perspectives on old questions that may have otherwise become obsolete.

  10. Hyphenated hydrology: Multidisciplinary evolution of water resource science

    Science.gov (United States)

    McCurley, K. 4553; Jawitz, J. W.

    2016-12-01

    Hydrology has advanced considerably as a scientific discipline since its recognized inception in the mid-20th century. While hydrology may have evolved from the singular viewpoint of a more rigid physical or engineering science, modern water resource related questions have forced adaptation toward a deliberate interdisciplinary context. Over the past few decades, many of the eventual manifestations of this evolution have been foreseen by prominent expert hydrologists, though their narrative descriptions were not substantially quantified. This study addresses that gap by directly measuring and inspecting the words that hydrologists use to define and describe their research endeavors. We analyzed 16,591 journal article titles from 1965-2015 in Water Resources Research, through which the scientific dialogue and its time-sensitive progression emerges. Word frequency and term concurrence reveal the dynamic timing of the lateral movement of hydrology across multiple disciplines and a deepening of scientific discourse with respect to traditional hydrologic questions. This study concludes that formerly exotic disciplines are increasingly modifying hydrology, prompting new insights as well as inspiring unconventional perspectives on old questions.

  11. Automated method for simultaneous lead and strontium isotopic analysis applied to rainwater samples and airborne particulate filters (PM10).

    Science.gov (United States)

    Beltrán, Blanca; Avivar, Jessica; Mola, Montserrat; Ferrer, Laura; Cerdà, Víctor; Leal, Luz O

    2013-09-03

    A new automated, sensitive, and fast system for the simultaneous online isolation and preconcentration of lead and strontium by sorption on a microcolumn packed with Sr-resin using an inductively coupled plasma mass spectrometry (ICP-MS) detector was developed, hyphenating lab-on-valve (LOV) and multisyringe flow injection analysis (MSFIA). Pb and Sr are directly retained on the sorbent column and eluted with a solution of 0.05 mol L(-1) ammonium oxalate. The detection limits achieved were 0.04 ng for lead and 0.03 ng for strontium. Mass calibration curves were used since the proposed system allows the use of different sample volumes for preconcentration. Mass linear working ranges were between 0.13 and 50 ng and 0.1 and 50 ng for lead and strontium, respectively. The repeatability of the method, expressed as RSD, was 2.1% and 2.7% for Pb and Sr, respectively. Environmental samples such as rainwater and airborne particulate (PM10) filters as well as a certified reference material SLRS-4 (river water) were satisfactorily analyzed obtaining recoveries between 90 and 110% for both elements. The main features of the LOV-MSFIA-ICP-MS system proposed are the capability to renew solid phase extraction at will in a fully automated way, the remarkable stability of the column which can be reused up to 160 times, and the potential to perform isotopic analysis.

  12. NMR-based metabolomics and hyphenated NMR techniques – a perfect match in natural products research

    DEFF Research Database (Denmark)

    Vinther, Joachim Møllesøe; Wubshet, Sileshi Gizachew; Stærk, Dan

    2015-01-01

    Ethnopharmacology is one of the world’s fastest-growing scientific disciplines encompassing a diverse range of subjects. It links natural sciences research on medicinal, aromatic and toxic plants with socio-cultural studies and has often been associated with the development of new drugs...

  13. Bacterial-Fungal Interactions: Hyphens between Agricultural, Clinical, Environmental, and Food Microbiologists

    Science.gov (United States)

    Frey-Klett, P.; Burlinson, P.; Deveau, A.; Barret, M.; Tarkka, M.; Sarniguet, A.

    2011-01-01

    Summary: Bacteria and fungi can form a range of physical associations that depend on various modes of molecular communication for their development and functioning. These bacterial-fungal interactions often result in changes to the pathogenicity or the nutritional influence of one or both partners toward plants or animals (including humans). They can also result in unique contributions to biogeochemical cycles and biotechnological processes. Thus, the interactions between bacteria and fungi are of central importance to numerous biological questions in agriculture, forestry, environmental science, food production, and medicine. Here we present a structured review of bacterial-fungal interactions, illustrated by examples sourced from many diverse scientific fields. We consider the general and specific properties of these interactions, providing a global perspective across this emerging multidisciplinary research area. We show that in many cases, parallels can be drawn between different scenarios in which bacterial-fungal interactions are important. Finally, we discuss how new avenues of investigation may enhance our ability to combat, manipulate, or exploit bacterial-fungal complexes for the economic and practical benefit of humanity as well as reshape our current understanding of bacterial and fungal ecology. PMID:22126995

  14. Four new degradation products of doxorubicin: An application of forced degradation study and hyphenated chromatographic techniques

    Directory of Open Access Journals (Sweden)

    Dheeraj Kaushik

    2015-10-01

    Full Text Available Forced degradation study on doxorubicin (DOX was carried out under hydrolytic condition in acidic, alkaline and neutral media at varied temperatures, as well as under peroxide, thermal and photolytic conditions in accordance with International Conference on Harmonization (ICH guidelines Q1(R2. It was found extremely unstable to alkaline hydrolysis even at room temperature, unstable to acid hydrolysis at 80 °C, and to oxidation at room temperature. It degraded to four products (O-I–O-IV in oxidative condition, and to single product (A-I in acid hydrolytic condition. These products were resolved on a C8 (150 mm×4.6 mm, 5 µm column with isocratic elution using mobile phase consisting of HCOONH4 (10 mM, pH 2.5, acetonitrile and methanol (65:15:20, v/v/v. Liquid chromatography–photodiode array (LC–PDA technique was used to ascertain the purity of the products noted in LC–UV chromatogram. For their characterization, a six stage mass fragmentation (MS6 pattern of DOX was outlined through mass spectral studies in positive mode of electrospray ionization (+ESI as well as through accurate mass spectral data of DOX and the products generated through liquid chromatography–time of flight mass spectrometry (LC–MS–TOF on degraded drug solutions. Based on it, O-I–O-IV were characterized as 3-hydroxy-9-desacetyldoxorubicin-9-hydroperoxide, 1-hydroxy-9-desacetyldoxorubicin-9-hydroperoxide, 9-desacetyldoxorubicin-9-hydroperoxide and 9-desacetyldoxorubicin, respectively, whereas A-I was characterized as deglucosaminyl doxorubicin. While A-I was found to be a pharmacopoeial impurity, all oxidative products were found to be new degradation impurities. The mechanisms and pathways of degradation of doxorubicin were outlined and discussed. Keywords: Doxorubicin, TOF, Forced degradation, Liquid chromatography, Degradation product, Mass fragmentation pattern

  15. Hybrid Spaces and Hyphenated Musicians: Secondary Students' Musical Engagement in a Songwriting and Technology Course

    Science.gov (United States)

    Tobias, Evan S.

    2012-01-01

    This case study investigates how secondary students (three individuals and three groups) engaged with music and acted as musicians in a Songwriting and Technology Class (STC), a course involving the creation, performance, recording and production of original music with instruments and music technology. The following research question guided the…

  16. Stability constants determination of successive metal complexes by hyphenated CE-ICPMS.

    Science.gov (United States)

    Petit, Jeremy; Aupiais, Jean; Topin, Sylvain; Geertsen, Valérie; Beaucaire, Catherine; Stambouli, Moncef

    2010-01-01

    The study of radionuclides speciation requires accurate evaluation of stability constants, which can be achieved by CE-ICPMS. We have previously described a method for 1:1 metal complexes stability constants determination. In this paper, we present its extension to the case of successive complexations and its application to uranyl-oxalate and lanthanum-oxalate systems. Several significant steps are discussed: analytical conditions choice, mathematical treatment by non-linear regression, ligand concentration and ionic strength corrections. The following values were obtained: at infinite dilution, log(beta(1) degrees (UO(2)Oxa))=6.93+/-0.05, log(beta(2) degrees (UO(2)(Oxa)(2) (2-)))=11.92+/-0.43 and log(beta(3) degrees (UO(2)(Oxa)(3) (4-)))=15.11+/-0.12; log(beta(1) degrees (LaOxa(+)))=5.90+/-0.07, log(beta(2) degrees (La(Oxa)(2) (-)))=9.18+/-0.19 and log(beta(3) degrees (La(Oxa)(3) (3-)))=9.81+/-0.33. These values are in good agreement with the literature data, even though we suggest the existence of a new lanthanum-oxalate complex: La(Oxa)(3) (3-). This study confirms the suitability of CE-ICPMS for complexation studies.

  17. Latin@ Advocacy in the Hyphen: Faculty Identity and Commitment in a Hispanic-Serving Institution

    Science.gov (United States)

    Murakami-Ramalho, Elizabeth; Nunez, Anne-Marie; Cuero, Kimberley K.

    2010-01-01

    This study examines our experiences as female junior scholars with multicultural backgrounds teaching at the same Hispanic-serving institution. As education scholars with mixed-heritage families, we identify with the commitment to serving Latinos and the number of mixed-heritage people in the USA. The election of Barack Obama, whose racial…

  18. Analysis of xanthines in beverages using a fully automated SPE-SPC-DAD hyphenated system

    Energy Technology Data Exchange (ETDEWEB)

    Medvedovici, A. [Bucarest Univ., Bucarest (Romania). Faculty of Chemistry, Dept. of Analytical Chemistry; David, F.; David, V.; Sandra, P. [Research Institute of Chromatography, Kortrijk (Belgium)

    2000-08-01

    Analysis of some xanthines (caffeine, theophylline and theobromine) in beverages has been achieved by a fully automated on-line Solid Phase Extraction - Supercritical Fluid Chromatography - Diode Array Detection (Spe - Sofc - Dad). Three adsorbents have been tested for the Spe procedure: octadecyl modified silicagel (ODS) and two types of styrene-divinylbenzen copolymer based materials, from which Porapack proved to be the most suitable adsorbent. Optimisation and correlation of both Spe and Sofc operational parameters are also discussed. By this technique, caffeine was determined in ice tea and Coca-Cola in a concentration of 0.15 ppm, theobromine - 1.5 ppb, and theophylline - 0.15 ppb. [Italian] Si e' realizzata l'analis di alcune xantine (caffeina, teofillina e teobromina) mediante un sistema, in linea, completamente automatizzato basato su Estrazione in Fase Solida - Cromatografia in Fase Supercritica - Rivelazione con Diode Array (Spe - Sfc - Dad). Per la procedura Spe sono stati valutati tre substrati: silice ottadecilica (ODS) e due tipi di materiali polimerici a base stirene-divinilbenzene, di cui, quello denominato PRP-1, e' risultato essere il piu' efficiente. Sono discusse sia l'ottimizzazione che la correlazione dei parametri operazionali per la Spe e la Sfc. Con questa tecnica sono state determinate, in te' ghiacciato e Coca-Cola, la caffeina, la teobromina e la teofillina alle concentrazini di 0.15, 1.5 e 0.15 ppm.

  19. Prototype of an Interface for Hyphenating Distillation with Gas Chromatography and Mass Spectrometry

    Science.gov (United States)

    Tang, Ya-Ru; Yang, Hui-Hsien; Urban, Pawel L.

    2017-01-01

    Chemical analysis of complex matrices—containing hundreds of compounds—is challenging. Two-dimensional separation techniques provide an efficient way to reduce complexity of mixtures analyzed by mass spectrometry (MS). For example, gasoline is a mixture of numerous compounds, which can be fractionated by distillation techniques. However, coupling conventional distillation with other separations as well as MS is not straightforward. We have established an automatic system for online coupling of simple microscale distillation with gas chromatography (GC) and electron ionization MS. The developed system incorporates an interface between the distillation condenser and the injector of a fused silica capillary GC column. Development of this multidimensional separation (distillation-GC-MS) was preceded by a series of preliminary off-line experiments. In the developed technique, the components with different boiling points are fractionated and instantly analyzed by GC-MS. The obtained data sets illustrate dynamics of the distillation process. An important advantage of the distillation-GC-MS technique is that raw samples can directly be analyzed without removal of the non-volatile matrix residues that could contaminate the GC injection port and the column. Distilling the samples immediately before the injection to the GC column may reduce possible matrix effects—especially in the early phase of separation, when molecules with different volatilities co-migrate. It can also reduce losses of highly volatile components (during fraction collection and transfer). The two separation steps are partly orthogonal, what can slightly increase selectivity of the entire analysis. PMID:28337400

  20. Advances in field-flow fractionation for the analysis of biomolecules: instrument design and hyphenation.

    Science.gov (United States)

    Schachermeyer, Samantha; Ashby, Jonathan; Zhong, Wenwan

    2012-09-01

    Field-flow fractionation (FFF) separates analytes by use of an axial channel-flow and a cross-field. Its soft separation capability makes it an ideal tool for initial fractionation of complex mixtures, but large elution volumes and high flow rates have limited its applicability without significant user handling. Recent advances in instrumentation and miniaturization have successfully reduced channel size and elution speed, and thus the volume of each fraction, making it possible to conveniently couple FFF with orthogonal separation techniques for improved resolution. More detailed analysis can also be performed on the fractions generated by FFF by use of diverse analytical techniques, including MS, NMR, and even X-ray scattering. These developmental trends have given FFF more power in the analysis of different types of molecule, and will be the direction of choice for further advances in FFF technology.

  1. Solvent exchange module for LC-NMR hyphenation using machine vision-controlled droplet evaporation

    NARCIS (Netherlands)

    Schoonen, J.W.; Vulto, P.; Roo, de N.; Duynhoven, van J.P.M.; Linden, van der H.; Hankemeier, T.

    2013-01-01

    We report the use of pendant droplet evaporation for exchange of eluents for 1H nuclear magnetic resonance (1H NMR) purposes. Analytes are fed and retained in 500 nL droplets, which are concentrated by evaporation and subsequently redissolved in deuterated solvent. Droplet size is monitored by

  2. Capillary electrophoresis hyphenated with UV-native-laser induced fluorescence detection (CE/UV-native-LIF).

    Science.gov (United States)

    Couderc, François; Ong-Meang, Varravaddheay; Poinsot, Véréna

    2017-01-01

    Native laser-induced fluorescence using UV lasers associated to CE offers now a large related literature, for now 30 years. The main works have been performed using very expensive Ar-ion lasers emitting at 257 and 275 nm. They are not affordable for routine analyses, but have numerous applications such as protein, catecholamine, and indolamine analysis. Some other lasers such as HeCd 325 nm have been used but only for few applications. Diode lasers, emitting at 266 nm, cheaper, are extensively used for the same topics, even if the obtained sensitivity is lower than the one observed using the costly UV-Ar-ion lasers. This review presents various CE or microchips applications and different UV lasers used for the excitation of native fluorescence. We showed that CE/Native UV laser induced fluorescence detection is very sensitive for detection as well as small aromatic biomolecules than proteins containing Trp and Tyr amino acids. Moreover, it is a simple way to analyze biomolecules without derivatization. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Living GenoChemetics by hyphenating synthetic biology and synthetic chemistry in vivo.

    Science.gov (United States)

    Sharma, Sunil V; Tong, Xiaoxue; Pubill-Ulldemolins, Cristina; Cartmell, Christopher; Bogosyan, Emma J A; Rackham, Emma J; Marelli, Enrico; Hamed, Refaat B; Goss, Rebecca J M

    2017-08-09

    Marrying synthetic biology with synthetic chemistry provides a powerful approach toward natural product diversification, combining the best of both worlds: expediency and synthetic capability of biogenic pathways and chemical diversity enabled by organic synthesis. Biosynthetic pathway engineering can be employed to insert a chemically orthogonal tag into a complex natural scaffold affording the possibility of site-selective modification without employing protecting group strategies. Here we show that, by installing a sufficiently reactive handle (e.g., a C-Br bond) and developing compatible mild aqueous chemistries, synchronous biosynthesis of the tagged metabolite and its subsequent chemical modification in living culture can be achieved. This approach can potentially enable many new applications: for example, assay of directed evolution of enzymes catalyzing halo-metabolite biosynthesis in living cells or generating and following the fate of tagged metabolites and biomolecules in living systems. We report synthetic biological access to new-to-nature bromo-metabolites and the concomitant biorthogonal cross-coupling of halo-metabolites in living cultures.Coupling synthetic biology and chemical reactions in cells is a challenging task. The authors engineer bacteria capable of generating bromo-metabolites, develop a mild Suzuki-Miyaura cross-coupling reaction compatible with cell growth and carry out the cross-coupling chemistry in live cell cultures.

  4. Determination of iodide in samples with complex matrices by hyphenation of capillary isotachophoresis and zone electrophoresis

    Czech Academy of Sciences Publication Activity Database

    Pantůčková, Pavla; Urbánek, Marek; Křivánková, Ludmila

    2007-01-01

    Roč. 28, č. 20 (2007), s. 3777-3785 ISSN 0173-0835 R&D Projects: GA ČR GA203/05/2106; GA AV ČR IAA400310703; GA AV ČR IAA400310609 Institutional research plan: CEZ:AV0Z40310501 Keywords : serum * urine * seawater Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.609, year: 2007

  5. Hyphenated chromatographic techniques for the rapid screening and identification of antioxidants in methanolic extracts of pharmaceutically used plants .

    NARCIS (Netherlands)

    Exarchou, V.; Fiamegos, Y.C.; Beek, van T.A.; Nanos, C.G.; Vervoort, J.J.M.

    2006-01-01

    Phytochemical analysis is an important scientific research area, which normally relies on a number of rather laborious and time-consuming techniques for compound identification. Isolation of the ingredients of plant extracts in adequate quantities for spectral and biological analysis was the basis

  6. Characterization of volatile and polar compounds of Jiaogulan Tea [Gynostemma pentaphyllum (Thunb.) Makino] by hyphenated analytical techniques

    Science.gov (United States)

    Jiaogulan [Gynostemma pentaphyllum (Thunb.) Makino] is a Chinese medical plant from southern Asia that has rapidly gained popularity and interest for its health-promotive and therapeutic properties. The volatile composition of jiaogulan tea was analyzed by using headspace-solid phase microextraction...

  7. Tuneable surface enhanced Raman spectroscopy hyphenated to chemically derivatized thin-layer chromatography plates for screening histamine in fish.

    Science.gov (United States)

    Xie, Zhengjun; Wang, Yang; Chen, Yisheng; Xu, Xueming; Jin, Zhengyu; Ding, Yunlian; Yang, Na; Wu, Fengfeng

    2017-09-01

    Reliable screening of histamine in fish was of urgent importance for food safety. This work presented a highly selective surface enhanced Raman spectroscopy (SERS) method mediated by thin-layer chromatography (TLC), which was tailored for identification and quantitation of histamine. Following separation and derivatization with fluram, plates were assayed with SERS, jointly using silver nanoparticle and NaCl. The latter dramatically suppressed the masking effect caused by excessive fluram throughout the plate, thus offering clear baseline and intensive Raman fingerprints specific to the analyte. Under optimized conditions, the usability of this method was validated by identifying the structural fingerprints of both targeted and unknown compounds in fish samples. Meanwhile, the quantitative results of this method agreed with those by an HPLC method officially suggested by EU for histamine determination. Showing remarkable cost-efficiency and user-friendliness, this facile TLC-SERS method was indeed screening-oriented and may be more attractive to controlling laboratories of limited resource. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Dual-Stage Consumable-Free Thermal Modulator for the Hyphenation of Thermal Analysis, Gas Chromatography, and Mass Spectrometry.

    Science.gov (United States)

    Wohlfahrt, Sebastian; Fischer, Michael; Varga, Janos; Saraji-Bozorgzad, Mohammad-Reza; Matuschek, Georg; Denner, Thomas; Zimmermann, Ralf

    2016-01-05

    The design of the so-called "Peltier modulator" is presented. It is a new dual-stage consumable-free thermal modulator for thermal analysis-gas chromatography-mass spectrometry (TA-GC-MS). It requires only electrical power for operation as it facilitates thermo-electric coolers instead of cryogenics for trapping and resistive on-column heating for reinjection. Trapping and desorption temperatures as well as modulation cycles are freely adjustable. The stationary phase for the trapping region can be selected to suit the specific application, since common fused silica capillary is used. The Peltier modulator's performance is demonstrated with a broad range of different standard substances and with heavy crude oil as a complex real life sample. Successful modulation from n-pentane to pyrene (boiling points = 36/394 °C) is presented. The produced peaks show the narrowest bandwidths ever reported for a consumable-free thermal modulator, i.e., 12.8 ± 1.2 ms for n-pentadecane. The Peltier modulator is rugged, cost-effective, requires low maintenance, and decreases security issues significantly, compared to commercial available solutions using liquid N2/CO2.

  9. Analysis of European oak bark beetle (.I.Scolytus intricatus./I.) extracts using hyphenated and chiral chromatography techniques

    Czech Academy of Sciences Publication Activity Database

    Vrkočová, Pavlína; Kalinová, Blanka; Valterová, Irena; Koutek, Bohumír

    2003-01-01

    Roč. 59, - (2003), s. 107-114 ISSN 0039-9140 R&D Projects: GA ČR GA203/00/0219; GA MŠk OC E16.10 Institutional research plan: CEZ:AV0Z4055905 Keywords : GC-EAD * .I.Scolytus intricatus./I. Subject RIV: GF - Plant Pathology, Vermin, Weed, Plant Protection Impact factor: 2.091, year: 2003

  10. A Hyphenation of Stripping Voltammetry with Electrospray Ionization Mass Spectrometry; an Effect of Sodium Perchlorate on Ferrocene Oxidation

    Czech Academy of Sciences Publication Activity Database

    Jaklová Dytrtová, Jana; Jakl, M.; Navrátil, Tomáš; Schröder, Detlef

    2013-01-01

    Roč. 8, č. 2 (2013), s. 1623-1634 ISSN 1452-3981 R&D Projects: GA ČR GAP206/11/1638 Institutional support: RVO:61388963 ; RVO:61388955 Keywords : ESI-MS * anodic stripping voltammetry * electrochemistry * ferrocene * ferricene * base electrolyte Subject RIV: CG - Electrochemistry Impact factor: 1.956, year: 2013

  11. In situ generation of copper cations and complexation with tebuconazole in a hyphenation of electrochemistry with mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Jaklová Dytrtová, Jana; Jakl, M.; Schröder, Detlef; Norková, Renáta

    2013-01-01

    Roč. 338, 15 MAR (2013), s. 45-49 ISSN 1387-3806 R&D Projects: GA ČR GP13-21409P Institutional support: RVO:61388963 Keywords : electrochemical ion generation * ESI-MS * coupling * fungicide * tebuconazole * soil solution Subject RIV: CG - Electrochemistry Impact factor: 2.227, year: 2013

  12. Symbols of Hyphenated Identity Drawing Maps (IDM) for Arab and Jewish Students at the University of Haifa

    Science.gov (United States)

    Hertz-Lazarowitz, Rachel; Farah, Abeer; Zelniker, Tamar

    2013-01-01

    In 2008, we conducted a large scale study following our methodology developed for the analysis of drawings to assess identity (Hertz-Lazarowitz, Farah & Yosef-Meitav, 2012). We gathered interviews and asked for Identity Drawing Maps (IDM) from 184 students aged from 20-30 years. The symbols in the drawings were grouped in five categories:…

  13. Sustainability Study on Heavy Metal Uptake in Neem Biodiesel Using Selective Catalytic Preparation and Hyphenated Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Mirella Elkadi

    2014-04-01

    Full Text Available It is common knowledge that the presence of trace metals in biofuels can be detrimental to the environment and long-term sustainable development. This study provides an insight into selective catalytic preparation of biofuel to compare uptake of trace metals in the biodiesel fraction with preferential base catalysts. The role of specific metal hydroxides in controlling trace metal content in biofuel production is relatively unexplored, and the effect of different homogeneous catalysts (NaOH, KOH on metal retention in biodiesel from commercial neem oil was examined. A detailed study of this nature of catalyst vs. metal uptake is in the interest of sustainable living and could make a significant contribution to biofuels research. Both catalysts displayed variable uptake for certain toxic elements, which was attributed to the behavior of the catalyst in the reaction mixture. A general comparison reflected specific trends in metal retention (ICP-MS with the use of different base catalysts. Challenges encountered by extending the study and using a heterogeneous catalyst (CaO are presented. Our work could play a significant role in influencing catalyzed transesterfication processes to control elemental and toxic metal uptake in biofuels. The impact of our work on sustainable living is presented.

  14. Hyphenation of a near-infrared Echelle spectrometer to a microplasma for element-selective detection in gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Cziesla, K.; Otto, M. [Inst. of Analytical Chemistry, Freiberg University of Mining and Technology (Germany); Platzer, B. [Graz Univ. of Technology, Dept. of Analytical Chemistry (Austria); Okruss, M. [Gesellschaft zur Foerderung angewandter Optik, Optoelektronik, Quantenelektronik und Spektroskopie (GOS) e.V., Berlin (Germany); Florek, S. [Inst. of Spectrochemistry and Applied Spectroscopy, Institutsteil Berlin (Germany)

    2001-12-01

    The coupling of a near-infrared Echelle spectrometer (NIRES) with a gas chromatograph for element-selective detection is introduced. The miniaturized capacitive plasma device is operated at a frequency of 40.68 MHz and is mounted directly on an Hewlett-Packard HP6890 GC. First results with a mixture of halogenated standard compounds are presented and discussed in terms of the advantages and problems with this system. (orig.)

  15. Hyphenating the curtius rearrangement with Morita-Baylis-Hillman adducts: synthesis of biologically active acyloins and vicinal aminoalcohols

    Energy Technology Data Exchange (ETDEWEB)

    Amarante, Giovanni W.; Cavallaro, Mayra; Coelho, Fernando, E-mail: coelho@iqm.unicamp.b [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Quimica. Lab. de Sintese de Produtos Naturais e Farmacos

    2011-07-01

    Using Morita-Baylis-Hillman adducts as substrates, the Curtius rearrangement was performed in a sequence that allowed the synthesis of several hydroxy-ketones (acyloins) with great structural diversity and in good overall yields. These acyloins in turn were easily transformed into 1,2-anti aminoalcohols through a highly diastereoselective reductive amination step. The synthetic utility of these approaches was exemplified by performing the syntheses of (+-)-bupropion, a drug used to treat the abstinence syndrome of smoker and (+-)-spisulosine, a potent anti-tumoral compound originally isolated from a marine source. (author)

  16. Trends and perspectives of flow injection/sequential injection on-line sample-pretreatment schemes coupled to ETAAS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2005-01-01

    Flow injection (FI) analysis, the first generation of this technique, became in the 1990s supplemented by its second generation, sequential injection (SI), and most recently by the third generation (i.e.,Lab-on-Valve). The dominant role played by FI in automatic, on-line, sample pretreatments in ...

  17. On-line dynamic extraction system hyphenated to inductively coupled plasma optical emission spectrometry for automatic determination of oral bioaccessible trace metal fractions in airborne particulate matter.

    Science.gov (United States)

    Mohr, Victoria; Miró, Manuel; Limbeck, Andreas

    2017-04-01

    For a realistic evaluation of the potential hazard emanating from airborne particulate matter (APM), the determination of the total inhaled metal amounts associated with APM is insufficient in risk assessment. Additional information about metal fractions that can be mobilized by the human body is necessary, because only those soluble (also called bioaccessible) fractions can be absorbed by the human body, and thus potentially cause adverse health effects. In the present study, a dynamic flow-through approach as a front end to inductively coupled plasma optical emission spectrometry (ICP-OES) exploiting advanced flow analysis is employed for on-line handling of multiple APM samples and determination of bioaccessible trace metals under worst case extraction scenarios. The method is based on on-line continuous extraction of filter samples with synthetic gastric fluid followed by on-line ICP-OES measurement of the dissolved fraction of trace metals. The assembly permits an automated successive measurement of three sample replicates in less than 19 min. The on-line extraction procedure offers increased sample throughput and reduced risk of sample contamination and overcomes metal re-adsorption processes compared to the traditional batch-wise counterparts. Furthermore, it provides deeper information on the kinetics of the leaching process. The developed procedure was applied to the determination of bioaccessible metal fractions (Al, Ba, Cu, Fe and Mn as model analytes) in PM10 samples from Palma de Mallorca (Spain) and Vienna (Austria). Graphical Abstract On-line gastric bioaccessibility of elements in airborne particulate matter.

  18. Hyphenating size-exclusion chromatography with electrospray mass spectrometry; using on-line liquid-liquid extraction to study the lipid composition of lipoprotein particles.

    Science.gov (United States)

    Osei, Michael; Griffin, Julian L; Koulman, Albert

    2015-11-15

    Lipoproteins belong to the most commonly measured clinical biochemical parameters. Lipidomics is an orthogonal approach and aims to profile the individual lipid molecules that jointly form the lipoprotein particles. However, in the first step of the extraction of lipid molecules from serum, an organic solvent is used leading to dissociation of the lipoproteins. Thus far it has been impossible to combine lipidomics and lipoprotein analysis in one analytical system. Human plasma was diluted in phosphate-buffered saline (PBS) and injected onto a Superose 6 PC 3.2 column with PBS as a mobile phase to separate lipoproteins. The eluent was led to a Syrris FLLEX module, which also received CHCl3 /MeOH (3:1). The two phases were mixed and subsequently separated using a Teflon membrane in an especially designed pressurized flow chamber. The organic phase was led to a standard electrospray source of an Orbitrap mass spectrometer. Size-exclusion chromatography (SEC) has been commonly applied to separate lipoproteins and is considered a practical alternative to ultracentrifugation. Through the on-line liquid-liquid extraction method it becomes possible to obtained detailed mass spectra of lipids across different lipoprotein fractions. The extracted ion chromatograms of specific lipid signals showed their distribution against the size of lipoprotein particles. The application of on-line liquid-liquid extraction allows for the continuous electrospray-based mass spectral analysis of SEC eluent, providing the detailed lipid composition of lipoprotein particles separated by size. This approach provides new possibilities for the study of the biochemistry of lipoproteins. © 2015 The Authors. Rapid Communications in Mass Spectrometry Published by John Wiley & Sons Ltd.

  19. Arsenic speciation based on ion exchange high-performance liquid chromatography hyphenated with hydride generation atomic fluorescence and on-line UV photo oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Bin He; Jiang Gui-bin; Xu Xiao-bai [Chinese Academy of Scinces, Beijing (China). Research Center for Eco-Environmental Sciences

    2000-12-01

    An on-line method capable of the separation of arsenic species was developed for the speciation of arsenite As(III), arsenate As(V), monomethylarsenic (MMA) and dimethylarsenic acid (DMA) in biological samples. The method is based on the combination of high-performance liquid chromatograph (HPLC) for separation, UV photo oxidation for sample digestion and hydride generation atomic fluorescence spectrometry (HGAFS) for sensitive detection. The best separation results were obtained with an anion-exchange AS11 column protected by an AG11 guard column, and gradient elution with NaH{sub 2}PO{sub 4} and water as mobile phase. The on-line UV photo oxidation with 1.5% K{sub 2}S{sub 2}O{sub 8} in 0.2 mol L{sup -1} NaOH in an 8 m PTFE coil for 40 s ensures the digestion of organoarsenic compounds. Detection limits for the four species were in the range of 0.11-0.15 ng (20 {mu}L injected). Procedures were validated by analysis of the certified reference materials GBW09103 freeze-dried human urine and the results were in good agreement with the certified values of total arsenic concentration. The method has been successfully applied to speciation studies of blood arsenic species with no need of sample pretreatment. Speciation of arsenic in blood samples collected from two patients after the ingestion of realgar-containing drug reveals slight increase of arsenite and DMA, resulting from the digestion of realgar. (orig.)

  20. Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry-A review

    Energy Technology Data Exchange (ETDEWEB)

    Popp, Maximilian [Department of Chemistry, Division of Analytical Chemistry, University of Natural Resources and Applied Life Sciences, BOKU Vienna, Muthgasse 18, A-1190 Vienna (Austria); Hann, Stephan [Department of Chemistry, Division of Analytical Chemistry, University of Natural Resources and Applied Life Sciences, BOKU Vienna, Muthgasse 18, A-1190 Vienna (Austria); Koellensperger, Gunda, E-mail: Gunda.Koellensperger@boku.ac.at [Department of Chemistry, Division of Analytical Chemistry, University of Natural Resources and Applied Life Sciences, BOKU Vienna, Muthgasse 18, A-1190 Vienna (Austria)

    2010-06-04

    In recent years the number of environmental applications of elemental speciation analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. The analytical characteristics, such as extremely low detection limits (LOD) for almost all elements, the wide linear range, the possibility for multi-elemental analysis and the possibility to apply isotope dilution mass spectrometry (IDMS) make ICP-MS an attractive tool for elemental speciation analysis. Two methodological approaches, i.e. the combination of ICP-MS with high performance liquid chromatography (HPLC) and gas chromatography (GC), dominate the field. Besides the investigation of metals and metalloids and their species (e.g. Sn, Hg, As), representing 'classic' elements in environmental science, more recently other elements (e.g. P, S, Br, I) amenable to ICP-MS determination were addressed. In addition, the introduction of isotope dilution analysis and the development of isotopically labeled species-specific standards have contributed to the success of ICP-MS in the field. The aim of this review is to summarize these developments and to highlight recent trends in the environmental application of ICP-MS coupled to GC and HPLC.

  1. Alkaloids Profiling of Fumaria capreolata by Analytical Platforms Based on the Hyphenation of Gas Chromatography and Liquid Chromatography with Quadrupole-Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    María del Mar Contreras

    2017-01-01

    Full Text Available Two analytical platforms, gas chromatography (GC coupled to quadrupole-time-of-flight (QTOF mass spectrometry (MS and reversed-phase ultrahigh performance liquid chromatography (UHPLC coupled to diode array (DAD and QTOF detection, were applied in order to study the alkaloid profile of Fumaria capreolata. The use of these mass analyzers enabled tentatively identifying the alkaloids by matching their accurate mass signals and suggested molecular formulae with those previously reported in libraries and databases. Moreover, the proposed structures were corroborated by studying their fragmentation pattern obtained by both platforms. In this way, 8 and 26 isoquinoline alkaloids were characterized using GC-QTOF-MS and RP-UHPLC-DAD-QTOF-MS, respectively, and they belonged to the following subclasses: protoberberine, protopine, aporphine, benzophenanthridine, spirobenzylisoquinoline, morphinandienone, and benzylisoquinoline. Moreover, the latter analytical method was selected to determine at 280 nm the concentration of protopine (9.6 ± 0.7 mg/g, a potential active compound of the extract. In conclusion, although GC-MS has been commonly used for the analysis of this type of phytochemicals, RP-UHPLC-DAD-QTOF-MS provided essential complementary information. This analytical method can be applied for the quality control of phytopharmaceuticals containing Fumaria extracts currently found in the market.

  2. Development of a triple hyphenated HPLC-radical scavenging detection-DAD-SPE-NMR system for the rapid identification of antioxidants in complex plant extracts

    NARCIS (Netherlands)

    Pukalskas, A.; Beek, van T.A.; Waard, de P.

    2005-01-01

    A rapid method for the simultaneous detection and identification of radical scavenging compounds in plant extracts was developed by combining an HPLC with on-line radical scavenging using DPPH as a model radical and an HPLC¿DAD¿SPE¿NMR system. Using this method a commercial rosemary extract was

  3. Separation and determination of seleno amino acids using gas chromatography hyphenated with inductively coupled plasma mass spectrometry after hollow fiber liquid phase microextraction.

    Science.gov (United States)

    Duan, Jiankun; Hu, Bin

    2009-05-01

    A new derivatization-extraction method for preconcentration of seleno amino acids using hollow fiber liquid phase microextraction (HF-LPME) was developed for the separation and determination of seleno amino acids in biological samples by gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS). Derivatization was performed with ethyl chloroformate (ECF) to improve the volatility of seleno amino acids. Parameters influencing microextraction, including extraction solvent, pH of sample solution, extraction time, stirring speed, and inorganic salt concentration have been investigated. Under the optimal conditions, the limits of detection (LODs) obtained for Se-methyl-selenocysteine (SeMeCys), selenomethionine (SeMet), and selenoethionine (SeEth) were 23, 15, and 11 ng Se l(-1), respectively. The relative standard deviations (RSDs) were 14.6%, 16.4%, and 19.4% for SeMeCys, SeMet, and SeEth (c = 1.0 ng ml(-1), n = 7), respectively, and the RSDs for SeMeCys, SeMet could be improved obviously if SeEth was utilized as the internal standard. The proposed method was applied for the determination of seleno amino acids in extracts of garlic, cabbage, and mushroom samples, and the recoveries for the spiked samples were in the range of 96.8-108% and 93.4-115% with and without the use of SeEth as internal standard. The developed method was also applied to the analysis of SeMet in a certified reference material of SELM-1 yeast and the determined value is in good agreement with the certified value. 2008 John Wiley & Sons, Ltd.

  4. Analytical developments for the determination of monomethylmercury complexes with low molecular mass thiols by reverse phase liquid chromatography hyphenated to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Bouchet, Sylvain; Björn, Erik

    2014-04-25

    The behavior of monomethylmercury (MMHg) is markedly influenced by its distribution among complexes with low molecular mass (LMM) thiols but analytical methodologies dedicated to measure such complexes are very scarce up to date. In this work, we selected 15 LMM thiols often encountered in living organisms and/or in the environment and evaluated the separation of the 15 corresponding MMHg-thiol complexes by various high performance liquid chromatography (HPLC) columns. Two C18 (Phenomenex Synergi Hydro-RP and LunaC18(2)), two phenyl (Inertsil Ph 3 and 5μm) and one mixed-mode (Restek Ultra IBD) stationary phases were tested for their retention and resolution capacities of the various complexes. The objective was to find simple separation conditions with low organic contents in the mobile phase to provide optimal conditions for detection by inductively coupled plasma mass spectrometry (ICPMS). The 15 complexes were synthesized in solution and characterized by electrospray ionization-mass spectrometry (ESI-MS). The C18 columns tested were either not resolutive enough or too retentive. The 3μm phenyl stationary phase was able to resolve 10 out of the 15 complexes in less than 25min, under isocratic conditions. The mixed-mode column was especially effective at separating the most hydrophilic complexes (6 complexes out of the 15), corresponding to the main LMM thiols found in living organisms. The detection limits (DLs) for these two columns were in the low nanomolar range and overall slightly better for the phenyl column. The possibilities offered by such methodology were exemplified by monitoring the time-course concentrations of four MMHg-thiol complexes within a phytoplankton incubation containing MMHg in the presence of an excess of four added thiols. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Reversed phase liquid chromatography hyphenated to continuous flow-extractive desorption electrospray ionization-mass spectrometry for analysis and charge state manipulation of undigested proteins

    Czech Academy of Sciences Publication Activity Database

    Li, L.; Yang, S.; Vidová, Veronika; Rice, E. M.; Wijeratne, A.; Havlíček, Vladimír; Schug, K. A.

    2015-01-01

    Roč. 21, č. 3 (2015), s. 361-368 ISSN 1469-0667 R&D Projects: GA ČR(CZ) GAP206/12/1150; GA MŠk(CZ) LH14064; GA MŠk LO1509 Institutional support: RVO:61388971 Keywords : protein chromatography * ambient ionization * charge-state manipulation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 1.011, year: 2015

  6. Antioxidant properties and hyphenated HPLC-PDA-MS profiling of Chilean Pica mango fruits (Mangifera indica L. Cv. piqueño).

    Science.gov (United States)

    Ramirez, Javier E; Zambrano, Ricardo; Sepúlveda, Beatriz; Simirgiotis, Mario J

    2013-12-31

    Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu), 13 in Pica peel (ppe) 11 in Tommy Atkins pulp (tpu) and 12 in Tommy Atkins peel (tpe). Three procyanidin dimers (peaks 6, 9 and 10), seven acid derivatives (peaks 1-4, 11, 20 and 21) and four xanthones were identified, mainly mangiferin (peak 12) and mangiferin gallate, (peak 7), which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13) was also present in both fruit pulps and dimethylmangiferin (peak 14) was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively) than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively). The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW) measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  7. Antioxidant Properties and Hyphenated HPLC-PDA-MS Profiling of Chilean Pica Mango Fruits (Mangifera indica L. Cv. piqueño

    Directory of Open Access Journals (Sweden)

    Javier E. Ramirez

    2013-12-01

    Full Text Available Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu, 13 in Pica peel (ppe 11 in Tommy Atkins pulp (tpu and 12 in Tommy Atkins peel (tpe. Three procyanidin dimers (peaks 6, 9 and 10, seven acid derivatives (peaks 1–4, 11, 20 and 21 and four xanthones were identified, mainly mangiferin (peak 12 and mangiferin gallate, (peak 7, which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13 was also present in both fruit pulps and dimethylmangiferin (peak 14 was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively. The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  8. Speciation analysis of mercury in sediments, zoobenthos and river water samples by high-performance liquid chromatography hyphenated to atomic fluorescence spectrometry following preconcentration by solid phase extraction

    International Nuclear Information System (INIS)

    Margetinova, Jana; Houserova-Pelcova, Pavlina; Kuban, Vlastimil

    2008-01-01

    A high-pressure microwave digestion was applied for microwave-assisted extraction (MAE) of mercury species from sediments and zoobenthos samples. A mixture containing 3 mol L -1 HCl, 50% aqueous methanol and 0.2 mol L -1 citric acid (for masking co-extracted Fe 3+ ) was selected as the most suitable extraction agent. The efficiency of proposed extraction method was better than 95% with R.S.D. below 6%. A preconcentration method utilizing a 'homemade' C18 solid phase extraction (SPE) microcolumns was developed to enhance sensitivity of the mercury species determination using on-column complex formation of mercury-2-mercaptophenol complexes. Methanol was chosen for counter-current elution of the retained mercury complexes achieving a preconcentration factor as much as 1000. The preconcentration method was applied for the speciation analysis of mercury in river water samples. The high-performance liquid chromatography-cold vapour atomic fluorescence spectrometric (HPLC/CV-AFS) method was used for the speciation analysis of mercury. The complete separation of four mercury species was achieved by an isocratic elution of aqueous methanol (65%/35%) on a Zorbax SB-C18 column (4.6 mm x 150 mm, 5 μm) using the same complexation reagent (2-mercaptophenol). The limits of detection were 4.3 μg L -1 for methylmercury (MeHg + ), 1.4 μg L -1 for ethylmercury (EtHg + ), 0.8 μg L -1 for inorganic mercury (Hg 2+ ), 0.8 μg L -1 for phenylmercury (PhHg + )

  9. Investigation of porous graphitic carbon for triterpenoids and natural resinous materials analysis by high performance liquid chromatography hyphenated to mass spectrometry.

    Science.gov (United States)

    Rhourri-Frih, B; Chaimbault, P; Dequeral, D; André, P; Lafosse, M

    2012-06-01

    Natural resinous materials are mainly composed of pentacyclic triterpenes which exhibit a large number of interesting medicinal activities. However, the presence of numerous isomers within the active substances makes their screening by HPLC very challenging. Porous graphitic carbon was investigated as stationary phase to achieve triterpenes isomers separation. The influence of various parameters (temperature, formic acid concentration and mobile phase composition) on the retention was considered. A usual decrease of the retention of triterpenes was observed with the increase of the temperature. Therefore, separation in resinous materials was performed at 25°C. Acetonitrile-isopropanol mixture was chosen as mobile phase in gradient elution and leads to the best compromise between efficiency and high resolution. The lack of chromophore groups in the pentacyclic triterpenes structures required the use of mass spectrometry detection. Moreover, atmospheric pressure photo-ionisation mass spectrometry prevents compounds fragmentation which was helpful for spectra interpretation and compounds identification. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Urea functionalized surface-bonded sol-gel coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

    Science.gov (United States)

    Jillani, Shehzada Muhammad Sajid; Alhooshani, Khalid

    2018-03-30

    Sol-gel urea functionalized-[bis(hydroxyethyl)amine] terminated polydimethylsiloxane coating was developed for capillary microextraction-high performance liquid chromatographic analysis from aqueous samples. A fused silica capillary is coated from the inside with surface bonded coating material and is created through in-situ sol-gel reaction. The urea-functionalized coating was immobilized to the inner surface of the capillary by the condensation reaction of silanol groups of capillary and sol-solution. The characterization of the coating material was successfully done by using X-ray photoelectron spectroscopy, thermogravimetric analysis, field emission scanning electron microscope, and energy dispersive X-ray spectrometer. To make a setup of online capillary microextraction-high performance liquid chromatography, the urea functionalized capillary was installed in the HPLC manual injection port. The analytes of interest were pre-concentrated in the coated sampling loop, desorbed by the mobile phase, chromatographically separated on C-18 column, and analyzed by UV detector. Sol-gel coated capillaries were used for online extraction and high-performance liquid chromatographic analysis of phenols, ketones, aldehydes, and polyaromatic hydrocarbons. This newly developed coating showed excellent extraction for a variety of analytes ranging from highly polar to non-polar in nature. The analysis using sol-gel coating showed excellent overall sensitivity in terms of lower detection limits (S/N = 3) for the analytes (0.10 ng mL -1 -14.29 ng mL -1 ) with acceptable reproducibility that is less than 12.0%RSD (n = 3). Moreover, the capillary to capillary reproducibility of the analysis was also tested by changing the capillary of the same size. This provided excellent%RSD of less than 10.0% (n = 3). Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Multidimensional monitoring of anaerobic/aerobic azo dye based wastewater treatments by hyphenated UPLC-ICP-MS/ESI-Q-TOF-MS techniques.

    Science.gov (United States)

    Frindt, Benjamin; Mattusch, Jürgen; Reemtsma, Thorsten; Griesbeck, Axel G; Rehorek, Astrid

    2017-04-01

    Sulfonated reactive azo dyes, such as Reactive Orange 107, are extensively used in textile industries. Conventional wastewater treatment systems are incapable of degrading and decolorizing reactive azo dyes completely from effluents, because of their stability and resistance to aerobic biodegradation. However, reactive azo dyes are degradable under anaerobic conditions by releasing toxic aromatic amines. To clarify reaction mechanisms and the present toxicity, the hydrolyzed Reactive Orange 107 was treated in anaerobic-aerobic two-step batch experiments. Sulfonated transformation products were identified employing coupled ICP-MS and Q-TOF-MS measurements. Suspected screening lists were generated using the EAWAG-BBD. The toxicity of the reactor content was determined utilizing online measurements of the inhibition of Vibrio fischeri. The OCHEM web platform for environmental modeling was instrumental in the estimations of the environmental impact of generated transformation products.

  12. Method development for speciation analysis of nanoparticle and ionic forms of gold in biological samples by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Malejko, Julita; Świerżewska, Natalia; Bajguz, Andrzej; Godlewska-Żyłkiewicz, Beata

    2018-04-01

    A new method based on coupling high performance liquid chromatography (HPLC) to inductively coupled plasma mass spectrometry (ICP MS) has been developed for the speciation analysis of gold nanoparticles (AuNPs) and dissolved gold species (Au(III)) in biological samples. The column type, the composition and the flow rate of the mobile phase were carefully investigated in order to optimize the separation conditions. The usefulness of two polymeric reversed phase columns (PLRP-S with 100 nm and 400 nm pore size) to separate gold species were investigated for the first time. Under the optimal conditions (PLRP-S400 column, 10 mmol L-1 SDS and 5% methanol as the mobile phase, 0.5 mL min-1 flow rate), detection limits of 2.2 ng L-1 for Au(III), 2.8 ng L-1 for 10 nm AuNPs and 3.7 ng L-1 for 40 nm AuNPs were achieved. The accuracy of the method was proved by analysis of reference material RM 8011 (NIST) of gold nanoparticles of nominal diameter of 10 nm. The HPLC-ICP MS method has been successfully applied to the detection and size characterization of gold species in lysates of green algae Acutodesmus obliquus, typical representative of phytoplankton flora, incubated with 10 nm AuNPs or Au(III).

  13. Investigation of mercury-containing proteins by enriched stable isotopic tracer and size-exclusion chromatography hyphenated to inductively coupled plasma-isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Shi Junwen; Feng Weiyue; Wang Meng; Zhang Fang; Li Bai; Wang Bing; Zhu Motao; Chai Zhifang

    2007-01-01

    In order to investigate trace mercury-containing proteins in maternal rat and their offspring, a method of enriched stable isotopic tracer ( 196 Hg and 198 Hg) combined with size-exclusion chromatography (SEC) coupled to inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS) was developed. Prior to the analysis, 196 Hg- and 198 Hg-enriched methylmercury was administrated to the pregnant rats. Then the mercury-containing proteins in serum and brain cytosol of the dam and pup rats were separated by size-exclusion columns and the mercury was detected by ICP-MS. The ICP-MS spectrogram of the tracing samples showed significantly elevated 196 Hg and 198 Hg isotopic signals compared with the natural ones, indicating that the detection sensitivity could be increased by the tracer method. The contents of mercury in chromatographic fractions of the dam and pup rat brain cytosol were quantitatively estimated by post-column reverse ID-ICP-MS. The quantitative speciation differences of mercury in brain cytosol between the dam and pup rats were observed, indicating that such studies could be useful for toxicological estimation. Additionally, the isotopic ratio measurement of 198 Hg/ 202 Hg in the tracing samples could be used to identify the artifact mercury species caused in the analytical procedure. The study demonstrates that the tracer method combined with high-performance liquid chromatography (HPLC)-ICP-IDMS could provide reliably qualitative and quantitative information on mercury-containing proteins in organisms

  14. Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives

    DEFF Research Database (Denmark)

    Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente

    2006-01-01

    Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, t...

  15. Alkaloids Profiling of Fumaria capreolata by Analytical Platforms Based on the Hyphenation of Gas Chromatography and Liquid Chromatography with Quadrupole-Time-of-Flight Mass Spectrometry

    Science.gov (United States)

    Bribi, Noureddine; Gómez-Caravaca, Ana María

    2017-01-01

    Two analytical platforms, gas chromatography (GC) coupled to quadrupole-time-of-flight (QTOF) mass spectrometry (MS) and reversed-phase ultrahigh performance liquid chromatography (UHPLC) coupled to diode array (DAD) and QTOF detection, were applied in order to study the alkaloid profile of Fumaria capreolata. The use of these mass analyzers enabled tentatively identifying the alkaloids by matching their accurate mass signals and suggested molecular formulae with those previously reported in libraries and databases. Moreover, the proposed structures were corroborated by studying their fragmentation pattern obtained by both platforms. In this way, 8 and 26 isoquinoline alkaloids were characterized using GC-QTOF-MS and RP-UHPLC-DAD-QTOF-MS, respectively, and they belonged to the following subclasses: protoberberine, protopine, aporphine, benzophenanthridine, spirobenzylisoquinoline, morphinandienone, and benzylisoquinoline. Moreover, the latter analytical method was selected to determine at 280 nm the concentration of protopine (9.6 ± 0.7 mg/g), a potential active compound of the extract. In conclusion, although GC-MS has been commonly used for the analysis of this type of phytochemicals, RP-UHPLC-DAD-QTOF-MS provided essential complementary information. This analytical method can be applied for the quality control of phytopharmaceuticals containing Fumaria extracts currently found in the market. PMID:29348751

  16. Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, Th.

    2006-01-01

    The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical

  17. Investigation of mercury-containing proteins by enriched stable isotopic tracer and size-exclusion chromatography hyphenated to inductively coupled plasma-isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shi Junwen [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Feng Weiyue [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]. E-mail: fengwy@mail.ihep.ac.cn; Wang Meng [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Zhang Fang [Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Li Bai [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Wang Bing; Zhu Motao [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Chai Zhifang [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Institute of Nuclear Technology, Shenzhen University, Shenzhen 518060 (China)]|[Institute of Nanochemistry and Nanosafety, Shanghai University, Shanghai (China)

    2007-01-30

    In order to investigate trace mercury-containing proteins in maternal rat and their offspring, a method of enriched stable isotopic tracer ({sup 196}Hg and {sup 198}Hg) combined with size-exclusion chromatography (SEC) coupled to inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS) was developed. Prior to the analysis, {sup 196}Hg- and {sup 198}Hg-enriched methylmercury was administrated to the pregnant rats. Then the mercury-containing proteins in serum and brain cytosol of the dam and pup rats were separated by size-exclusion columns and the mercury was detected by ICP-MS. The ICP-MS spectrogram of the tracing samples showed significantly elevated {sup 196}Hg and {sup 198}Hg isotopic signals compared with the natural ones, indicating that the detection sensitivity could be increased by the tracer method. The contents of mercury in chromatographic fractions of the dam and pup rat brain cytosol were quantitatively estimated by post-column reverse ID-ICP-MS. The quantitative speciation differences of mercury in brain cytosol between the dam and pup rats were observed, indicating that such studies could be useful for toxicological estimation. Additionally, the isotopic ratio measurement of {sup 198}Hg/{sup 202}Hg in the tracing samples could be used to identify the artifact mercury species caused in the analytical procedure. The study demonstrates that the tracer method combined with high-performance liquid chromatography (HPLC)-ICP-IDMS could provide reliably qualitative and quantitative information on mercury-containing proteins in organisms.

  18. Characterization of oligosaccharides with capillary high performance anion exchange chromatography hyphenated to pulsed amperometric detection and ion trap mass spectrometry : application to the analysis of human lysosomal disorders

    NARCIS (Netherlands)

    Bruggink, Cornelis

    The development of a capillary ion chromatograph is described together with a matching desalter. This desalter made it possible to use on-line a mass spectrometer. The mass spectrometer enables partly to characterize carbohydrates eluting from the anion exchange column. This separation technology is

  19. Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry-A review

    International Nuclear Information System (INIS)

    Popp, Maximilian; Hann, Stephan; Koellensperger, Gunda

    2010-01-01

    In recent years the number of environmental applications of elemental speciation analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. The analytical characteristics, such as extremely low detection limits (LOD) for almost all elements, the wide linear range, the possibility for multi-elemental analysis and the possibility to apply isotope dilution mass spectrometry (IDMS) make ICP-MS an attractive tool for elemental speciation analysis. Two methodological approaches, i.e. the combination of ICP-MS with high performance liquid chromatography (HPLC) and gas chromatography (GC), dominate the field. Besides the investigation of metals and metalloids and their species (e.g. Sn, Hg, As), representing 'classic' elements in environmental science, more recently other elements (e.g. P, S, Br, I) amenable to ICP-MS determination were addressed. In addition, the introduction of isotope dilution analysis and the development of isotopically labeled species-specific standards have contributed to the success of ICP-MS in the field. The aim of this review is to summarize these developments and to highlight recent trends in the environmental application of ICP-MS coupled to GC and HPLC.

  20. MPTS-silica coated capillary microextraction on line hyphenated with inductively coupled plasma atomic emission spectrometry for the determination of Cu, Hg and Pb in biological samples.

    Science.gov (United States)

    Zheng, Fei; Hu, Bin

    2007-09-15

    A novel sol-gel 3-mercaptopropyltrimethoxysilane (MPTS) modified silica coating was developed for capillary microextraction (CME) of trace Cu, Hg and Pb prior to their on line determination by inductively coupled plasma-atomic emission spectrometry (ICP-AES). This organic-inorganic hybrid coating was in situ created on the inner walls of fused silica capillary using a sol solution containing TMOS (tetramethoxysilane) as a precursor, MPTS as a co-precursor, ethanol as the solvent and hydrochloric acid as a catalyst. The structure of the capillary coating was characterized by FT-IR spectroscopy, Raman spectroscopy, SEM and TEM. The factors affecting on the capillary microextraction of analytes such as pH, sample flow rate and volume, elution solution and interfering ions had been investigated, and the optimized experimental parameters were obtained. Under the optimized conditions, the absorption capacity of MPTS-silica coated capillary was found to be 1.17, 1.96 and 1.19mugm(-1) for Cu, Hg and Pb, and the limits of detection were as low as 0.17 0.22 and 0.52ngmL(-1), respectively. With a sampling frequency of 12h(-1), the relative standard deviations (R.S.D.s) were 4.2, 2.6 and 3.8% (C=4ngmL(-1), n=7, sample volume=1mL) for Cu, Hg and Pb, respectively. The proposed method had been successfully applied to the determination of Cu, Hg and Pb in human urine, human serum and preserved egg. To validate the proposed method, certified reference materials of BCR151 milk powder, GBW07601 (GSH-1) human hair, GSBZ 50016-90 and GSB 07-1183-2000 water samples were analyzed and the determined values were in a good agreement with the certified values.

  1. Rapid identification of cyclic tetrapyrrolic photosensitisers for photodynamic therapy using on-line hyphenated LC-PDA-MS coupled with photo-cytotoxicity assay.

    Science.gov (United States)

    Tan, P J; Appleton, D R; Mustafa, M R; Lee, H B

    2012-01-01

    Photodynamic therapy is a treatment modality that involves site-directed generation of cytotoxic reactive oxygen species by light-activated photosensitisers. In order to rapidly identify new photosensitisers from natural extracts, we developed a liquid chromatography-photodiode array-mass spectrometry (LC-PDA-MS) method to rapidly identify plant extracts that contain photosensitisers, particularly those possessing a cyclic tetrapyrrole structure. Six previously isolated compounds (1-6) were identified in bioactive fractions derived from 15 plant extracts on the basis of their chromatographic retention times, UV-visible profiles, accurate mass and fragmentation patterns. Samples containing uncommon photosensitisers were rapidly identified using this method, and subsequent scale-up isolation efforts led to two new compounds (7 and 8) which were confirmed to be active photosensitisers in a photo-cytotoxicity assay. This method serves as a useful tool in prioritising samples that may contain new photosensitisers out of a larger group of photo-cytotoxic natural products extracts. Copyright © 2011 John Wiley & Sons, Ltd.

  2. Living organisms as an alternative to hyphenated techniques for metal speciation. Evaluation of baker's yeast immobilized on silica gel for Hg speciation*1

    Science.gov (United States)

    Pérez-Corona, Teresa; Madrid-Albarrán, Yolanda; Cámara, Carmen; Beceiro, Elisa

    1998-02-01

    The use of living organisms for metal preconcentration and speciation is discussed. Among substrates, Saccharomyces cerevisiae baker's yeast has been successfully used for the speciation of mercury [Hg(II) and CH 3Hg +], selenium [Se(IV) and Se(VI)] and antimony [Sb(III) and Sb(V)]. To illustrate the capabilities of these organisms, the analytical performance of baker's yeast immobilized on silica gel for on-line preconcentration and speciation of Hg(II) and methylmercury is reported. The immobilized cells were packed in a PTFE microcolumn, through which mixtures of organic and inorganic mercury solutions were passed. Retention of inorganic and organic mercury solutions took place simultaneously, with the former retained in the silica and the latter on the yeast. The efficiency uptake for both species was higher than 95% over a wide pH range. The speciation was carried out by selective and sequential elution with 0.02 mol L -1 HCl for methylmercury and 0.8 mol L -1 CN - for Hg(II). This method allows both preconcentration and speciation of mercury. The preconcentration factors were around 15 and 100 for methylmercury and mercury(II), respectively. The method has been successfully applied to spiked sea water samples.

  3. Comprehensive two-dimensional liquid chromatography and hyphenated liquid chromatography to study the degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, T.

    2005-01-01

    Size exclusion chromatography (SEC), gradient polymer elution chromatography (GPEC) and liquid chromatography at critical conditions (LC-CC) have been developed and applied to observe chemical changes in poly(bisphenol A)carbonate (PC) due to hydrolytic degradation. Especially LC-CC appeared to be

  4. The potential of asymmetric flow field-flow fractionation hyphenated to multiple detectors for the quantification and size estimation of silica nanoparticles in a food matrix.

    Science.gov (United States)

    Heroult, Julien; Nischwitz, Volker; Bartczak, Dorota; Goenaga-Infante, Heidi

    2014-06-01

    This work represents a first systematic approach to the size-based elemental quantification and size estimation of metal(loid) oxide nanoparticles such as silica (SiO2) in a real food matrix using asymmetric flow field-flow fractionation coupled online with inductively coupled plasma mass spectrometry (ICP-MS) and multi-angle light scattering (MALS) and offline with transmission electron microscopy (TEM) with energy-dispersive X-ray analysis (EDAX). Coffee creamer was selected as the model sample since it is known to contain silica as well as metal oxides such as titania at the milligramme per kilogramme levels. Optimisation of sample preparation conditions such as matrix-to-solvent ratio, defatting with organic solvents and sonication time that may affect nanoparticle size and size distribution in suspensions was investigated. Special attention was paid to the selection of conditions that minimise particle transformation during sample preparation and analysis. The coffee creamer matrix components were found to stabilise food grade SiO2 particles in comparison with water suspensions whilst no significant effect of defatting using hexane was found. The use of sample preparation procedures that mimic food cooking in real life was also investigated regarding their effect on particle size and particle size distribution of silica nanoparticles in the investigated food matrix; no significant effect of the water temperature ranging from ambient temperature to 60 °C was observed. Field-flow fractionation coupled to inductively coupled plasma-mass spectrometry (FFF-ICP-MS) analysis of extracts of both unspiked coffee creamer and coffee creamer spiked with food grade silicon dioxide, using different approaches for size estimation, enabled determination of SiO2 size-based speciation. Element-specific detection by ICP-MS and post-FFF calibration with elemental calibration standards was used to determine the elemental composition of size fractions separated online by FFF. Quantitative data on mass balance is provided for the size-based speciation of the investigated inorganic nano-objects in the complex matrix. The combination of FFF with offline fractionation by filtration and with detection by ICP-MS and TEM/EDAX has been proven essential to provide reliable information of nanoparticle size in the complex food matrix.

  5. Joint approximate diagonalization of eigenmatrices as a high-throughput approach for analysis of hyphenated and comprehensive two-dimensional gas chromatographic data.

    Science.gov (United States)

    Zarghani, Maryam; Parastar, Hadi

    2017-11-17

    The objective of the present work is development of joint approximate diagonalization of eigenmatrices (JADE) as a member of independent component analysis (ICA) family, for the analysis of gas chromatography-mass spectrometry (GC-MS) and comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS) data to address incomplete separation problem occurred during the analysis of complex sample matrices. In this regard, simulated GC-MS and GC×GC-MS data sets with different number of components, different degree of overlap and noise were evaluated. In the case of simultaneous analysis of multiple samples, column-wise augmentation for GC-MS and column-wise super-augmentation for GC×GC-MS was used before JADE analysis. The performance of JADE was evaluated in terms of statistical parameters of lack of fit (LOF), mutual information (MI) and Amari index as well as analytical figures of merit (AFOMs) obtained from calibration curves. In addition, the area of feasible solutions (AFSs) was calculated by two different approaches of MCR-BANDs and polygon inflation algorithm (FACPACK). Furthermore, JADE performance was compared with multivariate curve resolution-alternating least squares (MCR-ALS) and other ICA algorithms of mean-field ICA (MFICA) and mutual information least dependent component analysis (MILCA). In all cases, JADE could successfully resolve the elution and spectral profiles in GC-MS and GC×GC-MS data with acceptable statistical and calibration parameters and their solutions were in AFSs. To check the applicability of JADE in real cases, JADE was used for resolution and quantification of phenanthrene and anthracene in aromatic fraction of heavy fuel oil (HFO) analyzed by GC×GC-MS. Surprisingly, pure elution and spectral profiles of target compounds were properly resolved in the presence of baseline and interferences using JADE. Once more, the performance of JADE was compared with MCR-ALS in real case. On this matter, the mutual information (MI) values were 1.01 and 1.13 for resolved profiles by JADE and MCR-ALS, respectively. In addition, LOD values (μg/mL) were respectively 1.36 and 1.24 for phenanthrene and 1.26 and 1.09 for anthracene using MCR-ALS and JADE which showed outperformance of JADE over MCR-ALS. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Enantioselective column coupled electrophoresis employing large bore capillaries hyphenated with tandem mass spectrometry for ultra-trace determination of chiral compounds in complex real samples.

    Science.gov (United States)

    Piešťanský, Juraj; Maráková, Katarína; Kovaľ, Marián; Havránek, Emil; Mikuš, Peter

    2015-12-01

    A new multidimensional analytical approach for the ultra-trace determination of target chiral compounds in unpretreated complex real samples was developed in this work. The proposed analytical system provided high orthogonality due to on-line combination of three different methods (separation mechanisms), i.e. (1) isotachophoresis (ITP), (2) chiral capillary zone electrophoresis (chiral CZE), and (3) triple quadrupole mass spectrometry (QqQ MS). The ITP step, performed in a large bore capillary (800 μm), was utilized for the effective sample pretreatment (preconcentration and matrix clean-up) in a large injection volume (1-10 μL) enabling to obtain as low as ca. 80 pg/mL limits of detection for the target enantiomers in urine matrices. In the chiral CZE step, the different chiral selectors (neutral, ionizable, and permanently charged cyclodextrins) and buffer systems were tested in terms of enantioselectivity and influence on the MS detection response. The performance parameters of the optimized ITP - chiral CZE-QqQ MS method were evaluated according to the FDA guidance for bioanalytical method validation. Successful validation and application (enantioselective monitoring of renally eliminated pheniramine and its metabolite in human urine) highlighted great potential of this chiral approach in advanced enantioselective biomedical applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 78 FR 43115 - Receipt of Several Pesticide Petitions Filed for Residues of Pesticide Chemicals in or on Various...

    Science.gov (United States)

    2013-07-19

    ...; passionfruit at 4.0 ppm; onion, green, subgroup 3-07B at 3.0 ppm; and spice, subgroup19B at 40 ppm. Since... produced by the reaction of either 1,6[hyphen]hexane-diisocyanate; 2,4,4[hyphen]trimethyl[hyphen]1,6[hyphen... Decision Document to support this petition which includes a chemistry that was also in the Screening...

  8. Development of a chromatographic separation method hyphenated to electro-spray ionization mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS): application to the lanthanides speciation analysis

    International Nuclear Information System (INIS)

    Beuvier, Ludovic

    2015-01-01

    This work focuses on the development of a chromatographic separation method coupled to both ESI-MS and ICP-MS in order to achieve the comprehensive speciation analysis of lanthanides in aqueous phase representative of back-extraction phases of advanced spent nuclear fuel treatment processes. This analytical method allowed the separation, the characterization and the quantitation of lanthanides complexes holding poly-aminocarboxylic ligands, such as DTPA and EDTA, used as complexing agents in these processes. A HILIC separation method of lanthanides complexes has been developed with an amide bonded stationary phase. A screening of a wide range of mobile phase compositions demonstrated that the adsorption mechanism was predominant. This screening allowed also obtaining optimized separation conditions. Faster analysis conditions with shorter amide column packed with sub 2 μm particles reduced analysis time by 2.5 and 25% solvent consumption. Isotopic and structural characterization by HILIC ESI-MS was performed as well as the development of external calibration quantitation method. Analytical performances of quantitation method were determined. Finally, the development of the HILIC coupling to ESI-MS and ICP-MS was achieved. A simultaneous quantitation method by ESI-MS and ICP-MS was performed to determine the species quantitative distribution in solution. Analytical performances of quantitation method were also determined. (author) [fr

  9. Mastering analytical challenges for the characterization of pentacyclic triterpene mono- and diesters of Calendula officinalis flowers by non-aqueous C30 HPLC and hyphenation with APCI-QTOF-MS.

    Science.gov (United States)

    Nicolaus, Christoph; Sievers-Engler, Adrian; Murillo, Renato; D'Ambrosio, Michele; Lämmerhofer, Michael; Merfort, Irmgard

    2016-01-25

    Pentacyclic triterpene mono- and diesters have been isolated from Calendula officinalis flowers. GC-MS, APCI-Exactive Orbitrap HR-MS and NMR allowed to identify the triterpene skeleton in various samples (different triterpene mixtures from Calendula n-hexane extract). NMR provided evidence that triterpene diesters are present in the samples as well. However, the corresponding quasi-molecular ions could not be detected by APCI-Exactive Orbitrap HR-MS. Instability of triterpene diesters and loss of a fatty acid residue, respectively, in the ion-source made their MS detection challenging. Thus, a set of new APCI-QTOF-MS methods (using the TripleTOF 5600+ mass spectrometer) were developed which made it eventually possible to solve this problem and confirm the diester structures by MS via quasi-molecular ion [M+H](+) detection. Direct infusion APCI-QTOF MS experiments in MS/MS high sensitivity scan mode with low collision energy and multi-channel averaging acquisition (MCA) allowed the detection of quasi-molecular ions of triterpene diesters for the first time and unequivocally confirmed the presence of faradiol 3,16-dimyristate and -dipalmitate, as well as the corresponding mixed diesters faradiol 3-myristate,16-palmitate and faradiol 3-palmitate,16-myristate. Preferential loss of the fatty acid in 16-position made it possible to distinguish the mixed diesters by MS/MS spectra. Their chromatographic separations turned out to be challenging due to their bulkiness and extended molecular dimensions. However, separation could be achieved by an uncommon non-aqueous RPLC mode with an in-house synthesized C30 phase. Finally, two (U)HPLC-APCI-QTOF-MS methods with C18- and C30-based non-aqueous RPLC provided suitable, sensitive assays to monitor the presence of monoesters and diesters of various triterpenes (faradiol, maniladiol, arnidiol, arnitriol A and lupane-3β,16β,20-triol esters) in the n-hexane extract of C. officinalis with high mass resolution and good mass accuracy. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Post-polymerization photografting on methacrylate-based monoliths for separation of intact proteins and protein digests with comprehensive two-dimensional liquid chromatography hyphenated with high-resolution mass spectrometry

    NARCIS (Netherlands)

    Vonk, R.J.; Wouters, S.; Barcaru, A.; Vivó-Truyols, G.; Eeltink, S.; de Koning, L.J.; Schoenmakers, P.J.

    2015-01-01

    Post-polymerization photografting is a versatile tool to alter the surface chemistry of organic-based monoliths so as to obtain desired stationary phase properties. In this study, 2-acrylamido-2-methyl-1-propanesulfonic acid was grafted to a hydrophobic poly(butyl methacrylate-co-ethylene glycol

  11. Methodology for monitoring gold nanoparticles and dissolved gold species in culture medium and cells used for nanotoxicity tests by liquid chromatography hyphenated to inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    López-Sanz, Sara; Fariñas, Nuria Rodríguez; Vargas, Rosario Serrano; Martín-Doimeadios, Rosa Del Carmen Rodríguez; Ríos, Ángel

    2017-03-01

    An analytical methodology based on coupling reversed-phase liquid chromatography (HPLC) to an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the characterization and identification of gold nanoparticles (AuNPs) and gold dissolved species (Au 3+ ) in culture medium (Dulbecco's Modified Eagle Medium, DMEM) and HeLa cells (a human cervical adenocarcinoma cell line) used in nanotoxicity tests. The influence of the culture medium was also studied and the method applied for nanotoxicity tests. It was also observed that AuNPs can undergo an oxidation process in the supernatants and only a small amount of AuNPs and dissolved Au 3+ was associated with cells. To evaluate the biological impact of AuNPs, a classical viability assay onto HeLa cells was performed using cellular media DMEM in the presence of increasing dosage of 10nm AuNPs. The results showed that 10nm AuNPs exhibit a slight toxic effect. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid–Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase

    OpenAIRE

    Sánchez, Raquel; Horstkotte, Burkhard; Fikarová, Kateřina; Sklenářová, Hana; Maestre, Salvador E.; Miró, Manuel; Todolí Torró, José Luis

    2017-01-01

    A proof of concept study involving the online coupling of automatic dispersive liquid–liquid microextraction (DLLME) to inductively coupled plasma optical emission spectrometry (ICP OES) with direct introduction and analysis of the organic extract is herein reported for the first time. The flow-based analyzer features a lab-in-syringe (LIS) setup with an integrated stirring system, a Meinhard nebulizer in combination with a heated single-pass spray chamber, and a rotary injection valve, used ...

  13. Fully Automatic In-Syringe Magnetic Stirring-Assisted Dispersive Liquid-Liquid Microextraction Hyphenated to High-Temperature Torch Integrated Sample Introduction System-Inductively Coupled Plasma Spectrometer with Direct Injection of the Organic Phase.

    Science.gov (United States)

    Sánchez, Raquel; Horstkotte, Burkhard; Fikarová, Kateřina; Sklenářová, Hana; Maestre, Salvador; Miró, Manuel; Todolí, Jose-Luis

    2017-03-21

    A proof of concept study involving the online coupling of automatic dispersive liquid-liquid microextraction (DLLME) to inductively coupled plasma optical emission spectrometry (ICP OES) with direct introduction and analysis of the organic extract is herein reported for the first time. The flow-based analyzer features a lab-in-syringe (LIS) setup with an integrated stirring system, a Meinhard nebulizer in combination with a heated single-pass spray chamber, and a rotary injection valve, used as an online interface between the microextraction system and the detection instrument. Air-segmented flow was used for delivery of a fraction of the nonwater miscible extraction phase, 12 μL of xylene, to the nebulizer. All sample preparative steps including magnetic stirring assisted DLLME were carried out inside the syringe void volume as a size-adaptable yet sealed mixing and extraction chamber. Determination of trace level concentrations of cadmium, copper, lead, and silver as model analytes has been demonstrated by microextraction as diethyldithiophosphate (DDTP) complexes. The automatic LIS-DLLME method features quantitative metal extraction, even in troublesome sample matrixes, such as seawater, salt, and fruit juices, with relative recoveries within the range of 94-103%, 93-100%, and 92-99%, respectively. Furthermore, no statistically significant differences at the 0.05 significance level were found between concentration values experimentally obtained and the certified values of two serum standard reference materials.

  14. Ultra-Performance Liquid Chromatography Hyphenated with Quadrupole-Orbitrap Mass Spectrometry for Simultaneous Determination of Necine-Core-Structure Pyrrolizidine Alkaloids in Crotalaria sessiliflora L. without all Corresponding Standards.

    Science.gov (United States)

    Zhang, Wei; Huai, Wenbei; Zhang, Yi; Shen, Jincan; Tang, Xunyou; Xie, Xiujuan; Wang, Ke; Fan, Huajun

    2017-09-01

    Crotalaria sessiliflora L. is a Chinese traditional herb for treatment of cutaneum carcinoma and cervical carcinoma. In addition to monocrotaline, coexisting pyrrolizidine alkaloids (PAs) also require further quantification for quality control and pharmaceutical uses of the herb. To establish a UPLC-Q-Orbitrap/MS method of simultaneous determination of coexisting PAs with same parent structure for quality control and comprehensive researches of Crotalaria sessiliflora L. PAs in Crotalaria sessiliflora L. were analysed by UPLC-Q-Orbitrap/MS method. Coexisting PAs were identified by mass data of full MS-dd-MS 2 based on the characteristic fragmentation pattern and necine-core structure. Moreover, quantification of PAs was conducted by parallel reaction monitoring (PRM) mode using m/z 138, m/z 120 and m/z 94 from identical necine-core structure as quantitative ions with single monocrotaline standard for accurate calibration. Five PAs, named monocrotaline, retrorsine, senecionine, integerrimine, O-9-angeloylretronecine, were indentified and confirmed. Quantitative ions of m/z 138, m/z 120 and m/z 94 were used for quantification of PAs containing the necine-core structure in Crotalaria sessiliflora L. The results demonstrated that contents, precision and recoveries of the five PAs mentioned earlier were respectively 3.307-30.35 μg/g, 1.1-4.5% and 88.91-92.33% while using m/z 120 as the best quantitative ion. The UPLC-Q-Orbitrap/MS method was established for simultaneous determination of five PAs in Crotalaria sessiliflora L. without all corresponding standards, and was proved that it was simple, convenient and effective for comprehensive quality control and pharmaceutical uses. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  15. A novel ultra-performance liquid chromatography hyphenated with quadrupole time of flight mass spectrometry method for rapid estimation of total toxic retronecine-type of pyrrolizidine alkaloids in herbs without requiring corresponding standards.

    Science.gov (United States)

    Zhu, Lin; Ruan, Jian-Qing; Li, Na; Fu, Peter P; Ye, Yang; Lin, Ge

    2016-03-01

    Nearly 50% of naturally-occurring pyrrolizidine alkaloids (PAs) are hepatotoxic, and the majority of hepatotoxic PAs are retronecine-type PAs (RET-PAs). However, quantitative measurement of PAs in herbs/foodstuffs is often difficult because most of reference PAs are unavailable. In this study, a rapid, selective, and sensitive UHPLC-QTOF-MS method was developed for the estimation of RET-PAs in herbs without requiring corresponding standards. This method is based on our previously established characteristic and diagnostic mass fragmentation patterns and the use of retrorsine for calibration. The use of a single RET-PA (i.e. retrorsine) for construction of calibration was based on high similarities with no significant differences demonstrated by the calibration curves constructed by peak areas of extract ion chromatograms of fragment ion at m/z 120.0813 or 138.0919 versus concentrations of five representative RET-PAs. The developed method was successfully applied to measure a total content of toxic RET-PAs of diversified structures in fifteen potential PA-containing herbs. Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. On-line sample-pre-treatment schemes for trace-level determinations of metals by coupling flow injection or sequential injection with ICP-MS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2003-01-01

    a polytetrafluoroethylene (PTFE) knotted reactor (KR), solvent extraction-back extraction and hydride/vapor generation. It also addresses a novel, robust approach, whereby the protocol of SI-LOV-bead injection (BI) on-line separation and pre-concentration of ultra-trace levels of metals by a renewable microcolumn...

  17. Inflammasome components ASC and AIM2 modulate the acute phase of biomaterial implant-induced foreign body responses.

    Science.gov (United States)

    Christo, Susan N; Diener, Kerrilyn R; Manavis, Jim; Grimbaldeston, Michele A; Bachhuka, Akash; Vasilev, Krasimir; Hayball, John D

    2016-02-10

    Detailing the inflammatory mechanisms of biomaterial-implant induced foreign body responses (FBR) has implications for revealing targetable pathways that may reduce leukocyte activation and fibrotic encapsulation of the implant. We have adapted a model of poly(methylmethacrylate) (PMMA) bead injection to perform an assessment of the mechanistic role of the ASC-dependent inflammasome in this process. We first demonstrate that ASC(-/-) mice subjected to PMMA bead injections had reduced cell infiltration and altered collagen deposition, suggesting a role for the inflammasome in the FBR. We next investigated the NLRP3 and AIM2 sensors because of their known contributions in recognising damaged and apoptotic cells. We found that NLRP3 was dispensable for the fibrotic encapsulation; however AIM2 expression influenced leukocyte infiltration and controlled collagen deposition, suggesting a previously unexplored link between AIM2 and biomaterial-induced FBR.

  18. 78 FR 17744 - Social Security Ruling, SSR 13-2p; Titles II and XVI: Evaluating Cases Involving Drug Addiction...

    Science.gov (United States)

    2013-03-22

    ...; Titles II and XVI: Evaluating Cases Involving Drug Addiction and Alcoholism (DAA); Correction AGENCY... c. i., third sentence, hyphenate ``nonmedical'' to read ``non-medical''. On page 11944, third column...., first sentence, hyphenate ``nonmedical'' to read ``non-medical''. On page 11944, footnote 22, replace...

  19. Rapid semi-quantification of zilpaterol from biological matrices using ASAP and DESI-like MS from a commercial heated electrospray ionization probe

    Science.gov (United States)

    Quantitation of contaminants in food animal products by regulatory officials is mostly conducted using hyphenated mass spectrometry (MS) technologies. While hyphenated MS approaches can be used for multi-residue sample analysis in an effective manner, it is time consuming, expensive, and labor inten...

  20. Thymus Gland Anatomy

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Thymus Gland, Adult, Anatomy Add to My Pictures View / ... 1500x1200 View Download Large: 3000x2400 View Download Title: Thymus Gland, Adult, Anatomy Description: Anatomy of the thymus ...

  1. High-performance thin-layer chromatography (HPTLC)

    National Research Council Canada - National Science Library

    Srivastava, ManMohan

    2011-01-01

    ... on HPTLC fundamentals: principle, theory, understanding; instrumentation: implementation, optimization, validation, automation and qualitative and quantitative analysis; applications: phytochemical analysis, biomedical analysis, herbal drug quantification, analytical analysis, finger print analysis and potential for hyphenation: HPTLC future to combinat...

  2. ACTINET-I3 Summer School on Analytical Innovation in the field of actinide recycling - Slides of the presentations

    International Nuclear Information System (INIS)

    Poinssot, Ch.; Nash, K.L.; Puget, P.; Szabo, Z.; Vallet, V.; Berthon, L.; Duhamet, J.; Wipff, G.; Dufreche, J.F.; Walter, P.; Thiebaut, D.; Toulhoat, P.; Aupiais, J.; Amatore, C.

    2011-01-01

    This conference dealt with 3 main topics: analytical innovation in separation processes (hyphenated techniques, analytical chips,...), actinide recycling (extraction, interfaces, processes,...) and chemistry and thermodynamics of actinides. This document is composed of the slides of the presentations

  3. Determination of methylmercury and inorganic mercury in shark fillets

    NARCIS (Netherlands)

    Krystek, Petra; Ritsema, Rob

    2004-01-01

    Three samples of deep-frozen shark fillets were analysed according to the following procedure: dissolution in tetramethylammonium hydroxide, derivatization/ethylation with sodium tetraethylborate, extraction into iso-octane and measurement with gas chromatography hyphenated to inductively coupled

  4. Characterization of Proteins, Peptides, and Polynucleotides by Mass Spectrometry

    NARCIS (Netherlands)

    Bischoff, Rainer

    2002-01-01

    Hyphenation of efficient separation methods such as high performance liquid chromatography (HPLC) or capillary electrophoresis (CE) with detection methods that provide structural or functional information is a powerful tool for the analysis of biological macromolecules. In particular,

  5. Plasticidad fenotípica en plantas de lippia dulcis (verbenaceae) sometidas a déficit hídrico

    OpenAIRE

    Villamizar Cújar, Javier Mauricio

    2012-01-01

  1. Cervical Cancer Stage IIIA

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Cervical Cancer Stage IIIA Add to My Pictures View /Download : ... 1275x1275 View Download Large: 2550x2550 View Download Title: Cervical Cancer Stage IIIA Description: Stage IIIA cervical cancer; drawing ...

  2. Cervical Cancer Stage IVA

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Cervical Cancer Stage IVA Add to My Pictures View /Download : ... 1575x1200 View Download Large: 3150x2400 View Download Title: Cervical Cancer Stage IVA Description: Stage IVA cervical cancer; drawing ...

  3. Cervical Cancer Stage IVB

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Cervical Cancer Stage IVB Add to My Pictures View /Download : ... 1200x1305 View Download Large: 2400x2610 View Download Title: Cervical Cancer Stage IVB Description: Stage IVB cervical cancer; drawing ...

  4. Cervical Cancer Stage IIIB

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Cervical Cancer Stage IIIB Add to My Pictures View /Download : ... 1425x1326 View Download Large: 2850x2651 View Download Title: Cervical Cancer Stage IIIB Description: Stage IIIB cervical cancer; drawing ...

  5. Cervical Cancer Stage IB

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Cervical Cancer Stage IB Add to My Pictures View /Download : ... 1613x1200 View Download Large: 3225x2400 View Download Title: Cervical Cancer Stage IB Description: Stage IB1 and IB2 cervical ...

  6. Expatriate Experience and the Fictional World of Diaspora

    Science.gov (United States)

    Ilyas, Mohammed

    2018-01-01

    Expatriate Writing, diaspora writing or immigrant writing is yet to be established as an independent genre of study. It came into origin as a result of "marginalization" or "hyphenated" existence of such immigrants and expatriates that narrated their traumatic experiences of multiple racial discrimination, ethnicity, nostalgia,…

  7. Chemometrics for drug impurity profiling : optimisation of capillary electrophoresis and deconvolution of overlapping peaks

    NARCIS (Netherlands)

    Zomeren, Paul Vincent van

    2008-01-01

    The potential of chemometrics for drug impurity profiling has been examined in this thesis. Generally, various hyphenated methods are used for the analysis of drug sub¬stance and product in order to enable the identification and quantification of impuri¬ties. chemometrics can be used to enhance the

  8. Authenticity Revisited : the production, distribution, and consumption of independent folk music in the Netherlands (1993-present)

    NARCIS (Netherlands)

    N. van Poecke (Niels)

    2017-01-01

    textabstractIn ways similar to the 1960s ‘urban folk revival’ – that is, through live performance, mass mediation and sales successes – the genre of folk music rose the surface of the global music industry once more during the first decade of the new millennium. The new labels are hyphenated, as in

  9. 342 analytical investigation of selected pesticide residues from fruits

    African Journals Online (AJOL)

    Osondu

    Keywords: Pesticide residues, reverse phase high performance liquid chromatography, chlorpyrifos, ... liquid chromatography hyphenated with tandem ..... Toxicology,. Applications. Toronto: Wiley-VCH. p. 541. Ortelli, D., Edder, P. and Corvi, C. (2004),. Multiresidue analysis of 74 pesticides in fruits and vegetables by liquid.

  10. Eletroforese capilar acoplada à espectrometria com plasma: uma ferramenta eficiente para a especiação Capillary electrophoresis coupled to plasma spectrometry: an efficient tool for speciation

    Directory of Open Access Journals (Sweden)

    Ana Paula G. Gervasio

    2003-01-01

    Full Text Available The most important features of the CE-ICP hyphenation, as well as its advantages and drawbacks as a tool for speciation are discussed. The fundamental principles of capillary electrophoresis and inductively coupled plasma mass spectrometry are also presented. Some applications involving different designs proposed in the literature to couple CE and ICP system for elemental speciation are reviewed.

  11. Molecular population genetics of the β-esterase gene cluster of ...

    Indian Academy of Sciences (India)

    Unknown

    fold (Claverys and Lacks 1986; Waldman and Liskay 1987;. Rayssiguier et al. ... iously used to tag these lines. The letter after the hyphen in most Zimbabwe lines (except Zim S. -. 44F) refers to the locality of collection (Sengwa or Harare). The line Zim. -S ...... 437–484. Ame- rican Society for Microbiology, Washington, D. C..

  12. Giulio Natta and the Origins of Stereoregular Polymers

    Indian Academy of Sciences (India)

    Ziegler and Natta, whose hyphenated names are inextricably linked to one of the most successful catalysts for the manufacture of polyolefins, were in fact, like cheese and chalk, in terms of their personalities and research philosophies. While Ziegler was a purist when it came to research pursuits and abhorred problems that ...

  13. Modern methods for the determination of physicochemical states of microelements in natural waters

    International Nuclear Information System (INIS)

    Polyakov, Evgenii V; Egorov, Yurii V

    2003-01-01

    The state-of-the-art in studies on the determination of ion-molecular and colloidal forms of microelements in aqueous solutions is analysed. Instrumental and hyphenated methods for the determination of such forms of microelements as aqua-ions, complexes, true and adsorption colloids are considered.

  14. Bayesian networks for omics data analysis

    NARCIS (Netherlands)

    Gavai, A.K.

    2009-01-01

    This thesis focuses on two aspects of high throughput technologies, i.e. data storage and data analysis, in particular in transcriptomics and metabolomics. Both technologies are part of a research field that is generally called ‘omics’ (or ‘-omics’, with a leading hyphen), which refers to genomics,

  15. Volatile compound fingerprinting of mixed cultutre fermentations

    NARCIS (Netherlands)

    Bok, de F.A.M.; Janssen, P.W.M.; Bayjanov, J.R.; Sieuwerts, S.; Lommen, A.; Hylckama, van J.; Molenaar, D.

    2011-01-01

    With the advent of the -omics era, classical technology platforms, such as hyphenated mass spectrometry, are currently undergoing a transformation toward high-throughput application. These novel platforms yield highly detailed metabolite profiles in large numbers of samples. Such profiles can be

  16. Volatile compound fingerprinting of mixed-culture fermentations.

    NARCIS (Netherlands)

    Bok, F.A. de; Janssen, P.W.; Bayjanov, J.; Sieuwerts, S.; Lommen, A.; Hylckama Vlieg, J.E. van; Molenaar, D

    2011-01-01

    With the advent of the -omics era, classical technology platforms, such as hyphenated mass spectrometry, are currently undergoing a transformation toward high-throughput application. These novel platforms yield highly detailed metabolite profiles in large numbers of samples. Such profiles can be

  17. Studies of Scleral Biomechanical Behavior Related to Susceptibility for Retinal Ganglion Cell Loss in Experimental Mouse Glaucoma

    Science.gov (United States)

    Nguyen, Cathy; Cone, Frances E.; Nguyen, Thao D.; Coudrillier, Baptiste; Pease, Mary E.; Steinhart, Matthew R.; Oglesby, Ericka N.; Jefferys, Joan L.; Quigley, Harry A.

    2013-01-01

    Purpose. To study anatomical changes and mechanical behavior of the sclera in mice with experimental glaucoma by comparing CD1 to B6 mice. Methods. Chronic experimental glaucoma for 6 weeks was produced in 2- to 4-month-old CD1 (43 eyes) and B6 mice (42 eyes) using polystyrene bead injection into the anterior chamber with 126 control CD1 and 128 control B6 eyes. Intraocular pressure (IOP) measurements were made with the TonoLab at baseline and after bead injection. Axial length and scleral thickness were measured after sacrifice in the CD1 and B6 animals and compared to length data from 78 eyes of DBA/2J mice. Inflation testing of posterior sclera was conducted, and circumferential and meridional strain components were determined from the displacement response. Results. Experimental glaucoma led to increases in axial length and width by comparison to fellow eyes (6% in CD1 and 10% in B6; all P glaucoma, the remainder of the sclera uniformly thinned in CD1, but thickened in B6. Peripapillary sclera in CD1 controls had significantly greater temporal meridional strain than B6 and had differences in the ratios of meridional to effective circumferential strain from B6 mice. In both CD1 and B6 mice, exposure to chronic IOP elevation resulted in stiffer pressure–strain responses for both the effective circumferential and meridional strains (multivariable regression model, P = 0.01–0.03). Conclusions. Longer eyes, greater scleral strain in some directions at baseline, and generalized scleral thinning after glaucoma were characteristic of CD1 mice that have greater tendency to retinal ganglion cell damage than B6 mice. Increased scleral stiffness after glaucoma exposure in mice mimics findings in monkey and human glaucoma eyes. PMID:23404116

  18. On-line liquid phase micro-extraction based on drop-in-plug sequential injection lab-at-valve platform for metal determination

    International Nuclear Information System (INIS)

    Mitani, Constantina; Anthemidis, Aristidis N.

    2013-01-01

    Highlights: ► Drop-in-plug micro-extraction based on SI-LAV platform for metal preconcentration. ► Automatic liquid phase micro-extraction coupled with FAAS. ► Organic solvents with density higher than water are used. ► Lead determination in environmental water and urine samples. -- Abstract: A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 μL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 μg L −1 and the precision expressed as relative standard deviation (RSD) at 50.0 μg L −1 of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples

  19. Erotic(izing Cubans

    Directory of Open Access Journals (Sweden)

    Virginia R. Domínguez

    1996-07-01

    Full Text Available [First paragraph] Sugar's Secrets: Race and the Erotics of Cuban Nationalism. VERA M. KUTZINSKI. Charlottesville: University Press of Virginia, 1993. xvii + 287 pp. (Cloth US$ 40.00, Paper US$ 17.95 Life on the Hyphen: The Cuban-American Way. GUSTAVO PÉREZ FlRMAT. Austin: University of Texas Press, 1994. xii + 217 pp. (Cloth US$ 30.00, Paper US$ 12.95 When a country is subjected to as much external political and ideological scrutiny as Cuba in the post-Batista years, scholarly explorations of something other than its foreign policy, its political economy, and its human rights abuses provide a breath of fresh air. But I am struck by the other things Sugar's Secrets and Life on the Hyphen have in common and how suspicious I am of their commonalities.

  20. Chemometrics tools used in analytical chemistry: an overview.

    Science.gov (United States)

    Kumar, Naveen; Bansal, Ankit; Sarma, G S; Rawal, Ravindra K

    2014-06-01

    This article presents various important tools of chemometrics utilized as data evaluation tools generated by various hyphenated analytical techniques including their application since its advent to today. The work has been divided into various sections, which include various multivariate regression methods and multivariate resolution methods. Finally the last section deals with the applicability of chemometric tools in analytical chemistry. The main objective of this article is to review the chemometric methods used in analytical chemistry (qualitative/quantitative), to determine the elution sequence, classify various data sets, assess peak purity and estimate the number of chemical components. These reviewed methods further can be used for treating n-way data obtained by hyphenation of LC with multi-channel detectors. We prefer to provide a detailed view of various important methods developed with their algorithm in favor of employing and understanding them by researchers not very familiar with chemometrics. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Gas Chromatography/Atmospheric Pressure Chemical Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry of Pyrolysis Oil from German Brown Coal

    Directory of Open Access Journals (Sweden)

    Jan Zuber

    2016-01-01

    Full Text Available Pyrolysis oil from the slow pyrolysis of German brown coal from Schöningen, obtained at a temperature of 500°C, was separated and analyzed using hyphenation of gas chromatography with an atmospheric pressure chemical ionization source operated in negative ion mode and Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS. Development of this ultrahigh-resolving analysis method is described, that is, optimization of specific GC and APCI parameters and performed data processing. The advantages of GC-APCI-FT-ICR-MS hyphenation, for example, soft ionization, ultrahigh-resolving detection, and most important isomer separation, were demonstrated for the sample liquid. For instance, it was possible to separate and identify nine different propylphenol, ethylmethylphenol, and trimethylphenol isomers. Furthermore, homologous series of different acids, for example, alkyl and alkylene carboxylic acids, were verified, as well as homologous series of alkyl phenols, alkyl dihydroxy benzenes, and alkoxy alkyl phenols.

  2. Gas Chromatography/Atmospheric Pressure Chemical Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry of Pyrolysis Oil from German Brown Coal.

    Science.gov (United States)

    Zuber, Jan; Kroll, Marius M; Rathsack, Philipp; Otto, Matthias

    2016-01-01

    Pyrolysis oil from the slow pyrolysis of German brown coal from Schöningen, obtained at a temperature of 500°C, was separated and analyzed using hyphenation of gas chromatography with an atmospheric pressure chemical ionization source operated in negative ion mode and Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS). Development of this ultrahigh-resolving analysis method is described, that is, optimization of specific GC and APCI parameters and performed data processing. The advantages of GC-APCI-FT-ICR-MS hyphenation, for example, soft ionization, ultrahigh-resolving detection, and most important isomer separation, were demonstrated for the sample liquid. For instance, it was possible to separate and identify nine different propylphenol, ethylmethylphenol, and trimethylphenol isomers. Furthermore, homologous series of different acids, for example, alkyl and alkylene carboxylic acids, were verified, as well as homologous series of alkyl phenols, alkyl dihydroxy benzenes, and alkoxy alkyl phenols.

  3. Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    Directory of Open Access Journals (Sweden)

    Jamshed Haneef

    2013-10-01

    Full Text Available Liquid chromatography tandem mass chromatography (LC–MS/MS is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC–MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase as well as different acquisition modes (SIM, MRM for quantitative analysis of glucocorticoids and stimulants. This review is not meant to be exhaustive but rather to provide a general overview for detection and confirmation of target drugs using LC–MS/MS and thus useful in the doping analysis, toxicological studies as well as in pharmaceutical analysis. Keywords: LC–MS/MS, Ionization techniques, Glucocorticoids, Stimulants, Hyphenated techniques, Biological fluid

  4. New Oxford style manual

    CERN Document Server

    2012-01-01

    The New Oxford Style Manual brings together two essential reference works in a single volume: New Hart's Rules and the New Oxford Dictionary for Writers and Editors. New Hart's Rules, Oxford's definitive guide to style, consists of 20 chapters that provide authoritative and expert advice on how to prepare copy for publication. Topics covered include how to use italic, roman, and other type treatments, numbers and dates, law and legal references, illustrations, notes and references, and bibliographies. The guidelines are complemented by the New Oxford Dictionary for Writers and Editors, which features 25,000 alphabetically arranged entries giving authoritative advice on those words and names which raise questions time and time again because of spelling, capitalization, hyphenation, or cultural and historical context. Entries give full coverage of recommended spellings, variant forms, confusable words, hyphenation, capitalization, foreign and specialist terms, proper names, and abbreviations. The dictionary a...

  5. Spojení elektrochemických metod s hmotnostní spektrometrií – potenciál pro analytickou a fyzikální chemii a biochemii

    Czech Academy of Sciences Publication Activity Database

    Jaklová Dytrtová, Jana; Jakl, M.

    2016-01-01

    Roč. 110, č. 1 (2016), s. 31-39 ISSN 0009-2770 R&D Projects: GA ČR GP13-21409P Institutional support: RVO:61388963 Keywords : hyphenation * electrochemistry * mass spectrometry * mimetics Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 0.387, year: 2016 http://www.chemicke-listy.cz/docs/full/2016_01_31-39.pdf

  6. Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    OpenAIRE

    Haneef, Jamshed; Shaharyar, Mohammad; Husain, Asif; Rashid, Mohd; Mishra, Ravinesh; Parveen, Shama; Ahmed, Niyaz; Pal, Manoj; Kumar, Deepak

    2013-01-01

    Liquid chromatography tandem mass chromatography (LCâMS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LCâMS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisiti...

  7. Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    OpenAIRE

    Haneef, Jamshed; Shaharyar, Mohammad; Husain, Asif; Rashid, Mohd; Mishra, Ravinesh; Parveen, Shama; Ahmed, Niyaz; Pal, Manoj; Kumar, Deepak

    2013-01-01

    Liquid chromatography tandem mass chromatography (LC–MS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC–MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisiti...

  8. Purification of drugs from biological fluids by counter-current chromatography.

    Science.gov (United States)

    Hochlowski, Jill E; Pan, Jeffrey Y; Searle, Philip A; Buck, Wayne R; Spanton, Stephen G

    2009-08-21

    Experiments were performed to demonstrate the potential of counter-current chromatography (CCC) for the isolation of drugs and their metabolites from biological matrices relevant to the metabolism studies of pharmaceutical research. Examples of typical drugs are spiked into biological media ex vivo to provide test samples for analysis. A mass spectrometer hyphenated to a CCC allows for the detection of small molecule drugs within the matrix through selected ion monitoring, and fraction collection can provide material for further structural elucidation by NMR.

  9. Raman spectroscopy in pharmaceutical product design

    DEFF Research Database (Denmark)

    Paudel, Amrit; Raijada, Dhara; Rantanen, Jukka

    2015-01-01

    molecular-based drug discovery, design of innovative drug delivery systems and quality control of finished products. This review presents concise accounts of various conventional and emerging Raman instrumentations including associated hyphenated tools of pharmaceutical interest. Moreover, relevant...... application cases of Raman spectroscopy in early and late phase pharmaceutical development, process analysis and micro-structural analysis of drug delivery systems are introduced. Finally, potential areas of future advancement and application of Raman spectroscopic techniques are discussed....

  10. Analytical strategy based on the use of liquid chromatography and gas chromatography with triple-quadrupole and time-of-flight MS analyzers for investigating organic contaminants in wastewater

    OpenAIRE

    Pitarch Arquimbau, María Elena; Portolés Nicolau, Tania; Marín Ramos, José Manuel; Ibáñez Martínez, María; Albarrán, Fernando; Hernández Hernández, Félix

    2010-01-01

    The presence of a wide variety of organic pollutants with different physico-chemical characteristics has been investigated in wastewater samples from a municipal solid waste treatment plant placed at Castellón, Spain. An advanced analytical strategy has been applied, consisting on the combined used of two powerful and complementary techniques, GC and LC, both hyphenated with tandem mass spectrometry with triple quadrupole analyzers. The GC-MS/MS method was based on sample extraction using C18...

  11. Ndel1-derived peptides modulate bidirectional transport of injected beads in the squid giant axon

    Directory of Open Access Journals (Sweden)

    Michal Segal

    2012-01-01

    Bidirectional transport is a key issue in cellular biology. It requires coordination between microtubule-associated molecular motors that work in opposing directions. The major retrograde and anterograde motors involved in bidirectional transport are cytoplasmic dynein and conventional kinesin, respectively. It is clear that failures in molecular motor activity bear severe consequences, especially in the nervous system. Neuronal migration may be impaired during brain development, and impaired molecular motor activity in the adult is one of the hallmarks of neurodegenerative diseases leading to neuronal cell death. The mechanisms that regulate or coordinate kinesin and dynein activity to generate bidirectional transport of the same cargo are of utmost importance. We examined how Ndel1, a cytoplasmic dynein binding protein, may regulate non-vesicular bidirectional transport. Soluble Ndel1 protein, Ndel1-derived peptides or control proteins were mixed with fluorescent beads, injected into the squid giant axon, and the bead movements were recorded using time-lapse microscopy. Automated tracking allowed for extraction and unbiased analysis of a large data set. Beads moved in both directions with a clear bias to the anterograde direction. Velocities were distributed over a broad range and were typically slower than those associated with fast vesicle transport. Ironically, the main effect of Ndel1 and its derived peptides was an enhancement of anterograde motion. We propose that they may function primarily by inhibition of dynein-dependent resistance, which suggests that both dynein and kinesin motors may remain engaged with microtubules during bidirectional transport.

  12. Scleral fibroblast response to experimental glaucoma in mice

    Science.gov (United States)

    Tezel, Gülgün; Cone-Kimball, Elizabeth; Steinhart, Matthew R.; Jefferys, Joan; Pease, Mary E.; Quigley, Harry A.

    2016-01-01

    Purpose To study the detailed cellular and molecular changes in the mouse sclera subjected to experimental glaucoma. Methods Three strains of mice underwent experimental bead-injection glaucoma and were euthanized at 3 days and 1, 3, and 6 weeks. Scleral protein expression was analyzed with liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) using 16O/18O labeling for quantification in 1- and 6-week tissues. Sclera protein samples were also analyzed with immunoblotting with specific antibodies to selected proteins. The proportion of proliferating scleral fibroblasts was quantified with Ki67 and 4’,6-diamidino-2-phenylindole (DAPI) labeling, and selected proteins were studied with immunohistochemistry. Results Proteomic analysis showed increases in molecules involved in integrin-linked kinase signaling and actin cytoskeleton signaling pathways at 1 and 6 weeks after experimental glaucoma. The peripapillary scleral region had more fibroblasts than equatorial sclera (p=0.001, n=217, multivariable regression models). There was a sixfold increase in proliferating fibroblasts in the experimental glaucoma sclera at 1 week and a threefold rise at 3 and 6 weeks (p=0.0005, univariate regression). Immunoblots confirmed increases for myosin, spectrin, and actinin at 1 week after glaucoma. Thrombospondin-1 (TSP-1), HINT1, vimentin, actinin, and α-smooth muscle actin were increased according to immunohistochemistry. Conclusions Scleral fibroblasts in experimental mouse glaucoma show increases in actin cytoskeleton and integrin-related signaling, increases in cell division, and features compatible with myofibroblast transition. PMID:26900327

  13. Cre-expressing neurons in the cortical white matter of Ntsr1-Cre GN220 mice.

    Science.gov (United States)

    Sundberg, Sofie C; Granseth, Björn

    2018-03-23

    Genetically modified mouse strains that express Cre-recombinase in specific neuronal sub-populations have become widely used tools for investigating neuronal function. The Ntsr1-Cre GN220 mouse expresses this enzyme in corticothalamic neurons in layer 6 of cerebral cortex. We observed that about 7% of Cre-expressing cells in the primary visual cortex are found within the white matter bordering layer 6. By using the immunohistochemical marker for layer 6 neurons, Forkhead box protein 2 (FoxP2), and fluorescently conjugated latex beads injected into the dorsal lateral geniculate nucleus, we show that about half of these cells are similar to and could belong to the layer 6 corticothalamic neuron population. The other half seems to be a distinct white matter (WM) neuron sub-population that we estimate to constitute 2-4% of the total cortical Cre-expressing population. Staining for the neuronal marker Neuronal nuclei (NeuN) revealed that about 15-40% of WM neurons are Cre-expressing. Thus, the potential contribution from WM neurons needs to be considered when interpreting the results from experiments using the Ntsr1-Cre GN220 mouse for investigating corticothalamic neuronal function. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Bead-Based Microfluidic Sediment Analogues: Fabrication and Colloid Transport.

    Science.gov (United States)

    Guo, Yang; Huang, Jingwei; Xiao, Feng; Yin, Xiaolong; Chun, Jaehun; Um, Wooyong; Neeves, Keith B; Wu, Ning

    2016-09-13

    Mobile colloids can act as carriers for low-solubility contaminants in the environment. However, the dominant mechanism for this colloid-facilitated transport of chemicals is unclear. Therefore, we developed a bead-based microfluidic platform of sediment analogues and measured both single and population transport of model colloids. The porous medium is assembled through a bead-by-bead injection method. This approach has the versatility to build both electrostatically homogeneous and heterogeneous media at the pore scale. A T-junction at the exit also allowed for encapsulation and enumeration of colloids effluent at single particle resolution to give population dynamics. Tortuosity calculated from pore-scale trajectory analysis and its comparison with lattice Boltzmann simulations revealed that transport of colloids was influenced by the size exclusion effect. The porous media packed by positively and negatively charged beads into two layers showed distinctive colloidal particle retention and significant remobilization and re-adsorption of particles during water flushing. We demonstrated the potential of our method to fabricate porous media with surface heterogeneities at the pore scale. With both single and population dynamics measurement, our platform has the potential to connect pore-scale and macroscale colloid transport on a lab scale and to quantify the impact of grain surface heterogeneities that are natural in the subsurface environment.

  15. Size exclusion and anion exchange high performance liquid chromatography for characterizing metals bound to marine dissolved organic matter

    International Nuclear Information System (INIS)

    García-Otero, Natalia; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2013-01-01

    Highlights: ► Fractionation methods for assessing metals bound to marine DOM were developed. ► SEC and AEC with UV detection and hyphenated with inductively coupled plasma-mass spectrometry were used. ► SEC-UV showed marine DOM of molecular weights from 16 to 1 kDa. ► Cobalt, manganese, strontium and zinc are bound to marine DOM. - Abstract: Size exclusion chromatography (SEC) followed by anion exchange chromatography (AEC) hyphenated with inductively coupled plasma-mass spectrometry (ICP-MS) was applied for fractionating metals bound to marine dissolved organic matter (DOM). Surface seawater samples (100 L) were subjected to tangential flow ultrafiltration (10,000 Da cut off) for isolating and pre-concentrating dissolved large molecules. The isolated fraction (retentate) consisted of 1 L, which was further freeze-dried and re-dissolved to 250 mL with ultrapure water. After HI Trap desalting of the re-dissolved retentate, SEC with UV detection showed marine DOM ranging from 6.5 kDa (lower than the permeable volume of the SEC column) to 16 kDa. A further characterization of this fraction by AEC with UV detection revealed the existence of four groups of macromolecules exhibiting retention times of 2.3, 2.8, 4.5 and 14.0 min. AEC hyphenated with ICP-MS showed the presence of strontium and zinc in the first AE fraction isolated from the SEC fraction; while manganese was found to be bound to the second AE fraction. Cobalt was found to be bound to molecules comprising the third AE fraction.

  16. Size exclusion and anion exchange high performance liquid chromatography for characterizing metals bound to marine dissolved organic matter

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Otero, Natalia; Bermejo-Barrera, Pilar [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela (Spain); Moreda-Pineiro, Antonio, E-mail: antonio.moreda@usc.es [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela (Spain)

    2013-01-14

    Highlights: Black-Right-Pointing-Pointer Fractionation methods for assessing metals bound to marine DOM were developed. Black-Right-Pointing-Pointer SEC and AEC with UV detection and hyphenated with inductively coupled plasma-mass spectrometry were used. Black-Right-Pointing-Pointer SEC-UV showed marine DOM of molecular weights from 16 to 1 kDa. Black-Right-Pointing-Pointer Cobalt, manganese, strontium and zinc are bound to marine DOM. - Abstract: Size exclusion chromatography (SEC) followed by anion exchange chromatography (AEC) hyphenated with inductively coupled plasma-mass spectrometry (ICP-MS) was applied for fractionating metals bound to marine dissolved organic matter (DOM). Surface seawater samples (100 L) were subjected to tangential flow ultrafiltration (10,000 Da cut off) for isolating and pre-concentrating dissolved large molecules. The isolated fraction (retentate) consisted of 1 L, which was further freeze-dried and re-dissolved to 250 mL with ultrapure water. After HI Trap desalting of the re-dissolved retentate, SEC with UV detection showed marine DOM ranging from 6.5 kDa (lower than the permeable volume of the SEC column) to 16 kDa. A further characterization of this fraction by AEC with UV detection revealed the existence of four groups of macromolecules exhibiting retention times of 2.3, 2.8, 4.5 and 14.0 min. AEC hyphenated with ICP-MS showed the presence of strontium and zinc in the first AE fraction isolated from the SEC fraction; while manganese was found to be bound to the second AE fraction. Cobalt was found to be bound to molecules comprising the third AE fraction.

  17. On-line sample processing methods in flow analysis

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald

    2008-01-01

    In this chapter, the state of the art of flow injection and related approaches thereof for automation and miniaturization of sample processing regardless of the aggregate state of the sample medium is overviewed. The potential of the various generation of flow injection for implementation of in-line...... dilution, derivatization, separation and preconcentration methods encompassing solid reactors, solvent extraction, sorbent extraction, precipitation/coprecipitation, hydride/vapor generation and digestion/leaching protocols as hyphenated to a plethora of detection devices is discussed in detail...

  18. Occurrence, biological activities and {sup 13}C NMR data of amides from Piper (Piperaceae)

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Jeferson C. do; Paula, Vanderlucia F. de [Universidade Estadual do Sudoeste da Bahia, Jequie, BA (Brazil). Dept. de Quimica e Exatas; David, Jorge M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; David, Juceni P., E-mail: jmdavid@ufba.br [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Fac. de Farmacia

    2012-07-01

    This manuscript describes an update review with up to 285 references concerning the occurrence of amides from a variety of species of the genus Piper (Piperaceae). Besides addressing occurrence, this review also describes the biological activities attributed to extracts and pure compounds, a compiled {sup 13}C NMR data set, the main correlations between structural and NMR spectroscopic data of these compounds, and employment of hyphened techniques such as LC-MS, GC-MS and NMR for analysis of amides from biological samples and crude Piper extracts. (author)

  19. [Processing GC-FTIR by the blind source separation].

    Science.gov (United States)

    Yao, Zhi-Xiang; Huang, Hong; Liu, Huan-Bin

    2006-08-01

    An analysis method for separating chromatographic overlapped peaks and purifying infrared spectra is put forward, based on the blind source separation technique and the multi-dimensional data of GC-FTIR, Using various information from hyphenated instruments, this method was used to separate completely a organic mixture, the xylene isomerism system, a problem unable to solve usually. The method can confirm the rationality of theory and algorithm and give integral explanations of the independent component analysis data. The reason for the error in quantitative analysis is discussed.

  20. Ionophores in the Environment

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Björklund, Erland

    , and ground waters, due to their continuously increased and constant application as feed additives in modern livestock production. This presentation will focus on the development of new analytical method for determination of ionophores in liquid and solid matrices. The hyphenated method consist of pressurised...... liquid extraction with integrated clean-up followed by solid phase extraction and high-performance liquid chromatography tandem in space mass spectrometry (PLE-SPE-LC-MS/MS). Halling-Sørensen B, Sengelov G, Tjornelund J (2002) Arch Environ Contam Toxicol, 42: 3, p. 263-271. DOI: 10.1007/s00244...

  1. Appendices on provisional nomenclature, symbols, terminology and conventions - number 55

    International Nuclear Information System (INIS)

    1976-01-01

    Ten numerically-based syllables (nil, un, bi, etc) are used to provide recommended names of elements of atomic numbers greater than 100. The symbol of the element is composed of the initial letters of the numerical roots which make up the name. Abbreviated forms of the names of elements 101 to 199 are proposed. Thus: element 105 would be named Un-nil-pentium [hyphens not part of name but shown in the recommendatoins to assist comprehension], symbol Unp, abbreviation Pentium. (U.K.)

  2. Occurrence, biological activities and 13C NMR data of amides from Piper (Piperaceae

    Directory of Open Access Journals (Sweden)

    Jeferson C. do Nascimento

    2012-01-01

    Full Text Available This manuscript describes an update review with up to 285 references concerning the occurrence of amides from a variety of species of the genus Piper (Piperaceae. Besides addressing occurrence, this review also describes the biological activities attributed to extracts and pure compounds, a compiled 13C NMR data set, the main correlations between structural and NMR spectroscopic data of these compounds, and employment of hyphened techniques such as LC-MS, GC-MS and NMR for analysis of amides from biological samples and crude Piper extracts.

  3. Shared Task System Description: Frustratingly Hard Compositionality Prediction

    DEFF Research Database (Denmark)

    Johannsen, Anders Trærup; Martinez Alonso, Hector; Rishøj, Christian

    2011-01-01

    We considered a wide range of features for the DiSCo 2011 shared task about compositionality prediction for word pairs, including COALS-based endocentricity scores, compositionality scores based on distributional clusters, statistics about wordnet-induced paraphrases, hyphenation......, and the likelihood of long translation equivalents in other languages. Many of the features we considered correlated significantly with human compositionality scores, but in support vector regression experiments we obtained the best results using only COALS-based endocentricity scores. Our system was nevertheless...

  4. Extraction and detection of Ionophores in the Aquatic Environment

    DEFF Research Database (Denmark)

    Bak, Søren Alex; Hansen, Martin; Krogh, Kristine Andersen

    . Coccidiosis is a major disease in poultry as well as in many other hosts. Ionophores are the most heavily applied sup-group of the two sub-groups of anticoccidial agents, because they also have antibacterial properties. After the ban of antibiotic growth promoters Ionophores are used extensively worldwide...... compounds on the soil bacterial community (Halling-Sørensen et al. 2002; Hansen et al. 2009c). The focus of the present study is on the recent advances of a new analytical method for sampling, extraction and detection of ionophores in liquid matrices. The hyphenated method consists of an integrated clean...

  5. Some tools to implement linguistics applications oriented to the Romanian language

    Directory of Open Access Journals (Sweden)

    Elena Boian

    1996-09-01

    Full Text Available In the article the Romanian Spelling Pack is proposed which is a set of dynamic link libraries work under MS Windows. They implement checking a Romanian word against the vocabulary base; search through word base for one close to a given word; Romanian hyphenation; user vocabulary extension; Romanian word inflection. These procedures can be used in processing Romanian texts in Windows environment and in writing interface and tutorial programs for the Romanian language. As an example of the approach, Romanian spelling checker for MS Word 6.0 is described.

  6. Mass spectrometry at the Pittsburgh conference

    International Nuclear Information System (INIS)

    Borman, S.

    1987-01-01

    Each year analytical chemists flock to the Pittsburgh Conference to learn about the latest trends in analytical instrumentation. In this Focus, a number of prominent mass spectroscopists who attended this year's meeting in Atlantic City, NJ, discuss their perceptions of current developments in the field of mass spectrometry (MS). In the June 1 issue of Analytical Chemistry, the authors coverage of the Pittsburgh Conferences continues with a follow-up article on specific developments in hyphenated mass spectrometry - primarily liquid chromatography - MS (LC/MS) and gas chromatography - infrared spectrometry MS (GC/IR/MS)

  7. Analysis of nanoparticles using the ICAP Q ICP-MS

    DEFF Research Database (Denmark)

    Kutscher, Daniel; McSheehy-Ducos, Shona; Lindemann, Torsten

    2014-01-01

    The analysis of Nanoparticles (NPs) has become one of the hot topics in analytical chemistry. However, detailed knowledge about potential risks or hazards is still unavailable. Two approaches have been developed in recent years using ICP-MS as a detection system: hyphenation of an appropriate...... be analyzed. In this presentation, the basic terms of both techniques will be presented. The key benefits and drawbacks of each technique are illustrated in results from samples contain NPs of different structure and size. The challenges that remain for the characterization of NPs in real samples...

  8. Genes for 7S RNAs can replace the gene for 4.5S RNA in growth of Escherichia coli

    DEFF Research Database (Denmark)

    Brown, S

    1991-01-01

    4.5S RNAs of eubacteria and 7S RNAs of archaebacteria and eukaryotes exist in a hairpin conformation. The apex of this hairpin displays structural and sequence similarities among both 4.5S and 7S RNAs. Furthermore, a hyphenated sequence of 16 nucleotides is conserved in all eubacterial 4.5S RNAs...... examined. In this article I report that 7S RNAs that contain this 16-nucleotide sequence are able to replace 4.5S RNAs and permit growth of Escherichia coli....

  9. Dual High-Resolution α-Glucosidase and Radical Scavenging Profiling Combined with HPLC-HRMS-SPE-NMR for Identification of Minor and Major Constituents Directly from the Crude Extract of Pueraria lobata

    DEFF Research Database (Denmark)

    Liu, Bingrui; Kongstad, Kenneth Thermann; Qinglei, Sun

    2015-01-01

    The crude methanol extract of Pueraria lobata was investigated by dual high-resolution α-glucosidase inhibition and radical scavenging profiling combined with hyphenated HPLC-HRMS-SPE-NMR. Direct analysis of the crude extract without preceding purification was facilitated by combining chromatograms...... chromatogram of the crude methanol extract. Subsequent HPLC-HRMS-SPE-NMR analysis allowed identification of 21 known compounds in addition to two new compounds, i.e., 3′-methoxydaidzein 8-C-[α-d-apiofuranosyl-(1→6)]-β-d-glucopyranoside and 6″-O-malonyl-3′-methoxydaidzin, as well as an unstable compound...

  10. Triple aldose reductase/α-glucosidase/radical scavenging high-resolution profiling combined with high-performance liquid chromatography – high-resolution mass spectrometry – solid-phase extraction – nuclear magnetic resonance spectroscopy for identification of antidiabetic constituents in crude, extract of Radix Scutellariae

    DEFF Research Database (Denmark)

    Tahtah, Yousof; Kongstad, Kenneth Thermann; Wubshet, Sileshi Gizachew

    2015-01-01

    /α-glucosidase/radical scavenging high-resolution inhibition profile - allowing proof of concept with Radix Scutellariae crude extract as a polypharmacological herbal drug. The triple bioactivity high-resolution profiles were used to pinpoint bioactive compounds, and subsequent structure elucidation was performed with hyphenated...... high-performance liquid chromatography – high-resolution mass spectrometry – solid-phase extraction – nuclear magnetic resonance spectroscopy. The only α-glucosidase inhibitor was baicalein, whereas main aldose reductase inhibitors in the crude extract were baicalein and skullcapflavone II, and main...

  11. Targeted natural product isolation guided by HPLC-SPE-NMR: Constituents of Hubertia species

    DEFF Research Database (Denmark)

    Sprogoe, K.; Staek, D.; Jager, A.K.

    2007-01-01

    The hyphenated technique, high-performance liquid chromatography-solid-phase extraction-nuclear magnetic resonance spectroscopy (HPLC-SPE-NMR), has been applied for rapid identification of novel natural products in crude extracts of Hubertia ambavilla and Hubertia tomentosa. The technique allowed...... full or partial identification of all major extract constituents and demonstrated the presence of unusual quinic acid derivatives containing the (1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl residue that exhibit strongly coupled ABXY patterns, the parameters of which were obtained by spin simulations...

  12. Separation and identification of multiple constituents in Xiao Chai Hu Decoction (Sho-saiko-to) by bioactivity-guided fractionation combined with LC-ESI-QTOFMS/MS.

    Science.gov (United States)

    Wu, Yingying; Peng, Ying; Song, Cui; Li, Lingzhi; Ma, Hui; Li, Danqi; Wang, Fang; Yang, Jingyu; Song, Shaojiang; Wu, Chunfu

    2015-08-01

    Xiao Chai Hu Decoction (XCHD), named Sho-saiko-to in Japanese, is a well-known traditional Chinese medicine formula used in Asia. However, the characterization methods used in the past have lacked sensitivity and the nature of the active constituents of XCHD remains unclear. This study was carried out to establish the hyphenated method of bioactivity-guided fractionation and liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (LC-ESI-QTOFMS/MS) in order to identify the major bioactive constituents of XCHD. D101 macroporous resin was used to separate and enrich the material base into four fractions, XCHD-1, XCHD-2, XCHD-3 and XCHD-4. Each fraction was then evaluated for its antidepressant effect using depression-related parameters. An LC-ESI-QTOFMS/MS method in both positive and negative ion mode was also applied for separation and identification of the biological active fractions of XCHD. As a result, 79 compounds including polysaccharides, flavonoids, saikosaponins, ginsenosides, licoricesaponins and gingerols were detected, 69 of them were identified or tentatively characterized. Based on our preliminary characterization investigations, polysaccharides, gingerols and flavonoids in XCHD may contribute to the antidepressant effect of XCHD. In conclusion, the hyphenated method of bioactivity-guided fractionation and LC-ESI-QTOFMS/MS was meaningful for the isolation and preliminary identification of the biological active components in complex matrices of traditional Chinese medicine. Copyright © 2014 John Wiley & Sons, Ltd.

  13. Horseradish peroxidase and antibody labeled gold nanoparticle probe for amplified immunoassay of ciguatoxin in fish samples based on capillary electrophoresis with electrochemical detection.

    Science.gov (United States)

    Zhang, Zhaoxiang; Liu, Ying; Zhang, Chaoying; Luan, Wenxiu

    2015-03-01

    This paper describes a new amplified immunoassay with horseradish peroxidase (HRP) and antibody (Ab) labeled gold nanoparticles (AuNPs) probe hyphenated to capillary electrophoresis (CE) with electrochemical (EC) detection for ultrasensitive determination of ciguatoxin CTX1B. AuNPs were conjugated with HRP and Ab, and then incubated with limited amount of CTX1B to produce immunocomplex. The immunoreactive sample was injected into capillary for CE separation and EC detection. Enhanced sensitivity was obtained by adopting the AuNPs as carriers of HRP and Ab at high HRP/Ab molar ratio. The calibration curve of CTX1B was in the range of 0.06-90 ng/mL. The detection limit was 0.045 ng/mL, which is 38-fold lower than that of HPLC-MS method for CTX1B analysis. The proposed method was successfully applied for the quantification of CTX1B in contamined fish samples by simultaneously labeling Ab and HRP on AuNPs. The amplified IA with HRP and Ab labeled AuNPs probe hyphenated to CE and EC detection provides a sensitive analytical approach for the determination of trace ciguatoxin in complex samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. A Practical Guide on Coupling a Scanning Mobility Sizer and Inductively Coupled Plasma Mass Spectrometer (SMPS-ICPMS)

    Science.gov (United States)

    Tarik, Mohamed; Foppiano, Debora; Hess, Adrian; Ludwig, Christian

    2017-01-01

    A large variety of analytical methods are available to characterize particles in aerosols and suspensions. The choice of the appropriate technique depends on the properties to be determined. In many fields information about particle size and chemical composition are of great importance. While in aerosol techniques particle size distributions of gas-borne particles are determined online, their elemental composition is commonly analyzed offline after an appropriate sampling and preparation procedure. To obtain both types of information online and simultaneously, a hyphenated setup was recently developed, including a Scanning Mobility Particle Sizer (SMPS) and an Inductively Coupled Plasma Mass Spectrometer (ICPMS). This allows first to classify the particles with respect to their mobility diameter, and then to determine their number concentration and elemental composition in parallel. A Rotating Disk Diluter (RDD) is used as the introduction system, giving more flexibility regarding the use of different aerosol sources. In this work, a practical guide is provided describing the different steps for establishing this instrumentation, and how to use this analysis tool. The versatility of this hyphenated technique is demonstrated in example measurements on three different aerosols generated out of a) a salt solution, b) a suspension, and c) emitted by a thermal process. PMID:28745635

  15. WFST-based ground truth alignment for difficult historical documents with text modification and layout variations

    Science.gov (United States)

    Al Azawi, Mayce; Liwicki, Marcus; Breuel, Thomas M.

    2013-01-01

    This work proposes several approaches that can be used for generating correspondences between real scanned books and their transcriptions which might have different modifications and layout variations, also taking OCR errors into account. Our approaches for the alignment between the manuscript and the transcription are based on weighted finite state transducers (WFST). In particular, we propose adapted WFSTs to represent the transcription to be aligned with the OCR lattices. The character-level alignment has edit rules to allow edit operations (insertion, deletion, substitution). Those edit operations allow the transcription model to deal with OCR segmentation and recognition errors, and also with the task of aligning with different text editions. We implemented an alignment model with a hyphenation model, so it can adapt the non-hyphenated transcription. Our models also work with Fraktur ligatures, which are typically found in historical Fraktur documents. We evaluated our approach on Fraktur documents from Wanderungen durch die Mark Brandenburg" volumes (1862-1889) and observed the performance of those models under OCR errors. We compare the performance of our model for three different scenarios: having no information about the correspondence at the word (i), line (ii), sentence (iii) or page (iv) level.

  16. Arsenic, Antimony, Chromium, and Thallium Speciation in Water and Sediment Samples with the LC-ICP-MS Technique

    Directory of Open Access Journals (Sweden)

    Magdalena Jabłońska-Czapla

    2015-01-01

    Full Text Available Chemical speciation is a very important subject in the environmental protection, toxicology, and chemical analytics due to the fact that toxicity, availability, and reactivity of trace elements depend on the chemical forms in which these elements occur. Research on low analyte levels, particularly in complex matrix samples, requires more and more advanced and sophisticated analytical methods and techniques. The latest trends in this field concern the so-called hyphenated techniques. Arsenic, antimony, chromium, and (underestimated thallium attract the closest attention of toxicologists and analysts. The properties of those elements depend on the oxidation state in which they occur. The aim of the following paper is to answer the question why the speciation analytics is so important. The paper also provides numerous examples of the hyphenated technique usage (e.g., the LC-ICP-MS application in the speciation analysis of chromium, antimony, arsenic, or thallium in water and bottom sediment samples. An important issue addressed is the preparation of environmental samples for speciation analysis.

  17. ISIDORE, a probe for in situ trace metal speciation based on Donnan membrane technique with related electrochemical detection part 1: Equilibrium measurements

    Energy Technology Data Exchange (ETDEWEB)

    Parat, Corinne, E-mail: corinne.parat@univ-pau.fr [Université de Pau et des Pays de l’Adour, CNRS UMR 5254, LCABIE, 64000 Pau (France); Pinheiro, J.P. [Université de Lorraine/ENSG, CNRS UMR 7360, LIEC, 54500 Nancy (France)

    2015-10-08

    This work presents the development of a new probe (ISIDORE probe) based on the hyphenation of a Donnan Membrane Technique device (DMT) to a screen-printed electrode through a flow-cell to determine the free zinc, cadmium and lead ion concentration in natural samples, such as a freshwater river. The probe displays many advantages namely: (i) the detection can be performed on-site, which avoids all problems inherent to sampling, transport and storage; (ii) the low volume of the acceptor solution implies shorter equilibration times; (ii) the electrochemical detection system allows monitoring the free ion concentration in the acceptor solution without sampling. - Highlights: • A new probe has been developed for on-site analyses of free metal ion. • A screen-printed electrode has been hyphenated to a DMT device. • Analysis time has been reduced to 6H against 36H when using a classical DMT device. • This new probe has been successfully applied on a synthetic freshwater sample.

  18. Engenharia de Software – Essencial para próximas décadas

    Directory of Open Access Journals (Sweden)

    Antonio Mendes Silva Filho

    2011-06-01

    Full Text Available Engenharia compreende o uso de princípios e conhecimento empírico e científico obtidos a partir de estudos, investigações e experiências visando o desenvolvimento de um produto, que dependendo da área pode ser um motor, um dispositivo eletrônico, um prédio ou um sistema de software. Para tanto, três aspectos essenciais devem ser considerados: custo (orçamento de desenvolvimento, tempo (cronograma de execução e qualidade. Dentro deste contexto, a engenharia de software (a exemplo de outras engenharia também visa o desenvolvimento de um produto (software que pressupõe satisfazer aos requisitos de qualidade, dentro do prazo e sem estourar o orçamento. Nesse sentido, este artigo destaca que o profissional de engenharia de sofware é crucial para momento atual e também será durante as próximas décadas, esteja ele atuando como analista, desenvolvedor ou gerente de equipe de projeto.

  19. Review on ion mobility spectrometry. Part 1: current instrumentation.

    Science.gov (United States)

    Cumeras, R; Figueras, E; Davis, C E; Baumbach, J I; Gràcia, I

    2015-03-07

    Ion Mobility Spectrometry (IMS) is a widely used and 'well-known' technique of ion separation in the gaseous phase based on the differences in ion mobilities under an electric field. All IMS instruments operate with an electric field that provides space separation, but some IMS instruments also operate with a drift gas flow that provides also a temporal separation. In this review we will summarize the current IMS instrumentation. IMS techniques have received an increased interest as new instrumentation and have become available to be coupled with mass spectrometry (MS). For each of the eight types of IMS instruments reviewed it is mentioned whether they can be hyphenated with MS and whether they are commercially available. Finally, out of the described devices, the six most-consolidated ones are compared. The current review article is followed by a companion review article which details the IMS hyphenated techniques (mainly gas chromatography and mass spectrometry) and the factors that make the data from an IMS device change as a function of device parameters and sampling conditions. These reviews will provide the reader with an insightful view of the main characteristics and aspects of the IMS technique.

  20. Educação politécnica ou educação política nas condições atuais do trabalho

    Directory of Open Access Journals (Sweden)

    José Mario Angeli

    2009-11-01

    Full Text Available Nestes tempos recentes, tornou-se freqüente no pensamento social, decretar o fim do trabalhoe, consequentemente, asseverar a crise vivida pelas teorias alicerçadas nesta categoria, dentre as quais particularmente a teoria marxista, cujo materialismo histórico por ela concebido repousa no trabalho.

  1. China - 60 anos de República Popular

    Directory of Open Access Journals (Sweden)

    Wladimir Pomar

    2009-10-01

    Full Text Available Em dezembro de 1949, após mais de 23 anos de guerras, tanto civis, quanto de resistência contra a agressão japonesa, a China assistiu à fundação da República Popular, com a vitória do Exército Popular de Libertação, tendo à frente o Partido Comunista, sobre os exércitos comandados pelo Guomindang.

  2. Mass Spectrometry Applications for Toxicology.

    Science.gov (United States)

    Mbughuni, Michael M; Jannetto, Paul J; Langman, Loralie J

    2016-12-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MS n ) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology.

  3. Arsenic, Antimony, Chromium, and Thallium Speciation in Water and Sediment Samples with the LC-ICP-MS Technique

    Science.gov (United States)

    Jabłońska-Czapla, Magdalena

    2015-01-01

    Chemical speciation is a very important subject in the environmental protection, toxicology, and chemical analytics due to the fact that toxicity, availability, and reactivity of trace elements depend on the chemical forms in which these elements occur. Research on low analyte levels, particularly in complex matrix samples, requires more and more advanced and sophisticated analytical methods and techniques. The latest trends in this field concern the so-called hyphenated techniques. Arsenic, antimony, chromium, and (underestimated) thallium attract the closest attention of toxicologists and analysts. The properties of those elements depend on the oxidation state in which they occur. The aim of the following paper is to answer the question why the speciation analytics is so important. The paper also provides numerous examples of the hyphenated technique usage (e.g., the LC-ICP-MS application in the speciation analysis of chromium, antimony, arsenic, or thallium in water and bottom sediment samples). An important issue addressed is the preparation of environmental samples for speciation analysis. PMID:25873962

  4. NRC [Nuclear Regulatory Commission] editorial style guide

    International Nuclear Information System (INIS)

    Beeson, J.F.; Calure, B.A.; Gable, D.; Lesar, M.T.; Mejac, M.F.; Sanders, R.F.

    1989-10-01

    Editorial style refers to the choices that writers, editors, and secretaries make to eliminate inconsistencies in their documents. These choices apply to the recurrent features of a document such as abbreviations, capitalization, compound words, numbers, symbols, and punctuation, as well as to references and footnotes. Making these choices is sometimes difficult because usage changes as the language evolves. Consider the use of hyphens, for example. Do we write non-power reactor or nonpower reactor? Is it on-site incident or onsite incident? Although usage is moving away from the use of hyphens with prefixes, the authorities who compile style guides do not always agree about which choice to use at a given time. Moreover, each discipline -- law, physics, mathematics -- has specific standards that apply to the publications for that discipline. Even in an area as seemingly certain as spelling, overlapping usage exists. Reputable dictionaries show both ''align'' and ''aline'' as correct spellings. Likewise, ''disc, disk, and diskette'' currently coexist as equally valid choices

  5. Development of salt-tolerance interface for an high performance liquid chromatography/inductively coupled plasma mass spectrometry system and its application to accurate quantification of DNA samples.

    Science.gov (United States)

    Takasaki, Yuka; Sakagawa, Shinnosuke; Inagaki, Kazumi; Fujii, Shin-Ichiro; Sabarudin, Akhmad; Umemura, Tomonari; Haraguchi, Hiroki

    2012-02-03

    Accurate quantification of DNA is highly important in various fields. Determination of phosphorus by ICP-MS is one of the most effective methods for accurate quantification of DNA due to the fixed stoichiometry of phosphate to this molecule. In this paper, a smart and reliable method for accurate quantification of DNA fragments and oligodeoxythymidilic acids by hyphenated HPLC/ICP-MS equipped with a highly efficient interface device is presented. The interface was constructed of a home-made capillary-attached micronebulizer and temperature-controllable cyclonic spray chamber (IsoMist). As a separation column for DNA samples, home-made methacrylate-based weak anion-exchange monolith was employed. Some parameters, which include composition of mobile phase, gradient program, inner and outer diameters of capillary, temperature of spray chamber etc., were optimized to find the best performance for separation and accurate quantification of DNA samples. The proposed system could achieve many advantages, such as total consumption for small amount sample analysis, salt-tolerance for hyphenated analysis, high accuracy and precision for quantitative analysis. Using this proposed system, the samples of 20 bp DNA ladder (20, 40, 60, 80, 100, 120, 140, 160, 180, 200, 300, 400, 500 base pairs) and oligodeoxythymidilic acids (dT(12-18)) were rapidly separated and accurately quantified. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Multidrug analysis of pharmaceutical and urine matrices by on-line coupled capillary electrophoresis and triple quadrupole mass spectrometry.

    Science.gov (United States)

    Maráková, Katarína; Piešt'anský, Juraj; Veizerová, Lucia; Galba, Jaroslav; Dokupilová, Svetlana; Havránek, Emil; Mikuš, Peter

    2013-06-01

    The present work illustrates potentialities of CE hyphenated with MS/MS for the simultaneous determination and identification of a mixture of simultaneously acting drugs in pharmaceutical and biological matrices. Here, the hyphenation was provided by ESI interface, while the MS/MS technique was based on the triple quadrupole configuration. Three drugs, namely pheniramine, phenylephrine, and paracetamol were determined and identified with high reliability due to their characterization in three different dimensions, i.e. electrophoresis and MS/MS, that prevented practically any interference. Appropriately selected transitions of the analytes (parent ion-quantifier product ion-qualifier product ion) provided their selective determination at maximum S/N. The proposed CE-MS/MS method was validated (LOD/LOQ, linearity, precision, recovery, accuracy) and applied for (i) the multidrug composition pharmaceuticals, namely Theraflu®, and (ii) human urine taken after per-oral administration of the same pharmaceutical preparation. The method was applied also for the investigation of potential weak associates of the drugs and monitoring of predicted (bio)degradation products of the drugs. Successful validation and application of the proposed method suggest its routine use in highly effective and reliable advanced drug control and biomedical research. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Two distinct populations of projection neurons in the rat lateral parafascicular thalamic nucleus and their cholinergic responsiveness.

    Science.gov (United States)

    Beatty, J A; Sylwestrak, E L; Cox, C L

    2009-08-04

    The lateral parafascicular nucleus (lPf) is a member of the intralaminar thalamic nuclei, a collection of nuclei that characteristically provides widespread projections to the neocortex and basal ganglia and is associated with arousal, sensory, and motor functions. Recently, lPf neurons have been shown to possess different characteristics than other cortical-projecting thalamic relay neurons. We performed whole cell recordings from lPf neurons using an in vitro rat slice preparation and found two distinct neuronal subtypes that were differentiated by distinct morphological and physiological characteristics: diffuse and bushy. Diffuse neurons, which had been previously described, were the predominant neuronal subtype (66%). These neurons had few, poorly-branching, extended dendrites, and rarely displayed burst-like action potential discharge, a ubiquitous feature of thalamocortical relay neurons. Interestingly, we discovered a smaller population of bushy neurons (34%) that shared similar morphological and physiological characteristics with thalamocortical relay neurons of primary sensory thalamic nuclei. In contrast to other thalamocortical relay neurons, activation of muscarinic cholinergic receptors produced a membrane hyperpolarization via activation of M(2) receptors in most lPf neurons (60%). In a minority of lPf neurons (33%), muscarinic agonists produced a membrane depolarization via activation of predominantly M(3) receptors. The muscarinic receptor-mediated actions were independent of lPf neuronal subtype (i.e. diffuse or bushy neurons); however the cholinergic actions were correlated with lPf neurons with different efferent targets. Retrogradely-labeled lPf neurons from frontal cortical fluorescent bead injections primarily consisted of bushy type lPf neurons (78%), but more importantly, all of these neurons were depolarized by muscarinic agonists. On the other hand, lPf neurons labeled by striatal injections were predominantly hyperpolarized by muscarinic

  8. Dispersed particle extraction--a new procedure for trace element enrichment from natural aqueous samples with subsequent ICP-OES analysis.

    Science.gov (United States)

    Bauer, Gerald; Neouze, Marie-Alexandra; Limbeck, Andreas

    2013-01-15

    A novel sample pre-treatment method for multi trace element enrichment from environmental waters prior to optical emission spectrometry analysis with inductively coupled plasma (ICP-OES) is proposed, based on dispersed particle extraction (DPE). This method is based on the use of silica nanoparticles functionalized with strong cation exchange ligands. After separation from the investigated sample solution, the nanoparticles used for the extraction are directly introduced in the ICP for measurement of the adsorbed target analytes. A prerequisite for the successful application of the developed slurry approach is the use of sorbent particles with a mean size of 500 nm instead of commercially available μm sized beads. The proposed method offers the known advantages of common bead-injection (BI) techniques, and further circumvents the elution step required in conventional solid phase extraction procedures. With the use of 14.4 mL sample and addition of ammonium acetate buffer and particle slurry limits of detection (LODs) from 0.03 μg L(-1) for Be to 0.48 μg L(-1) for Fe, with relative standard deviations ranging from 1.7% for Fe and 5.5% for Cr and an average enrichment factor of 10.4 could be achieved. By implementing this method the possibility to access sorbent materials with irreversible bonding mechanisms for sample pre-treatment is established, thus improvements in the selectivity of sample pre-treatment procedures can be achieved. The presented procedure was tested for accuracy with NIST standard reference material 1643e (fresh water) and was applied to drinking water samples from the vicinity of Vienna. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. LC-NMR: profiling and dereplication of natural product extracts

    International Nuclear Information System (INIS)

    Urban, Sylvia

    2006-01-01

    mixtures can also be achieved by the application of sophisticated hyphenated spectroscopic techniques. Hyphenated techniques offer an efficient scheme for the chemical screening of extracts required to detect new leads, which potentially can be interesting from a chemical viewpoint. The direct hyphenation of an efficient separation technique with powerful spectroscopic methods has great potential to speed up the dereplication process

  10. Mental illness in the nursing workplace: a collective autoethnography.

    Science.gov (United States)

    Kidd, Jacquie Dianne; Finlayson, Mary P

    2010-01-01

    Many nurses are burned out, exhausted and have a high intent to leave their jobs. These factors, when experienced over a period of time, are consistent with the development of mental illness. This study takes a collective autoethnographical approach to mental illness in the nursing workplace by focusing on the stories of nurses who have experienced mental illness in clinical practice. It highlights three ways in which nursing and mental illness are connected; the nurse who is vulnerable to mental illness prior to entering the profession, the nurse who develops mental illness that is independent of her work but is nevertheless impacted by it, and the nurse who develops mental illness as a result of her work and/or role. This paper explores the hyphenated lives and bullying these nurses experience, and recommends strategies that the profession, employing organisations, and individuals can adopt to reduce nurses' progression from stress to distress and mental illness.

  11. The role of visual acuity and segmentation cues in compound word identification

    Directory of Open Access Journals (Sweden)

    Jukka eHyönä

    2012-06-01

    Full Text Available Studies are reviewed that demonstrate how the foveal area of the eye constrains how compound words are identified during reading. When compound words are short, their letters can be identified during a single fixation, leading to the whole-word route dominating word recognition from early on. Hence, visually marking morpheme boundaries by hyphens slows down processing by encouraging morphological decomposition when holistic processing is a feasible option. In contrast, the decomposition route dominates the early stages of identifying long compound words. Thus, visual marking of morpheme boundaries facilitates processing of long compound words, unless the initial fixation made on the word lands very close to the morpheme boundary. The reviewed pattern of results is explained by the visual acuity principle (Bertram & Hyönä, 2003 and the dual-route framework of morphological processing.

  12. Vigo, vulgo Almereyda e Jean Vigo: Paulo Emílio Salles Gomes e a interlocução entre anarquismo e cinema

    Directory of Open Access Journals (Sweden)

    Julierme Sebastião Morais

    2009-11-01

    Full Text Available

    Resenha:

  1. Comparison of Miniaturized and Conventional Asymmetrical Flow Field-Flow Fractionation (AF4 Channels for Nanoparticle Separations

    Directory of Open Access Journals (Sweden)

    Zengchao You

    2017-03-01

    Full Text Available The performance of a miniaturized channel for the separation of polymer and metal nanoparticles (NP using Asymmetrical Flow Field-Flow Fractionation (AF4 was investigated and compared with a conventional AF4 system. To develop standard separation methods, experimental parameters like cross flow, gradient profile and injection time were varied and optimized. Corresponding chromatographic parameters were calculated and compared. Our results indicate that the chromatographic resolution in the miniaturized channel is lower, whereas significantly shorter analyses time and less solvent consumption were obtained. Moreover, the limit of detection (LOD and limit of quantification (LOQ obtained from hyphenation with a UV-detector are obviously lower than in a conventional channel, which makes the miniaturized channel interesting for trace analysis.

  2. HPLC-SPE-NMR characterization of major metabolites in Salvia fruticosa Mill. extract with antifungal potential: relevance of carnosic acid, carnosol, and hispidulin.

    Science.gov (United States)

    Exarchou, Vassiliki; Kanetis, Loukas; Charalambous, Zenovia; Apers, Sandra; Pieters, Luc; Gekas, Vassilis; Goulas, Vlasios

    2015-01-21

    Plant pathogenic fungi are considered of significant economic importance for adversely affecting both quantitatively and qualitatively fresh and processed produce. Extracts of Salvia fruticosa were initially screened for their antifungal activity, and the ethyl acetate fraction, being the most active, was further analyzed using HPLC-SPE-NMR hyphenation. The methoxylated flavones hispidulin, salvigenin, and cirsimaritin and the diterpenes carnosic acid, carnosol, and 12-methoxycarnosic acid were identified as the major components of the extract. In addition, the concentration levels of all identified components were determined using q-NMR. The antifungal activity of the crude extract and selected phytochemicals was estimated against the fungal species Aspergillus tubingensis, Botrytis cinerea, and Penicillium digitatum. The estimated MIC and MFC values of the ethyl acetate extract of S. fruticosa, as well as three of its major constituents, carnosic acid, carnosol, and hispidulin, support their antifungal activity, especially against B. cinerea and P. digitatum, suggesting their potential use in food and agricultural systems.

  3. Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies.

    Science.gov (United States)

    De Luca, Michele; Ragno, Gaetano; Ioele, Giuseppina; Tauler, Romà

    2014-07-21

    An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid-base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Analytical developments for screening of lanthanides/ligands interactions

    International Nuclear Information System (INIS)

    Varenne, F.

    2012-01-01

    This work investigates the potential of hyphenated capillary electrophoresis and inductively coupled mass spectrometry to classify different ligands according to their europium binding affinity in a hydro-organic medium. On the one hand, this method enables to evaluate the affinity of phosphorus-containing ligands in less than two hours and using less than 15 ng of ligand. On the other hand, complexation constants could be determined. The results are in excellent agreement with the values obtained by spectrophotometric titrations.Moreover, a library of copolymers for solid/liquid extraction of europium is investigated. The extraction protocol enables to classify copolymers according to their europium affinity in a hydro-organic medium. This screening requires 60 mg of copolymers. For the most promising recognition properties and selectivity La 3+ /Eu 3+ /Lu 3+ are evaluated. (author)

  5. The pentavalent actinide solution chemistry in the environment.

    Science.gov (United States)

    Topin, Sylvain; Aupiais, Jean

    2016-03-01

    With regard to environmental monitoring of certain nuclear facilities, pentavalent actinides, in particular neptunium and plutonium, play a key role, as the chief soluble, mobile forms of actinides. In the past five years, investigations carried out by hyphenating capillary electrophoresis to ICP-MS (CE-ICP-MS) have allowed a number of hitherto unknown thermodynamic data to be determined for Np(V) and Pu(V) interactions with the chief environmentally abundant anions. For the first time, data were provided for Pu(V) interactions with carbonate, sulfate, oxalate, chloride, and nitrate ions, allowing the Np(V)/Pu(V) analogy to be verified experimentally. Knowledge of Np(V) chemistry, especially in carbonate, and sulfate media, was also refined. These CE-ICP-MS studies, combined with some earlier findings, have brought about a renewal in the knowledge of An(V) chemistry in solution. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. The master plot in the audiovisual narrative. The western case.

    Directory of Open Access Journals (Sweden)

    José Félix GONZÁLEZ SÁNCHEZ

    2015-05-01

    Full Text Available A plot provides us the story that it offers a hyphen and later a film. Plots are limited, however possibilities, argument them that these offer music infinite. At the same time, we can say that all cultures avail themselves of some plots and similar arguments to structure their mythical stories. In addition, United States is the modern nation where better a dialectic relation between the myth and story keeps. At this nation, the significance of the event has been shown and you have gotten free through the myth. We will see through this article how the western is the kind of American cinema what else and better answer for the folkloric traditional story to the cánones, because your plots have been taken directly of the classical legends.

  7. Automotive Painting Technology A Monozukuri-Hitozukuri Perspective

    CERN Document Server

    Salazar, Abraham; Saito, Kozo

    2013-01-01

    This book offers unique and valuable contributions to the field. It offers breadth and inclusiveness. Most existing works on automotive painting cover only a single aspect of this complex topic, such as the chemistry of paint or paint booth technology. Monozukuri and Hitozukuri are Japanese terms that can be translated as “making things” and “developing people” but their implications in Japanese are richer and more complex than this minimal translation would indicate. The Monozukuri-Hitozukuri perspective is drawn from essential principles on which the Toyota approach to problem-solving and continuous improvement is based. From this perspective, neither painting technology R&D nor painting technology use in manufacturing can be done successfully without integrating technological and human concerns involved with making and learning in the broadest sense, as the hyphen is meant to indicate. The editors provide case studies and examples -- drawn from Mr. Toda’s 33 years of experience with automotiv...

  8. Neolignans as xanthine oxidase inhibitors from Hyptis rhomboides.

    Science.gov (United States)

    Tsai, Sheng-Fa; Lee, Shoei-Sheng

    2014-05-01

    The active fraction from the EtOH extract of Hyptis rhomboides against xanthine oxidase was identified by use of an HPLC microfractionation-centrifugal vacuum evaporation-bioassay hyphenated technique. Scale-up separation of the active subfractions using semi-preparative RP-HPLC provided 13 phenylpropanoid compounds, including O-styrenylneolignans, hyprhombins A-C, epihyprhombin B, and hyprhombin B methyl ester, and O-caffeoylnorneolignans, hyprhombins D and E. All of these compounds shared a common 1,4-benzodioxane skeleton, as established by spectroscopic analyses. Hyprhombin C and epihyprhombin B exhibited better anti-xanthine oxidase activity than allopurinol, with IC50 values of 0.6 and 2.0 μM, respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

    DEFF Research Database (Denmark)

    Buanuam, Janya; Tiptanasup, Kasipa; Shiowatana, Juwadee

    2006-01-01

    A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now...... the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate...... and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates ≤ 10 mL min–1. The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order...

  10. Chlorococcalean microalgae Ankistrodesmus convolutes biodiesel characterization with Fourier transform-infrared spectroscopy and gas chromatography mass spectroscopy techniques

    Directory of Open Access Journals (Sweden)

    Swati SONAWANE

    2015-12-01

    Full Text Available The Chlorococcalean microalgae Ankistrodesmus convolutes was found in fresh water Godawari reservoir, Ahmednagar district of Maharashtra State, India. Microalgae are modern biomass for the production of liquid biofuel due to its high solar cultivation efficiency. The collection, harvesting and drying processes were play vital role in converting algal biomass into energy liquid fuel. The oil extraction was the important step for the biodiesel synthesis. The fatty acid methyl ester (FAME synthesis was carried through base catalyzed transesterification method. The product was analyzed by using the hyphened techniques like Fourier Transform-Infrared spectroscopy (FT-IR and Gas Chromatography Mass Spectroscopy (GCMS. FT-IR Spectroscopy was results the ester as functional group of obtained product while the Gas Chromatography Mass Spectroscopy was results the six type of fatty acid methyl ester with different concentration. Ankistrodesmus convolutes biodiesel consist of 46.5% saturated and 49.14% unsaturated FAME.

  11. Prosecuting the Leaders: Promises, Politics and Practicalities

    Directory of Open Access Journals (Sweden)

    Robert Cryer

    2009-02-01

    Full Text Available Given recent developments in relation to the prosecution of international crimes,  it might be thought that one of the last bastions of sovereignty has been breached, and international criminal law has not only entrenched itself in international law. Indeed further to this, it has assumed a supranational position that stands entirely above States, promising justice for all and as a trump card over depredations committed in the name of State sovereignty. After all, Charles Taylor from Liberia is standing trial before the Special Court for Sierra Leone, Slobodan Milošević only escaped judgment by the International Criminal Tribunal for the former

  12. Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

    Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... electrolytic or aqueous leaching, on-line dialysis/microdialysis, in-line filtration, and pervaporation-based procedures have been successfully implemented in continuous flow/flow injection systems. In this communication, the new generation of flow analysis, including sequential injection, multicommutated flow...... with the potential hyphenation with modern analytical instrumentation for automated monitoring of the content of targeted species in the on-line generated extracts [3,4]. [1] Z.-L. Zhi, A. Ríos, M. Valcárcel, Crit. Rev. Anal. Chem., 26 (1996) 239. [2] M. Miró, E.H. Hansen, R. Chomchoei, W. Frenzel, TRAC-Trends Anal...

  13. Developments and trends in inductively coupled plasma mass spectrometry and its influence on the recent advances in trace element analysis

    International Nuclear Information System (INIS)

    Balaram, V.

    1995-01-01

    A brief introduction to the various instrumental methods such as atomic absorption spectrometry, x-ray fluorescence spectrometry, neutron activation analysis, inductively coupled plasma atomic emission spectrometry, thermal ionization mass spectrometry, etc. are presented highlighting their relative merits and demerits. The history and developments of inductively coupled plasma mass spectrometry (ICP-MS) and its advantages and limitations over other multi-element instrumental techniques are reviewed. Extended capabilities by hyphenating ICP-MS to various other well-known sample introduction techniques such as flow-injection, electrothermal vaporization, chromatographic methods and laser ablation are discussed in brief. The recent development of high resolution multi-collector double-focusing magnetic mass spectrometer with inductively coupled plasma at atmospheric pressure as source is also discussed. Some of the areas where more developments can be expected in future are suggested. (author). 77 refs., 4 tabs., 3 figs

  14. Development of a micro flow-through cell for high field NMR spectroscopy.

    Energy Technology Data Exchange (ETDEWEB)

    Alam, Todd Michael; McIntyre, Sarah K.

    2011-05-01

    A highly transportable micro flow-through detection cell for nuclear magnetic resonance (NMR) spectroscopy has been designed, fabricated and tested. This flow-through cell allows for the direct coupling between liquid chromatography (LC) and gel permeation chromatography (GPC) resulting in the possibility of hyphenated LC-NMR and GPC-NMR. The advantage of the present flow cell design is that it is independent and unconnected to the detection probe electronics, is compatible with existing commercial high resolution NMR probes, and as such can be easily implemented at any NMR facility. Two different volumes were fabricated corresponding to between {approx}3.8 and 10 {micro}L detection volume. Examples of the performance of the cell on different NMR instruments, and using different NMR detection probes were demonstrated.

  15. Quantitative analysis of pharmacokinetic study samples by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Mück, W

    1999-09-01

    The basis of all pharmacokinetic evaluations are powerful assays to quantify drugs and/or metabolites in biological matrices using modern sensitive instrumental analytical techniques, such as capillary gas chromatography and high-performance liquid chromatography (HPLC). Being both specific and universal, mass spectrometry (MS) is an ideal chromatographic detector. Due to recent exciting achievements in the interfacing of liquid chromatography (LC) and MS, LC-MS, like the successfully preceding hyphenated technique gas chromatography-mass spectrometry (GC-MS), has now become a valuable technique in the analyst's toolbox. The key features of LC-MS are explained and four examples demonstrating its potential for highly specific and sensitive routine drug assays with the option of high sample throughput in pharmacokinetic investigations are presented.

  16. Dual reductive/oxidative electrochemistry/liquid chromatography/mass spectrometry: Towards peptide and protein modification, separation and identification.

    Science.gov (United States)

    Büter, Lars; Frensemeier, Lisa M; Vogel, Martin; Karst, Uwe

    2017-01-06

    A new hyphenated technique based on on-line dual (oxidative and reductive) electrochemistry coupled to liquid chromatography and high resolution electrospray mass spectrometry is presented. Two liquid streams are combined, with one containing a disulfide, which is reduced to the respective thiol in an electrochemical cell based on a titanium working electrode. The other stream contains phenol, which is electrochemically activated to benzoquinone on a boron-doped diamond working electrode. Upon combination of the two streams, a Michael addition takes places, leading to the covalent coupling of thiol to quinone. In continuous flow, the reaction mixture is transferred into an injection valve and the products are separated by reversed phase liquid chromatography and detected by electrospray-high resolution mass spectrometry. Proof of concept is demonstrated for low molecular mass disulfides and peptides, but further optimization will be required in future work to achieve efficient protein labelling. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. A reunificação da Alemanha

    Directory of Open Access Journals (Sweden)

    Carl Goerdeler

    2009-12-01

    Full Text Available

    Resenha:

    BANDEIRA, Moniz.

  1. Role of advances in chromatographic techniques in phytochemistry.

    Science.gov (United States)

    Marston, Andrew

    2007-01-01

    Chromatography is the lynchpin of phytochemistry and is the key to obtaining pure compounds for structure elucidation, for pharmacological testing or for development into therapeuticals. It also plays a fundamental role as an analytical technique for quality control and standardisation of phytotherapeuticals. Although liquid chromatography is barely 100 years old, an extraordinary variety of instrumental and ancillary equipment is available, notably in the domain of high-performance liquid chromatography. It is impossible to touch all areas of chromatography in such a review but certain areas are worthy of mention: HPLC, HPTLC, UPLC and countercurrent chromatography. Another important addition has been the development of hyphenated techniques involving HPLC: LC/UV, LC/MS, LC/MS(n) and LC/NMR. These are indispensable nowadays for the early detection and identification of compounds in crude plant extracts.

  2. From retrospective assessment to prospective decisions in natural product isolation

    DEFF Research Database (Denmark)

    Johansen, Kenneth T; Wubshet, Sileshi G; Nyberg, Nils T

    2011-01-01

    , HPLC-HRMS-guided, targeted isolation scheme aiming exclusively at a series of identified spiro compounds. Thus, HPLC-PDA-HRMS-SPE-NMR is a dereplication technique of choice, allowing economical acquisition of comprehensive data about compounds in crude extracts, which can be used for rational......An extract of Carthamus oxyacantha (wild safflower) was investigated using two approaches: a traditional, nontarget fractionation by VLC and HPLC, and the hyphenated technique HPLC-PDA-HRMS-SPE-NMR followed by targeted isolation of selected constituents for inclusion in a screening library of pure......, prospective decisions about further isolation efforts. A total of 15 compounds were identified in the extract. Six spiro compounds, of which four have not previously been characterized, and tracheloside (a lignin glucoside) are presented with assigned (1)H and (13)C chemical shifts....

  3. Marine environment pollution: The contribution of mass spectrometry to the study of seawater.

    Science.gov (United States)

    Magi, Emanuele; Di Carro, Marina

    2016-09-09

    The study of marine pollution has been traditionally addressed to persistent chemicals, generally known as priority pollutants; a current trend in environmental analysis is a shift toward "emerging pollutants," defined as newly identified or previously unrecognized contaminants. The present review is focused on the peculiar contribution of mass spectrometry (MS) to the study of pollutants in the seawater compartment. The work is organized in five paragraphs where the most relevant groups of pollutants, both "classical" and "emerging," are presented and discussed, highlighting the relative data obtained by the means of different MS techniques. The hyphenation of MS and separative techniques, together with the development of different ion sources, makes MS and tandem MS the analytical tool of choice for the determination of trace organic contaminants in seawater. © 2016 Wiley Periodicals, Inc. Mass Spec Rev. © 2016 Wiley Periodicals, Inc.

  4. Ultrasensitive Speciation Analysis of Mercury in Rice by Headspace Solid Phase Microextraction Using Porous Carbons and Gas Chromatography-Dielectric Barrier Discharge Optical Emission Spectrometry.

    Science.gov (United States)

    Lin, Yao; Yang, Yuan; Li, Yuxuan; Yang, Lu; Hou, Xiandeng; Feng, Xinbin; Zheng, Chengbin

    2016-03-01

    Rice consumption is a primary pathway for human methylmercury (MeHg) exposure in inland mercury mining areas of Asia. In addition, the use of iodomethane, a common fumigant that significantly accelerates the methylation of mercury in soil under sunlight, could increase the MeHg exposure from rice. Conventional hyphenated techniques used for mercury speciation analysis are usually too costly for most developing countries. Consequently, there is an increased interest in the development of sensitive and inexpensive methods for the speciation of mercury in rice. In this work, gas chromatography (GC) coupled to dielectric barrier discharge optical emission spectrometry (DBD-OES) was developed for the speciation analysis of mercury in rice. Prior to GC-DBD-OES analysis, mercury species were derivatized to their volatile species with NaBPh4 and preconcentrated by headspace solid phase microextraction using porous carbons. Limits of detection of 0.5 μg kg(-1) (0.16 ng), 0.75 μg kg(-1) (0.24 ng), and 1.0 μg kg(-1) (0.34 ng) were obtained for Hg(2+), CH3Hg(+), and CH3CH2Hg(+), respectively, with relative standard deviations (RSDs) better than 5.2% and 6.8% for one fiber or fiber-to-fiber mode, respectively. Recoveries of 90-105% were obtained for the rice samples, demonstrating the applicability of the proposed technique. Owing to the small size, low power, and low gas consumption of DBD-OES as well as efficient extraction of mercury species by porous carbons headspace solid phase micro-extraction, the proposed technique provides several advantages including compactness, cost-effectiveness, and potential to couple with miniature GC to accomplish the field speciation of mercury in rice compared to conventional hyphenated techniques.

  5. Esboço para a História da Esquerda no Brasil

    Directory of Open Access Journals (Sweden)

    Antonio Ozaí da Silva

    2009-12-01

    Full Text Available O que é esquerda? É a partir dessa questão que analisamos, de maneira sintética, a trajetória da esquerda brasileira, das origens à formação do Partido dos Trabalhadores. A “era petista” inaugura uma nova fase para a militância dos movimentos sociais e da esquerda brasileira. Assim, na parte final, enfatizamos, sem a preocupação de concluir ou dar a palavra final, os dilemas e desafios do tempo presente. O objetivo é contribuir para o estudo e a reflexão sobre a história da esquerda brasileira e sua práxis na contemporaneidade. Nesta perspectiva, nos concentramos sobre a esquerda que se reivindica marxista e vinculada a esta tradição política e ideológica.

  6. Asymmetric flow field-flow fractionation coupled to inductively coupled plasma mass spectrometry for the quantification of quantum dots bioconjugation efficiency.

    Science.gov (United States)

    Menéndez-Miranda, Mario; Encinar, Jorge Ruiz; Costa-Fernández, José M; Sanz-Medel, Alfredo

    2015-11-27

    Hyphenation of asymmetric flow field-flow fractionation (AF4) to an on-line elemental detection (inductively coupled plasma-mass spectrometry, ICP-MS) is proposed as a powerful diagnostic tool for quantum dots bioconjugation studies. In particular, conjugation effectiveness between a "model" monoclonal IgG antibody (Ab) and CdSe/ZnS core-shell Quantum Dots (QDs), surface-coated with an amphiphilic polymer, has been monitored here by such hybrid AF4-ICP-MS technique. Experimental conditions have been optimized searching for a proper separation between the sought bioconjugates from the eventual free reagents excesses employed during the bioconjugation (QDs and antibodies). Composition and pH of the carrier have been found to be critical parameters to ensure an efficient separation while ensuring high species recovery from the AF4 channel. An ICP-MS equipped with a triple quadropole was selected as elemental detector to enable sensitive and reliable simultaneous quantification of the elemental constituents, including sulfur, of the nanoparticulated species and the antibody. The hyphenated technique used provided nanoparticle size-based separation, elemental detection, and composition analysis capabilities that turned out to be instrumental in order to investigate in depth the Ab-QDs bioconjugation process. Moreover, the analytical strategy here proposed allowed us not only to clearly identify the bioconjugation reaction products but also to quantify nanoparticle:antibodies bioconjugation efficiency. This is a key issue in future development of analytical and bioanalytical photoluminescent QDs applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Effect-directed fingerprints of 77 botanical extracts via a generic high-performance thin-layer chromatography method combined with assays and mass spectrometry.

    Science.gov (United States)

    Krüger, S; Hüsken, L; Fornasari, R; Scainelli, I; Morlock, G E

    2017-12-22

    Quantitative effect-directed profiles of 77 industrially and freshly extracted botanicals like herbs, spices, vegetables and fruits, widely used as food ingredients, dietary supplements or traditional medicine, gave relevant information on their quality. It allows the assessment of food, dietary supplements and phytomedicines with regard to potential health-promoting activities. In contrary to sum parameter assays and targeted analysis, chromatography combined with effect-directed analysis allows fast assignment of single active compounds and evaluation of their contribution to the overall activity, originating from a food or botanical sample. High-performance thin-layer chromatography was hyphenated with UV/Vis/FLD detection and effect-directed analysis, using the 2,2-diphenyl-1-picrylhydrazyl radical, Gram-negative Aliivibrio fischeri, Gram-positive Bacillus subtilis, acetylcholinesterase and tyrosinase assays. Bioactive compounds of interest were eluted using an elution head-based interface and further characterized by electrospray ionization (high-resolution) mass spectrometry. This highly streamlined workflow resulted in a hyphenated HPTLC-UV/Vis/FLD-EDA-ESI + /ESI - -(HR)MS method. The excellent quantification power of the method was shown on three compounds. For rosmarinic acid, contents ranged from 4.5mg/g (rooibos) to 32.6mg/g (rosemary), for kaempferol-3-glucoside from 0.6mg/g (caraway) to 4.4mg/g (wine leaves), and for quercetin-3-glucoside from 1.1mg/g (hawthorn leaves) to 17.7mg/g (thyme). Three mean repeatabilities (%RSD) over 18 quantifications for the three compounds were ≤2.2% and the mean intermediate precision over three different days (%RSD, n=3) was 5.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Dostoievski e o enigma humano

    Directory of Open Access Journals (Sweden)

    Elton Moreira Quadros

    2009-12-01

    Full Text Available

    Discute a interpretação realizada pelo filósofo russo Berdiaeff sobre a obra de Dostoievski e comparar a antropologia do romancista com a antropologia do filósofo Nietzsche

  9. O Muro, dois Estados, dois Mundos

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    Luis Edmundo de Souza Moraes

    2009-11-01

    Full Text Available

    O  artigo trata do problema das fronteiras sociais e políticas na Berlim do pós-II Guerra Mundial relacionadas à divisão da cidade em zonas de ocupação e, posteriormente, à construção do Muro. Ele reflete sobre o fato de que o muro, que dividiu uma cidade de forma artificial, produziu divisões e diferenças concretas pela ação do tempo, criando descontinuidades onde haviam continuidades. O artigo ainda aponta para uma forma de pensar o encontro não planejado entre as duas partes da cidade naquilo que foi chamada de reunificação.

  10. User Experience – Essencial para Usabilidade de Produtos

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    Antonio Mendes Silva Filho

    2011-07-01

    Full Text Available Usabilidade tem sido um dos fatores utilizados por empresas para conquistar novos usuários (consumidores. De acordo com a Norma 9241-11 da ISO (International Organization for Standardization, a usabilidade é definida como “The extent to which a product can be used by specified users to achieve specified goals with effectiveness, efficiency, and satisfaction in a specified context of use”. Esses objetivos compreendem a base do que é denominado “user experience”. Mas, o que é user experience? Trata-se da experiência do usuário quando interage com produtos ou serviços. Um produto pode ser qualquer coisa como, por exemplo, um notebook, um aparelho celular ou smartphone, um painel de automóvel ou software. Qualquer desses produtos ou até serviços (como oferecidos em web sites, têm a usabilidade como atributo determinante da qualidade perceptível aos usuários. Nesse sentido, o objetivo deste artigo é discutir e explorar experiência e percepção do usuário no uso e adoção de novas tecnologias. O artigo destaca como a Apple tem inovado em seus produtos provendo usabilidade levando em consideração a experiência do usuário.

  11. Notas sobre a liberdade e a tirania da maioria em Stuart Mill

    Directory of Open Access Journals (Sweden)

    Antonio Ozaí da Silva

    2009-10-01

    Full Text Available O liberalismo é uma doutrina política que, em suas origens, tem como alicerce vários autores clássicos do pensamento político: Locke, Montesquieu, Kant, Adam Smith, Humboldt, Benjamin Constant, Alexis de Tocqueville, Stuart Mil e outros. Portanto, a exemplo do socialismo, cabe perfeitamente a pergunta: Qual liberalismo? Como o(s marxismo(s, o pensamento liberal não é homogêneo. Da mesma forma, o conceito de liberdade no pensamento liberal tem mais de uma conotação, como também a sua crítica. Estes apontamentos se limitam a expor o pensamento político de John Stuart Mill, mais precisamente sobre a sua argumentação em defesa da liberdade individual e a crítica à tirania da maioria no ensaio “Sobre a Liberdade” (MILL, 1991.

  12. As bregafestas de fim de ano (apenas uma reflexão pessoal

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    Raymundo de Lima

    2010-01-01

    Full Text Available Peço perdão aos festeiros de fim de ano, pela minha irritação com o mesmismo dessa época. Acho horrorosas as musiquinhas com arpa, os anúncios televisivos, os enfeites bregaluminosos nas árvores urbanas, as filas, a obrigação de desejar feliz Natal e Próspero Ano Novo, receber-enviar mensagens etc. Na verdade, me irrito com o consumismo e a profanação do significado do nascimento de Jesus. Incomodo-me especialmente com as mulheres que entram em frenesi com as compras de roupas pra si, para parentes e crianças exigentes com presentes de griffes, a ansiedade dos preparativos para a ceia de Natal, seleção dos convidados. Por que ceia? Por que “tem que ter” peru? No Rio “tem que ter” rabanada gordurosa?

  13. Don Quijote en Brasil: de la mitología a las historietas

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    Kenia Almeida Pereira

    2009-11-01

    Full Text Available Este artículo es una pequeña reflexión sobre el libro El ingenioso hidalgo Don Quijote de la Mancha, de Miguel de Cervantes, publicada en 1605. Esta obra ha sido considerada como una de las mejores novelas de todos los tiempos. En ella podemos transitar de lo popular a lo erudito. Esta narrativa está llena de antítesis y metáforas barrocas que contienen desde los refranes populares hasta la erudición de los mitos griegos, así como de la locura y jocosidad de Don Quijote y también de la mediocridad y lucidez de Sancho Panza.

  14. Um gramsciano a serviço da união dos povos

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    Marco Aurélio Nogueira

    2010-02-01

    Full Text Available Quarta-feira, 20 de janeiro, soube da morte de Giorgio Baratta. Poucos brasileiros sabem quem foi ele. Era conhecido e admirado por marxistas gramscianos, com quem mantinha relações estreitas, aqui no Brasil e em diversas partes do mundo. A todos encantava com sua ironia fina, seu conhecimento enciclopédico, sua admiração incondicional por Gramsci – uma admiração que não o cegava nem o fechava em tolos dogmatismos.

  15. Redes Sociais na Era da Conectividade (“The good, the bad and the Ugly”

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    Antonio Mendes Silva Filho

    2010-12-01

    Full Text Available O mundo caminha para uma população que deverá atingir a população de 7 bilhões de pessoas. Entretanto, muito antes disso, a impressionante marca de 2 bilhões de usuários da Internet será alcançada. E, nada mais encanta mais o ser humano que a comunicação. Por natureza, o ser humano precisa viver em sociedade. Trata-se de uma característica intrínseca do homem. Ao longo de sua história, a humanidade tem sido marcada por tragédias e avanços e, especificamente, o século XX foi rico no avanço científico. A década de 90 foi marcada pela popularização da Internet, a qual foi intensificada nesta última década, destacando-se o crescente número de usuários e tempo de permanência nas redes sociais. O que isso indica? Um novo brinquedo? Necessidade de comunicação ? Um novo vício? Este artigo parte desses questionamentos e dados estatísticos para explorar como novas tecnologias impactam sobre o cotidiano humano e corporativo.

  16. Quantitative analysis of major dibenzocyclooctane lignans in Schisandrae fructus by online TLC-DART-MS.

    Science.gov (United States)

    Kim, Hye Jin; Oh, Myung Sook; Hong, Jongki; Jang, Young Pyo

    2011-01-01

    Direct analysis in real time (DART) ion source is a powerful ionising technique for the quick and easy detection of various organic molecules without any sample preparation steps, but the lack of quantitation capacity limits its extensive use in the field of phytochemical analysis. To improvise a new system which utilize DART-MS as a hyphenated detector for quantitation. A total extract of Schisandra chinensis fruit was analyzed on a TLC plate and three major lignan compounds were quantitated by three different methods of UV densitometry, TLC-DART-MS and HPLC-UV to compare the efficiency of each method. To introduce the TLC plate into the DART ion source at a constant velocity, a syringe pump was employed. The DART-MS total ion current chromatogram was recorded for the entire TLC plate. The concentration of each lignan compound was calculated from the calibration curve established with standard compound. Gomisin A, gomisin N and schisandrin were well separated on a silica-coated TLC plate and the specific ion current chromatograms were successfully acquired from the TLC-DART-MS system. The TLC-DART-MS system for the quantitation of natural products showed better linearity and specificity than TLC densitometry, and consumed less time and solvent than conventional HPLC method. A hyphenated system for the quantitation of phytochemicals from crude herbal drugs was successfully established. This system was shown to have a powerful analytical capacity for the prompt and efficient quantitation of natural products from crude drugs. Copyright © 2010 John Wiley & Sons, Ltd.

  17. Elimination of suction effect in interfacing microchip electrophoresis with inductively coupled plasma mass spectrometry using porous monolithic plugs.

    Science.gov (United States)

    Cheng, Heyong; Liu, Jinhua; Yin, Xuefeng; Shen, Hong; Xu, Zigang

    2012-07-07

    A suction-free interfacing method was developed for microchip electrophoresis hyphenated with inductively coupled plasma mass spectrometry (MCE-ICP-MS). The hyphenated system was composed of a microchip, a demountable capillary microflow nebulizer (d-CMN) combined with a heated single pass spray chamber, a negative pressure sampling device, a high voltage power supply, a syringe pump and an ICP-MS. To eliminate the nebulizer suction generated by the pneumatic nebulizer and to ensure that the makeup solution flowed into the nebulizer, two porous polymer plugs were fabricated in the microchip. As a result, reasonably true electropherograms were obtained when compared to the CE separation performed in the traditional MCE-ICP-MS mode without porous polymer plugs. Electrophoretic separation of I(-) and IO(3)(-) was achieved within 25 s in a microchip with an effective separation length of only 15 mm at an electric field of 857 V cm(-1) using 10 mmol L(-1) borate (pH 9.2) as the running buffer. A resolution of 1.3 was obtained and the absolute detection limits for I(-) and IO(3)(-) were 0.12 and 0.13 fg, respectively. The precisions (RSD, n = 10) of the migration time and peak height for I(-) and IO(3)(-) were in the range of 1.1-1.6% and 2.5-2.8%, respectively. Two table salt samples were analyzed by an external calibration method. The iodate contents were in accordance with their labeled values. The recoveries of I(-) and IO(3)(-) in the table salt samples were in the range of 92-105%.

  18. Development of anion-exchange/reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry methods for the speciation of bio-available iodine and bromine from edible seaweed.

    Science.gov (United States)

    Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2012-05-04

    Anion exchange high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry has been novelly applied to assess inorganic (iodide and iodate) and organic (3-iodotyrosine - MIT, and 3,5-diiodotyrosine - DIT) iodine species in a single chromatographic run. The optimized operating conditions (Dionex IonPac AS7, gradient elution with 175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase and flow rates within the 0.5-1.5 mL min(-1) range) have also been used to perform inorganic bromine speciation analysis (bromide and bromate). The developed method has been applied for determining the bio-available contents of iodine and bromine species in dialyzates from edible seaweed. Reverse phase high performance liquid chromatography (Zorbax Eclipse XDB-C8, gradient elution with 0.2% (m/m) acetic acid, and 0.2% (m/m) acetic acid in methanol, as mobile phases, and a constant flow rate of 0.75 mL min(-1)) also hyphenated with inductively coupled plasma-mass spectrometry was used to confirm the presence of organic iodine species (MIT and DIT) in the dialyzates. The verification of the presence of iodinated amino acids (MIT and DIT) in the extracts was also performed by reverse phase high performance liquid chromatography-electrospray ionization-mass spectrometry (LTQ Orbitrap). The developed methods have provided good repeatability (RSD values lower than 10% for both anion exchange and reverse phase separations) and analytical recoveries within the 90-105% range for all cases. The in vitro bio-availability method consisted of a simulated gastric and an intestinal digestion/dialysis (10 kDa molecular weight cut-off - MWCO) two-stage procedure. Iodide and MIT were the main bio-available species quantified, whereas bromide was the major bromine species found in the extracts. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. BIOCHEMICAL ATTRIBUTES OF TWO SAVANNAH SOILS UNDER DIFFERENT MANAGEMENT SYSTEMS AND USE ATRIBUTOS BIOQUÍMICOS EM DOIS SOLOS DE CERRADO SOB DIFERENTES SISTEMAS DE MANEJO E USO

    Directory of Open Access Journals (Sweden)

    Américo Nunes da Silveira Neto

    2008-11-01

    Full Text Available

    Soil biochemical attributes can be used as sensitive indicators of alterations promoted by the agricultural use, being a tool to guide tillage practices planning and evaluation to maintain soil sustainability. The objective of this study was to evaluate alterations in the soil organic carbon, biomass and microbial activity, urease and acid phosphatase activity, in two savannah soils, as affected by soil management systems. The study consisted of five soil management systems in a Typic Quartzipsamment, four in an Oxisol, and reference areas without alterations in the two soil types. The management systems changed the biochemical attributes of both soils. The Typic Quartzipsamment area under the soybean/Brachiaria decumbens sequence decreased the soil organic carbon and the microbial biomass carbon, and increased the respiration and qCO2, while the Oxisol, in all the areas, except for pasture, promoted reductions in the biochemical attributes. Among the management systems studied,  the pasture provided improvements in the evaluated attributes, in both soils.

    KEY-WORDS: Soil quality; microbial biomass; soil enzymatic activity.

  1. Picturing the Other: Targets of Delegitimization across Time

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    Luca Andrighetto

    2010-12-01

    Full Text Available

     

    Italian Fascist propaganda was compared with contemporary right-wing material to explore how political propaganda depicts specific target groups in different historical periods. Taking the theory of delegitimization as the theoretical framework, we analyzed visual images concerning despised social groups used by the Fascist regime and current images of contemporary targets of social resentment used by Lega Nord (currently part of the governing coalition. Images of Jewish and Black people published in the Fascist magazine La Difesa della Razza were classified according to eight delegitimizing strategies, as were images of immigrants used on Lega Nord propaganda posters. Although the target group has changed, six of the eight strategies of delegitimization were used in both periods. In most cases, overlap was found in the way target groups were portrayed in the past and in the present.

     

    Utopia can have an uplifting and a dark side, but usually the dark side ends up trumping the initial idealism. The reason for this is that utopians inevitably adopt a messianic image of the world. The three messianic revolutions in history—the American, French and Bolshevik—were led by men who thought their ideas were universal. This essay examines the writings of French existentialist Albert Camus, who argues that there are no transcendental values, at the same time he does not accept nihilism. Camus makes a distinction between a rebel and a revolutionary, and concludes that a rebellion will try to end the specific oppression, whereas the revolution will try to create a “new man,” with common values throughout the world.

  2. Os perigos da utopia

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    Larry Hufford

    2009-06-01

    Full Text Available

    A utopia pode ter um lado que eleva e um lado sinistro, mas geralmente o lado sinistro acaba destruindo o idealismo inicial. A razão para isto é que os utópicos inevitavelmente adotam uma imagem messiânica do mundo. As três revoluções messiânicas na história—a americana, a francesa e a bolchevique—foram lideradas por homens que pensavem que suas idéias eram universais. Este ensaio examina os escritos do existencialista francês Albert Camus, que argumenta que não existem valores transcendentais, ao mesmo tempo que ele não aceita o niilismo. Camus faz uma distinção entre um rebelde e um revolucionário, e conclui que uma rebelião tentará terminar com uma opressão espedífica, enquanto que uma revolução tentará criar “um novo

  3. Are you kidding me? Are you kidding me?

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    Rosanna Lauriola

    2010-04-01

    Full Text Available Are you kidding me?

    The presence of a picture such as the one that appears in the site (http://farm4.static.flickr.com/3252/2843406747_3c135d63d9.jpg?v=0 brings to mind both the enormous efforts made throughout many years to raise awareness about the dangers or rape, and the horrors of rape for women all over the world. To joke with such a subject is offensive both for people—men and women—who have been struggling for so long, and for the victims of this crime. People who use the subject of rape for fun cause immense pain and immense damage.

  4. Se um leão soubesse falar: vegetarianismo e saúde

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    Eva Paulino Bueno

    2009-09-01

    Full Text Available

    Analise do vegetarianismo, suas origens, sua filosofia, suas relações com algumas religiões, e seus benefícios para a saúde das pessoas. O texto também fala da nossa relação com os animais, e de como eles expressam seu medo e sua dor ao serem mortos pelos seres humanos.

  5. Applicability of multisyringe chromatography coupled to cold-vapor atomic fluorescence spectrometry for mercury speciation analysis

    International Nuclear Information System (INIS)

    Guzmán-Mar, J.L.; Hinojosa-Reyes, L.; Serra, A.M.; Hernández-Ramírez, A.; Cerdà, V.

    2011-01-01

    Graphical abstract: An automatic system, based on the applicability of multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) detection is developed for mercury speciation. Highlights: ► The on-line coupling of MSC to CV/AFS was developed for mercury speciation analysis. ► The speciation of MeHg + , Hg 2+ and EtHg + was achieved on a RP C18 monolithic column. ► The hyphenated system provided higher sample throughput compared to HPLC–CV/AFS. ► The limits of detection for mercury species were comparable or better than those reported by HPLC–CV/AFS. ► The developed method also provided low instrumental and operational costs. - Abstract: In this paper, a novel automatic approach for the speciation of inorganic mercury (Hg 2+ ), methylmercury (MeHg + ) and ethylmercury (EtHg + ) using multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) was developed. For the first time, the separation of mercury species was accomplished on a RP C18 monolithic column using a multi-isocratic elution program. The elution protocol involved the use of 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)–acetonitrile (99:1, v/v), followed by 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)–acetonitrile (90:10, v/v). The eluted mercury species were then oxidized under post-column UV radiation and reduced using tin(II) chloride in an acidic medium. Subsequently, the generated mercury metal were separated from the reaction mixture and further atomized in the flame atomizer and detected by AFS. Under the optimized experimental conditions, the limits of detection (3σ) were found to be 0.03, 0.11 and 0.09 μg L −1 for MeHg + , Hg 2+ and EtHg + , respectively. The relative standard deviation (RSD, n = 6) of the peak height for 3, 6 and 3 μg L −1 of MeHg + , Hg 2+ and EtHg + (as Hg) ranged from 2.4 to 4.0%. Compared with the conventional HPLC–CV/AFS hyphenated systems

  6. Os limites da competitividade

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    Henrique Rattner

    2009-08-01

    Full Text Available

    Costuma-se destacar os aspectos aparentemente positivos e as vantagens hipotéticas da concorrência e da competitividade entre empresas e também entre nações. Não se pode negar que a concorrência nos mercados tenha exercido uma função central e fundamental na gênese e na expansão do sistema de produção capitalista. Ela contribuiu para a geração e acumulação de riquezas materiais. Também estimulou e fortaleceu as aspirações de seus principais atores sociais, os empreendedores, de exigir uma organização política mais democrática em oposição ao regime feudal ou absolutista, em determinado período da história do mundo ocidental.

  7. O primeiro ano de governo de Barack Obama: tempestades à toda volta

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    Eva Paulino Bueno

    2010-02-01

    Full Text Available O primeiro ano de Barak Obama à frente do governo americano foi um ano de grandes dificuldades, não só para ele, mas também para o seu partido democrata. Não só para os democratas, mas também para o povo americano. Não só para o povo americano, mas também para o povo iraquiano, e o povo do Afeganistão. E, por extensão, para todas as pessoas do mundo que ouviram seu discurso de aceitação do cargo, no dia 20 de janeiro de 2009. Os únicos que não sofreram, pelo que pude averiguar ouvindo rádio, lendo jornais e assistindo as notícias, foram os comentaristas republicanos, especialmente os ligados à tropa da cadeia de televisão Fox. Para eles, foi um ano de exultação.  Só não foi melhor porque o país não sofreu um ataque terrorista de

  8. Afinidades eletivas: EZLN e MST na contramão da história do progresso dos vencedores

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    Fabio Querido

    2011-04-01

    Full Text Available

    Inspirando-se em algumas reflexões de Walter Benjamin e, em menor medida, de José Carlos Mariátegui, o objetivo deste pequeno artigo é esboçar algumas afinidades eletivas entre o Exército Zapatista de Libertação Nacional e o Movimento dos Trabalhadores Sem Terra, particularmente no que se refere à importância que eles conferem ao resgate e rememoração das lutas sociais do passado – transformadas em fonte de inspiração das lutas do presente.

  9. O Programa Bolsa Família: lições da experiência alemã

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    Clóvis Roberto Zimmermann

    2009-07-01

    Full Text Available

    Esse artigo tece uma comparação do Bolsa Família com a experiência internacional, argumentando que os programas de transferência de renda brasileiros jamais podem ser visto como “barbaridade”, e de forma alguma “assombram o Brasil”, assim como também não contribuem para manter e tornar operativa a “pobreza brasileira”. Conforme demonstramos no artigo, programas de transferência de renda similares ao Bolsa Família, porém mais justos e generosos, existem em muitos países da Europa, não sendo encarados como “barbaridade”. Além disso, não existe a intenção política de se extinguir tais programas, pois contribuem para reduzir a fome e diminuir consideravelmente os níveis de

  10. On-line coupling of physiologically relevant bioaccessibility testing to inductively coupled plasma spectrometry: Proof of concept for fast assessment of gastrointestinal bioaccessibility of micronutrients from soybeans.

    Science.gov (United States)

    Herrera, Mónica Alejandra; Rosende, María; Arruda, Marco Aurélio Zezzi; Miró, Manuel

    2016-10-05

    In-vitro physiologically relevant gastrointestinal extraction based on the validated Unified BARGE Method (UBM) is in this work hyphenated to inductively coupled plasma optical emission spectrometry in a batch-flow configuration for real-time monitoring of oral bioaccessibility assays with high temporal resolution. A fully automated flow analyzer is designed to foster in-line filtration of gastrointestinal extracts at predefined times (≤15 min) followed by on-line multi-elemental analysis of bioaccessible micro-nutrients, viz., Cu, Fe and Mn, in well-defined volumes of extracts (300 μL) of transgenic and non-transgenic soybean seeds taken as model samples. The hyphenated flow setup allows for recording of temporal extraction profiles to gain full knowledge of the kinetics of the gastrointestinal digestion processes, including element leaching and concomitant precipitation and complexation reactions hindering bioavailability. Simplification of the overall standard procedure is also feasible by identification of steady-state extraction conditions. Our findings indicate that reliable measurement of oral bioaccessible pools of Cu, Fe and Mn in soybean might be obtained in less than 180 min rather than 240 min as endorsed by UBM. Using a matrix-matched external calibration, limits of detection according to the 3s criteria were 0.5 μg/g for Mn, 0.6 μg/g for Cu and 2.3 μg/g for Fe. Trueness of the automatic bioaccessibility method was confirmed by mass balance validation with recoveries ranging from 87 to 116% regardless of the target element and sample. Cu was the micronutrient with the highest oral bioaccessibility ranging from 73% to 83% (7.5-7.9 μg/g) for non-transgenic and transgenic soybeans, respectively, followed by Mn and Fe within the ranges of 29-31% (10.8-11.4 μg/g) and 11-15% (8-14 μg/g), respectively, regardless of transgenesis. The proposed kinetic method is proven suitable for fast and expedient estimation of the nutritional value of

  11. Acusar ou não acusar? In dubio pro societate é (? a solução. Uma forma perversa de lidar com a dúvida no processo penal brasileiro

    Directory of Open Access Journals (Sweden)

    Marcio Ferreira Rodrigues Pereira

    2011-02-01

    Full Text Available No âmbito do Direito Processual Penal, em pelo menos dois momentos marcantes da persecução penal em juízo (recebimento da denúncia e decisão de pronúncia, a fórmula in dubio pro societate vem sendo repetida à exaustão por significativo setor da comunidade jurídica. A pretensão deste estudo é desvelar tanto o caráter perverso que tal discurso encobre como a carência de base constitucional para o referido brocardo.

  12. Violence Research from North Africa to South Asia: A Historical and Structural Overview

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    Jochen Hippler

    2011-07-01

    Full Text Available

    This is a historical and sociological overview of violence and violence research in and on North Africa, West Asia, and South Asia, considering only studies for a global audience. The main focus is on political violence, with a brief look at religious and communal violence, youth violence, and domestic and gendered violence. These regions have been consistently affected by political violence for many decades, the main source of which seems to be the ongoing state formation process, as well as social transformation in general. The literature on violence is dominated by international debates, at

  13. O campo religioso brasileiro: pesquisas e produção do conhecimento – à guisa do crescimento pentecostal

    Directory of Open Access Journals (Sweden)

    Fábio Alves Ferreira

    2010-03-01

    Full Text Available Este artigo aponta as mudanças recentes no campo religioso brasileiro e a forma como elas foram captadas pela academia. A produção acadêmica sobre religião é intensa e plural. O debate em torno de um possível encantamento, desencantamento e reencantamento, transversalmente cortado pelas idéias de secularização e racionalização, tem sido basilar em toda a discussão. O pentecostalismo tem ocupado um lugar privilegiado, sobretudo por seu vertiginoso crescimento e pulverização nos espaços públicos e laicos. Tudo isso é uma tentativa de compreender as variações da religião na contemporaneidade e a forma em que ela tem se inscrito na

  14. Transnational Refugees: The Transformative Role of Art?

    Directory of Open Access Journals (Sweden)

    Maggie O'Neill

    2008-05-01

    Full Text Available This paper focuses upon the transfor­m­ative role of art and the methodological approach of working with artists to conduct ethnographic research with refugees and asylum seekers. In exploring the space or hyphen between ethnog­raphy (sociology and arts based practice (photos, in­stallations, textual practice I suggest that the combination of biography/narrative (ethnography and art (mimesis becomes a "potential space" for transformative possibilities. More specifically, draw­ing upon Walter BENJAMIN's (1992 The Story­teller I will discuss the methodological contribution of combining biography/narrative with art forms (ethno-mimesis in creating a "potential space", a reflective/safe space for dialogue and narratives to emerge around the themes of transnational identities, home and belonging. The importance of renewing methodologies for the work we do within the area of forced migration, humiliation, "egaliza­tion" and human rights (LINDNER, 2006, the role of the arts in processes of social inclusion, and the vital importance for creating spaces for dialogue and performative praxis through participatory methodologies are also discussed. URN: urn:nbn:de:0114-fqs0802590

  15. Qualitative Profiling of Polyglucose Degradation Products in Peritoneal Dialysis Fluids.

    Science.gov (United States)

    Gensberger, Sabrina; Knabner, Carina; Waibel, Reiner; Huppert, Jochen; Pischetsrieder, Monika

    2015-06-16

    Heat sterilization of peritoneal dialysis (PD) fluids leads to partial degradation of the osmotic agent to form reactive carbonyl structures, which significantly reduce the biocompatibility of PD fluids and impair long-term PD therapy. Hence, it is important to know the exact composition of the degradation products to improve biocompatibility of PD fluids. Our study conducted targeted screening for degradation products in polyglucose (icodextrin)-containing PD fluids (pGDPs) by applying o-phenylenediamine (OPD) to form stable derivatives, which were analyzed by ultrahigh-performance liquid chromatography with hyphenated diode array tandem mass spectrometry (UHPLC-DAD-MS/MS). For the first time, specific degradation products of polyglucose, namely, 4-deoxyglucosone (4-DG) and 3,4-dideoxypentosone (3,4-DDPS), could be identified in PD fluids. Further, a reaction product of 5-hydroxymethylfurfural (5-HMF) and OPD could be characterized to be (5-(1H-benzo[d]imidazol-2-yl)furan-2-yl)methanol. Additionally, 3-deoxyglucosone (3-DG) and 3-deoxygalactosone (3-DGal), both known to be present in glucose-based PD fluids, were also detected in polyglucose-containing fluids. Trapping a hitherto unknown degradation product with OPD yielded 1,4-bis(1H-benzo[d]imidazol-2-yl)-3,4-dihydroxybutan-1-one, which was present in heat- as well as filter-sterilized PD fluids.

  16. Rapid and sensitive determination of phytosterols in functional foods and medicinal herbs by using UHPLC-MS/MS with microwave-assisted derivatization combined with dual ultrasound-assisted dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Sun, Jing; Zhao, Xian-En; Dang, Jun; Sun, Xiaoyan; Zheng, Longfang; You, Jinmao; Wang, Xiao

    2017-02-01

    In this work, a hyphenated technique of dual ultrasound-assisted dispersive liquid-liquid microextraction combined with microwave-assisted derivatization followed by ultra high performance liquid chromatography tandem mass spectrometry has been developed for the determination of phytosterols in functional foods and medicinal herbs. Multiple reaction monitoring mode was used for the tandem mass spectrometry detection. A mass spectrometry sensitive reagent, 4'-carboxy-substituted rosamine, has been used as the derivatization reagent for five phytosterols, and internal standard diosgenin was used for the first time. Parameters for the dual microextraction, microwave-assisted derivatization, and ultra high performance liquid chromatography tandem mass spectrometry were all optimized in detail. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect, extremely low limits of detection (0.005-0.015 ng/mL) and limits of quantification (0.030-0.10 ng/mL) were achieved. The proposed method was compared with previously reported methods. It showed better sensitivity, selectivity, and accuracy. The matrix effect was also significantly reduced. The proposed method was successfully applied to the determination of five phytosterols in vegetable oil (sunflower oil, olive oil, corn oil, peanut oil), milk and orange juice (soymilk, peanut milk, orange juice), and medicinal herbs (Ginseng, Ganoderma lucidum, Cordyceps, Polygonum multiflorum) for the quality control of functional foods and medicinal herbs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. On-line coupling of supercritical fluid extraction and chromatographic techniques.

    Science.gov (United States)

    Sánchez-Camargo, Andrea Del Pilar; Parada-Alfonso, Fabián; Ibáñez, Elena; Cifuentes, Alejandro

    2017-01-01

    This review summarizes and discusses recent advances and applications of on-line supercritical fluid extraction coupled to liquid chromatography, gas chromatography, and supercritical fluid chromatographic techniques. Supercritical fluids, due to their exceptional physical properties, provide unique opportunities not only during the extraction step but also in the separation process. Although supercritical fluid extraction is especially suitable for recovery of non-polar organic compounds, this technique can also be successfully applied to the extraction of polar analytes by the aid of modifiers. Supercritical fluid extraction process can be performed following "off-line" or "on-line" approaches and their main features are contrasted herein. Besides, the parameters affecting the supercritical fluid extraction process are explained and a "decision tree" is for the first time presented in this review work as a guide tool for method development. The general principles (instrumental and methodological) of the different on-line couplings of supercritical fluid extraction with chromatographic techniques are described. Advantages and shortcomings of supercritical fluid extraction as hyphenated technique are discussed. Besides, an update of the most recent applications (from 2005 up to now) of the mentioned couplings is also presented in this review. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

    Science.gov (United States)

    Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

    2017-12-01

    Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Recent developments in HPLC analysis of β-blockers in biological samples.

    Science.gov (United States)

    Saleem, Kishwar; Ali, Imran; Kulsum, Umma; Aboul-Enein, Hassan Y

    2013-09-01

    β-Adrenergic blockers represent a very important class of drugs that are used worldwide for treating various cardiac diseases. The present article describes the state-of-the art of analyses of β-adrenergic blockers using high-performance liquid chromatography (HPLC). Sample preparation techniques such as liquid-liquid extraction, solid-phase extraction and solid-phase microextraction have been discussed, which are essential prior to HPLC analysis. Additionally, applications of liquid chromatography coupled with tandem mass spectrometry are included. HPLC methods have been reported to include 0.6-26 min as the run times and 0.01 ng/mL to 25 µg/mL as detection limits. The most commonly used columns were C18 with various buffers as the mobile phases, along with various organic modifiers. The optimization of HPLC conditions has been discussed. It has been observed that the reported methods are quite satisfactory for the analyses of β-adrenergic blockers in biological samples. Future perspectives in the hyphenation of solid-phase microextraction-nano-liquid chromatography-tandem mass spectrometry have also been highlighted to achieve detections at nanogram and picogram levels. The present article is very useful for academicians, scientists, drug and pharmaceutical personnel and government regulatory authorities.

  1. Quantitative mass spectrometry of unconventional human biological matrices

    Science.gov (United States)

    Dutkiewicz, Ewelina P.; Urban, Pawel L.

    2016-10-01

    The development of sensitive and versatile mass spectrometric methodology has fuelled interest in the analysis of metabolites and drugs in unconventional biological specimens. Here, we discuss the analysis of eight human matrices-hair, nail, breath, saliva, tears, meibum, nasal mucus and skin excretions (including sweat)-by mass spectrometry (MS). The use of such specimens brings a number of advantages, the most important being non-invasive sampling, the limited risk of adulteration and the ability to obtain information that complements blood and urine tests. The most often studied matrices are hair, breath and saliva. This review primarily focuses on endogenous (e.g. potential biomarkers, hormones) and exogenous (e.g. drugs, environmental contaminants) small molecules. The majority of analytical methods used chromatographic separation prior to MS; however, such a hyphenated methodology greatly limits analytical throughput. On the other hand, the mass spectrometric methods that exclude chromatographic separation are fast but suffer from matrix interferences. To enable development of quantitative assays for unconventional matrices, it is desirable to standardize the protocols for the analysis of each specimen and create appropriate certified reference materials. Overcoming these challenges will make analysis of unconventional human biological matrices more common in a clinical setting. This article is part of the themed issue 'Quantitative mass spectrometry'.

  2. Azoniaspiro salts: towards bridging the gap between room-temperature ionic liquids and molten salts.

    Science.gov (United States)

    Clough, Matthew T; Geyer, Karolin; Hunt, Patricia A; McIntosh, Alastair J S; Rowe, Rebecca; Welton, Tom; White, Andrew J P

    2016-01-28

    In a continued effort to improve the suitability of ionic liquids in applications operating at raised temperatures, novel spirocyclic 'azoniaspiro' salts (with cations derived from five-, six-, seven- and eight-membered rings) are prepared and characterised. The structural and thermal properties of these salts are compared against those of established analogues. The stable geometries and ion pairing behaviour of these species are investigated via a combined experimental/computational approach, employing X-ray crystallography and Density Functional Theory (DFT) methods. Subsequently, the thermal stabilities of these organic salts are characterised and compared using a broad range of techniques. Hyphenated Thermogravimetry-Mass Spectrometry investigations enable complex mechanisms underlying thermal decomposition to be elucidated. Lastly, transition state structures are optimised, corresponding to plausible decomposition mechanisms of the azoniaspiro salt, 6-azoniaspiro[6.5]dodecanium chloride, and one prototypical monocyclic species 1-butyl-1-methylpiperidinium chloride, using DFT. The observed improved thermal stabilities of the azoniaspiro salts, and their potential higher-temperature stable-liquid ranges, render them promising candidates for future ionic liquid applications.

  3. Evaluation and prevention of the negative matrix effect of terpenoids on pesticides in apples quantification by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

    2017-02-03

    The sample matrix can enhance the gas chromatography signal of pesticide residues relative to that obtained with the same concentration of pesticide in solvent. This paper is related to negative matrix effects observed in coupled gas chromatography-mass spectrometry ion trap (GC/MS 2 ) quantification of pesticides in concentrated extracts of apple peel prepared by the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method. It is focused on the pesticides most frequently used on the apple varieties studied, throughout the crop cycle, right up to harvest, to combat pests and diseases and to improve fruit storage properties. Extracts from the fleshy receptacle (flesh), the epiderm (peel) and fruit of three apple varieties were studied by high-performance thin-layer chromatography hyphenated with UV-vis light detection (HPTLC/UV visible). The peel extracts had high concentrations of triterpenic acids (oleanolic and ursolic acids), reaching 25mgkg -1 , whereas these compounds were not detected in the flesh extracts (negative matrix effects in GC/MS 2 . The differences in the behavior of pesticides with respect to matrix effects can be accounted for by the physicochemical characteristics of the molecules (lone pairs, labile hydrogen, conjugation). The HPTLC/UV visible method developed here for the characterization of QuEChERS extracts acts as a complementary clean-up method, aimed to decrease the negative matrix effects of such extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Analytical methods in sphingolipidomics: Quantitative and profiling approaches in food analysis.

    Science.gov (United States)

    Canela, Núria; Herrero, Pol; Mariné, Sílvia; Nadal, Pedro; Ras, Maria Rosa; Rodríguez, Miguel Ángel; Arola, Lluís

    2016-01-08

    In recent years, sphingolipidomics has emerged as an interesting omic science that encompasses the study of the full sphingolipidome characterization, content, structure and activity in cells, tissues or organisms. Like other omics, it has the potential to impact biomarker discovery, drug development and systems biology knowledge. Concretely, dietary food sphingolipids have gained considerable importance due to their extensively reported bioactivity. Because of the complexity of this lipid family and their diversity among foods, powerful analytical methodologies are needed for their study. The analytical tools developed in the past have been improved with the enormous advances made in recent years in mass spectrometry (MS) and chromatography, which allow the convenient and sensitive identification and quantitation of sphingolipid classes and form the basis of current sphingolipidomics methodologies. In addition, novel hyphenated nuclear magnetic resonance (NMR) strategies, new ionization strategies, and MS imaging are outlined as promising technologies to shape the future of sphingolipid analyses. This review traces the analytical methods of sphingolipidomics in food analysis concerning sample extraction, chromatographic separation, the identification and quantification of sphingolipids by MS and their structural elucidation by NMR. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Extracellular synthesis of silver nanoparticles by novel Pseudomonas veronii AS41G inhabiting Annona squamosa L. and their bactericidal activity

    Science.gov (United States)

    Baker, Syed; Mohan Kumar, K.; Santosh, P.; Rakshith, D.; Satish, S.

    2015-02-01

    In present investigation extracellular synthesis of silver nanoparticles were synthesized using cell free supernatant of Pseudomonas veronii AS41G isolated from Annona squamosa L. The bacterium significantly reduced silver nitrate to generate silver nanoparticles which was characterized with hyphenated techniques. Synthesis of silver nanoparticles preliminary confirmed by UV-Visible spectrophotometry with the intense peak at 410 nm, Further FTIR analysis revealed the possible role of biomolecules in the supernatant responsible for mediating the nanoparticles formation. The XRD spectra exhibited the characteristic Bragg peaks of 1 0 0, 1 1 1, 2 0 0, and 2 2 0 facets of the face centred cubic symmetry of nanoparticles suggesting that these nanoparticles were crystalline in nature. TEM microgram showed polydispersity of nanoparticles with size ranging from 5 to 50 nm. Synthesized silver nanoparticles showed antibacterial activity against human and environmental pathogens including MRSA. The study enlightens the role of biosynthesized silver nanoparticles as an emerging alternative for drug resistant microorganisms. The obtained results are promising enough to pave the environmentally benign nanoparticle synthesis processes without use of any toxic chemicals and also envision the emerging role of endophytes towards synthesis of nanoparticles. With scanty reports available on P.veronii species, a new role has been reported in this study which will be very valuable for future researchers working on it.

  6. Evaluation of direct analysis in real time for the determination of highly polar pesticides in lettuce and celery using modified Quick Polar Pesticides Extraction method.

    Science.gov (United States)

    Lara, Francisco J; Chan, Danny; Dickinson, Michael; Lloyd, Antony S; Adams, Stuart J

    2017-05-05

    Direct analysis in real time (DART) was evaluated for the determination of a number of highly polar pesticides using the Quick Polar Pesticides Extraction (QuPPe) method. DART was hyphenated to high resolution mass spectrometry (HRMS) in order to get the required selectivity that allows the determination of these compounds in complex samples such as lettuce and celery. Experimental parameters such as desorption temperature, scanning speed, and distances between the DART ion source and MS inlet were optimized. Two different mass analyzers (Orbitrap and QTOF) and two accessories for sample introduction (Dip-it ® tips and QuickStrip™ sample cards) were evaluated. An extra clean-up step using primary-secondary amine (PSA) was included in the QuPPe method to improve sensitivity. The main limitation found was in-source fragmentation, nevertheless QuPPe-DART-HRMS proved to be a fast and reliable tool with quantitative capabilities for at least seven compounds: amitrole, cyromazine, propamocarb, melamine, diethanolamine, triethanolamine and 1,2,4-triazole. The limits of detection ranged from 20 to 60μg/kg. Recoveries for fortified samples ranged from 71 to 115%, with relative standard deviations <18%. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Multielemental fractionation in human peripheral blood mononuclear cells by size exclusion liquid chromatography coupled to UV and ICP-MS detection.

    Science.gov (United States)

    Alvarado, Gladys; Murillo, Miguel

    2010-10-01

    An analytical methodology is presented in this work to determine metal-biomolecule complexes size distribution patterns of several elements, among different compounds present in human peripheral blood mononuclear cells (PBMC). A hyphenated technique based on size exclusion chromatography (SEC) coupled online to UV and inductively coupled plasma mass spectrometry (ICP-MS) detection is used. Two different SEC columns with separation ranges between 1,500-1,000,000 relative molecular mass (M(r)) (Nanofilm SEC-250) and 5,000 and 100,000 relative molecular mass (M(r)) (TSK-Gel G2000 SW) are used with 10 mmol/L tris-HCl at pH 7.3 as mobile phase. Retention behavior (retention time and peak-area ratios) remained unchanged for several successive separations. Metal-containing compounds are found to a wide range of M(r). Copper-zinc superoxide dismutase, copper and zinc metallothionein, and copper and zinc transferrin are identified in PBMC samples. A high M(r) (147,000) metal-binding protein containing copper and zinc and a high M(r) (107,000) manganese-binding protein were also found; however, these remained unknown.

  8. Liquid chromatography-high resolution mass spectrometry for the analysis of phytochemicals in vegetal-derived food and beverages.

    Science.gov (United States)

    La Barbera, Giorgia; Capriotti, Anna Laura; Cavaliere, Chiara; Montone, Carmela Maria; Piovesana, Susy; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

    2017-10-01

    The recent years witnessed a change in the perception of nutrition. Diet does not only provide nutrients to meet the metabolic requirements of the body, but it also constitutes an active way for the consumption of compounds beneficial for human health. Fruit and vegetables are an excellent source of such compounds, thus the growing interest in characterizing phytochemical sources, structures and activities. Given the interest for phytochemicals in food, the development of advanced and suitable analytical techniques for their identification is fundamental for the advancement of food research. In this review, the state of the art of phytochemical research in food plants is described, starting from sample preparation, throughout extract clean-up and compound separation techniques, to the final analysis, considering both qualitative and quantitative investigations. In this regard, from an analytical point of view, fruit and vegetable extracts are complex matrices, which greatly benefit from the use of modern hyphenated techniques, in particular from the combination of high performance liquid chromatography separation and high resolution mass spectrometry, powerful tools which are being increasingly used in the recent years. Therefore, selected applications to real samples are presented and discussed, in particular for the analysis of phenols, polyphenols and phenolic acids. Finally, some hot points are discussed, such as waste characterization for high value-compounds recovery and the untargeted metabolomics approach. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. 4-hydroxyphenylacetic acid derivatives of inositol from dandelion (Taraxacum officinale) root characterised using LC-SPE-NMR and LC-MS techniques.

    Science.gov (United States)

    Kenny, O; Smyth, T J; Hewage, C M; Brunton, N P; McLoughlin, P

    2014-02-01

    The combination of hyphenated techniques, LC-SPE-NMR and LC-MS, to isolate and identify minor isomeric compounds from an ethyl acetate fraction of Taraxacum officinale root was employed in this study. Two distinct fractions of 4-hydroxyphenylacetic acid derivatives of inositol were isolated and characterised by spectroscopic methods. The (1)H NMR spectra and MS data revealed two groups of compounds, one of which were derivatives of the di-4-hydroxyphenylacetic acid derivative of the inositol compound tetrahydroxy-5-[2-(4-hydroxyphenyl)acetyl] oxycyclohexyl-2-(4-hydroxyphenyl) acetate, while the other group consisted of similar tri-substituted inositol derivatives. For both fractions the derivatives of inositols vary in the number of 4-hydroxyphenylacetic acid groups present and their position and geometry on the inositol ring. In total, three di-substituted and three tri-substituted 4-hydroxyphenylacetic acid inositol derivates were identified for the first time along with a further two previously reported di-substituted inositol derivatives. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. THEORETICAL FOUNDATIONS OF COMPOSING A REFERENCE BOOK OF REGIONAL TOPONYMS

    Directory of Open Access Journals (Sweden)

    Ilyin Dmitriy Yuryevich

    2014-09-01

    Full Text Available The article deals with the linguistic issues of composing a reference book of regional toponyms – a genre that requires special consideration in national lexicography. The assortment of these issues gave the possibility to carry out complex description of regional toponyms on the basis of semantic, functional, and orpthologuos criteria that let unify the names of Volgograd region settlements that are registered in various documents. The significance of the composed reference book is determined by several factors – the presence of local subsystems of geographical names in Russian toponymy; the inconsistency of current orthography norms on using capital letter in compound proprius names and fused-with-hyphen spelling of toponyms and off-toponym derivations; the lack of linguistically justified explanation of peculiarities of grammatical norms in the field of proper names use. The reference book of regional toponyms is based on the object description (toponymic vocabulary, principles of lexical units selection (description of spelling and grammatical properties of toponyms, encyclopedic information, the glossary (full list of toponyms of Volgograd region, typical article. The articles in the reference book are arranged in lexicographical zones with grammatical and semantic markers, lexicographical illustrations, other lexicographical labels, word etymology including. The reference book on Volgograd region toponymy is addressed to executive and administration authorities, journalists, regional ethnographers.

  11. ISMAS international discussion meet on elemental mass spectrometry in health and environmental sciences

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.

    2011-04-01

    Mass spectrometry is an indispensable analytical tool associated with almost all branches of science including biology, chemistry, earth sciences, nuclear science, physics, etc. The technique holds tremendous potential owing to its high sensitivity, selectivity and its ability to measure small changes in the isotopic abundances of different elements. Innovations in mass spectrometry instrumentation are further widening the scope by making it possible to handle very large bio-molecules and polymers. New techniques for mass analysis, novel designs for ionization and developments in electronic accessories have contributed to elevate mass spectrometry to a position of prime importance in research. Development in mass spectrometry has revolutionized the study of micro-nutrient metabolism, of biologically active compounds and for drug discovery in pharmaceutical research. Elemental mass spectrometry is making major contributions to food toxicology, food forensics, and study of metabolism of nutrient minerals including Fe, Zn, Ca, Cu and Se. The area of speciation analysis using hyphenated techniques as well as electro-spray ionization have undergone a phenomenal evolution and development in the recent past. Impressive progress in mass spectrometry towards lower detection limits, higher resolution and molecule-specific detection at trace levels in complex matrices allows new frontiers to be crossed. Papers relevant to INIS are indexed separately

  12. Acylated flavonol glycosides from the forage legume, Onobrychis viciifolia (sainfoin).

    Science.gov (United States)

    Veitch, Nigel C; Regos, Ionela; Kite, Geoffrey C; Treutter, Dieter

    2011-04-01

    Ten acylated flavonol glycosides were isolated from aqueous acetone extracts of the aerial parts of the forage legume, Onobrychis viciifolia, and their structures determined using spectroscopic methods. Among these were eight previously unreported examples which comprised either feruloylated or sinapoylated derivatives of 3-O-di- and 3-O-triglycosides of kaempferol (3,5,7,4'-tetrahydroxyflavone) or quercetin (3,5,7,3',4'-pentahydroxyflavone). The diglycosides were acylated at the primary Glc residue of O-α-Rhap(1→6)-β-Glcp (rutinose), whereas the triglycosides were acylated at the terminal Rha residues of the branched trisaccharides, O-α-Rhap(1→2)[α-Rhap(1→6)]-β-Galp or O-α-Rhap(1→2)[α-Rhap(1→6)]-β-Glcp. Identification of the primary 3-O-linked hexose residues as either Gal or Glc was carried out by negative ion electrospray and serial MS, and cryoprobe NMR spectroscopy. Analysis of UV and MS spectra of the acylated flavonol glycosides provided additional diagnostic features relevant to direct characterisation of these compounds in hyphenated analyses. Quantitative analysis of the acylated flavonol glycosides present in different aerial parts of sainfoin revealed that the highest concentrations were in mature leaflets. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. In-capillary approach to eliminate SDS interferences in antibody analysis by capillary electrophoresis coupled to mass spectrometry.

    Science.gov (United States)

    Sánchez-Hernández, Laura; Montealegre, Cristina; Kiessig, Steffen; Moritz, Bernd; Neusüß, Christian

    2017-04-01

    Capillary electrophoresis is an important technique for the characterization of monoclonal antibodies (mAbs), especially in the pharmaceutical context. However, identification is difficult as upscaling and hyphenation of used methods directly to mass spectrometry is often not possible due to separation medium components that are incompatible with MS detection. Here a CE-MS method for the analysis of mAbs is presented analyzing SDS-complexed samples. To obtain narrow and intensive peaks of SDS-treated antibodies, an in-capillary strategy was developed based on the co-injection of positively charged surfactants and methanol as organic solvent. For samples containing 0.2% (v/v) of SDS, recovered MS peak intensities up to 97 and 95% were achieved using cetyltrimethylammonium bromide or benzalkonium chloride, respectively. Successful removal of SDS was shown in neutral coated capillaries but also in a capillary with a positively charged coating applying reversed polarity. The usefulness of this in-capillary strategy was demonstrated also for other proteins and for antibodies dissolved in up to 10% v/v SDS solution, and in other SDS-containing matrices, including the sieving matrix used in a standard CE-SDS method and gel-buffers applied in SDS-PAGE methods. The developed CE-MS approaches enable fast and reproducible characterization of SDS-complexed antibodies. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Pyrolysis-gas chromatography-isotope ratio mass spectrometry of polyethylene.

    Science.gov (United States)

    González-Pérez, J A; Jiménez-Morillo, N T; de la Rosa, J M; Almendros, G; González-Vila, F J

    2015-04-03

    Polyethylene is probably the most used plastic material in daily life and its accurate analysis is of importance. In this communication the chemical structure of polyethylenes is studied in detail using conventional analytical pyrolysis (Py-GC/MS), bulk stable isotopic analysis (IRMS) and pyrolysis compound specific stable isotopic analysis (Py-CSIA) to measure stable isotope proportions (δ(13)C, δ(15)N and δD) of polyethylene pyrolysis compounds. Polyethylene pyrolysis yields triplet peaks of n-alkanes, α-alkenes and α,ω-alkanedienes. No differences were found for bulk δ(13)C among different polyethylene types. However, conspicuous differences in δD were evident. It was possible to assign structure δ(13)C and δD values to specific polyethylene pyrolysis products in the range 12-18 carbon chain length. Conspicuous differences were found for the pyrolysis products with unsaturated moieties showing significant higher δD values than saturated chains (alkanes) that were deuterium depleted. In addition, a full isotopic fingerprinting (δ(13)C, δ(15)N and δD) for a dye (o-chloroaniline) contained in a polyethylene is reported. To the best of our knowledge this is the first application Py-CSIA to the study of a synthetic polymer. This hyphenated analytical technique is a promising tool to study synthetic materials, providing not only a fingerprinting, but also allowing the traceability of the polymerization process and the origin of the materials. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. An Integrated Strategy for Global Qualitative and Quantitative Profiling of Traditional Chinese Medicine Formulas: Baoyuan Decoction as a Case

    Science.gov (United States)

    Ma, Xiaoli; Guo, Xiaoyu; Song, Yuelin; Qiao, Lirui; Wang, Wenguang; Zhao, Mingbo; Tu, Pengfei; Jiang, Yong

    2016-12-01

    Clarification of the chemical composition of traditional Chinese medicine formulas (TCMFs) is a challenge due to the variety of structures and the complexity of plant matrices. Herein, an integrated strategy was developed by hyphenating ultra-performance liquid chromatography (UPLC), quadrupole time-of-flight (Q-TOF), hybrid triple quadrupole-linear ion trap mass spectrometry (Qtrap-MS), and the novel post-acquisition data processing software UNIFI to achieve automatic, rapid, accurate, and comprehensive qualitative and quantitative analysis of the chemical components in TCMFs. As a proof-of-concept, the chemical profiling of Baoyuan decoction (BYD), which is an ancient TCMF that is clinically used for the treatment of coronary heart disease that consists of Ginseng Radix et Rhizoma, Astragali Radix, Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle, and Cinnamomi Cortex, was performed. As many as 236 compounds were plausibly or unambiguously identified, and 175 compounds were quantified or relatively quantified by the scheduled multiple reaction monitoring (sMRM) method. The findings demonstrate that the strategy integrating the rapidity of UNIFI software, the efficiency of UPLC, the accuracy of Q-TOF-MS, and the sensitivity and quantitation ability of Qtrap-MS provides a method for the efficient and comprehensive chemome characterization and quality control of complex TCMFs.

  16. Effect-directed analysis supporting monitoring of aquatic ...

    Science.gov (United States)

    Aquatic environments are often contaminated with complex mixtures of chemicals that may pose a risk to ecosystems and human health. This contamination cannot be addressed with target analysis alone but tools are required to reduce this complexity and identify those chemicals that might cause adverse effects. Effect-directed analysis (EDA) is designed to meet this challenge and faces increasing interest in water and sediment quality monitoring. Thus, the present paper summarizes current experience with the EDA approach and the tools required,and provides practical advice on their application. The paper highlights the need for proper problem formulation and gives general advice for study design. As the EDA approach is directed by toxicity, basic principles for the selection of bioassays are given as well as a comprehensive compilation of appropriate assays, includingtheir strengths andweaknesses. A specific focus is given to strategies for sampling, extraction and bioassay dosing since they strongly impact prioritization of toxicants in EDA. Reduction of sample complexity mainly relies onfractionation procedures, which are discussed in this paper, including quality assurance and quality control. Automated combinations of fractionation, biotesting and chemical analysis using so-called hyphenated tools can enhance the throughput and might reduce the risk of artifacts in laboratory work. The key to determiningthe chemical structures causing effects is analytical toxi

  17. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

    2008-01-01

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

  18. Analytical developments for the speciation of uranium in zebra fish (Danio rerio) gills after exposure

    International Nuclear Information System (INIS)

    Bucher, Guillaume

    2013-01-01

    The objective of this thesis is to study the cellular compartmentalization and the chelation of uranium (U) by cytosolic proteins of gill cells of the zebra fish (Danio rerio, model specie in aquatic toxicology) under different direct exposure conditions (chronic vs. acute, 20 and 250 μg.L -1 ). This study required the development of hyphenated techniques (SEC, IEF off-gel, RP-UHPLC for the separation, ICP-SFMS, ESI-FTMS/MS for the detection) with the main challenges of maintaining the non-covalent U-biomolecule interactions and enhancing sensitivity for the analysis of environmentally relevant samples. After extraction, 24% to 32% of the total U detected in the gills were present in the cytosolic fraction, in which the U distribution on the biomolecules (as a function of their MW and pI) varied depending on the exposure level. Finally, U target biomolecules mapping allowed us (i) to highlight a particular affinity of U for acidic and/or P-containing proteins and (ii) to identify 24 protein candidates for U binding. (author) [fr

  19. Characterization of petroleum distillates by GC-AED (coupling with gas chromatography and atomic emission detection); Caracterisation des distillats petroliers par couplage chromatographie en phase gazeuse et detection par emission atomique

    Energy Technology Data Exchange (ETDEWEB)

    Baco, F.

    1997-05-21

    This thesis describes the characterization of atmospheric petroleum distillates (kerosenes and gas-oils) and vacuum distillates by hyphenated technic of Gas Chromatography and Atomic Emission Detector (GC-AED). A gas chromatographic simulated distillation, which gives the weight % of sample as a function of the petroleum cut temperature, was adapted to the GC-AED to obtain an original information about the elemental composition profile. After generalities, historic of the development of the instrument and the first petroleum applications are described. In the experimental part, analytical conditions used, different technics of characterisation of distillates and the base of samples analyzed are exposed. After a study of the GC-AED`s performances for the target elements (C, H, S, N), a quantitative method for the elemental analysis of distillates was developed and validated at three levels: total elemental analysis, simulated distillation and elemental composition as a function of the distillation profile. Finally, different ways for the applications of the GC-AED in order to characterize the distillates were explored, in particular to classify products and predict some petroleum properties (cetane number, density,...). The more interesting outlook seems to be the prediction of some properties as a function of the distillation profile. (author) 155 refs.

  20. Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

    Science.gov (United States)

    Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

    2017-04-14

    An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg + ), ethylmercury (EtHg + ) and inorganic mercury (Hg 2+ ) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL -1 for EtHg + and 5-450ngL -1 for MeHg + and Hg 2+ . Limits of detection were 3.0ngL -1 for EtHg + and 1.5ngL -1 for MeHg + and Hg 2+ . Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Gas Chromatography Coupled to Atmospheric Pressure Chemical Ionization FT-ICR Mass Spectrometry for Improvement of Data Reliability.

    Science.gov (United States)

    Schwemer, Theo; Rüger, Christopher P; Sklorz, Martin; Zimmermann, Ralf

    2015-12-15

    Atmospheric pressure chemical ionization (APCI) offers the advantage of molecular ion information with low fragmentation. Hyphenating APCI to gas chromatography (GC) and ultrahigh resolution mass spectrometry (FT-ICR MS) enables an improved characterization of complex mixtures. Data amounts acquired by this system are very huge, and existing peak picking algorithms are usually extremely time-consuming, if both gas chromatographic and ultrahigh resolution mass spectrometric data are concerned. Therefore, automatic routines are developed that are capable of handling these data sets and further allow the identification and removal of known ionization artifacts (e.g., water- and oxygen-adducts, demethylation, dehydrogenation, and decarboxylation). Furthermore, the data quality is enhanced by the prediction of an estimated retention index, which is calculated simply from exact mass data combined with a double bond equivalent correction. This retention index is used to identify mismatched elemental compositions. The approach was successfully tested for analysis of semivolatile components in heavy fuel oil and diesel fuel as well as primary combustion particles emitted by a ship diesel research engine. As a result, 10-28% of the detected compounds, mainly low abundant species, classically assigned by using only the mass spectrometric information, were identified as not valid and removed. Although GC separation is limited by the slow acquisition rate of the FT-ICR MS (<1 Hz), a database driven retention time comparison, as commonly used for low resolution GC/MS, can be applied for revealing isomeric information.

  2. Chemometrics: A new scenario in herbal drug standardization

    Directory of Open Access Journals (Sweden)

    Ankit Bansal

    2014-08-01

    Full Text Available Chromatography and spectroscopy techniques are the most commonly used methods in standardization of herbal medicines but the herbal system is not easy to analyze because of their complexity of chemical composition. Many cutting-edge analytical technologies have been introduced to evaluate the quality of medicinal plants and significant amount of measurement data has been produced. Chemometric techniques provide a good opportunity for mining more useful chemical information from the original data. Then, the application of chemometrics in the field of medicinal plants is spontaneous and necessary. Comprehensive methods and hyphenated techniques associated with chemometrics used for extracting useful information and supplying various methods of data processing are now more and more widely used in medicinal plants, among which chemometrics resolution methods and principal component analysis (PCA are most commonly used techniques. This review focuses on the recent various important analytical techniques, important chemometrics tools and interpretation of results by PCA, and applications of chemometrics in quality evaluation of medicinal plants in the authenticity, efficacy and consistency. Key words: Chemometrics, HELP, Herbal drugs, PCA, OPA

  3. Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

    Science.gov (United States)

    Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

    2016-04-01

    We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Analytical Methods for Chemical and Sensory Characterization of Scent-Markings in Large Wild Mammals: A Review

    Directory of Open Access Journals (Sweden)

    Simone B. Soso

    2014-03-01

    Full Text Available In conjoining the disciplines of “ethology” and “chemistry” the field of “Ethochemistry” has been instituted. Ethochemistry is an effective tool in conservation efforts of endangered species and the understanding of behavioral patterns across all species. Chemical constituents of scent-markings have an important, yet poorly understood function in territoriality, reproduction, dominance, and impact on evolutionary biology, especially in large mammals. Particular attention has recently been focused on scent-marking analysis of great cats (Kalahari leopards (Panthera pardus, puma (Puma concolor snow leopard (Panthera uncia, African lions (Panthera leo, cheetahs (Acinonyx jubatus, and tigers (Panthera tigris for the purpose of conservation. Sensory analyses of scent-markings could address knowledge gaps in ethochemistry. The objective of this review is to summarize the current state-of-the art of both the chemical and sensory analyses of scent-markings in wild mammals. Specific focus is placed on sampling and sample preparation, chemical analysis, sensory analysis, and simultaneous chemical and sensory analyses. Constituents of exocrine and endocrine secretions have been most commonly studied with chromatography-based analytical separations. Odor analysis of scent-markings provides an insight into the animal’s sensory perception. A limited number of articles have been published in the area of sensory characterization of scent marks. Simultaneous chemical and sensory analyses with chromatography-olfactometry hyphenation could potentially aid conservation efforts by linking perceived odor, compounds responsible for odor, and resulting behavior.

  5. Elemental ratios for characterization of quantum-dots populations in complex mixtures by asymmetrical flow field-flow fractionation on-line coupled to fluorescence and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Menendez-Miranda, Mario; Fernandez-Arguelles, Maria T; Costa-Fernandez, Jose M; Encinar, Jorge Ruiz; Sanz-Medel, Alfredo

    2014-08-11

    Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches. Copyright © 2014. Published by Elsevier B.V.

  6. Square-Toed Boots and Felt Hats: Irish Revolutionaries and the Invasion of Canada (1848-1871

    Directory of Open Access Journals (Sweden)

    Marta Ramón-García

    2010-03-01

    Full Text Available The Fenian movement was born in 1858 as an alliance between the Irish Republican Brotherhood, a revolutionary secret society, and the Fenian Brotherhood, an Irish-American organisation intended to supply this society with funds and trained officers. This was not the first time that Irish nationalists on both sides of the Atlantic had tried to cooperate, but it was the first time that there was a steady arrangement in place. The Fenian partnership was extremely successful on the surface, but it was undermined by fundamental differences in customs, political attitudes and ultimate goals between Irish and American Fenians. The clearest evidence of these differences was afforded by the Fenian Brotherhood’s successive attempts to invade Canada between 1866 and 1871. As military episodes the Canadian raids were negligible; as Irish revolutionary attempts they seem absurd. However, they were a perfectly coherent manifestation of the Irish-American “hyphenated identity”. The present article traces the parallel evolution of the Irish Republican Brotherhood and the Fenian Brotherhood up to 1866, and reconstructs the cultural and political reasons for the revival of the Canadian scheme, the ensuing split in the Fenian Brotherhood, and the final collapse of the Fenian alliance.

  7. Non-Polar Natural Products from Bromelia laciniosa, Neoglaziovia variegata and Encholirium spectabile (Bromeliaceae

    Directory of Open Access Journals (Sweden)

    Ole Johan Juvik

    2017-09-01

    Full Text Available Extensive regional droughts are already a major problem on all inhabited continents and severe regional droughts are expected to become an increasing and extended problem in the future. Consequently, extended use of available drought resistant food plants should be encouraged. Bromelia laciniosa, Neoglaziovia variegata and Encholirium spectabile are excellent candidates in that respect because they are established drought resistant edible plants from the semi-arid Caatinga region. From a food safety perspective, increased utilization of these plants would necessitate detailed knowledge about their chemical constituents. However, their chemical compositions have previously not been determined. For the first time, the non-polar constituents of B. laciniosa, N. variegata and E. spectabile have been identified. This is the first thorough report on natural products from N. variegata, E. spectabile, and B. laciniosa. Altogether, 20 non-polar natural products were characterized. The identifications were based on hyphenated gas chromatography-high resolution mass spectrometry (GC-HRMS and supported by 1D and 2D Nuclear Magnetic Resonance (NMR plant metabolomics.

  8. Non-Polar Natural Products from Bromelia laciniosa, Neoglaziovia variegata and Encholirium spectabile (Bromeliaceae).

    Science.gov (United States)

    Juvik, Ole Johan; Holmelid, Bjarte; Francis, George W; Lie Andersen, Heidi; de Oliveira, Ana Paula; Gonçalves de Oliveira Júnior, Raimundo; Guedes da Silva Almeida, Jackson Roberto; Fossen, Torgils

    2017-09-06

    Extensive regional droughts are already a major problem on all inhabited continents and severe regional droughts are expected to become an increasing and extended problem in the future. Consequently, extended use of available drought resistant food plants should be encouraged. Bromelia laciniosa , Neoglaziovia variegata and Encholirium spectabile are excellent candidates in that respect because they are established drought resistant edible plants from the semi-arid Caatinga region. From a food safety perspective, increased utilization of these plants would necessitate detailed knowledge about their chemical constituents. However, their chemical compositions have previously not been determined. For the first time, the non-polar constituents of B. laciniosa , N. variegata and E. spectabile have been identified. This is the first thorough report on natural products from N. variegata , E. spectabile , and B. laciniosa . Altogether, 20 non-polar natural products were characterized. The identifications were based on hyphenated gas chromatography-high resolution mass spectrometry (GC-HRMS) and supported by 1D and 2D Nuclear Magnetic Resonance (NMR) plant metabolomics.

  9. Global approach for the selection of high temperature comprehensive two-dimensional gas chromatography experimental conditions and quantitative analysis in regards to sulfur-containing compounds in heavy petroleum cuts.

    Science.gov (United States)

    Mahé, Laure; Dutriez, Thomas; Courtiade, Marion; Thiébaut, Didier; Dulot, Hugues; Bertoncini, Fabrice

    2011-01-21

    Extending the knowledge on sulfur-containing compounds is crucial for the petroleum industry because they contribute to atmospheric pollution by combustion. Most of them are concentrated in heavy petroleum cuts, such as vacuum gas oils (VGOs). However, the resolution of the existing analytical methods does not allow a quantitative speciation of S-compounds contained in VGOs. Therefore, a high temperature GC×GC chromatograph hyphenated to a SCD was implemented in this study to obtain a quantitative S-compounds speciation. Firstly, various thermally stable stationary phases, in particular the new ionic liquid IL59 and Mega Wax-HT, were investigated in 1D-GC as a way to reduce the number of columns sets to be used in GC×GC. Consequently, several normal and reversed configurations of these columns were selected and tested in GC×GC. Then, a decision method was applied to facilitate the choice of the best combination of columns. Finally, the most adapted methods led to an innovative group type quantification and to a quantitative distribution of heavy sulfur species contained in a VGO sample. These results represent a major step towards the study of S-compounds in heavy petroleum cuts. Copyright © 2010 Elsevier B.V. All rights reserved.

  10. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  11. Resolution-optimized headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS) for non-targeted olive oil profiling.

    Science.gov (United States)

    Gerhardt, Natalie; Birkenmeier, Markus; Sanders, Daniel; Rohn, Sascha; Weller, Philipp

    2017-06-01

    A prototype gas chromatography-ion mobility spectrometry (GC-IMS) system, hyphenating temperature-ramped headspace GC to a modified drift time IMS cell, was evaluated and compared to a conventional, isothermal capillary column (CC)-IMS system on the example of the geographical differentiation of extra virgin olive oils (EVOO) from Spain and Italy. It allows orthogonal, 2D separation of complex samples and individual detection of compounds in robust and compact benchtop systems. The information from the high-resolution 3D fingerprints of volatile organic compound (VOC) fractions of EVOO samples were extracted by specifically developed chemometric MATLAB® routines to differentiate between the different olive oil provenances. A combination of unsupervised principal component analysis (PCA) with two supervised procedures, linear discriminant analysis (LDA) and k-nearest neighbors (kNN), was applied to the experimental data. The results showed very good discrimination between oils of different geographical origins, featuring 98 and 92% overall correct classification rate for PCA-LDA and kNN classifier, respectively. Furthermore, the results showed that the higher resolved 3D fingerprints obtained from the GC-IMS system provide superior resolving power for non-targeted profiling of VOC fractions from highly complex samples such as olive oil. Graphical abstract Principle of the determination of geographic origins of olive oils by chemometric analysis of three-dimensional HS-GC-IMS fingerprints.

  12. Punctuation as readability and textuality factor in technical discourse

    Directory of Open Access Journals (Sweden)

    Carmen Sancho Guinda

    2002-04-01

    Full Text Available This paper studies the incidence of punctuation on the reading comprehension of technical discourse and its role as a factor of textuality. Starting out from the notions of textuality and punctuation functions formulated by different linguistic approaches, an analysis has been made to quantify the decoding skills and punctuating competence of 60 Aeronautical Engineering students, as well as to determine the nature and effects of their punctuation errors. The survey has been focused on the Full Stop, the comma and the hyphen due to their highly conflicting uses as regards the identification of immediate sentence constituents and semantic relationships. The results obtained suggest that most students have a poor knowledge of punctuation rules and little awareness of punctuation as a textual elementaffecting readability. Errors are in the main related to comma use and produced by transference, either of Spanish punctuating habits into English, or of individual prosodic patterns into writing, while meaning appears to be the prevailing punctuating criterion over sound and syntax. Punctuation proves an effective tool for the anticipation of implicit meanings and an untapped resource in the teaching of the diverse communicative and stylistic possibilities offered by technical texts.

  13. PY-GC-MS applied to the identification of synthetic resins in Brazilian painting

    International Nuclear Information System (INIS)

    Redigolo, Marcelo M.; Amaral, Priscila O.; Leao, Claudio; Crepaldi, Caike; Munita, Casimiro S.; Bustillos, Oscar V.; Russo, Tatiana; Mendonca, Valeria de

    2015-01-01

    Works of art are appreciated for their material and immaterial value. Restoring objects of art is a delicate procedure, mostly due to the irreversibility of the interventions. Hence, it is recommended to study the chemical composition of the object to avoid errors. The premise for restoring or conserving these objects is their physical preservation, i.e., it is advisable to avoid sampling and, when necessary, samples must be minute. The analytical techniques that fulfill these requirements are limited. Mass spectrometry (MS) is a versatile technique due to its hyphenation possibilities. Recently, it has being employed in the identification of natural and synthetic resins in works of art. Electron ionization (EI) is a powerful method of molecular fragmentation employed in the detection of volatile organic compounds by mass spectrometry. In this work, two micrograms (μg) of sample from a Brazilian contemporary painting were analyzed by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) technique. A microfurnace-type pyrolyzer was coupled to a gas chromatograph, using a non-polar capillary column. The electron ionization was achieved applying 70 eV electron energy. This technique is suitable for the analysis of material from objects of art, being specific, accurate and requiring minimal sampling. The synthetic resin diallyl phthalate (DAP) was identified by the Py-GC/MS technique. (author)

  14. Coupling HPLC-SPE-NMR with a microplate-based high-resolution antioxidant assay for efficient analysis of antioxidants in food--validation and proof-of-concept study with caper buds.

    Science.gov (United States)

    Wiese, Stefanie; Wubshet, Sileshi G; Nielsen, John; Staerk, Dan

    2013-12-15

    This work describes the coupling of a microplate-based antioxidant assay with a hyphenated system consisting of high-performance liquid chromatography-solid-phase extraction-nuclear magnetic resonance spectroscopy, i.e., HPLC-SPE-NMR/high-resolution antioxidant assay, for the analysis of complex food extracts. The applicability of the microplate-based antioxidant assay for high-resolution screening of common food phenolics as well as parameters related to their trapping efficiency, elution behavior, and recovery on/from SPE cartridges are described. It was found that the microplate-based high-resolution antioxidant assay is an attractive and easy implementable alternative to direct on-line screening methods. Furthermore, it was shown that Resin SH and Resin GP SPE material are superior to RP C18HD for trapping of phenolic compounds. Proof-of-concept study was performed with caper bud extract, revealing the most important antioxidants to be quercetin, kaempferol, rutin, kaempferol-3-O-β-rutinoside and N(1),N(5),N(10)-triphenylpropenoyl spermidine amides. Targeted isolation of the latter, and comprehensive NMR experiments showed them to be N(1),N(10)-di-(E)-caffeoyl-N(5)-p-(E)-coumaroyl spermidine, N(1)-(E)-caffeoyl-N(5),N(10)-di-p-(E)-coumaroyl spermidine, N(10)-(E)-caffeoyl-N(1),N(5)-di-p-(E)-coumaroyl spermidine, and N(1),N(5),N(10)-tri-p-(E)-coumaroyl spermidine amides. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Do interoperable national information systems enhance availability of data to assess the effect of scale-up of HIV services on health workforce deployment in resource-limited countries?

    Science.gov (United States)

    Oluoch, Tom; Muturi, David; Kiriinya, Rose; Waruru, Anthony; Lanyo, Kevin; Nguni, Robert; Ojwang, James; Waters, Keith P; Richards, Janise

    2015-01-01

    Sub-Saharan Africa (SSA) bears the heaviest burden of the HIV epidemic. Health workers play a critical role in the scale-up of HIV programs. SSA also has the weakest information and communication technology (ICT) infrastructure globally. Implementing interoperable national health information systems (HIS) is a challenge, even in developed countries. Countries in resource-limited settings have yet to demonstrate that interoperable systems can be achieved, and can improve quality of healthcare through enhanced data availability and use in the deployment of the health workforce. We established interoperable HIS integrating a Master Facility List (MFL), District Health Information Software (DHIS2), and Human Resources Information Systems (HRIS) through application programmers interfaces (API). We abstracted data on HIV care, health workers deployment, and health facilities geo-coordinates. Over 95% of data elements were exchanged between the MFL-DHIS and HRIS-DHIS. The correlation between the number of HIV-positive clients and nurses and clinical officers in 2013 was R2=0.251 and R2=0.261 respectively. Wrong MFL codes, data type mis-match and hyphens in legacy data were key causes of data transmission errors. Lack of information exchange standards for aggregate data made programming time-consuming.

  16. Chemometrics: A new scenario in herbal drug standardization.

    Science.gov (United States)

    Bansal, Ankit; Chhabra, Vikas; Rawal, Ravindra K; Sharma, Simant

    2014-08-01

    Chromatography and spectroscopy techniques are the most commonly used methods in standardization of herbal medicines but the herbal system is not easy to analyze because of their complexity of chemical composition. Many cutting-edge analytical technologies have been introduced to evaluate the quality of medicinal plants and significant amount of measurement data has been produced. Chemometric techniques provide a good opportunity for mining more useful chemical information from the original data. Then, the application of chemometrics in the field of medicinal plants is spontaneous and necessary. Comprehensive methods and hyphenated techniques associated with chemometrics used for extracting useful information and supplying various methods of data processing are now more and more widely used in medicinal plants, among which chemometrics resolution methods and principal component analysis (PCA) are most commonly used techniques. This review focuses on the recent various important analytical techniques, important chemometrics tools and interpretation of results by PCA, and applications of chemometrics in quality evaluation of medicinal plants in the authenticity, efficacy and consistency.

  17. Optimizing separations in online comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

    2018-01-01

    Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

  18. Bioanalytical Applications of Fluorescence Line-Narrowing and Non-Line-Narrowing Spectroscopy Interfaced with Capillary Electrophoresis and High-Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, Kenneth Paul [Iowa State Univ., Ames, IA (United States)

    2001-01-01

    Capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) are widely used analytical separation techniques with many applications in chemical, biochemical, and biomedical sciences. Conventional analyte identification in these techniques is based on retention/migration times of standards; requiring a high degree of reproducibility, availability of reliable standards, and absence of coelution. From this, several new information-rich detection methods (also known as hyphenated techniques) are being explored that would be capable of providing unambiguous on-line identification of separating analytes in CE and HPLC. As further discussed, a number of such on-line detection methods have shown considerable success, including Raman, nuclear magnetic resonance (NMR), mass spectrometry (MS), and fluorescence line-narrowing spectroscopy (FLNS). In this thesis, the feasibility and potential of combining the highly sensitive and selective laser-based detection method of FLNS with analytical separation techniques are discussed and presented. A summary of previously demonstrated FLNS detection interfaced with chromatography and electrophoresis is given, and recent results from on-line FLNS detection in CE (CE-FLNS), and the new combination of HPLC-FLNS, are shown.

  19. Prealamethicin F50 and related peptaibols fromTrichoderma arundinaceum: Validation of their authenticity viain situchemical analysis.

    Science.gov (United States)

    Rivera-Chávez, José; Raja, Huzefa A; Graf, Tyler N; Gallagher, Jacklyn M; Metri, Prashant; Xue, Ding; Pearce, Cedric J; Oberlies, Nicholas H

    2017-01-01

    In the field of natural products chemistry, a common question pertains to the authenticity of an isolated compound, i.e. are the interesting side chains biosynthesized naturally or an artefact of the isolation/purification processes? The droplet-liquid microjunction-surface sampling probe (droplet-LMJ-SSP) coupled to a hyphenated system (UPLC-UV-HRESIMS) empowers the analysis of natural product sources in situ , providing data on the biosynthetic timing and spatial distribution of secondary metabolites. In this study the droplet-LMJ-SSP was utilized to validate the authenticity of two new peptaibols ( 2 and 3 ) as biosynthesized secondary metabolites, even though both them had structural features that could be perceived as artefacts. Compounds 2 and 3 were isolated from the scaled up fermentation of Trichoderma arundinaceum (strain MSX70741), along with a new member of the trichobrevin BIII complex ( 1 ), and four known compounds ( 4 - 7 ). The structures of the isolates were established using a set of spectroscopic and spectrometric methods, and their absolute configurations were determined by Marfey's analysis. The cytotoxic activity of compounds 1 , 3 , 4 and 6 was evaluated against a panel of cancer cell lines, where cytotoxic activity in the single digit μM range was observed.

  20. Trying to detect gas-phase ions? Understanding Ion Mobility Spectrometry

    Science.gov (United States)

    Cumeras, R.; Figueras, E.; Davis, C.E.; Baumbach, J.I.; Gràcia, I.

    2014-01-01

    Ion Mobility Spectrometry (IMS) is a widely used and ‘well-known’ technique of ion separation in gaseous phase based on the differences of ion mobilities under an electric field. This technique has received increased interest over the last several decades as evidenced by the pace and advances of new IMS devices available. In this review we explore the hyphenated techniques that are used with IMS, especially mass spectrometry as identification approach and multi-capillary column as pre-separation approach. Also, we will pay special attention to the key figures of merit of the ion mobility spectrum and how data is treated, and the influences of the experimental parameters in both a conventional drift time IMS (DTIMS) and a miniaturized IMS also known as high Field Asymmetric IMS (FAIMS) in the planar configuration. The current review article is preceded by a companion review article which details the current instrumentation and to the sections that configures both a conventional DTIMS and FAIMS devices. Those reviews will give the reader an insightful view of the main characteristics and aspects of the IMS technique. PMID:25465248

  1. Current advances and challenges in microfluidic free-flow electrophoresis-A critical review.

    Science.gov (United States)

    Novo, Pedro; Janasek, Dirk

    2017-10-23

    The research field on microfluidic free-flow electrophoresis has developed vast amounts of devices, methods, applications and raised new questions, often in analogy to conventional techniques from which it derives. Most efforts have been employed on device development and a myriad of architectures and fabrication techniques have been reported using simple proof-of-principle separations. As technological aspects reach a quite mature state, researchers' new challenges include the development of protocols for the separation of complex mixtures, as required in the fields of application. The success of this effort is extremely dependent on the capability to transfer the device's fabrication to an industrial setting as well as to ensure interfacing simplicity, namely at the solutions' supply and collection, and actuation such as electric potential application and temperature control. Other advanced applications such as direct interfacing to downstream systems such as mass spectrometry, integration of sensing and feedback controls will require further development in the laboratory. In this review we provide an overview on the field, from basic concepts, through advanced developments both in the theoretical and experimental arenas, and addressing the above details. A comprehensive survey of designs, materials and applications is presented with particular highlights to most recent developments, namely the integration of electrodes, flow control and hyphenation of microfluidic free-flow electrophoresis with other techniques. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Characterization and Quantification of Compounds in the Hydroalcoholic Extract of the Leaves from Terminalia catappa Linn. (Combretaceae and Their Mutagenic Activity

    Directory of Open Access Journals (Sweden)

    Francisco José Mininel

    2014-01-01

    Full Text Available Terminalia is a genus of Combretaceous plants widely distributed in tropical and subtropical regions. Thus, the aim of this study was to quantify the majority compounds of the hydroalcoholic extract (7 : 3, v/v of the leaves from T. catappa by HPLC-PDA, chemically characterize by hyphenated techniques (HPLC-ESI-IT-MSn and NMR, and evaluate its mutagenic activity by the Salmonella/microsome assay on S. typhimurium strains TA98, TA97a, TA100, and TA102. The quantification of analytes was performed using an external calibration standard. Punicalagin is the most abundant polyphenol found in the leaves. The presence of this compound as a mixture of anomers was confirmed using HPLC-PDA and 1H and 13C NMR. Mutagenic activity was observed in strains TA100 and TA97a. As the extract is a complex mixture of punicalagin, its derivatives, and several other compounds, the observed mutagenicity may be explained in part by possible synergistic interaction between the compounds present in the extract. These studies show that mutagenic activity of T. catappa in the Ames test can only be observed when measured at high concentrations. However, considering the mutagenic effects observed for T. catappa, this plant should be used cautiously for medicinal purposes.

  3. Characterization and Quantification of Compounds in the Hydroalcoholic Extract of the Leaves from Terminalia catappa Linn. (Combretaceae) and Their Mutagenic Activity.

    Science.gov (United States)

    Mininel, Francisco José; Leonardo Junior, Carlos Sérgio; Espanha, Lívia Greghi; Resende, Flávia Aparecida; Varanda, Eliana Aparecida; Leite, Clarice Queico Fujimura; Vilegas, Wagner; Dos Santos, Lourdes Campaner

    2014-01-01

    Terminalia is a genus of Combretaceous plants widely distributed in tropical and subtropical regions. Thus, the aim of this study was to quantify the majority compounds of the hydroalcoholic extract (7 : 3, v/v) of the leaves from T. catappa by HPLC-PDA, chemically characterize by hyphenated techniques (HPLC-ESI-IT-MS(n)) and NMR, and evaluate its mutagenic activity by the Salmonella/microsome assay on S. typhimurium strains TA98, TA97a, TA100, and TA102. The quantification of analytes was performed using an external calibration standard. Punicalagin is the most abundant polyphenol found in the leaves. The presence of this compound as a mixture of anomers was confirmed using HPLC-PDA and (1)H and (13)C NMR. Mutagenic activity was observed in strains TA100 and TA97a. As the extract is a complex mixture of punicalagin, its derivatives, and several other compounds, the observed mutagenicity may be explained in part by possible synergistic interaction between the compounds present in the extract. These studies show that mutagenic activity of T. catappa in the Ames test can only be observed when measured at high concentrations. However, considering the mutagenic effects observed for T. catappa, this plant should be used cautiously for medicinal purposes.

  4. Online coupling of pure O{sub 2} thermo-optical methods – {sup 14}C AMS for source apportionment of carbonaceous aerosols

    Energy Technology Data Exchange (ETDEWEB)

    Agrios, Konstantinos [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, Bern (Switzerland); Paul Scherrer Institute, Villigen (Switzerland); Salazar, Gary [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, Bern (Switzerland); Zhang, Yan-Lin; Uglietti, Chiara [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, Bern (Switzerland); Paul Scherrer Institute, Villigen (Switzerland); Battaglia, Michael [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, Bern (Switzerland); Luginbühl, Marc [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Ciobanu, Viorela Gabriela [Paul Scherrer Institute, Villigen (Switzerland); Vonwiller, Matthias [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, Bern (Switzerland); Paul Scherrer Institute, Villigen (Switzerland); Szidat, Sönke, E-mail: szidat@dcb.unibe.ch [Department of Chemistry and Biochemistry, University of Bern, Bern (Switzerland); Oeschger Centre for Climate Change Research, University of Bern, Bern (Switzerland)

    2015-10-15

    This paper reports on novel separation methods developed for the direct determination of {sup 14}C in organic carbon (OC) and elemental carbon (EC), two sub-fractions of total carbon (TC) of atmospheric air particulate matter. Until recently, separation of OC and EC has been performed off-line by manual and time-consuming techniques that relied on the collection of massive CO{sub 2} fractions. We present here two on-line hyphenated techniques between a Sunset OC/EC analyzer and a MICADAS (MIni radioCArbon DAting System) accelerator mass spectrometer (AMS) equipped with a gas ion source. The first implementation facilitates the direct measurement in the low sample size range (<10 μg C) with high throughput on a routine basis, while the second explores the potential for a continuous-flow real-time CO{sub 2} gas feed into the ion source. The performance achieved with reference materials and real atmospheric samples will be discussed to draw conclusions on the improvement offered in the field of {sup 14}C aerosol source apportionment.

  5. Anionic metabolite profiling by capillary electrophoresis-mass spectrometry using a noncovalent polymeric coating. Orange juice and wine as case studies.

    Science.gov (United States)

    Acunha, Tanize; Simó, Carolina; Ibáñez, Clara; Gallardo, Alberto; Cifuentes, Alejandro

    2016-01-08

    In several metabolomic studies, it has already been demonstrated that capillary electrophoresis hyphenated to mass spectrometry (CE-MS) can detect an important group of highly polar and ionized metabolites that are overseen by techniques such as NMR, LC-MS and GC-MS, providing complementary information. In this work, we present a strategy for anionic metabolite profiling by CE-MS using a cationic capillary coating. The polymer, abbreviated as PTH, is composed of a poly-(N,N,N',N'-tetraethyldiethylenetriamine, N-(2-hydroxypropyl) methacrylamide, TEDETAMA-co-HPMA (50:50) copolymer. A CE-MS method based on PTH-coating was optimized for the analysis of a group of 16 standard anionic metabolites. Separation was achieved within 12min, with high separation efficiency (up to 92,000 theoretical plates per meter), and good repeatability, namely, relative standard deviation values for migration times and peak areas were below 0.2 and 2.1%, respectively. The optimized method allowed the detection of 87 metabolites in orange juice and 142 metabolites in red wine, demonstrating the good possibilities of this strategy for metabolomic applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. [E]motion in the Nineteenth Century: A Culture of Fidgets

    Directory of Open Access Journals (Sweden)

    Karen Chase

    2014-10-01

    Full Text Available I see the fidget as a neglected aspect of the sense of touch, which collects a range of suggestive imaginative movements and which opens towards a rereading of Dickens's construal of character, its relation to the self, and its social world. An affective swamping of personality repeatedly overwhelms the barriers of personality. A tic, a flick, an insult, a plea, a joke, a contortion, a wink, a tickle, a prod - such fidgets lead an active life in the novels. They often reflect the friction of inter-subjectivity, but also the abrasions between character and the universe of objects. The twittering of a Miss Flite in 'Bleak House', Bradley Headstone's physical eruptions of rage, Mr F's Aunt's proleptic warnings and Flora Finching's galloping tale-telling in 'Little Dorrit', the handiwork of Uriah Heep in 'David Copperfield', the insuppressible hyphenated speech of Jingle in 'Pickwick Papers' - these are radiant instances. My article looks to give the fidget its due and to initiate more scholarly conversation on the circle of issues that it generates: mind and body, subjects and objects, textual continuity and its disruptions.

  7. Online coupling of pure O2 thermo-optical methods – 14C AMS for source apportionment of carbonaceous aerosols

    International Nuclear Information System (INIS)

    Agrios, Konstantinos; Salazar, Gary; Zhang, Yan-Lin; Uglietti, Chiara; Battaglia, Michael; Luginbühl, Marc; Ciobanu, Viorela Gabriela; Vonwiller, Matthias; Szidat, Sönke

    2015-01-01

    This paper reports on novel separation methods developed for the direct determination of 14 C in organic carbon (OC) and elemental carbon (EC), two sub-fractions of total carbon (TC) of atmospheric air particulate matter. Until recently, separation of OC and EC has been performed off-line by manual and time-consuming techniques that relied on the collection of massive CO 2 fractions. We present here two on-line hyphenated techniques between a Sunset OC/EC analyzer and a MICADAS (MIni radioCArbon DAting System) accelerator mass spectrometer (AMS) equipped with a gas ion source. The first implementation facilitates the direct measurement in the low sample size range (<10 μg C) with high throughput on a routine basis, while the second explores the potential for a continuous-flow real-time CO 2 gas feed into the ion source. The performance achieved with reference materials and real atmospheric samples will be discussed to draw conclusions on the improvement offered in the field of 14 C aerosol source apportionment.

  8. Analytical Strategies Involved in the Detailed Componential Characterization of Biooil Produced from Lignocellulosic Biomass

    Directory of Open Access Journals (Sweden)

    Yao Lu

    2017-01-01

    Full Text Available Elucidation of chemical composition of biooil is essentially important to evaluate the process of lignocellulosic biomass (LCBM conversion and its upgrading and suggest proper value-added utilization like producing fuel and feedstock for fine chemicals. Although the main components of LCBM are cellulose, hemicelluloses, and lignin, the chemicals derived from LCBM differ significantly due to the various feedstock and methods used for the decomposition. Biooil, produced from pyrolysis of LCBM, contains hundreds of organic chemicals with various classes. This review covers the methodologies used for the componential analysis of biooil, including pretreatments and instrumental analysis techniques. The use of chromatographic and spectrometric methods was highlighted, covering the conventional techniques such as gas chromatography, high performance liquid chromatography, Fourier transform infrared spectroscopy, nuclear magnetic resonance, and mass spectrometry. The combination of preseparation methods and instrumental technologies is a robust pathway for the detailed componential characterization of biooil. The organic species in biooils can be classified into alkanes, alkenes, alkynes, benzene-ring containing hydrocarbons, ethers, alcohols, phenols, aldehydes, ketones, esters, carboxylic acids, and other heteroatomic organic compounds. The recent development of high resolution mass spectrometry and multidimensional hyphenated chromatographic and spectrometric techniques has considerably elucidated the composition of biooils.

  9. Rapid and sensitive determination of carbohydrates in foods using high temperature liquid chromatography with evaporative light scattering detection.

    Science.gov (United States)

    Terol, Amanda; Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2012-04-01

    In the present work, an evaporative light scattering detector was used as a high-temperature liquid chromatography detector for the determination of carbohydrates. The compounds studied were glucose, fructose, galactose, sucrose, maltose, and lactose. The effect of column temperature on the retention times and detectability of these compounds was investigated. Column heating temperatures ranged from 25 to 175°C. The optimum temperature in terms of peak resolution and detectability with pure water as mobile phase and a liquid flow rate of 1 mL/min was 150°C as it allowed the separation of glucose and the three disaccharides here considered in less than 3 min. These conditions were employed for lactose determination in milk samples. Limits of quantification were between 2 and 4.7 mg/L. On the other hand, a temperature gradient was developed for the simultaneous determination of glucose, fructose, and sucrose in orange juices, due to coelution of monosaccharides at temperatures higher than 70°C, being limits of quantifications between 8.5 and 12 mg/L. The proposed hyphenation was successfully applied to different types of milk and different varieties of oranges and mandarins. Recoveries for spiked samples were close to 100% for all the studied analytes. © 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Aspectos toxicológicos e inmunológicos del veneno del escorpión Tityus pachyurus

    Directory of Open Access Journals (Sweden)

    Rafael Valderrama

    2001-04-01

    Full Text Available

  1. Elemental Bioimaging by Means of Fast Scanning Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry

    Science.gov (United States)

    Wehe, Christoph A.; Thyssen, Georgina M.; Herdering, Christina; Raj, Indra; Ciarimboli, Giuliano; Sperling, Michael; Karst, Uwe

    2015-08-01

    One of the most common setups for elemental bioimaging, the hyphenation of a laser ablation (LA) system and an inductively coupled plasma mass spectrometer (ICP-MS), was expanded by adding full scan mass spectrometric information as another dimension of information. While most studies deal with the analysis of typically not more than up to 10 isotopes per scan cycle, a fast scanning quadrupole mass analyzer was utilized to record the full mass spectrum of interest in this work. Mass-to-charge ratios from 6 to 250 were observed within one cycle. Besides the x- and y-position on the ablated sample and the intensity, the m/z-ratio served as fourth variable for each pixel of the obtained data, closing thereby the gap between "inorganic" and "organic" mass spectrometric imaging techniques. The benefits of this approach include an improved control of interferences, the discovery of unexpected elemental distributions, the possibility to plot isotopic ratios, and to integrate the intensities of a certain number of mass channels recorded for each isotope, thus virtually increasing sensitivity. The respective data are presented for dried droplets as well as embedded animal and human tissue slices. Limits of detection were calculated and found to be in accordance with counting statistics. A dedicated software macro was developed for data manipulation prior to common evaluation and image creation.

  2. Determination of target fat-soluble micronutrients in rainbow trout's muscle and liver tissues by liquid chromatography with diode array-tandem mass spectrometry detection.

    Science.gov (United States)

    Pérez Fernández, Virginia; Ventura, Salvatore; Tomai, Pierpaolo; Curini, Roberta; Gentili, Alessandra

    2017-03-01

    This paper describes an analytical approach, based on LC-diode array detector-MS/MS (LC-DAD-MS/MS), for characterizing the fat-soluble micronutrient fraction in rainbow trout (Oncorhynchus mykiss). Two different procedures were applied to isolate the analytes from liver and muscle tissue: overnight cold saponification to hydrolyze bound forms and to simplify the analysis; matrix solid-phase dispersion to avoid artifacts and to maintain unaltered the naturally occurring forms. Analytes were separated on a C 30 analytical column by using a nonaqueous reversed mobile phase compatible with the atmospheric pressure chemical ionization. Compared to other works, the most relevant advantage of the here illustrated method is the large amount of information obtained with few analytical steps: nine fat-soluble vitamins (3,4-dehydroretinol, retinol, cholecalciferol, ergocalciferol, α-tocopherol, γ-tocopherol, δ-tocopherol, phylloquinone, and menaquinone-4) and eight carotenoids (all-trans-lutein, all-trans-astaxanthin, all-trans-zeaxanthin, all-trans-β-cryptoxanthin, all-trans-canthaxanthin, all-trans-ζ-carotene, all-trans-β-carotene, and all-trans-γ-carotene) were quantified after the method validation, while other untargeted carotenoids were tentatively identified by exploiting the identification power of the LC-DAD-MS/MS hyphenation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Sb(V) reactivity with human blood components: redox effects.

    Science.gov (United States)

    López, Silvana; Aguilar, Luis; Mercado, Luis; Bravo, Manuel; Quiroz, Waldo

    2015-01-01

    We assessed the reactivity of Sb(V) in human blood. Sb(V) reactivity was determined using an HPLC-HG-AFS hyphenated system. Sb(V) was partially reduced to Sb(III) in blood incubation experiments; however, Sb(III) was a highly unstable species. The addition of 0.1 mol L(-1) EDTA prevented Sb(III) oxidation, thus enabling the detection of the reduction of Sb(V) to Sb(III). The transformation of Sb(V) to Sb(III) in human whole blood was assessed because the reduction of Sb(V) in human blood may likely generate redox side effects. Our results indicate that glutathione was the reducing agent in this reaction and that Sb(V) significantly decreased the GSH/GSSG ratio from 0.32 ± 0.09 to 0.07 ± 0.03. Moreover, the presence of 200 ng mL(-1) of Sb(V) increased the activity of superoxide dismutase from 4.4 ± 0.1 to 7.0 ± 0.4 U mL(-1) and decreased the activity of glutathione peroxidase from 62 ± 1 to 34 ± 2 nmol min(-1) mL(-1).

  4. Sb(V reactivity with human blood components: redox effects.

    Directory of Open Access Journals (Sweden)

    Silvana López

    Full Text Available We assessed the reactivity of Sb(V in human blood. Sb(V reactivity was determined using an HPLC-HG-AFS hyphenated system. Sb(V was partially reduced to Sb(III in blood incubation experiments; however, Sb(III was a highly unstable species. The addition of 0.1 mol L(-1 EDTA prevented Sb(III oxidation, thus enabling the detection of the reduction of Sb(V to Sb(III. The transformation of Sb(V to Sb(III in human whole blood was assessed because the reduction of Sb(V in human blood may likely generate redox side effects. Our results indicate that glutathione was the reducing agent in this reaction and that Sb(V significantly decreased the GSH/GSSG ratio from 0.32 ± 0.09 to 0.07 ± 0.03. Moreover, the presence of 200 ng mL(-1 of Sb(V increased the activity of superoxide dismutase from 4.4 ± 0.1 to 7.0 ± 0.4 U mL(-1 and decreased the activity of glutathione peroxidase from 62 ± 1 to 34 ± 2 nmol min(-1 mL(-1.

  5. Metabolomics and Proteomics of Brassica napus Guard Cells in Response to Low CO2

    Directory of Open Access Journals (Sweden)

    Sisi Geng

    2017-07-01

    Full Text Available Stomatal guard cell response to various stimuli is an important process that balances plant carbon dioxide (CO2 uptake and water transpiration. Elevated CO2 induces stomatal closure, while low CO2 promotes stomatal opening. The signaling process of elevated CO2 induced stomatal closure has been extensively studied in recent years. However, the mechanism of low CO2 induced stomatal opening is not fully understood. Here we report metabolomic and proteomic responses of Brassica napus guard cells to low CO2 using hyphenated mass spectrometry technologies. A total of 411 metabolites and 1397 proteins were quantified in a time-course study of low CO2 effects. Metabolites and proteins that exhibited significant changes are overrepresented in fatty acid metabolism, starch and sucrose metabolism, glycolysis and redox regulation. Concomitantly, multiple hormones that promote stomatal opening increased in response to low CO2. Interestingly, jasmonic acid precursors were diverted to a branch pathway of traumatic acid biosynthesis. These results indicate that the low CO2 response is mediated by a complex crosstalk between different phytohormones.

  6. Integrating ontologies of rare diseases and radiological diagnosis.

    Science.gov (United States)

    Kahn, Charles E

    2015-11-01

    The author sought to integrate an ontology of rare diseases with a large ontological model of radiological diagnosis. The Orphanet Rare Disease Ontology (ORDO) comprised 6794 rare diseases. The Radiology Gamuts Ontology (RGO) incorporated 16 197 terms and 53,425 causal relations linking disorders to imaging manifestations. Semi-automated string-matching was used to match ORDO terms to RGO terms. Of 6794 ORDO terms, 1587 (23.3%) were matched to RGO terms. An additional 700 ORDO terms whose names were hyphenated lists of phenotypic features were added to RGO with causal links from the disease name to the various features. Matched terms were more likely to have higher disease prevalence. Integrating these ontologies expanded the set of terms and scope of knowledge available for radiological differential diagnosis, and can support translational rare-disease research by linking knowledge of genetics and imaging phenotypes. © The Author 2015. Published by Oxford University Press on behalf of the American Medical Informatics Association. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  7. Identification of Polish cochineal (Porphyrophora polonica L.) in historical textiles by high-performance liquid chromatography coupled with spectrophotometric and tandem mass spectrometric detection.

    Science.gov (United States)

    Lech, Katarzyna; Jarosz, Maciej

    2016-05-01

    The present work reports a method for identification of Polish cochineal (Porphyrophora polonica L.) in historical fabrics by the use of high-performance liquid chromatography coupled with diode array and tandem mass spectrometric detection with electrospray ionization (HPLC-DAD-ESI MS/MS). This hyphened technique allows detection and identification of 16 new minor colorants present in the discussed scale insect (including two previously observed by Wouters and Verhecken (Ann Soc Entomol Fr. 1989;25:393-410), but specified only as compounds of unknown structures) that do not occur (e.g., in American cochineal). The MS/MS experiments, complemented with UV-VIS data, enable identification of mono- and di-, C- and O-hexosides of kermesic and flavokermesic acids or their derivatives. The present paper introduces a fingerprint of color compounds present in Polish cochineal and defines them, particularly pp6 (ppI, O-hexoside of flavokermesic acid), as its markers allow distinguishing of Polish-cochineal reds from the American ones. Usefulness of the selected set of markers for identification of Polish cochineal has been demonstrated in the examination of textiles from the collection of the National Museum in Warsaw using the multiple reaction monitoring (MRM) method, originally elaborated on the basis of this study.

  8. Microfluidic chip for stacking, separation and extraction of multiple DNA fragments.

    Science.gov (United States)

    Wu, Ruige; Seah, Y P; Wang, Zhiping

    2016-03-11

    A disposable integrated microfluidic device was developed for rapid sample stacking, separation and extraction of multiple DNA fragments from a relatively large amount of sample. Isotachophoresis hyphenated gel electrophoresis (ITP-GE) was used to pre-concentrate and separate DNA fragments, followed by extraction of pure DNA fragments with electroelution on-chip. DNA fragments of 200bp, 500bp and 1kbp were successfully separated and collected in the extraction chamber within 25min. The extraction efficiency obtained from the chip was 49.9%, 52.1% and 53.7% for 200bp, 500bp and 1kbp DNA fragments, respectively. The extracted DNA fragments exhibited compatibility with downstream enzymatic reactions, for example PCR. The chip was also used to extract DNA fragments with specific size range from sheared genomic DNA and demonstrated similar performance to that using traditional gel cutting method. The whole assay can finish in 32min, 6 times faster than traditional method. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Application of Chromatographic and Electrophoretic Methods for the Analysis of Imidazolium and Pyridinium Cations as Used in Ionic Liquids

    Directory of Open Access Journals (Sweden)

    P. Stepnowski

    2006-11-01

    Full Text Available Interest in ionic liquids for their potential in different chemical processes isconstantly increasing, as they are claimed to be environmentally benign – excellent, non-volatile solvents for a wide range of applications. The wide applicability of thesecompounds also demands reliable, relatively simple and reproducible analytical techniques.These methods must be applicable not only to different technical or natural matrices but alsoto the very low concentrations that are likely to be present in biological and environmentalsystems. In this review, therefore, methods for separating and analysing imidazolium- andpyridinium-type ionic liquids in aqueous matrices using high performance liquidchromatography (HPLC and capillary electrophoresis (CE are examined. The techniquesfor identifying ionic liquids are meant primarily to track the concentrations of ionic liquidsas residues not only in products and wastes but also in biological or environmental samples.The application of hyphenated techniques in this field is intended to selectively separate thequaternary entity from other cationic and non-ionic species present in the matrix, and toenable its fine-scale quantification. Nowadays, methods developed for cation analysis arebased mostly on reversed-phase high-performance liquid chromatography, ionchromatography, ion-pair chromatography and capillary electrophoresis, where variousbuffered mobile phases are used.

  10. Determination of atractylon in rat plasma by a GC–MS method and its application to a pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Han Yan

    2015-10-01

    Full Text Available A sensitive and selective method based on gas chromatography hyphenated to mass spectrometry (GC–MS was developed and validated for the determination of atractylon in rat plasma. Plasma samples were processed by liquid–liquid extraction with ethyl acetate-n-hexane (1:1, v/v using acetophenone as an internal standard (IS. Analytes were determined in selective ion monitoring (SIM mode using target ions at m/z 108.1 for atractylon and m/z 105.1 for acetophenone. The calibration curve was linear over the concentration range of 10–1000 ng/mL with lower limit of quantification of 10 ng/mL. The intra- and inter-day precision variations were not more than 10.4% and 9.6%, respectively, whilst accuracy values ranged from −6.5% to 4.9%. Extraction recovery of the assay was satisfactory. This method was successfully applied to quantification and pharmacokinetic study of atractylon in rat plasma after intragastric administration of Atractylodis extract. Keywords: Atractylon, Atractylodis, Rat plasma, Pharmacokinetics, GC–MS

  11. Analytical performances of Hemoclot Protein C Reagent on ACL TOP analyzer.

    Science.gov (United States)

    Calmette, Leyla; Charpentier, Nicole; Tircot, Caroline; Bigot, Delphine; Dunois, Claire; Amiral, Jean; Tetegan, Marcelle; Sep Hieng, Sonnthida; Peltier, Jean-Yves

    2016-12-01

    Our study aimed to evaluate and validate according to standard NF EN ISO 15189 the original protocol ajustement of Hemoclot Protein C (PC) (Hyphen BioMed), clotting-based assay of PC on ACL TOP analyzer (Werfen/Instrumentation Laboratory). We evaluated the performance in terms of imprecision and we validate additional parameters in range B required by the SH GTA 04 (COFRAC): repeatability, reproducibility, detection and quantification limits, limits of linearity, stability, inter-samples and inter-reagents contamination, inaccuracy, evaluation of interferences (hemolysis, bilirubinemia and chyles). A comparison with Hemoclot PC on STA Compact analyzer (Stago) was performed. Coefficients of variation were lower than 5 %. Detection and quantification limits were respectively 8.3 % and 9.3 %. Superior limit of linearity was 140 %. The test didn't diplay any inter-samples and inter-reagents contamination. Reagent after reconstitution was stable 6 hours on ACL TOP. No interferences were observed for hemoglobin lower than 500 mg/dL, for bilirubin lower than and for chyles lower than 300 mg/dL. Comparison with Hemoclot PC on STA analyzer (Stago) was satisfactory. Hemoclot PC adjusted on ACL TOP analyzer showed satisfactory analytical performances with criteria chosen in our study. These data allow a better knowledge of the performances of this test and were useful to make a validation file in range B as recommended by SH GTA 04.

  12. A new combined method of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in rat brain microdialysates by ultra high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Zheng, Longfang; Zhao, Xian-En; Zhu, Shuyun; Tao, Yanduo; Ji, Wenhua; Geng, Yanling; Wang, Xiao; Chen, Guang; You, Jinmao

    2017-06-01

    In this work, for the first time, a new hyphenated technique of stable isotope-labeling derivatization-ultrasound-assisted dispersive liquid-liquid microextraction has been developed for the simultaneous determination of monoamine neurotransmitters (MANTs) and their biosynthesis precursors and metabolites. The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry detection using multiple-reaction monitoring mode. A pair of mass spectrometry sensitizing reagents, d 0 -10-methyl-acridone-2-sulfonyl chloride and d 3 -10-methyl-acridone-2-sulfonyl chloride, as stable isotope probes was utilized to facilely label neurotransmitters, respectively. The heavy labeled MANTs standards were prepared and used as internal standards for quantification to minimize the matrix effects in mass spectrometry analysis. Low toxic bromobenzene (extractant) and acetonitrile (dispersant) were utilized in microextraction procedure. Under the optimized conditions, good linearity was observed with the limits of detection (S/N>3) and limits of quantification (S/N>10) in the range of 0.002-0.010 and 0.015-0.040nmol/L, respectively. Meanwhile, it also brought acceptable precision (4.2-8.8%, peak area RSDs %) and accuracy (recovery, 96.9-104.1%) results. This method was successfully applied to the simultaneous determination of monoamine neurotransmitters and their biosynthesis precursors and metabolites in rat brain microdialysates of Parkinson's disease and normal rats. This provided a new method for the neurotransmitters related studies in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Correlations between dioxin-like and indicators PCBs: Potential consequences for environmental studies involving fish or sediment

    Energy Technology Data Exchange (ETDEWEB)

    Babut, M., E-mail: marc.babut@cemagref.f [Cemagref, UR BELY, 3bis quai Chauveau - CP 220, F-69336 Lyon (France); Miege, C. [Cemagref, UR QELY, F-69336 Lyon (France); Villeneuve, B. [Cemagref, UR BELY, 3bis quai Chauveau - CP 220, F-69336 Lyon (France); Abarnou, A. [IFREMER Departement Biogeochimie et Ecotoxicologie, Centre de Brest, BP70, F 29280 Plouzane (France); Duchemin, J. [Agence de l' Eau Seine-Normandie, DDD Eau et Sante, 21 rue l' Homme-de-Bois, F-14600 Honfleur (France); Marchand, P. [LABERCA, Ecole Nationale Veterinaire, Atlanpole La Chantrerie - BP 50707, F 44307 Nantes (France); Narbonne, J.F. [LPTC, Bordeaux 1-CNRS, Bat A12, 351 cours de la Liberation, F-33405 Talence (France)

    2009-12-15

    Among the numerous PCB congeners, most of the dioxin-like PCBs (DL-PCBs) need to be characterized by hyphenated techniques. It has been shown in several instances that these congeners are well related to the total PCB content in fish. We examined datasets collected mainly in France, on freshwater and marine fish and sediments. A statistical model linking DL- and indicator PCBs was developed for a dataset composed of freshwater fishes, and proved to predict well DL-PCBs from indicator PCBs in all other fish sets, including marine ones. Type II error rates remained low in almost all fish sets. A similar correlation was observed in sediments. Non-dioxin-like PCBs elicit various adverse effects and represent 95% of the total PCBs. A European guideline for them is needed; the correlation between DL- and indicator PCBs could help develop this standard in the future. - Dioxin-like PCBs in fish and maybe sediments are rather well predicted by indicator PCBs.

  14. Turbulent flow chromatography TFC-tandem mass spectrometry supporting in vitro/vivo studies of NCEs in high throughput fashion.

    Science.gov (United States)

    Verdirame, Maria; Veneziano, Maria; Alfieri, Anna; Di Marco, Annalise; Monteagudo, Edith; Bonelli, Fabio

    2010-03-11

    Turbulent Flow Chromatography (TFC) is a powerful approach for on-line extraction in bioanalytical studies. It improves sensitivity and reduces sample preparation time, two factors that are of primary importance in drug discovery. In this paper the application of the ARIA system to the analytical support of in vivo pharmacokinetics (PK) and in vitro drug metabolism studies is described, with an emphasis in high throughput optimization. For PK studies, a comparison between acetonitrile plasma protein precipitation (APPP) and TFC was carried out. Our optimized TFC methodology gave better S/N ratios and lower limit of quantification (LOQ) than conventional procedures. A robust and high throughput analytical method to support hepatocyte metabolic stability screening of new chemical entities was developed by hyphenation of TFC with mass spectrometry. An in-loop dilution injection procedure was implemented to overcome one of the main issues when using TFC, that is the early elution of hydrophilic compounds that renders low recoveries. A comparison between off-line solid phase extraction (SPE) and TFC was also carried out, and recovery, sensitivity (LOQ), matrix effect and robustness were evaluated. The use of two parallel columns in the configuration of the system provided a further increase of the throughput. Copyright 2009 Elsevier B.V. All rights reserved.

  15. Isolation of α-Amylase Inhibitors from Kadsura longipedunculata Using a High-Speed Counter-Current Chromatography Target Guided by Centrifugal Ultrafiltration with LC-MS

    Directory of Open Access Journals (Sweden)

    Yin Cen

    2016-09-01

    Full Text Available In this study, a high-speed counter-current chromatography (HSCCC separation method target guided by centrifugal ultrafiltration with high-performance liquid chromatography-mass spectrometry (CU-LC-MS was proposed. This method was used to analyze α-amylase inhibitors from Kadsura longipedunculata extract. According to previous screening with CU-LC-MS, two screened potential α-amylase inhibitors was successfully isolated from Kadsura longipedunculata extract using HSCCC under the optimized experimental conditions. The isolated two target compounds (with purities of 92.3% and 94.6% were, respectively, identified as quercetin-3-O-rhamnoside (1 and protocatechuic acid (2 based on the MS, UV, and 1H-NMR spectrometry data. To verify the inhibition of screened compounds, the inhibitory activities of quercetin-3-O-rhamnoside (1 and protocatechuic acid (2 on α-amylase were tested, and it demonstrated that the experimental IC50 values of quercetin-3-O-rhamnoside (1 and protocatechuic acid (2 were 28.8 and 12.5 μmol/L. These results proved that the hyphenated technique using CU-LC-MS and HSCCC was a rapid, competent, and reproductive method to screen and separate potential active compounds, like enzyme inhibitors from the extract of herbal medicines.

  16. Isolation of α-Amylase Inhibitors from Kadsura longipedunculata Using a High-Speed Counter-Current Chromatography Target Guided by Centrifugal Ultrafiltration with LC-MS.

    Science.gov (United States)

    Cen, Yin; Xiao, Aiping; Chen, Xiaoqing; Liu, Liangliang

    2016-09-07

    In this study, a high-speed counter-current chromatography (HSCCC) separation method target guided by centrifugal ultrafiltration with high-performance liquid chromatography-mass spectrometry (CU-LC-MS) was proposed. This method was used to analyze α-amylase inhibitors from Kadsura longipedunculata extract. According to previous screening with CU-LC-MS, two screened potential α-amylase inhibitors was successfully isolated from Kadsura longipedunculata extract using HSCCC under the optimized experimental conditions. The isolated two target compounds (with purities of 92.3% and 94.6%) were, respectively, identified as quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) based on the MS, UV, and ¹H-NMR spectrometry data. To verify the inhibition of screened compounds, the inhibitory activities of quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) on α-amylase were tested, and it demonstrated that the experimental IC50 values of quercetin-3-O-rhamnoside (1) and protocatechuic acid (2) were 28.8 and 12.5 μmol/L. These results proved that the hyphenated technique using CU-LC-MS and HSCCC was a rapid, competent, and reproductive method to screen and separate potential active compounds, like enzyme inhibitors from the extract of herbal medicines.

  17. Current and Future Perspectives on the Structural Identification of Small Molecules in Biological Systems

    Directory of Open Access Journals (Sweden)

    Daniel A. Dias

    2016-12-01

    Full Text Available Although significant advances have been made in recent years, the structural elucidation of small molecules continues to remain a challenging issue for metabolite profiling. Many metabolomic studies feature unknown compounds; sometimes even in the list of features identified as “statistically significant” in the study. Such metabolic “dark matter” means that much of the potential information collected by metabolomics studies is lost. Accurate structure elucidation allows researchers to identify these compounds. This in turn, facilitates downstream metabolite pathway analysis, and a better understanding of the underlying biology of the system under investigation. This review covers a range of methods for the structural elucidation of individual compounds, including those based on gas and liquid chromatography hyphenated to mass spectrometry, single and multi-dimensional nuclear magnetic resonance spectroscopy, and high-resolution mass spectrometry and includes discussion of data standardization. Future perspectives in structure elucidation are also discussed; with a focus on the potential development of instruments and techniques, in both nuclear magnetic resonance spectroscopy and mass spectrometry that, may help solve some of the current issues that are hampering the complete identification of metabolite structure and function.

  18. Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

    International Nuclear Information System (INIS)

    Luca, Michele De; Ragno, Gaetano; Ioele, Giuseppina; Tauler, Romà

    2014-01-01

    Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described

  19. In-time and in-space tandem mass spectrometry to determine the metabolic profiling of flavonoids in a typical sweet cherry (Prunus avium L.) cultivar from Southern Italy.

    Science.gov (United States)

    Crupi, Pasquale; Genghi, Rosalinda; Antonacci, Donato

    2014-10-01

    This paper presents a comprehensive analytical methodology, based on 'in-time' and 'in-space' tandem mass spectrometry (MS) techniques, to identify and quantify flavonoid compounds in a typical Italian sweet cherry cultivar (cv. Ferrovia). Five anthocyanins, four flavan-3-ols and nine flavonols were determined by means of hyphenated high-performance liquid chromatography - multi-stage MS (HPLC-MS(n)) analyses (MS(n) up to MS(4)), among which quercetin-3-O-rutinoside-7-O-glucoside, kaempferol-3-O-rutinoside-7-O-glucoside, quercetin-3-O-galactosyl-rhamnoside and quercetin-3-O-coumaroylglucoside were tentatively identified in sweet cherries for the first time. Ultrafast HPLC and tandem MS (UHPLC-MS/MS) analyses through multiple reaction monitoring experiments showed that cyanidin-3-O-rutinoside and cyanidin-3-O-glucoside were the main anthocyanins of cv. Ferrovia at maturity. Moreover, consistent levels of catechin and epicatechin as well as quercetin-3-O-rutinoside and kaempferol-3-O-rutinoside were also found. Because flavonoids have been ascribed as potential health-promoting compounds, gathered findings provide new insight into the knowledge of the quali-quantitative profile of these phytochemicals into a widespread fruit such as sweet cherry. Copyright © 2014 John Wiley & Sons, Ltd.

  20. Chemical characterisation of Hoodia gordonii extract.

    Science.gov (United States)

    Russell, P J; Swindells, C

    2012-01-01

    The chemical composition of a solvent extract of Hoodia gordonii termed 'H.gordonii extract' has been characterised by hyphenated chromatographic methods and traditional analytical techniques. The extract consists of a mixture of steroid glycosides, fatty acids, plant sterols and polar organic material. High performance liquid chromatography (HPLC) with ultra violet (UV) and mass spectrometric (MS) detection was used to quantify and confirm the identity of a number of steroid glycosides (73.7% w/w) present in the extract. Gas chromatography (GC) with MS and flame ionisation detection (FID) was applied to determine the fatty acid (3.12% w/w) sterol (0.39% w/w) and alcohol (0.03% w/w) content of a saponified sample of the extract. Polar organic material was quantified by gravimetric methodology using C(18) SPE separation and was determined to be a minimum of 3% w/w. Moisture content was measured by Karl Fischer coulometric titration (0.81% w/w). The protein content was investigated by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE) with SYPRO Ruby staining and a negative result was determined with a limit of detection of <0.001%w/w of protein per band. The chemical composition of the extract remained stable for 19 months when stored in re-sealable plastic bags at ambient (21-24°C) temperature and <60% relative humidity. Copyright © 2011 Elsevier Ltd. All rights reserved.

  1. The use of laser-induced fluorescence or ultraviolet detectors for sensitive and selective analysis of tobramycin or erythropoietin in complex samples

    Science.gov (United States)

    Ahmed, Hytham M.; Ebeid, Wael B.

    2015-05-01

    Complex samples analysis is a challenge in pharmaceutical and biopharmaceutical analysis. In this work, tobramycin (TOB) analysis in human urine samples and recombinant human erythropoietin (rhEPO) analysis in the presence of similar protein were selected as representative examples of such samples analysis. Assays of TOB in urine samples are difficult because of poor detectability. Therefore laser induced fluorescence detector (LIF) was combined with a separation technique, micellar electrokinetic chromatography (MEKC), to determine TOB through derivatization with fluorescein isothiocyanate (FITC). Borate was used as background electrolyte (BGE) with negative-charged mixed micelles as additive. The method was successively applied to urine samples. The LOD and LOQ for Tobramycin in urine were 90 and 200 ng/ml respectively and recovery was >98% (n = 5). All urine samples were analyzed by direct injection without sample pre-treatment. Another use of hyphenated analytical technique, capillary zone electrophoresis (CZE) connected to ultraviolet (UV) detector was also used for sensitive analysis of rhEPO at low levels (2000 IU) in the presence of large amount of human serum albumin (HSA). Analysis of rhEPO was achieved by the use of the electrokinetic injection (EI) with discontinuous buffers. Phosphate buffer was used as BGE with metal ions as additive. The proposed method can be used for the estimation of large number of quality control rhEPO samples in a short period.

  2. Biogenic nanoparticles bearing antibacterial activity and their synergistic effect with broad spectrum antibiotics: Emerging strategy to combat drug

    Directory of Open Access Journals (Sweden)

    Syed Baker

    2017-01-01

    Full Text Available The present study emphasizes on synthesis of bimetallic silver–gold nanoparticles from cell free supernatant of Pseudomonas veronii strain AS41G inhabiting Annona squamosa L. The synthesized nanoparticles were characterized using hyphenated techniques with UV–Visible spectra ascertained absorbance peak between 400 and 800 nm. Possible interaction of biomolecules in mediating and stabilization of nanoparticles was depicted with Fourier transform infrared spectroscopy (FTIR. X-ray diffraction (XRD displayed Bragg’s peak conferring the 100, 111, 200, and 220 facets of the face centered cubic symmetry of nanoparticles suggesting that these nanoparticles were crystalline in nature. Size and shape of the nanoparticles were determined using Transmission electron microscopy (TEM microgram with size ranging from 5 to 50 nm forming myriad shapes. Antibacterial activity of nanoparticles against significant human pathogens was conferred with well diffusion assay and its synergistic effect with standard antibiotics revealed 87.5% fold increased activity with antibiotic “bacitracin” against bacitracin resistant strains Bacillus subtilis, Escherichia coli and Klebsiella pneumoniae followed by kanamycin with 18.5%, gentamicin with 11.15%, streptomycin with 10%, erythromycin with 9.7% and chloramphenicol with 9.4%. Thus the study concludes with biogenic and ecofriendly route for synthesizing nanoparticles with antibacterial activity against drug resistant pathogens and attributes growing interest on endophytes as an emerging source for synthesis of nanoparticles.

  3. Determination of gaseous compounds using online mass spectrometry

    International Nuclear Information System (INIS)

    Praun, S.

    1999-08-01

    The work is divided in three major parts and describes various measurements of gaseous compounds. The first part tasks the problem of transit traffic along the motorway from Kufstein, Northern Tyrol/Austria until Ala, Trentino/Italy. During three periods measurements of the immissions of many compounds were carried out simultaneously in Northern Tyrol, Southern Tyrol and Trentino. The influence of the ban of heavy lorry traffic during the weekend and during the night on the reduction of NO 2 could be demonstrated. Furthermore certain compounds (e.g. Benzene) were monitored online for the first time along the motorway at lowest concentrations using the mass spectrometer 'Airsense 500'. In the second part online measurements of exhaled human breath after the oral application of a medicine against bronchitis was performed. In that way beside clinical and pharmacological studies the effectiveness of this pharmacon could be proved. The last part of the present work shows adsorption- and desorption measurements on four different adsorbents. During this procedure seven different gases with an increasing number of carbon atoms were monitored online by the hyphenation of these adsorbents with the mass spectrometer 'Airsense 500'. Thereby, the various properties of the adsorbents in the interaction with the gases could be demonstrated. (author)

  4. Biomimetic Synthesis of Silver Nanoparticles Using Endosymbiotic Bacterium Inhabiting Euphorbia hirta L. and Their Bactericidal Potential

    Directory of Open Access Journals (Sweden)

    Baker Syed

    2016-01-01

    Full Text Available The present investigation aims to evaluate biomimetic synthesis of silver nanoparticles using endophytic bacterium EH 419 inhabiting Euphorbia hirta L. The synthesized nanoparticles were initially confirmed with change in color from the reaction mixture to brown indicating the synthesis of nanoparticles. Further confirmation was achieved with the characteristic absorption peak at 440 nm using UV-Visible spectroscopy. The synthesized silver nanoparticles were subjected to biophysical characterization using hyphenated techniques. The possible role of biomolecules in mediating the synthesis was depicted with FTIR analysis. Further crystalline nature of synthesized nanoparticles was confirmed using X-ray diffraction (XRD with prominent diffraction peaks at 2θ which can be indexed to the (111, (200, (220, and (311 reflections of face centered cubic structure (fcc of metallic silver. Transmission electron microscopy (TEM revealed morphological characteristics of synthesized silver nanoparticles to be polydisperse in nature with size ranging from 10 to 60 nm and different morphological characteristics such as spherical, oval, hexagonal, and cubic shapes. Further silver nanoparticles exhibited bactericidal activity against panel of significant pathogenic bacteria among which Pseudomonas aeruginosa was most sensitive compared to other pathogens. To the best of our knowledge, present study forms first report of bacterial endophyte inhabiting Euphorbia hirta L. in mediating synthesizing silver nanoparticles.

  5. Biomimetic Synthesis of Silver Nanoparticles Using Endosymbiotic Bacterium Inhabiting Euphorbia hirta L. and Their Bactericidal Potential.

    Science.gov (United States)

    Syed, Baker; Yashavantha Rao, Hoovinakola Chinnappa; Nagendra-Prasad, Mysore Nagalingaswamy; Prasad, Ashwini; Harini, Ballagere Puttaraju; Azmath, Pasha; Rakshith, Devaraju; Satish, Sreedharamurthy

    2016-01-01

    The present investigation aims to evaluate biomimetic synthesis of silver nanoparticles using endophytic bacterium EH 419 inhabiting Euphorbia hirta L. The synthesized nanoparticles were initially confirmed with change in color from the reaction mixture to brown indicating the synthesis of nanoparticles. Further confirmation was achieved with the characteristic absorption peak at 440 nm using UV-Visible spectroscopy. The synthesized silver nanoparticles were subjected to biophysical characterization using hyphenated techniques. The possible role of biomolecules in mediating the synthesis was depicted with FTIR analysis. Further crystalline nature of synthesized nanoparticles was confirmed using X-ray diffraction (XRD) with prominent diffraction peaks at 2θ which can be indexed to the (111), (200), (220), and (311) reflections of face centered cubic structure (fcc) of metallic silver. Transmission electron microscopy (TEM) revealed morphological characteristics of synthesized silver nanoparticles to be polydisperse in nature with size ranging from 10 to 60 nm and different morphological characteristics such as spherical, oval, hexagonal, and cubic shapes. Further silver nanoparticles exhibited bactericidal activity against panel of significant pathogenic bacteria among which Pseudomonas aeruginosa was most sensitive compared to other pathogens. To the best of our knowledge, present study forms first report of bacterial endophyte inhabiting Euphorbia hirta L. in mediating synthesizing silver nanoparticles.

  6. HPTLC-aptastaining - Innovative protein detection system for high-performance thin-layer chromatography

    Science.gov (United States)

    Morschheuser, Lena; Wessels, Hauke; Pille, Christina; Fischer, Judith; Hünniger, Tim; Fischer, Markus; Paschke-Kratzin, Angelika; Rohn, Sascha

    2016-05-01

    Protein analysis using high-performance thin-layer chromatography (HPTLC) is not commonly used but can complement traditional electrophoretic and mass spectrometric approaches in a unique way. Due to various detection protocols and possibilities for hyphenation, HPTLC protein analysis is a promising alternative for e.g., investigating posttranslational modifications. This study exemplarily focused on the investigation of lysozyme, an enzyme which is occurring in eggs and technologically added to foods and beverages such as wine. The detection of lysozyme is mandatory, as it might trigger allergenic reactions in sensitive individuals. To underline the advantages of HPTLC in protein analysis, the development of innovative, highly specific staining protocols leads to improved sensitivity for protein detection on HPTLC plates in comparison to universal protein derivatization reagents. This study aimed at developing a detection methodology for HPTLC separated proteins using aptamers. Due to their affinity and specificity towards a wide range of targets, an aptamer based staining procedure on HPTLC (HPTLC-aptastaining) will enable manifold analytical possibilities. Besides the proof of its applicability for the very first time, (i) aptamer-based staining of proteins is applicable on different stationary phase materials and (ii) furthermore, it can be used as an approach for a semi-quantitative estimation of protein concentrations.

  7. UHPLC-MS/MS based target profiling of stress-induced phytohormones.

    Science.gov (United States)

    Floková, Kristýna; Tarkowská, Danuše; Miersch, Otto; Strnad, Miroslav; Wasternack, Claus; Novák, Ondřej

    2014-09-01

    Stress-induced changes in phytohormone metabolite profiles have rapid effects on plant metabolic activity and growth. The jasmonates (JAs) are a group of fatty acid-derived stress response regulators with roles in numerous developmental processes. To elucidate their dual regulatory effects, which overlap with those of other important defence-signalling plant hormones such as salicylic acid (SA), abscisic acid (ABA) and indole-3-acetic acid (IAA), we have developed a highly efficient single-step clean-up procedure for their enrichment from complex plant matrices that enables their sensitive quantitative analysis using hyphenated mass spectrometry technique. The rapid extraction of minute quantities of plant material (less than 20mg fresh weight, FW) into cold 10% methanol followed by one-step reversed-phase polymer-based solid phase extraction significantly reduced matrix effects and increased the recovery of labile JA analytes. This extraction and purification protocol was paired with a highly sensitive and validated ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method and used to simultaneously profile sixteen stress-induced phytohormones in minute plant material samples, including endogenous JA, several of its biosynthetic precursors and derivatives, as well as SA, ABA and IAA. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Development of a comprehensive two-dimensional hydrophilic interaction chromatography/quadrupole time-of-flight mass spectrometry system and its application in separation and identification of saponins from Quillaja saponaria.

    Science.gov (United States)

    Wang, Yuan; Lu, Xin; Xu, Guowang

    2008-02-15

    Hydrophilic interaction chromatography (HILIC) was used in two dimensions in a comprehensive two-dimensional HILIC hyphenated with a quadrupole time-of-flight mass spectrometry (HILICxHILIC-Q-TOF-MS) system for the analysis of complex samples of hydrophilic compounds. A TSKgel Amide-80 column was employed as the first dimension, and a short PolyHydroxyethyl A column was as the second dimension. The column system showed moderate orthogonality at defined operational conditions. A high speed Q-TOF-MS detector as a third complementary dimension significantly improved the peak capacity. The separation capability of the developed HILICxHILIC-Q-TOF-MS system was tested by separating an extract from Quillaja saponaria. The major components, quillaja saponins, in the extract were well identified by means of [M-H](-) ions, characteristic product ions, and their two-dimensional retention behaviors. Several pairs of isomers, which were often co-eluted on conventional LC-MS methods and had similar fragmentation characteristics in MS/MS spectra, were well separated on the two-dimensional system based on their different hydrophilicity. The developed comprehensive two-dimensional HILIC system demonstrates unique selectivity for hydrophilic compounds and satisfactory peak capacity and resolution for analogues by making sufficient use of two-dimensional separation plane.

  9. On the frontiers of knowledge: the enlargement of experience and the new forms of rationality doi:10.5007/1807-1384.2010v7n2p1

    Directory of Open Access Journals (Sweden)

    Ivan Domingues

    2010-12-01

    Full Text Available The article discusses the panorama of knowledge today, focusing on the inflation of knowledge, the fragmentation of disciplines and the density loss of cognitive processes as well as the search for alternatives through multi-, inter- and transdisciplinary experiments. Other points emphasized: the emergence of the hyphenated disciplines (bio-chemistry, ethno-music, etc.; the approach of science, technology, art and philosophy; the end of the generalist and the specialist. The sense of the analyses is epistemological and the goal is to demonstrate, in contrast, two real approaches that define cognitive strategies in different fields of knowledge: the reductionist and the non-reductionist. The stress falls on the non-reductionist approaches, highlighting the following topics or aspects: the dilatation of the experience and the expansion of reason, the conquest of different levels of reality, new perspectives for the humanities and social sciences. Finally, after emphasizing the importance of discipline, its centrality anchor is placed in context, through the recognition of themes and issues as important challenges and opportunities acquis, enabling the advancement of knowledge.

  10. Identification of marker compounds in herbal drugs on TLC with DART-MS.

    Science.gov (United States)

    Kim, Hye Jin; Jee, Eun Hye; Ahn, Kwang Sung; Choi, Hyo Sook; Jang, Young Pyo

    2010-09-01

    This study was conducted to provide a more versatile and specific information on Thin Layer Chromatographic (TLC) analysis of medicinal plants. TLC plates developed with the extract of herbal medicines were analyzed with direct analysis in real time (DART) ion source. Three well known herbal drugs were extracted and developed on a silica-coated TLC plate with the conditions pre-established in Korean Pharmacopoeia IX. The developed plate was placed between the DART ion source and TOF-MS analyzer to get real time mass spectra from the bands on the TLC plate directly. The marker coumarin compounds, decursin and decursinol were successfully identified from the TLC plate developed with Angelicae gigantis radix, along with alkaloid compounds of rutaecarpine and evodiamine from Evodiae fructus, and lignan molecules of gomisin A, N, and schisandrin from Schisandrae fructus. This hyphenation system of TLC and DART-MS could provide unique and specific information on the major constituents of crude plant drug on TLC through uncovering high resolution mass number of each band on the TLC plate directly in real time.

  11. Proceedings of the DAE-BRNS theme meeting on ion chromatography separations - state of art and perspectives

    International Nuclear Information System (INIS)

    Jeyakumar, S.; Ramakumar, K.L.

    2012-01-01

    Ion Chromatography (IC) plays a vital role in all disciplines of science and technology. In the field of trace separations and speciation studies, use of IC techniques becomes indispensable. In nuclear technology, IC plays a pivotal role in the reactor water chemistry, in the front end of fuel cycle especially in the characterization of nuclear materials including the reactor fuels, post irradiation examination, actinide speciation studies and in understanding the interaction and migration of actinide species in the geo environment. Ion chromatography is also useful in the studies related to waste management particularly for the separation and determination of fission products. The aim of this meeting is to provide a forum to all the researchers in the area of ion chromatography to discuss their recent findings and information, to learn from the mutual experiences and interests, and to promote cooperation both nationally and internationally. Ion chromatography techniques including Ion Chromatography Separations and Nuclear Materials, Speciation Studies by Ion chromatography, Hyphenated -IC Techniques, Reactor Water Chemistry and Ion Chromatography, Solid Phase Extraction and Sample Preparations for IC and Separation of Bio-molecules and Environmental aspects etc are discussed. Papers relevant to INIS are indexed separately

  12. Intermethod comparison of the particle size distributions of colloidal silica nanoparticles.

    Science.gov (United States)

    Tuoriniemi, Jani; Johnsson, Ann-Cathrin J H; Holmberg, Jenny Perez; Gustafsson, Stefan; Gallego-Urrea, Julián A; Olsson, Eva; Pettersson, Jan B C; Hassellöv, Martin

    2014-06-01

    There can be a large variation in the measured diameter of nanoparticles depending on which method is used. In this work, we have strived to accurately determine the mean particle diameter of 30-40 nm colloidal silica particles by using six different techniques. A quantitative agreement between the particle size distributions was obtained by scanning electron microscopy (SEM), and electrospray-scanning mobility particle sizer (ES-SMPS). However, transmission electron microscopy gave a distribution shifted to smaller sizes. After confirming that the magnification calibration was consistent, this was attributed to sample preparation artifacts. The hydrodynamic diameter, d h , was determined by dynamic light scattering (DLS) both in batch mode, and hyphenated with sedimentation field flow fractionation. Surprisingly the d h were smaller than the SEM, and ES-SMPS diameters. A plausible explanation for the smaller sizes found with DLS is that a permeable gel layer forms on the particle surface. Results from nanoparticle tracking analysis were strongly biased towards larger diameters, most likely because the silica particles provide low refractive index contrast. Calculations confirmed that the sensitivity is, depending on the shape of the laser beam, strongly size dependent for particles with diameters close to the visualization limit.

  13. Analysis of sugar degradation products with α-dicarbonyl structure in carbonated soft drinks by UHPLC-DAD-MS/MS.

    Science.gov (United States)

    Gensberger, Sabrina; Glomb, Marcus A; Pischetsrieder, Monika

    2013-10-30

    Sugar-sweetened carbonated soft drinks (CSDs) are broadly consumed worldwide. The added sugar, particularly high-fructose corn syrup (HFCS), can be an important source of sugar degradation products, such as α-dicarbonyl compounds. This study recorded the α-dicarbonyl profile in CSDs by ultrahigh-performance liquid chromatography with hyphenated diode array-tandem mass spectrometry after derivatization with o-phenylenediamine. Thus, 3-deoxy-D-erythro-hexos-2-ulose (3-DG), D-lyxo-hexos-2-ulose (glucosone), 3-deoxy-D-threo-hexos-2-ulose (3-DGal), 1-deoxy-D-erythro-hexos-2,3-diulose (1-DG), 3,4-dideoxyglucosone-3-ene (3,4-DGE), methylglyoxal, and glyoxal were identified as major α-dicarbonyls and, with the exception of glyoxal, quantified (recovery rates, 85.6-103.1%; RSD, 0.8-3.6%). Total α-dicarbonyl concentration in 25 tested commercial products ranged between 0.3 and 116 μg/mL and was significantly higher in HFCS-sweetened CSDs compared to CSDs sweetened with HFCS and sucrose or with sucrose alone. Predominant was 3-DG (≤87 μg/mL) followed by glucosone (≤21 μg/mL), 3-DGal (≤7.7 μg/mL), 1-DG (≤2.8 μg/mL), methylglyoxal (≤0.62 μg/mL), and 3,4-DGE (≤0.45 μg/mL).

  14. Recent trends in the impurity profile of pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Kavita Pilaniya

    2010-01-01

    Full Text Available Various regulatory authorities such as the International Conference on Harmonization (ICH, the United States Food and Drug administration (FDA, and the Canadian Drug and Health Agency (CDHA are emphasizing on the purity requirements and the identification of impurities in Active Pharmaceutical Ingredients (APIs. The various sources of impurity in pharmaceutical products are - reagents, heavy metals, ligands, catalysts, other materials like filter aids, charcoal, and the like, degraded end products obtained during \\ after manufacturing of bulk drugs from hydrolysis, photolytic cleavage, oxidative degradation, decarboxylation, enantiomeric impurity, and so on. The different pharmacopoeias such as the British Pharmacopoeia, United State Pharmacopoeia, and Indian Pharmacopoeia are slowly incorporating limits to allowable levels of impurities present in APIs or formulations. Various methods are used to isolate and characterize impurities in pharmaceuticals, such as, capillary electrophoresis, electron paramagnetic resonance, gas-liquid chromatography, gravimetric analysis, high performance liquid chromatography, solid-phase extraction methods, liquid-liquid extraction method, Ultraviolet Spectrometry, infrared spectroscopy, supercritical fluid extraction column chromatography, mass spectrometry, Nuclear magnetic resonance (NMR spectroscopy, and RAMAN spectroscopy. Among all hyphenated techniques, the most exploited techniques for impurity profiling of drugs are Liquid Chromatography (LC-Mass Spectroscopy (MS, LC-NMR, LC-NMR-MS, GC-MS, and LC-MS. This reveals the need and scope of impurity profiling of drugs in pharmaceutical research.

  15. Metabolomic Analysis of Two Parmotrema Lichens: P. robustum (Degel. Hale and P. andinum (Mull. Arg. Hale Using UHPLC-ESI-OT-MS-MS

    Directory of Open Access Journals (Sweden)

    Alfredo Torres-Benítez

    2017-10-01

    Full Text Available Lichens are symbiotic associations of fungi with microalgae and/or cyanobacteria. Lichens belonging to the Parmeliaceae family comprise 2700 species of lichens, including the Parmotrema genus which is composed of 300 species. The metabolites of this genus include depsides, depsidones, phenolics, polysaccharides, lipids, diphenylethers and dibenzofurans, which are responsible for the biological activities reported including antidiabetic, antihelmintic, anticancer, antioxidant, antibacterial, anti-inflammatory, antimitotic, antitumoral, antifungal, and antioxidant enzyme inhibitory. Due to scarce knowledge of metabolomic profiles of Parmotrema species (P. andinum and P. robustum, a full metabolome study based on ultra-high performance liquid chromatography- diode array detector-electrospray ionization-quadrupole-orbitrap-mass-spectrometry (UHPLC-DAD-ESI-Q-orbitrap MS was performed for a comprehensive characterization of their substances. From the methanolic extracts of these species, a total of 54 metabolites were identified for the first time using this hyphenated technique, including thirty compounds in P. andinum, and thirty-seven in P. robustum. Moreover, two compounds were not identified as known compounds, and could be new structures, according to our data. This report shows that this technique is effective and accurate for rapid chemical identification of lichen substances and the compounds identified could serve as chemotaxonomic markers to differentiate these ruffle lichens.

  16. Applications of HPLC/MS in the analysis of traditional Chinese medicines

    Science.gov (United States)

    Li, Miao; Hou, Xiao-Fang; Zhang, Jie; Wang, Si-Cen; Fu, Qiang; He, Lang-Chong

    2012-01-01

    In China, traditional Chinese medicines (TCMs) have been used in clinical applications for thousands of years. The successful hyphenation of high-Performance liquid chromatography (HPLC) and mass spectrometry (MS) has been applied widely in TCMs and biological samples analysis. Undoubtedly, HPLC/MS technique has facilitated the understanding of the treatment mechanism of TCMs. We reviewed more than 350 published papers within the last 5 years on HPLC/MS in the analysis of TCMs. The present review focused on the applications of HPLC/MS in the component analysis, metabolites analysis, and pharmacokinetics of TCMs etc. 50% of the literature is related to the component analysis of TCMs, which show that this field is the most populär type of research. In the metabolites analysis, HPLC coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry has been demonstrated to be the powerful tool for the characterization of structural features and fragmentation behavior patterns. This paper presented a brief overview of the applications of HPLC/MS in the analysis of TCMs. HPLC/MS in the fingerprint analysis is reviewed elsewhere. PMID:29403684

  17. Off-line coupling of new generation centrifugal partition chromatography device with preparative high pressure liquid chromatography-mass spectrometry triggering fraction collection applied to the recovery of secoiridoid glycosides from Centaurium erythraea Rafn. (Gentianaceae).

    Science.gov (United States)

    Mandova, Tsvetelina; Audo, Grégoire; Michel, Sylvie; Grougnet, Raphaël

    2017-09-01

    A purification sequence including a Gilson CPC 250 PRO device coupled to PrepHPLC hyphenated with a MS triggering fraction collector was applied to isolate secoiridoid glycosides from a complex methanolic extract of Centaurium erythraea. This species is widely used for ethnomedicinal purposes around the Mediterranean Sea. The solvent system ethyle acetate/ethanol/water 7.5/3/5 was determined using shake-flask method targeting swertiamarin, the major secoiridoid of the extract. Optimization of CPC experimental parameters enabled the injection of 4g of extract with a flow rate of 40mL/min at 3000rpm to provide a secoiridoid glycosides enriched fraction. 130mg of this latter was submitted to a second step of purification by preparative HPLC (gradient water/formic acid (19:1) (A) and methanol (B) as follows: 0min, 85% A; 8min, 60% A; 12min, 55% A; 35min, 55% A; 40min, 10% A; 50min, 10% A; 52min, 85% A; 55min, 85% A) to give swertiamarin (36mg, yield 27.7%, purity 98.2%). Other secoiridoid glycosides (sweroside, gentiopicroside, secologanol, secoxyloganin) were also isolated in minor amounts. As these monoterpene derivatives are responsible for several biological activities, their quick recovery with high yield and purity may serve as a model for further scale-up and industrial development. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Feasibility study of online supercritical fluid extraction-liquid chromatography-UV absorbance-mass spectrometry for the determination of proanthocyanidins in grape seeds.

    Science.gov (United States)

    Wang, Zhenyu; Ashraf-Khorassani, Mehdi; Taylor, Larry T

    2005-03-01

    Online coupling of supercritical fluid extraction (SFE) with liquid chromatography (LC)-UV absorbance-electrospray ionization (ESI)-mass spectrometry (MS) is evaluated for the determination of proanthocyanidins in grape seeds. The solid-phase intermediate trap is optimized in order to enhance the collection efficiency for the extracted polar components. Pure supercritical CO2 is used first to remove the oil in the seeds. Then methanol-modified CO2 is used to remove the polar components (e.g., phenolic compounds). Catechin and epicatechin (90%) are extracted out of the de-oiled after 240 min with 40% methanol as a modifier. Both singly-linked (B-type) and doubly-linked (A-type) procyanidins are identified by LC-ESI-MS, as well as their galloylated derivatives. The hyphenated system combines the extraction, separation, and detection in series. The experimental design minimizes the chance of analyte oxidation, degradation, and contamination. The traditional off-line SFE-LC method is also studied for comparison with the online method. Both advantages and disadvantages are observed for the online mode.

  19. Headspace-solid phase microextraction approach for dimethylsulphoniopropionate quantification in Solanum lycopersicum plants subjected to water stress

    Directory of Open Access Journals (Sweden)

    Stefano Catola

    2016-08-01

    Full Text Available Dimethylsulphoniopropionate (DMSP and dimethyl sulphide (DMS are compounds found mainly in marine phytoplankton and in some halophytic plants. DMS is a globally important biogenic volatile in regulating of global sulphur cycle and planetary albedo, whereas DMSP is involved in the maintenance of plant-environment homeostasis. Plants emit minute amounts of DMS compared to marine phytoplankton and there is a need for hypersensitive analytic techniques to enable its quantification in plants. Solid Phase Micro Extraction from Head Space (HS-SPME is a simple, rapid, solvent-free and cost-effective extraction mode, which can be easily hyphenated with GC-MS for the analysis of volatile organic compounds (VOCs. Using tomato (Solanum lycopersicum plants subjected to water stress as a model system, we standardized a sensitive and accurate protocol for detecting and quantifying DMSP pool sizes, and potential DMS emissions, in cryoextracted leaves. The method relies on the determination of DMS free and from DMSP pools before and after the alkaline hydrolysis via HS-SPME-GC-MS. We found a significant (2.5 time increase of DMSP content in water-stressed leaves reflecting clear stress to the photosynthetic apparatus. We hypothesize that increased DMSP, and in turn DMS, in water-stressed leaves are produced by carbon sources other than direct photosynthesis, and function to protect plants either osmotically or as antioxidants. Finally, our results suggest that SPME is a powerful and suitable technique for the detection and quantification of biogenic gases in trace amounts.

  20. Phytochemical profile of aerial parts and roots of Wachendorfia thyrsiflora L. studied by LC-DAD-SPE-NMR.

    Science.gov (United States)

    Fang, Jingjing; Kai, Marco; Schneider, Bernd

    2012-09-01

    Hyphenated liquid chromatography - diode array detection - solid phase extraction - nuclear magnetic resonance spectroscopy (LC-DAD-SPE-NMR) was used to investigate the phytochemical composition of aerial parts and roots of Wachendorfia thyrsiflora (Haemodoraceae). Eleven phenylphenalenones and related compounds were identified in the aerial parts of the plant, ten compounds were found in the roots, and four additional compounds occurred in both plant parts. Twelve compounds are previously unreported natural products including five alkaloids (phenylbenzoisoquinolinones) are described here for the first time. In the work presented here, phenylphenalenones with an intact C(19) core structure were found only in the roots. Oxa analogs with a C(18)O scaffold occurred both in the roots and in the aerial plant parts, while most of the aza analogs with a C(18)N scaffold were detected in the aerial plant parts. This distribution pattern suggests that phenylphenalenones form in the roots, then the intact C(19) skeleton is converted into oxa analogs in the roots, translocated into the leaves and further reacted with amines or amino acids to form aza analogs (phenylbenzoisoquinolin-1,6-dione alkaloids). Copyright © 2012 Elsevier Ltd. All rights reserved.

  1. Evidence of different stoichiometries for the limiting carbonate complexes of lanthanides(3)

    International Nuclear Information System (INIS)

    Philippini, V.

    2007-12-01

    Two stoichiometries have been proposed by different laboratories to interpret measurements on the limiting carbonate complexes of An 3+ and Ln 3+ cations. The study of the solubility of double carbonates (AlkLn(CO 3 ) 2 ,xH 2 O) in concentrated carbonate solutions at room temperature and high ionic strengths has shown that on the one hand the lightest lanthanides (La and Nd) form Ln(CO 3 ) 4 5- whereas the heaviest (Eu and Dy) form Ln(CO 3 ) 3 3- in the studied chemical conditions, and on the other hand, that the kinetics of precipitation of double carbonates depends on the alkali metal and the lanthanide ions. The existence of two stoichiometries for the limiting carbonate complexes was confirmed by capillary electrophoresis hyphenated to an inductively coupled plasma mass spectrometer (CE-ICP-MS), used to extend the study to the whole series of lanthanides (except Ce, Pm and Yb). Two behaviours have been put forward comparing the electrophoretic mobilities: La to Tb form Ln(CO 3 ) 4 5- while Dy to Lu form Ln(CO 3 ) 3 3- . Measurements by time resolved laser fluorescence spectroscopy (TRLFS) on Eu(III) indicate small variations of the geometry of Eu(CO 3 ) 3 3- complex, specially with Cs + . Although analogies are currently used among the 4f-block trivalent elements, different aqueous speciations are evidenced in concentrated carbonate solutions across the lanthanide series. (author)

  2. Functional analysis of the cytochrome P450 monooxygenase gene bcbot1 of Botrytis cinerea indicates that botrydial is a strain-specific virulence factor.

    Science.gov (United States)

    Siewers, Verena; Viaud, Muriel; Jimenez-Teja, Daniel; Collado, Isidro G; Gronover, Christian Schulze; Pradier, Jean-Marc; Tudzynski, Bettina; Tudzynski, Paul

    2005-06-01

    The micrographic phytopathogen Botrytis cinerea causes gray mold diseases in a large number of dicotyledonous crop plants and ornamentals. Colonization of host tissue is accompanied by rapid killing of plant cells ahead of the growing hyphen, probably caused by secretion of nonspecific phytotoxins, e.g., the sesquiterpene botrydial. Although all pathogenic strains tested so far had been shown to secrete botrydial and although the toxin causes comparable necrotic lesions as infection by the fungus, the role of botrydial in the infection process has not been elucidated so far. Here, we describe the functional characterization of bcbot1, encoding a P450 monooxygenase and provide evidence that it is involved in the botrydial pathway, i.e., it represents the first botrydial biosynthetic gene identified. We show that bcbot1 is expressed in planta and that expression in vitro and in planta is controlled by an alpha-subunit of a heterotrimeric GTP-binding protein, BCG1. Deletion of bcbot1 in three standard strains of B. cinerea shows that the effect on virulence (on several host plants) is strain-dependent; only deletion in one of the strains (T4) led to reduced virulence.

  3. Speciation of arsenic in rice and estimation of daily intake of different arsenic species by Brazilians through rice consumption.

    Science.gov (United States)

    Batista, Bruno L; Souza, Juliana M O; De Souza, Samuel S; Barbosa, Fernando

    2011-07-15

    Rice is an important source of essential elements. However, rice may also contain toxic elements such as arsenic. Therefore, in the present study, the concentration of total arsenic and five main chemical species of arsenic (As(3+), As(5+), DMA, MMA and AsB) were evaluated in 44 different rice samples (white, parboiled white, brown, parboiled brown, parboiled organic and organic white) from different Brazilian regions using high-performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The mean level of total arsenic was 222.8 ng g(-1) and the daily intake of inorganic arsenic (the most toxic form) from rice consumption was estimated as 10% of the Provisional Tolerable Daily Intake (PTDI) with a daily ingestion of 88 g of rice. Inorganic arsenic (As(3+), As(5+)) and dimethylarsinic acid (DMA) are the predominant forms in all samples. The percentages of species were 38.7; 39.7; 3.7 and 17.8% for DMA, As(3+), MMA and As(5+), respectively. Moreover, rice samples harvested in the state of Rio Grande do Sul presented more fractions of inorganic arsenic than rice in Minas Gerais or Goiás, which could lead to different risks of arsenic exposure. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Analytical methods for the endocrine disruptor compounds determination in environmental water samples.

    Science.gov (United States)

    Locatelli, Marcello; Sciascia, Francesco; Cifelli, Roberta; Malatesta, Luciano; Bruni, Pantaleone; Croce, Fausto

    2016-02-19

    The potential risk of exposure to different xenobiotics, which can modulate the endocrine system and represent a treat for the wellness of an increasing number of people, has recently drawn the attention of international environmental and health agencies. Several agents, characterized by structural diversity, may interfer with the normal endocrine functions that regulate cell growth, homeostasis and development. Substances such as pesticides, herbicides, plasticizers, metals, etc. having endocrine activity (EDCs) are used in agriculture and industry and are also used as drugs for humans and animals. A difficulty in the analytical determination of these substances is the complexity of the matrix in which they are present. In fact, the samples most frequently analyzed consist of groundwater and surface water, including influent and effluent of wastewater treatment plants and drinking water. In this review, several sample pretreatment protocols, assays and different instrumental techniques recently used in the EDCs determination have been considered. This review concludes with a paragraph in which the most recent hyphenated-instrument techniques are treated, highlighting their sensitivity and selectivity for the analyses of environmental water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Biotransformation and Incorporation into Proteins along a Simulated Terrestrial Food Chain

    Energy Technology Data Exchange (ETDEWEB)

    Unrine, J.M., B.P. Jackson and W.A. Hopkins

    2007-01-01

    Selenium is an essential trace element in vertebrates, but there is a narrow concentration range between dietary requirement and toxicity threshold. Although a great deal is known about the biochemistry of Se from a nutritional perspective, considerably less attention has been focused on the specific biochemistry of Se as an environmental toxicant. Recent advances in hyphenated analytical techniques have provided the capability of quantifying specific chemical forms of Se in biological tissues as well as the distribution of Se among macromolecules. We applied liquid chromatography coupled to inductively coupled plasma mass spectrometry to investigate biotransformations of selenomethionine along a simulated terrestrial food chain consisting of selenomethionine exposed crickets (Acheta domesticus) fed to western fence lizards (Sceloporus occidentalis). Evidence was obtained for selenomethionine biotransformation as well as for sex-specific differences in the metabolism of Se compounds and their subsequent incorporation into proteins in the lizard. The results demonstrate the complexities involved in trophic transfer of Se due to the potential for extensive biotransformation and the species- and even sex-specific nature of these biotransformations.

  6. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J.M.; García Alonso, J.I., E-mail: jiga@uniovi.es

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS.

  7. Comprehensive two-dimensional liquid chromatography for polyphenol analysis in foodstuffs.

    Science.gov (United States)

    Cacciola, Francesco; Farnetti, Sara; Dugo, Paola; Marriott, Philip John; Mondello, Luigi

    2017-01-01

    Polyphenols are a class of plant secondary metabolites that are recently drawing a special interest because of their broad spectrum of pharmacological effects. As they are characterized by an enormous structural variability, the identification of these molecules in food samples is a difficult task, and sometimes having only a limited number of commercially available reference materials is not of great help. One-dimensional liquid chromatography is the most widely applied analytical approach for their analysis. In particular, the hyphenation of liquid chromatography to mass spectrometry has come to play an influential role by allowing relatively fast tentative identification and accurate quantification of polyphenolic compounds at trace levels in vegetable media. However, when dealing with very complex real-world food samples, a single separation system often does not provide sufficient resolving power for attaining rewarding results. Comprehensive two-dimensional liquid chromatography is a technique of great analytical impact, since it offers much higher peak capacities than separations in a single dimension. In the present review, we describe applications in the field of comprehensive two-dimensional liquid chromatography for polyphenol analysis in real-world food samples. Comprehensive two-dimensional liquid chromatography applications to nonfood matrices fall outside the scope of the current report and will not be discussed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Environmental impact of flood: the study of arsenic speciation in exchangeable fraction of flood deposits of Warta river (Poland) in determination of "finger prints" of the pollutants origin and the ways of the migration.

    Science.gov (United States)

    Kozak, Lidia; Skolasińska, Katarzyna; Niedzielski, Przemysław

    2012-09-01

    The paper presents the application of the hyphenated technique - high-performance liquid chromatography with atomic absorption spectrometry detection with hydride generation (HPLC-HG-AAS) - in the determinations of inorganic forms of arsenic: As(III) and As(V) in the exchangeable fraction of flood deposits. The separation of analytical signals of the determined arsenic forms was obtained using an ion-exchange column in a chromatographic system with the atomic absorption spectrometer as a detector, at the determination limits of 5 ngg(-1) for As(III) and 10 ngg(-1) for As(V). Flood deposits were collected after big flood event in valley of the Warta river which took place in summer 2010. Samples of overbank deposits were taken in Poznań agglomeration and vicinity (NW Poland). The results of determinations of arsenic forms in the exchangeable fraction of flood deposits allowed indication of a hypothetical path of deposits migration transported by a river during flood and environmental threats posed by their deposition by flood. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. Targeted natural product isolation guided by HPLC-SPE-NMR: constituents of Hubertia species.

    Science.gov (United States)

    Sprogøe, Kennett; Staerk, Dan; Jäger, Anna K; Adsersen, Anne; Hansen, Steen Honoré; Witt, Matthias; Landbo, Anne-Katrine R; Meyer, Anne S; Jaroszewski, Jerzy W

    2007-09-01

    The hyphenated technique, high-performance liquid chromatography-solid-phase extraction-nuclear magnetic resonance spectroscopy (HPLC-SPE-NMR), has been applied for rapid identification of novel natural products in crude extracts of Hubertia ambavilla and Hubertia tomentosa. The technique allowed full or partial identification of all major extract constituents and demonstrated the presence of unusual quinic acid derivatives containing the (1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl residue that exhibit strongly coupled ABXY patterns, the parameters of which were obtained by spin simulations. Using homo- and heteronuclear 2D NMR data acquired in the HPLC-SPE-NMR mode, complete structure determination of three new natural products, i.e., 3,5-di-O-caffeoyl-4-O-[(1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl]quinic acid (1), its 2-hydroxy derivative (2), and 3,5-di-O-caffeoyl-4-O-[(4-hydroxyphenyl)acetyl]quinic acid (3), was performed. Finally, targeted isolation of 1 was achieved by SPE fractionation and preparative HPLC, followed by evaluation of its antioxidant and antimicrobial activity. In contrast to chlorogenic acid and 3,5-di-O-caffeoylquinic acid, which act as antioxidants, compound 1 proved at the same conditions to possess prooxidant activity in an assay evaluating the oxidation of human low-density lipoprotein induced by Cu(2+).

  10. Separation of polypeptides by isoelectric point focusing in electrospray-friendly solution using a multiple-junction capillary fractionator.

    Science.gov (United States)

    Chingin, Konstantin; Astorga-Wells, Juan; Pirmoradian Najafabadi, Mohammad; Lavold, Thorleif; Zubarev, Roman A

    2012-08-07

    We introduce an online multiple-junction capillary isoelectric focusing fractionator (OMJ-CIEF) for separation of biological molecules in solution by pI. In OMJ-CIEF, the separation capillary is divided into seven equal sections joined with each other via tubular Nafion membrane insertions. Each junction is communicated with its own external electrolytic buffer which is used both to supply electrical contact and for solvent exchange. The performance of the fractionator was explored using protein and peptide samples covering broad pI range. Separation was achieved in ionic and ampholytic buffers, including ammonium formate, ammonium hydroxide, histidine, and arginine. By maintaining electric potential across upstream segments of the capillary after the focusing stage, selective release of downstream analyte fractions could be achieved. The selective release mode circumvents the problem of peak broadening during mobilization and enables convenient comprehensive sampling for orthogonal separation methods. Using single-component ampholyte buffers with well-defined pI cutoff values, controlled separation of protein mixture into basic and acidic fractions was demonstrated. The device is cheap and easy to fabricate in-house, simple in operation, and straightforward in interfacing to hyphened analytical platforms. OMJ-CIEF has a potential of becoming a practical add-on unit in a wide range of bioanalytical setups, in particular as a first-dimension separation in mass spectrometry based proteomics or as a preparative tool for analyte purification, fractionation, and preconcentration.

  11. Improvement of accuracy for the quantitation of selenoproteins in post-column isotope dilution technique with HPLC ICP/MS

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Soo Jin; Pak, Yong Nam [Dept. of Chemistry Education, Korea National University of Education, Cheongju (Korea, Republic of)

    2016-11-15

    Post-column isotope dilution (PCID) or species-unspecific isotope dilution (ID) is a very useful quantitative technique in chromatography hyphenated with inductively coupled plasma–mass spectrometer (ICP/MS). In quantitative analysis, the calibration curve method is the most common one. However, it is not an absolute technique for the determination of concentration for the samples. ID method is the absolute one for the quantitative measurement technique, which means the quantity could be determined by the fundamental unit such as weight. To use the technique, it needs some requirements and there are several restrictions especially in the application for high-performance liquid chromatography (HPLC). The impurities in eluting solvent were in question. Thus, different purity of AA was examined and the result is shown in Figure 3. Figure 3(a) is the one for low (98%) and Figure 3(b) is high (99.999%) purity AA. The dotted area is for the eluting solvent. When low purity of 98% AA was introduced, the background was increasing while it remained the same for high-purity AA.

  12. INSERÇÃO NO AGRONEGÓCIO PELO COOPERATIVISMO: A EXPERIÊNCIA DA “COOPERAÇAFRÃO” EM MARA ROSA-GO CO-OPERATIVISM AS A DEVICE FOR TAKING PART IN AGRIBUSINESS: THE “COOPERAÇAFRÃO” EXPERIENCE IN MARA ROSA-GO

    Directory of Open Access Journals (Sweden)

    Carlos Shiley Domiciano

    2008-09-01

    afrão de Mara Rosa (Cooperaçafrão. With the intention of analysing this experience, as an instrument for insertion of family farmers in the turmeric agribusiness (pigment and seasoning, the text approaches, under a historical perspective, the genesis and growth of the agribusiness for this product in the region. The approach is focused on the conflictive social relations stabilished by social agents that take part in the production chain,exposing the difficulties faced by farmers, and pointing out specially the action of intermediary agents involved in the commercialization process. The study covers the creation of Cooperaçafrão, as a ";social capital"; establishing experience, characterized in what has been known as ";solidary co-operativism";, which aims to make possible the social and economic reproduction of family farmers in this production chain.

    KEY-WORDS: Agricultural co-operativism; family agriculture;social capital.

    This work aimed to study the interaction between genotypes and environments, using the BLUP/REML procedure for evaluation of precocious cashew clones. The purpose of this work was to identify genotypes that simultaneously aggregate high productivity and

  13. Tetanus: still a public health problem! Tétanos: ¡Todavía un problema de salud pública!

    Directory of Open Access Journals (Sweden)

    Augusto Quevedo Vélez

    2008-06-01

    Full Text Available

    Tetanus is an immune-preventable disease which still causes ravages in nations without protective vaccination coverage. Its lethality rate is almost 50%. It is necessary that health personnel are familiarized with its prevention, diagnosis, treatment and

  14. Reanimación del paciente quemado Resuscitation of burned patients

    Directory of Open Access Journals (Sweden)

    Marco Antonio Hoyos Franco

    2008-06-01

    Full Text Available

    The aim of this work was to diagnose relevant aspects of the “cachaça” production

  15. The Greeks and the Utopia: an overview through ancient Greek Literature

    Directory of Open Access Journals (Sweden)

    Rosanna Lauriola

    2009-06-01

    Full Text Available

    Abstract

    It is a common experience to dream of a world where everyone would live happy and in harmony with both the environment and the other people, without sufferings and injustice, under a perfect socio-political system, without wars or hunger. This dream has inspired different people form different eras and cultures to build imaginary worlds for compensating the dissatisfaction with the current one. Utopia is the name of the imaginary world they proposed either as alternative one or as temporary oasis able to release people from the reality. Literally meaning ‘no-place’, the

  1. The Right to a Fair Trial in Times of Terrorism: A Method to Identify the Non-Derogable Aspects of Article 14 of the International Covenant on Civil and Political Rights

    Directory of Open Access Journals (Sweden)

    Evelyne Schmid

    2009-02-01

    Full Text Available Contrary to what is often asserted in debates on the “war on terror”, international law provides specific rules on what is allowed in bringing suspected terrorists to trial. This article suggests a method to identify the minimum fair trial

  2. Hepatitis C: análisis de asociación a marcadores microsatélites que tamizan el HLA

    Directory of Open Access Journals (Sweden)

    Mauricio Camargo

    2001-04-01

    Full Text Available

    En varios trabajos se ha publicado la existencia de asociación estadística entre polimorfismos del HLA y el pronóstico de individuos seropositivos al virus de la hepatitis C (VHC pero no existen estudios que demuestren asociación entre genes y ser infectado por VHC

  3. Bilimsel Toplantı Duyuruları

    Directory of Open Access Journals (Sweden)

    Adli Tıp Uzmanları Derneği ATUD

    1997-10-01

    Full Text Available 1\tForensicon 98, International Conference of Forensic Medicine and XIX Annual Conference of Indian Academy of Forensic Medicine, 11-13 Şubat 1998, Imphal, India. Dr Fimate, Dept. Forensic Medicine, Regional Institute of Medical Sciences, Imphal 795 004, Manipur, India. 2\t5th International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers 11-13 Şubat 1998, Bruges, Belgium. Ordibo bvba, Lucas Henninckstraat 18, B-2610 Wilrijk (Antwerp, Belgium. Tel: +32 561 2831 Fax: +32 3 827 8439. 3\tAAFS Meeting 9-14 Şubat 1998, San Francisco. Jan Bashinski, Tel: (916 227-9564. Fax: (916 227-3639. Email: BASHINSJ@hdcdojnet.state.ca. us 4\t28th Annual International Symposium on Environmental Analytical Chemistry, 2-\t5 Mart 1998, Geneva, Switzerland. Mrs M. Frei-Hausler, IAEAC Secretariat, PO Box 46, CH-4123 Allschwil 2, Switzerland. 5\tExpert Witness and Government Liaison Group, 12\tMart 1998, London, Forensic handwriting ‘The write side of the law’. Assoc, of Consulting Scientists, PO Box 4040, Thorpe-le-Soken, COl6 OEL. 6\t5th Meeting on Supercritical Fluids, Materials and Natural Products Processing, 23-25 Mart 1998, Nice, France. F Brionne, ISASE, 1 rue Grandville - BP 451, F-54001 Nancy Cedex, France. 7\tMedical and Forensic Imaging, 2-\t4\tNisan 1998, The Guildhall, Bath, UK. Mr RL Tapper, Dept of Medical Photography, The Royal London Hospital, Stepney Way, Whitechapel, London El IBB. Tel: 0171 377 7000 ext. 2432. Fax: 0171 377 7435. 8\tHPLC 98 22nd International symposium on high performance liquid phase separations and related techniques 3-\t8\tMayıs 1998, St Louis, Minnesota. Janet Cunningham, Barr Enterprises, PO Box 279, Walkersvillé MD 21793, US. 9\tNorthwest Association of Forensic Scientists Spring 1998 Workshops and Seminar 4-\t8\tMayıs 1998 Portland, Oregon, USA Ms.Deborah Newville Oregon State Police Forensic Laboratory 1111 SW 2nd Ave. Portland, OR 97204 USA (503229-5017 (voice (503229

  4. Os gregos e a utopia: uma visão panorâmica através da literatura grega antiga

    Directory of Open Access Journals (Sweden)

    Rosanna Lauriola

    2009-06-01

    Full Text Available

    É uma experiência comum sonhar com um mundo onde todos viveriam felizes e em harmonia com a natureza e outras pesaos, sem sofrimento e injustiça,  sob um sistema sócio-político perfeito, sem guerras e sem fome. Este sonho inspirou pessoas de diferentes eras e culturas, e as levou a compensar  sua dissatisfação com o presente construindo mundos imaginários, que são chamados de utopias, que funcionam tanto como um mundo alternativo ou um oásis temporário que pode libertar as pessoas da realidade. Literalmente significando “lugar nenhum,” o termo tem uma raiz antiga grega mas  ele não existe no vocabulário da língua grega antiga. Embora os

  5. ADAPTACIÓN, VALIDACIÓN Y ESTANDARIZACIÓN DEL CUESTIONARIO DE VIVENCIAS ACADÉMICAS EN SU VERSIÓN REDUCIDA (QVA-R

    Directory of Open Access Journals (Sweden)

    DIANA PAOLA MÁRQUEZ RODRÍGUEZ

    2009-08-01

    Full Text Available

    Anthropometric and functional characteristics of phisically active individuals Características antropométricas y funcionales de individuos físicamente activos

    Directory of Open Access Journals (Sweden)

    Liliana Constanza Marmolejo

    2008-06-01

    Full Text Available

    In order to determine their health status and physical fitness, studies were carried out in 57 women and 60 men

  6. Displacement across the Trecastagni Fault (Mt. Etna and induced seismicity: the October 2009 to January 2010 episode

    Directory of Open Access Journals (Sweden)

    Vincenza Maiolino

    2011-08-01

    Full Text Available The Trecastagni Fault (TF is a NNW-SSE tectonic structure inside Mt. Etna that is characterized by evident morphological scarps and normal and right-lateral type movements that directly affect roads and buildings. The TF has an important role in the instability that affects the south-eastern flank of Mt. Etna, and it represents part of the southern boundary of the unstable sector. Starting from 2005, the TF has been monitored using continuous wire extensometers and by carrying out periodic direct measurements across the northern and central sectors. From 2005 to September 2009, the measurements show that the TF has undergone continuous extension of about 2-3 mm/yr. During the October 2009 to January 2010 period, the creep rate of the TF reached up to 5.5 to 7.0 mm/yr, and this was accompanied by several shallow, low magnitude earthquakes that were felt by local people. This episode appears to be linked to the increase in the sliding velocity of the eastern flank that occurred during 2009.

    Sleep is one of the basic needs in a child’s life and it is essential for day time alert state. Any sleep

  7. Applicability of multisyringe chromatography coupled to cold-vapor atomic fluorescence spectrometry for mercury speciation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Guzman-Mar, J.L.; Hinojosa-Reyes, L. [Department of Chemistry Sciences, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, Pedro de Alba s/n, C.P. 66451 San Nicolas de los Garza, Nuevo Leon (Mexico); Serra, A.M. [Department of Chemistry, University of the Balearic Islands, E-07122 Palma de Mallorca (Spain); Hernandez-Ramirez, A. [Department of Chemistry Sciences, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, Pedro de Alba s/n, C.P. 66451 San Nicolas de los Garza, Nuevo Leon (Mexico); Cerda, V., E-mail: victor.cerda@uib.es [Department of Chemistry, University of the Balearic Islands, E-07122 Palma de Mallorca (Spain)

    2011-12-05

    Graphical abstract: An automatic system, based on the applicability of multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) detection is developed for mercury speciation. Highlights: Black-Right-Pointing-Pointer The on-line coupling of MSC to CV/AFS was developed for mercury speciation analysis. Black-Right-Pointing-Pointer The speciation of MeHg{sup +}, Hg{sup 2+} and EtHg{sup +} was achieved on a RP C18 monolithic column. Black-Right-Pointing-Pointer The hyphenated system provided higher sample throughput compared to HPLC-CV/AFS. Black-Right-Pointing-Pointer The limits of detection for mercury species were comparable or better than those reported by HPLC-CV/AFS. Black-Right-Pointing-Pointer The developed method also provided low instrumental and operational costs. - Abstract: In this paper, a novel automatic approach for the speciation of inorganic mercury (Hg{sup 2+}), methylmercury (MeHg{sup +}) and ethylmercury (EtHg{sup +}) using multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) was developed. For the first time, the separation of mercury species was accomplished on a RP C18 monolithic column using a multi-isocratic elution program. The elution protocol involved the use of 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (99:1, v/v), followed by 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (90:10, v/v). The eluted mercury species were then oxidized under post-column UV radiation and reduced using tin(II) chloride in an acidic medium. Subsequently, the generated mercury metal were separated from the reaction mixture and further atomized in the flame atomizer and detected by AFS. Under the optimized experimental conditions, the limits of detection (3{sigma}) were found to be 0.03, 0.11 and 0.09 {mu}g L{sup -1} for MeHg{sup +}, Hg{sup 2+} and EtHg{sup +}, respectively. The relative standard deviation (RSD, n = 6) of the

  8. La Revolución (¿libertaria? Mexicana - Cien años de una lectura del proceso revolucionario de México pela prensa obrera brasileña

    Directory of Open Access Journals (Sweden)

    Fabio da Silva Sousa

    2010-11-01

    Full Text Available

    En el umbral de completar cien años desde su eclosión, pocas fueron las producciones historiográficas brasileñas que trataron de investigar cómo este acontecimiento sui generis, repercutió en nuestra república recién instaurada. Con el objetivo de cubrir esta laguna, pretendo, explorar los principales puntos y los avances de mi investigación, cuya meta es indagar cómo la Revolución de México fue publicada en la prensa operaria producida por los militantes anarquistas de Brasil en el inicio del

  9. Formal Variability of Terms in the Sphere of Network Technologies

    Directory of Open Access Journals (Sweden)

    Roman Viktorovich Deniko

    2015-09-01

    Full Text Available The article addresses the problem of formal variability of terms in the sphere of network terminology in the Russian language. The research is based on data from the Internet communication in the sphere of network technologies. Such formal variability types as graphical, phonemic, word building and complex (graphic and phonetic, morphologic and accentual are discussed in this article. The authors reveal the reasons for graphic variability of foreign origin terms making up the international terminological fund. These reasons cover such aspects as the use of graphics of source language and recipient language; the presence or absence of hyphenation, etc. It is determined that the phonemic variants of terms appear as a result of oral or written borrowings. The existence of such variants is also connected with the stage of their adaptation in the Russian language after borrowing. In this case the variants are related with soft or hard pronunciation of consonants. There are also some cases of phonemic variability on the graphic level. The complex variability is regarded as a part of active processes taking place in the modern Russian language, and these processes involve both native and foreign origin terms. The particular attention is paid to the word-building variants – word-building affixes the variability of which is peculiar of network technologies. The results of the research show that the variability of professional units belonging to the network technologies sublanguage is caused by the active process of borrowing of specialpurpose vocabulary into the Russian language. The process is due to the intensification of intercultural communication in the professional spheres.

  10. Robust microwave-assisted extraction protocol for determination of total mercury and methylmercury in fish tissues

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, L. Hinojosa; Rahman, G.M. Mizanur [Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, PA 15282 (United States); Kingston, H.M. Skip [Department of Chemistry and Biochemistry, Duquesne University, Pittsburgh, PA 15282 (United States)], E-mail: kingston@duq.edu

    2009-01-12

    A rapid and efficient closed vessel microwave-assisted extraction (MAE) method based on acidic leaching was developed and optimized for the extraction of total mercury (Hg), inorganic mercury (Hg{sup 2+}) and methylmercury (CH{sub 3}Hg{sup +}) from fish tissues. The quantitative extraction of total Hg and mercury species from biological samples was achieved by using 5 mol L{sup -1} HCl and 0.25 mol L{sup -1} NaCl during 10 min at 60 deg. C. Total Hg content was determined using inductively coupled plasma mass spectrometry (ICP-MS). Mercury species were measured by liquid chromatography hyphenated with inductively coupled plasma mass spectrometry (LC-ICP-MS). The method was validated using biological certified reference materials ERM-CE464, DOLT-3, and NIST SRM-1946. The analytical results were in good agreement with the certified reference values of total Hg and CH{sub 3}Hg{sup +} at a 95% confidence level. Further, accuracy validation using speciated isotope-dilution mass spectrometry (SIDMS, as described in the EPA Method 6800) was carried out. SIDMS was also applied to study and correct for unwanted species transformation reactions during and/or after sample preparation steps. For the studied reference materials, no statistically significant transformation between mercury species was observed during the extraction and determination procedures. The proposed method was successfully applied to fish tissues with good agreement between SIDMS results and external calibration (EC) results. Interspecies transformations in fish tissues were slightly higher than certified reference materials due to differences in matrix composition. Depending on the type of fish tissue, up to 10.24% of Hg{sup 2+} was methylated and up to 1.75% of CH{sub 3}Hg{sup +} was demethylated to Hg{sup 2+}.

  11. A method for simultaneous analysis of phytosterols and phytosterol esters in tobacco leaves using non aqueous reversed phase chromatography and atmospheric pressure chemical ionization mass spectrometry detector.

    Science.gov (United States)

    Ishida, Naoyuki

    2014-05-02

    While numerous analytical methods for phytosterols have been reported, the similar polarity and large molecules of phytosterol esters have made the methods lengthy and complicated. For this reason, an analytical method that could completely separate phytosterol esters including the higher fatty acids such as palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid in addition to phytosterols without preliminary separation was developed. The separation was accomplished by non-aqueous reversed phase chromatography technique using only acetone and acetonitrile. An atmospheric pressure chemical ionization/mass spectrometry detector configured at selected ion monitoring mode was hyphenated with the separation system to detect phytosterols and phytosterol esters. Twenty-four types of these were consequently separated and then identified with their authentic components. The calibration curve was drawn in the range of about 5 to 25,000 ng/mL with a regression coefficient over 0.999. The limit of detection and limit of quantification, respectively, ranged from 0.9 to 3.0 ng/mL and from 3.0 to 11.0 ng/mL. Recovery rates ranged from 80 to 120%. The quantification results were subjected to statistical analysis and hierarchical clustering analysis, and were used to determine the differences in the amounts of phytosterols and phytosterol esters across tobacco leaves. The newly developed method succeeded in clarifying the whole composition of phytosterols and phytosterol esters in tobacco leaves and in explaining compositional differences across the variety of tobacco leaves. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Supercritical fluid extraction of lipids from linseed with on-line evaporative light scattering detection.

    Science.gov (United States)

    Abrahamsson, Victor; Rodriguez-Meizoso, Irene; Turner, Charlotta

    2015-01-01

    Supercritical fluid extraction (SFE) is a green alternative method of extraction for neutral lipids in seeds compared to conventional methods utilizing organic solvents. In this work, a novel method where SFE is hyphenated with an evaporative light scattering detector is presented. The method was subsequently applied to determine lipid content in crushed linseed. The new method enables rapid quantification of extracted lipids as well as be ability to continuously monitor the extraction rate in real-time, thus being able to determine the time point of completed extraction. Both the detector and the method was validated. The results show that any of several tested oils can be used to calibrate the detection method for the determination of lipids extraction from linseed. The overall method repeatability and intermediate precision was 2.6% relative standard deviations. The extracted amount was significantly less than that obtained using the standard method of Soxhlet with petroleum ether, 26.0±0.4% (95% CI, n=9) compared to 32.3±1.3% (95% CI, n=3) of extracted amounts. It was found that channeling effects were present, and by either performing sequential repeated extractions with decompression in-between or by using a relatively large vessel a more complete extraction could be obtained. Interestingly, a substantially higher extracted amount (approximately 50%) was obtained compared to both a single extraction by SFE and the Soxhlet method. Therefore, it is recommended that an additional extraction including a rapid decompression in-between should be included in the validation of a method using supercritical fluid extraction, in order to either rule out channeling effects or to acquire a full recovery. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. In-line coupling of supported liquid membrane extraction to capillary electrophoresis for simultaneous analysis of basic and acidic drugs in urine.

    Science.gov (United States)

    Pantůčková, Pavla; Kubáň, Pavel

    2017-10-13

    Simultaneous extraction of basic and acidic drugs across thin supported liquid membrane (SLM) and direct injection of the extracted drugs from SLM surface into capillary electrophoresis (CE) were demonstrated. A microextraction device compatible with injection system of commercial CE instrument was filled with 20μL of sample and 10μL of acceptor solution, which were interspaced by the SLM impregnated with 5μL of organic solvent. Extractions of three basic drugs (nortriptyline, haloperidol and loperamide) and two acidic drugs (ketoprofen and naproxen) were achieved at optimized conditions including 1-ethyl-2-nitrobenzene as SLM solvent, natural pH of sample solution, 2.5mM NaOH acceptor solution and 30min extraction time. The extracted drugs were directly injected into CE for separation and quantification in a background electrolyte solution consisting of 30mM ammonium acetate adjusted to pH 4.2 with acetic acid. The entire analytical procedure including drugs extraction, injection, separation and quantification was automated in the CE instrument and the only manual procedures were SLM impregnation and filling the microextraction device with sample and acceptor solutions. The analytical method was suitable for simultaneous determination of basic and acidic drugs in undiluted human urine samples and was used for direct determination of naproxen in urine after oral administration of Nalgesin S tablet. Efficient elimination of sample matrix and selective transfer of basic and acidic drugs were achieved and the hyphenated SLM-CE method was characterized by repeatability of peak areas ranging from 3.7 to 13.4%, linear relationship between peak areas and concentrations (r 2 =0.994-0.999) and limits of detection between 0.05 and 1.5μg/mL. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Degradation effects in the extraction of antioxidants from birch bark using water at elevated temperature and pressure.

    Science.gov (United States)

    Co, Michelle; Zettersten, Camilla; Nyholm, Leif; Sjöberg, Per J R; Turner, Charlotta

    2012-02-24

    Experiments with birch bark samples have been carried to enable a distinction between extraction and degradation effects during pressurised hot water extraction. Two samples, E80 and E180, contained birch bark extracts obtained after extraction at 80 and 180°C for up to 45 min, respectively. Two other samples, P80 and P180, were only extracted for 5 min at the two temperatures and were thereafter filtered and hydrothermally treated at 80 and 180°C, respectively. During the latter treatment, samples were collected at different times to assess the stability of the extracted compounds. An offline DPPH (2,2-diphenyl-1-picrylhydrazyl) assay, as well as a high performance liquid chromatographic separation coupled to an electrochemical detector, were used to determine the antioxidant capacity of the processed samples. The results obtained with the different techniques were compared to assess the yield of the extraction and degradation processes. In addition, an online hyphenated system comprising high performance liquid chromatography coupled to diode-array; electrochemical; and tandem mass spectrometric detection (HPLC-DAD-ECD-MS/MS) was used to study the compositions of the extracts in more detail. The results for the samples processed at 80°C showed that the extraction reached a steady-state already after 5 min, and that the extracted compounds were stable throughout the entire extraction process. Processing at 180°C, on the other hand, gave rise to partly degraded extracts with a multitude of peaks in both the diode array and electrochemical detectors, and a higher antioxidant capacity compared to for the extracts obtained at 80°C. It is concluded that HPLC-DAD-ECD is a more appropriate technique for the determination of antioxidants than the DPPH assay. The mass spectrometric results indicate that one of the extracted antioxidants, catechin, was isomerised to its diastereoisomers; (+)-catechin, (-)-catechin, (+)-epicatechin, and (-)-epicatechin. Copyright

  15. Anti-inflammatory properties of phenolic compounds and crude extract from Porphyra dentata.

    Science.gov (United States)

    Kazłowska, Katarzyna; Hsu, Todd; Hou, Chia-Chung; Yang, Wen-Chin; Tsai, Guo-Jane

    2010-03-02

    Porphyra dentata, a red edible seaweed, has long been used worldwide in folk medicine for the treatment of inflammatory diseases such as hypersensitivity, lymphadenitis, bronchitis. To clarify the anti-inflammatory role of Porphyra dentata crude extract and its identified phenolic compounds by investigating their effect on the nitric oxide (NO)/inducible nitric oxide synthase (iNOS) transcription pathway in macrophage RAW 264.7 cells. Porphyra dentata crude extract was prepared with methanol. High performance liquid chromatography (HPLC) hyphenated to electrospray ionization mass spectrometry (ESI-MS) and UV detection were utilized to analyze the extract fingerprints. Nitrite measurement, iNOS promoter activity and nuclear factor-kappaB (NF-kappaB) enhancer activity were used to assess the anti-inflammatory effect in lipopolysaccharide (LPS) challenged mouse RAW 264.7 cell line. Phenolic compounds (catechol, rutin and hesperidin) were identified in the crude extract of Porphyra dentata. The crude extract and the phenolic compounds inhibited the production of NO in LPS-stimulated RAW 264.7 cells. Catechol was a more potent suppressor of the up-regulation of iNOS promoter and NF-kappaB enhancer than rutin and yet, hesperidin alone failed to inhibit either activity. Our results indicate that catechol and rutin, but not hesperidin, are primary bioactive phenolic compounds in the crude extract to suppress NO production in LPS-stimulated macrophages via NF-kappaB-dependent iNOS gene transcription. The data also explain the anti-inflammatory use and possible mechanism of Porphyra dentata in iNOS implicated diseases. Copyright (c) 2009 Elsevier Ireland Ltd. All rights reserved.

  16. Analysis of petroleum hydrocarbons in soil from view of bioremediation process

    International Nuclear Information System (INIS)

    Mracnova, R.; Sojak, L.; Kubinec, R.; Kraus, A.; Eszenyiova, A.; Ostrovsky, I.

    2002-01-01

    The pollution of the environment by petroleum hydrocarbons is the most often pollution of them all. Nevertheless, hydrocarbons present in environment can be not only of petroleum or anthropogenic origin, but of biogenic as well. Typically the hydrocarbons are presented in the environment as very complex mixtures of individual compounds with very different chemical structure, wide range of the boiling points (∼800 0 C) as well as with the wide range of the number of carbon atoms. Immediately they are spread in any environmental matrix the complex physical, chemical and biochemical reactions start. A lot of methods have been developed and new are permanently in progress for the monitoring and control of petroleum hydrocarbons contamination and/or soils bioremediation. Generally, all methods by whose the hydrocarbons contaminants are determined in GC-FID system do not satisfied recommendations for enough accurate and precise results. Hyphenation of capillary gas chromatography and mass selective detector operated in the selective ion monitoring mode essentially allows detailed specification of non-polar extractable hydrocarbons. Isoprenoid alkanes, alkylhomologues of aromatic hydrocarbons and polycyclic alkanes hopanes-like were investigated as markers for recognition of petroleum and biogenic contamination. C 30 17α(H)21β(H)-hopane (C 30 -hopane) seems to be a suitable marker to identify hydrocarbons origin, to determine composting rates for nonpolar extractable compounds and to calculate real content of non-polar extractable compounds in final composting status on the assumption that the contamination is of mineral oil type. This is the survey into the results obtained in this field published in the literature as well as reached in our laboratory. (author)

  1. Transparency and the logic of auto-immunity

    Directory of Open Access Journals (Sweden)

    Emanuele Antonelli

    2011-12-01

    Full Text Available In Voyous, Jacques Derrida develops his argument starting from the presupposition that democracy as such is the entity whose integrity and immunity are at stake and, therefore, under investigation. This gesture reflects the setting in which ten years before, in Foi et savoir, he had cast his reasoning about the logic of immunity. There, it was one of the sources of religion, the immunity of the sacred, that operated according to this logic. The hyphen between these two essays, beside Derrida’s own crossed references, is the genealogical reasoning on the meaning and essence of the concept of democracy: contrary to what Derrida claims, it will be maintained that Athenian democracy had a clear immune matrix, whose constant exercise is clearly defined, in spite of himself, by Vernant, and it will be shown how modern democracy has been forced to change policy. Modern democracy is an entity characterized by an immune deficiency. In order to save Derrida’s intuition from both the collapse of different vantage points and from a quite bizarre reticence in taking into account of the immune value of rituals, our starting point will be René Girard’s œuvre and his reading of the role of immune logic in sacred systems and, more generally, in modernity. The threshold between the auto-immune reaction, immune deficiency and auto-immune disease, between the sacrifice who delimits and constitutes the self and the holocauste du peuple en détail, is the space where, constantly exposed to the risk of auto-denial, democracy lives. 

  2. Discovered acetylcholinesterase inhibition and antibacterial activity of polyacetylenes in tansy root extract via effect-directed chromatographic fingerprints.

    Science.gov (United States)

    Móricz, Ágnes M; Ott, Péter G; Morlock, Gertrud E

    2018-03-30

    The knowledge about the activity of polyacetylenes was extended by their new acetylcholinesterase inhibition and antibacterial activity against plant pathogenic bacteria. For this discovery, an utmost streamlined workflow, which we consider to be of high potential in the field of natural product or superfood search was developed. It demonstrates the combined power of biological, biochemical and chemical fingerprints. Bioactive components of tansy (Tanacetum vulgare L.) root extract were profiled and identified by high-performance thin-layer chromatography hyphenated with in situ effect-directed analysis, chemical derivatizations and high-resolution mass spectrometry (HPTLC-UV/Vis/FLD-EDA-HRMS). The effect-directed profiling was performed using four bacterial bioassays including two plant pathogens, an antioxidant assay and acetyl- and butyrylcholinesterase inhibitory assays. The chromatographic, spectral and powerful mass spectrometric study of zones that exerted substantial antibacterial and/or antioxidant and/or acetylcholinesterase inhibitory effects allowed these multi-potent zones to be identified as polyacetylenes. Five polyacetylene compounds were assigned to be 2-non-1-ene-3,5,7-triynyl-3-vinyl-oxirane, 2-(2,4-hexadiynylidene)-3,4-epoxy-1,6-dioxaspiro[4.5]decane, trans- and cis-2-(2,4-hexadiynylidene)-1,6-dioxaspiro[4.5]dec-3-ene and tetradeca-2,4,6-triine-8-en-12-one. This study clearly showed the advantage of the combined use of different ionization sources, i.e. electrospray ionization via an elution-head based interface and also the Direct Analysis in Real Time interface, for HRMS analysis of compounds from the same class with very similar chromatographic behavior and polarity. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Van los linyeras... Construction and circulation of a positive view of romantic individualism in early twentieth century Argentina Van los linyeras… Construcción y circulación de una noción positiva del individualismo romántico vitalista durante la primera mitad del siglo XX argentino

    Directory of Open Access Journals (Sweden)

    Lucas Rubinich

    2008-09-01

    Full Text Available

    The article explains how a positive view of romantic individualism embodied in the hobos circulated and established in the first half of 20

  4. Pregnancy and glomerulonephritis. A review Glomerulonefritis y embarazo. Revisión de tema

    Directory of Open Access Journals (Sweden)

    Luis Fernando Arias Restrepo

    2008-06-01

    Full Text Available

    Antecedent: Glomerulal involvement is rare during pregnancy, but the associated morbidity is serious and potentially lethal. How does it affect prognosis? Objective: To define guidelines for the care of women affected by glomerulal disease during the

  5. Two new tropolonic alkaloids from Colchicum speciosum Steven bulbs

    Directory of Open Access Journals (Sweden)

    S. Tayyeb*

    2017-11-01

    Full Text Available Background and objectives: The genus Colchicum belongs to the family Colchicaceae, which comprises of 19 genera, and 225 species worldwide. They have been recognized for more than 2000 years for their noticeable biological properties. The Colchicum species are well known for presence of tropolonic alkaloids, mainly colchicine. Colchicine, is still the drug of choice for treatment of gout, and is used for the treatment of a number of proinflammatory disorders, such as familial Mediterranean fever, and Behcet’s disease. Clinical studies have proved colchicine to posses potent anti-tumor activity. Colchicum speciosum Steven is an indigenous perennial herbaceous plant widely distributed in northern, central and western regions of Iran.  Methods: In the present study, the phytochemical composition of MeOH extract from bulbs of C. speciosum collected fromSavadkouh region, Iranwas investigated by combination of HPLC-PDA-MS spectrometry and NMR specroscopy. The fractionation of MeOH extract was carried out by partitioning on CH2Cl2, EtOAc and water. Results: The isolation and purification of CH2Cl2 portion by combination of reverse and normal phase chromatography resulted in the isolation, purification and identification of two new tropolonic alkaloids, compounds (1 and (2, as well as two known compound colchicine (3 and demecolcine (4. Their structures were established by extensive spectroscopic methods, including 1D (1H NMR and 2D-NMR (COSY, HSQC and HMBC. The absolute configurations of isolated compounds were established by aid of circular dichroism. Conclusion: Phytochemical investigation of CH2Cl2 extract of C. speciosum by combination of HPLC, column chromatography and hyphenated spectroscopic techniques led to identification two new alkaloids with potential as lead compounds.

  6. Studies on the origin and transformation of selenium and its chemical species along the process of petroleum refining

    Science.gov (United States)

    Stivanin de Almeida, Cibele M.; Ribeiro, Anderson S.; Saint'Pierre, Tatiana D.; Miekeley, Norbert

    2009-06-01

    Inductively coupled plasma optical emission spectrometry and mass spectrometry (ICPMS), the latter hyphenated to flow injection hydride generation, electrothermal vaporization or ion chromatography, have been applied to the chemical characterization of crude oil, aqueous process stream samples and wastewaters from a petroleum refinery, in order to get information on the behavior of selenium and its chemical species along effluent generation and treatment. Multielemental characterization of these effluents by ICPMS revealed a complex composition of most of them, with high salinity and potential spectral and non-spectral interferents present. For this reason, a critical re-assessment of the analytical techniques for the determination of total selenium and its species was performed. Methane was employed as gas in dynamic reaction cell ICPMS and cell parameters were optimized for a simulated brine matrix and for diluted aqueous solutions to match the expected process and treated wastewaters samples. The signal-to-background ratios for 78Se and 80Se were used as criteria in optimization, the first isotope resulting in better detection limits for the simulated brine matrix ( 78Se: 0.07 μg L - 1 , 80Se: 0.31 μg L - 1 ). A large variability in the concentration of selenium (from concentrations changes of this element measured in aqueous process stream and wastewater samples. Highest concentrations of total selenium were analyzed in samples from the hydrotreater (up to about 1800 μg L - 1 ). The predominance of selenocyanate (SeCN -) was observed in most of the wastewaters so far investigated, but also other species were detected with retention times different from Se(IV), Se(VI) and SeCN -. Colloidal selenium (Se 0) was the only Se-species observed in samples from the atmospheric distillation unit, but was also identified in other samples, most probably formed by the decomposition of SeCN - or other unstable species.

  7. Lab-on-a-Valve Mesofluidic Platform for On-Chip Handling of Carbon-Coated Titanium Dioxide Nanotubes in a Disposable Microsolid Phase-Extraction Mode.

    Science.gov (United States)

    García-Valverde, María Teresa; Rosende, María; Lucena, Rafael; Cárdenas, Soledad; Miró, Manuel

    2018-04-03

    Mesofluidic lab-on-a-valve (LOV) platforms have been proven suitable to accommodate automatic micro-solid-phase extraction (μSPE) approaches with on-chip handling of micrometer-bead materials in a fully disposable mode to prevent sample cross-contamination and pressure-drop effects. The efficiency of the extraction process notably depends upon the sorptive capacity of the material because the sorbent mass is usually down to 10 mg in LOV devices. Nanomaterials, capitalizing upon their enhanced surface-to-volume ratio and diversity of potential chemical moieties, are appealing alternatives to microbead sorbents. However, the handling and confinement of nanomaterials in fluidic chip structures have been challenging to date. This is most likely a consequence of the aggregation tendency of a number of nanomaterials, including carbon-based sorbents, that leads to excessive back-pressure in flowing systems along with irreproducible bead loading. This paper addresses these challenges by ad hoc synthesis of hybrid nanomaterials, such as porous carbon-coated titanium dioxide nanotubes (TiO 2 -NT@pC). Tailoring of the surface polarity of the carbon coating is proven to foster the dispersion of TiO 2 -NT@pC in LOV settings while affording superior extraction capability of moderately nonpolar species from aqueous matrices. The determination of trace-level concentrations of butylparaben (BPB) and triclosan (TCS) in seawater samples is herein selected as a proof-of-concept of the exploitation of disposable nanomaterials in LOV. The mesofluidic platform accommodating μSPE features online hyphenation to liquid chromatography/tandem mass spectrometry (LC/MS/MS) for reliable determination of the target analytes with excellent limits of detection (0.5 and 0.6 ng/L for BPB and TCS, respectively) and intermediate precision (relative standard deviation handling troublesome environmental samples.

  8. DEVELOPMENT OF Annona crassiflora Mart. (ARATICUM SEEDLINGS IN SUBSTRATA WITH SUGAR CANE BAGASSE ASH DESENVOLVIMENTO DE MUDAS DE Annona crassiflora Mart. (ARATICUM EM SUBSTRATOS COM CINZA DE BAGAÇO DE CANA

    Directory of Open Access Journals (Sweden)

    Andréia Luiza Salgado

    2009-01-01

    Full Text Available

    The effect of five growing media, in different proportions of subsoil, limestone, and sugar cane bagasse ash, in the height, stem diameter, and fresh and dry weight of the aerial part and roots of araticum seedlings (Annona crassiflora Mart. was analyzed. The five growing media were

  9. Hollow-fiber flow field-flow fractionation and multi-angle light scattering investigation of the size, shape and metal-release of silver nanoparticles in aqueous medium for nano-risk assessment.

    Science.gov (United States)

    Marassi, Valentina; Casolari, Sonia; Roda, Barbara; Zattoni, Andrea; Reschiglian, Pierluigi; Panzavolta, Silvia; Tofail, Syed A M; Ortelli, Simona; Delpivo, Camilla; Blosi, Magda; Costa, Anna Luisa

    2015-03-15

    Due to the increased use of silver nanoparticles in industrial scale manufacturing, consumer products and nanomedicine reliable measurements of properties such as the size, shape and distribution of these nano particles in aqueous medium is critical. These properties indeed affect both functional properties and biological impacts especially in quantifying associated risks and identifying suitable risk-mediation strategies. The feasibility of on-line coupling of a fractionation technique such as hollow-fiber flow field flow fractionation (HF5) with a light scattering technique such as MALS (multi-angle light scattering) is investigated here for this purpose. Data obtained from such a fractionation technique and its combination thereof with MALS have been compared with those from more conventional but often complementary techniques e.g. transmission electron microscopy, dynamic light scattering, atomic absorption spectroscopy, and X-ray fluorescence. The combination of fractionation and multi angle light scattering techniques have been found to offer an ideal, hyphenated methodology for a simultaneous size-separation and characterization of silver nanoparticles. The hydrodynamic radii determined by fractionation techniques can be conveniently correlated to the mean average diameters determined by multi angle light scattering and reliable information on particle morphology in aqueous dispersion has been obtained. The ability to separate silver (Ag(+)) ions from silver nanoparticles (AgNPs) via membrane filtration during size analysis is an added advantage in obtaining quantitative insights to its risk potential. Most importantly, the methodology developed in this article can potentially be extended to similar characterization of metal-based nanoparticles when studying their functional effectiveness and hazard potential. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Evaluation of stable isotope labelling strategies for the quantitation of CP4 EPSPS in genetically modified soya

    Energy Technology Data Exchange (ETDEWEB)

    Ocana, Mireia Fernandez [Centre for Chemical and Bioanalytical Sciences, Royal Holloway, University of London, Egham TW20 0EX (United Kingdom)], E-mail: Mireia.FernandezOcana@pfizer.com; Fraser, Paul D. [Centre for Chemical and Bioanalytical Sciences, Royal Holloway, University of London, Egham TW20 0EX (United Kingdom); Patel, Raj K.P.; Halket, John M. [Specialist Bioanalytical Services Ltd., Royal Holloway, University of London, Egham TW20 0EX (United Kingdom); Bramley, Peter M. [Centre for Chemical and Bioanalytical Sciences, Royal Holloway, University of London, Egham TW20 0EX (United Kingdom)

    2009-02-16

    The introduction of genetically modified (GM) crops into the market has raised a general alertness relating to the control and safety of foods. The applicability of protein separation hyphenated to mass spectrometry to identify the bacterial enolpyruvylshikimate-3-phosphate synthase (CP4 EPSPS) protein expressed in GM crops has been previously reported [M.F. Ocana, P.D. Fraser, R.K.P. Patel, J.M. Halket, P.M. Bramley, Rapid Commun. Mass Spectrom. 21 (2007) 319.]. Herein, we investigate the suitability of two strategies that employ heavy stable isotopes, i.e. AQUA and iTRAQ, to quantify different levels of CP4 EPSPS in up to four GM preparations. Both quantification strategies showed potential to determine whether the presence of GM material is above the limits established by the European Union. The AQUA quantification procedure involved protein solubilisation/fractionation and subsequent separation using SDS-PAGE. A segment of the gel in which the protein of interest was located was excised, the stable isotope labeled peptide added at a known concentration and proteolytic digestion initiated. Following recovery of the peptides, on-line separation and detection using LC-MS was carried out. A similar approach was used for the iTRAQ workflow with the exception that proteins were digested in solution and generated tryptic peptides were chemically tagged. Both procedures demonstrated the potential for quantitative detection at 0.5% (w/w) GM soya which is a level below the current European Union's threshold for food-labelling. In this context, a comparison between the two procedures is provided within the present study.

  11. Evaluation of stable isotope labelling strategies for the quantitation of CP4 EPSPS in genetically modified soya

    International Nuclear Information System (INIS)

    Ocana, Mireia Fernandez; Fraser, Paul D.; Patel, Raj K.P.; Halket, John M.; Bramley, Peter M.

    2009-01-01

    The introduction of genetically modified (GM) crops into the market has raised a general alertness relating to the control and safety of foods. The applicability of protein separation hyphenated to mass spectrometry to identify the bacterial enolpyruvylshikimate-3-phosphate synthase (CP4 EPSPS) protein expressed in GM crops has been previously reported [M.F. Ocana, P.D. Fraser, R.K.P. Patel, J.M. Halket, P.M. Bramley, Rapid Commun. Mass Spectrom. 21 (2007) 319.]. Herein, we investigate the suitability of two strategies that employ heavy stable isotopes, i.e. AQUA and iTRAQ, to quantify different levels of CP4 EPSPS in up to four GM preparations. Both quantification strategies showed potential to determine whether the presence of GM material is above the limits established by the European Union. The AQUA quantification procedure involved protein solubilisation/fractionation and subsequent separation using SDS-PAGE. A segment of the gel in which the protein of interest was located was excised, the stable isotope labeled peptide added at a known concentration and proteolytic digestion initiated. Following recovery of the peptides, on-line separation and detection using LC-MS was carried out. A similar approach was used for the iTRAQ workflow with the exception that proteins were digested in solution and generated tryptic peptides were chemically tagged. Both procedures demonstrated the potential for quantitative detection at 0.5% (w/w) GM soya which is a level below the current European Union's threshold for food-labelling. In this context, a comparison between the two procedures is provided within the present study

  12. Effects of ice crystal surface roughness and air bubble inclusions on cirrus cloud radiative properties from remote sensing perspective

    International Nuclear Information System (INIS)

    Tang, Guanglin; Panetta, R. Lee; Yang, Ping; Kattawar, George W.; Zhai, Peng-Wang

    2017-01-01

    polarimetric observations when both factors are considered. • Cirrus cloud particle habit model of the MODIS collection 6 achieves better self[HYPHEN]consistency and consistency with polarimetric observations when both factors are considered.

  13. 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.

  14. Heart-cutting two-dimensional gas chromatography-isotope ratio mass spectrometry analysis of monoaromatic hydrocarbons in complex groundwater and gas-phase samples.

    Science.gov (United States)

    Ponsin, Violaine; Buscheck, Timothy E; Hunkeler, Daniel

    2017-04-07

    Compound-specific isotope analysis (CSIA) is increasingly used to evaluate the origin and fate of petroleum hydrocarbons in the environment. However, as samples often contain a complex mixture of compounds and the method requires a full chromatographic separation, it can be challenging to obtain accurate and precise isotope values. In this study, in order to develop a method to analyze carbon isotopes in benzene, toluene, ethylbenzene, and xylenes (BTEX) in complex environmental samples, a two-dimensional heart-cutting gas chromatograph (GC) was hyphenated to an isotope ratio mass spectrometer (IRMS). The focus was placed on benzene and toluene, which are the main compounds of concern in contaminated sites. A full separation for BTEX was successfully achieved using a 60m polar column in the first dimension and a 30m non-polar column in the second dimension. Accuracy and precision of carbon isotope measurements of standards were not impacted by the new setup compared to classic one-dimensional (1D) GC-C-IRMS. For benzene and toluene, precision remained very good (≤0.2‰) for concentrations comprised between 5 and 20μg/L. A high matrix load did not influence the precision and accuracy of isotope measurements. The method was tested on several samples from two different field sites. For all samples tested, full chromatographic baseline resolution was achieved for benzene and toluene. Spatial variability of isotopes values linked to biodegradation was evidenced for one field site. This new 2D-GC-C-IRMS method will broaden the spectrum of samples suitable for isotope analysis and will be therefore able to give new insights into attenuation processes of BTEX in contaminated sites or source fingerprinting. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Using In Silico Fragmentation to Improve Routine Residue Screening in Complex Matrices

    Science.gov (United States)

    Kaufmann, Anton; Butcher, Patrick; Maden, Kathryn; Walker, Stephan; Widmer, Mirjam

    2017-12-01

    Targeted residue screening requires the use of reference substances in order to identify potential residues. This becomes a difficult issue when using multi-residue methods capable of analyzing several hundreds of analytes. Therefore, the capability of in silico fragmentation based on a structure database ("suspect screening") instead of physical reference substances for routine targeted residue screening was investigated. The detection of fragment ions that can be predicted or explained by in silico software was utilized to reduce the number of false positives. These "proof of principle" experiments were done with a tool that is integrated into a commercial MS vendor instrument operating software (UNIFI) as well as with a platform-independent MS tool (Mass Frontier). A total of 97 analytes belonging to different chemical families were separated by reversed phase liquid chromatography and detected in a data-independent acquisition (DIA) mode using ion mobility hyphenated with quadrupole time of flight mass spectrometry. The instrument was operated in the MSE mode with alternating low and high energy traces. The fragments observed from product ion spectra were investigated using a "chopping" bond disconnection algorithm and a rule-based algorithm. The bond disconnection algorithm clearly explained more analyte product ions and a greater percentage of the spectral abundance than the rule-based software (92 out of the 97 compounds produced ≥1 explainable fragment ions). On the other hand, tests with a complex blank matrix (bovine liver extract) indicated that the chopping algorithm reports significantly more false positive fragments than the rule based software. [Figure not available: see fulltext.

  16. Contribution of analytical techniques coupled to the knowledge of the uranium speciation in natural conditions

    International Nuclear Information System (INIS)

    Petit, J.

    2009-06-01

    To understand the transport mechanisms and the radionuclides behaviour in the bio-geosphere is necessary to evaluate healthy and environmental risks of nuclear industry. These mechanisms are monitored by radioelements speciation, namely the distribution between their different physico-chemical forms in the environment. From this perspective, this PhD thesis deals with uranium speciation in a natural background. A detailed summary of uranium biogeochemistry has been written, which enables to restrict the PhD issue to uranium complexation with oxalic acid, a hydrophilic organic acid with good binding properties, ubiquitous in soil waters. Analytical conditions have been established by means of speciation diagrams. The speciation diagrams building by means of literature stability constants has allowed to define the analytical conditions of complex formation. The chosen analytical technique is the hyphenation of a separative technique (liquid chromatography LC or capillary electrophoresis CE) with mass spectrometry (ICPMS). The studied complexes presence in the synthetic samples has been confirmed with UV/visible spectrophotometry. LC-ICPMS analyses have proved the lability of the uranyl-organic acid complexes, namely their tendency to dissociate during analysis, which prevents from studying uranium speciation. CE-ICPMS study of labile complexes from a metal-ligand system has been made possible by employing affinity capillary electrophoresis, which enables to determine stability constants and electrophoretic mobilities. This PhD thesis has allowed to compare the different mathematical treatments of binding isotherm and to take into account ionic strength and real ligand concentration. Affinity CE has been applied successfully to lanthanum-oxalate (model system) and uranium-oxalate systems. The obtained results have been applied to a real system (situated in Le Bouchet). This shows the contribution of the developed method to the modelling of uranium speciation. (author)

  17. Simultaneous determination of Hg(II) and alkylated Hg, Pb, and Sn species in human body fluids using SPME-GC/MS-MS

    Energy Technology Data Exchange (ETDEWEB)

    Dunemann, L.; Hajimiragha, H.; Begerow, J. [Department of Analytical Chemistry, Medizinisches Inst. fuer Umwelthygiene, Duesseldorf (Germany)

    1999-03-01

    A GC/MS-MS method for the determination of Hg(II) and alkylated Hg, Pb, and Sn species in human urine is described. Separation and identification of the metal species are performed by capillary gas chromatography coupled with an ion-trap mass spectrometer with electron impact ionization in the tandem-MS mode. For sample preparation a very promising technique was applied that is based on a derivatization with sodium tetraethylborate followed by headspace solid phase microextraction (SPME). Operation of the used ion trap in the tandem-MS mode yields in improved detection limits because of a signal-to-noise ratio that is at least one order of magnitude better than in the MS mode. The detection limits in real matrices like urine are between 7 and 22 ng/L for all species investigated. Urinary levels of inorganic Hg in non-occupationally exposed persons with and without dental amalgam were found to be between 0.1 and 1.4 {mu}g/L. A reference material (``ClinRep, Level I``) was used for quality assurance. Compared to the coupling of GC with ICP-MS (``inorganic`` MS), the advantage of the proposed method using an ``organic`` MS is that (i) the species can be directly identified via their precursor and daughter ions and (ii) analysis can be performed with a commercially available hyphenated technique at moderate costs and needs no lab-made interfacing. Moreover, it offers a real multi-element/multi-species capability with low detection limits and a minimum of sample preparation. (orig.) With 1 fig., 1 tab., 9 refs.

  18. Antioxidant and Antiglycating Constituents from Leaves of Ziziphus oxyphylla and Cedrela serrata

    Directory of Open Access Journals (Sweden)

    Rizwan Ahmad

    2016-03-01

    Full Text Available Ziziphus oxyphylla and Cedrela Serrata plants have a folkloric use in Pakistan for treatments of different ailments, i.e., Jaundice, Hepatitis, Diabetes, and antimicrobial. Until now, none of the research studies have reported any phytochemical work on leaves of these two plants. This study aimed to isolate and perform phytochemical analysis in order to search for the constituent having the active role in treatment of the aforementioned ailments. A bioassay-guided fractionation and isolation procedure was used to isolate the concerned phytochemicals present in leaf extracts of Z. oxyphylla and C. serrata. The process involved the hyphenated techniques, i.e., Flash Chromatography, Semi-Preparative HPLC/DAD, UPLC/MS, and NMR in order to isolate and elucidate the structure of the phytochemicals. Seven compounds (1–7 were isolated and identified as flavonoids, more in particular glycosides of quercetin and kaempferol. They showed DPPH scavenging activity, compound 3 (isoquercitrin being the most active one with an IC50 of 10.8 µg/mL (positive control quercetin; IC50 3.6 µg/mL. The superoxide-radical scavenging and total antioxidant (ABTS assays indicated IC50 values ranging from 200 to 910 µg/mL and 170 to 320 µg/mL, respectively (positive control quercetin: 374 and 180 µg/mL, respectively. Furthermore, these compounds had low IC50 values for inhibition of protein glycation (AGEs inhibition, ranging from 530 to 818 µg/mL, comparable to aminoguanidine (510 µg/mL used as a positive control. This study resulted in the identification of seven flavonoid glycosides for the first time from the leaves of Z. oxyphylla and C. serrata with antioxidative and antiglycating activities.

  19. The intelectual exile in Mexico. Notes on the Argentinean experience 1974-1983 El exilio intelectual en México. Notas sobre la experiencia argentina 1974-1983

    Directory of Open Access Journals (Sweden)

    José María Casco

    2008-09-01

    Full Text Available

    The article analyzes the process of renewal

  20. Mercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation of Hg{sup 0}

    Energy Technology Data Exchange (ETDEWEB)

    Quadros, Daiane P.C. de [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Campanella, Beatrice; Onor, Massimo; Bramanti, Emilia [National Research Council of Italy, C.N.R., Instituto di Chimica dei Composti Organo Metallici – ICCOM – UOS Pisa, Area della Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Borges, Daniel L.G. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); D' Ulivo, Alessandro, E-mail: dulivo@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Instituto di Chimica dei Composti Organo Metallici – ICCOM – UOS Pisa, Area della Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2014-11-01

    We described the hyphenation of photo-induced chemical vapor generation with high performance liquid chromatography–atomic fluorescence spectrometry (HPLC–AFS) for the quantification of inorganic mercury, methylmercury (MeHg) and ethylmercury (EtHg). In the developed procedure, formic acid in mobile phase was used for the photodecomposition of organomercury compounds and reduction of Hg{sup 2+} to mercury vapor under microwave/ultraviolet (MW/UV) irradiation. We optimized the proposed method studying the influence of several operating parameters, including the type of organic acid and its concentration, MW power, composition of HPLC mobile phase and catalytic action of TiO{sub 2} nanoparticles. Under the optimized conditions, the limits of detection were 0.15, 0.15 and 0.35 μg L{sup −1} for inorganic mercury, MeHg and EtHg, respectively. The developed method was validated by determination of the main analytical figures of merit and applied to the analysis of three certified reference materials. The online interfacing of liquid chromatography with photochemical-vapor generation–atomic fluorescence for mercury determination is simple, environmentally friendly, and represents an attractive alternative to the conventional tetrahydroborate (THB) system. - Highlights: • Inorganic and organic mercury were determined by photochemical vapor generation using a MW/UV photochemical reactor. • The optimized procedure has been applied to the speciation of Hg(II), MeHg and EtHg coupling HPLC with PVG–AFS. • The proposed method is simple, sensitive, and is established for mercury determination in biological materials.

  1. Dereplication of Natural Products Using GC-TOF Mass Spectrometry: Improved Metabolite Identification By Spectral Deconvolution Ratio Analysis

    Directory of Open Access Journals (Sweden)

    Fausto Carnevale Neto

    2016-09-01

    Full Text Available Dereplication based on hyphenated techniques has been extensively applied in plant metabolomics, avoiding re-isolation of known natural products. However, due to the complex nature of biological samples and their large concentration range, dereplication requires the use of chemometric tools to comprehensively extract information from the acquired data. In this work we developed a reliable GC-MS-based method for the identification of non-targeted plant metabolites by combining the Ratio Analysis of Mass Spectrometry deconvolution tool (RAMSY with Automated Mass Spectral Deconvolution and Identification System software (AMDIS. Plants species from Solanaceae, Chrysobalanaceae and Euphorbiaceae were selected as model systems due to their molecular diversity, ethnopharmacological potential and economical value. The samples were analyzed by GC-MS after methoximation and silylation reactions. Dereplication initiated with the use of a factorial design of experiments to determine the best AMDIS configuration for each sample, considering linear retention indices and mass spectral data. A heuristic factor (CDF, compound detection factor was developed and applied to the AMDIS results in order to decrease the false-positive rates. Despite the enhancement in deconvolution and peak identification, the empirical AMDIS method was not able to fully deconvolute all GC-peaks, leading to low MF values and/or missing metabolites. RAMSY was applied as a complementary deconvolution method to AMDIS to peaks exhibiting substantial overlap, resulting in recovery of low-intensity co-eluted ions. The results from this combination of optimized AMDIS with RAMSY attested to the ability of this approach as an improved dereplication method for complex biological samples such as plant extracts.

  2. Evidence of different stoichiometries for the limiting carbonate complexes of lanthanides(3); Mise en evidence d'un changement de stoechiometrie du complexe carbonate limite au sein de la serie des lanthanides(3)

    Energy Technology Data Exchange (ETDEWEB)

    Philippini, V

    2007-12-15

    Two stoichiometries have been proposed by different laboratories to interpret measurements on the limiting carbonate complexes of An{sup 3+} and Ln{sup 3+} cations. The study of the solubility of double carbonates (AlkLn(CO{sub 3}){sub 2},xH{sub 2}O) in concentrated carbonate solutions at room temperature and high ionic strengths has shown that on the one hand the lightest lanthanides (La and Nd) form Ln(CO{sub 3}){sub 4}{sup 5-} whereas the heaviest (Eu and Dy) form Ln(CO{sub 3}){sub 3}{sup 3-} in the studied chemical conditions, and on the other hand, that the kinetics of precipitation of double carbonates depends on the alkali metal and the lanthanide ions. The existence of two stoichiometries for the limiting carbonate complexes was confirmed by capillary electrophoresis hyphenated to an inductively coupled plasma mass spectrometer (CE-ICP-MS), used to extend the study to the whole series of lanthanides (except Ce, Pm and Yb). Two behaviours have been put forward comparing the electrophoretic mobilities: La to Tb form Ln(CO{sub 3}){sub 4}{sup 5-} while Dy to Lu form Ln(CO{sub 3}){sub 3}{sup 3-}. Measurements by time resolved laser fluorescence spectroscopy (TRLFS) on Eu(III) indicate small variations of the geometry of Eu(CO{sub 3}){sub 3}{sup 3-} complex, specially with Cs{sup +}. Although analogies are currently used among the 4f-block trivalent elements, different aqueous speciations are evidenced in concentrated carbonate solutions across the lanthanide series. (author)

  3. PBPK-Based Probabilistic Risk Assessment for Total Chlorotriazines in Drinking Water.

    Science.gov (United States)

    Breckenridge, Charles B; Campbell, Jerry L; Clewell, Harvey J; Andersen, Melvin E; Valdez-Flores, Ciriaco; Sielken, Robert L

    2016-04-01

    The risk of human exposure to total chlorotriazines (TCT) in drinking water was evaluated using a physiologically based pharmacokinetic (PBPK) model. Daily TCT (atrazine, deethylatrazine, deisopropylatrazine, and diaminochlorotriazine) chemographs were constructed for 17 frequently monitored community water systems (CWSs) using linear interpolation and Krieg estimates between observed TCT values. Synthetic chemographs were created using a conservative bias factor of 3 to generate intervening peaks between measured values. Drinking water consumption records from 24-h diaries were used to calculate daily exposure. Plasma TCT concentrations were updated every 30 minutes using the PBPK model output for each simulated calendar year from 2006 to 2010. Margins of exposure (MOEs) were calculated (MOE = [Human Plasma TCTPOD] ÷ [Human Plasma TCTEXP]) based on the toxicological point of departure (POD) and the drinking water-derived exposure to TCT. MOEs were determined based on 1, 2, 3, 4, 7, 14, 28, or 90 days of rolling average exposures and plasma TCT Cmax, or the area under the curve (AUC). Distributions of MOE were determined and the 99.9th percentile was used for risk assessment. MOEs for all 17 CWSs were >1000 at the 99.9(th)percentile. The 99.9(th)percentile of the MOE distribution was 2.8-fold less when the 3-fold synthetic chemograph bias factor was used. MOEs were insensitive to interpolation method, the consumer's age, the water consumption database used and the duration of time over which the rolling average plasma TCT was calculated, for up to 90 days. MOEs were sensitive to factors that modified the toxicological, or hyphenated appropriately no-observed-effects level (NOEL), including rat strain, endpoint used, method of calculating the NOEL, and the pharmacokinetics of elimination, as well as the magnitude of exposure (CWS, calendar year, and use of bias factors). © The Author 2016. Published by Oxford University Press on behalf of the Society of

  4. Speciation studies of vanadium in human liver (HepG2) cells after in vitro exposure to bis(maltolato)oxovanadium(IV) using HPLC online with elemental and molecular mass spectrometry.

    Science.gov (United States)

    Nischwitz, Volker; Davies, Julie T; Marshall, Damian; González, Macarena; Gómez Ariza, Jose Luis; Goenaga-Infante, Heidi

    2013-12-01

    A large number of studies has been published proposing a range of vanadium containing compounds as potential new anti-diabetic drugs due to the observed insulin mimetic function of V(IV) complexes. Vanadium uptake and distribution within the body have been investigated in animal models by determination of total vanadium concentrations. Phase I and phase IIa human clinical trials have been completed with the ethyl analogue of bis(maltolato)oxovanadium(IV) (BMOV). Mass spectrometry studies have focused on the characterisation of vanadium transferrin in body fluids after incubation with BMOV. However, the application of hyphenated mass spectrometric techniques for the identification of low molecular mass mediating vanadium metabolites in human body fluids or tissues after exposure to BMOV or in more simplified and cheaper models such as in vitro diabetes models has not been reported yet. This paper describes for the first time methodology for the characterisation of the predominant anionic vanadium metabolite in a liver cell model after exposure to BMOV. Total vanadium determination in cell lysates indicated significant uptake of vanadium. Size exclusion chromatography was applied with combined elemental and molecular mass spectrometric detection for vanadium speciation analysis in the cell lysates. The effect of cell medium and lysis conditions on the observed vanadium metabolites was studied. For the first time stable isotope labelling was applied to BMOV in order to achieve unambiguous correlation between elemental and molecular mass spectrometric results. Candidate elemental formulae for the unknown metabolite were derived based on accurate mass measurements. The most likely candidate formula combined with MS/MS fragmentation data is consistent with the presence of a divanadate-phosphate derivate.

  5. Detection and Characterization of ZnO Nanoparticles in Surface and Waste Waters Using Single Particle ICPMS.

    Science.gov (United States)

    Hadioui, Madjid; Merdzan, Vladimir; Wilkinson, Kevin J

    2015-05-19

    The increasing production of ZnO nanoparticles (nZnO) makes their analysis and characterization extremely important from an ecological risk perspective, especially at the low concentrations at which they are expected to be found in natural waters. Single particle ICPMS (SP-ICPMS) is one of the few techniques available to detect and characterize nanoparticles at environmentally relevant concentrations. Unfortunately, at the very low particle concentrations where SP-ICPMS is performed, significant dissolution of the nZnO generally increases background levels of dissolved Zn to the point where measurements are not generally possible. By hyphenating SP-ICPMS with an ion-exchange resin, it was possible to characterize and quantify nZnO in order to gain insight into the nature of the nZnO in natural waters. Spiked and unspiked water samples were analyzed using a SP-ICPMS that was coupled to a column containing a strong metal binding resin (Chelex 100). In addition to the detection of ZnO nanoparticles and the determination of a size distribution in natural waters, it was possible to partition the dissolved Zn among free and/or labile and strongly bound Zn fractions. In two natural waters, a high proportion (ca. 93-100%) of dissolved Zn was measured, and the residual ZnO particles were mainly composed of small agglomerates (average sizes ranging from 133.6 to 172.4 nm in the surface water and from 167.6 to 216.4 nm in the wastewater effluent). Small numbers of small nanoparticles were also detected in nonspiked waters.

  6. Novel analytical methods for characterising binding media and protective coatings in artworks

    International Nuclear Information System (INIS)

    Domenech-Carbo, Maria Teresa

    2008-01-01

    Since the first reported analytical studies and technical examinations of art and archaeological objects conducted in the late 18th century, analytical techniques and methods applied to the study of artworks have constantly grown. Among the materials composing the art object, organic compounds used as binding media or protective coatings have attracted the attention of the conservation profession given their noticeable ability for undergoing morphological and chemical changes on ageing. Thus, the aim of this paper is to review the most recent advances in the identification and determination of organic compounds present in art and art conservation materials. Immunofluorescence techniques have been proposed in recent decades as an alternative to the classical and simpler microchemical tests. Besides, a variety of instrumental techniques have also been improved in an attempt to enhance the sensitivity, repeatability and accuracy of the analytical results. Spectroscopic techniques, such as UV-vis, FTIR and Raman spectroscopy, have been coupled with light microscopes for these purposes. Synchrotron radiation FTIR microspectroscopy has also been successfully applied to the analysis of artworks. Mass spectrometry has also been increasingly used as a detector system coupled with a chromatographic device. Chromatographic methods have also improved in recent years. Paper and thin layer chromatographic techniques have been progressively replaced with gas chromatography (GC), pyrolysis-GC, high performance liquid chromatography and capillary electrophoresis. More complex proteomics hyphenated techniques, such as nano-liquid chromatography-nano-electrospray ionisation/collision quadrupole time-of-flight tandem mass spectrometry, have been recently applied to the identification and determination of proteinaceous binders. Microbeam analytical techniques have also been incorporated into the list of advanced instrumental techniques for art conservation purposes. Finally, a number

  7. On-line complexation/cloud point preconcentration for the sensitive determination of dysprosium in urine by flow injection inductively coupled plasma-optical emission spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ortega, Claudia; Cerutti, Soledad; Silva, Maria F. [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700, San Luis (Argentina); Olsina, Roberto A.; Martinez, Luis D. [Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, Chacabuco y Pedernera, 5700, San Luis (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Avda. Rivadavia 1917, CP C1033AAJJ, Buenos Aires (Argentina)

    2003-01-01

    An on-line dysprosium preconcentration and determination system based on the hyphenation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with ICP-OES was studied. For the preconcentration of dysprosium, a Dy(III)-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex was formed on-line at pH 9.22 in the presence of nonionic micelles of PONPE-7.5. The micellar system containing the complex was thermostated at 30 C in order to promote phase separation, and the surfactant-rich phase was retained in a microcolumn packed with cotton at pH 9.2. The surfactant-rich phase was eluted with 4 mol L{sup -1} nitric acid at a flow rate of 1.5 mL min{sup -1}, directly in the nebulizer of the plasma. An enhancement factor of 50 was obtained for the preconcentration of 50 mL of sample solution. The detection limit value for the preconcentration of 50 mL of aqueous solution of Dy was 0.03 {mu}g L{sup -1}. The precision for 10 replicate determinations at the 2.0 {mu}g L{sup -1}Dy level was 2.2% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for dysprosium was linear with a correlation coefficient of 0.9994 at levels near the detection limits up to at least 100 {mu}g L {sup -1}. The method was successfully applied to the determination of dysprosium in urine. (orig.)

  8. [Infectious corneal ulcers--once with endophthalmitis--after photorefractive keratotomy with disposable contact lens].

    Science.gov (United States)

    Faschinger, C; Faulborn, J; Ganser, K

    1995-02-01

    Infections of the cornea with or without involvement of intraocular tissues are severe complications after photorefractive keratectomy. We report on three cases with ulcerative keratitis and one case with severe endophthalmitis, which developed some days after laser treatment. After 39 photo-therapeutic and 118 photo-refractive treatments without complications four young treated persons suffered from corneal infiltrations. Three of them developed severe corneal ulcerations, one a severe endophthalmitis. We used the laser machine of the company Schwind (193 nm wavelength, repetition rate 10 Hz, fluence 180-200 mJ/cm2). One part of the treatment which all patients had in common was the application of a disposable contact lens postoperatively, which was worn overnight. THERAPY AND FOLLOW-UP: Because all three patients with ulcerations revealed hyphen of fungi in their corneal-scratch material they were treated with antifungal agents locally and systemically. Due to the local and temporal connection the patient with the endophthalmitis was treated with antifungal agents, too. All corneal ulcerations healed with scars similar to a haze graded 3 to 4, the eye with the endophthalmitis healed almost completely. Probably the use of disposable contact lenses postoperatively, especially the overnight wear, during an extremely hot and humid summer lead to the described severe infections of the eyes after the "traumatisation" of the cornea by the excimer laser. A known higher concentration of Aspergillus in the air due to renovations of buildings in the clinical area might have been an additional negative effect. The avoidance of the use of disposable contact lenses postoperatively, especially the overnight wear, is emphasized.

  9. Granulomatous peritonitis due to Ascaris lumbricoides. Case report Granulomatosis peritoneal por Ascaris lumbricoides.Presentación de un caso

    Directory of Open Access Journals (Sweden)

    Carlos Aguirre Muñoz

    2008-06-01

    Full Text Available

    Ascariasis is one of the most prevalent and widespread human helminthic infections, especially in children of

  10. Plasmonic Interrogation of Biomimetic Systems for Enhanced Toxicity Assays

    Science.gov (United States)

    Hinman, Samuel Stuart

    fabrication of new plasmonic materials for membrane-based assays is presented, as well as method developments in membrane array formation and opportunities for hyphenation with complementary analytical techniques.

  11. Thermal degradation kinetics of polylactic acid/acid fabricated cellulose nanocrystal based bionanocomposites.

    Science.gov (United States)

    Monika; Dhar, Prodyut; Katiyar, Vimal

    2017-11-01

    Cellulose nanocrystals (CNC) are fabricated from filter paper (as cellulosic source) by acid hydrolysis using different acids such as sulphuric (H 2 SO 4 ), phosphoric (H 3 PO 4 ), hydrochloric (HCl) and nitric (HNO 3 ) acid. The resulting acid derived CNC are melt mixed with Polylactic acid (PLA) using extruder at 180°C. Thermogravimetric (TGA) result shows that increase in 10% and 50% weight loss (T 10 , T 50 ) temperature for PLA-CNC film fabricated with HNO 3 , H 3 PO 4 and HCl derived CNC have improved thermal stability in comparison to H 2 SO 4 -CNC. Nonisothermal kinetic studies are carried out with modified-Coats-Redfern (C-R), Ozawa-Flynn-Wall (OFW) and Kissinger method to predict the kinetic and thermodynamic parameters. Subsequently prediction of these parameter leads to the proposal of thermal induced degradation mechanism of nanocomposites using Criado method. The distribution of E a calculated from OFW model are (PLA-H 3 PO 4 -CNC: 125-139 kJmol -1 ), (PLA-HNO 3 -CNC: 126-145 kJmol -1 ), (PLA-H 2 SO 4 -CNC: 102-123 kJmol -1 ) and (PLA-HCl-CNC: 140-182 kJmol -1 ). This difference among E a for the decomposition of PLA-CNC bionanocomposite is probably due to various acids used in this study. The E a calculated by these two methods are found in consonance with that observed from Kissinger method. Further, hyphenated TG-Fourier transform infrared spectroscopy (FTIR) result shows that gaseous products such as CO 2 , CO, lactide, aldehydes and other compounds are given off during the thermal degradation of PLA-CNC nanocomposite. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Circulating ultrasound-assisted extraction, countercurrent chromatography, and liquid chromatography for the simultaneous extraction, isolation, and analysis of the constituents of Uncaria tomentosa.

    Science.gov (United States)

    Zhang, Yuchi; Liu, Chunming; Qi, Yanjuan; Li, Sainan; Pan, Yan; Li, Yuchun

    2015-04-03

    A hyphenated automated technique for the online extraction, isolation, analysis, and identification of natural organic compounds was established. Circulating ultrasound-assisted extraction (CUAE) was coupled with countercurrent chromatography (CCC), high performance liquid chromatography (HPLC), and a diode array detector (DAD). This approach was applied to the fractionation and purification of alkaloids from Uncaria tomentosa. A biphasic solvent system of chloroform-methanol-water (6:4:5, v:v:v) was used for the CUAE and CCC separation of compounds from 500 g of U. tomentosa. Two CUAE/CCC/HPLC/DAD modes were established. Either the upper aqueous phase or the lower organic phase of the solvent system could be used as the extraction solvent. The target compounds were extracted by CUAE, and the extract was pumped into a sample loop before being directly injected into the CCC column, or pre-purified using a flash chromatography column before injection. The target compounds were eluted using either the organic or aqueous phase of the solvent system and the fractions were monitored using a UV detector. The target fractions were collected by a sample loop via a six-port valve, and analyzed by HPLC/DAD for purity and structural identification. This system isolated of 8.2mg, 7.4 mg, and 12.9 mg of rhynchophylline, corynoxine, and corynoxine B with HPLC purities of 96.15%, 95.34%, and 95.49%, respectively via the first mode; and isolated 26.6 mg, 24.6 mg, and 45.3mg of rhynchophylline, corynoxine, and corynoxine B with a HPLC purities of 98.22%, 97.18%, and 97.93% via the second mode. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  13. Benefits and Limitations of DNA Barcoding and Metabarcoding in Herbal Product Authentication

    Science.gov (United States)

    Raclariu, Ancuta Cristina; Heinrich, Michael; Ichim, Mihael Cristin

    2017-01-01

    Abstract Introduction Herbal medicines play an important role globally in the health care sector and in industrialised countries they are often considered as an alternative to mono‐substance medicines. Current quality and authentication assessment methods rely mainly on morphology and analytical phytochemistry‐based methods detailed in pharmacopoeias. Herbal products however are often highly processed with numerous ingredients, and even if these analytical methods are accurate for quality control of specific lead or marker compounds, they are of limited suitability for the authentication of biological ingredients. Objective To review the benefits and limitations of DNA barcoding and metabarcoding in complementing current herbal product authentication. Method Recent literature relating to DNA based authentication of medicinal plants, herbal medicines and products are summarised to provide a basic understanding of how DNA barcoding and metabarcoding can be applied to this field. Results Different methods of quality control and authentication have varying resolution and usefulness along the value chain of these products. DNA barcoding can be used for authenticating products based on single herbal ingredients and DNA metabarcoding for assessment of species diversity in processed products, and both methods should be used in combination with appropriate hyphenated chemical methods for quality control. Conclusions DNA barcoding and metabarcoding have potential in the context of quality control of both well and poorly regulated supply systems. Standardisation of protocols for DNA barcoding and DNA sequence‐based identification are necessary before DNA‐based biological methods can be implemented as routine analytical approaches and approved by the competent authorities for use in regulated procedures. © 2017 The Authors. Phytochemical Analysis Published by John Wiley & Sons Ltd. PMID:28906059

  14. Comprehensive two-dimensional gas chromatography-mass spectrometry analysis of volatile constituents in Thai vetiver root oils obtained by using different extraction methods.

    Science.gov (United States)

    Pripdeevech, Patcharee; Wongpornchai, Sugunya; Marriott, Philip J

    2010-01-01

    Vetiver root oil is known as one of the finest fixatives used in perfumery. This highly complex oil contains more than 200 components, which are mainly sesquiterpene hydrocarbons and their oxygenated derivatives. Since conventional GC-MS has limitation in terms of separation efficiency, the comprehensive two-dimensional GC-MS (GC x GC-MS) was proposed in this study as an alternative technique for the analysis of vetiver oil constituents. To evaluate efficiency of the hyphenated GC x GC-MS technique in terms of separation power and sensitivity prior to identification and quantitation of the volatile constituents in a variety of vetiver root oil samples. METHODOLOGY. Dried roots of Vetiveria zizanioides were subjected to extraction using various conditions of four different methods; simultaneous steam distillation, supercritical fluid, microwave-assisted, and Soxhlet extraction. Volatile components in all vetiver root oil samples were separated and identified by GC-MS and GC x GC-MS. The relative contents of volatile constituents in each vetiver oil sample were calculated using the peak volume normalization method. Different techniques of extraction had diverse effects on yield, physical and chemical properties of the vetiver root oils obtained. Overall, 64 volatile constituents were identified by GC-MS. Among the 245 well-resolved individual components obtained by GC x GC-MS, the additional identification of 43 more volatiles was achieved. In comparison with GC-MS, GC x GC-MS showed greater ability to differentiate the quality of essential oils obtained from diverse extraction conditions in terms of their volatile compositions and contents.

  15. Zirconium silicate assisted removal of residual proteins after organic solvent deproteinization of human plasma, enhancing the stability of the LC–ESI-MS response for the bioanalysis of small molecules

    Energy Technology Data Exchange (ETDEWEB)

    Hussain, Shah; Pezzei, Cornelia [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Güzel, Yüksel [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); ADSI-Austrian Drug Screening Institute, Innrain 66a, 6020 Innsbruck (Austria); Rainer, Matthias [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Huck, Christian W., E-mail: Christian.W.Huck@uibk.ac.at [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); Bonn, Günther K. [Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University, Innrain 80/82, 6020 Innsbruck (Austria); ADSI-Austrian Drug Screening Institute, Innrain 66a, 6020 Innsbruck (Austria)

    2014-12-10

    Highlights: • A novel sample preparation technique for isolation of small molecules from human plasma. • Effectiveness of zirconium silicate for the removal of residual proteins after protein precipitation. • Abolishing the consumption of salts for the depletion of residual proteins after protein precipitation. • More than 99.6% removal of plasma proteins. - Abstract: An efficient blood plasma clean-up method was developed, where methanol protein precipitation was applied, followed by zirconium silicate assisted exclusion of residual proteins. A strong binding of zirconium (IV) silicate to the proteins enabled the elimination of remaining proteins after solvent deproteinization through a rapid solid-phase extraction (SPE) procedure. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF MS) was used for monitoring the proteins during clean-up practice applied to human plasma samples. The proteins were quantified by colorimetric detection using the bicinchoninic acid (BCA) assay. The presented analytical strategy resulted in the depletion of >99.6% proteins from human plasma samples. Furthermore, high-performance liquid chromatography hyphenated to diode-array and electrospray ionization mass spectrometric detection (HPLC–DAD/ESI MS) was applied for qualitative and quantitative analysis of the caffeoylquinic acids (CQAs) and their metabolites in human plasma. The procedure demonstrated high recoveries for the standard compounds spiked at different concentrations. Cynarin and chlorogenic acid were recovered in the range of 81–86% and 78–83%, respectively. Caffeic acid was extracted in the excess of 89–92%, while ferulic acid and dihydroxyhydrocinnamic acid showed a recovery of 87–91% and 92–95%, respectively. The method was partially validated in accordance with FDA-Industry Guidelines for Bioanalytical Method Validation (2001). The presented scheme improves the clean-up efficacy of the methanol deproteinization

  16. Metal-metallothioneins like proteins investigation by heteroatom-tagged proteomics in two different snails as possible sentinel organisms of metal contamination in freshwater ecosystems

    Energy Technology Data Exchange (ETDEWEB)

    Franca Maltez, Heloisa [Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Claveria 8, 33006 Oviedo (Spain); Villanueva Tagle, Margarita [Faculty of Chemistry, University of La Habana (Cuba); Rosario Fernandez de la Campa, Maria del [Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Claveria 8, 33006 Oviedo (Spain); Sanz-Medel, Alfredo, E-mail: asm@uniovi.es [Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Claveria 8, 33006 Oviedo (Spain)

    2009-09-21

    Metal speciation analysis in MLPs was carried out in two snails, Marisa cornuarietis and Pomacea bridgesi, in order to investigate them as possible sentinel organisms of heavy metal contamination. To carry out this study snails born in a non-contaminated environment were divided into two groups: a control group and a contaminated one with cadmium administered for 40 days. Subsequently, we investigated the speciation of the induced MLPs in exposed animals in relation to controls. In order to obtain the MLP fraction, cytosols from both snail species where subjected to size-exclusion fractionation, monitoring on-line the metal signal (Cd, Cu and Zn) by ICP-MS while protein elution was followed by on-line UV detection. MLP fraction was then separated by anion-exchange (AE)-FPLC using optimal chromatographic conditions for the separation of the different MLP isoforms in both snail species. Specific detection of separated metalloforms was carried out again by the hyphenation of the AE chromatographic system with ICP-MS. The determination of the amount of metal bound to MLPs was carried out by post-column isotope dilution analysis ICP-MS, finding that the snail M. cornuarietis accumulated higher concentrations of cadmium than P. bridgesi. Thus this first snail could therefore be a better candidate sentinel organism of pollution in natural waters. Identification and characterization of the isoforms separated in M. cornuarietis was carried out for the entire or intact isoforms by MALDI-TOF and then conventional triptic digestion was also carried out to identify the nature of the formed peptides. The presence identification of a MLP isoform of relatively low molecular weight in M. cornuarietis is reported.

  17. Antimicrobial and efflux pump inhibitory activity of caffeoylquinic acids from Artemisia absinthium against gram-positive pathogenic bacteria.

    Directory of Open Access Journals (Sweden)

    Yiannis C Fiamegos

    2011-04-01

    Full Text Available Traditional antibiotics are increasingly suffering from the emergence of multidrug resistance amongst pathogenic bacteria leading to a range of novel approaches to control microbial infections being investigated as potential alternative treatments. One plausible antimicrobial alternative could be the combination of conventional antimicrobial agents/antibiotics with small molecules which block multidrug efflux systems known as efflux pump inhibitors. Bioassay-driven purification and structural determination of compounds from plant sources have yielded a number of pump inhibitors which acted against gram positive bacteria.In this study we report the identification and characterization of 4',5'-O-dicaffeoylquinic acid (4',5'-ODCQA from Artemisia absinthium as a pump inhibitor with a potential of targeting efflux systems in a wide panel of gram-positive human pathogenic bacteria. Separation and identification of phenolic compounds (chlorogenic acid, 3',5'-ODCQA, 4',5'-ODCQA was based on hyphenated chromatographic techniques such as liquid chromatography with post column solid-phase extraction coupled with nuclear magnetic resonance spectroscopy and mass spectroscopy. Microbial susceptibility testing and potentiation of well know pump substrates revealed at least two active compounds; chlorogenic acid with weak antimicrobial activity and 4',5'-ODCQA with pump inhibitory activity whereas 3',5'-ODCQA was ineffective. These initial findings were further validated with checkerboard, berberine accumulation efflux assays using efflux-related phenotypes and clinical isolates as well as molecular modeling methodology.These techniques facilitated the direct analysis of the active components from plant extracts, as well as dramatically reduced the time needed to analyze the compounds, without the need for prior isolation. The calculated energetics of the docking poses supported the biological information for the inhibitory capabilities of 4',5'-ODCQA and

  18. UHR-Q-TOF Analysis Can Address Common Challenges in Targeted and Untargeted Metabolomics

    Science.gov (United States)

    Zurek, G.; Krug, D.; Muller, R.; Barsch, A.

    2011-01-01

    Here, we present an ESI-UHR-Q-TOF based analysis of myxobacterial secondary metabolites, which permits to solve several challenges frequently encountered in metabolite profiling studies. Myxobacteria are promising producers of natural products exhibiting potent biological activities, and several myxobacterial metabolites are currently under investigation as potential leads for novel drugs. However, the myxobacteria are also a striking example for the divergence between the genetic capacity for the production of secondary metabolites and the number of compounds that could be characterised to date. Wild type and mutant strains were analyzed concerning the production patterns of known metabolites and with regard to the discovery of new metabolites. Sample throughput: Since mass accuracy and resolution of TOF instruments are independent of the acquisition rate, they are perfectly suited for a coupling to UHPLC separations. These hyphenations enable a reduction of analysis time in combination with a high chromatographic resolution and therefore permit an increased sample throughput. The UHR-TOF analysis revealed that an acquisition rate of up to 20Hz did not compromise the achieved mass accuracy or resolution. Targeted and untargeted metabolite profiling: Acquisition of full scan accurate mass spectra enable the targeted screening for known compounds e.g. from the class of DKxanthenes based on very selective high resolution EIC (hrEIC) traces with small mass windows of 1.0–0.5mDa. A comparison of several datasets following a “comprehensive feature extraction” combined with a statistical analysis permits an untargeted discovery of novel biomarkers using the same data files as for the targeted analysis. Identification: Even a mass accuracy of 0.1ppm is not sufficient for an unambiguous formula identification for m/z values above 500. A combination of accurate mass data and isotopic pattern information in MS and MS/MS spectra can extend this m/z range for reliable

  19. Metabolic Profiling of a Corynebacterium Glutamicum DeltaprpD2 by GC-APCI High Resolution Q-TOF Analysis

    Science.gov (United States)

    Zurek, G.; Persike, M.; Plassmeier, J.; Niehaus, K.; Barsch, A.

    2011-01-01

    Metabolomics studies based on Gas chromatography–Mass spectrometry (GC-MS) are well established and typically employ electron impact (EI) ionisation. Target compounds of interest can be identified by comparison to commercial or public databases. Unfortunately, many possible biomarkers detected in metabolic profiling experiments cannot be identified due to the lack of reference spectra for a majority of biologically relevant compounds. Therefore, many possible biomarkers remain “unknowns” up till now. Hyphenating gas chromatography with high resolution TOF-MS technology with soft atmospheric pressure ionisation (APCI) can preserve the molecular ion information and delivers accurate mass and isotopic pattern information. This data enables a sum formula generation for known and unknown target compounds. Additionally, optionally acquired MS/ MS data can extend the capabilities for structural elucidation. Mass accuracy, resolution and isotopic fidelity are independent of the TOFMS acquisition rate. Therefore, these instruments can be coupled to gas chromatography, which typically delivers narrow peak width requiring fast MS scan speeds. Corynebactrium glutamicum, a gram positive, nontoxic bacterium, is used in the industrial production of amino acids like lysine and glutamate. C. glutamicum can be grown on different carbon sources. Glucose is metabolised via glycolysis and the tricarboxylic acid (TCA) cycle, whereas propionate is catabolised through the methylcitric acid pathway. The prpD2 gene encodes a 2-methylcitrate dehydratase which is involved in the degradation of propionate. Metabolic profiling of Corynebacterium glutamicum delta-prpD2 extracts of cells grown on glucose or glucose and propionate analyzed by GC-APCI-TOF-MS revealed several compounds elevated in cells grown on propionate. Identification of 2-methylcitric acid and alanine using accurate mass and isotopic pattern information in MS and MS/MS spectra provided a proof of concept for the

  20. La trama maestra en la narrativa audiovisual. El caso del cine del Oeste

    Directory of Open Access Journals (Sweden)

    González Sánchez, José Félix

    2010-01-01

    Full Text Available Una trama nos proporciona la historia que ofrece un guión y más tarde una película. Las tramas son limitadas, sin embargo las posibilidades argumentales que éstas ofrecen son infinitas. Al mismo tiempo, podemos decir que todas las culturas se valen de unas tramas y argumentos semejantes para estructurar sus narraciones míticas. Por otro lado, Estados Unidos es la nación moderna donde mejor se mantiene una relación dialéctica entre el mito y la historia. En esta nación, el significado del acontecimiento se ha mostrado y se ha liberado a través del mito. A través de este artículo veremos cómo el western es el género de cine americano que más y mejor responde a los cánones del relato folklórico tradicional, pues sus tramas han sido tomadas directamente de las leyendas clásicas.Abstract in English: A plot provides us the story that it offers a hyphen and later a film. Plots are limited, however possibilities, argument them that these offer music infinite. At the same time, we can say that all cultures avail themselves of some plots and similar arguments to structure their mythical stories. In addition, United States is the modern nation where better a dialectic relation between the myth and story keeps. At this nation, the significance of the event has been shown and you have gotten free through the myth. We will see through this article how the western is the kind of American cinema what else and better answer for the folkloric traditional story to the cánones, because your plots have been taken directly of the classical legends.