WorldWideScience

Sample records for residual mass groups

  1. Residual nilpotence and residual solubility of groups

    International Nuclear Information System (INIS)

    Mikhailov, R V

    2005-01-01

    The properties of the residual nilpotence and the residual solubility of groups are studied. The main objects under investigation are the class of residually nilpotent groups such that each central extension of these groups is also residually nilpotent and the class of residually soluble groups such that each Abelian extension of these groups is residually soluble. Various examples of groups not belonging to these classes are constructed by homological methods and methods of the theory of modules over group rings. Several applications of the theory under consideration are presented and problems concerning the residual nilpotence of one-relator groups are considered.

  2. Detection of Gunshot Residues Using Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Regina Verena Taudte

    2014-01-01

    Full Text Available In recent years, forensic scientists have become increasingly interested in the detection and interpretation of organic gunshot residues (OGSR due to the increasing use of lead- and heavy metal-free ammunition. This has also been prompted by the identification of gunshot residue- (GSR- like particles in environmental and occupational samples. Various techniques have been investigated for their ability to detect OGSR. Mass spectrometry (MS coupled to a chromatographic system is a powerful tool due to its high selectivity and sensitivity. Further, modern MS instruments can detect and identify a number of explosives and additives which may require different ionization techniques. Finally, MS has been applied to the analysis of both OGSR and inorganic gunshot residue (IGSR, although the “gold standard” for analysis is scanning electron microscopy with energy dispersive X-ray microscopy (SEM-EDX. This review presents an overview of the technical attributes of currently available MS and ionization techniques and their reported applications to GSR analysis.

  3. Complex scaling and residual flavour symmetry in the neutrino mass ...

    Indian Academy of Sciences (India)

    2017-10-09

    Oct 9, 2017 ... Using the residual symmetry approach, we propose a complex extension of the scaling ansatz on the neutrino Majorana mass matrix M ν which allows a nonzero mass for each of the three light neutrinos as well as a nonvanishing θ 13 . Leptonic Dirac CP violation must be maximal while atmospheric ...

  4. Tuberculosis in postchemotherapy residual masses in germ cell tumor of the testis

    Directory of Open Access Journals (Sweden)

    Rajesh Bansal

    2011-01-01

    Full Text Available Residual masses following chemotherapy in testicular tumors have been characterized as necrosis, mature or immature teratoma, and malignant tumors. Twenty four patients had retroperitoneal lymph node dissection for postchemotherapy residual masses between January 2000 and December 2008. We report two patients; one with late relapse and other with postchemotherapy residual mass, who had tuberculosis. Tumor markers were normal, and PET scan showed increased uptake in residual mass. There are no previous reports of tuberculosis in postchemotherapy residual masses.

  5. Comparison of mineral dust and droplet residuals measured with two single particle aerosol mass spectrometers

    Science.gov (United States)

    Wonaschütz, Anna; Ludwig, Wolfgang; Zawadowicz, Maria; Hiranuma, Naruki; Hitzenberger, Regina; Cziczo, Daniel; DeMott, Paul; Möhler, Ottmar

    2017-04-01

    Single Particle mass spectrometers are used to gain information on the chemical composition of individual aerosol particles, aerosol mixing state, and other valuable aerosol characteristics. During the Mass Spectrometry Intercomparison at the Fifth Ice Nucleation (FIN-01) Workshop, the new LAAPTOF single particle aerosol mass spectrometer (AeroMegt GmbH) was conducting simultaneous measurements together with the PALMS (Particle Analysis by Laser Mass Spectrometry) instrument. The aerosol particles were sampled from the AIDA chamber during ice cloud expansion experiments. Samples of mineral dust and ice droplet residuals were measured simultaneously. In this work, three expansion experiments are chosen for a comparison between the two mass spectrometers. A fuzzy clustering routine is used to group the spectra. Cluster centers describing the ensemble of particles are compared. First results show that while differences in the peak heights are likely due to the use of an amplifier in PALMS, cluster centers are comparable.

  6. Complex scaling and residual flavour symmetry in the neutrino mass ...

    Indian Academy of Sciences (India)

    Probir Roy

    Centre for Astroparticle Physics and Space Science, Bose Institute, Kolkata 700 054, India. (In collaboration with Rome Samanta and Ambar Ghosal of Saha Institute). E-mail: probirrana@gmail.com. Published online 9 October 2017. Abstract. Using the residual symmetry approach, we propose a complex extension of the ...

  7. X-ray group and cluster mass profiles in MOND: unexplained mass on the group scale

    Science.gov (United States)

    Angus, G. W.; Famaey, B.; Buote, D. A.

    2008-07-01

    Although very successful in explaining the observed conspiracy between the baryonic distribution and the gravitational field in spiral galaxies without resorting to dark matter (DM), the modified Newtonian dynamics (MOND) paradigm still requires DM in X-ray bright systems. Here, to get a handle on the distribution and importance of this DM, and thus on its possible form, we deconstruct the mass profiles of 26 X-ray emitting systems in MOND, with temperatures ranging from 0.5 to 9 keV. Initially, we compute the MOND dynamical mass as a function of radius, then subtract the known gas mass along with a component of galaxies which include the cD galaxy with M/LK = 1. Next, we test the compatibility of the required DM with ordinary massive neutrinos at the experimental limit of detection (mν = 2 eV), with density given by the Tremaine-Gunn limit. Even by considering that the neutrino density stays constant and maximal within the central 100 or 150 kpc (which is the absolute upper limit of a possible neutrino contribution there), we show that these neutrinos can never account for the required DM within this region. The natural corollary of this finding is that, whereas clusters (T >~ 3 keV) might have most of their mass accounted for if ordinary neutrinos have a 2 eV mass, groups (T cluster baryonic dark matter (CBDM, Milgrom) or even sterile neutrinos would present a more satisfactory solution to the problem of missing mass in MOND X-ray emitting systems.

  8. Standardized martingale residuals applied to grouped left truncated observations of dementia cases.

    Science.gov (United States)

    Commenges, D; Rondeau, V

    2000-09-01

    The use of martingale residuals have been proposed for model checking and also to get a non-parametric estimate of the effect of an explanatory variable. We apply this approach to an epidemiological problem which presents two characteristics: the data are left truncated due to delayed entry in the cohort; the data are grouped into geographical units (parishes). This grouping suggests a natural way of smoothing the graph of residuals which is to compute the sum of the residuals for each parish. It is also natural to present a graph with standardized residuals. We derive the variances of the estimated residuals for left truncated data which allows computing the standardized residuals. This method is applied to the study of dementia in a cohort of old people, and to the possible effect of the concentration of aluminum and silica in drinking water on the risk of developing dementia.

  9. Mass residuals in implicit finite volume models for overland and groundwater flow

    Science.gov (United States)

    Lal, A. M. Wasantha; Wang, Naming; Moustafa, M. Z.; Brown, M. C.

    2010-04-01

    SummaryA primary advantage in using the finite volume method for simulating groundwater flow and overland flow is the conservation property or the ability to conserve mass. However, when implicit finite volume methods are used with large time steps, small cell areas, or parameters with extreme value ranges, the conservation of mass equation becomes slightly unbalanced with a residual. Problems with large mass residuals can be predicted using the condition number of the solution matrix, and the convergence criterion used in the sparse matrix solver. The amount of practical guidance available on how to manage the magnitude of the mass residual or the matrix condition number is limited. To address this need, the current paper shows the usefulness of the mesh ratio. The mesh ratio is a dimensionless number that is a function of the mesh resolution and the temporal resolution. It is directly related to the condition number of the matrix, which in turn affects the mass residual and the model run time. During the current study, several numerical experiments are carried out to determine how the mesh ratio and the water level are related to the condition number, how the critical mesh ratio is related to the number of cells, how the run time is related to the mesh ratio, and how the mass residual is related to the mesh ratio. The results are useful in creating guidelines for mesh design during large-scale model applications. These guidelines can be applied to reducing the mass residual and the run time. The usefulness of the mesh ratio is illustrated using a Regional Simulation Model (RSM) (Lal, A.M.W., Van Zee, Randy, Belnap, Mark, 2005. Case study: model to simulate regional flow in South Florida. Journal of Hydraulic Engineering 131 (4), 247-258) application in south Florida.

  10. Effects of heating durations on normal concrete residual properties: compressive strength and mass loss

    Science.gov (United States)

    Nazri, Fadzli Mohamed; Shahidan, Shahiron; Khaida Baharuddin, Nur; Beddu, Salmia; Hisyam Abu Bakar, Badorul

    2017-11-01

    This study investigates the effects of high temperature with five different heating durations on residual properties of 30 MPa normal concrete. Concrete cubes were being heated up to 600°C for 30, 60, 90, 120 and 150 minutes. The temperature will keep constant for 30, 60, 90, 120 and 150 minutes. The standard temperature-time curve ISO 834 is referred to. After heating the specimen were left to cool in the furnace and removed. After cooling down to ambient temperature, the residual mass and residual compressive strength were observed. The obtained result shows that, the compressive strength of concrete decrease as the heating duration increases. This heating duration influence, might affects the loss of free water present and decomposition of hydration products in concrete. As the heating duration increases, the amount of water evaporated also increases led to loss in concrete mass. Conclusively, the percentage of mass and compressive strength loss increased as the heating duration increased.

  11. Abelian groups and quadratic residues in weak arithmetic

    Czech Academy of Sciences Publication Activity Database

    Jeřábek, Emil

    2010-01-01

    Roč. 56, č. 3 (2010), s. 262-278 ISSN 0942-5616 R&D Projects: GA AV ČR IAA1019401; GA MŠk(CZ) 1M0545 Institutional research plan: CEZ:AV0Z10190503 Keywords : bounded arithmetic * abelian group * Fermat's little theorem * quadratic reciprocity Subject RIV: BA - General Mathematics Impact factor: 0.361, year: 2010 http://onlinelibrary.wiley.com/doi/10.1002/malq.200910009/abstract;jsessionid=9F636FFACB84C025FD90C7E6880350DD.f03t03

  12. Mass-to-light ratios of nearby groups of galaxies

    CERN Document Server

    Materne, J

    1980-01-01

    The application of a probability density function gives the possibility of determining groups of galaxies and membership probabilities of the galaxies in a reliable unbiased way. For the five nearest groups so defined, the mean mass-to-light ratio was derived using the concept of negative energy. These groups have a mass-to- light ratio of 16 M/sub (.)//L/sub (.)/. The probability function gives also the possibility of deriving masses of groups in a direct and independent way. (22 refs).

  13. Evaluation of clayey masses compositions starting from the residue incorporation of the red ceramic industry to obtain tubular ceramic membranes

    International Nuclear Information System (INIS)

    Silva, Adriano Lima da; Chaves, Alexsandra Cristina; Luna, Carlos Bruno Barreto; Neves, Gelmires de Araujo; Lira, Helio de Lucena

    2017-01-01

    The inappropriate residue disposal of red ceramic industry is very high. Nowadays, one of the major challenges is the investigation of processes to obtain alternative materials, enabling the use of these residues to manufacture new materials. This work's objective is to study clayey masses' compositions starting from the residue incorporation of the red ceramic industry to be used in tubular ceramic membranes. Two compositions of ceramic masses were established, composition A (50% of residue) and composition B (70% of residue). Granulometric analysis of the ceramic masses presented an average size of particles, what indicates membranes in the microfiltration scale. Another observed factor is related to the increase of residue amount, what favored a decrease in the ceramic mass' plasticity. A rise in the apparent porosity was also observed, probably because of a possible growing in the bigger pores numbers, due to the sintering high temperature and the elevation of residue quantity itself. (author)

  14. Comparison of communities of stored product mites in grain mass and grain residues in the Czech Republic.

    Science.gov (United States)

    Hubert, Jan; Munzbergová, Zuzana; Kucerová, Zuzana; Stejskal, Václav

    2006-01-01

    In storage facilities one can find grain either in stored grain mass or in grain residues in the store corners or machinery. Although it is claimed that grain residues are serious pest reservoirs since they harbor numbers of stored product arthropods and are connected via continuous emigration with grain mass, the documentation for this is not convincing. Therefore in 78 selected grain stores, we simultaneously sampled the grain mass and residues in order to compare concurrent mite communities in these two different habitats. We found 30 species in about 614,000 individuals in residues and 23 species in about 20 000 individuals in grain mass. Canonical correspondence analysis (CCA) of transformed abundance data showed differences in the communities of mites in grain mass and residues: (i) species associated to grain residues (e.g. Tyrophagus longior, Tydeus interruptus, Acarus farris and Cheyletus eruditus) and (ii) species associated to both grain mass and grain residues (e.g. Tarsonemus granarius, Acarus siro, Tyrophagus putrescentiae, Lepidoglyphus destructor and Cheyletus malaccensis). Although the residue samples had more mites and higher species diversity than the stored grain mass, no correlation in mite abundance and species numbers between samples from grain residues and grain mass was found, thereby indicating low connectivity of these two habitats.

  15. Field desorption mass spectrometric analysis of organic compound residues in the environment. I--Organochlorine insecticides.

    Science.gov (United States)

    Suzuki, M; Yamato, Y; Koga, M

    1978-09-01

    Field desorption mass spectrometry is applied to the positive identification of organochlorine insecticides and their related compounds residing in field soil environment. Additionally, standard field desorption mass spectra of these compounds are presented. Soil samples were collected in lettuce and spinach fields, and insecticides were extracted, cleaned up, and separated with thin-layer chromatography. Residue levels were measured by injecting the extract into a gas chromatography equipped with an electron capture detector. Residues of p,p'-DDT and dieldrin in field soil samples were clearly identified by field desorption mass spectrometry using the emitter dipping method. Moreover, mixed residues of these insecticides were simultaneously confirmed. However, residues of insecticides and their related compounds other than p,p'-DDT and dieldrin could not be characterized. All spectra of standard showed prominent [M].+, [M(35Cl(n-1), 37Cl)].+ and [M(35Cl(n-2, 37Cl2)].+ ions, and the [M(35Cl(n-1), 37Cl)].+ ion was the base peak in all spectra obtained.

  16. Amphoteric surfactants containing ?-hydroxy ester group and an amino acid residue

    Directory of Open Access Journals (Sweden)

    Eissa, A. M. F.

    2006-09-01

    Full Text Available A series of amphoteric surfactants containing α-hydroxy ester group and an amino acid residue were prepared with the addition of epoxy derivatives (which were prepared from epoxidation of alkyl methacrylate to different types of amino acids (glycine, alanine, valine, isoleucine, phenylalanine, tyrosine, serine, threonine, aspartic and anthranilic acid.The structures of the prepared compounds were confirmed by infrared spectra, proton magnetic resonance spectra, Mass spectra and elementary analysis. Surface tension, Kraft point, foaming power, critical micelle concentration emulsion and Ca++ stabilities were determined. Antimicrobial activity and biodegradability were also screened.Se prepararon una serie de tensioactivos anfóteros conteniendo un grupo alfa hidroxi éster y un residuo de aminoácido por adición de derivados epoxy (obtenidos mediante epoxidación de metacrilato de alquilo a diferentes tipos de aminoácidos (glicina, alanina, valina, isoleucina, fenilalanina, tirosina, serina, treonina y ácidos aspártico y antranílico. Las estructuras de los compuestos preparados se confirmaron por los espectros de infrarrojo, de masa, resonancia magnética nuclear de protones y análisis elemental. Se determinaron la tensión superficial, el punto de Kraft, el poder espumante, la concentración micelar crítica en emulsión y las estabilidades de Ca++. También se estudiaron la actividad antimicrobiana y la biodegradabilidad.

  17. Effects of the application of different particle sizes of mill scale (residue) in mass red ceramic

    International Nuclear Information System (INIS)

    Arnt, A.B.C.; Rocha, M.R.; Meller, J.G.

    2012-01-01

    This study aims to evaluate the influence of particle size of mill scale, residue, when added to a mass ceramic. This residue rich in iron oxide may be used as pigment in the ceramics industry. The use of pigments in ceramic products is related to the characteristics of non-toxicity, chemical stability and determination of tone. The tendency to solubilize the pigment depends on the specific surface area. The residue study was initially subjected to physical and chemical characterization and added in a proportion of 5% at a commercial ceramic white burning, with different particle sizes. Both formulations were sintered at a temperature of 950 ° C and evaluated for: loss on ignition, firing linear shrinkage, water absorption, flexural strength and difference of tone. Samples with finer particles of mill scale 0.038 μ showed higher mechanical strength values in the order of 18 MPa. (author)

  18. Minimal Residual Disease and Childhood Leukemia: Standard of Care Recommendations From the Pediatric Oncology Group of Ontario MRD Working Group.

    Science.gov (United States)

    Athale, Uma H; Gibson, Paul J; Bradley, Nicole M; Malkin, David M; Hitzler, Johann

    2016-06-01

    Minimal residual disease (MRD) is an independent predictor of relapse risk in children with leukemia and is widely used for risk-adapted treatment. This article summarizes current evidence supporting the use of MRD, including clinical significance, current international clinical practice, impact statement, and recommended indications. The proposed MRD recommendations have been endorsed by the MRD Working Group of the Pediatric Oncology Group of Ontario and provide the foundation for a strategy that aims at equitable access to MRD evaluation for children with leukemia. © 2016 Wiley Periodicals, Inc.

  19. Controlling residual hydrogen gas in mass spectra during pulsed laser atom probe tomography.

    Science.gov (United States)

    Kolli, R Prakash

    2017-01-01

    Residual hydrogen (H 2 ) gas in the analysis chamber of an atom probe instrument limits the ability to measure H concentration in metals and alloys. Measuring H concentration would permit quantification of important physical phenomena, such as hydrogen embrittlement, corrosion, hydrogen trapping, and grain boundary segregation. Increased insight into the behavior of residual H 2 gas on the specimen tip surface in atom probe instruments could help reduce these limitations. The influence of user-selected experimental parameters on the field adsorption and desorption of residual H 2 gas on nominally pure copper (Cu) was studied during ultraviolet pulsed laser atom probe tomography. The results indicate that the total residual hydrogen concentration, H TOT , in the mass spectra exhibits a generally decreasing trend with increasing laser pulse energy and increasing laser pulse frequency. Second-order interaction effects are also important. The pulse energy has the greatest influence on the quantity H TOT , which is consistently less than 0.1 at.% at a value of 80 pJ.

  20. The Higgs mass derived from the U(3) Lie group

    DEFF Research Database (Denmark)

    Trinhammer, Ole; Bohr, Henrik; Jensen, Mogens O Stibius

    2015-01-01

    The Higgs mass value is derived from a Hamiltonian on the Lie group U(3) where we relate strong and electroweak energy scales. The baryon states of nucleon and delta resonances originate in specific Bloch wave degrees of freedom coupled to a Higgs mechanism which also gives rise to the usual gauge...... in scattering cross-sections for negative pions on protons, in photoproduction on neutrons, in neutron diffraction dissociation experiments and in invariant mass spectra of protons and negative pions in B-decays. The fundamental predictions are based on just one length scale and the fine structure constant...

  1. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Science.gov (United States)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Bro¿żek-Mucha, Z.; Biegstraaten, J.; Horváth, R.

    2007-09-01

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  2. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    International Nuclear Information System (INIS)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Brozek-Mucha, Z.; Biegstraaten, J.; Horvath, R.

    2007-01-01

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification

  3. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Steffen, S. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Otto, M. [TU Bergakademie Freiberg (TU BAF), Institute for Analytical Chemistry, Leipziger Str. 29, D - 09599 Freiberg (Germany)], E-mail: matthias.otto@chemie.tu-freiberg.de; Niewoehner, L.; Barth, M. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Brozek-Mucha, Z. [Instytut Ekspertyz Sadowych (IES), Westerplatte St. 9, PL - 31-033 Krakow (Poland); Biegstraaten, J. [Nederlands Forensisch Instituut (NFI), Fysische Technologie, Laan van Ypenburg 6, NL-2497 GB Den Haag (Netherlands); Horvath, R. [Kriminalisticky a Expertizny Ustav (KEU PZ), Institute of Forensic Science, Sklabinska 1, SK - 812 72 Bratislava (Slovakia)

    2007-09-15

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  4. Extended scaling and residual flavor symmetry in the neutrino Majorana mass matrix

    Energy Technology Data Exchange (ETDEWEB)

    Samanta, Rome; Ghosal, Ambar [Saha Institute of Nuclear Physics, HBNI, Astroparticle Physics and Cosmology Division, Kolkata (India); Roy, Probir [Bose Institute, Center for Astroparticle Physics and Space Science, Kolkata (India)

    2016-12-15

    The residual symmetry approach, along with a complex extension for some flavor invariance, is a powerful tool to uncover the flavor structure of the 3 x 3 neutrino Majorana mass matrix M{sub ν} toward gaining insights into neutrino mixing. We utilize this to propose a complex extension of the real scaling ansatz for M{sub ν} which was introduced some years ago. Unlike the latter, our proposal allows a nonzero mass for each of the three light neutrinos as well as a nonvanishing θ{sub 13}. The generation of light neutrino masses via the type-I seesaw mechanism is also demonstrated. A major result of this scheme is that leptonic Dirac CP-violation must be maximal while atmospheric neutrino mixing does not need to be exactly maximal. Moreover, each of the two allowed Majorana phases, to be probed by the search for nuclear 0νββ decay, has to be at one of its two CP-conserving values. There are other interesting consequences such as the allowed occurrence of a normal mass ordering which is not favored by the real scaling ansatz. Our predictions will be tested in ongoing and future neutrino oscillation experiments at T2K, NOνA and DUNE. (orig.)

  5. Screening and confirmation criteria for hormone residue analysis using liquid chromatography accurate mass time-of-flight, Fourier transform ion cyclotron resonance and orbitrap mass spectrometry techniques

    NARCIS (Netherlands)

    Nielen, M.W.F.; Engelen, M.C. van; Zuiderent, R.; Ramaker, R.

    2007-01-01

    An emerging trend is recognised in hormone and veterinary drug residue analysis from liquid chromatography tandem mass spectrometry (LC/MS/MS) based screening and confirmation towards accurate mass alternatives such as LC coupled with time-of-flight (TOF), Fourier transform ion cyclotron resonance

  6. Long-term follow-up of residual mediastinal masses in treated Hodgkin's disease using MR imaging

    International Nuclear Information System (INIS)

    Nyman, R.; Forsgren, G.; Glimelius, B.

    1995-01-01

    Ten patients, with substantial residual mediastinal masses of low signal intensity (SI) in the T2-weighted image (T2WI), were reinvestigated with MR 19-79 months after completing treatment of Hodgkin's disease. All patients were in complete remission. During the follow-up period, the masses had decreased in size by 0-95% (median 67%) as compared to their initial post-therapy size. The SI continued to be low in the T2WI and was unaffected by the degree of size reduction. It is speculated that these mainly fibrotic residual masses undergo slow degradation of the fibrotic part and/or resorption of remaining inflammatory tissue. It is important to understand the natural, long-term MR imaging changes of these residual masses in order more easily to recognize tumour recurrence or other pathologic conditions. (orig.)

  7. Supervised multivariate analysis of sequence groups to identify specificity determining residues

    Directory of Open Access Journals (Sweden)

    Higgins Desmond G

    2007-04-01

    Full Text Available Abstract Background Proteins that evolve from a common ancestor can change functionality over time, and it is important to be able identify residues that cause this change. In this paper we show how a supervised multivariate statistical method, Between Group Analysis (BGA, can be used to identify these residues from families of proteins with different substrate specifities using multiple sequence alignments. Results We demonstrate the usefulness of this method on three different test cases. Two of these test cases, the Lactate/Malate dehydrogenase family and Nucleotidyl Cyclases, consist of two functional groups. The other family, Serine Proteases consists of three groups. BGA was used to analyse and visualise these three families using two different encoding schemes for the amino acids. Conclusion This overall combination of methods in this paper is powerful and flexible while being computationally very fast and simple. BGA is especially useful because it can be used to analyse any number of functional classes. In the examples we used in this paper, we have only used 2 or 3 classes for demonstration purposes but any number can be used and visualised.

  8. Profiling the effects of process changes on residual host cell proteins in biotherapeutics by mass spectrometry.

    Science.gov (United States)

    Schenauer, Matthew R; Flynn, Gregory C; Goetze, Andrew M

    2013-01-01

    An advanced liquid chromatography/mass spectrometry (MS) platform was used to identify and quantify residual Escherichia coli host cell proteins (HCPs) in the drug substance (DS) of several peptibodies (Pbs). Significantly different HCP impurity profiles were observed among different biotherapeutic Pbs as well as one Pb purified via multiple processes. The results can be rationally interpreted in terms of differences among the purification processes, and demonstrate the power of this technique to sensitively monitor both the quantity and composition of residual HCPs in DS, where these may represent a safety risk to patients. The breadth of information obtained using MS is compared to traditional multiproduct enzyme-linked immunosorbent assay (ELISA) values for total HCP in the same samples and shows that, in this case, the ELISA failed to detect multiple HCPs. The HCP composition of two upstream samples was also analyzed and used to demonstrate that HCPs that carry through purification processes to be detectable in DS are not always among those that are the most abundant upstream. Compared to ELISA, we demonstrate that MS can provide a more comprehensive, and accurate, characterization of DS HCPs, thereby facilitating process development as well as more rationally assessing potential safety risks posed by individual, identified HCPs. © 2013 American Institute of Chemical Engineers.

  9. TECHNOLOGICAL TESTS USING QUARTZITE RESIDUES AS COMPONENT OF CERAMIC MASS AT THE PORCELAIN STONEWARE PRODUCTION

    Directory of Open Access Journals (Sweden)

    Marcondes Mendes Souza

    2015-03-01

    Full Text Available This work aims to evaluate through technological tests the use of quartzite residues as component at the the production of porcelain stoneware. Were collected five samples of quartzites called of green quartzite, black quartzite, pink quartzite, goldy quartzite, white quartzite. After, the raw materials were milled, passed by a sieve with a Mesh of 200# (Mesh and characterized by chemical analysis in fluorescence of x-rays and also analysis of the crystalline phases by diffraction of x-rays. The porcelain tiles mass is composed of five formulations containing 57% of feldspar, 37% of clay and 6% of residues of quartzite with different coloration. For the preparation of the specimens, it was used uniaxial pressing, which afterwards were synthesized at 1150°C, 1200°C and 1250°C. After the sintering, the specimens were submit for tests of technological characterization like: water absorption, linear shrinkage, apparently porosity, density and flexural strain at three points. The results presented in the fluorescence of x-rays showed a high-content of iron oxide on black quartzite that is why it was discarded the utilization of it in porcelain stoneware. All quartzite formulations had low water absorption achieved when synthesized at 1200°C, getting 0.1 to 0.36% without having gone through the atomization process. At the tests of flexural strain, all the quartzite had in acceptance limits, according to the European norm EN 100, overcoming 27 MPA at 1200°C

  10. Protein hydrogen exchange measured at single-residue resolution by electron transfer dissociation mass spectrometry

    DEFF Research Database (Denmark)

    Rand, Kasper D; Zehl, Martin; Jensen, Ole Nørregaard

    2009-01-01

    Because of unparalleled sensitivity and tolerance to protein size, mass spectrometry (MS) has become a popular method for measuring the solution hydrogen (1H/2H) exchange (HX) of biologically relevant protein states. While incorporated deuterium can be localized to different regions by pepsin...... proteolysis of the labeled protein, the assignment of deuteriums to individual residues is typically not obtained, thereby limiting a detailed understanding of HX and the dynamics of protein structure. Here we use gas-phase fragmentation of peptic peptides by electron transfer dissociation (ETD) to measure...... the HX of individual amide linkages in the amyloidogenic protein beta2-microglobulin. A comparison of the deuterium levels of 60 individual backbone amides of beta2-microglobulin measured by HX-ETD-MS analysis to the corresponding values measured by NMR spectroscopy shows an excellent correlation...

  11. Evaluation of nanoflow liquid chromatography high resolution mass spectrometry for pesticide residue analysis in food.

    Science.gov (United States)

    Moreno-González, David; Pérez-Ortega, Patricia; Gilbert-López, Bienvenida; Molina-Díaz, Antonio; García-Reyes, Juan F; Fernández-Alba, Amadeo R

    2017-08-25

    This article reports on the evaluation of nanoflow liquid chromatography-mass spectrometry (LC-MS) for pesticide residue analysis in food. The approach is based on the use of reversed-phase C18nano columns with an integrated emitter, so that separation, ionization and detection are performed minimizing dead volumes. The use of nanoflow not only increases ionization efficiency and minimizes ionization suppression but also boost sensitivity compared to analytical-scale LC-MS methods. The nanoflow LC system was combined with full-scan high resolution mass spectrometry using a Q-Exactive Orbitrap instrument. The analytical performance was assessed for over 60 representative pesticides in five representative commodities (tomato, baby food, orange, fruit-based jam and olive oil). The sensitivity achieved with this configuration enables the implementation of high dilution factors (eg. 1:20, 1:50 or beyond) in pesticide residue workflows without compromising sensitivity, featuring limits of quantitation in the low ng kg -1 range. Using this dilution factors, signal suppression was found negligible in most cases (<10% in most cases, especially with 1:50 dilution), so that matrix-matched standards may be skipped, thus simplifying laboratory workflows. The robustness of the nanoflow LC system and its capability to withstand long analytical runs was also evaluated. Appropriate precision in terms of peak area and retention time was obtained at different concentration levels for over 125 injections without any instrument servicing. The main benefits of the nanoflow liquid chromatography approach are the high sensitivity gain and the outstanding reduction in matrix effects thanks to the high sample dilution factors that can be implemented, along with the substantial reduction in solvent usage. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Renormalization group analysis of the gluon mass equation

    Science.gov (United States)

    Aguilar, A. C.; Binosi, D.; Papavassiliou, J.

    2014-04-01

    We carry out a systematic study of the renormalization properties of the integral equation that determines the momentum evolution of the effective gluon mass in pure Yang-Mills theory, without quark effects taken into account. A detailed, all-order analysis of the complete kernel appearing in this particular equation, derived in the Landau gauge, reveals that the renormalization procedure may be accomplished through the sole use of ingredients known from the standard perturbative treatment of the theory, with no additional assumptions. However, the subtle interplay of terms operating at the level of the exact equation gets distorted by the approximations usually employed when evaluating the aforementioned kernel. This fact is reflected in the form of the obtained solutions, for which the deviations from the correct behavior are best quantified by resorting to appropriately defined renormalization-group invariant quantities. This analysis, in turn, provides a solid guiding principle for improving the form of the kernel, and furnishes a well-defined criterion for discriminating between various possibilities. Certain renormalization-group inspired Ansätze for the kernel are then proposed, and their numerical implications are explored in detail. One of the solutions obtained fulfills the theoretical expectations to a high degree of accuracy, yielding a gluon mass that is positive definite throughout the entire range of physical momenta, and displays in the ultraviolet the so-called "power-law" running, in agreement with standard arguments based on the operator product expansion. Some of the technical difficulties thwarting a more rigorous determination of the kernel are discussed, and possible future directions are briefly mentioned.

  13. Outcome of residual mediastinal masses of thoracic lymphomas in children: impact on management and radiological follow-up strategy

    International Nuclear Information System (INIS)

    Brisse, H.; Pacquement, H.; Burdairon, E.; Plancher, C.; Neuenschwander, S.

    1998-01-01

    Background. Following treatment with chemotherapy and radiotherapy, patients with thoracic lymphomas may demonstrate benign residual mediastinal masses, composed of inflammatory, fibrous or necrotic tissue. Because of the potential risk of viable tumour cells within the mass, histological verification of the nature of these masses may be requested. Objective. To study the outcome of thoracic lymphomas in children in order to optimise the radiological follow-up strategy of residual mediastinal masses (RMM). Materials and methods. A retrospective study of 39 children [24 with Hodgkin's disease (HD), 10 with non-Hodgkin's lymphoma (NHL), and 5 with anaplastic lymphoma (AL)]. The results of chest X-rays (CXR) and thoracic CT performed at the time of re-assessment were compared with the histology of the residual masses (n = 11) or the clinical course (n = 28). Results. At the time of re-evaluation, 16/39 patients had residual mediastinal enlargement (RME) on CXR, and 18/39 patients had RMM on CT. Good concordance was observed between the two imaging modalities (K = 0.69). Two children with a RMM died from extra-mediastinal progression. Two children with NHL had active residual mediastinal lesions but neither had RMM. Sixteen cases of RMM were observed in the remaining 35 children and 9 of these masses were histologically verified as benign. A favourable course was observed in these 35 cases. Conclusions. RMM are frequent and generally benign. They are well shown on CXR and have a non-specific appearance on CT. Except when required by a treatment protocol, they could be submitted to further radiological follow-up before contemplating surgical verification. (orig.)

  14. Use of the extraction residue of emeralds in a formulation mass of ceramic tiles

    International Nuclear Information System (INIS)

    Cavalcante, R. F.; Nascimento, R.M.; Paskocimas, C.A.; Dutra, R.P.S.

    2012-01-01

    Companies involved in mining and beneficiation of emerald represent an important area of industrial development in Brazil, with a significant contribution to world production of this ore. As a result, large volumes of waste generated and emerald are constantly abandoned in the environment, contributing negatively to their preservation. On the other hand the interest in the use of mining waste as an additive in production of ceramic materials has grown among researchers in recent years. The ceramic industry is constantly seeking to expand the market for the sector and trying to improve product quality and increase the variety of applications. The technology of obtaining ceramic coating that uses waste from mining is still a largely unexplored market. Thus, the purpose of this study was to characterize the waste generated from mining emerald as well as to evaluate its potential use as raw material for production melting of ceramic tiles. Ceramic mixtures were prepared from raw materials characterized by X-ray fluorescence and X-ray diffraction. Five compositions were prepared using the waste codes of emeralds from 0%, 10%, 20%, 30% and 40%. Samples were prepared by pressing, sintered at 1000, 1100 and 1200 deg C and characterized to establish their mineralogical composition, water absorption, linear shrinkage and modulus of rupture. The results showed that the residue of emeralds studied can be embedded in the mass of ceramic tiles up to 20% in replacement of feldspar without compromising the end product properties. (author)

  15. Prediction of Gas Chromatography-Mass Spectrometry Retention Times of Pesticide Residues by Chemometrics Methods

    Directory of Open Access Journals (Sweden)

    Elaheh Konoz

    2013-01-01

    Full Text Available A quantitative structure-retention relationships (QSRRs method is employed to predict the retention time of 300 pesticide residues in animal tissues separated by gas chromatography-mass spectroscopy (GC-MS. Firstly, a six-parameter QSRR model was developed by means of multiple linear regression. The six molecular descriptors that were considered to account for the effect of molecular structure on the retention time are number of nitrogen, Solvation connectivity index-chi 1, Balaban Y index, Moran autocorrelation-lag 2/weighted by atomic Sanderson electronegativity, total absolute charge, and radial distribution function-6.0/unweighted. A 6-7-1 back propagation artificial neural network (ANN was used to improve the accuracy of the constructed model. The standard error values of ANN model for training, test, and validation sets are 1.559, 1.517, and 1.249, respectively, which are less than those obtained reveals by multiple linear regressions model (2.402, 1.858, and 2.036, resp.. Results obtained the reliability and good predictability of nonlinear QSRR model to predict the retention time of pesticides.

  16. The Effect of Welding-Pass Grouping on the Prediction Accuracy of Residual Stress in Multipass Butt Welding

    Directory of Open Access Journals (Sweden)

    Jeongung Park

    2017-01-01

    Full Text Available The residual stress analysis of a thick welded structure requires a lot of time and computer memory, which are different from those in thin welded structure analysis. This study investigated the effect of residual stress due to welding-pass grouping as a way to reduce the analysis time in multipass thick butt welding joint. For this purpose, the parametric analysis which changes the number of grouping passes was conducted in the multipass butt weld of a structure with a thickness of 25 mm and 70 mm. In addition, the residual stress by thermal elastoplastic FE analysis is compared with the results by the neutron diffraction method for verifying the reliability of the FE analysis. The welding sequence is considered in order to predict the residual stress more accurately when using welding-pass grouping method. The results of the welding-pass grouping model and half model occurred between the results of the left/right of the full model. If the total number of welding-pass grouping is less than half of that of welding pass, a large difference with real residual stress is found. Therefore, the total number of the welding-pass grouping should not be reduced to more than half.

  17. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review.

    Science.gov (United States)

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. EPA Selects Lawrence, Mass. Group for Brownfields Job Training Grant

    Science.gov (United States)

    Today, EPA announced that the Merrimack Valley Workforce Investment Board, of Lawrence, Mass., was one of 14 organizations nationwide selected to receive funding to operate environmental job training programs for local unemployed residents.

  19. Predictors of viable germ cell tumor in postchemotherapeutic residual retroperitoneal masses

    Directory of Open Access Journals (Sweden)

    Khalid Al Othman

    2014-01-01

    Full Text Available Objective: The aim of this study was to identify predictors of viable germ cell tumor (GCT in postchemotherapeutic residual retroperitoneal masses. Materials and Methods: The pertinent clinical and pathologic data of 16 male patients who underwent postchemotherapeutic retroperitoneal lymph node dissection (PC-RPLND at King Faisal Specialist Hospital and Research Centre between 1994 and 2005 were reviewed retrospectively. It was found that all patients received cisplatin-based chemotherapy for advanced testicular GCT. Results: Out of the 16 male patients, 2 (13%, 8 (50%, and 6 (37% had viable GCT, fibrosis, and teratoma, respectively. Ten (10 of the patients with prechemotherapeutic S1 tumor markers did not have viable GCT, and two of the six patients who had prechemotherapeutic S2 tumor markers have viable GCT. All tumor marker levels normalized after chemotherapy even in patients with viable GCT. Four patients had vascular invasion without viable GCT. Furthermore, four patients had more than 60% embryonal elements in the original pathology, but only 1 had viable GCT at PC-RPLND. Four of the five patients with immature teratoma had teratoma at PC-RPLND but no viable GCT; however, out of the four patients with mature teratoma, one had viable GCT and two had teratoma at PC-RPLND. Of the two patients with viable GCT, one had 100% embryonal cancer in the original pathology, prechemotherapeutic S2 tumor markers, history of orchiopexy, and no vascular invasion; the other patient had yolk sac tumor with 25% embryonal elements and 40% teratoma in the original pathology, and prechemotherapeutic S2 tumor markers. Conclusion: None of the clinical or pathological parameters showed a strong correlation with the presence of viable GCT in PC-RPLND. However, patients with ≥S2 may be at higher risk to have viable GCT. Further studies are needed to clarify this.

  20. Multi-residue method for the confirmation of four avermectin residues in food products of animal origin by ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wang, Fengmei; Chen, Junhui; Cheng, Hongyan; Tang, Zhixu; Zhang, Gang; Niu, Zengyuan; Pang, Shiping; Wang, Xiaoru; Lee, Frank Sen-Chun

    2011-05-01

    A confirmatory method was developed for the rapid determination of abamectin, ivermectin, doramectin and eprinomectin residues in various food products of animal origin, such as pork muscle, pork liver, fish and milk. Samples were homogenized, extracted and de-proteinized by acetonitrile, cleaned via two-step cleaning procedure using Bond Elut C(18) SPE columns and then alumina-N cartridges. All the four avermectin residues in different animal-food products were simultaneously separated and determined by ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) within 3.5 min. Data acquisition under positive ESI-MS/MS was performed by applying multiple reaction monitoring (MRM) for both identification and quantification, and mass spectrometric conditions were optimized to increase selectivity and sensitivity. The matrix-matched calibration curves for different matrices, such as pork muscle, pork liver, fish and milk, were constructed and the interference effect of different sample matrices on the ionization was effectively eliminated. The UPLC-MS/MS method was validated with satisfactory linearity, recovery, precision and stability. Matrix-matched calibration curves of abamectin, ivermectin, doramectin and eprinomectin in four different matrices were linear (r(2)( )≥ 0.990, goodness-of-fit coefficients ≤12.8%) in the range 2.5-200 µg kg(-1). The limits of detection and quantification for the four avermectins were in the range 0.05-0.68 and 0.17-2.27 µg kg(-1), respectively. Recoveries were 62.4-104.5% with good intra- and inter-day precision. The method was rapid, sensitive and reliable, and can be applied to the quantitative analysis of avermectin residues in different animal-food products.

  1. Trace metal occurrences in acid-insoluble residues of the Ordovician Galena Group, southeastern Minnesota

    Energy Technology Data Exchange (ETDEWEB)

    Lively, R.S.; Mossler, J.H.; Morey, G.B. (Minnesota Geological Survey, St. Paul, MN (United States)); Hauck, S.A. (Univ. of Minnesota, Duluth, MN (United States). Natural Resources Research Inst.)

    1993-03-01

    Regional geochemical, studies on insoluble residues from Paleozoic carbonate rocks have become an integral part of the search for new Upper Mississippi Valley-type mineral deposits in the northern Midcontinent. The authors have extended these studies to southeastern Minnesota, an area well to the north of known lead-zinc deposits of commercial size and grade. In this region, a thin sequence of Upper Cambrian to Middle Ordovician strata unconformably overlies a complex Precambrian basement. More than 500 samples of limestone and dolomite from 40 drill holes and outcrops were analyzed for 29 related trace elements. Preliminary interpretations are based on the analysis of 380 samples of the Ordovician Galena Group from 37 localities. Results indicate that anomalous concentrations of Pb, Cu, zn, As, Cd, and Ni are confined to the southern half of the Galena subgroup area and extend less than 30 miles north of the Iowa border. The anomalous areas, as well as saddles between the, have a distinct northwest trend, coincident with structural features previously recognized in the Precambrian basement. The spatial relationships of the anomalies and the lack of direct correlation imply deposition from fluids moving north out of the main lead-zinc district along structural pathways. The lack of significant anomalies in the northern part of the subcrop area implies northwest weakening of the forces driving the metal-bearing fluids, as well as a decrease over distance in the absolute metal content of the migrating fluids.

  2. Evaluation of gas chromatography – electron ionization – full scan high resolution Orbitrap mass spectrometry for pesticide residue analysis

    Energy Technology Data Exchange (ETDEWEB)

    Mol, Hans G.J., E-mail: hans.mol@wur.nl; Tienstra, Marc; Zomer, Paul

    2016-09-07

    Gas chromatography with electron ionization and full scan high resolution mass spectrometry with an Orbitrap mass analyzer (GC-EI-full scan Orbitrap HRMS) was evaluated for residue analysis. Pesticides in fruit and vegetables were taken as an example application. The relevant aspects for GC-MS based residue analysis, including the resolving power (15,000 to 120,000 FWHM at m/z 200), scan rate, dynamic range, selectivity, sensitivity, analyte identification, and utility of existing EI-libraries, are assessed and discussed in detail. The optimum acquisition conditions in full scan mode (m/z 50–500) were a resolving power of 60,000 and an automatic-gain-control target value of 3E6. These conditions provided (i) an optimum mass accuracy: within 2 ppm over a wide concentration range, with/without matrix, enabling the use of ±5 ppm mass extraction windows (ii) adequate scan speed: minimum 12 scans/peak, (iii) an intra-scan dynamic range sufficient to achieve LOD/LOQs ≤0.5 pg in fruit/vegetable matrices (corresponding to ≤0.5 μg kg{sup −1}) for most pesticides. EI-Orbitrap spectra were consistent over a very wide concentration range (5 orders) with good match values against NIST (EI-quadrupole) spectra. The applicability for quantitative residue analysis was verified by validation of 54 pesticides in three matrices (tomato, leek, orange) at 10 and 50 μg/kg. The method involved a QuEChERS-based extraction with a solvent switch into iso-octane, and 1 μL hot splitless injection into the GC-HRMS system. A recovery between 70 and 120% and a repeatability RSD <10% was obtained in most cases. Linearity was demonstrated for the range ≤5–250 μg kg{sup −1}. The pesticides could be identified according to the applicable EU criteria for GC-HRMS (SANTE/11945/2015). GC-EI-full scan Orbitrap HRMS was found to be highly suited for quantitative pesticide residue analysis. The potential of qualitative screening to extend the scope makes it an attractive

  3. [Determination of residual mass in left ventricle by intraoperative transesophageal echocardiography after a giant and floating left atrial myxoma resection].

    Science.gov (United States)

    Kavakli, Ali Sait; Kavrut Ozturk, Nilgun

    2017-12-20

    Atrial myxoma is a benign tumor of the heart that occurs primarily in the left atrium. Floating or large left atrial myxomas frequently cause functional mitral stenosis, may also affect mitral valve structure and flow, and lead to mitral regurgitation. Systemic embolization occurs in around 30% of cases either from tumor fragmentation or complete tumor detachment hence it should be removed as soon as it is detected. Intraoperative transesophageal echocardiography has a vital importance in the surgery. After resection of myxoma, intraoperative transesophageal echocardiography must be performed to rule out residual mass. The case here reported is of a 48-year old female, who presented with giant and floating left atrial myxoma. Residue mass was detected with intraoperative transesophageal echocardiography in the left ventricle after the resection of myxoma. Subsequently, the residue mass was successfully removed. Complete resection must be required to prevent possible complications such as recurrence, embolization in atrial myxomas. Transesophageal echocardiography performed intraoperatively is vital importance to confirm that the myxoma is completely resected. Copyright © 2017 Sociedade Brasileira de Anestesiologia. Publicado por Elsevier Editora Ltda. All rights reserved.

  4. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Masiá, Ana [Food and Environmental Safety Research Group, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); Research Center on Desertification (CIDE, UV-CSIC-GV), Carretera Moncada-Náquera, Moncada (Spain); Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin [Unit of Public Health, Hygiene and Environmental Health, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); CIBER Epidemiología y Salud Pública (CIBERESP), Madrid (Spain); Center for Advanced Research in Public Health (CSISP-FISABIO), Valencia (Spain); Picó, Yolanda, E-mail: Yolanda.Pico@uv.es [Food and Environmental Safety Research Group, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); Research Center on Desertification (CIDE, UV-CSIC-GV), Carretera Moncada-Náquera, Moncada (Spain); CIBER Epidemiología y Salud Pública (CIBERESP), Madrid (Spain)

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. - Highlights: • An overview of status and future trends in this field. • Analytical method's compliance with guidelines to ensure reliability. • QuEChERS platform is a referent to extract both, pesticides and veterinary drugs in food. • The progress that liquid chromatography has shown in recent years is revised. • Determination of target, non-target and unknowns is

  5. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review

    International Nuclear Information System (INIS)

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-01-01

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. - Highlights: • An overview of status and future trends in this field. • Analytical method's compliance with guidelines to ensure reliability. • QuEChERS platform is a referent to extract both, pesticides and veterinary drugs in food. • The progress that liquid chromatography has shown in recent years is revised. • Determination of target, non-target and unknowns is

  6. Hydrothermal carbonization of biomass residues: mass spectrometric characterization for ecological effects in the soil-plant system.

    Science.gov (United States)

    Jandl, Gerald; Eckhardt, Kai-Uwe; Bargmann, Inge; Kücke, Martin; Greef, Jörg-Michael; Knicker, Heike; Leinweber, Peter

    2013-01-01

    Hydrochars, technically manufactured by hydrothermal carbonization (HTC) of biomass residues, are recently tested in high numbers for their suitability as feedstock for bioenergy production, the bioproduct industry, and as long-term carbon storage in soil, but ecological effects in the soil-plant system are not sufficiently known. Therefore, we investigated the influence of different biomass residues and process duration on the molecular composition of hydrochars, and how hydrochar addition to soils affected the germination of spring barley ( L.) seeds. Samples from biomass residues and the corresponding hydrochars were analyzed by pyrolysis-field ionization mass spectrometry (Py-FIMS) and gaseous emissions from the germination experiments with different soil-hydrochar mixtures by gas chromatography/mass spectrometry (GC/MS). The molecular-level characterization of various hydrochars by Py-FIMS clearly showed that the kind of biomass residue influenced the chemical composition of the corresponding hydrochars more strongly than the process duration. In addition to various detected possible toxic substances, two independent mass spectrometric methods (Py-FIMS and GC/MS) indicated long C-chain aliphatic compounds which are typically degraded to the C-unit ethylene that can evoke phytotoxic effects in high concentrations. This showed for the first time possible chemical compounds to explain toxic effects of hydrochars on plant growth. It is concluded that the HTC process did not result in a consistent product with defined chemical composition. Furthermore, possible toxic effects urgently need to be investigated for each individual hydrochar to assess effects on the soil organic matter composition and the soil biota before hydrochar applications as an amendment on agricultural soils. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  7. Histidine hydrogen-deuterium exchange mass spectrometry for probing the microenvironment of histidine residues in dihydrofolate reductase.

    Directory of Open Access Journals (Sweden)

    Masaru Miyagi

    2011-02-01

    Full Text Available Histidine Hydrogen-Deuterium Exchange Mass Spectrometry (His-HDX-MS determines the HDX rates at the imidazole C(2-hydrogen of histidine residues. This method provides not only the HDX rates but also the pK(a values of histidine imidazole rings. His-HDX-MS was used to probe the microenvironment of histidine residues of E. coli dihydrofolate reductase (DHFR, an enzyme proposed to undergo multiple conformational changes during catalysis.Using His-HDX-MS, the pK(a values and the half-lives (t(1/2 of HDX reactions of five histidine residues of apo-DHFR, DHFR in complex with methotrexate (DHFR-MTX, DHFR in complex with MTX and NADPH (DHFR-MTX-NADPH, and DHFR in complex with folate and NADP+ (DHFR-folate-NADP+ were determined. The results showed that the two parameters (pK(a and t(1/2 are sensitive to the changes of the microenvironment around the histidine residues. Although four of the five histidine residues are located far from the active site, ligand binding affected their pK(a, t(1/2 or both. This is consistent with previous observations of ligand binding-induced distal conformational changes on DHFR. Most of the observed pK(a and t(1/2 changes could be rationalized using the X-ray structures of apo-DHFR, DHFR-MTX-NADPH, and DHFR-folate-NADP+. The availability of the neutron diffraction structure of DHFR-MTX enabled us to compare the protonation states of histidine imidazole rings.Our results demonstrate the usefulness of His-HDX-MS in probing the microenvironments of histidine residues within proteins.

  8. Histidine hydrogen-deuterium exchange mass spectrometry for probing the microenvironment of histidine residues in dihydrofolate reductase.

    Science.gov (United States)

    Miyagi, Masaru; Wan, Qun; Ahmad, Md Faiz; Gokulrangan, Giridharan; Tomechko, Sara E; Bennett, Brad; Dealwis, Chris

    2011-02-16

    Histidine Hydrogen-Deuterium Exchange Mass Spectrometry (His-HDX-MS) determines the HDX rates at the imidazole C(2)-hydrogen of histidine residues. This method provides not only the HDX rates but also the pK(a) values of histidine imidazole rings. His-HDX-MS was used to probe the microenvironment of histidine residues of E. coli dihydrofolate reductase (DHFR), an enzyme proposed to undergo multiple conformational changes during catalysis. Using His-HDX-MS, the pK(a) values and the half-lives (t(1/2)) of HDX reactions of five histidine residues of apo-DHFR, DHFR in complex with methotrexate (DHFR-MTX), DHFR in complex with MTX and NADPH (DHFR-MTX-NADPH), and DHFR in complex with folate and NADP+ (DHFR-folate-NADP+) were determined. The results showed that the two parameters (pK(a) and t(1/2)) are sensitive to the changes of the microenvironment around the histidine residues. Although four of the five histidine residues are located far from the active site, ligand binding affected their pK(a), t(1/2) or both. This is consistent with previous observations of ligand binding-induced distal conformational changes on DHFR. Most of the observed pK(a) and t(1/2) changes could be rationalized using the X-ray structures of apo-DHFR, DHFR-MTX-NADPH, and DHFR-folate-NADP+. The availability of the neutron diffraction structure of DHFR-MTX enabled us to compare the protonation states of histidine imidazole rings. Our results demonstrate the usefulness of His-HDX-MS in probing the microenvironments of histidine residues within proteins.

  9. A multi-residue method for 17 anticoccidial drugs and ractopamine in animal tissues by liquid chromatography-tandem mass spectrometry and time-of-flight mass spectrometry.

    Science.gov (United States)

    Matus, Johanna L; Boison, Joe O

    2016-05-01

    A new and sensitive multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) and liquid chromatography-quadrupole time-of-flight-mass spectrometry (LC-QToF-MS) method was developed and validated for the determination and confirmation of residues of 17 anticoccidials, plus free ractopamine in poultry muscle and liver, and bovine muscle, liver, and kidney tissues. The 17 anticoccidials are lasalocid, halofuginone, narasin, monensin, semduramicin, ethopabate, robenidine, buquinolate, toltrazuril as its sulfone metabolite, maduramicin, salinomycin, diclazuril, amprolium, decoquinate, dinitolmide, clopidol, and the nicarbazin metabolite DNC (N,N1-bis(4-nitrophenyl)urea). The analytes were extracted and cleaned up within a 3-hour period by simply extracting the analytes into a solvent mixture with salts followed by centrifugation, dilution, and filtration. The validated method was used in a pilot study for the analysis of 173 samples that included quail liver, bovine kidney, liver, muscle, and horse muscle. The predominant residues found in this study were monensin, ractopamine, and lasalocid. The results of this pilot study showed that this new method is applicable to real samples, and is fit for use in a regulatory testing programme. © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis. © 2016 John Wiley & Sons, Ltd. © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis. © 2016 John Wiley & Sons, Ltd.

  10. Determination of 86 Pesticide Residues in Leafy Vegetables using gas Chromatography Mass Spectrometry

    OpenAIRE

    , M. T. Selim; , I. Al-Dossary

    2016-01-01

    A multiresidue method is described for detection and determination of 86 compounds of pesticide residues which commonly used in the pest control programs for crop protection. Good sensitivity and selectivity of the method are obtained with limits of quantiŞcation 0.01 mg/kg in almost all cases. The method was applied very satisfactorily to routine analysis as a complement to traditional GC-MS method and Şnally, limit of detection were also 10-20 times lower than maximum residue levels (MRL) e...

  11. Determination of chlorantraniliprole residues in crops by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry/mass spectrometry.

    Science.gov (United States)

    Grant, Joann; Rodgers, Carol A; Chickering, Clark D; Hill, Sidney J; Stry, James J

    2010-01-01

    An analytical method is presented for the determination of chlorantraniliprole residues in crops. Chlorantraniliprole residues were extracted from crop matrixes with acetonitrile after a water soak. The extracts were passed through a strong anion-exchange (SAX) SPE cartridge stacked on top of a reversed-phase (RP) polymer cartridge. After both cartridges were rinsed and vacuum-dried, the SAX cartridge was removed, and chlorantraniliprole was eluted from the RP polymer cartridge with acetonitrile. The acetonitrile eluate was evaporated to dryness, reconstituted, and analyzed using an LC/MS/MS instrument equipped with an atmospheric pressure chemical ionization source. The method was successfully validated at 0.010, 0.10, and 10 mg/kg for the following crop matrixes: potatoes, sugar beets (tops), lettuce, broccoli, soybeans, soybean forage, tomatoes, cucumbers, oranges, apples, pears, peaches, almonds (nutmeat), rice grain, wheat grain, wheat hay, corn stover, alfalfa forage, cottonseed, grapes, and corn grain. The average recoveries from all crop samples fortified at the method LOQ ranged from 91 to 108%, with an overall average recovery of 97%. The average recoveries from all crop samples fortified at 10 times the method LOQ ranged from 89 to 115%, with an overall average recovery of 101%. For all of the fortified control samples analyzed in this study, the overall average recovery was 99%.

  12. Multiclass methods for the analysis of antibiotic residues in milk by liquid chromatography coupled to mass spectrometry: A review.

    Science.gov (United States)

    Rossi, Rosanna; Saluti, Giorgio; Moretti, Simone; Diamanti, Irene; Giusepponi, Danilo; Galarini, Roberta

    2018-02-01

    Milk is an important and beneficial food from a nutritional point of view, being an indispensable source of high quality proteins. Furthermore, it is a raw material for many dairy products, such as yoghurt, cheese, cream etc. Before reaching consumers, milk goes through production, processing and circulation. Each step involves potentially unsafe factors, such as chemical contamination that can affect milk quality. Antibiotics are widely used in veterinary medicine for dry cow therapy and mastitis treatment in lactating cows, which can cause the presence of antimicrobial residues in milk. In order to ensure consumers' safety, milk is analyzed to make sure that the fixed Maximum Residue Limits (MRLs) for antibiotics are not exceeded. Multiclass methods can monitor more drug classes through a single analysis, so they are faster, less time-consuming and cheaper than traditional methods (single-class); this aspect is particularly important for milk, which is a highly perishable food. Nevertheless, multiclass methods for veterinary drug residues in foodstuffs are real analytical challenges. This article reviews the major multiclass methods published for the determination of antibiotic residues in milk by liquid chromatography coupled to mass spectrometry, with a special focus on sample preparation approaches.

  13. Multi-residue determination of plant growth regulators in apples and tomatoes by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Xue, Jiaying; Wang, Suli; You, Xiangwei; Dong, Jiannan; Han, Lijun; Liu, Fengmao

    2011-11-15

    A sensitive and rapid multi-residue analytical method for plant growth regulators (PGRs) (i.e., chlormequat, mepiquat, paclobutrazol, uniconazole, ethephon and flumetralin) in apples and tomatoes was developed using high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). A homogenised sample was extracted with a mixture of methanol/water (90:10, v/v) and adjusted to pH <3 with formic acid. Primary secondary amine (PSA) adsorbent was used to clean up the sample. The determination was performed using electrospray ionisation (ESI) and a triple quadrupole (QqQ) analyser. Under the optimised method, the results showed that, except for ethephon, the recoveries were 81.8-98.1% in apples and tomatoes at the spiked concentrations of 0.005 to 2 mg/kg, with relative standard deviations (RSDs) of less than 11.7%. The limits of quantification (LOQs) were lower than their maximum residue limits (MRLs). The procedure was concluded as a practical method to determine the PGR residues in fruit and vegetables and is also suitable for the simultaneous analysis of the amounts of samples for routine monitoring. The analytical method described herein demonstrates a strong potential for its application in the field of PGR multi-residue analysis to help assure food safety. Copyright © 2011 John Wiley & Sons, Ltd.

  14. Occurrence of C-Terminal Residue Exclusion in Peptide Fragmentation by ESI and MALDI Tandem Mass Spectrometry

    Science.gov (United States)

    Dupré, Mathieu; Cantel, Sonia; Martinez, Jean; Enjalbal, Christine

    2012-02-01

    By screening a data set of 392 synthetic peptides MS/MS spectra, we found that a known C-terminal rearrangement was unexpectedly frequently occurring from monoprotonated molecular ions in both ESI and MALDI tandem mass spectrometry upon low and high energy collision activated dissociations with QqTOF and TOF/TOF mass analyzer configuration, respectively. Any residue localized at the C-terminal carboxylic acid end, even a basic one, was lost, provided that a basic amino acid such arginine and to a lesser extent histidine and lysine was present in the sequence leading to a fragment ion, usually depicted as (bn-1 + H2O) ion, corresponding to a shortened non-scrambled peptide chain. Far from being an epiphenomenon, such a residue exclusion from the peptide chain C-terminal extremity gave a fragment ion that was the base peak of the MS/MS spectrum in certain cases. Within the frame of the mobile proton model, the ionizing proton being sequestered onto the basic amino acid side chain, it is known that the charge directed fragmentation mechanism involved the C-terminal carboxylic acid function forming an anhydride intermediate structure. The same mechanism was also demonstrated from cationized peptides. To confirm such assessment, we have prepared some of the peptides that displayed such C-terminal residue exclusion as a C-terminal backbone amide. As expected in this peptide amide series, the production of truncated chains was completely suppressed. Besides, multiply charged molecular ions of all peptides recorded in ESI mass spectrometry did not undergo such fragmentation validating that any mobile ionizing proton will prevent such a competitive C-terminal backbone rearrangement. Among all well-known nondirect sequence fragment ions issued from non specific loss of neutral molecules (mainly H2O and NH3) and multiple backbone amide ruptures (b-type internal ions), the described C-terminal residue exclusion is highly identifiable giving raise to a single fragment ion in

  15. Analysis of glyphosate residues in cereals using liquid chromatography-mass spectrometry (LC-MS/MS)

    DEFF Research Database (Denmark)

    Granby, Kit; Johannesen, S.; Gabrielsen, Martin Vahl

    2003-01-01

    monitored m/z 168--> 150 (glyphosate) and 170-->152 (internal standard 2- 13 (CN)-N-15-glyphosate) for quantification. The mean recovery was 85% ( n =32) at spiking levels from 0.03 to 0.33 mg kg(-1) . From 1998 to 2001, from the analysis of about 50 samples per annum, a reduction in the glyphosate residues...

  16. Detection of chloramphenicol residue in bovine meat using Liquid Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Widiastuti R

    2014-03-01

    Full Text Available Chloramphenicol (CAP is a broad spectrum antibiotic that has been banned in many countries due to its serius side effect to human. Detection of CAP residue in food has been determined to a minimum required performance limit (MRPL of 0.3 ng/g. The purpose of this research was to conduct the analysis of CAP residue in bovine meat by using LCMS and to study the presence of CAP residue in marketed bovine meat samples. LC separation was done on a Shimpack column C18 with ammonium acetate 10 mM/water as mobile phase, and ESI-MS analysis in negative ion mode. The coefficient of determination, R2 = 0.9981 at concentration of 0.125, 0.25, 0.63, 1,00 and 2.00 ng/g. Recovery at three fortification levels (0.25, 0.50 and 1.00 ng/g was in the range 77.5, 97.3 and 83.4%. The decision limit and the detection capability were 0.15 ng/g and 0.17 ng/g respectively. Analysis results of 52 marketed samples showed that CAP residue were detected in 9 samples in the concentration range of 0.14 to 2.70 ng/g and 6 among those positive samples were above the MRPL value. Therefore, it is important to increase the awareness and also to monitor regularly CAP residues in food originated from animal to provide safe food for the consumers.

  17. Uncertainty assessment of gamma-aminobutyric acid concentration of different brain regions in individual and group using residual bootstrap analysis.

    Science.gov (United States)

    Chen, Meng; Liao, Congyu; Chen, Song; Ding, Qiuping; Zhu, Darong; Liu, Hui; Yan, Xu; Zhong, Jianhui

    2017-06-01

    The aim of this work is to quantify individual and regional differences in the relative concentration of gamma-aminobutyric acid (GABA) in human brain with in vivo magnetic resonance spectroscopy. Spectral editing Mescher-Garwood point resolved spectroscopy (MEGA-PRESS) sequence and GABA analysis toolkit (Gannet) were used to detect and quantify GABA in anterior cingulate cortex (ACC) and occipital cortex (OCC) of healthy volunteers. Residual bootstrap, a model-based statistical analysis technique, was applied to resample the fitting residuals of GABA from the Gaussian fitting model (referred to as GABA + thereafter) in both individual and group data of ACC and OCC. The inter-subject coefficient of variation (CV) of GABA + in OCC (20.66 %) and ACC (12.55 %) with residual bootstrap was lower than that of a standard Gaussian model analysis (21.58 % and 16.73 % for OCC and ACC, respectively). The intra-subject uncertainty and CV of OCC were lower than that of ACC in both analyses. The residual bootstrap analysis thus provides a more robust uncertainty estimation of individual and group GABA + detection in different brain regions, which may be useful in our understanding of GABA biochemistry in brain and its use for the diagnosis of related neuropsychiatric diseases.

  18. RESIDUAL GAS MOTIONS IN THE INTRACLUSTER MEDIUM AND BIAS IN HYDROSTATIC MEASUREMENTS OF MASS PROFILES OF CLUSTERS

    International Nuclear Information System (INIS)

    Lau, Erwin T.; Kravtsov, Andrey V.; Nagai, Daisuke

    2009-01-01

    We present analysis of bulk and random gas motions in the intracluster medium using high-resolution Eulerian cosmological simulations of 16 simulated clusters, including both very relaxed and unrelaxed systems and spanning a virial mass range of 5 x 10 13 - 2 x 10 15 h -1 M-odot. We investigate effects of the residual subsonic gas motions on the hydrostatic estimates of mass profiles and concentrations of galaxy clusters. In agreement with previous studies, we find that the gas motions contribute up to ∼5%-15% of the total pressure support in relaxed clusters with contribution increasing with the cluster-centric radius. The fractional pressure support is higher in unrelaxed systems. This contribution would not be accounted for in hydrostatic estimates of the total mass profile and would lead to systematic underestimate of mass. We demonstrate that total mass can be recovered accurately if pressure due to gas motions measured in simulations is explicitly taken into account in the equation of hydrostatic equilibrium. Given that the underestimate of mass is increasing at larger radii, where gas is less relaxed and contribution of gas motions to pressure is larger, the total density profile derived from hydrostatic analysis is more concentrated than the true profile. This may at least partially explain some high values of concentrations of clusters estimated from hydrostatic analysis of X-ray data.

  19. Multi-residue determination of 115 veterinary drugs and pharmaceutical residues in milk powder, butter, fish tissue and eggs using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Dasenaki, Marilena E; Thomaidis, Nikolaos S

    2015-06-23

    A simple and sensitive multi-residue method for the determination of 115 veterinary drugs and pharmaceuticals, belonging in more than 20 different classes, in butter, milk powder, egg and fish tissue has been developed. The method involves a simple generic solid-liquid extraction step (solvent extraction, SE) with 0.1% formic acid in aqueous solution of EDTA 0.1% (w/v)-acetonitrile (ACN)-methanol (MeOH) (1:1:1, v/v) with additional ultrasonic-assisted extraction. Precipitation of lipids and proteins was promoted by subjecting the extracts at very low temperature (-23°C) for 12h. Further cleanup with hexane ensures fat removal from the matrix. Analysis was performed by liquid chromatography coupled with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS). Two separate runs were performed for positive and negative ionization in multiple reaction monitoring mode (MRM). Particular attention was devoted to extraction optimization: different sample-to-extracting volume ratios, different concentrations of formic acid in the extraction solvent and different ultrasonic extraction temperatures were tested in butter, egg and milk powder samples. The method was also applied in fish tissue samples. It was validated, on the basis of international guidelines, for all four matrices. Quantitative analysis was performed by means of standard addition calibration. For over 80% of the analytes, the recoveries were between 50% and 120% in all matrices studied, with RSD values in the range of 1-18%. Limits of detection (LODs) and quantification (LOQs) ranged from 0.008 μg kg(-1) (oxfendazole in butter) to 3.15 μg kg(-1) (hydrochlorthiazide in egg). The evaluated method provides reliable screening, quantification, and identification of 115 veterinary drug and pharmaceutical residues in foods of animal origin and has been successfully applied in real samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. TECHNOLOGICAL TESTS USING QUARTZITE RESIDUES AS COMPONENT OF CERAMIC MASS AT THE PORCELAIN STONEWARE PRODUCTION

    OpenAIRE

    Souza, Marcondes Mendes; Instituto Federal de Educação, Ciência e Tecnologia do Rio Grande do Norte; da Costa, Francine Alves; Departamento de Engenharia Mecânica (UFRN)

    2015-01-01

    This work aims to evaluate through technological tests the use of quartzite residues as component at the the production of porcelain stoneware. Were collected five samples of quartzites called of green quartzite, black quartzite, pink quartzite, goldy quartzite, white quartzite. After, the raw materials were milled, passed by a sieve with a Mesh of 200# (Mesh) and characterized by chemical analysis in fluorescence of x-rays and also analysis of the crystalline phases by diffraction of x-rays....

  1. Simultaneous determination of organochlorine and pyrethriod pesticide residues in the Chinese patent medicines by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Mao, Xue J; Zhong, Yao; Yan, Ai P; Wang, Bin; Wang, Yuan X; Wan, Yi Q

    2018-02-01

    A simple, sensitive, reliable method was developed for the simultaneous determination of organochlorine and pyrethriod pesticide residues in Chinese patent medicines Six ingredient rehmannia pills and Xiaoyao pills. These pesticides were extracted by ethyl acetate. The extraction time and volume of ethyl acetate were optimized. Cleanup of extracts was performed with dispersive-solid phase extraction using graphitized carbon black as the sorbent. The determination of pesticides in the final extracts was carried out by gas chromatography-tandem mass spectrometry in multiple reaction monitoring mode (GC-MS/MS, MRM). The linearity of the calibration curves is good in matrix-matched standard and yields the coefficients of determination (R 2 ) ≥0.99 for all of the target analytes. Under optimized conditions, the average recoveries (five replicates) for most pesticides range from 75.5% to 114.6%, and RSDs are less than 10.0%. The LODs of 18 pesticides in Six ingredient rehmannia pill and Xiaoyao pills are in the range of 0.01-8.82 μg kg -1 . The developed method meets the requirements of pesticide residue analysis and could be effectively used for routine analysis of the organochlorine and pyrethriod pesticide residues in Six ingredient rehmannia pills and Xiaoyao pills.

  2. Analysis of nifursol residues in turkey and chicken meat using liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Gabrielsen, Martin Vahl

    2005-01-01

    on conversion of nifursol and its metabolites with an intact 3,5-dinitrosalicylic acid hydrazide (DNSH) side chain to the 2-nitrophenyl analogue of nifursol (NPDNSH) by treatment with dilute hydrochloric acid and 2-nitrobenzaldehyde. Nifuroxazide (salicylic acid (5-nitrofurfurylidene) hydrazide) added......Nifursol (3,5-dinitrosalicylic acid (5-nitrofurfurylidene) hydrazide) is mainly used as a feed additive for the prevention of blackhead disease in turkeys. The objective of the present work was to establish information on nifursol residues in turkey and chicken meat. The analytical method was based...

  3. [Simultaneous analysis the residues of 20 hormones in foods of animal origin by liquid chromatography tandem mass spectrometry].

    Science.gov (United States)

    Liu, Guihua; Qin, Wei; Liu, Honghe; Zhu, Zhou

    2013-01-01

    To develop a quick and accurate method for simultaneous determining the multi-residues of hormones in foods of animal origin by liquid chromatography-tandem mass spectrometry (LC-MS/MS), and to investigate these residues in swine, bovine, egg and milk collected from local markets in Shenzhen. The sample was firstly extracted with acetonitrile, and then subjected to solid-phase extraction clean-up using HLB-NH2 cartridges after defatted with hexane, lastly detected by high performance liquid chromatography-tandem mass spectrometry. Identification was achieved by electrospray ionization (ESI) in both positive and negative mode using multiple reaction monitoring. Quantification was performed by internal standard calibration. The study showed that there was a certain amount of endogenous hormones in collected samples. The limits of quantification were 0.5 - 1.0 microg/kg for 20 hormones in swine, bovine, egg and milk. Average recoveries were 60.4% -118.2%, and the relative standard deviations were 2.5% - 16.2%. This method was quick and accurate which could be used for determination of hormones in foods of animal origin (such as swine, bovine, egg and milk).

  4. [Determination of paraquat residue in plant-derived foodstuffs by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Bo, Haibo

    2011-02-01

    A sensitive and selective method is presented for the determination of paraquat residue in fruits, vegetables, beans and grain by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Paraquat in samples was extracted with water and cleaned-up with a weak cation exchange (WCX) column to obtain an extract suitable for analysis using HPLC-MS/MS. The paraquat was separated by a CAPCELL PAK ST column (150 mm x 2.0 mm) and with acetonitrile-10 mmol/L ammonium acetate solution (adjusted to pH 4.0 by formic acid) as the mobile phase, and multiple reaction monitoring (MRM) was used with electrospray ionization in the positive ion mode. The calibration curve was linear between the peak area and the mass concentration of paraquat from 0.01 to 0.1 mg/L with the correlation coefficient of 0.993. Recoveries of paraquat spiked in samples at three levels ranged from 84.0% to 106.0% with the relative standard deviations of 7.8% - 18.8%. The limits of detection (LODs) of paraquat were 0.01 mg/kg in fruits and vegetables and 0.05 mg/kg in beans and grain. The LODs can meet the requirements of international maximum residue limit.

  5. Use of mass spectrometry methods as a strategy for detection and determination of residual solvents in pharmaceutical products.

    Science.gov (United States)

    Pérez Pavón, José Luis; del Nogal Sanchez, Miguel; García Pinto, Carmelo; Fernandez Laespada, M Esther; Moreno Cordero, Bernardo

    2006-07-15

    In the present work a strategy for the qualitative and quantitative analysis of residual solvents in pharmaceutical products is reported. First, a low-resolution chromatogram is generated for the identification of the solvents present in the samples by means of headspace generation-fast gas chromatography-mass spectrometry (HS-fast GC/MS). From the plotting of this information by means of contour plots with time and mass/charge axes, it is decided whether quantification of such compounds can be accomplished without chromatographic separation or whether it should be done by fast gas chromatography. The nonseparative method is based on direct coupling of a headspace sampler with a mass spectrometer (HS-MS) and requires a signal recording time of only 3 min, while with fast gas chromatography the time required to obtain a chromatogram is 7.16 min. The use of headspace generation for introducing the sample and standard addition as a quantification technique provided satisfactory results and minimized the matrix effect. An important advantage of the methodologies used here is related to the fact that no prior treatment of the sample is required, thus minimizing the creation of analytical artifacts and the errors associated with this step of the analytical process. The methods were applied to the determination of residual solvents in 27 different pharmaceutical products. Detection and quantitation limits were sufficiently low to enable the estimation of organic volatile impurities according to the International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use.

  6. Structural characteristics and forage mass of Tifton 85 pastures managed under three post-grazing residual leaf areas

    Directory of Open Access Journals (Sweden)

    Wilton Ladeira da Silva

    2013-04-01

    Full Text Available The experiment was carried out on Cynodon spp cv. Tifton 85 pastures grazed by sheep under rotational stocking, with the objective of evaluating the structural characteristics as well as the forage mass of the pastures subjected to three grazing intensities in successive cycles. Treatments were composed of three residual leaf area indices (rLAI; 2.4; 1.6 and 0.8, allocated in completely randomized blocks with seven replications, totaling 21 experimental units. Tiller population density, pasture height, leaf area index, forage morphological composition and pasture forage mass were evaluated. The rLAI modified the tiller population density, which increased linearly with decrease in the rLAI of the pastures. Dry masses of leaf blade, stem and dead material were inferior when the rLAI imposed were lower, which resulted in differentiated forage production among the treatments. Tifton 85 pastures grazed by sheep in rotational stocking under tropical conditions with different rLAI show a modified sward structure over successive grazing cycles, mainly by alteration in the height and LAI of the plants at pre-grazing and by light interception post-grazing, which change the tiller population density. The residual leaf area index of 1.6 is the most suitable for pasture management for being equivalent to the heights of entrance and exit of animals on and from paddocks of 33 and 19 cm, respectively, which avoid great accumulation of dead material and excessive stem elongation, in addition to ensuring tillering in the sward.

  7. The virial mass distribution of ultradiffuse galaxies in clusters and groups

    Science.gov (United States)

    Amorisco, N. C.

    2018-03-01

    We use the observed abundances of ultradiffuse galaxies (UDGs) in clusters and groups and Λ cold dark matter subhalo mass functions to put constraints on the distribution of present-day halo masses of satellite UDGs. If all of the most massive subhaloes in the cluster host a UDG, UDGs occupy all subhaloes with log Msub/M⊙ ≳ 11. For a model in which the efficiency of UDG formation is higher around some characteristic halo mass, higher fractions of massive UDGs require larger spreads in the UDG mass distribution. In a cluster with a virial mass of 1015 M⊙, the 90 per cent upper limit for the fraction of UDGs with log Msub/M⊙ > 12 is 7 per cent, occupying 70 per cent of all cluster subhaloes above the same mass. To reproduce the observed abundances, however, the mass distribution of satellite UDGs has to be broad, with > 30 per cent having log Msub/M⊙ continuous distribution in which a majority are hosted by low-mass haloes. The abundance of satellite UDGs may fall short of the linear relation with the cluster/group mass Mhost in low-mass hosts, log Mhost/M⊙ ˜ 12. Characterizing these deviations - or the lack thereof - will allow for stringent constraints on the UDG virial mass distribution.

  8. Correlation between the Total Gravitating Mass of Groups and Clusters and the Supermassive Black Hole Mass of Brightest Galaxies

    Science.gov (United States)

    Bogdán, Ákos; Lovisari, Lorenzo; Volonteri, Marta; Dubois, Yohan

    2018-01-01

    Supermassive black holes (BHs) residing in the brightest cluster galaxies are over-massive relative to the stellar bulge mass or central stellar velocity dispersion of their host galaxies. As BHs residing at the bottom of the galaxy cluster’s potential well may undergo physical processes that are driven by the large-scale characteristics of the galaxy clusters, it is possible that the growth of these BHs is (indirectly) governed by the properties of their host clusters. In this work, we explore the connection between the mass of BHs residing in the brightest group/cluster galaxies (BGGs/BCGs) and the virial temperature, and hence total gravitating mass, of galaxy groups/clusters. To this end, we investigate a sample of 17 BGGs/BCGs with dynamical BH mass measurements and utilize XMM-Newton X-ray observations to measure the virial temperatures and infer the {M}500 mass of the galaxy groups/clusters. We find that the {M}{BH}{--}{kT} relation is significantly tighter and exhibits smaller scatter than the {M}{BH}{--}{M}{bulge} relations. The best-fitting power-law relations are {{log}}10({M}{BH}/{10}9 {M}ȯ )=0.20+1.74{{log}}10({kT}/1 {keV}) and {{log}}10({M}{BH}/{10}9 {M}ȯ ) = -0.80+1.72{{log}}10({M}{bulge}/{10}11 {M}ȯ ). Thus, the BH mass of BGGs/BCGs may be set by physical processes that are governed by the properties of the host galaxy group/cluster. These results are confronted with the Horizon-AGN simulation, which reproduces the observed relations well, albeit the simulated relations exhibit notably smaller scatter.

  9. Application of capillary electrophoresis-mass spectrometry for determining organic food contaminants and residues.

    Science.gov (United States)

    Font, Guillermina; Ruiz, Maria José; Fernández, Monica; Picó, Yolanda

    2008-05-01

    Food contamination continues to be a serious problem around the world. Surveillance of chemical contaminants in foods is important not only for public health but also because of the negative economic impact of contamination. From the analytical perspective, analysis of contaminants in food is an extremely challenging area. There is a wide variety of questions, ranging from the quantification of extremely low levels of individual components to the detailed assessment and evaluation of the analytical technique possibilities. This review considers the applications of CE coupled to MS detection (CE-MS) for the analysis of organic contaminants in food. Analytical information on sample concentration techniques, as well as on the CE separation conditions and recoveries obtained from water and food are provided. Different sections include several fields of application, such as pesticides, drug residues, or toxic formed during food processing in different matrices. A number of tables report a comprehensive listing of CE-MS applications. As a result, this work presents an update overview on the principal application of CE-MS together with a discussion of their main advantages and drawbacks, and an outline of future trends on analysis of organic contaminants.

  10. Residue Modification and Mass Spectrometry for the Investigation of Structural and Metalation Properties of Metallothionein and Cysteine-Rich Proteins.

    Science.gov (United States)

    Irvine, Gordon W; Stillman, Martin J

    2017-04-26

    Structural information regarding metallothioneins (MTs) has been hard to come by due to its highly dynamic nature in the absence of metal-thiolate cluster formation and crystallization difficulties. Thus, typical spectroscopic methods for structural determination are limited in their usefulness when applied to MTs. Mass spectrometric methods have revolutionized our understanding of protein dynamics, structure, and folding. Recently, advances have been made in residue modification mass spectrometry in order to probe the hard-to-characterize structure of apo- and partially metalated MTs. By using different cysteine specific alkylation reagents, time dependent electrospray ionization mass spectrometry (ESI-MS), and step-wise "snapshot" ESI-MS, we are beginning to understand the dynamics of the conformers of apo-MT and related species. In this review we highlight recent papers that use these and similar techniques for structure elucidation and attempt to explain in a concise manner the data interpretations of these complex methods. We expect increasing resolution in our picture of the structural conformations of metal-free MTs as these techniques are more widely adopted and combined with other promising tools for structural elucidation.

  11. Multi-Residue Analysis of Pesticides in Pistachio Using Gas Chromatography-Mass Spectrometry (GC/MS

    Directory of Open Access Journals (Sweden)

    Azadeh Emami

    2014-12-01

    Full Text Available Background: Analysis of pesticide residues in food and other environmental commodities have become an essential requirement for consumers, producers, food inspectors and authorities. This study is focused on validation of an accurate, rapid and reliable method for multi-residual analysis of pesticides in pistachio as a strategic crop for export and one of the main nuts in Iranian food basket. Methods: We developed a "Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS method based on spiking blank samples and used the data for drawing calibration curves instead of standard solutions. Sample preparations were developed for determination of 12 pesticide residues in pistachio by gas chromatography-mass spectrometry (GC/MS. Results: Recovery of pesticides at 5 concentration levels (n=3 was in the range of 81.40% - 93.08 %. The method proved to be repeatable in the majority of samples with relative standard deviation (RSD of lower than 20%. The limits of detection and quantification for all pesticides were 2 ppb and 10 ppb, respectively. Conclusion: The calibration curves of pesticides were linear in the range of 10-500 (ng/g and correlation coefficient of entire pesticides was higher than 0.994. The recovery of pesticides at 5 concentration levels (n=3 was in range of 81.41- 91.80 %. The method was proved to be repeatable with the majority of RSDs being lower than 20%. The limits of detection and quantification for all pesticides were 2 and 10 ppb, respectively. The recoveries and repeatabilities were in accordance with the criteria set by SANCO Guideline (Commission of the European Communities, 2006.

  12. Characterization of biomass burning smoke from cooking fires, peat, crop residue and other fuels with high resolution proton-transfer-reaction time-of-flight mass spectrometry

    Science.gov (United States)

    Stockwell, C. E.; Veres, P. R.; Williams, J.; Yokelson, R. J.

    2014-08-01

    We deployed a high-resolution proton-transfer-reaction time-of-flight mass spectrometer (PTR-TOF-MS) to measure biomass burning emissions from peat, crop-residue, cooking fires, and many other fire types during the fourth Fire Lab at Missoula Experiment (FLAME-4) laboratory campaign. A combination of gas standards calibrations and composition sensitive, mass dependent calibration curves were applied to quantify gas-phase non-methane organic compounds (NMOCs) observed in the complex mixture of fire emissions. We used several approaches to assign best identities to most major "exact masses" including many high molecular mass species. Using these methods approximately 80-96% of the total NMOC mass detected by PTR-TOF-MS and FTIR was positively or tentatively identified for major fuel types. We report data for many rarely measured or previously unmeasured emissions in several compound classes including aromatic hydrocarbons, phenolic compounds, and furans; many of which are suspected secondary organic aerosol precursors. A large set of new emission factors (EFs) for a range of globally significant biomass fuels is presented. Measurements show that oxygenated NMOCs accounted for the largest fraction of emissions of all compound classes. In a brief study of various traditional and advanced cooking methods, the EFs for these emissions groups were greatest for open 3-stone cooking in comparison to their more advanced counterparts. Several little-studied nitrogen-containing organic compounds were detected from many fuel types that together accounted for 0.1-8.7% of the fuel nitrogen and some may play a role in new particle formation.

  13. [Determination of avermectin, diclazuril, toltrazuril and metabolite residues in pork by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Gong, Xiaoming; Sun, Jun; Dong, Jing; Yu, Jinling; Wang, Hongtao

    2011-03-01

    A method for the determination of avermectin, ivermectin, doramectin, moxidectin, eprinomectin, diclazuril, toltrazuril and its two metabolite residues in pork was developed using QuEChERS method with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with acetonitrile and purified through QuEChERS method using ODS as the sorbent. The target compounds were separated on a Venusil ASB C18 column (150 mm x 2.1 mm, 3.0 microm) and detected by HPLC-MS/MS. The linear ranges were 0.005 - 0.2 mg/L and the correlation coefficients were all above 0.990. The average recoveries and the relative standard deviations ranged from 73.2% to 91.5% and from 12% to 17% at the spiked levels of 0.005, 0.01 and 0.02 mg/kg for the 9 analytes in pork matrix. This method is reliable, and suitable for the determination of the residues of avermectin and related compounds in pork.

  14. Analysis of 10 systemic pesticide residues in various baby foods using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Yang, Angel; Abd El-Aty, A M; Park, Jong-Hyouk; Goudah, Ayman; Rahman, Md Musfiqur; Do, Jung-Ah; Choi, Ok-Ja; Shim, Jae-Han

    2014-06-01

    Ten systemic pesticides, comprising methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazole, and difenoconazole, were detected in 13 baby foods (cereals, boiled potatoes, fruit and milk) using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for sample preparation and liquid chromatography tandem mass spectrometry for analysis. The matrix-matched calibration curves showed good linearity with determination coefficients (R(2) ) >0.992. The limits of detection and quantitation were 0.0015-0.003 and 0.005-0.01 mg/kg, respectively. The mean recoveries of three different concentrations ranged from 69.2 to 127.1% with relative standard deviations market, and none of the samples were found to contain pesticide residues. This method is suitable for the identification and quantification of systemic pesticides with matrix-matched standards in various baby foods. Copyright © 2013 John Wiley & Sons, Ltd.

  15. Grouping of residual solvents present in pharmaceuticals using experimental planning and chemometric methods.

    Science.gov (United States)

    Grodowska, Katarzyna; Parczewski, Andrzej

    2013-01-01

    The main effects of six experimental factors on the efficiency of HS (headspace) extraction in headspace gas chromatography--flame ionization detector (HS-GC-FID) determination of twenty organic solvents routinely used in production of pharmaceuticals were obtained on the basis of the results of experiments carried out according to the Plackett-Burman factorial design. The effects were used as a basis for grouping the solvents into five groups, the solvents belonging to a group responded similarly to changes of HS conditions. To this end, visualization approaches were used as well as chemometric methods: cluster analysis (CA) and principal component analysis (PCA). Moreover, the most important HS experimental factors were selected for further optimization of the HS-GC determination procedure.

  16. Assessment of the nature of residual masses at end of treatment in lymphoma patients using volume perfusion computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Syha, R.; Gruenwald, L.; Spira, D.; Ketelsen, D.; Claussen, C.D.; Horger, M. [Eberhard Karls University, Department of Diagnostic Radiology, Tuebingen (Germany); Horger, T. [Technische Universitaet Muenchen, M2 - Lehrstuhl fuer Numerische, Garching (Germany); Vogel, W. [Eberhard Karls University, Department of Medical Oncology and Haematology, Tuebingen (Germany)

    2014-03-15

    To determine the diagnostic benefit of volume perfusion computed tomography (VPCT) at end of treatment for response assessment in lymphoma patients. Seventy-five patients with different lymphoma subtypes were included: 50/75 patients had residual masses at end of treatment, 26/50 patients underwent VPCT at baseline and at end of treatment, and 24/50 patients only had end-of-treatment VPCTs. We evaluated the size of the main lymphoma mass, its blood flow (BF), blood volume (BV) and k-trans, calculated ratios (baseline and end of treatment) as well as sensitivity/specificity/negative (NPV)/positive predictive values (PPV). For VPCT at end of treatment, a cutoff threshold between responders and non-responders was calculated. For patients undergoing VPCT at baseline and end of treatment, reduction in size, BF, BV and k-trans was significant (P < 0.001). Identification of non-response was reached at: <53 % reduction in size (sensitivity/specificity/accuracy/PPV/NPV of 88.89 %/62.5 %/80.77 %/84.21 %/71.43 %), <15 % reduction of BF (sensitivity/specificity/accuracy/PPV/NPV of 100 %/37.5 %/80.77 %/0.26 %/100 %), or <45 % reduction of k-trans (sensitivity/specificity/accuracy/PPV/NPV of 88.89 %/75 %/84.62 %/88.89 %/75 %). In the subgroup undergoing VPCT at end of treatment, BF >18.51 ml/100 ml indicated non-responsiveness (sensitivity 92.86 %, specificity 72.73 %, accuracy 84 %, PPV 81.25 %, NPV 88.89 %). VPCT seems adequate for assessment of lymphoma response at end of treatment. The degree of residual lymphoma perfusion at end of treatment helps to identify patients likely to remain in remission 1 year after completion of therapy. (orig.)

  17. New tendencies in isotopic analysis of pesticide residues from wines by mass spectrometry in concordance with the European standards

    International Nuclear Information System (INIS)

    Costinel, Diana; Lazar, Roxana Elena; Vremera, Raluca; Irimescu, Rodica; Saros-Rogobete, Gili

    2006-01-01

    Multi-isotope analysis, the determination of isotope ratios by mass spectrometry or magnetic resonance spectroscopy, becomes increasingly used in the food industry and by national food control laboratories as a method of authenticating both raw materials and finished products. These highly sophisticated techniques are capable of determining the botanical and geographical origin of a wide variety of foodstuffs, thus providing a means of detecting product adulteration and controlling mislabelling practices which are virtually impossible to circumvent. The European Union has officially adopted the used of isotope analysis as a means of controlling sugar addition in wines. Its successful implementation in the wine-producing Member States has considerably reduced the financial losses which the Community had incurred due to over - capitalisation. Coupling mass spectrometer with gas chromatograph is used for quantitative and qualitative analysis of traces of pesticides from food. The presence of pesticides in foods is harmful for the nervous system, the cardiovascular apparatus and decreases the immunity of human body. In addition, ensuring the foods quality and safety is a requirement, which must be fulfilled for the integration in EU. The subject of this paper is the presentation of the tests results of the isotopic analysis for pesticide residues in wines, in concordance with European Standard. (authors)

  18. Coiled-coil destabilizing residues in the group A Streptococcus M1 protein are required for functional interaction.

    Science.gov (United States)

    Stewart, Chelsea M; Buffalo, Cosmo Z; Valderrama, J Andrés; Henningham, Anna; Cole, Jason N; Nizet, Victor; Ghosh, Partho

    2016-08-23

    The sequences of M proteins, the major surface-associated virulence factors of the widespread bacterial pathogen group A Streptococcus, are antigenically variable but have in common a strong propensity to form coiled coils. Paradoxically, these sequences are also replete with coiled-coil destabilizing residues. These features are evident in the irregular coiled-coil structure and thermal instability of M proteins. We present an explanation for this paradox through studies of the B repeats of the medically important M1 protein. The B repeats are required for interaction of M1 with fibrinogen (Fg) and consequent proinflammatory activation. The B repeats sample multiple conformations, including intrinsically disordered, dissociated, as well as two alternate coiled-coil conformations: a Fg-nonbinding register 1 and a Fg-binding register 2. Stabilization of M1 in the Fg-nonbinding register 1 resulted in attenuation of Fg binding as expected, but counterintuitively, so did stabilization in the Fg-binding register 2. Strikingly, these register-stabilized M1 proteins gained the ability to bind Fg when they were destabilized by a chaotrope. These results indicate that M1 stability is antithetical to Fg interaction and that M1 conformational dynamics, as specified by destabilizing residues, are essential for interaction. A "capture-and-collapse" model of association accounts for these observations, in which M1 captures Fg through a dynamic conformation and then collapses into a register 2-coiled coil as a result of stabilization provided by binding energy. Our results support the general conclusion that destabilizing residues are evolutionarily conserved in M proteins to enable functional interactions necessary for pathogenesis.

  19. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marguí, Eva, E-mail: eva.margui@udg.edu [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain); Queralt, Ignasi, E-mail: iqueralt@ictja.csic.es [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences “Jaume Almera”, CSIC, Solé Sabarís s/n, 08028 Barcelona (Spain); Hidalgo, Manuela, E-mail: manuela.hidalgo@udg.edu [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain)

    2013-08-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2–4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods. - Highlights: • A TXRF method for PGM catalyst residue determination in API samples is presented. • Analysis can be performed using 10 μL of the internal standardized dissolved API. • The method is rapid, simple and suitable according to the USP requirements.

  20. Mass sensitivity of acoustic wave devices from group and phase velocity measurements

    Science.gov (United States)

    McHale, G.; Martin, F.; Newton, M. I.

    2002-09-01

    The effect of dispersion on acoustic wave sensors is considered. The discussion is focused upon layer guided surface acoustic waves (Love waves), which obtain their high mass sensitivity for the first Love wave mode by optimizing the guiding layer thickness, d, such that dapprox][lambdal/4; the wavelength in the layer is given by lambdal=f/vl where f is the operating frequency and vl is the shear acoustic speed of the guiding layer. We show that this optimization of guiding layer thickness corresponds to strong dispersion so that the phase and group velocities can be quite different. From the definition of the phase velocity mass sensitivity, we show that it can be determined from either the slope of the curve of phase velocity with normalized guiding layer thickness, z=d/lambdal, or from the phase and group velocities measured for a given guiding layer thickness. Experimental data for a poly(methylmethacrylate) polymer guiding layer on 36deg XY Lithium Tantalate is presented. Measurements of phase velocity and group velocity determined by a network analyzer were obtained for systematically increasing guiding layer thicknesses; a pulse transit experiment was also used to provide independent confirmation of the group velocity data. Two independent estimates of the mass sensitivity are obtained for z=d/lambdal<0.22 from (i) the slope of the phase velocity curve and (ii) the measurements of the group and phase velocity. These two estimates are shown to be consistent and we, therefore, conclude that it is possible to determine the mass sensitivity for a Love wave device with a given guiding layer thickness from measurements of the phase and group velocities. Moreover, we argue that the formula using group velocity to determine phase velocity mass sensitivity can be extended to a wide range of other acoustic wave sensors. In addition, we suggest that variations in the group velocity due to deposited mass may be a more sensitive parameter than variations in the phase

  1. Pesticide residues in fruit samples: comparison of different QuEChERS methods using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Christia, C; Bizani, E; Christophoridis, C; Fytianos, K

    2015-09-01

    Acetate- and citrate-buffered quick, easy, cheap, effective, rugged, safe (QuEChERS) pretreatment methods were evaluated for the determination of various pesticides in peaches, grapes, apples, bananas, pears, and strawberries from various regions of Greece, using LC-MS/MS. The purposes of this study were (i) to evaluate which type of QuEChERS method was the most appropriate and effective for each matrix; (ii) to apply the selected QuEChERS method for each matrix, in order to detect and quantify pesticide residues in various fruit samples using UPLC-MS/MS; (iii) to examine the concentration distribution of pesticide classes among fruit originating from various areas; and (iv) to assess pesticide concentration distribution between peel and flesh of fruit in order to evaluate the penetration of pesticide residues in the fruit flesh. Acetate-buffered QuEChERS was found to be the most suitable technique for most of the fruit matrices. According to the recovery values at two different concentration levels, peaches should preferably be treated by the citrate-buffered type, whereas grapes, bananas, apples, pears, and strawberries are best treated by the acetate-buffered version, although the differences in efficiency were small. The addition of graphitized carbon black significantly decreases the recovery of specific pesticides in all matrices except for strawberries. The majority of values do not exceed the official maximum residue levels set by the European Commission. Organophosphates proved to be the most commonly detected category along with triazines-triazoles-conazoles group and by carbamates. Apples and pears seem to be the most contaminated fruit matrices among those tested. Distribution of pesticide classes shows variations between different regions, suggesting different pesticide application practices. In the case of peaches and pears, there is an equal distribution of detected pesticides between peel and flesh, indicating penetration of contaminants into the

  2. Practical application of in silico fragmentation based residue screening with ion mobility high-resolution mass spectrometry.

    Science.gov (United States)

    Kaufmann, Anton; Butcher, Patrick; Maden, Kathry; Walker, Stephan; Widmer, Mirjam

    2017-07-15

    A screening concept for residues in complex matrices based on liquid chromatography coupled to ion mobility high-resolution mass spectrometry LC/IMS-HRMS is presented. The comprehensive four-dimensional data (chromatographic retention time, drift time, mass-to-charge and ion abundance) obtained in data-independent acquisition (DIA) mode was used for data mining. An in silico fragmenter utilizing a molecular structure database was used for suspect screening, instead of targeted screening with reference substances. The utilized data-independent acquisition mode relies on the MS E concept; where two constantly alternating HRMS scans (low and high fragmentation energy) are acquired. Peak deconvolution and drift time alignment of ions from the low (precursor ion) and high (product ion) energy scan result in relatively clean product ion spectra. A bond dissociation in silico fragmenter (MassFragment) supplied with mol files of compounds of interest was used to explain the observed product ions of each extracted candidate component (chromatographic peak). Two complex matrices (fish and bovine liver extract) were fortified with 98 veterinary drugs. Out of 98 screened compounds 94 could be detected with the in silico based screening approach. The high correlation among drift time and m/z value of equally charged ions was utilized for an orthogonal filtration (ranking). Such an orthogonal ion mobility based filter removes multiply charged ions (e.g. peptides and proteins from the matrix) as well as noise and artefacts. Most significantly, this filtration dramatically reduces false positive findings but hardly increases false negative findings. The proposed screening approach may offer new possibilities for applications where reference compounds are hardly or not at all commercially available. Such areas may be the analysis of metabolites of drugs, pyrrolizidine alkaloids, marine toxins, derivatives of sildenafil or novel designer drugs (new psychoactive substances

  3. Density-body mass relationships: Inconsistent intercontinental patterns among termite feeding-groups

    Science.gov (United States)

    Dahlsjö, Cecilia A. L.; Parr, Catherine L.; Malhi, Yadvinder; Meir, Patrick; Rahman, Homathevi; Eggleton, Paul

    2015-02-01

    Allometric relationships are useful for estimating and understanding resource distribution in assemblages with species of different masses. Damuth's law states that body mass scales with population density as M-0.75, where M is body mass and -0.75 is the slope. In this study we used Damuth's law (M-0.75) as a null hypothesis to examine the relationship between body mass and population density for termite feeding-groups in three different countries and regions (Cameroon, West Africa; Peru South America; and Malaysia SE Asia). We found that none of the feeding-groups had a relationship where M-0.75 while the data suggested that population density-body mass relationships for true soil-feeding termites in Cameroon (M2.7) and wood-feeding termites in Peru (M1.5) were significantly different from the expected values given by Damuth's law. The dominance of large-bodied true soil-feeding termites in Cameroon and the absence of fungus-growing termites from Peru suggest that these allometric patterns are due to heterogeneities in termite biogeographical evolution. Additionally, as these feeding-groups have higher population density than expected by their body masses it may be suggested that they also have a higher energy throughput than expected. The results presented here may be used to gain further understanding of resource distribution among termite feeding-groups across regions and an insight into the importance of evolutionary history and biogeography on allometric patterns. Further understanding of population density-body mass relationships in termite feeding-groups may also improve understanding of the role these feeding-groups play in ecosystem processes in different regions.

  4. Identification of functionally important acidic residues in transducin by group-specific labeling

    Directory of Open Access Journals (Sweden)

    ANA KOSOY

    2003-01-01

    Full Text Available Transducin (T, a GTP-binding protein involved in phototransduction of rod photoreceptor cells, is a heterotrimer arranged as two units, the a-subunit (Ta and the bg-complex (Tbg. The role of the carboxyl groups in T was evaluated by labeling with N, N'-dicyclohexylcarbodiimide (DCCD and 1-ethyl 3-(3-dimethylaminopropyl carbodiimide (EDC. Only a minor effect on the binding of b, g-imido guanosine 5'-triphosphate (GMPpNp to T was observed in the presence of the hydrophobic carbodiimide, DCCD. Similarly, the GMPpNp binding activity of the reconstituted holoenzyme was not significantly affected when Ta was combined with DCCD-treated Tbg. However, the binding of guanine nucleotides to the reconstituted T was ~50% inhibited when DCCD-labeled Ta was incubated with Tbg. In contrast, treatment of T with the hydrophilic carbodiimide, EDC, completely impaired its GMPpNp-binding ability. EDC-modified T was incapable of interacting with illuminated rhodopsin, as determined by sedimentation experiments. However, rhodopsin only partially protected against the inactivation of T. Additionally, analyses of trypsin digestion patterns showed that fluoroaluminate was not capable of activating the EDC-labeled T sample. The function of the reconstituted holoenzyme was also disrupted when EDC-modified Ta was combined with Tbg, and when EDC-treated Tbg was incubated with Ta

  5. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    Science.gov (United States)

    Marguí, Eva; Queralt, Ignasi; Hidalgo, Manuela

    2013-08-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2-4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods.

  6. Ultra performance liquid chromatography-tandem mass spectrometry for the determination of amicarthiazol residues in soil and water samples.

    Science.gov (United States)

    Gui, Wen-jun; Tian, Jie; Tian, Chun-xia; Li, Shu-ying; Ma, You-ning; Zhu, Guo-nian

    2014-12-01

    A reliable and rapid method has been optimized to determine the residue of amicarthiazol in soil and environmental water samples. After extraction and evaporation, the extraction was carried out with solid phase extraction (SPE) cleanup using HLB cartridge (only soil samples) and for the quantitative determination by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The resulting residues of amicarthiazol were analyzed by a gradient separation performed on a UPLC system with a C18 column, methanol and water containing 0.1% (v v(-1)) formic acid as the mobile phase in the mode of electrospray positive ionization (ESI(+)) and multiple reaction monitoring (MRM). Results showed that the recoveries for spiked samples were 74.4-97.1% and 72.1-109.9% for soil and water, respectively, with the relative standard deviation (RSD) less than 10.2% when fortified at 10, 100 and 1000μgL(-1). The limits of detection (LODs) and the limits of quantification (LOQs) for matrix matched standards ranged from 0.073-0.425μgL(-1) and 0.243-1.42μgL(-1). The intra-day precision (n=5) and the inter-day precision over 10 days (n=10) for the amicarthiazol in soils and water samples spiked at 100μgL(-1) was 7.9% and 15.9%, respectively. Results indicated that the developed method could be a helpful tool for the controlling and monitoring of the risks posed by amicarthiazol to human health and environment safety. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Determination of pesticide residues in animal origin baby foods by gas chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Amendola, Graziella; Pelosi, Patrizia; Attard Barbini, Danilo

    2015-01-01

    A simple, fast and multiresidue method for the determination of pesticide residues in baby foods of animal origin has been developed in order to check the compliance with the Maximum Residue Levels (MRLs) set at a general value of 0.01 mg/kg by Commission Directive 2006/125/EC for infant foods. The main classes of organochlorine, organophosphorus and pyrethroid compounds have been considered, which are mainly fat soluble pesticides. The analytical procedure consists in the extraction of baby food samples by acetonitrile (ACN) followed by a clean up using C18 solid-phase extraction column eluted with ACN. The compounds were determined by gas chromatography-triple quadrupole mass spectrometry equipped with a Programmed Temperature Vaporizer (PTV) injection and a backflush system. In order to compensate for matrix effects PTV and matrix matched standard calibrations have been used. The method has been fully validated for 57 pesticides according to the Document SANCO/12571/2013. Accuracy and precision (repeatability) have been studied by recoveries at two spiking levels, the Limit of Quantitation (LOQ) (0.003-0.008 mg/kg) and 10 time greater (0.03-0.08 mg/kg), and the results were in the acceptable range of 70-120% with Relative Standards Deviations (RSD) ≤20%. Selectivity, linearity, LOQ and uncertainty of measurement were also determined for all the compounds. The method has been also applied for the analysis of 18 baby food animal origin samples, bought form the local market in Rome (Italy), and no pesticide in the scope of the method has been found above the MRL or the LOQ.

  8. Direct residue analysis of systemic insecticides and some of their relevant metabolites in wines by liquid chromatography - mass spectrometry.

    Science.gov (United States)

    Berset, J D; Mermer, S; Robel, A E; Walton, V M; Chien, M L; Field, J A

    2017-07-14

    A direct large volume injection (DI-LVI) high performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS) method was developed and validated for the quantitative determination of 16 systemic insecticides and their main plant metabolites. The assays were conducted on commercial red and white wines made from grapes grown in major wine-producing regions nationally and internationally. Using a 1:20 dilution and an injection volume of 800μL, a limit of quantitation (LOQ) of 1μgL -1 for all analytes was achieved. Matrix-matched standards (MM) were used for accurate quantitation. Imidacloprid (IMI) and methoxyfenozide (MET) were the most frequently detected parent insecticides in the wines reaching concentrations of 1-132μgL -1 . Two important plant metabolites imidacloprid-olefin (IMI-OLE) and spirotetramat-enol (SPT-EN) were found at higher concentrations. In five samples SPT-EN was detected in the mgL -1 range with a maximum concentration of 16.3mgL -1 measured in a conventional white wine sample. Most "organic" wines contained no detectable or low insecticide residues, except for one sample, which showed the highest IMI (14.7μgL -1 ) and IMI-OLE (331μgL -1 ) concentrations. Considering the maximum residue limit (MRL) definition for the different insecticides, three "conventional" wine samples were non-compliant for SPT. This study highlights the importance to determine both parent and metabolite forms of systemic insecticides in the finished product. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Mass of the Local Group from Proper Motions of Distant Dwarf Galaxies

    Science.gov (United States)

    van der Marel, Roeland

    2010-09-01

    The Local Group and its two dominant spirals, the Milky Way and M31, have become the benchmark for testing many aspects of cosmological and galaxy formation theories, due to many exciting new discoveries in the past decade. However, it is difficult to put results in a proper cosmological context, because our knowledge of the mass M of the Local Group remains uncertain by a factor 4. In units of 10^{12} solar masses, a spherical infall model for the zero-velocity surface gives M 1.3; the sum of estimates for the Milky Way and M31 masses gives M 2.6; and the Local Group Timing argument for the M31 orbit gives M 5.6. It is possible to discriminate between the proposed masses by calculating the orbits of galaxies at the edge of the Local Group, which requires knowledge of transverse velocity components. We therefore propose to use ACS/WFC to determine the proper motions of the 4 dwarf galaxies near the edge of the Local Group {Cetus, Leo A, Tucana, Sag DIG} for which deep first epoch data {with 5-7 year time baselines} already exist in the HST Archive. Our team has extensive expertise with HST astrometric science, and our past/ongoing work for, e.g., Omega Cen, LMC/SMC and M31 show that the necessary astrometric accuracy is within the reach of HST's demonstrated capabilities. We have developed, tested, and published a new technique that uses compact background galaxies as astrometric reference sources, and we have already reduced the first epoch data. The final predicted transverse velocity accuracy, 36 km/s when averaged over the sample, will be sufficient to discriminate between each of the proposed Local Group masses at 2-sigma significance {4-sigma between the most extreme values}. Our project will yield the most accurate Local Group mass determination to date, and only HST can achieve the required accuracy.

  10. Recovery of Silver Using Adsorption Gels Prepared from Microalgal Residue Immobilized with Functional Groups Containing Sulfur or Nitrogen.

    Science.gov (United States)

    Khunathai, Kanjana; Inoue, Katsutoshi; Ohto, Keisuke; Kawakita, Hidetaka; Kurata, Minoru; Atsumi, Kinya; Fukuda, Hiroaki; Alam, Shafiq

    2017-06-10

    Although biodiesel oil extracted from microalgae attracts much attention as one of the most promising green energies, its high production cost is a big problem, impeding its extensive use. In order to lower the production cost, the effective use of microalgal residue after extracting biofuel was investigated as a feed material of functional materials. In the present work, a new adsorbent for silver(I) was prepared by immobilizing functional groups of polyethylene-polyamine or dithiooxamide, which exhibita high affinity for soft Lewis acids such as silver(I) ions. Their adsorption behaviors for silver(I) were investigated from aqueous nitrate and acidothiourea media. The effects of the concentrations of nitrate and thiourea, as well as of sulfuric acid, were qualitatively interpreted. From the study of adsorption isotherms on these gels, they were found to exhibita higher adsorption capacity than the majority of those reported to date.

  11. Recovery of Silver Using Adsorption Gels Prepared from Microalgal Residue Immobilized with Functional Groups Containing Sulfur or Nitrogen

    Directory of Open Access Journals (Sweden)

    Kanjana Khunathai

    2017-06-01

    Full Text Available Although biodiesel oil extracted from microalgae attracts much attention as one of the most promising green energies, its high production cost is a big problem, impeding its extensive use. In order to lower the production cost, the effective use of microalgal residue after extracting biofuel was investigated as a feed material of functional materials. In the present work, a new adsorbent for silver(I was prepared by immobilizing functional groups of polyethylene-polyamine or dithiooxamide, which exhibita high affinity for soft Lewis acids such as silver(I ions. Their adsorption behaviors for silver(I were investigated from aqueous nitrate and acidothiourea media. The effects of the concentrations of nitrate and thiourea, as well as of sulfuric acid, were qualitatively interpreted. From the study of adsorption isotherms on these gels, they were found to exhibita higher adsorption capacity than the majority of those reported to date.

  12. Matrix effect in analysis of pesticide residues in fruits and vegetables by high performance liquid chromatography with quadrupole-time of flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    Andoralov A.M.

    2017-03-01

    Full Text Available For modern food safety control are using techniques that allow to determinate a large number of components. So for determination of pesticide residues in fruits and vegetables commonly used methods of gas and liquid chromatography with time-of-flight mass-spectrometric detection. This system allows to carry out quantitative determination several hundreds of pesticides and their identification by the characteristic fragments of the mass spectrum. The main problem when using mass spectrometric detection is a matrix effect, which is caused by the influence of matrix components extracted with pesticides from the sample. In this work, attempts have been made to reduce the influence of the matrix in the analysis of pesticide residues by high performance liquid chromatography with time of flight mass spectrometry (HPLC / TOFMS.

  13. Determination of cyanuric acid residues in catfish, trout, tilapia, salmon and shrimp by liquid chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Karbiwnyk, Christine M. [Animal Drugs Research Center, U.S. Food and Drug Administration, P.O. Box 25087, Denver, CO 80225-0087 (United States)], E-mail: christine.karbiwnyk@fda.hhs.gov; Andersen, Wendy C.; Turnipseed, Sherri B. [Animal Drugs Research Center, U.S. Food and Drug Administration, P.O. Box 25087, Denver, CO 80225-0087 (United States); Storey, Joseph M.; Madson, Mark R. [Denver District Laboratory, U.S. Food and Drug Administration, P.O. Box 25087, Denver, CO 80225-0087 (United States); Miller, Keith E. [Center for Veterinary Medicine, U.S. Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708 (United States); Gieseker, Charles M.; Miller, Ron A.; Rummel, Nathan G.; Reimschuessel, Renate [University of Denver, Department of Chemistry and Biochemistry, Denver, CO 80208 (United States)

    2009-04-01

    In May 2007, investigators discovered that waste material from the pet food manufacturing process contaminated with melamine (MEL) and/or cyanuric acid (CYA) had been added to hog and chicken feeds. At this time, investigators also learned that adulterated wheat gluten had been used in the manufacture of aquaculture feeds. Concern that the contaminated feed had been used in aquaculture and could enter the human food supply prompted the development of a method for the determination of CYA residues in the edible tissues of fish and shrimp. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) was employed as a sensitive technique for the analysis of CYA in catfish, tilapia, salmon, trout and shrimp tissue. CYA was extracted from ground fish or shrimp with an acetic acid solution, defatted with hexane, and isolated with a graphitic carbon black solid-phase extraction column. Residues were separated from matrix components using a porous graphitic carbon LC column, and then analyzed with electrospray ionization in negative ion mode on a triple quadrupole mass spectrometer. Selective reaction monitoring was performed on the [M-H]{sup -}m/z 128 ion resulting in the product ions m/z 85 and 42. Recoveries from catfish, tilapia and trout fortified with 10-100 {mu}g kg{sup -1} of CYA averaged 67% with a relative standard deviation (R.S.D.) of 18% (n = 107). The average method detection limit (MDL) for catfish, tilapia and trout is 3.5 {mu}g kg{sup -1}. An internal standard, {sup 13}C{sub 3}-labeled CYA, was used in the salmon and shrimp extractions. Average recovery of CYA from salmon was 91% (R.S.D. = 15%, n = 18) with an MDL of 7.4 {mu}g kg{sup -1}. Average recovery of CYA from shrimp was 85% (R.S.D. = 10%, n = 13) with an MDL of 3.5 {mu}g kg{sup -1}.

  14. Radiological conditions in areas of Kuwait with residues of depleted uranium. Report by an international group of experts

    International Nuclear Information System (INIS)

    2003-01-01

    radiological assessment of compliance with international radiation protection criteria and standards for areas with residues of DU munitions that has been carried out under the auspices of the IAEA. The IAEA assembled an international team of senior experts, including a representative of the United Nations Environment Programme (UNEP). The team was led by R.H. Clarke, Chairman of the International Commission on Radiological Protection.The experts visited Kuwait in September 2001 to assess the sites identified by the Government of Kuwait and to evaluate the available information. The 11 locations selected for the investigation included sites of military action during the Gulf War in which DU munitions were used, sites where DU residues still exist and areas where concern has been expressed about the possible contamination of water and foodstuffs with DU. In February 2002 a mission was conducted to collect samples at the identified sites.The sampling team included scientists from the IAEA Secretariat and from the Spiez Laboratory in Switzerland, representing the UNEP, together with experts from the laboratory of the Radiation Protection Department of the Ministry of Health of Kuwait. Around 200 environmental samples, including soil, water and vegetation, were collected during the campaign and subsequently analysed. The international team of experts prepared a report describing the findings of the measurement programme and the subsequent assessment performed by the team. This report provides a detailed description of the IAEA's investigation of the radiological conditions in Kuwait in relation to residues of DU, the results of the radiological assessment, the overall and site specific findings and conclusions of the assessment, and the recommendations of the expert group. On the basis of the measurements carried out at the sites investigated in the IAEA's study and summarized in this report, DU does not pose a radiological hazard to the population of Kuwait. No persons who might

  15. Mass-loss rates from decomposition of plant residues in spruce forests near the northern tree line subject to strong air pollution.

    Science.gov (United States)

    Lukina, Natalia V; Orlova, Maria A; Steinnes, Eiliv; Artemkina, Natalia A; Gorbacheva, Tamara T; Smirnov, Vadim E; Belova, Elena A

    2017-08-01

    Mass-loss rates during the early phase of decomposition of plant residues were studied for a period of 3 years in Norway spruce forests subjected to air pollution by Cu-Ni smelters on the Kola Peninsula, northwest Russia. Litterbags were deployed in two main patches of forests at the northern tree line, between and below the crowns of spruce trees older than 100 years. The study results demonstrated the dependence of the decomposition rates on the initial concentrations of nutrients and the C/N and lignin/N ratios in plant residues. Lower rates of mass loss in forests subject to air pollution may be related to low quality of plant residues, i.e. high concentrations of heavy metals, low concentrations of nutrients, and high lignin/N and C/N ratios. The increased losses of Ca, Mg, K, and Mn from plant residues in these forests compared to the reference were, probably, related to leaching of their compounds from the residues. The relatively high rates of heavy metal accumulation in the residues were most likely related to uptake of pollutants from the atmosphere, as well as to the lower mass-loss rates. The present study results demonstrate that the forest patchiness should be taken into account in assessment and predictions of decomposition rates in Norway spruce forests. Mass-loss rates of plant residues below the crowns of old spruce trees were significantly lower than those in the patches between the crowns. This was explained by the high C/N and lignin/N ratios in the residues of evergreens which contribute significantly to litterfall below the crowns and by lower soil temperature during winter and spring below the crowns. In addition, a lower amount of precipitation reaching the forest floor below the dense, long crowns of old Norway spruce trees may result in considerably lower washing out of the organic compounds from the residues. Lower mass-loss rates below the crowns of old spruce trees may be part of the evidence that the old-growth spruce forests can

  16. Effect of deuteration on some structural parameters of methyl groups in proteins as evaluated by residual dipolar couplings

    International Nuclear Information System (INIS)

    Mittermaier, Anthony; Kay, Lewis E.

    2002-01-01

    One bond methyl 1 H- 13 C and 13 C methyl - 13 C scalar and residual dipolar couplings have been measured at sites in an 15 N, 13 C, ∼ 50% 2 H labeled sample of the B1 immunoglobulin binding domain of peptostreptococcal protein L to investigate changes in the structure of methyl groups in response to deuterium substitution. Both one bond methyl 1 H- 13 C and 13 C methyl - 13 C scalar coupling constants have been found to decrease slightly with increasing deuterium content. Previous studies have shown that 1 H- 13 C couplings in methyl groups are exquisitely sensitive to electronic structure, with decreases in coupling values as a function of deuteration consistent with a slight lengthening of the remaining H-C bonds. Changes in the H methyl C methyl C angle are found to be small, with average differences on the order of 0.3 ± 0.1 deg. and 0.4 ± 0.2 deg. between CH 3 , CH 2 D and CH 3 , CHD 2 isotopomers, respectively. Knowledge of methyl geometry is a prerequisite for the extraction of accurate dynamics parameters from spin relaxation studies involving these groups

  17. [Determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes by gas chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Qun; Liu, Chunhua; Wu, Nancun; Wu, Xiaofang; Li, Shuhuai

    2014-08-01

    An analytical method was established for the determination of propargite, tebuconazole and bromopropylate in Taiwan green jujubes (Zizyphus mauritiana Lam) by gas chromatography-tandem mass spectrometry (GC-MS/MS). The sample was extracted with acetonitrile from the Taiwan green jujubes after treated with a homogenizer. The organic phase was then separated from water phase by adding NaCl. The extract was further purified on a carbon/ NH2 cartridge with elution solvents of acetonitrile/toluene (3:1, v/v). Finally, the target analytes were separated by a capillary gas chromatographic column SLB-5MS (30 m x 0. 25 mm x 0. 25 μm). A tandem quadrupole mass spectrometer operated in either full scan mode or in MS/MS mode for multiple reaction monitoring (MRM) was used for the qualitative and quantitative analysis of the constituents, respectively. The results showed that the average recoveries of the three pesticides ranged from 75. 8% to 103. 6% with the RSDs of 1. 7%-9. 3% at the spiking levels from 0.01 mg/kg to 0. 50 mg/kg (n= 5). The calibration curves showed good linearity in the range of 0.01-0.50 mg/kg, with the determination coefficients over 0.99 (R2>0.99). The limits of quantification (LOQs) were 0.01 mg/kg for propargite, tebuconazole and bromopropylate in Taiwan green jujubes. The method is available for the determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes.

  18. Variability of matrix effects in liquid and gas chromatography - mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops

    Science.gov (United States)

    Gas and liquid chromatography (GC and LC) coupled to sophisticated mass spectrometry (MS) instruments are among the most powerful analytical tools currently available to monitor pesticide residues in food, among other applications. However, both GC-MS and LC-MS are susceptible to matrix effects whi...

  19. Residuation theory

    CERN Document Server

    Blyth, T S; Sneddon, I N; Stark, M

    1972-01-01

    Residuation Theory aims to contribute to literature in the field of ordered algebraic structures, especially on the subject of residual mappings. The book is divided into three chapters. Chapter 1 focuses on ordered sets; directed sets; semilattices; lattices; and complete lattices. Chapter 2 tackles Baer rings; Baer semigroups; Foulis semigroups; residual mappings; the notion of involution; and Boolean algebras. Chapter 3 covers residuated groupoids and semigroups; group homomorphic and isotone homomorphic Boolean images of ordered semigroups; Dubreil-Jacotin and Brouwer semigroups; and loli

  20. A Liquid Chromatography - Tandem Mass Spectrometry Approach for the Identification of Mebendazole Residue in Pork, Chicken, and Horse.

    Directory of Open Access Journals (Sweden)

    Ji Sun Lee

    Full Text Available A confirmatory and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS/MS for the determination of mebendazole and its hydrolyzed and reduced metabolites in pork, chicken, and horse muscles was developed and validated in this study. Anthelmintic compounds were extracted with ethyl acetate after sample mixture was made alkaline followed by liquid chromatographic separation using a reversed phase C18 column. Gradient elution was performed with a mobile phase consisting of water containing 10 mM ammonium formate and methanol. This confirmatory method was validated according to EU requirements. Evaluated validation parameters included specificity, accuracy, precision (repeatability and within-laboratory reproducibility, analytical limits (decision limit and detection limit, and applicability. Most parameters were proved to be conforming to the EU requirements. The decision limit (CCα and detection capability (CCβ for all analytes ranged from 15.84 to 17.96 μgkg-1. The limit of detection (LOD and the limit of quantification (LOQ for all analytes were 0.07 μgkg-1 and 0.2 μgkg-1, respectively. The developed method was successfully applied to monitoring samples collected from the markets in major cities and proven great potential to be used as a regulatory tool to determine mebendazole residues in animal based foods.

  1. Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

    Directory of Open Access Journals (Sweden)

    Gajda Anna

    2015-09-01

    Full Text Available A liquid chromatography – tandem mass spectrometry (LC-MS/MS method for the determination of oxytetracycline (OTC, 4-epi oxytetracycline (4-epi OTC, tetracycline (TC, 4-epi tetracycline (4-epi TC, chlortetracycline (CTC, 4-epi chlortetracycline (4-epi CTC, doxycycline (DC, minocycline (MINO, methacycline (META and rolitetracycline (ROLI residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% – 103.6%. The decision limits were from 109.0 to 119.8 μg/kg and detection capability varied within the range of 122.2 to 137.6 μg/kg, depending on the analyte.

  2. Determination of alkylphenolic residues in fresh fruits and vegetables by extractive steam distillation and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Deng-Kai; Ding, Wang-Hsien

    2005-09-23

    This study describes a simple and sensitive method for determining the alkylphenolic compounds, 4-tert-octylphenol (4-t-OP), 4-nonylphenol isomers (4-NPs), and their monoethoxylates (4-t-OP1EO and 4-NP1EOs), in fresh fruits and vegetables. The method involves extracting a sample by a modified Nielson-Kryger steam distillation extraction using n-hexane for 1 h. The alkylphenolic compounds were identified and quantitated by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. Various pH values and amounts of NaCl added to the sample solution were evaluated as extraction conditions. The quantitation limit of this method was less than 0.2 ng/g in 10 g (fresh weight) of sample. Recovery of alkylphenolic compounds in spiked samples exceeded 64% while R.S.D. ranged from 1.0 to 9.8%. Alkylphenolic residues were detected in fresh fruits and vegetables at concentrations of 4-NPs and 4-t-OP from n.d. to 16 ng/g and from n.d. to 4.8 ng/g (fresh weight), respectively. NP1EO and OP1EO were always below the quantitation limit.

  3. Determination of alkylphenol residues in baby-food purees by steam distillation extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Chia-Tien; Cheng, Chin-Yuan; Ding, Wang-Hsien

    2008-02-01

    This paper describes a simple and sensitive method for determining alkylphenols namely 4-tert-octylphenol (4-t-OP) and the isomers of 4-nonylphenol (4-NPs) present in various types of baby-food purees. The method involves extracting a sample with n-hexane for 1h using a modified Nielson-Kryger steam distillation extraction system and then identifying and quantitating the alkylphenols using a gas chromatography-mass spectrometry (GC-MS) operated in the selected ion monitoring (SIM) mode. The extraction conditions were evaluated at various values of pH of the sample solution. The limits of quantitation for this method were 0.2 ng/g from 1.0 g (wet weight) samples of 4-t-OP and the 4-NPs. The intra- and interbatch precisions and accuracies were also determined. The precision, in terms of the relative standard deviation (RSD), were less than 8%. Most of the recoveries of the alkylphenols from various spiked samples exceeded 60%, while the values of RSD ranged from 1% to 10%. Alkylphenol residues were detected in baby-food purees at concentrations of up to 19 ng/g (wet weight) for 4-t-OP and up to 21 ng/g (wet weight) for the 4-NPs.

  4. Pesticide residue determination in surface waters by stir bar sorptive extraction and liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Giordano, A; Fernández-Franzón, M; Ruiz, M J; Font, G; Picó, Y

    2009-03-01

    In this stir bar sorptive extraction (SBSE) method, 16 pesticides were extracted from surface water samples by sorption onto 1 mm polydimethylsiloxane layer coated on a 10-mm-length stir bar magnet. After liquid desorption of the analytes with 1 ml of methanol, the detection was performed on a liquid chromatography-tandem mass spectrometry with a triple quadrupole (QqQ) analyzer using selected reaction monitoring mode via electrospray ionization. Parameters affecting SBSE operation, including sample volume, salt addition, extraction time, stirring rate, and desorption conditions, have been evaluated. The optimized SBSE method required two 50 ml aliquots of surface water samples, one aliquot was added of 30% NaCl and stirred at 900 rpm during 1 h for testing five pesticides with log K(o/w) 3. The method was validated in spiked surface water samples at limits of quantifications (LOQs) and ten times the LOQs showing recoveries Albufera Lake and surrounding channels, showing that SBSE is a powerful tool for routine control analysis of pesticide residues in surface water.

  5. Renormalization group and relations between scattering amplitudes in a theory with different mass scales

    International Nuclear Information System (INIS)

    Gulov, A.V.; Skalozub, V.V.

    2000-01-01

    In the Yukawa model with two different mass scales the renormalization group equation is used to obtain relations between scattering amplitudes at low energies. Considering fermion-fermion scattering as an example, a basic one-loop renormalization group relation is derived which gives possibility to reduce the problem to the scattering of light particles on the external field substituting a heavy virtual state. Applications of the results to problem of searching new physics beyond the Standard Model are discussed [ru

  6. Estimating the mass of the Local Group using machine learning applied to numerical simulations

    Science.gov (United States)

    McLeod, M.; Libeskind, N.; Lahav, O.; Hoffman, Y.

    2017-12-01

    We present a new approach to calculating the combined mass of the Milky Way (MW) and Andromeda (M31), which together account for the bulk of the mass of the Local Group (LG). We base our work on an ensemble of 30,190 halo pairs from the Small MultiDark simulation, assuming a ΛCDM (Cosmological Constant and Cold Dark Matter) cosmology. This is used in conjunction with machine learning methods (artificial neural networks, ANN) to investigate the relationship between the mass and selected parameters characterising the orbit and local environment of the binary. ANN are employed to take account of additional physics arising from interactions with larger structures or dynamical effects which are not analytically well understood. Results from the ANN are most successful when the velocity shear is provided, which demonstrates the flexibility of machine learning to model physical phenomena and readily incorporate new information. The resulting estimate for the Local Group mass, when shear information is included, is 4.9×1012Msolar, with an error of ±0.8×1012Msolar from the 68% uncertainty in observables, and a r.m.s. scatter interval of +1.7‑1.3×1012Msolar estimated scatter from the differences between the model estimates and simulation masses for a testing sample of halo pairs. We also consider a recently reported large relative transverse velocity of M31 and the Milky Way, and produce an alternative mass estimate of 3.6±0.3+2.1‑1.3×1012Msolar. Although the methods used predict similar values for the most likely mass of the LG, application of ANN compared to the traditional Timing Argument reduces the scatter in the log mass by approximately half when tested on samples from the simulation.

  7. Thermal desorption extraction proton transfer reaction mass spectrometer (TDE-PTR-MS) for rapid determination of residual solvent and sterilant in disposable medical devices.

    Science.gov (United States)

    Wang, Yujie; Shen, Chengyin; Li, Jianquan; Wang, Hongmei; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2011-07-15

    Thermal desorption extraction proton transfer reaction mass spectrometer (TDE-PTR-MS) has been exploited to provide rapid determination of residual solvent and sterilant like cyclohexanone (CHX) and ethylene oxide (EO) in disposable medical devices. Two novel methods are proposed for the quantification of residual chemicals in the polyvinyl chloride infusion sets with our homemade PTR-MS. In the first method, EO residue in the solid infusion sets (y, mgset(-1)) is derived through the determination of EO gas concentration within its packaging bag (x, ppm) according to the correlative equation of y=0.00262x. In the second one, residual EO and CHX in the solid infusion sets are determined through a time integral of their respective mass emission rates. The validity of the proposed methods is demonstrated by comparison with the experimental results from the exhaustive extraction method. Due to fast response, absolute concentration determination and high sensitivity, the TDE-PTR-MS is suggested to be a powerful tool for the quality inspection of disposable medical devices including the quantitative determination of residual solvent and sterilant like CHX and EO. Copyright © 2011 Elsevier B.V. All rights reserved.

  8. Application and evaluation of a high-resolution mass spectrometry screening method for veterinary drug residues in incurred fish and imported aquaculture samples.

    Science.gov (United States)

    Turnipseed, Sherri B; Storey, Joseph M; Wu, I-Lin; Gieseker, Charles M; Hasbrouck, Nicholas R; Crosby, Tina C; Andersen, Wendy C; Lanier, Shanae; Casey, Christine R; Burger, Robert; Madson, Mark R

    2018-02-14

    The ability to detect chemical contaminants, including veterinary drug residues in animal products such as fish, is an important example of food safety analysis. In this paper, a liquid chromatography high-resolution mass spectrometry (LC-HRMS) screening method using a quadrupole-Orbitrap instrument was applied to the analysis of veterinary drug residues in incurred tissues from aquacultured channel catfish, rainbow trout, and Atlantic salmon and imported aquacultured products including European eel, yellow croaker, and tilapia. Compared to traditional MS methods, the use of HRMS with nontargeted data acquisition and exact mass measurement capability greatly increased the scope of compounds that could be monitored simultaneously. The fish samples were prepared for analysis using a simple efficient procedure that consisted of an acidic acetonitrile extraction followed by solid phase extraction cleanup. Two different HRMS acquisition programs were used to analyze the fish extracts. This method detected and identified veterinary drugs including quinolones, fluoroquinolones, avermectins, dyes, and aminopenicillins at residue levels in fish that had been dosed with those compounds. A metabolite of amoxicillin, amoxicillin diketone, was also found at high levels in catfish, trout, and salmon. The method was also used to characterize drug residues in imported fish. In addition to confirming findings of fluoroquinolone and sulfonamide residues that were found by traditional targeted MS methods, several new compounds including 2-amino mebendazole in eel and ofloxacin in croaker were detected and identified. Graphical Abstract Aquacultured samples are analyzed with a high-resolution mass spectrometry screening method to detect and identify unusual veterinary drug residues including ofloxacin in an imported fish.

  9. Liquid chromatography with mass spectrometry in tandem mode applied for the identification of wine markers in residues from ancient Egyptian vessels.

    Science.gov (United States)

    Guasch-Jané, Maria Rosa; Ibern-Gómez, Maite; Andrés-Lacueva, Cristina; Jáuregui, Olga; Lamuela-Raventós, Rosa Maria

    2004-03-15

    Presented in this paper is a new method for the identification of tartaric acid as a wine marker in archaeological residues from Egyptian vessels using liquid chromatography with mass spectrometry in tandem mode (LC/MS/MS). Owing to the special characteristics of these samples, such as the dryness and the small quantity available for analysis, it was necessary to have a very sensitive and highly specific analytical method to detect tartaric acid at trace levels in the residues. Furthermore, an alkaline fusion was carried out to identify syringic acid derived from malvidin as a red wine marker, in a deposit residue from a wine jar found at the tomb of king Tutankhamun. Malvidin-3-glucoside, the main anthocyanin that gives young wines their red color, polymerizes with aging into more stable pigments. However, the presence of malvidin in ancient residues can be proved by alkaline fusion of the residue to release syringic acid from the pigment, which has been identified, here for the first time, by using the LC/MS/MS method revealing the red grape origin of an ancient Egyptian wine residue.

  10. Flexible xxx-asp/asn and gly-xxx residues of equine cytochrome C in matrix-assisted laser desorption/ionization in-source decay mass spectrometry.

    Science.gov (United States)

    Takayama, Mitsuo

    2012-01-01

    The backbone flexibility of a protein has been studied from the standpoint of the susceptibility of amino acid residues to in-source decay (ISD) in matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). Residues more susceptible to MALDI-ISD, namely Xxx-Asp/Asn and Gly-Xxx, were identified from the discontinuous intense peak of c'-ions originating from specific cleavage at N-Cα bonds of the backbone of equine cytochrome c. The identity of the residues susceptible to ISD was consistent with the known flexible backbone amides as estimated by hydrogen/deuterium exchange (HDX) experiments. The identity of these flexible amino acid residues (Asp, Asn, and Gly) is consistent with the fact that these residues are preferred in flexible secondary structure free from intramolecular hydrogen-bonded structures such as α-helix and β-sheet. The MALDI-ISD spectrum of equine cytochrome c gave not only intense N-terminal side c'-ions originating from N-Cα bond cleavage at Xxx-Asp/Asn and Gly-Xxx residues, but also C-terminal side complement z'-ions originating from the same cleavage sites. The present study implies that MALDI-ISD can give information about backbone flexibility of proteins, comparable with the protection factors estimated by HDX.

  11. Flexible Xxx–Asp/Asn and Gly–Xxx Residues of Equine Cytochrome c in Matrix-Assisted Laser Desorption/Ionization In-Source Decay Mass Spectrometry

    Science.gov (United States)

    Takayama, Mitsuo

    2012-01-01

    The backbone flexibility of a protein has been studied from the standpoint of the susceptibility of amino acid residues to in-source decay (ISD) in matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). Residues more susceptible to MALDI-ISD, namely Xxx–Asp/Asn and Gly–Xxx, were identified from the discontinuous intense peak of c′-ions originating from specific cleavage at N–Cα bonds of the backbone of equine cytochrome c. The identity of the residues susceptible to ISD was consistent with the known flexible backbone amides as estimated by hydrogen/deuterium exchange (HDX) experiments. The identity of these flexible amino acid residues (Asp, Asn, and Gly) is consistent with the fact that these residues are preferred in flexible secondary structure free from intramolecular hydrogen-bonded structures such as α-helix and β-sheet. The MALDI-ISD spectrum of equine cytochrome c gave not only intense N-terminal side c′-ions originating from N–Cα bond cleavage at Xxx–Asp/Asn and Gly–Xxx residues, but also C-terminal side complement z′-ions originating from the same cleavage sites. The present study implies that MALDI-ISD can give information about backbone flexibility of proteins, comparable with the protection factors estimated by HDX. PMID:24349908

  12. Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

    2016-01-01

    The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed.

  13. A research on relationship between ABO blood groups and body mass index among Turkish seafarers.

    Science.gov (United States)

    Nas, Selçuk; Fışkın, Remzi

    2017-01-01

    The present study aims to investigate and to reveal the relationship between ABO blood groups and body mass index (BMI) and obesity among Turkish seafarers by using the health examination reports data obtained from 2009 to 2016. The data on age, gender, weight, height and blood groups obtained from 298,247 medical examination reports of Turkish seafarers were used with the official permission of Directorate General of Health for Border and Coastal Areas. Only 116,871 reports included blood group data. Regression and analysis of variance (ANOVA) tests were performed to survey relationship between variables. The results of the study were compared with other studies in the related literature. It has been revealed that AB Rh (-) group was associated the highest mean BMI value (mean: 25.952). It is suggested that seafarers with AB Rh (-) blood group, who have the highest mean BMI value, should pay special attention to their weight.

  14. Functional group composition of ambient and source organic aerosols determined by tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    J. Dron

    2010-08-01

    Full Text Available The functional group composition of various organic aerosols (OA is investigated using a recently developed analytical approach based on atmospheric pressure chemical ionisation-tandem mass spectrometry (APCI-MS/MS. The determinations of three functional groups contents are performed quantitatively by neutral loss (carboxylic and carbonyl groups, R-COOH and R-CO-R´ respectively and precursor ion (nitro groups, R-NO2 scanning modes of a tandem mass spectrometer. Major organic aerosol sources are studied: vehicular emission and wood combustion for primary aerosol sources; and a secondary organic aerosol (SOA produced through photooxidation of o-xylene. The results reveal significant differences in the functional group contents of these source aerosols. The laboratory generated SOA is dominated by carbonyls while carboxylics are preponderate in the wood combustion particles. On the other hand, vehicular emissions are characterised by a strong nitro content. The total amount of the three functional groups accounts for 1.7% (vehicular to 13.5% (o-xylene photooxidation of the organic carbon. Diagnostic functional group ratios are then used to tentatively discriminate sources of particles collected in an urban background environment located in an Alpine valley (Chamonix, France during a strong winter pollution event. The three functional groups under study account for a total functionalisation rate of 2.2 to 3.8% of the organic carbon in this ambient aerosol, which is also dominated by carboxylic moieties. In this particular case study of a deep alpine valley during winter, we show that the nitro- and carbonyl-to-carboxylic diagnostic ratios can be a useful tool to discriminate sources. In these conditions, the total OA concentrations are highly dominated by wood combustion OA. This result is confirmed by an organic markers source apportionment approach which assess a wood burning organic carbon contribution of about 60

  15. Functional group composition of ambient and source organic aerosols determined by tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dron, J.; El Haddad, I.; Temime-Roussel, B.; Wortham, H.; Marchand, N. [Univ Aix Marseille, CNRS, Lab Chim Provence, Equipe Instrumentat and React Atmospher, UMR 6264, F-13331 Marseille 3 (France); Jaffrezo, J.L. [Univ Grenoble 1, CNRS, UMR 5183, Lab Glaciol and Geophys Environm, F-38402 St Martin Dheres (France)

    2010-07-01

    The functional group composition of various organic aerosols (OA) is investigated using a recently developed analytical approach based on atmospheric pressure chemical ionisation-tandem mass spectrometry (APCIMS/MS). The determinations of three functional groups contents are performed quantitatively by neutral loss (carboxylic and carbonyl groups, R-COOH and R-CO-R' respectively) and precursor ion (nitro groups, R-NO{sub 2}) scanning modes of a tandem mass spectrometer. Major organic aerosol sources are studied: vehicular emission and wood combustion for primary aerosol sources; and a secondary organic aerosol (SOA) produced through photooxidation of o-xylene. The results reveal significant differences in the functional group contents of these source aerosols. The laboratory generated SOA is dominated by carbonyls while carboxylics are preponderate in the wood combustion particles. On the other hand, vehicular emissions are characterised by a strong nitro content. The total amount of the three functional groups accounts for 1.7% (vehicular) to 13.5% (o-xylene photooxidation) of the organic carbon. Diagnostic functional group ratios are then used to tentatively discriminate sources of particles collected in an urban background environment located in an Alpine valley (Chamonix, France) during a strong winter pollution event. The three functional groups under study account for a total functionalization rate of 2.2 to 3.8% of the organic carbon in this ambient aerosol, which is also dominated by carboxylic moieties. In this particular case study of a deep alpine valley during winter, we show that the nitro- and carbonyl-to-carboxylic diagnostic ratios can be a useful tool to discriminate sources. In these conditions, the total OA concentrations are highly dominated by wood combustion OA. This result is confirmed by an organic markers source apportionment approach which assess a wood burning organic carbon contribution of about 60%. Finally, examples of functional

  16. Development and validation of a multi-residue method for the detection of a wide range of hormonal anabolic compounds in hair using gas chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    Rambaud, Lauriane; Monteau, Fabrice; Deceuninck, Yoann; Bichon, Emmanuelle; Andre, Francois; Le Bizec, Bruno

    2007-01-01

    The monitoring of anabolic steroid residues in hair is undoubtedly one of the most efficient strategies to demonstrate the long-term administration of these molecules in meat production animals. A multi-residue sample preparation procedure was developed and validated for 28 steroids. A 100 mg hair sample was grinded into powder and extracted at 50 deg. C with methanol. After acidic hydrolysis and extraction with ethyl acetate, phenolsteroids, such as estrogens, resorcyclic acid lactones and stilbens in one hand, are separated from androgens and progestagens in the other hand. Solid phase extractions were performed before applying a specific derivatisation for each compound sub-group. Detection and identification were achieved using gas chromatography-tandem mass spectrometry with acquisition in the selected reaction monitoring mode after electron ionisation. The method was validated according to the 2002/657/EC guideline. Decision limits (CCα) for main steroids were in the 0.1-10 μg kg -1 range

  17. A CORRELATION BETWEEN ABO BLOOD GROUPS AND BODY MASS INDEX AMONG MEDICAL STUDENTS

    Directory of Open Access Journals (Sweden)

    Sarbjit Singh

    2017-11-01

    Full Text Available BACKGROUND ABO blood groups are associated with some important chronic diseases, obesity being the major risk factor is rising rapidly globally. The present study seeks to determine if there is any association between ABO blood groups and body mass index. MATERIALS AND METHODS The present study involve 200 medical students, 102 boys and 98 girls in the age group of 18-23 years in the Government Medical College, Amritsar. Weight, height for BMI and blood groups were determined in order to find any association between ABO blood group and BMI. RESULTS Overweight and obesity was found more prevalent in boys than girls, 22.5% students were overweight and 15.5% were obese. The prevalence of overweight was (24.52% boys and 20.40% girls and prevalence of obesity was (25.49% boys and 5.10% girls. Blood group B was reported the most common blood groups (37.5% followed by blood group O (32.0%, while blood groups A and AB were found 19.5% and 11% of participants, respectively. The prevalence of overweight (BMI 25-29.9 among participants based on blood group O, A, AB and B was 29.69%, 25.64%, 18.18%, 16.00%, while obesity (BMI >30 among participants based on blood groups B, O, A and AB was 24.00%, 10.94%, 10.26% and 9.09%. CONCLUSION Prevalence of overweight and obesity was more in blood group O and B respectively and was more in males than females

  18. Wide-Scope Screening Method for Multiclass Veterinary Drug Residues in Fish, Shrimp, and Eel Using Liquid Chromatography-Quadrupole High-Resolution Mass Spectrometry.

    Science.gov (United States)

    Turnipseed, Sherri B; Storey, Joseph M; Lohne, Jack J; Andersen, Wendy C; Burger, Robert; Johnson, Aaron S; Madson, Mark R

    2017-08-30

    A screening method for veterinary drug residues in fish, shrimp, and eel using LC with a high-resolution MS instrument has been developed and validated. The method was optimized for over 70 test compounds representing a variety of veterinary drug classes. Tissues were extracted by vortex mixing with acetonitrile acidified with 2% acetic acid and 0.2% p-toluenesulfonic acid. A centrifuged portion of the extract was passed through a novel solid phase extraction cartridge designed to remove interfering matrix components from tissue extracts. The eluent was then evaporated and reconstituted for analysis. Data were collected with a quadrupole-Orbitrap high-resolution mass spectrometer using both nontargeted and targeted acquisition methods. Residues were detected on the basis of the exact mass of the precursor and a product ion along with isotope pattern and retention time matching. Semiquantitative data analysis compared MS 1 signal to a one-point extracted matrix standard at a target testing level. The test compounds were detected and identified in salmon, tilapia, catfish, shrimp, and eel extracts fortified at the target testing levels. Fish dosed with selected analytes and aquaculture samples previously found to contain residues were also analyzed. The screening method can be expanded to monitor for an additional >260 veterinary drugs on the basis of exact mass measurements and retention times.

  19. Mass, momentum, and energy flux conservation between linear and nonlinear steady-state wave groups

    Science.gov (United States)

    Liu, Zeng; Xu, Dali; Liao, Shijun

    2017-12-01

    This paper provides a mass, momentum, and energy flux conservation analysis between the linear and nonlinear steady-state wave groups. Convergent high-order solutions for nonlinear wave groups with multiple steady-state near resonances in deep water have been obtained by means of the homotopy analysis method. The small divisors associated with nearly resonant components are transformed to singularities that are originally caused by exact resonances by a piecewise auxiliary linear operator. Both two primary components and other nearly resonant ones are considered in the initial guess to search for finite amplitude wave groups. It is found that as nonlinearity of wave groups increases, more wave components appear in the spectrum due to the nearly resonant interactions. The nonlinear wave fields change from the initial bi-chromatic waves that contain only two nontrivial primary components into the steady-state resonant waves that contain both two primary components and other nearly resonant ones. The conservation of mean rates of mass, momentum, and energy fluxes is established between the nonlinear wave groups and linear waves that are combined by two primary components with the same frequencies as in nonlinear wave groups. Comparison of the linear and nonlinear wave fields shows that the nearly resonant components influence the wave field distribution significantly: the nonlinear free surfaces have more peaked crests, steeper troughs, and more flatten wave nodes, and the related velocities at the crests and troughs increase more rapidly with the nonlinearity. All of these findings are helpful to enrich and deepen our understanding about nonlinear wave groups.

  20. Carboxylic acid functional group analysis using constant neutral loss scanning-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dron, Julien [Laboratoire de Chimie et Environnement, Marseille Universites (case 29), 3 place Victor Hugo, 13331 Marseille Cedex 3 (France)], E-mail: julien.dron@up.univ-mrs.fr; Eyglunent, Gregory; Temime-Roussel, Brice; Marchand, Nicolas; Wortham, Henri [Laboratoire de Chimie et Environnement, Marseille Universites (case 29), 3 place Victor Hugo, 13331 Marseille Cedex 3 (France)

    2007-12-12

    The present study describes the development of a new analytical technique for the functional group determination of the carboxylic moiety using atmospheric pressure chemical ionization-mass spectrometry (APCI-MS/MS) operated in the constant neutral loss scanning (CNLS) mode. Carboxylic groups were first derivatized into their corresponding methyl esters by reacting with BF{sub 3}/methanol mix and the reaction mixture was then directly injected into the APCI chamber. The loss of methanol (m/z = 32 amu) resulting from the fragmentation of the protonated methyl esters was then monitored. Applying this method together with a statistical approach to reference mixtures containing 31 different carboxylic acids at randomly calculated concentrations demonstrated its suitability for quantitative functional group measurements with relative standard deviations below 15% and a detection limit of 0.005 mmol L{sup -1}. Its applicability to environmental matrices was also shown through the determination of carboxylic acid concentrations inside atmospheric aerosol samples. To the best of our knowledge, it is the first time that the tandem mass spectrometry was successfully applied to functional group analysis, offering great perspectives in the characterization of complex mixtures which are prevailing in the field of environmental analysis as well as in the understanding of the chemical processes occurring in these matrices.

  1. Carboxylic acid functional group analysis using constant neutral loss scanning-mass spectrometry

    International Nuclear Information System (INIS)

    Dron, Julien; Eyglunent, Gregory; Temime-Roussel, Brice; Marchand, Nicolas; Wortham, Henri

    2007-01-01

    The present study describes the development of a new analytical technique for the functional group determination of the carboxylic moiety using atmospheric pressure chemical ionization-mass spectrometry (APCI-MS/MS) operated in the constant neutral loss scanning (CNLS) mode. Carboxylic groups were first derivatized into their corresponding methyl esters by reacting with BF 3 /methanol mix and the reaction mixture was then directly injected into the APCI chamber. The loss of methanol (m/z = 32 amu) resulting from the fragmentation of the protonated methyl esters was then monitored. Applying this method together with a statistical approach to reference mixtures containing 31 different carboxylic acids at randomly calculated concentrations demonstrated its suitability for quantitative functional group measurements with relative standard deviations below 15% and a detection limit of 0.005 mmol L -1 . Its applicability to environmental matrices was also shown through the determination of carboxylic acid concentrations inside atmospheric aerosol samples. To the best of our knowledge, it is the first time that the tandem mass spectrometry was successfully applied to functional group analysis, offering great perspectives in the characterization of complex mixtures which are prevailing in the field of environmental analysis as well as in the understanding of the chemical processes occurring in these matrices

  2. A 17-billion-solar-mass black hole in a group galaxy with a diffuse core.

    Science.gov (United States)

    Thomas, Jens; Ma, Chung-Pei; McConnell, Nicholas J; Greene, Jenny E; Blakeslee, John P; Janish, Ryan

    2016-04-21

    Quasars are associated with and powered by the accretion of material onto massive black holes; the detection of highly luminous quasars with redshifts greater than z = 6 suggests that black holes of up to ten billion solar masses already existed 13 billion years ago. Two possible present-day 'dormant' descendants of this population of 'active' black holes have been found in the galaxies NGC 3842 and NGC 4889 at the centres of the Leo and Coma galaxy clusters, which together form the central region of the Great Wall--the largest local structure of galaxies. The most luminous quasars, however, are not confined to such high-density regions of the early Universe; yet dormant black holes of this high mass have not yet been found outside of modern-day rich clusters. Here we report observations of the stellar velocity distribution in the galaxy NGC 1600--a relatively isolated elliptical galaxy near the centre of a galaxy group at a distance of 64 megaparsecs from Earth. We use orbit superposition models to determine that the black hole at the centre of NGC 1600 has a mass of 17 billion solar masses. The spatial distribution of stars near the centre of NGC 1600 is rather diffuse. We find that the region of depleted stellar density in the cores of massive elliptical galaxies extends over the same radius as the gravitational sphere of influence of the central black holes, and interpret this as the dynamical imprint of the black holes.

  3. Mass spectrometric profiling of valepotriates possessing various acyloxy groups from Valeriana jatamansi.

    Science.gov (United States)

    Lin, Sheng; Ye, Ji; Liang, Xu; Zhang, Xi; Su, Juan; Fu, Peng; Lv, Di-Ya; Shan, Lei; Shen, Yun-Heng; Li, Hui-Liang; Yang, Xian-Wen; Zhang, Wei-Dong

    2015-11-01

    Valepotriates, plant secondary metabolites of the family Valerianaceae, contain various acyloxy group linkages to the valepotriate nucleus and exhibit significant biological activities. Identification of valepotriates is important to uncover potential lead compounds for the development of new sedative and antitumor drugs. However, making their structure elucidation by nuclear magnetic resonance (NMR) experiments is too difficult to be realized because of the overlapped carbonyl carbon signals of acyloxy groups substituted at different positions. Thus, the mass spectrometric profiling of these compounds in positive ion mode was developed to unveil the exact linkage of acyloxy group and the core of valepotriate. In this study, electrospray ionization tandem multistage mass spectrometry (ESI-MS/MS(n)) in ion trap and collision-induced dissociation tandem MS were used to investigate the fragmentation pathways of four types of valepotriates in Valeriana jatamansi, including 5-hydroxy-5,6-dihydrovaltrate hydrin (5-hydroxy-5,6-dihydrovaltrate chlorohydrin), 5,6-dihydrovaltrate hydrin (5,6-dihydrovaltrate chlorohydrin), 5-hydroxy-5,6-dihydrovaltrate and valtrate hydrin (valtrate chlorohydrin). The high-resolution mass spectrum (HRMS) data of all the investigated valepotriates from quadrupole time-of-flight MS/MS were used as a supportive of the fragmentation rules we hypothesized from ion-trap stepwise MS(n). As a result, the loss sequence of acyloxy groups and the abundance of key product ions, in combination with the characteristic product ions corresponding to the valepotriate nucleus, could readily differentiate the four different types of valepotriates. The summarized fragmentation rules were also successfully exploited for the structural characterization of three new trace valepotriates from V. jatamansi. The results indicated that the developed analytical method could be employed as a rapid, effective technique for structural characterization of valepotriates

  4. Luminosities and mass-loss rates of Local Group AGB stars and red supergiants

    Science.gov (United States)

    Groenewegen, M. A. T.; Sloan, G. C.

    2018-01-01

    Context. Mass loss is one of the fundamental properties of asymptotic giant branch (AGB) stars, and through the enrichment of the interstellar medium, AGB stars are key players in the life cycle of dust and gas in the universe. However, a quantitative understanding of the mass-loss process is still largely lacking. Aims: We aim to investigate mass loss and luminosity in a large sample of evolved stars in several Local Group galaxies with a variety of metalliticies and star-formation histories: the Small and Large Magellanic Cloud, and the Fornax, Carina, and Sculptor dwarf spheroidal galaxies (dSphs). Methods: Dust radiative transfer models are presented for 225 carbon stars and 171 oxygen-rich evolved stars in several Local Group galaxies for which spectra from the Infrared Spectrograph on Spitzer are available. The spectra are complemented with available optical and infrared photometry to construct spectral energy distributions. A minimization procedure was used to determine luminosity and mass-loss rate (MLR). Pulsation periods were derived for a large fraction of the sample based on a re-analysis of existing data. Results: New deep K-band photometry from the VMC survey and multi-epoch data from IRAC (at 4.5 μm) and AllWISE and NEOWISE have allowed us to derive pulsation periods longer than 1000 days for some of the most heavily obscured and reddened objects. We derive (dust) MLRs and luminosities for the entire sample. The estimated MLRs can differ significantly from estimates for the same objects in the literature due to differences in adopted optical constants (up to factors of several) and details in the radiative transfer modelling. Updated parameters for the super-AGB candidate MSX SMC 055 (IRAS 00483-7347) are presented. Its current mass is estimated to be 8.5 ± 1.6 M⊙, suggesting an initial mass well above 8 M⊙ in agreement with estimates based on its large Rubidium abundance. Using synthetic photometry, we present and discuss colour-colour and

  5. A natural grouping of motifs with an aspartate or asparagine residue forming two hydrogen bonds to residues ahead in sequence: their occurrence at alpha-helical N termini and in other situations.

    Science.gov (United States)

    Wan, W Y; Milner-White, E J

    1999-03-12

    Examination of the ways side-chain carboxylate and amide groups in high-resolution protein crystal structures form hydrogen bonds with main-chain atoms reveals that the most common category is a two-hydrogen-bond four to five residue motif with an aspartate or asparagine (Asx) at the first residue, for which we propose the name Asx-motif. Similar motifs with glutamate or glutamine residues at that position are rare. Asx-motifs occur typically as (1) a common feature of the N termini of alpha-helices called the Asx N-cap motif; (2) an independent motif, usually a beta-turn with an appropriately hydrogen-bonded Asx as the first residue; and (3) a motif incorporated in a beta-bulge loop. Asx-motifs are common, there being just under two-and-a-half in an average-sized protein subunit; of these, about 55 % are Asx N-cap motifs. Because they occur often in many situations, it seems that these motifs have an inherent propensity to form on their own rather than just being a feature stabilised at the end of a helix. Asx-motifs also occur in functionally interesting situations in aspartyl proteases, citrate synthase, EF hands, haemoglobins, lipocalins, glutathione reductase and the alpha/beta hydrolases. Copyright 1999 Academic Press.

  6. Galaxy And Mass Assembly (GAMA): The effect of galaxy group environment on active galactic nuclei

    Science.gov (United States)

    Gordon, Yjan A.; Pimbblet, Kevin A.; Owers, Matt S.; Bland-Hawthorn, Joss; Brough, Sarah; Brown, Michael J. I.; Cluver, Michelle E.; Croom, Scott M.; Holwerda, Benne W.; Loveday, Jonathan; Mahajan, Smriti; Wang, Lingyu

    2018-01-01

    In galaxy clusters, efficiently accreting active galactic nuclei (AGN) are preferentially located in the infall regions of the cluster projected phase-space, and are rarely found in the cluster core. This has been attributed to both an increase in triggering opportunities for infalling galaxies, and a reduction of those mechanisms in the hot, virialised, cluster core. Exploiting the depth and completeness (98 per cent at r 9.9 in 695 groups with 11.53 ≤ log10(M200/M⊙) ≤ 14.56 at z 13.5, AGN are preferentially found in the infalling galaxy population with 3.6σ confidence. At lower halo masses we observe no difference in AGN fraction between core and infalling galaxies. These observations support a model where a reduced number of low-speed interactions, ram pressure stripping and intra-group/cluster medium temperature, the dominance of which increase with halo mass, work to inhibit AGN in the cores of groups and clusters with log10(M200/M⊙) > 13.5, but do not significantly affect nuclear activity in cores of less massive structures.

  7. Galaxy And Mass Assembly (GAMA): the effect of galaxy group environment on active galactic nuclei

    Science.gov (United States)

    Gordon, Yjan A.; Pimbblet, Kevin A.; Owers, Matt S.; Bland-Hawthorn, Joss; Brough, Sarah; Brown, Michael J. I.; Cluver, Michelle E.; Croom, Scott M.; Holwerda, Benne W.; Loveday, Jonathan; Mahajan, Smriti; Wang, Lingyu

    2018-04-01

    In galaxy clusters, efficiently accreting active galactic nuclei (AGNs) are preferentially located in the infall regions of the cluster projected phase-space, and are rarely found in the cluster core. This has been attributed to both an increase in triggering opportunities for infalling galaxies, and a reduction of those mechanisms in the hot, virialized, cluster core. Exploiting the depth and completeness (98 per cent at r 9.9 in 695 groups with 11.53 ≤ log10(M200/M⊙) ≤ 14.56 at z 13.5, AGNs are preferentially found in the infalling galaxy population with 3.6σ confidence. At lower halo masses, we observe no difference in AGN fraction between core and infalling galaxies. These observations support a model where a reduced number of low-speed interactions, ram pressure stripping and intra-group/cluster medium temperature, the dominance of which increase with halo mass, work to inhibit AGN in the cores of groups and clusters with log10(M200/M⊙) > 13.5, but do not significantly affect nuclear activity in cores of less massive structures.

  8. Global histone analysis by mass spectrometry reveals a high content of acetylated lysine residues in the malaria parasite Plasmodium falciparum

    DEFF Research Database (Denmark)

    Trelle, Morten Beck; Salcedo-Amaya, Adriana M; Cohen, Adrian

    2009-01-01

    P. falciparum histone PTMs using advanced mass spectrometry driven proteomics. Acid-extracted proteins were resolved in SDS-PAGE, in-gel trypsin digested and analyzed by reversed-phase LC-MS/MS. Through the combination of Q-TOF and LTQ-FT mass spectrometry we obtained high mass accuracy of both...

  9. Properties of simulated Milky Way-mass galaxies in loose group and field environments

    Science.gov (United States)

    Few, C. G.; Gibson, B. K.; Courty, S.; Michel-Dansac, L.; Brook, C. B.; Stinson, G. S.

    2012-11-01

    Aims: We test the validity of comparing simulated field disk galaxies with the empirical properties of systems situated within environments more comparable to loose groups, including the Milky Way's Local Group. Methods: Cosmological simulations of Milky Way-mass galaxies have been realised in two different environment samples: in the field and in loose groups environments with similar properties to the Local Group. Apart from the differing environments of the galaxies, the samples are kept as homogeneous as possible with equivalent ranges in last major merger time, halo mass and halo spin. Comparison of these two samples allow for systematic differences in the simulations to be identified. A kinematic decomposition is employed to objectively quantify the spheroid-to-disk ratio and to isolate the disk-star population. Metallicity gradients, disk scale lengths, colours, magnitudes and age-velocity dispersion relations are studied for each galaxy in the suite and the strength of the link between these and environment of the galaxies is studied. Results: Metallicity gradients are consistent with observations of HII regions in spiral galaxies and, in agreement with observations, correlate with total galaxy mass. The bulge-to-disk ratio of the galaxies show that these galaxies are less spheroid dominated than many other simulated galaxies in literature with the majority of both samples being disk dominated. We find that secular evolution and mergers dominate the spread of morphologies and metallicity gradients with no visible differences between the two environment samples. In contrast with this consistency in the two samples there is tentative evidence for a systematic difference in the velocity dispersion-age relations of galaxies in the different environments. Loose group galaxies appear to have more discrete steps in their velocity dispersion-age relations, if this is true it suggests that impulsive heating is more efficient in the stars of galaxies in denser

  10. 40 CFR Table 4 to Subpart IIIi of... - Default Organic HAP Mass Fraction for Petroleum Solvent Groups a

    Science.gov (United States)

    2010-07-01

    ... Petroleum Solvent Groups a 4 Table 4 to Subpart IIII of Part 63 Protection of Environment ENVIRONMENTAL... Organic HAP Mass Fraction for Petroleum Solvent Groups a You may use the mass fraction values in the... Spirits, Petroleum Spirits, Petroleum Oil, Petroleum Naphtha, Solvent Naphtha, Solvent Blend. c E.g...

  11. Psychosocial correlates of body mass index in four groups of Quebec adults.

    Science.gov (United States)

    Plourde, Hugues; Nolin, Bertrand; Receveur, Olivier; Ledoux, Marielle

    2010-09-01

    The objective of the present analysis was to study the associations between body weight psychosocial correlates and body mass index (BMI) among four groups of adults in the Quebec population. Data were taken from the Social Lifestyles and Health 1998 Survey performed by the Institut de la Statistique du Québec (ISQ). The suggested guidelines of the ISQ were used to estimate the population's proportions and for statistical analysis. The groups studied were 25- to 44- and the 45- to 64-year-old men and women. In all groups, currently trying to lose weight increased the odds of reporting an excess weight. Better perceived eating habits was associated with lower BMI in most groups except in the 25- to 44-year-old women, where the trend was not significant. Higher number of physical activities related to transport and cigarette smoking were associated with lower BMI in both men groups. In both women groups, more frequent consumption of alcoholic beverages decreased significantly the odds of reporting excess body weight. A university degree was associated with a lower BMI only in the 25- to 44-year-old men. Regular practise of leisure time physical activity was associated with a lower BMI only in 45- to 64-year-old women. Opposite associations were observed between perceived health and BMI. In the 45- to 64-year-old men, better perceived health increased the odds of reporting an excess weight. Conversely, the odds of reporting excess weight decreased with better health in 25- to 44-year-old women. Many correlates differ between age group and sex. The identification of these factors illustrates the need to adapt obesity-related programmes toward specific sub-groups within the general population.

  12. Confirmation of sulfamethazine, sulfathiazole, and sulfadimethoxine residues in condensed milk and soft-cheese products by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Clark, Susan B; Turnipseed, Sherri B; Madson, Mark R; Hurlbut, Jeffrey A; Kuck, Laura R; Sofos, John N

    2005-01-01

    A liquid chromatography/tandem mass spectrometry method (LC/MS/MS) is described for the simultaneous detection of 3 sulfonamide drug residues at 1.25 ppb in condensed milk and soft-cheese products. The 3 sulfonamide drugs of interest are sulfathiazole (STZ), sulfamethazine (SMZ), and sulfadimethoxine (SDM). The method includes extraction of the product with phosphate buffer, centrifugation of the diluted product, and application of a portion of the extract onto a polymeric solid-phase extraction cartridge. The cartridge is washed with water, and the sulfonamides are eluted with methanol. After evaporation, the residue is dissolved in 0.1% formic acid solution, and the solution is filtered before analysis by LC/MS/MS. The LC/MS/MS program involved a series of time-scheduled selected-reaction monitoring transitions. The transitions of MH+ to the common product ions at m/z 156, 108, and 92 were monitored for each residue. In addition, SMZ and SDM had a fourth significant and unique product ion transition that could be measured. Validation was performed with control and fortified-control condensed bovine milk with 2.5, 5, and 10 ppb sulfonamides. This method was applied to imported flavored and unflavored condensed milk and cream cheese bars. The presence of STZ and SMZ residues was confirmed in 3 out of 6 products.

  13. [Determination of 35 antibiotic residues of tetracyclines, sulfonamides, penicillins, macrolides and amphenicols in milk by liquid chromatography-tandem mass spectromtery].

    Science.gov (United States)

    Wang, Hao; Zhao, Li; Yang, Hongmei; Pan, Hongyan; Shi, Hailiang; Qian, Cong; Zhang, Shan

    2015-09-01

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the simultaneous determination of 35 antibiotic residues of tetracyclines, sulfonamides, penicillins, macrolides and amphenicols in milk. The samples were extracted with alkaline acetonitrile and McIlvaine buffer solution under ultrasonication. The separation of target compounds was performed on an Eclipse XDB-C, column (150 mm x 2.1 mm, 3.5 µm) with gradient elution at a flow rate of 0.25 mL/min, and with an injection volume of 10 µL. The identification and quantification of the compounds were completed by liquid chromatography-tandem mass spectrometry in multiple reaction monitoring ( MRM) mode. The limits of detection were all below 10.0 µg/kg. The average spiked recoveries of the method ranged from 70. 1% to 109. 9% with relative standard deviations (RSDs) of 2.89%-9.99%. After validation, the method was applied to the analysis of antibiotic residues in milk products in China. Fifty samples were screened under the well defined methodology, and the results showed that chloramphenicol, only in one sample, was monitored with the content of 0.48 µg/kg. A risk of contamination of milk with chloramphenicol has been determined to exist. Therefore this method is convenient, rapid, sensitive and reliable, and can be successfully applied to the simultaneous detection of the 35 antibiotic residues of tetracyclines, sulfonamides, penicillins, macrolides and amphenicols in milk.

  14. Analysis of carbamate and phenylurea pesticide residues in fruit juices by solid-phase microextraction and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Sagratini, Gianni; Mañes, Jordi; Giardiná, Dario; Damiani, Pietro; Picó, Yolanda

    2007-04-20

    A new analysis method to detect carbamates and phenylurea pesticide residues in fruit juices was developed using solid-phase microextraction (SPME) coupled with liquid chromatography-single quadrupole mass spectrometry (LC/MS) and liquid chromatography-quadrupole ion trap mass spectrometry (LC/QIT-MS). The pesticide residues present in watery matrices as fruit juices were extracted using three types of fibers: 50-microm Carbowax/templated resin (CW/TPR), 60-mum poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) and 85-microm polyacrylate. The different extraction conditions were evaluated choosing as the best parameters 90 min (time), 20 degrees C (temperature) and 1 ml (volume). After extraction, the desorption (in a static mode) was performed in the specific interface chamber SPME/HPLC, previously filled with 70% methanol and 30% water. The best recoveries, evaluated at two fortification levels (0.2 and 0.5 mg kg(-1)) in fruit juices, were obtained using PDMS/DVB and CW/TPR fibers, and ranged from 25 to 82% (monolinuron, diuron and diethofencarb), with relative standard deviations (RSDs) from 1 to 17%. All the limits of quantification (LOQs) were in the range of 0.005-0.05 microg ml(-1) and, in any case, equal to, or lower than, maximum residue limits (MRLs) established by Italian and Spanish legislations. The mass spectrometry analyses were carried out using an electrospray ionization (ESI) source operating in the positive mode both for single quadrupole and for QIT mass analysers, operating in selected ion monitoring (SIM) and in multiple reaction monitoring (MRM) modes, respectively. The proposed new method can be applied to the determination of selected pesticides in real samples of fruit juices.

  15. High resolution FT-ICR mass spectral analysis of bio-oil and residual water soluble organics produced by hydrothermal liquefaction of the marine microalga Nannochloropsis salina

    Energy Technology Data Exchange (ETDEWEB)

    Sudasinghe, Nilusha; Dungan, Barry; Lammers, Peter; Albrecht, Karl O.; Elliott, Douglas C.; Hallen, Richard T.; Schaub, Tanner

    2014-03-01

    We report a detailed compositional characterization of a bio-crude oil and aqueous by-product from hydrothermal liquefaction of Nannochloropsis salina by direct infusion Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR MS) in both positive- and negative-ionization modes. The FT-ICR MS instrumentation approach facilitates direct assignment of elemental composition to >7000 resolved mass spectral peaks and three-dimensional mass spectral images for individual heteroatom classes highlight compositional diversity of the two samples and provide a baseline description of these materials. Aromatic nitrogen compounds and free fatty acids are predominant species observed in both the bio-oil and aqueous fraction. Residual organic compounds present in the aqueous fraction show distributions that are slightly lower in both molecular ring and/or double bond value and carbon number relative to those found in the bio-oil, albeit with a high degree of commonality between the two compositions.

  16. Screening of the presence organophosphates and organochlorines pesticide residues in vegetables and fruits using gas chromatography-mass spectrometry

    Science.gov (United States)

    Putri, Dillani; Aryana, Nurhani; Aristiawan, Yosi; Styarini, Dyah

    2017-01-01

    Pesticides is commonly used to improve the quality of agricultural product, especially in vegetables and fruits. Due to pesticide residues in the product become a concern to consumer health, monitoring and analysis of pesticide residues in agriculture product need to be established. The certified reference material (CRM) is often benefited to obtain accurate results in analysis. It is required as the quality control to improve quality assurance of the testing results. Unfortunately in Indonesia, the development of matrix CRM for the analysis of pesticide residues in vegetables and fruits is still limited. This study is aimed to determine the type of commodity and target analyte to be employed in the development of CRM for pesticides in vegetables and fruits. As the preliminary study, the screening of 11 commodities of fresh vegetables and fruits has been conducted to review the information about the presence of organophosphates (OPs) and organochlorines (OCs) in the sample. In this analysis, QuEChERS technique was used in the extraction process and the qualitative analysis was evaluated by using GC-MS. The results showed that strawberry and celery contain residues of pesticide chlorpyrifos. Further analysis of the commodity celery from seven different places has been conducted, resulting that from 3 of all 7 samples (43%) were positive containing chlorpyrifos. Therefore, the development of CRM for chlorpyrifos in celery will be our next research project.

  17. Multi-residue method for the detection of veterinary drugs in distillers grains by liquid chromatography-Orbitrap high resolution mass spectrometry.

    Science.gov (United States)

    Kaklamanos, George; Vincent, Ursula; von Holst, Christoph

    2013-12-27

    Distillers Grain (DG) is an important by-product of ethanol production. The ethanol production process uses only the starch portion of the plant and all the remaining nutrients, protein, fat, minerals, and vitamins remain in DGs, a valuable feed material for livestock. The use of antimicrobial drugs is helpful to limit harmful bacterial growth during the early part of the fermentation process. This can lead to the possible presence of contaminants in the by-products that are used in the food and feed industries, resulting in a major concern for the development of bacterial resistance in both humans and animals. To facilitate the detection of antimicrobial and other commonly used veterinary drugs in DGs, a liquid chromatography-high resolution mass spectrometry (LC-HRMS) method was developed targeting a wide range of 12 chemical classes of anti-bacterial substances and drugs, such as ionophore and non-ionophore authorized coccidiostats, banned coccidiostats, macrolides, tetracyclines, nitroimidazoles, amphenicols, quinolones, sulphonamides, tranquilizers, non-steroidal anti-inflammatory drugs and benzimidazoles. Following a simple and fast extraction step with a mixture of organic solvents, the extract was directly injected into the LC coupled to an Orbitrap mass analyzer. The identification of residues is based on accurate mass measurement. The high mass resolution of 50,000 full width at half maximum (FWHM) and corresponding narrow mass windows permitted a very selective and sensitive detection of the analytes in such a complex matrix. A single-laboratory validation procedure was carried out evaluating selectivity, sensitivity, linearity, precision and accuracy. The method showed satisfactory analytical performance for precision and trueness, and allowed the determination of the compounds at low concentration. The proposed multi-method demonstrated that liquid chromatography coupled to an Orbitrap mass spectrometer is a promising analytical technique, suitable for

  18. A sensitive estimation of residual ethylene glycol in ethylene oxide sterilized medical devices by HPLC with electrospray ionization mass spectrometric detection.

    Science.gov (United States)

    Hari, P R; Naseerali, C P; Sreenivasan, K

    2009-01-15

    A novel analytical methodology for the estimation of residual ethylene glycol (EG) in ethylene oxide sterilized polymer is reported. The method involves the monitoring of ammonium adduct of EG ions in the presence of 10 mM ammonium acetate buffer and methanol using electrospray ionization liquid chromatography and mass spectrometry (LC-ESI-MS). The method enables the detection and quantification of EG without prior derivatization up to a level of 0.06 microg/ml. The potentiality of the method is demonstrated by estimating EG in ethylene oxide (EtO) sterilized polyethylene terephthalate fabric used in heart valve sewing ring. The method is simple, rapid and can routinely be used for the quantification of residual EG in EtO sterilized medical devices.

  19. Rapid analysis of multiclass antibiotic residues and some of their metabolites in hospital, urban wastewater and river water by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry.

    Science.gov (United States)

    Gros, Meritxell; Rodríguez-Mozaz, Sara; Barceló, Damià

    2013-05-31

    The present work describes the development of a fast and robust analytical method for the determination of 53 antibiotic residues, covering various chemical groups and some of their metabolites, in environmental matrices that are considered important sources of antibiotic pollution, namely hospital and urban wastewaters, as well as in river waters. The method is based on automated off-line solid phase extraction (SPE) followed by ultra-high-performance liquid chromatography coupled to quadrupole linear ion trap tandem mass spectrometry (UHPLC-QqLIT). For unequivocal identification and confirmation, and in order to fulfill EU guidelines, two selected reaction monitoring (SRM) transitions per compound are monitored (the most intense one is used for quantification and the second one for confirmation). Quantification of target antibiotics is performed by the internal standard approach, using one isotopically labeled compound for each chemical group, in order to correct matrix effects. The main advantages of the method are automation and speed-up of sample preparation, by the reduction of extraction volumes for all matrices, the fast separation of a wide spectrum of antibiotics by using ultra-high-performance liquid chromatography, its sensitivity (limits of detection in the low ng/L range) and selectivity (due to the use of tandem mass spectrometry) The inclusion of β-lactam antibiotics (penicillins and cephalosporins), which are compounds difficult to analyze in multi-residue methods due to their instability in water matrices, and some antibiotics metabolites are other important benefits of the method developed. As part of the validation procedure, the method developed was applied to the analysis of antibiotics residues in hospital, urban influent and effluent wastewaters as well as in river water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Qualitative and Quantitative Drug residue analyses: Florfenicol in white-tailed deer (Odocoileus virginianus) and supermarket meat by liquid chromatography tandem-mass spectrometry.

    Science.gov (United States)

    Anderson, Shanoy C; Subbiah, Seenivasan; Gentles, Angella; Austin, Galen; Stonum, Paul; Brooks, Tiffanie A; Brooks, Chance; Smith, Ernest E

    2016-10-15

    A method for confirmation and detection of Florfenicol amine residues in white-tailed deer tissues was developed and validated in our laboratory. Tissue samples were extracted with ethyl acetate and cleaned up on sorbent (Chem-elut) cartridges. Liguid chromatography (LC) separation was achieved on a Zorbax Eclipse plus C18 column with gradient elution using a mobile phase composed of ammonium acetate in water and methanol at a flow rate of 300μL/min. Qualitative and quantitative analyses were carried out using liquid chromatography - heated electrospray ionization(HESI) and atmospheric pressure chemical ionization (APCI)-tandem mass spectrometry in the multiple reaction monitoring (MRM) interface. The limits of detection (LODs) for HESI and APCI probe were 1.8ng/g and 1.4ng/g respectively. Limits of quantitation (LOQs) for HESI and APCI probe were 5.8ng/g and 3.4ng/g respectively. Mean recovery values ranged from 79% to 111% for APCI and 30% to 60% for HESI. The validated method was used to determine white-tailed deer florfenicol tissue residue concentration 10-days after exposure. Florfenicol tissue residues concentration ranged from 0.4 to 0.6μg/g for liver and 0.02-0.05μg/g for muscle and a trace in blood samples. The concentration found in the tested edible tissues were lower than the maximum residual limit (MRL) values established by the federal drug administration (FDA) for bovine tissues. In summary, the resulting optimization procedures using the sensitivity of HESI and APCI probes in the determination of florfenicol in white-tailed deer tissue are the most compelling conclusions in this study, to the extent that we have applied this method in the evaluation of supermarket samples drug residue levels as a proof of principle. Copyright © 2016. Published by Elsevier B.V.

  1. Detection and imaging of chrome yellow (lead chromate) in latent prints, solid residues, and minerals by laser-desorption/ionization mass spectrometry (LDI-MS).

    Science.gov (United States)

    Zheng, Z; Pavlov, J; Attygalle, A B

    2017-06-01

    In the past, chrome yellow (lead chromate, PbCrO 4 ), a bright orange-red substance, has been widely used as an inorganic pigment in the production of paints, coatings, and plastics. Herein, we demonstrate that laser desorption/ionization mass spectrometry (LDI-MS) is a powerful tool for the detection of lead chromate in solid residues. In fact, lead chromate in trace amounts is easily detectable by LDI-MS even from residues left as latent prints. For example, a latent print obtained by stamping the exposed laterally cut surface of a pencil over 50 years old on an acetonitrile-moistened paper, was successfully imaged for both lead and chromate using a Synapt G2 HDMS mass spectrometer. After rastering the print with a 355 nm laser beam and recording positive- and negative-ion mass spectra over the range m/z 50-1200, we generated false-color 'heat maps' (single-ion images) for 208 Pb +• (m/z 207.98) and Cr 2 O 6 -• (m/z 199.85). The heat maps matched closely with the faint visual image of the pencil imprint. Moreover, our results confirmed that lead chromate was used in the pigment coatings of old pencils. Evidently, LDI-MS imaging is an efficient procedure to survey for the presence of lead and chromate in minerals and other materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  2. [Determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans by QuEChERS-liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Wang, Lianzhu; Huang, Xiaoyan; Wang, Dengfei; Chen, Yong; Xu, Dunming; Zhou, Yu

    2015-05-01

    A fast method based on QuEChERS methodology for the simultaneous determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The clean-up effects of three dispersive sorbents were evaluated in terms of the residue mass for extracts after evaporation and recoveries. The three sorbents were C18, a mixture of two sorbents--silica coated with zirconium dioxide (Z-Sep) and C18, a bonded C18 zirconia-coated silica (Z-Sep+). As a result, the best effects were obtained from using Z-Sep/C18 sorbents. The samples were extracted with acetonitrile, and salted out with anhydrous magnesium sulphate and sodium chloride. The extracts were cleaned up with dispersive solid phase extraction using Z-Sep/C18 sorbents. Chromatographic analysis was carried out using a CSH C18 column with gradient elution. The pesticides were analyzed by negative electrospray ionization tandem mass spectrometry under scheduled multiple reaction monitoring mode. The quantification was achieved using matrix-matched standard calibrations as the external standard. The recoveries at fortification levels of 10, 20, 100 µg/kg in sweet corns and green beans ranged from 80.0% to 108.2% with the relative standard deviations of 1.2%-13.0%. The limits of quantification (S/N ≥ 10) were 0.2-5.0 µg/kg. The method has been proven to be simple, sensitive, environmental, and thus suitable for the determination of the 32 sulfonylurea herbicide residues in sweet corns and green soy- beans.

  3. Leader-based and self-organized communication: modelling group-mass recruitment in ants.

    Science.gov (United States)

    Collignon, Bertrand; Deneubourg, Jean Louis; Detrain, Claire

    2012-11-21

    For collective decisions to be made, the information acquired by experienced individuals about resources' location has to be shared with naïve individuals through recruitment. Here, we investigate the properties of collective responses arising from a leader-based recruitment and a self-organized communication by chemical trails. We develop a generalized model based on biological data drawn from Tetramorium caespitum ant species of which collective foraging relies on the coupling of group leading and trail recruitment. We show that for leader-based recruitment, small groups of recruits have to be guided in a very efficient way to allow a collective exploitation of food while large group requires less attention from their leader. In the case of self-organized recruitment through a chemical trail, a critical value of trail amount has to be laid per forager in order to launch collective food exploitation. Thereafter, ants can maintain collective foraging by emitting signal intensity below this threshold. Finally, we demonstrate how the coupling of both recruitment mechanisms may benefit to collectively foraging species. These theoretical results are then compared with experimental data from recruitment by T. caespitum ant colonies performing group-mass recruitment towards a single food source. We evidence the key role of leaders as initiators and catalysts of recruitment before this leader-based process is overtaken by self-organised communication through trails. This model brings new insights as well as a theoretical background to empirical studies about cooperative foraging in group-living species. Copyright © 2012 Elsevier Ltd. All rights reserved.

  4. Mass

    International Nuclear Information System (INIS)

    Quigg, Chris

    2007-01-01

    In the classical physics we inherited from Isaac Newton, mass does not arise, it simply is. The mass of a classical object is the sum of the masses of its parts. Albert Einstein showed that the mass of a body is a measure of its energy content, inviting us to consider the origins of mass. The protons we accelerate at Fermilab are prime examples of Einsteinian matter: nearly all of their mass arises from stored energy. Missing mass led to the discovery of the noble gases, and a new form of missing mass leads us to the notion of dark matter. Starting with a brief guided tour of the meanings of mass, the colloquium will explore the multiple origins of mass. We will see how far we have come toward understanding mass, and survey the issues that guide our research today.

  5. Development of a multi-residue analytical method, based on liquid chromatography-tandem mass spectrometry, for the simultaneous determination of 46 micro-contaminants in aqueous samples.

    Science.gov (United States)

    Nödler, Karsten; Licha, Tobias; Bester, Kai; Sauter, Martin

    2010-10-15

    A multi-residue analytical method based on high-performance liquid chromatographic separation, electrospray ionization with tandem mass spectrometric detection (HPLC/MS-MS) was developed for the simultaneous analysis of 46 basic, neutral and acidic compounds covering a wide range of polarity (logK(OW)MQL) in surface and seawater ranged from 1.2 to 28 ng/L, in wastewater from 5.0 to 160 ng/L, respectively. In order to demonstrate the applicability of the method, river water, treated wastewater and seawater were analyzed. Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Hyperfunction solutions of the zero rest mass equations and representations of LIE groups

    Energy Technology Data Exchange (ETDEWEB)

    Dunne, E.G.

    1984-01-01

    Recently, hyperfunctions have arisen in an essential way in separate results in mathematical physics and in representation theory. In the setting of the twistor program, Wells, with others, has extended the Penrose transform to hyperfunction solutions of the zero rest mass equations, showing that the fundamental isomorphisms hold for this larger space. Meanwhile, Schmid has shown the existence of a canonical globalization of a Harish-Chandra module, V, to a representation of the group. This maximal globalization may be realized as the completion of V in a locally convex vector space in the hyperfunction topology. This thesis shows that the former is a particular case of the latter where the globalization can be done by hand. This explicit globalization is then carried out for a more general case of the Radon transform on homogeneous spaces.

  7. Residual gas analysis

    International Nuclear Information System (INIS)

    Berecz, I.

    1982-01-01

    Determination of the residual gas composition in vacuum systems by a special mass spectrometric method was presented. The quadrupole mass spectrometer (QMS) and its application in thin film technology was discussed. Results, partial pressure versus time curves as well as the line spectra of the residual gases in case of the vaporization of a Ti-Pd-Au alloy were demonstrated together with the possible construction schemes of QMS residual gas analysers. (Sz.J.)

  8. First Characterization of Biomass Burning Smoke from Cooking Fires, Peat, Crop Residue and Other Fuels By High Resolution PTR-TOF Mass Spectrometry and FTIR

    Science.gov (United States)

    Stockwell, C.; Veres, P. R.; Williams, J.; Yokelson, R. J.

    2014-12-01

    Biomass burning (BB) is a major influence on Earth's atmosphere, but for many fire-types the emissions have only been measured for a few species. For all types of BB, progress has been limited by a lack of information on the emissions of semi-volatile organic gases that are precursors for secondary aerosol and ozone. During the Fourth Fire Lab at Missoula Experiment (FLAME-4), the BB emissions from 158 laboratory fires were quantified by ~40 scientists for an assortment of globally relevant fuels including rarely sampled sources such as US and Asian crop residue; Indonesian and extratropical peat; and cooking fires in traditional and advanced stoves. In this work, we present the primary emissions of gas-phase non-methane organic compounds (NMOCs) measured using an advanced Proton-Transfer-Reaction time-of-flight mass spectrometer (PTR-TOF-MS) in tandem with measurements of other major emissions by Fourier transform infrared (FTIR) spectroscopy. We developed a composition and mass dependent sensitivity and best assignments for many observed peaks. The known and tentatively assigned peaks together account for ~80-96% of total observed NMOC mass. Much of the NMOC mass is rarely measured or previously unmeasured high molecular mass compounds including ringed aromatic hydrocarbons, phenolic compounds, and furans, which are all secondary organic aerosol precursors. Large air quality benefits are demonstrated for more advanced cooking technologies. This work produced globally relevant emission ratios and emission factors to better represent biomass burning in current atmospheric models.

  9. THE ARECIBO LEGACY FAST ALFA SURVEY. IX. THE LEO REGION H I CATALOG, GROUP MEMBERSHIP, AND THE H I MASS FUNCTION FOR THE LEO I GROUP

    International Nuclear Information System (INIS)

    Stierwalt, Sabrina; Haynes, Martha P.; Giovanelli, Riccardo; Martin, Ann M.; Kent, Brian R.; Saintonge, Amelie; Karachentsev, Igor D.; Karachentseva, Valentina E.

    2009-01-01

    We present the catalog of H I sources extracted from the ongoing Arecibo Legacy Fast ALFA (ALFALFA) extragalactic H I line survey, found within the sky region bounded by 9 h 36 m h 36 m and +08 0 0 . The H I catalog presented here for this 118 deg 2 region is combined with the ones derived from surrounding regions also covered by the ALFALFA survey to examine the large-scale structure in the complex Leo region. Because of the combination of wide sky coverage and superior sensitivity, spatial and spectral resolution, the ALFALFA H I catalog of the Leo region improves significantly on the numbers of low H I mass sources as compared with those found in previous H I surveys. The H I mass function of the Leo I group presented here is dominated by low-mass objects: 45 of the 65 Leo I members have M H I 8 M-odot, yielding tight constraints on the low-mass slope of the Leo I H I mass function. The best-fit slope is α ≅ -1.41 + 0.2 - 0.1. A direct comparison between the ALFALFA H I line detections and an optical search of the Leo I region proves the advantage of the ALFALFA strategy in finding low-mass, gas-rich dwarfs. These results suggest the existence of a significant population of low surface brightness, gas-rich, yet still very low H I mass galaxies, and may reflect the same type of morphological segregation as is seen in the Local Group. While the low-mass end slope of the Leo I H I mass function is steeper than that determined for luminosity functions of the group, the slope still falls short of the values predicted by simulations of structure formation in the lambda cold dark matter paradigm.

  10. Residue Analysis of 60 Pesticides in Red Swamp Crayfish Using QuEChERS with High-Performance Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Song, Shuangyu; Zhu, Kechen; Han, Lijun; Sapozhnikova, Yelena; Zhang, Zihao; Yao, Wei

    2018-02-05

    In this study, a multi-residue analytical method using quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and dispersive solid-phase extraction (d-SPE) cleanup, followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), was investigated for rapid determination of 60 pesticide residues in whole crayfish and crayfish meat. The final method used 10 mL of acetonitrile for extraction, 3 g of NaCl for partitioning, and 50 mg of primary secondary amine for d-SPE cleanup. The method was validated at three spiking levels (10, 50, and 100 ng/g) using triphenyl phosphate as an internal standard and both gradient and isocratic HPLC elution. Under gradient conditions, satisfactory recoveries (70-120%) and relative standard deviations of ≤20% were achieved for 83 and 88% of pesticides in whole crayfish and crayfish meat, respectively. Matrix effects were estimated using both gradient and isocratic HPLC elution. To our knowledge, this is the first study involving multi-residue analysis of HPLC-amenable pesticides in crayfish and mantis shrimp. The final method was successfully applied for analysis of 11 crayfish and mantis shrimp samples from markets in China, and propamocarb (shrimps.

  11. Bithionol residue analysis in animal-derived food products by an effective and rugged extraction method coupled with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zheng, Weijia; Park, Jin-A; Abd El-Aty, A M; Kim, Seong-Kwan; Cho, Sang-Hyun; Choi, Jeong-Min; Yi, Hee; Cho, Soo-Min; El-Banna, H A; Shim, Jae-Han; Chang, Byung-Joon; Wang, Jing; Kim, Jin-Suk; Shin, Ho-Chul

    2017-10-01

    Herein, we developed a simple analytical procedure for the quantitation of bithionol residues in animal-derived food products such as porcine muscle, eggs, milk, eel, flatfish, and shrimp using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI + /MS-MS). Samples were extracted with 0.1% solution of formic acid in acetonitrile and the extract was purified using a C18 sorbent. Separation was performed on a Waters XBridge™ C18 reversed-phase analytical column using 0.1% solution of formic acid/acetonitrile as the mobile phase. Six-point matrix-matched calibration indicated good linearity, with the calculated coefficients of determination (R 2 ) being≥0.9813. Intra- and inter-day recoveries (determined at spiking levels equivalent to 1×and 2×the limit of quantitation (0.25μg/kg)) ranged between 80.0 and 94.0%, with the corresponding relative standard deviations (RSDs) being≤8.2%. The developed experimental protocol was applied to different samples purchased from local markets in Seoul, which were tested negative for bithionol residues. In conclusion, the proposed method proved to be versatile and precise, being ideally suited for the routine detection of bithionol residues in animal-derived food products with various protein and fat contents. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Determination of cyflumetofen residue in water, soil, and fruits by modified quick, easy, cheap, effective, rugged, and safe method coupled to gas chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Li, Minmin; Liu, Xingang; Dong, Fengshou; Xu, Jun; Qin, Dongmei; Zheng, Yongquan

    2012-10-01

    A new, highly sensitive, and selective method was developed for the determination of the cyflumetofen residue in water, soil, and fruits by using gas chromatography quadruple mass spectrometry. The target compound was extracted using acetonitrile and then cleaned up using dispersive solid-phase extraction with primary and secondary amine and graphitized carbon black, and optionally by a freezing-out cleanup step. The matrix-matched standards gave satisfactory recoveries and relative standard deviation values in different matrices at three fortified levels (0.05, 0.5, and 1.0 mg kg(-1) ). The overall average recoveries for this method in water, soil, and all fruits matrix at three fortified levels ranged from 76.3 to 101.5% with relative standard deviations in the range of 1.2-11.8% (n = 5). The calculated limits of detection and quantification were typically below 0.005 and 0.015 μg kg(-1), which were much lower than the maximum residue levels established by Japanese Positive List. This study provides a theoretical basis for China to draw up maximum residue level and analytical method for cyflumetofen acaricide in different fruits. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Analysis of sulfonamides, tilmicosin and avermectins residues in typical animal matrices with multi-plug filtration cleanup by liquid chromatography-tandem mass spectrometry detection.

    Science.gov (United States)

    Qin, Yuhong; Jatamunua, Freedom; Zhang, Jingru; Li, Yanjie; Han, Yongtao; Zou, Nan; Shan, Jihao; Jiang, Yanbin; Pan, Canping

    2017-05-15

    The frequent use of various veterinary drugs could lead to residue bioaccumulation in animal tissues, which could cause dietary risks to human health. In order to quickly analyze the residues, a liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detecting Sulfonamides, Tilmicosin and Avermectins (AVMs) residues in animal samples. For sample preparation, modified QuEChERS (quick, easy, cheap, effective, rugged and safe) and ultrasound-assisted extraction (UAE) methods were used. For sample cleanup, n-Hexane delipidation and multi-plug filtration cleanup (m-PFC) method based on primary-secondary amine (PSA) and octadecyl-silica (C18) were used, followed by LC-MS/MS analysis. It was validated on 7 animal matrices (bovine, caprine, swine meat and their kidneys, milk) at two fortified concentration levels of 5 and 100μg/kg. The recoveries ranged from 82 to 107% for all analytes with relative standard deviations (RSDs) less than 15%. Matrix-matched calibrations were performed with coefficients of determination above 0.998 for all analytes within concentration levels of 5-500μg/kg. The developed method was successfully used to analysis veterinary drugs of real animal samples from local markets. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Analysis of Veterinary Drug and Pesticide Residues Using the Ethyl Acetate Multiclass/Multiresidue Method in Milk by Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Husniye Imamoglu

    2016-01-01

    Full Text Available A rapid and simple multiclass, ethyl acetate (EtOAc multiresidue method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS detection was developed for the determination and quantification of 26 veterinary drugs and 187 total pesticide residues in milk. Sample preparation was a simple procedure based on liquid–liquid extraction with ethyl acetate containing 0.1% acetic acid, followed by centrifugation and evaporation of the supernatant. The residue was dissolved in ethyl acetate with 0.1% acetic acid and centrifuged prior to LC-MS/MS analysis. Chromatographic separation of analytes was performed on an Inertsil X-Terra C18 column with acetic acid in methanol and water gradient. The repeatability and reproducibility were in the range of 2 to 13% and 6 to 16%, respectively. The average recoveries ranged from 75 to 120% with the RSD (n=18. The developed method was validated according to the criteria set in Commission Decision 2002/657/EC and SANTE/11945/2015. The validated methodology represents a fast and cheap alternative for the simultaneous analysis of veterinary drug and pesticide residues which can be easily extended to other compounds and matrices.

  15. Exploring matrix effects in liquid chromatography-tandem mass spectrometry determination of pesticide residues in tropical fruits.

    Science.gov (United States)

    Botero-Coy, Ana María; Marín, José M; Serrano, Roque; Sancho, Juan Vicente; Hernández, Félix

    2015-05-01

    Tropical fruits are being increasingly consumed around the world because of their appreciated characteristics, particularly their high nutritional value and distinctive taste, which are different from those of traditional fruits. Owing to their introduction into international markets it is necessary to have a reliable analytical methodology available for the sensitive determination of pesticide residues in order to monitor the compliance of maximum residue limits (MRLs). From an analytical point of view, tropical fruits have generally been far less studied than other fruits frequently consumed in the European Union or USA, which are among the most important markets. In this work, LC-MS/MS-based methodology using a triple quadrupole analyzer was developed for the multi-residue determination of selected pesticides and metabolites in tropical fruits, which were selected among the most popular in Colombia, one of the most important suppliers of tropical fruits around the world. After selection of a QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)-based sample treatment, the study focused on the evaluation of matrix effects, in order to find a simple way for their correction. Twelve different food matrices were selected to perform this study: the seven Colombian tropical fruits of highest value for domestic and international markets (uchuva, tamarillo, granadilla, gulupa, maracuya, papaya, and pithaya), and five more matrices highly consumed in Colombia (lulo, carambolo, feijoa, mangostan, and guayaba). Twenty compounds, including pesticides widely applied in tropical fruits pest control and several metabolites considered in residue definition, were used as model compounds in this work. Correction factors were used on the basis of calibration graphs obtained with standards in solvent and in matrix, and their usefulness was supported by validation of the method in all the matrices tested at 0.01 and 0.1 mg/kg. The analysis of real-world samples revealed the

  16. The masses of satellites in GAMA galaxy groups from 100 square degrees of KiDS weak lensing data

    NARCIS (Netherlands)

    Sifón, Cristóbal; Cacciato, Marcello; Hoekstra, Henk; Brouwer, Margot; van Uitert, Edo; Viola, Massimo; Baldry, Ivan; Brough, Sarah; Brown, Michael J. I.; Choi, Ami; Driver, Simon P.; Erben, Thomas; Grado, Aniello; Heymans, Catherine; Hildebrandt, Hendrik; Joachimi, Benjamin; de Jong, Jelte T. A.; Kuijken, Konrad; McFarland, John; Miller, Lance; Nakajima, Reiko; Napolitano, Nicola; Norberg, Peder; Robotham, Aaron S. G.; Schneider, Peter; Kleijn, Gijs Verdoes

    2015-01-01

    We use the first 100 deg2 of overlap between the Kilo-Degree Survey and the Galaxy And Mass Assembly survey to determine the average galaxy halo mass of ˜10 000 spectroscopically confirmed satellite galaxies in massive (M > 1013 h-1 M⊙) galaxy groups. Separating the sample as a function of projected

  17. Spontaneous mass generation and the small dimensions of the Standard Model gauge groups U(1, SU(2 and SU(3

    Directory of Open Access Journals (Sweden)

    Guillermo García Fernández

    2017-02-01

    The result follows from strong antiscreening of the running coupling for those larger groups (with an appropriately small number of flavors together with scaling properties of the Dyson–Schwinger equation for the fermion mass.

  18. New Developments in Mass Spectrometry for Group-Type Analysis of Petroleum Cuts (First Part

    Directory of Open Access Journals (Sweden)

    Fafet A.

    1999-07-01

    Full Text Available Characterization of petroleum cuts constitutes a necessary stage to perfect understanding of the reaction mechanisms and to the description of the kinetics of certain refining processes such as hydrotreating or catalytic cracking. Mass spectrometry (MS, thanks to group-type quantitative analysis methods, enables to access detailed description of complex hydrocarbon mixtures such as middle distillates or heavy cuts such as vacuum distillates. But these methods are also subject to some drawbacks and we shall expose, thereunder, two examples of improvements. In a first part, the accuracy of MS quantification of thiophenic sulphured compounds in middle distillates is studied by intertechnique comparison with the results obtained by gas phase chromatography coupled to sulphur-specific detection by chemiluminescence (GC/SCD. Improving on the MS method is suggested. In the second part, a new system for introducing the sample in the spectrometer source, dedicated to group-type analysis of heavy cuts is described. Its validation, by comparison of the MS results to those of liquid chromatography (LC as well as its performances, is exposed.

  19. Application of Gas Chromatography Coupled to Quadrupole-Orbitrap Mass Spectrometry for Pesticide Residue Analysis in Cereals and Feed Ingredients.

    Science.gov (United States)

    Tienstra, Marc; Mol, Hans G J

    2018-03-01

    A method for residue analysis of pesticides and polychlorinated biphenyls in cereals and feed ingredients based on QuEChERS extraction, programmed temperature vaporizer large-volume injection, and GC with electron ionization (EI) quadrupole Orbitrap full-scan high-resolution MS (60 000 full width at half-maximum at m/z 200) has been developed. In addition to full-scan acquisition, simultaneous full-scan and selected-ion monitoring acquisition was used to improve detectability in incidental cases in which analytes coeluted with intense signals from coextractants. The method was successfully validated down to 10 µg/kg for a single commodity (wheat) using matrix-matched calibration, and for multiple-feed matrixes using standard addition. Identification according to European Union requirements was achieved in >90% of the analyte/matrix combinations, and suggestions for further increasing identification rates have been made. Performance characteristics were compared to an existing method for residue analysis based on GC with EI tandem MS (triple quadrupole).

  20. Determination of pesticide residues (> 0.5 microg/L) in soft drinks and sports drinks by gas chromatography with mass spectrometry: collaborative study.

    Science.gov (United States)

    Miller, Kathleen D; Milne, Paul

    2008-01-01

    A collaborative study was conducted on a method for the measurement of 19 low-level pesticide residues in soft drinks and sports drinks by gas chromatography with mass spectrometry (GC/MS). The pesticide residues determined were 2,4'-dichlorodiphenyldichloroethylene (2,4'-DDE); 2,4'-dichlorodiphenyldichloroethane (2,4'-DDD); 4,4'-dichlorodiphenyldichloroethylene (4,4'-DDE); 2,4'-dichlorodiphenyltrichloroethane (2,4'-DDT); 4,4'-dichlorodiphenyltrichloroethane (4,4'-DDT); 4,4'-dichlorodiphenyldichloroethane (4,4'-DDD); alpha-endosulfan; endosulfan-sulfate; dieldrin; aldrin; ethion; chlorpyrifos; beta-endosulfan; malathion; methyl-parathion; alpha-hexachlorocyclohexane (alpha-HCH); beta-HCH; delta-HCH; and gamma-HCH. Blind fortification solutions containing 4 different levels of pesticide residues (0, 0.1, 0.5, and 1.0 microg/L) were provided to 8 collaborating laboratories who used them to create test samples in 6 matrixes (also provided): 2 colas, a diet cola, a clear lemon-lime soft drink, an orange soft drink, and a sports drink. Reproducibility (RSDR) for all 19 pesticide residues in all matrixes ranged from 7 to 151% at the 0.1 microg/L level, 11 to 121% at 0.5 microg/L, and 14 to 67% at 1.0 microg/L. Repeatability (RSDr), applicable to the diet cola and the sports drink, ranged from 1 to 76% for the 19 pesticide residues at the 0.1 microg/L level, 9 to 38% at 0.5 microg/L, and 9 to 38% at 1.0 microg/L. Recoveries for the 19 pesticide residues in all matrixes ranged from 77 to 645% at the 0.1 microg/L level, 60 to 231% at 0.5 microg/L, and 61 to 146% at 1.0 microg/L. It is recommended that the method be accepted by AOAC as Official First Action with a limit of quantification (LOQ) equal to 0.5 microg/L for 4,4'-DDT; 2,4'-DDT; 2,4'-DDD; 4,4'-DDE; 4,4'-DDD; 2,4'-DDE; aldrin; dieldrin; alpha-endosulfan; endosulfan-sulfate; chlorpyrifos; and ethion, and an LOQ equal to 1.0 microg/L for beta-endosulfan; alpha-HCH; beta-HCH; delta-HCH; gamma-HCH; methyl-parathion; and

  1. Determination of low-level pesticide residues in soft drinks and sports drinks by liquid chromatography with tandem mass spectrometry: collaborative study.

    Science.gov (United States)

    Miller, Kathleen D; Milne, Paul

    2008-01-01

    A collaborative study was conducted on a method for the measurement of 11 low-level pesticide residues in soft drinks and sports drinks by liquid chromatography with tandem mass spectrometry. The pesticide residues determined in this study were alachlor, atrazine, butachlor, isoproturon, malaoxon, monocrotophos, methyl paraoxon, phorate, phorate sulfone, phorate sulfoxide, and 2,4-dichlorophenoxyacetic acid (2,4-D). Blind fortification solutions containing 3 different levels of pesticide residues were provided to 9 collaborating laboratories to create test samples at concentrations of 0, 0.1, and 0.5 microg/L with a 10-fold concentration for phorate in a total of 6 matrixes (2 colas, 1 diet cola, 1 clear lemon-lime soft drink, 1 orange soft drink, and 1 sports drink). Good qualitative performance of the method was demonstrated for all pesticide residues. Reproducibility relative standard deviation (RSDR) ranged from 7 to 151% for alachlor, atrazine, butachlor, isoproturon, malaoxon, monocrotophos, methyl paraoxon, phorate, phorate sulfone, phorate sulfoxide, and 2,4-D at the 0.1 microg/L level (1.0 microg/L for phorate). At 0.5 microg/L (5.0 microg/L for phorate), RSDR ranged from 9 to 57% for alachlor, atrazine, butachlor isoproturon, malaoxon, monocrotophos, methyl paraoxon, phorate, phorate sulfone, phorate sulfoxide, and 2,4-D in all matrixes. Repeatability relative standard deviation (RSDr), applicable to the diet cola and sports drink, ranged from 0 to 124% for the 11 pesticide residues at the 0.1 microg/L level (1.0 microg/L for phorate). At 0.5 microg/L (5.0 microg/L for phorate), RSDr ranged from 4 to 26%. Recoveries for the 11 pesticide residues in all matrixes ranged from 84 to 300% at the 0.1 microg/L level (1.0 microg/L for phorate) and from 66 to 127% at the 0.5 microg/L (5.0 microg/L for phorate) level. Coefficients of determination (r2) of the matrix-matched calibration curves were > or = 0.95. It is recommended that the method be accepted by AOAC

  2. Dynamic behaviour and residual pattern of thiamethoxam and its metabolite clothianidin in Swiss chard using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Rahman, Md Musfiqur; Farha, Waziha; Abd El-Aty, A M; Kabir, Md Humayun; Im, So Jeong; Jung, Da-I; Choi, Jeong-Heui; Kim, Sung-Woo; Son, Young Wook; Kwon, Chan-Hyeok; Shin, Ho-Chul; Shim, Jae-Han

    2015-05-01

    A simultaneous method was developed to analyse thiamethoxam and its metabolite clothianidin in Swiss chard using tandem mass spectrometry (in the positive electrospray ionisation mode using multiple reaction monitoring mode) to estimate the dissipation pattern and the pre-harvest residue limit (PHRL). Thiamethoxam (10%, WG) was sprayed on Swiss chard grown in two different areas under greenhouse conditions at the recommended dose rate of 10 g/20 L water. Samples were collected randomly up to 14 days post-application, extracted using quick, easy, cheap, effective, rugged, safe (QuEChERS) acetate-buffered method and purified via a dispersive solid phase extraction (d-SPE) procedure. Matrix matched calibration showed good linearity with determination coefficients (R(2)) ⩾ 0.998. The limits of detection (LOD) and quantification (LOQ) were 0.007 and 0.02 mg/kg. The method was validated in triplicate at two different spiked concentration levels. Good recoveries (n=3) of 87.48-105.61% with relative standard deviations (RSDs) < 10 were obtained for both analytes. The rate of disappearance of total thiamethoxam residues in/on Swiss chard was best described by first-order kinetics with half-lives of 6.3 and 4.2 days. We predicted from the PHRL curves that if the residues were <19.21 or 26.98 mg/kg at 10 days before harvest, then total thiamethoxam concentrations would be below the maximum residue limits during harvest. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Research of nitroxynil residues in bovine milk following a single administration in the dry period by ultra-performance liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Claudia Chirollo

    2013-10-01

    Full Text Available Nitroxynil (NIT is a halogenated phenol used to control fascioliasis in cattle and sheep. The Commission Regulation EU No 37/2010 has established maximum residue limits for NIT in bovine and ovine muscle (400 μg kg−1, fat (200 μg kg−1, liver (20 μg kg−1 and kidney (400 μg kg−1, and more recently in bovine and ovine milk (20 μg kg−1. Thirty-five pregnant dairy cows were treated in this study with nitroxynil (340 mg/mL solution for injection at the recommended dose of 10 mg/kg body weight at the start of the dry period, i.e. 53 to 74 days before the expected calving. Calving occurred between 43 days and 79 days after treatment. The concentrations of NIT in the milk were monitored for up to 120 days after calving. NIT residues were extracted using acetonitrile; magnesium sulfate and sodium chloride were added to induce liquid-liquid partitioning and purified by dispersive solid phase extraction for clean-up. NIT was detected by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS in negative ionization mode. The highest concentrations of this drug were found in two animals at the first milking, 48 and 53 day post treatment with levels of 362 and 657 μg kg–1, respectively. NIT residues were below the limit of detection of the method (0.24 μg/kg–1 between 67 and 106 day post-treatment. Following calving, residues rapidly depleted in animals and were non-detectable from 10 to 38 days post-calving. In particular, in all animals milk resulted compliant (<20 μg/kg−1 three days post partum.

  4. [Determination of 51 carbamate pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry based on optimization of QuEChERS sample preparation method].

    Science.gov (United States)

    Wang, Lianzhu; Zhou, Yu; Huang, Xiaoyan; Wang, Ruilong; Lin, Zixu; Chen, Yong; Wang, Dengfei; Lin, Dejuan; Xu, Dunming

    2013-12-01

    The raw extracts of six vegetables (tomato, green bean, shallot, broccoli, ginger and carrot) were analyzed using gas chromatography-mass spectrometry (GC-MS) in full scan mode combined with NIST library search to confirm main matrix compounds. The effects of cleanup and adsorption mechanisms of primary secondary amine (PSA) , octadecylsilane (C18) and PSA + C18 on co-extractives were studied by the weight of evaporation residue for extracts before and after cleanup. The suitability of the two versions of QuEChERS method for sample preparation was evaluated for the extraction of 51 carbamate pesticides in the six vegetables. One of the QuEChERS methods was the original un-buffered method published in 2003, and the other was AOAC Official Method 2007.01 using acetate buffer. As a result, the best effects were obtained from using the combination of C18 and PSA for extract cleanup in vegetables. The acetate-buffered version was suitable for the determination of all pesticides except dioxacarb. Un-buffered QuEChERS method gave satisfactory results for determining dioxacarb. Based on these results, the suitable QuEChERS sample preparation method and liquid chromatography-positive electrospray ionization-tandem mass spectrometry under the optimized conditions were applied to determine the 51 carbamate pesticide residues in six vegetables. The analytes were quantified by matrix-matched standard solution. The recoveries at three levels of 10, 20 and 100 microg/kg spiked in six vegetables ranged from 58.4% to 126% with the relative standard deviations of 3.3%-26%. The limits of quantification (LOQ, S/N > or = 10) were 0.2-10 microg/kg except that the LOQs of cartap and thiofanox were 50 microg/kg. The method is highly efficient, sensitive and suitable for monitoring the 51 carbamate pesticide residues in vegetables.

  5. [Monitoring of the residue of fosthiazate in water samples using solid-phase extraction coupled with gas chromatography/mass spectrometry].

    Science.gov (United States)

    Zhu, Jing; Zhou, Xin; Fu, Chunmei; Liu, Sankang; Li, Zhangwan

    2004-11-01

    Solid-phase extraction (SPE) coupled with gas chromatography/mass spectrometry (GC/MS) was used to determine the fosthiazate residue in water samples. The water samples were first filtered through cellulose filters (0.45 microm pore size). A 100 mL volume of filtered water, in which 1 mL of methanol has been added, was then passed through a pre-conditioned 3 cm C18 cartridge at a flow-rate of 1.5 mL/min. Elution was performed by 1 mL of methanol. The eluant was finally dried under reduced pressure for solvent evaporation. The volume was quantitatively adjusted to 0.5 mL with methanol. The analysis was carried out on GC/MS. The mass spectrometer was operated in selected ion monitoring (SIM) mode. According to mass spectrum of fosthiazate, three selected ions at m/z of 126, 195, 283, respectively, were monitored for identification and quantification. High sensitivity and selectivity were achieved by using this method. The limit of detection for fosthiazate in water samples was determined to be 56.4 ng/L. The linearity was demonstrated over a wide range of concentrations covering from 0.282 to 141 microg/L. The recoveries were more than 85.5% and the relative standard deviations for the overall procedure were less than 4.42%. The fosthiazate residue was detected in the water samples from a pool near cropland where fosthiazate was used. The results demonstrate the suitability of the SPE-GC/MS approach for the analysis of fosthiazate in water.

  6. Fermion Masses and Mixing in SUSY Grand Unified Gauge Models with Extended Gut Gauge Groups

    Energy Technology Data Exchange (ETDEWEB)

    Chou, Chih-Lung

    2005-04-05

    The authors discuss a class of supersymmetric (SUSY) grand unified gauge (GUT) models based on the GUT symmetry G x G or G x G x G, where G denotes the GUT group that has the Standard Model symmetry (SU(3){sub c} x SU(2){sub L} x U(1){sub Y}) embedded as a subgroup. As motivated from string theory, these models are constructed without introducing any Higgs field of rani two or higher. Thus all the Higgs fields are in the fundamental representations of the extended GUT symmetry or, when G = SO(10), in the spinorial representation. These Higgs fields, when acquiring their vacuum expectation values, would break the extended GUT symmetry down to the Standard Model symmetry. In this dissertation, they argue that the features required of unified models, such as the Higgs doublet-triplet splitting, proton stability, and the hierarchy of fermion masses and mixing angles, could have natural explanations in the framework of the extended SUSY GUTs. Furthermore, they argue that the frameworks used previously to construct SO(10) GUT models using adjoint Higgs fields can naturally arise from the SO(10) x SO(10) and SO(10) x SO(10) x SO(10) models by integrating out heavy fermions. This observation thus suggests that the traditional SUSY GUT SO(10) theories can be viewed as the low energy effective theories generated by breaking the extended GUT symmetry down to the SO(10) symmetry.

  7. Residual deposits (residual soil)

    International Nuclear Information System (INIS)

    Khasanov, A.Kh.

    1988-01-01

    Residual soil deposits is accumulation of new formate ore minerals on the earth surface, arise as a result of chemical decomposition of rocks. As is well known, at the hyper genes zone under the influence of different factors (water, carbonic acid, organic acids, oxygen, microorganism activity) passes chemical weathering of rocks. Residual soil deposits forming depends from complex of geologic and climatic factors and also from composition and physical and chemical properties of initial rocks

  8. Quantification, confirmation and screening capability of UHPLC coupled to triple quadrupole and hybrid quadrupole time-of-flight mass spectrometry in pesticide residue analysis.

    Science.gov (United States)

    Grimalt, Susana; Sancho, Juan V; Pozo, Oscar J; Hernández, Félix

    2010-04-01

    The potential of three mass spectrometry (MS) analyzers (triple quadrupole, QqQ; time of flight, TOF; and quadrupole time of flight, QTOF) has been investigated and compared for quantification, confirmation and screening purposes in pesticide residue analysis of fruit and vegetable samples. For this purpose, analytical methodology for multiresidue determination of 11 pesticides, taken as a model, has been developed and validated in nine food matrices for the three mass analyzers coupled to ultra high pressure liquid chromatography. In all cases, limits of quantification around 0.01 mg/kg were reached, fulfilling the most restrictive case of baby-food analysis. Regarding absolute sensitivity, the lower limits of detection were obtained, as expected, for QqQ (100 fg), whereas slightly higher limits (300 fg) were obtained for both TOF and QTOF. Confirmative capacity of each analyzer was studied for each analyte based on the identification points (IPs) criterion, useful for a comprehensive comparison. QTOF mass analyzer showed the highest confirmatory capacity, although QqQ normally led to sufficient number of IPs, even at lower concentration levels. The potential of TOF MS was also investigated for screening purposes. To this aim, around 50 commercial fruits and vegetables samples were analyzed, searching for more than 400 pesticides. TOF MS proved to be an attractive analytical tool for rapid detection and reliable identification of a large number of pesticides thanks to the full spectrum acquisition at accurate mass with satisfactory sensitivity. This process is readily boosted when combined with specialized software packages, together with theoretical exact mass databases. Several pesticides (e.g. carbendazim in citrus and indoxacarb in grape) were detected in the samples. Further unequivocal confirmation of the identity was performed using reference standards and/or QTOF MS/MS experiments. Copyright 2010 John Wiley & Sons, Ltd.

  9. Analysis of pesticide and veterinary drug residues in baby food by liquid chromatography coupled to Orbitrap high resolution mass spectrometry.

    Science.gov (United States)

    Gómez-Pérez, María Luz; Romero-González, Roberto; Luis Martínez, Vidal José; Garrido Frenich, Antonia

    2015-01-01

    Pesticide and veterinary drug residues have been simultaneously determined in several baby foods as meat, fish and vegetable-based baby food. A generic extraction method without clean-up step was applied. Moreover, the use of a representative matrix for proper quantification of all target compounds was studied and the best results were obtained when vegetable-based baby food was used as representative matrix, allowing the reliable quantification of more than 300 compounds. The method was validated and good recoveries were obtained for most of compounds at concentrations higher than 50 µg kg(-1). Limits of detection (LOD) ranged from 0.5 to 50 µg kg(-1), whereas limits of quantification (LOQ) were established between 10 and 100 µg kg(-1). Limits of identification (LOIs) ranged from 0.5 to 50 µg kg(-1). This method was applied to the analysis of 46 different baby food samples and no positive samples were found. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Multi-residue determination of micropollutants in Phragmites australis from constructed wetlands using microwave assisted extraction and ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Petrie, Bruce; Smith, Benjamin D; Youdan, Jane; Barden, Ruth; Kasprzyk-Hordern, Barbara

    2017-03-22

    In constructed wetlands micropollutants can be removed from water by phytoremediation. However, micropollutant uptake and metabolism by plants here is poorly understood due to the lack of good analytical approaches. Reported herein is the first methodology developed and validated for the multi-residue determination of 81 micropollutants (pharmaceuticals, personal care products and illicit drugs) in the emergent macrophyte Phragmites australis. The method involved extraction by microwave accelerated extraction (MAE), clean-up using off-line solid phase extraction and analysis by ultra-high-performance liquid chromatography tandem mass spectrometry. Development of the MAE method found the influence of studied variables on micropollutant recovery to be: extraction temperature > sample mass > solvent composition. Validation of the developed extraction protocol revealed method recoveries were in the range 80-120% for the majority of micropollutants. Method quantitation limits (MQLs) were generally MQL, up to concentrations of 200 ng g -1 . Other than uptake, the presence of several metabolites (carbamazepine 10,11 epoxide, desvenlafaxine, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine, N-desmethyltramadol and norketamine) indicated metabolism within the plant may also occur. This new analytical methodology will enable a process mass balance of the constructed wetland to be attained for the first time, and thus help understand the role of phytoremediation in micropollutant removal by such systems. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

  11. Comparison of magnetic resonance imaging and 67gallium scintigraphy in the evaluation of posttherapeutic residual mediastinal mass in the patients with Hodgkin's lymphoma

    International Nuclear Information System (INIS)

    Herman, Miroslav; Paucek, Boris; Raida, Ludek; Myslivecek, Miroslav; Zapletalova, Jana

    2007-01-01

    Introduction: Detection of residual disease following the completion of primary treatment in Hodgkin's lymphoma (HL) patients diagnosed with mediastinal tumor mass has an exceptional importance in the assessment of therapeutic response. Magnetic resonance imaging (MRI) and 67 gallium ( 67 Ga) scintigraphy can be used to identify active tumor tissue in the mediastinal residuum. Aims: To evaluate: the accuracy of MRI and 67 Ga scintigraphy in the prediction of clinical HL relapse/progression; congruence of findings and the probability of mediastinal disease relapse/progression regarding to the detection of active/inactive tissue by both imaging methods. Materials and methods: Thirty HL patients with abnormal mediastinal tissue following the completion of primary treatment were examined by MRI and 67 Ga scintigraphy. Positive findings were: high signal intensity on unenhanced T2-weighted images on MRI and the abnormal accumulation of gallium on scintigraphy or SPECT. These findings were compared with the clinical follow-up. Results: Sensitivity, specificity, accuracy, positive and negative predictive values were: 75.0%, 96.2%, 93.3%, 75.0%, 96.2% in MRI and 50.0%, 88.5%, 83.3%, 40.0%, 92.0% in 67 Ga scintigraphy. Discrepant results concerning the mediastinal tissue activity were found in 3 of 30 patients (10%). No statistically significant differences were found between both imaging methods in sensitivity, specificity and accuracy. Estimated 2-years progression free survival (PFS) for patients without and with active residual mediastinal tissue by MRI was 96% and 25% (p = 0.0001), respectively. The probability of 2-years PFS in the cases with negative and positive findings on 67 Ga scintigraphy was 92% and 60% (p = 0.026), respectively. Conclusion: Although MRI showed better results than 67 Ga scintigraphy in the assessment of residual mediastinal tissue activity in HL patients after primary treatment, the difference between these methods was not statistically

  12. Determination of low-level agricultural residues in soft drinks and sports drinks by liquid chromatography/tandem mass spectrometry: single-laboratory validation.

    Science.gov (United States)

    Paske, Nathan; Berry, Bryan; Schmitz, John; Sullivan, Darryl

    2007-01-01

    In this study, sponsored by PepsiCo Inc., a method was validated for measurement of 11 pesticide residues in soft drinks and sports drinks. The pesticide residues determined in this validation were alachlor, atrazine, butachlor, isoproturon, malaoxon, monocrotophos, paraoxon-methyl, phorate, phorate sulfone, phorate sulfoxide, and 2,4-dichlorophenoxyacetic acid (2,4-D) when spiked at 0.100 microg/L (1.00 microg/L for phorate). Samples were filtered (if particulate matter was present), degassed (if carbonated), and analyzed using liquid chromatography with tandem mass spectrometry. Quantitation was performed with matrix-matched external standard calibration solutions. The standard curve range for this assay was 0.0750 to 10.0 microg/L. The calibration curves for all agricultural residues had coefficient of determination (r2) values greater than or equal to 0.9900 with the exception of 2 values that were 0.9285 and 0.8514. Fortification spikes at 0.100 microg/L (1.00 microg/L for phorate) over the course of 2 days (n=8 each day) for 3 matrixes (7UP, Gatorade, and Diet Pepsi) yielded average percent recoveries (and percent relative standard deviations) as follows (n=48): 94.4 (15.2) for alachlor, 98.2 (13.5) for atrazine, 83.1 (41.6) for butachlor, 89.6 (24.5) for isoproturon, 87.9 (24.4) for malaoxon, 96.1 (9.26) for monocrotophos, 101 (25.7) for paraoxon-methyl, 86.6 (20.4) for phorate, 101 (16.5) for phorate sulfone, 93.6 (25.5) for phorate sulfoxide, and 98.2 (6.02) for 2,4-D.

  13. Determination of pesticide residues and related compounds in water and industrial effluent by solid-phase extraction and gas chromatography coupled to triple quadrupole mass spectrometry.

    Science.gov (United States)

    Martins, Manoel L; Donato, Filipe F; Prestes, Osmar D; Adaime, Martha B; Zanella, Renato

    2013-09-01

    Pollution of drinking water supplies from industrial waste is a result of several industrial processes and disposal practices, and the establishment of analytical methods for monitoring organic compounds related to environmental and health problems is very important. In this work, a method using solid-phase extraction (SPE) and gas chromatography coupled to triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) was developed and validated for the simultaneous determination of pesticide residues and related compounds in drinking and surface water as well as in industrial effluent. Optimization of the method was achieved by using a central composite design approach on parameters such as the sample pH and SPE eluent composition. A single SPE consisting of the loading on a polymeric sorbent of 100 mL of sample adjusted to pH 3 and elution with methanol/methylene chloride (10:90, v/v) permitted the obtaining of acceptable recoveries in most cases. The concentration factor associated with sensitivity of the chromatographic analysis permitted the achievement of the method limit of detection values between 0.01 and 0.25 μg L(-1). Recovery assays presented mean recoveries between 70 and 120% for most of the compounds with very good precision, despite the different chemical nature of the compounds analyzed. The selectivity of the method, evaluated through the relative intensity of quantification and qualification ions obtained by GC-QqQ-MS/MS, was considered adequate. The developed method was finally applied to the determination of target analytes in real samples. River water and treated industrial effluent samples presented residues of some compounds, but no detectable residues were found in the drinking water samples evaluated.

  14. Development of a multi-residue screening method for the determination of pesticides in cereals and dry animal feed using gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Walorczyk, Stanisław

    2007-09-21

    A multi-residue screening method for simultaneous analysis of 122 gas chromatography amenable pesticides in dry matrices such as cereal grain and certain feedingstuffs was developed. The method entails a simple extraction of re-hydrated sample with acetonitrile followed by a dispersive solid phase extraction (dispersive-SPE) clean-up step prior to the final determination by gas chromatography/triple quadrupole tandem mass spectrometry (GC-MS/MS). Due to complexity of analyzed matrices, two MS/MS transitions were set for each pesticide to eliminate the need for re-analysis of potentially positive samples, and provide unequivocal identification of detected pesticides in accordance with recent guidelines, in a single analytical run. Thus, in the developed GC-MS/MS acquisition method, a total of 216 different multiple reactions monitoring (MRM) transitions were monitored in one set of experimental conditions. To evaluate performance of the method, validation experiments were carried out on wheat grain at three spiking levels (0.01, 0.02 and 0.05 mg kg(-1)). Additional recovery tests at 0.05 mg kg(-1) were carried out on several other matrices. The recoveries ranged between 73 and 129% with associated relative standard deviations between 1 and 29% for the majority of pesticides. Limits of detection were less or equal to 0.01 mg kg(-1) for approximately 68% of pesticides. The applicability of the proposed method to detect and quantify pesticide residues has been demonstrated in the analysis of 136 real samples. Additionally, the method was favorably compared with an acetone extraction method (accepted as a reference method by some of European and U.S. authorities) in the analysis of real samples known to contain pesticide residues.

  15. First results from the IllustrisTNG simulations: the stellar mass content of groups and clusters of galaxies

    Science.gov (United States)

    Pillepich, Annalisa; Nelson, Dylan; Hernquist, Lars; Springel, Volker; Pakmor, Rüdiger; Torrey, Paul; Weinberger, Rainer; Genel, Shy; Naiman, Jill P.; Marinacci, Federico; Vogelsberger, Mark

    2018-03-01

    The IllustrisTNG project is a new suite of cosmological magnetohydrodynamical simulations of galaxy formation performed with the AREPO code and updated models for feedback physics. Here, we introduce the first two simulations of the series, TNG100 and TNG300, and quantify the stellar mass content of about 4000 massive galaxy groups and clusters (1013 ≤ M200c/M⊙ ≤ 1015) at recent times (z ≤ 1). The richest clusters have half of their total stellar mass bound to satellite galaxies, with the other half being associated with the central galaxy and the diffuse intracluster light. Haloes more massive than about 5 × 1014 M⊙ have more diffuse stellar mass outside 100 kpc than within 100 kpc, with power-law slopes of the radial mass density distribution as shallow as the dark matter's ( - 3.5 ≲ α3D ≲ -3). Total halo mass is a very good predictor of stellar mass, and vice versa: at z = 0, the 3D stellar mass measured within 30 kpc scales as ∝(M500c)0.49 with a ˜0.12 dex scatter. This is possibly too steep in comparison to the available observational constraints, even though the abundance of The Next Generation less-massive galaxies ( ≲ 1011 M⊙ in stars) is in good agreement with the measured galaxy stellar mass functions at recent epochs. The 3D sizes of massive galaxies fall too on a tight (˜0.16 dex scatter) power-law relation with halo mass, with r^stars_0.5 ∝ (M_200c)^{0.53}. Even more fundamentally, halo mass alone is a good predictor for the whole stellar mass profiles beyond the inner few kiloparsecs, and we show how on average these can be precisely recovered given a single-mass measurement of the galaxy or its halo.

  16. [Determination of pesticide residues in fugu, eel and prawn using gas chromatography-mass spectrometry with gel permeation chromatographic clean-up].

    Science.gov (United States)

    Zheng, Feng; Pang, Guofang; Li, Yan; Wang, Minglin; Fan, Chunlin

    2009-09-01

    A multiresidue analytical method was developed for the determination of 191 pesticides in fugu, eel and prawn using gas chromatography-mass spectrometry (GC-MS). The samples were extracted with ethyl acetate and cyclohexane (1:1, v/v), and cleaned-up by gel permeation chromatography (GPC). The GPC eluant collected from 26 min to 44 min was concentrated to 1 mL, then analyzed using GC-MS. A DB-1701 column was used for the separation. The MS detection was performed in selected ion monitoring mode. The recoveries were determined at the two spiked levels of I LOQ and 4 LOQ (LOQ: limit of quantification). The overall recoveries were from 50.2% to 120%, and in which the recoveries of 89.5% pesticides were from 70% to 120%. The relative standard deviations (RSDs) of the recoveries were from 0.6% to 21.6%. The calibration curves of all pesticides showed good linearities in the respective ranges with the correlation coefficient above 0.97. The limits of detection and the limits of quantification were 0.002-0.3 mg/kg and 0.007-1.2 mg/kg, respectively. The sensitivity and accuracy of the method met the requirements of the multiple pesticide residues. This method was applicable to determine 191 multiple pesticide residues in fugu, eel, prawn and other fishes.

  17. Determination of 1,2-dibromoethane, 1,4-dichlorobenzene and naphthalene residues in honey by gas chromatography--mass spectrometry using purge and trap thermal desorption extraction.

    Science.gov (United States)

    Tananaki, Chrisoula; Zotou, Anastasia; Thrasyvoulou, Andreas

    2005-08-12

    A highly sensitive method for the determination of 1,2-dibromoethane, 1,2-dichlorobenzene and naphthalene residues in honey was developed, using gas chromatography-mass spectrometry combined with a purge and trap thermal desorption system as the extraction technique. Optimal conditions for isolation and separation were established and calibration curves were constructed. Linearity was held between 2.4 and 300 microg kg(-1) honey for 1,2-dibromoethane, 0.5 and 300 microg kg(-1) for 1,4-dichlorobenzene and 0.125 and 3000 microg kg(-1) for naphthalene. The detection limits were found to be 0.8, 0.15 and 0.05 microg kg(-1) honey for 1,2-dibromoethane, 1,4-dichlorobenzene and naphthalene, respectively. The method was applied to the analysis of 25 Greek honey samples. 1,2-Dibromoethane was not found in the majority of the samples, while only one sample was found to contain both 1,4-dichlorobenzene and naphthalene residues at concentrations exceeding 10 microg kg(-1).

  18. [Determination of linuron and its metabolite 3,4-dichloroaniline residues in meat and meat products using liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Guo, Dehua; Yi, Xionghai; Qu, Li

    2011-10-01

    A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of linuron and its metabolite 3, 4-dichloroaniline residues in pork, liver, kidney, casings, canned steam pork and sausage. The sample was extracted with a mixture of acetone-acetonitrile (5: 95, v/v). Most of the lipids in the extract were eliminated by freezing-lipid filtration. After Florisil solid phase extraction cleanup, the linuron and its metabolite residues were determined by LC-MS/MS, and quantified by internal standard meth-od. In the range of 1 - 500 microg/L, both linuron and 3,4-dichloroaniline showed good linearity with the correlation coefficients (r) more than 0. 998. The limit of quantification (S/N > 10) was 10 microg/kg, and the limit of detection (S/N > 3) was 5 microg/kg for each analyte. The recoveries of linuron and 3,4-dichloroaniline in meat and meat products at three spiked levels were in the ranges of 88.3% - 101.2% and 91.6% - 101. 6%, and the relative standard deviations were in the ranges of 4. 8% - 13. 7% and 4. 7% - 11. 8%, respectively. The results demonstrated that the proposed method can meet the requirements for the determination of linuron and 3,4-dichloroaniline in meat and meat products.

  19. Activated sludge mass reduction and biodegradability of the endogenous residues by digestion under different aerobic to anaerobic conditions: Comparison and modeling.

    Science.gov (United States)

    Martínez-García, C G; Fall, C; Olguín, M T

    2016-03-01

    This study was performed to identify suitable conditions for the in-situ reduction of excess sludge production by intercalated digesters in recycle-activated sludge (RAS) flow. The objective was to compare and model biological sludge mass reduction and the biodegradation of endogenous residues (XP) by digestion under hypoxic, aerobic, anaerobic, and five intermittent-aeration conditions. A mathematical model based on the heterotrophic endogenous decay constant (bH) and including the biodegradation of XP was used to fit the long-term data from the digesters to identify and estimate the parameters. Both the bH constant (0.02-0.05 d(-1)) and the endogenous residue biodegradation constant (bP, 0.001-0.004 d(-1)) were determined across the different mediums. The digesters with intermittent aeration cycles of 12 h-12 h and 5 min-3 h (ON/OFF) were the fastest, compared to the aerobic reactor. The study provides a basis for rating RAS-digester volumes to avoid the accumulation of XP in aeration tanks. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Automated multi-plug filtration cleanup for liquid chromatographic-tandem mass spectrometric pesticide multi-residue analysis in representative crop commodities.

    Science.gov (United States)

    Qin, Yuhong; Zhang, Jingru; Zhang, Yuan; Li, Fangbing; Han, Yongtao; Zou, Nan; Xu, Haowei; Qian, Meiyuan; Pan, Canping

    2016-09-02

    An automated multi-plug filtration cleanup (m-PFC) method on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. The automatic device was aimed to reduce labor-consuming manual operation workload in the cleanup steps. It could control the volume and the speed of pulling and pushing cycles accurately. In this work, m-PFC was based on multi-walled carbon nanotubes (MWCNTs) mixed with other sorbents and anhydrous magnesium sulfate (MgSO4) in a packed tip for analysis of pesticide multi-residues in crop commodities followed by liquid chromatography with tandem mass spectrometric (LC-MS/MS) detection. It was validated by analyzing 25 pesticides in six representative matrices spiked at two concentration levels of 10 and 100μg/kg. Salts, sorbents, m-PFC procedure, automated pulling and pushing volume, automated pulling speed, and pushing speed for each matrix were optimized. After optimization, two general automated m-PFC methods were introduced to relatively simple (apple, citrus fruit, peanut) and relatively complex (spinach, leek, green tea) matrices. Spike recoveries were within 83 and 108% and 1-14% RSD for most analytes in the tested matrices. Matrix-matched calibrations were performed with the coefficients of determination >0.997 between concentration levels of 10 and 1000μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Determination of some selected pesticide residues in apple juice by solid-phase microextraction coupled to gas chromatography – mass spectrometry

    Directory of Open Access Journals (Sweden)

    Andrea Hercegová

    2011-01-01

    Full Text Available The performance of solid phase microextraction (SPME for enrichment of pesticides from apple juice was investigated. Samples were diluted with water, extracted by solid-phase microextraction and analysed by gas chromatography using mass-spectrometry detector (MSD in selected ion monitoring mode (SIM. The method was tested for the following pesticides used mostly in fruit culturing at Slovakia: tebuthylazine, fenitrothion, chlorpyrifos, myclobutanil, cyprodinil, phosalone, pyrimethanil, tebuconazole, kresoxim-methyl, methidathion, penconazole. All pesticides were extracted with polydimethylsiloxane fibre 100 μm thickness. The linear concentration range of application was 0.05 μg dm−3–10 μg dm−3. The method described provides detectabilities complying with the maximum residue levels (MRLs set by regulatory organizations for pesticides in apple juice matrices. The solvent – free SPME procedure was found to be quicker and more cost effective then the solvent extraction methods commonly used.

  2. Development and validation of a multi-residue method for the detection of a wide range of hormonal anabolic compounds in hair using gas chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rambaud, Lauriane [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Monteau, Fabrice [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Deceuninck, Yoann [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Bichon, Emmanuelle [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Andre, Francois [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Le Bizec, Bruno [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France)]. E-mail: lebizec@vet-nantes.fr

    2007-03-14

    The monitoring of anabolic steroid residues in hair is undoubtedly one of the most efficient strategies to demonstrate the long-term administration of these molecules in meat production animals. A multi-residue sample preparation procedure was developed and validated for 28 steroids. A 100 mg hair sample was grinded into powder and extracted at 50 deg. C with methanol. After acidic hydrolysis and extraction with ethyl acetate, phenolsteroids, such as estrogens, resorcyclic acid lactones and stilbens in one hand, are separated from androgens and progestagens in the other hand. Solid phase extractions were performed before applying a specific derivatisation for each compound sub-group. Detection and identification were achieved using gas chromatography-tandem mass spectrometry with acquisition in the selected reaction monitoring mode after electron ionisation. The method was validated according to the 2002/657/EC guideline. Decision limits (CC{alpha}) for main steroids were in the 0.1-10 {mu}g kg{sup -1} range.

  3. [Simultaneous determination of 18 β-agonist residues in feed using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zheng, Ling; Wu, Yujie; Zhao, Yongfeng; Li, Lihua; Ma, Yanjuan

    2014-08-01

    A multi-residue method was developed for the simultaneous determination of 18 β-agonist residues (clenbuterol, ractopamine, penbutolol, tulobuterol, etc) in feed by using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The feed samples were dispersed by water, then the analytes were extracted with acetonitrile containing 4% (v/v) ammonia and cleaned up by QuEChERS method with 25 mg octadecylsilyl (C18) and 50 mg primary secondary amine (PSA) adsorbents. The separation of compounds was carried on an Agilent ZORBAX Eclipse XDB-C,8 column (50 mm x 4. 6 mm, 1. 8 μm) by a gradient elution using methanol-0. 1% (v/v) formic acid aqueous solution as mobile phase. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+) and quantified by the matrix-matched external standard method. The results showed that the calibration curves of the 18 β-agonists were linear in the range of 5 - 200 μg/L with correlation coefficients of 0. 9912-0. 9995. The average recoveries of the 18 analytes at three spiked levels of 0.05, 0.1 and 0. 5 mg/kg ranged from 78. 4% to 107. 1% with the relative standard deviations (RSDs) of 3.5%-12.3%. The limit of quantification (LOQ, S/N≥10) was 0. 05 mg/kg for each analyte. The developed method is simple and sensitive, and can be applied as a screen and confirmatory method for the analysis of β-agonists in feed.

  4. Determination of pyrethroid pesticide residues in processed fruits and vegetables by gas chromatography with electron capture and mass spectrometric detection.

    Science.gov (United States)

    Sannino, Anna; Bandini, Mirella; Bolzoni, Luciana

    2003-01-01

    A gas chromatographic method was developed for the simultaneous determination of 12 pyrethroids (tefluthrin, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cyfluthrin, cypermethrin, alpha-cypermethrin, flucythrinate, fenvalerate, fluvalinate, and deltamethrin) in tomato puree, peach nectar, orange juice, and canned peas. A miniaturized extraction-partition procedure requiring small amounts of nonchlorinated solvents is used. Samples are extracted with acetone, partitioned with ethyl acetate-cyclohexane (50 + 50, v/v), and cleaned up on a Florisil cartridge. The final extract is analyzed by gas chromatography with both electron capture and mass spectrometric detection modes. Studies at fortification levels of 0.010-0.100 mg/kg gave mean recoveries ranging from 70.2 to 96.0% and coefficients of variation between 4.0 and 13.9% for all compounds. Quantitation limits were < 0.010 mg/kg for electron capture detection.

  5. A feasibility study to identify proteins in the residual Pap test fluid of women with normal cytology by mass spectrometry-based proteomics.

    Science.gov (United States)

    Boylan, Kristin Lm; Afiuni-Zadeh, Somaieh; Geller, Melissa A; Hickey, Kayla; Griffin, Timothy J; Pambuccian, Stefan E; Skubitz, Amy Pn

    2014-01-01

    The proteomic analysis of body fluids is a growing technology for the identification of protein biomarkers of disease. Given that Papanicolaou tests (Pap tests) are routinely performed on over 30 million women annually in the U.S. to screen for cervical cancer, we examined the residual Pap test fluid as a source of protein for analysis by mass spectrometry (MS). In the liquid-based Pap test, cervical cells are collected from the ectocervix and placed into an alcohol-based fixative prior to staining and pathologic examination. We hypothesized that proteins shed by cells of the female genital tract can be detected in the Pap test fixative by MS-based proteomic techniques. We examined the feasibility of using residual fluid from discarded Pap tests with cytologically "normal" results to optimize sample preparation for MS analysis. The protein composition of the cell-free Pap test fluid was determined by silver staining of sodium dodecyl sulfate -polyacrylamide gels, and the abundance of serum proteins was examined by Western immunoblot using an antibody against human serum albumin. Both pooled and individual samples were trypsin digested and analyzed by two-dimensional MS/MS. Proteins were identified by searching against the Human Uniprot database, and characterized for localization, function and relative abundance. The average volume of the residual Pap test fluid was 1.5 ml and the average protein concentration was 0.14 mg/ml. By Western immunoblot we showed that the amount of albumin in each sample was significantly reduced compared to normal serum. By MS/MS, we identified 714 unique proteins in pooled Pap test samples and an average of 431 proteins in individual samples. About 40% of the proteins identified were extracellular or localized to the plasma membrane. Almost 20% of the proteins identified were involved in immunity and defense, characteristic of the healthy cervical-vaginal proteome. By merging the protein sets from the individual and pooled Pap test

  6. Body Mass Index (BMI assessment among Macau students: age group differences and weight management strategies

    Directory of Open Access Journals (Sweden)

    Ho Walter King Yan

    2017-12-01

    Full Text Available There is evidence that rapid weight gain during the first year of life is associated with being overweight later in life. Therefore, overweight tendencies need to be detected at an appropriate age, and suitable strategies need to be implemented for weight management to achieve optimal long-term health. The objective of this study was to investigate comparisons in BMI status and associated categories in male and female students over ten years in two phases, including 2008-2013 and 2009-2014. Weight and height data were collected to obtain BMI (Body Mass Index over ten years in two phases. The first phase occurred from 2008 to 2013, and the second phase occurred from 2009 to 2014 in a population of 10846 school children (Males: 6970, 64.3%, and females: 3875, 35.7% in Macau. Their ages ranged from 6 years old in 2008 to 11 years old in 2013. The same age range was observed in the second phase, i.e., 2009-2014. Statistical analyses included descriptive statistics, such as the mean, standard deviation, t-tests to determine gender differences (year-wise and a Chi square test for independence to determine the relationship between BMI (Underweight, Standard, Overweight and Obese and age groups. In the first phase (2008-2013, the findings indicated a higher BMI level among the male students than the female students across all age groups (2008 t = 5.24, 2009 t = 88.25, 2010 t = 11.32, 2011 t = 17.45, 2012 t = 19.70 and 2013 t = 19.92. In the second phase (2009-2014, a higher BMI level was found among the male students than the female students across all age groups (2009 t = 2.68, 2010 t = 2.886, 2011 t = 3.076, 2013 t = 4.228, and 2014 t = 2.405. The results of the two phases combined (2008 to 2014 and 2009 to 2014 revealed that male students in 2008 had a higher BMI level than their counterparts in 2009 in the two age categories (8 years t = 3.025 and 11 years t = 3.377. Female students in the second phase (2009-2014 showed a higher BMI level than their

  7. Fast gas chromatographic residue analysis in animal feed using split injection and atmospheric pressure chemical ionisation tandem mass spectrometry.

    Science.gov (United States)

    Tienstra, M; Portolés, T; Hernández, F; Mol, J G J

    2015-11-27

    Significant speed improvement for instrumental runtime would make GC–MS much more attractive for determination of pesticides and contaminants and as complementary technique to LC–MS. This was the trigger to develop a fast method (time between injections less than 10 min) for the determination of pesticides and PCBs that are not (or less) amenable to LC–MS. A key factor in achieving shorter analysis time was the use of split injection (1:10) which allowed the use of a much higher initial GC oven temperature. A shorter column (15 m), higher temperature ramp, and higher carrier gas flow rate (6 mL/min) further contributed to analysis-time reduction. Chromatographic resolution was slightly compromised but still well fit-for-purpose. Due to the high sensitivity of the technique used (GC–APCI-triple quadrupole MS/MS), quantification and identification were still possible down to the 10 μg/kg level, which was demonstrated by successful validation of the method for complex feed matrices according to EU guidelines. Other advantages of the method included a better compatibility of acetonitrile extracts (e.g. QuEChERS) with GC, and a reduced transfer of co-extractants into the GC column and mass spectrometer.

  8. Simultaneous Determination of Hormonal Residues in Treated Waters Using Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Rayco Guedes-Alonso

    2013-01-01

    Full Text Available In the last years, hormone consumption has increased exponentially. Because of that, hormone compounds are considered emerging pollutants since several studies have determinted their presence in water influents and effluents of wastewater treatment plants (WWTPs. In this study, a quantitative method for the simultaneous determination of oestrogens (estrone, 17β-estradiol, estriol, 17α-ethinylestradiol, and diethylstilbestrol, androgens (testosterone, and progestogens (norgestrel and megestrol acetate has been developed to determine these compounds in wastewater samples. Due to the very low concentrations of target compounds in the environment, a solid phase extraction procedure has been optimized and developed to extract and preconcentrate the analytes. Determination and quantification were performed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS. The method developed presents satisfactory limits of detection (between 0.15 and 9.35 ng·L−1, good recoveries (between 73 and 90% for the most of compounds, and low relative standard deviations (under 8.4%. Samples from influents and effluents of two wastewater treatment plants of Gran Canaria (Spain were analyzed using the proposed method, finding several hormones with concentrations ranged from 5 to 300 ng·L−1.

  9. Determination of the limits of identification and quantitation of selected organochlorine and organophosphorous pesticide residues in surface water by full-scan gas chromatography/mass spectrometry.

    Science.gov (United States)

    Tahboub, Yahya R; Zaater, Mohammad F; Al-Talla, Zeiad A

    2005-12-09

    In this work, we report a reliable method for quantitation and determination of the limits of identification of 14 organochlorine and organophosphorous pesticide (OPP) residues in surface water. The method features the simultaneous identification and quantitation of targeted pesticides and the possibility of identification of any other eluting compounds. The method is based on liquid-liquid extraction (LLE) with a mixture of petroleum ether and dichloromethane (70:30, v/v) followed by gas chromatographic separation and a full-scan mass spectrometric detection (GC-MS). The method presents a new validation parameter, limit of identification (LOI) which is defined for our purpose as the lowest analyte concentration that yields a library searchable mass spectrum. The method is linear over the range 0.048-1.20microgL(-1) for nine pesticides and 0.024-0.60microgL(-1) for the other five pesticides. Correlation coefficients vary between 0.988 and 0.998. Limits of detection (LODs) vary between 0.005 and 0.05microgL(-1) for 4,4'-DDT and LOIs vary between 0.012 and 0.048microgL(-1).

  10. Analysis of veterinary drug and pesticide residues in animal feed by high-resolution mass spectrometry: comparison between time-of-flight and Orbitrap.

    Science.gov (United States)

    Gómez-Pérez, María Luz; Romero-González, Roberto; Martínez Vidal, José Luis; Garrido Frenich, Antonia

    2015-01-01

    The use of medium-high-resolution mass spectrometers (M-HRMS) provides many advantages in multi-residue analysis. A comparison between two mass spectrometers, medium-resolution (MRMS) time-of-flight (TOF) and high-resolution (HRMS) Orbitrap, has been carried out for the analysis of toxic compounds in animal feed. More than 300 compounds belonging to several classes of veterinary drugs (VDs) and pesticides have been determined in different animal feed samples using a generic extraction method. The use of a clean-up procedure has been evaluated in both instruments, and several validation parameters have been established, such as the matrix effect, linearity, recovery and sensitivity. Finally, both instruments have been used during the analysis of 18 different feed samples (including chicken, hen, rabbit and horse). Some VDs (sulfadiazine, trimethoprim, robenidine and monensin sodium) and one pesticide (chlorpyrifos) have been identified. In general, better results were obtained using the Orbitrap, such as sensitivity (1-12.5 µg kg(-1)) and recovery values (60-125%). Moreover, this analyser had several software tools, which reduced the time for data processing and were easy to use, performing quick screening for more than 450 compounds in less than 5 min. However, some disadvantages such as the high cost and a decrease in the number of detected compounds at low concentrations must be taken into account.

  11. Alendronate has a residual effect on bone mass in postmenopausal Danish women up to 7 years after treatment withdrawal

    DEFF Research Database (Denmark)

    Bagger, Yu Z; Tankó, László B; Alexandersen, Peter

    2003-01-01

    for 7, 5, or 3 yr, respectively. Bone mineral density of the lumbar spine, hip, and forearm was measured by dual-energy x-ray absorptiometry. Biochemical markers of bone turnover were induced serum C-terminal telopeptides of type I collagen (CTX) and osteocalcin. Women who received alendronate (2...... was found in women treated with alendronate 20 mg per day for 2 yr (9.7%, P=0.01 vs. placebo). The rate of bone loss after alendronate withdrawal was comparable to the bone loss observed in the placebo group. Bone markers tended to reverse back to normal levels, but were still affected even several years...

  12. Pleomorphic ichthyosis: proposed name for a heterogeneous group of congenital ichthyoses with phenotypic shifting and mild residual scaling.

    Science.gov (United States)

    Vahlquist, Anders

    2010-09-01

    Congenital ichthyosis is often associated with typical neonatal phenotypes, "Collodion baby" and "Harlequin foetus", later transforming into severe lamellar or erythrodermic ichthyosis. However, in a minority of cases the skin condition will improve spontaneously after birth, although slight scaling, xerosis, hypohidrosis and keratoderma usually persist. Some of these patients will eventually be diagnosed as suffering from self-improving collodion ichthyosis, ichthyosis prematurity syndrome, or other, even rarer, forms of ichthyosis also characterized by a phenotypic shift in early childhood. This paper summarizes newly described aetiologies for some of these diseases and discusses difficulties encountered when trying to distinguish them clinically from other types of autosomal recessive congenital ichthyosis. To remind health providers about this heterogeneous group of partially transient disorders of cornification, a new umbrella term, "pleomorphic ichthyosis", is proposed.

  13. Blood group genotyping: the power and limitations of the Hemo ID Panel and MassARRAY platform.

    Science.gov (United States)

    McBean, Rhiannon S; Hyland, Catherine A; Flower, Robert L

    2015-01-01

    Matrix-assisted laser desorption/ionization, time-of-flight mass spectrometry (MALDI-TOF MS), is a sensitive analytical method capable of resolving DNA fragments varying in mass by a single nucleotide. MALDI-TOF MS is applicable to blood group genotyping, as the majority of blood group antigens are encoded by single nucleotide polymorphisms. Blood group genotyping by MALDI-TOF MS can be performed using a panel (Hemo ID Blood Group Genotyping Panel, Agena Bioscience Inc., San Diego, CA) that is a set of genotyping assays that predict the phenotype for 101 antigens from 16 blood group systems. These assays involve three fundamental stages: multiplex target-specific polymerase chain reaction amplification, allele-specific single base primer extension, and MALDI-TOFMS analysis using the MassARRAY system. MALDI-TOF MS-based genotyping has many advantages over alternative methods including high throughput, high multiplex capability, flexibility and adaptability, and the high level of accuracy based on the direct detection method. Currently available platforms for MALDI-TOF MS-based genotyping are not without limitations, including high upfront instrumentation costs and the number of non-automated steps. The Hemo ID Blood Group Genotyping Panel, developed and optimized in a collaboration between the vendor and the Blood Transfusion Service of the Swiss Red Cross in Zurich, Switzerland, is not yet widely utilized, although several laboratories are currently evaluating the MassARRAY system for blood group genotyping. Based on the accuracy and other advantages offered by MALDITOF MS analysis, in the future, this method is likely to become widely adopted for blood group genotyping, in particular, for population screening.

  14. Multi-residue determination of 10 selected new psychoactive substances in wastewater samples by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Borova, Viola L; Gago-Ferrero, Pablo; Pistos, Constantinos; Thomaidis, Nikolaos S

    2015-11-01

    New psychoactive substances (NPSs) have become increasingly popular in recent years. The analysis of these substances in influent wastewater (IWW) can be used to track their use in communities. In addition, an evaluation of the amount of NPSs released to the aquatic environment can be performed through the analysis of effluent wastewater (EWW). This study presents the development, validation and application of an analytical methodology, based on solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), for the determination of 10 NPSs in IWW and EWW. Synthetic cannabinoids, cathinones, piperazines and pyrrolidophenones are included among the target analytes. To the authors' knowledge, it is the first time that eight out of these substances (4'-methylpyrrolidinobutyrophenone (MPPP), a-pyrrolidinopentiophenone (a-PVP), 2-[(1S,3R)-3-hydroxycyclohexyl]-5-(2-methyl-2-octanyl) phenol (CP47,497), (1-naphthyl(1-pentyl-1H-indol-3-yl) methanone (JWH-018), (1-butyl-1H-indol-3-yl)(1-naphthyl) methanone (JWH-073), (4-ethyl-1-naphthyl)(1-pentyl-1H-indol-3-yl) methanone (JWH-210), (4-methyl-1-naphthyl) (1-pentyl-1H-indol-3-yl) methanone (JWH-122) and 2-(2-methoxyphenyl)-1-(1-pentyl-1H-indol-3-yl) ethanone (JWH-250)) are investigated in wastewater. The optimized conditions for the analysis of this set of compounds included a SPE clean-up step using a polymeric sorbent and the use of a pentafluorophenyl (PFP) chromatographic column. Despite the broad range of physicochemical properties of the analytes the method allowed acceptable absolute recoveries (40-109%) for all the studied compounds at different levels of concentration. Low method limits of detection (MLODs) were achieved, ranging between 0.3 and 10 ng/L except for BZP and CP47,497 (20 and 23 ng/L, respectively), allowing a reliable and accurate quantification of the analytes. The method was successfully applied to the analysis of IWW and EWW samples from five wastewater treatment plants

  15. 40 CFR Table 5 to Subpart Oooo of... - Default Organic HAP Mass Fraction for Petroleum Solvent Groups a

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 12 2010-07-01 2010-07-01 true Default Organic HAP Mass Fraction for Petroleum Solvent Groups a 5 Table 5 to Subpart OOOO of Part 63 Protection of Environment ENVIRONMENTAL..., and Dyeing of Fabrics and Other Textiles Pt. 63, Subpt. OOOO, Table 5 Table 5 to Subpart OOOO of Part...

  16. 2MASS J13243553+6358281 Is an Early T-type Planetary-mass Object in the AB Doradus Moving Group

    Science.gov (United States)

    Gagné, Jonathan; Allers, Katelyn N.; Theissen, Christopher A.; Faherty, Jacqueline K.; Bardalez Gagliuffi, Daniella; Artigau, Étienne

    2018-02-01

    We present new radial velocity and trigonometric distance measurements indicating that the unusually red and photometrically variable T2 dwarf 2MASS J13243553+6358281 is a member of the young (∼150 Myr) AB Doradus moving group (ABDMG) based on its space velocity. We estimate its model-dependent mass in the range 11–12 M Jup at the age of the ABDMG, and its trigonometric distance of 12.7 ± 1.5 pc makes it one of the nearest known isolated planetary-mass objects. The unusually red continuum of 2MASS J13243553+6358281 in the near-infrared was previously suspected to be caused by an unresolved L + T brown dwarf binary, although it was never observed with high spatial resolution imaging. This new evidence of youth suggests that a low surface gravity may be sufficient to explain this peculiar feature. Using the new parallax we find that its absolute J-band magnitude is ∼0.4 mag fainter than equivalent-type field brown dwarfs, suggesting that the binary hypothesis is unlikely. The fundamental properties of 2MASS J13243553+6358281 follow the spectral type sequence of other known high-likelihood members of the ABDMG. The effective temperature of 2MASS J13243553+6358281 provides the first precise constraint on the L/T transition at a known young age and indicates that it happens at a temperature of ∼1150 K at ∼150 Myr, compared to ∼1250 K for field brown dwarfs.

  17. Measuring the accreting stellar and intermediate mass black hole populations in the Galaxy and Local Group

    NARCIS (Netherlands)

    Grindlay, J.; Barret, D.; Belloni, T.; Corbel, S.; Kaaret, P.; Allen, B.; Bazzano, A.; Berger, E.; Bignami, G.; Caraveo, P.; De Luca, A.; Fabbiano, P.; Finger, M.; Feroci, M.; Hong, J.; Jernigan, G.; van der Klis, M.; Kouveliotou, C.; Kutyrev, A.; Loeb, A.; Paizis, A.; Pareschi, G.; Skinner, G.; Di Stefano, R.; Ubertini, P.; Wilson-Hodge, C.A.

    2010-01-01

    The population of stellar black holes (SBHs) in the Galaxy and galaxies generally is poorly known in both number and distribution. SBHs are the fossil record of the massive stars in galaxy evolution and may have produced some (if not all) of the intermediate mass (≳100M⊙) black holes (IMBHs) and, in

  18. Ultrahigh-performance liquid chromatography electrospray ionization Q-Orbitrap mass spectrometry for the analysis of 451 pesticide residues in fruits and vegetables: method development and validation.

    Science.gov (United States)

    Wang, Jian; Chow, Willis; Chang, James; Wong, Jon W

    2014-10-22

    This paper presents an application of ultrahigh-performance liquid chromatography electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap MS) for the determination of 451 pesticide residues in fruits and vegetables. Pesticides were extracted from samples using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. UHPLC/ESI Q-Orbitrap MS in full MS scan mode acquired full MS data for quantification, and UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) (i.e., data-dependent scan mode) obtained product ion spectra for identification. UHPLC/ESI Q-Orbitrap MS quantification was achieved using matrix-matched standard calibration curves along with the use of isotopically labeled standards or a chemical analogue as internal standards to achieve optimal method accuracy. The method performance characteristics include overall recovery, intermediate precision, and measurement uncertainty evaluated according to a nested experimental design. For the 10 matrices studied, 94.5% of the pesticides in fruits and 90.7% in vegetables had recoveries between 81 and 110%; 99.3% of the pesticides in fruits and 99.1% of the pesticides in vegetables had an intermediate precision of ≤20%; and 97.8% of the pesticides in fruits and 96.4% of the pesticides in vegetables showed measurement uncertainty of ≤50%. Overall, the UHPLC/ESI Q-Orbitrap MS demonstrated acceptable performance for the quantification of pesticide residues in fruits and vegetables. The UHPLC/ESI Q-Orbitrap Full MS/dd-MS(2) along with library matching showed great potential for identification and is being investigated further for routine practice.

  19. On-line solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry as a powerful technique for the determination of sulfonamide residues in soils.

    Science.gov (United States)

    Tetzner, Natália Fernanda; Maniero, Milena Guedes; Rodrigues-Silva, Caio; Rath, Susanne

    2016-06-24

    Sulfonamides are antimicrobials used widely as veterinary drugs, and their residues have been detected in environmental matrices. An analytical method for determining sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline residues in soils employing a solid phase extraction on-line technique coupled with ultra-high performance liquid chromatography and tandem mass spectrometry (SPE-UHPLC-MS/MS) was developed and validated in this study. SPE and chromatographic separation were performed using an Oasis HLB column and an Acquity UPLC BEH C18 analytical column, respectively, at 40°C. Samples were prepared by extracting sulfonamides from soil using a solid-liquid extraction method with water:acetonitrile, 1:1v/v (recovery of 70.2-99.9%). The following parameters were evaluated to optimize the on-line SPE process: sorbent type (Oasis and C8), sample volume (100-400μL), loading solvent (water and different proportions of water:methanol) and washing volume (0.19-0.66mL). The method produced linear results for all sulfonamides from 0.5 to 12.5ngg(-1) with a linearity greater than 0.99. The precision of the method was less than 15%, and the matrix effect was -27% to -87%. The accuracy was in the range of 77-112% for all sulfonamides. The limit of quantitation in the two soils (clay and sand) was 0.5ngg(-1). The SPE column allowed for the analysis of many (more than 2000) samples without decreasing the efficiency. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Performance Assessment and Comparability of a Commercial Enzyme-Linked Immunosorbent Assay Kit with Liquid Chromatography-Tandem Mass Spectrometry for Chloramphenicol Residues in Crab and Shrimp.

    Science.gov (United States)

    Jester, Edward L E; Loader, Jared I; El Said, Kathleen R; Abraham, Ann; Flores Quintana, Harold A; Plakas, Steven M

    2016-01-01

    Monitoring for chloramphenicol (CAP) in aquaculture products is primarily performed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), which requires expensive equipment and specialized training. Many laboratories prefer to screen samples with facile and high-throughput enzyme-linked immunosorbent assay (ELISA) kits for CAP residues before submitting samples for LC-MS/MS quantification and confirmation. We evaluated the performance of a Ridascreen (R-Biopharm) ELISA kit for CAP in spiked and incurred crab and shrimp muscle at levels bracketing the minimum required performance level for analysis (0.3 ng/g). The Ridascreen ELISA kit incorporates antibody directed against CAP. Incurred CAP levels in crab and shrimp muscle were verified using LC-MS/MS. We found good repeatability (relative standard deviation) of the ELISA in spiked and incurred crab and shrimp muscle samples, with values ranging from 6.8 to 21.7%. Recoveries of CAP from tissues spiked at 0.15 to 0.60 ng/g ranged from 102 to 107%. Minimal cross-reactivity with blank crab and shrimp muscle matrix components was observed. ELISA data were highly correlated with those of LC-MS/MS for CAP in incurred muscle tissue. We believe this study to be the first evaluation of the performance and comparability of a CAP ELISA kit and LC-MS/MS for determination of CAP residues, as well as their elimination, in crab muscle. Our findings support the use of this ELISA kit for screening purposes and, when used in conjunction with validated instrumental methods, for regulatory monitoring of CAP in these species.

  1. Simultaneous determination of lincomycin and spectinomycin residues in animal tissues by gas chromatography-nitrogen phosphorus detection and gas chromatography-mass spectrometry with accelerated solvent extraction.

    Science.gov (United States)

    Tao, Y; Chen, D; Yu, G; Yu, H; Pan, Y; Wang, Y; Huang, L; Yuan, Z

    2011-02-01

    A new multi-dimensional analytical method using gas chromatography-nitrogen phosphorus detection (GC-NPD) and gas chromatography-mass spectrometry (GC-MS) was developed for qualitative and quantitative measurement of lincomycin and spectinomycin residues in food animal tissues. This method is based on a new extraction procedure using accelerated solvent extraction (ASE). The analytes were extracted by phosphate buffer with trichloroacetic acid deproteinization and clean-up by C₁₈ solid-phase extraction (SPE) adding dodecanesulfonic acid sodium salt as an ion-pair reagent. The eluted fraction was evaporated and derivatised with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) for GC-NPD analysis and GC-MS confirmation. Parameters for extraction pressure, temperature and cycle of ASE, clean-up, derivatisation and analysis procedure were optimised. The method was validated in muscle, kidney and liver of swine, bovine with a low concentration (limit of quantification) of 16.4 and 21.4 µg kg⁻¹ for these two analytes using GC-NPD. For GC-MS, the limits of quantification were 4.1 and 5.6 µg kg⁻¹, respectively. Spiked recoveries from levels of 20 to 200 µg kg⁻¹ were found to be between 73% and 99% with a relative standard deviation (RSD) of less than 17% in GC-NPD. For GC-MS, levels from 5 to 20 µg kg⁻¹ had between 70% and 93% with an RSD of less than 21%. This rapid and reliable method can be used for the characterisation and quantification of residues of lincomycin and spectinomycin in animal tissues.

  2. The influence of a residual group in low-molecular-weight allergoids of Artemisia vulgaris pollen on their allergenicity, IgE- and IgG-binding properties.

    Science.gov (United States)

    Cirković, T; Gavrović-Jankulović, M; Prisić, S; Jankov, R M; Burazer, L; Vucković, O; Sporcić, Z; Paranos, S

    2002-11-01

    Reaction of epsilon-amino groups of lysine with potassium cyanate, maleic, or succinic anhydride leads to allergoids of low molecular weight. No study has been performed to compare their properties and investigate the influence of a residual group on allergenicity and human IgE- and IgG-binding of these derivatives. Allergoids of a pollen extract of Artemisia vulgaris were obtained by means of potassium cyanate, and succinic and maleic anhydride. Biochemical properties were investigated by determination of amino groups, enzyme activity, isoelectric focusing IEF and SDS-PAGE. IgE- and IgG-binding was determined using immunoblots and ELISA inhibition. Allergenicity was investigated by skin prick tests (SPT) on a group of 52 patients, of which 6 were control subjects, 30 were patients with no previous immunotherapy (IT), and 16 were patients undergoing immunotherapy. The same degree of amino-group modification (more than 85%), residual enzyme activity (less then 15%), IEF, and SDS-PAGE pattern were noted. In the immunoblots of IgE-binding, there was more pronounced reduction in the succinyl and maleyl derivatives than in the carbamyl one. IgG-binding was less affected by carbamylation than by acid anhydride modification. The SPT showed that the succinylated derivative had the most reduced allergenicity (98% showed a reduced wheal diameter when tested with the succinyl derivative, 87% with the maleyl allergoid, and 83% with the carbamyl allergoid). The most significant difference among allergoids could be seen in the group of patients with high skin reactivity (83% of patients showed no reaction to the succinyl derivative when compared to the value of 28% for the carbamyl derivative or 22% for the maleyl derivative). According to our results, all three modification procedures yielded allergoids with a similar extent of modification. No single biochemical parameter investigated in the study could predict the degree of reduced allergenicity in vivo. The most reduced

  3. Comparison of magnetic resonance imaging and {sup 67}gallium scintigraphy in the evaluation of posttherapeutic residual mediastinal mass in the patients with Hodgkin's lymphoma

    Energy Technology Data Exchange (ETDEWEB)

    Herman, Miroslav E-mail: herman@fnol.cz; Paucek, Boris; Raida, Ludek; Myslivecek, Miroslav; Zapletalova, Jana

    2007-12-15

    Introduction: Detection of residual disease following the completion of primary treatment in Hodgkin's lymphoma (HL) patients diagnosed with mediastinal tumor mass has an exceptional importance in the assessment of therapeutic response. Magnetic resonance imaging (MRI) and {sup 67}gallium ({sup 67}Ga) scintigraphy can be used to identify active tumor tissue in the mediastinal residuum. Aims: To evaluate: the accuracy of MRI and {sup 67}Ga scintigraphy in the prediction of clinical HL relapse/progression; congruence of findings and the probability of mediastinal disease relapse/progression regarding to the detection of active/inactive tissue by both imaging methods. Materials and methods: Thirty HL patients with abnormal mediastinal tissue following the completion of primary treatment were examined by MRI and {sup 67}Ga scintigraphy. Positive findings were: high signal intensity on unenhanced T2-weighted images on MRI and the abnormal accumulation of gallium on scintigraphy or SPECT. These findings were compared with the clinical follow-up. Results: Sensitivity, specificity, accuracy, positive and negative predictive values were: 75.0%, 96.2%, 93.3%, 75.0%, 96.2% in MRI and 50.0%, 88.5%, 83.3%, 40.0%, 92.0% in {sup 67}Ga scintigraphy. Discrepant results concerning the mediastinal tissue activity were found in 3 of 30 patients (10%). No statistically significant differences were found between both imaging methods in sensitivity, specificity and accuracy. Estimated 2-years progression free survival (PFS) for patients without and with active residual mediastinal tissue by MRI was 96% and 25% (p = 0.0001), respectively. The probability of 2-years PFS in the cases with negative and positive findings on {sup 67}Ga scintigraphy was 92% and 60% (p = 0.026), respectively. Conclusion: Although MRI showed better results than {sup 67}Ga scintigraphy in the assessment of residual mediastinal tissue activity in HL patients after primary treatment, the difference between

  4. On new scaling group of transformation for Prandtl-Eyring fluid model with both heat and mass transfer

    Directory of Open Access Journals (Sweden)

    Khalil Ur Rehman

    2018-03-01

    Full Text Available A short communication is structured to offer a set of scaling group of transformation for Prandtl-Eyring fluid flow yields by stretching flat porous surface. The fluid flow regime is carried with both heat and mass transfer characteristics. To seek solution of flow problem a set of scaling group of transformation is proposed by adopting Lie approach. These transformations are used to step down the partial differential equations into ordinary differential equations. The reduced system is solved by numerical method termed as shooting method. A self-coded algorithm is executed in this regard. The obtain results are elaborated by means of figures and tables. Keywords: Heat and mass transfer, Scaling group of transformations, Prandtl-Eyring fluid

  5. Multi-residue analysis of drugs of abuse in wastewater and surface water by solid-phase extraction and liquid chromatography-positive electrospray ionisation tandem mass spectrometry.

    Science.gov (United States)

    Baker, David R; Kasprzyk-Hordern, Barbara

    2011-03-25

    A new-multi residue method was developed for the environmental monitoring of 65 stimulants, opiod and morphine derivatives, benzodiazepines, antidepressants, dissociative anaesthetics, drug precursors, human urine indicators and their metabolites in wastewater and surface water. The proposed analytical methodology offers rapid analysis for a large number of compounds, with low limits of quantification and utilises only one solid-phase extraction-ultra performance liquid chromatography-positive electrospray ionisation tandem mass spectrometry (SPE-LC-MS/MS) method, thus overcoming the drawbacks of previously published procedures. The method employed solid phase extraction with the usage of Oasis MCX sorbent and subsequent ultra performance liquid chromatography-positive electrospray ionisation tandem mass spectrometry. The usage of a 1.7 μm particle size column (1 mm×150 mm) resulted in very low flow rates (0.04 mLmin(-1)), and as a consequence gave good sensitivity, low mobile phase consumption and short retention times for all compounds (from 2.9 to 23.1 min). High SPE recoveries (>60%) were obtained for the majority of compounds. The mean correlation coefficients of the calibration curves were typically higher than 0.997 and showed good linearity in the range 0-1000 μgL(-1). The method limits of detection ranged from 0.1 ngL(-1) for compounds including cocaine, benzoylecgonine, norbenzoylecgonine and 2-oxo-3-hydroxy-LSD to 100 ngL(-1) for caffeine. Method quantification limits ranged from 0.5 to 154.2 ngL(-1). Intra- and inter-day repeatabilities were on average less than 10%. The method accuracy range was within -33.1 to 30.1%. The new multi-residue method was used to analyse drugs of abuse in wastewater and river water in the UK environment. Of the targeted 65 compounds, 46 analytes were detected at levels above the method quantification limit (MQL) in wastewater treatment plant (WWTP) influent, 43 in WWTP effluent and 36 compounds in river water. Copyright

  6. A Three-Year Follow-Up Study of Antibiotic and Metal Residues, Antibiotic Resistance and Resistance Genes, Focusing on Kshipra-A River Associated with Holy Religious Mass-Bathing in India: Protocol Paper.

    Science.gov (United States)

    Diwan, Vishal; Purohit, Manju; Chandran, Salesh; Parashar, Vivek; Shah, Harshada; Mahadik, Vijay K; Stålsby Lundborg, Cecilia; Tamhankar, Ashok J

    2017-05-29

    Antibiotic resistance (ABR) is one of the major health emergencies for global society. Little is known about the ABR of environmental bacteria and therefore it is important to understand ABR reservoirs in the environment and their potential impact on health. Quantitative and qualitative data will be collected during a 3-year follow-up study of a river associated with religious mass-bathing in Central India. Surface-water and sediment samples will be collected from seven locations at regular intervals for 3 years during religious mass-bathing and in absence of it to monitor water-quality, antibiotic residues, resistant bacteria, antibiotic resistance genes and metals. Approval has been obtained from the Ethics Committee of R.D. Gardi Medical College, Ujjain, India (No. 2013/07/17-311). The results will address the issue of antibiotic residues and antibiotic resistance with a focus on a river environment in India within a typical socio-behavioural context of religious mass-bathing. It will enhance our understanding about the relationship between antibiotic residue levels, water-quality, heavy metals and antibiotic resistance patterns in Escherichia coli isolated from river-water and sediment, and seasonal differences that are associated with religious mass-bathing. We will also document, identify and clarify the genetic differences/similarities relating to phenotypic antibiotic resistance in bacteria in rivers during religious mass-bathing or during periods when there is no mass-bathing.

  7. A Three-Year Follow-Up Study of Antibiotic and Metal Residues, Antibiotic Resistance and Resistance Genes, Focusing on Kshipra—A River Associated with Holy Religious Mass-Bathing in India: Protocol Paper

    Science.gov (United States)

    Diwan, Vishal; Purohit, Manju; Chandran, Salesh; Parashar, Vivek; Shah, Harshada; Mahadik, Vijay K.; Stålsby Lundborg, Cecilia; Tamhankar, Ashok J.

    2017-01-01

    Background: Antibiotic resistance (ABR) is one of the major health emergencies for global society. Little is known about the ABR of environmental bacteria and therefore it is important to understand ABR reservoirs in the environment and their potential impact on health. Method/Design: Quantitative and qualitative data will be collected during a 3-year follow-up study of a river associated with religious mass-bathing in Central India. Surface-water and sediment samples will be collected from seven locations at regular intervals for 3 years during religious mass-bathing and in absence of it to monitor water-quality, antibiotic residues, resistant bacteria, antibiotic resistance genes and metals. Approval has been obtained from the Ethics Committee of R.D. Gardi Medical College, Ujjain, India (No. 2013/07/17-311). Results: The results will address the issue of antibiotic residues and antibiotic resistance with a focus on a river environment in India within a typical socio-behavioural context of religious mass-bathing. It will enhance our understanding about the relationship between antibiotic residue levels, water-quality, heavy metals and antibiotic resistance patterns in Escherichia coli isolated from river-water and sediment, and seasonal differences that are associated with religious mass-bathing. We will also document, identify and clarify the genetic differences/similarities relating to phenotypic antibiotic resistance in bacteria in rivers during religious mass-bathing or during periods when there is no mass-bathing. PMID:28555050

  8. A Three-Year Follow-Up Study of Antibiotic and Metal Residues, Antibiotic Resistance and Resistance Genes, Focusing on Kshipra—A River Associated with Holy Religious Mass-Bathing in India: Protocol Paper

    Directory of Open Access Journals (Sweden)

    Vishal Diwan

    2017-05-01

    Full Text Available Background: Antibiotic resistance (ABR is one of the major health emergencies for global society. Little is known about the ABR of environmental bacteria and therefore it is important to understand ABR reservoirs in the environment and their potential impact on health. Method/Design: Quantitative and qualitative data will be collected during a 3-year follow-up study of a river associated with religious mass-bathing in Central India. Surface-water and sediment samples will be collected from seven locations at regular intervals for 3 years during religious mass-bathing and in absence of it to monitor water-quality, antibiotic residues, resistant bacteria, antibiotic resistance genes and metals. Approval has been obtained from the Ethics Committee of R.D. Gardi Medical College, Ujjain, India (No. 2013/07/17-311. Results: The results will address the issue of antibiotic residues and antibiotic resistance with a focus on a river environment in India within a typical socio-behavioural context of religious mass-bathing. It will enhance our understanding about the relationship between antibiotic residue levels, water-quality, heavy metals and antibiotic resistance patterns in Escherichia coli isolated from river-water and sediment, and seasonal differences that are associated with religious mass-bathing. We will also document, identify and clarify the genetic differences/similarities relating to phenotypic antibiotic resistance in bacteria in rivers during religious mass-bathing or during periods when there is no mass-bathing.

  9. Evaluation of clayey masses compositions starting from the residue incorporation of the red ceramic industry to obtain tubular ceramic membranes; Avaliacao das composicoes de massas argilosas a partir da incorporacao de residuo da industria de ceramica vermelha na obtencao de membranas ceramicas tubulares

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Adriano Lima da; Chaves, Alexsandra Cristina; Luna, Carlos Bruno Barreto; Neves, Gelmires de Araujo; Lira, Helio de Lucena, E-mail: adrianolimadasilva@hotmail.com, E-mail: alexsandra.chaves@ifap.edu.br, E-mail: brunobarretodemaufcg@hotmail.com, E-mail: gelmires@ufcg.edu.br, E-mail: helio@ufcg.edu.br [Universidade Federal de Campina Grande (UAEMa/CCT/UFCG), PB (Brazil). Unidade Academica de Engenharia de Materiais

    2017-01-15

    The inappropriate residue disposal of red ceramic industry is very high. Nowadays, one of the major challenges is the investigation of processes to obtain alternative materials, enabling the use of these residues to manufacture new materials. This work's objective is to study clayey masses' compositions starting from the residue incorporation of the red ceramic industry to be used in tubular ceramic membranes. Two compositions of ceramic masses were established, composition A (50% of residue) and composition B (70% of residue). Granulometric analysis of the ceramic masses presented an average size of particles, what indicates membranes in the microfiltration scale. Another observed factor is related to the increase of residue amount, what favored a decrease in the ceramic mass' plasticity. A rise in the apparent porosity was also observed, probably because of a possible growing in the bigger pores numbers, due to the sintering high temperature and the elevation of residue quantity itself. (author)

  10. Determination of low-level agricultural residues in soft drinks and sports drinks by gas chromatography with mass-selective detection: single-laboratory validation.

    Science.gov (United States)

    Paske, Nathan; Berry, Bryan; Schmitz, John; Sullivan, Darryl

    2007-01-01

    In this study, sponsored by PepsiCo Inc., a method was validated for measurement of 19 pesticide residues in soft drinks and sports drinks by gas chromatography/mass spectrometry (GC/MS) with mass selective detection The pesticide residues determined in this validation were alpha-benzenehexachloride (BHC); beta-BHC; gamma-BHC; delta-BHC; methyl parathion; malathion; chlorpyrifos; aldrin; 2,4-dichlorodiphenyldichloroethylene (DDE); alpha-endosulfan; 4,4-DDE; 2,4-dichlorodiphenyldichloroethane (DDD); dieldrin; ethion; 4,4-DDD; 2,4-dichlorodiphenyltrichloroethylene (DDT); beta-endosulfan; 4,4-DDT; and endosulfan sulfate when spiked into a 200 mL matrix sample at 0.50 microg/L. The samples were diluted with acetonitrile and water, then liquid-liquid phase extracted into petroleum ether. The resulting extract was concentrated to near dryness and diluted with hexane:dichloromethane (50:50). The concentrated samples were purified by gel permeation chromatography. The resulting solution was concentrated and separated on a Florisil substrate. The eluent was concentrated to near dryness, reconstituted to produce a 200-fold concentration, and analyzed using a GC/MS instrument operated in the selective ion monitoring mode. The GC/MS instrument was equipped with a large volume injector capable of injecting 25 microL. External standards prepared in dichloromethane were used for quantification without the need for matrix-matched calibration because the extraction step minimized the matrix effects. The calibration curves for all agricultural residues had coefficients of determination (r2) of greater than or equal to 0.9900, with the exception of one value that was 0.988. Fortification spikes at 0.50 microg/L in 3 matrixes (7UP, Gatorade, and Diet Pepsi) over the course of 2 days (4 days for Gatorade), where n=8 each day, yielded average percent recoveries (and percent relative standard deviations) as follows (n=64): 95.6 (24.8) for alpha-BHC; 91.9 (23.6) for beta-BHC; 89.1 (21

  11. Mass sensitivity of acoustic wave devices from group and phase velocity measurements

    OpenAIRE

    McHale, G; Martin, F; Newton, MI

    2002-01-01

    The effect of dispersion on acoustic wave sensors is considered. The discussion is focused upon layer guided surface acoustic waves ~Love waves!, which obtain their high mass sensitivity for the first Love wave mode by optimizing the guiding layer thickness, d, such that d;ll/4; the wavelength in the layer is given by ll5f /vl where f is the operating frequency and vl is the shear acoustic speed of the guiding layer. We show that this optimization of guiding layer thickness corresponds to str...

  12. Detection of residual oil-sand-derived organic material in developing soils of reclamation sites by ultra-high-resolution mass spectrometry.

    Science.gov (United States)

    Noah, Mareike; Poetz, Stefanie; Vieth-Hillebrand, Andrea; Wilkes, Heinz

    2015-06-02

    The reconstruction of disturbed landscapes back to working ecosystems is an issue of increasing importance for the oil sand areas in Alberta, Canada. In this context, the fate of oil-sand-derived organic material in the tailings sands used for reclamation is of utmost environmental importance. Here we use electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry of maltene fractions to identify compositional variations over a complete oil sand mining and recultivation process chain. On the basis of bulk compound class distributions and percentages of unique elemental compositions, we identify specific compositional features that are related to the different steps of the process chain. The double bond equivalent and carbon number distributions of the N1 and S1O2 classes are almost invariant along the process chain, despite a significant decrease in overall abundance. We thus suggest that these oil-sand-derived components can be used as sensitive tracers of residual bitumen, even in soils from relatively old reclamation sites. The patterns of the O2, O3, and O4 classes may be applied to assess process-chain-related changes in organic matter composition, including the formation of plant-derived soil organic matter on the reclamation sites. The N1O2 species appear to be related to unidentified processes in the tailings ponds but do not represent products of aerobic biodegradation of pyrrolic nitrogen compounds.

  13. Simultaneous determination of residues of thiamethoxam and its metabolite clothianidin in tobacco leaf and soil using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Meng, Banghua; Yu, Yurong; Zhang, Qingtao; Wang, Shouyi; Hu, Deyu; Zhang, Kankan

    2018-03-02

    A simple analytical method was developed to simultaneously determine thiamethoxam and its metabolite, clothianidin, in fresh tobacco leaf, soil and cured tobacco leaf using liquid chromatography with tandem mass spectrometry. Thiamethoxam and clothianidin in tobacco and soil samples were extracted with acetonitrile containing 0.1% formic acid and purified using an NH 2 -SPE column. The optimized method provided good linearity with coefficients of determination R 2  ≥ 0.9981. The limits of detection and quantification were between 0.006-0.12 and 0.02-0.4 mg/kg, respectively. Intra- and inter-day recovery assays were used to validate the established method. The average recoveries of thiamethoxam and clothianidin in fresh tobacco leaf, soil and cured tobacco leaf were 75.04-100.47%, 75.86-86.40% and 89.83-99.39%, respectively. The intra- and inter-day relative standard deviations were all clothianidin residues in actual tobacco and soil samples. The results indicated that the established method met the requirements for the analysis of trace amounts of thiamethoxam and clothianidin in fresh tobacco leaf, soil and cured tobacco leaf. Copyright © 2018 John Wiley & Sons, Ltd.

  14. Simultaneous determination of thiamethoxam, clothianidin, and metazachlor residues in soil by ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Valverde, Silvia; Ares, Ana M; Bernal, José Luis; Nozal, María Jesús; Bernal, José

    2017-03-01

    A rapid pioneering method has been developed to simultaneously determine residues of three pesticides (thiamethoxam, clothianidin, and metazachlor) in soil by ultrahigh performance liquid chromatography coupled to a mass spectrometry detector (quadrupole time-of-flight). An efficient extraction procedure (90-105% average analyte recoveries) has also been proposed, involving solid-liquid extraction by a mixture of water and methanol (60:40, v/v), centrifugation, and concentration. A chromatographic analysis of the compounds was achieved in 5.5 min by means of a core-shell technology based column (Kinetex ® EVO C 18 , 50 × 2.1 mm, 1.7 μm, 100 Å). The mobile phase (0.3 mL/min, gradient elution mode) consisted of 0.1% v/v formic acid in water and 0.1% v/v formic acid in acetonitrile. The method was fully validated in terms of selectivity, detection and quantification limits, matrix effect, linearity, trueness, and precision. Low limits of detection and quantification were obtained, ranging from 0.2 to 3.0 μg/kg, which are similar to those published in previous studies, while the absence of a significant matrix effect allowed quantification of the pesticides with standard calibration curves. The proposed method was applied for an analysis of pesticides in several soil samples from experimental fields dedicated to oilseed rape cultivars. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. [Simultaneous determination of ethephon, thidiazuron, diuroN residues in cotton by using high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Xie, Wen; Shi, Yingzhu; Hou, Jianbo; Huang, Chaoqun; Zhao, Dong; Pan, Lulu; Dong, Suozhuai

    2014-02-01

    A method for the determination of ethephon, thidiazuron and diuron in cotton samples has been developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with methanol-water. The separation was carried out on a C8 column (150 mm x 4.6 mm, 5 microm) with methanol-water (6:4, v/v) as mobile phase at a flow rate of 0.4 mL/min, and the injection volume was 20 microL. Then the sample solution was analyzed by HPLC-MS/MS in negative ion mode with multiple reaction monitoring (MRM). There were one precursor/two product ion transitions for each pesticide. The results showed that the working curves were linear in the range of 0-10 microg/L for ethephon and thidiazuron, and 0-1 microg/L for diuron. The correlation coefficients (r) were all over 0. 999. The limits of quantitation (LOQ) of ethephon, diuron were 40 microg/kg, that of thidiazuron was 4 microg/kg. The average recoveries varied from 89.4% to 100.2% with the relative standard deviations (RSDs) of 5.7%-11.5% at three spiked levels (LOQ, 2LOQ and 4LOQ). The method is simple, rapid and accurate, and can meet the requirements of the domestic and international legislation. The method adapts to confirm the residues of ethephon, thidiazuron and diuron pesticides in cotton samples.

  16. Determination of fenobucarb residues in animal and aquatic food products using liquid chromatography-tandem mass spectrometry coupled with a QuEChERS extraction method.

    Science.gov (United States)

    Zheng, Weijia; Park, Jin-A; Zhang, Dan; Abd El-Aty, A M; Kim, Seong-Kwan; Cho, Sang-Hyun; Choi, Jeong-Min; Shim, Jae-Han; Chang, Byung-Joon; Kim, Jin-Suk; Shin, Ho-Chul

    2017-07-15

    A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI + /MS-MS) was developed for quantification of fenobucarb residues in animal food products, such as porcine muscle, egg, and whole milk, and aquatic food products, such as eel, flatfish, and shrimp. Acetonitrile with the addition of 0.1% trifluoroacetic acid was employed as an extraction solvent and was compared with acetonitrile alone and 0.1% formic acid in acetonitrile. All extracted samples were purified using C18 sorbent. The best extraction efficiencies, expressed as recovery at two spiking levels equivalent to 1- and 2-times the limit of quantification (LOQ=2μg/kg) were achieved using 0.1% trifluoroacetic acid in acetonitrile and ranged from 61.38 to 102.21% in all matrices, with relative standard deviations (RSDs) 20%). Six-point matrix-matched calibration was used for quantification and the determination coefficients were good (R 2 ≥0.9865). The method was verified by application to samples purchased from local markets and none of the samples tested positive. In conclusion, the developed method is simple and versatile and can be used for the routine detection of fenobucarb in different animal food products having varying protein and fat contents with satisfactory accuracy and precision. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Competitive formation of b(2) and c(2)-H2O ions from b(3) ions containing Asp residue during tandem mass spectrometry: the influence of neighboring Arg.

    Science.gov (United States)

    Guo, Mengzhe; Guo, Cheng; Pan, Yuanjiang

    2014-08-01

    The fragmentation of b3 ions derived from protonated Arg-Xxx-Asp-Ala-Ala (Xxx = Ala, Asp, Glu, Cys) and Arg-Xxx-Glu-Ala-Ala was investigated by electrospray ionization tandem mass spectrometry (MS (n) ) with collision-induced dissociation. A particular ion, which is 1 Da less than b2 ion, is shown to be the c2-H2O ion. The mechanism for its formation involved the aspartic acid in the third position easily losing anhydride to form a c2 ion, which then lost water to form an eight-membered ring of azacyclooctane derivative under the participation of the guanidine of the N-terminal arginine. However, this phenomenon was not observed when the aspartic acid was replaced by glutamic acid. The Amber program was used to determine the conformation of the original c2 residue from the dynamic energy perspective, and then density functional theory-based calculations and changing N-terminal amino acid from arginine to phenylalanine supported this mechanism.

  18. Optimization of a multi-residue method for 101 pesticides in green tea leaves using gas chromatography–tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Xue Hou

    Full Text Available ABSTRACT A method for analysis of 101 pesticide residues in tea leaves was developed and validated for the first time. Pure acetonitrile was used as extraction solvent rather than acetonitrile after matrix hydration based on the amount of co-extracts and recoveries performance. During clean-up procedure, primary-secondary amine/graphitized carbon black (500 mg was selected, which exhibited outstanding properties in clean-up capabilities and recoveries of pesticides comparing to primary-secondary amine/graphitized carbon black (250 mg, NH2-Carbon and TPT absorbents. The method was validated employing gas chromatography coupled to tandem mass spectrometry at the spiked concentration levels of 0.050 and 0.100 mg kg−1. For most of the targeted pesticides, the percent recoveries range from 70 to 120%, with relative standard deviations <20%. The linear correlation coefficients (r 2 were higher than 0.99 at concentration levels of 0.025–0.250 mg kg−1. Limits of quantification ranged from 1.1 to 25.3 µg kg−1 for all pesticides. The developed method was successfully applied to the determination of pesticides in tea leaf samples.

  19. Validation of a liquid chromatography-mass spectrometry multi-residue method for the simultaneous determination of sulfonamides, tetracyclines, and pyrimethamine in milk.

    Science.gov (United States)

    Koesukwiwat, Urairat; Jayanta, Siripastr; Leepipatpiboon, Natchanun

    2007-01-26

    A multiresidue method suitable for confirmation and determination of six sulfonamides (SAs), three tetracyclines (TCs), and pyrimethamine (PYR) in cow milk was validated. Milk samples were extracted using copolymer Oasis HLB solid-phase extraction (SPE) and analyzed by liquid chromatography-electrospray mass spectrometry with positive ion mode. Estimated method detection limits (MDL) and method quantitation limits (MQL) ranged from 0.48 to 2.64 and 0.61 to 8.64ng/mL, respectively. These values are far lower than the maximum residue limits (MRLs) established by several control authorities. Excellent linear dynamic range was observed from the method quantitation limits to 300ng/mL with correlation coefficients better than 0.9900 for all compounds. The method was accurate with recoveries ranging from 72.01 to 97.39%. Good intra-precision and intermediate precision were obtained with RSD better than 11.08%. The method is fairly robust with sample pH being the only critical control point.

  20. A multi-residue method for determination of 70 organic micropollutants in surface waters by solid-phase extraction followed by gas chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Terzopoulou, Evangelia; Voutsa, Dimitra; Kaklamanos, George

    2015-01-01

    A multi-residue method, based on gas chromatography coupled to tandem mass spectrometry (GC-MS/MS), has been developed for the determination of 70 organic micropollutants from various chemical classes (organochlorinated, organophosphorous, triazines, carbamate and urea, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, pharmaceuticals, phenols, etc.) in surface waters. A single-step SPE extraction using OASIS HLB cartridges was employed for the recovery of target micropollutants. The method has been validated according to monitoring performance criteria of the Water Framework Directive, taking into account the approved guidelines on quality assurance and quality control. The recoveries ranged from 60 to 110 %, the coefficient of variation from 0.84 to 27.4 %, and the uncertainty from 6 to 37 %. The LOD varied from 6.0 to 40 ng/L. The limits of quantification for the priority pollutants anthracene, alachlor, atrazine, benzo(a)pyrene, chlorfenvinphos, diuron, isoproturon, nonylphenol, simazine, and terbutryn fulfill the criterion of diuron, isoproturon, salicylic acid, chlorfenvinphos, 1,2-benzanthracene, pyrene, diflubenzuron, and carbaryl exhibited the highest detection frequencies.

  1. Neutron to proton mass difference, parton distribution functions and baryon resonances from dynamics on the Lie group u(3)

    DEFF Research Database (Denmark)

    Trinhammer, Ole

    flavour singlet resonances are predicted and may show up around 4500 MeV in neutron diffraction dissociation experiments above the threshold in the free charm system SigmaCplus(2455)Dminus. They should also be visible in photoproduction of pPiMinus on neutrons and lower lying singlets may show up in p......PiMinus invariant mass in B decays. We give a controversial prediction of the relative neutron to proton mass difference 0.138 % as originating in period doublings of certain parametric states. The group space dynamics communicates with real space via the exterior derivative which projects out quark and gluon...... fields from the allospatial state. The allostate in turn is excited from space by the momentum operators which act as toroidal generators on the group manifold. Such generators can be used to trace out parton distribution functions and examples are shown to mimic the valence quark content of the proton....

  2. Relationship between body mass index, bone mineral density, and oral hygiene with periodontal disease in a Mexican elderly group.

    OpenAIRE

    José Francisco Murrieta; Ricardo Gustavo García; Brenda Contreras; Remedios Guadalupe Valdez; María Lilia Juárez

    2016-01-01

    The aim of this study was to evaluate the relationship of body mass index (BMI), bone mineral density (BMD), and oral hygiene with periodontal disease (PD) in a group of elderly adults in Mexico City. Material and Methods: A cross-sectional study with a convenience sample of 151 elderly adults was conducted. Before applying the epidemiological survey, each subject was asked to sign an informed consent. Standardization for measuring Ramfjord’s Periodontal Disease Index (PDI), BMI, and Green an...

  3. On new scaling group of transformation for Prandtl-Eyring fluid model with both heat and mass transfer

    Science.gov (United States)

    Rehman, Khalil Ur; Malik, Aneeqa Ashfaq; Malik, M. Y.; Tahir, M.; Zehra, Iffat

    2018-03-01

    A short communication is structured to offer a set of scaling group of transformation for Prandtl-Eyring fluid flow yields by stretching flat porous surface. The fluid flow regime is carried with both heat and mass transfer characteristics. To seek solution of flow problem a set of scaling group of transformation is proposed by adopting Lie approach. These transformations are used to step down the partial differential equations into ordinary differential equations. The reduced system is solved by numerical method termed as shooting method. A self-coded algorithm is executed in this regard. The obtain results are elaborated by means of figures and tables.

  4. Quantitative analysis of tylosin in eggs by high performance liquid chromatography with electrospray ionization tandem mass spectrometry: residue depletion kinetics after administration via feed and drinking water in laying hens.

    Science.gov (United States)

    Hamscher, Gerd; Limsuwan, Sasithorn; Tansakul, Natthasit; Kietzmann, Manfred

    2006-11-29

    Maximum residue limits (MRLs) have been established by the European Union when tylosin is used therapeutically. They are fixed at 200 microg/kg for eggs. A highly sensitive and selective quantitative liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI/MS/MS) method suitable for monitoring tylosin residues in eggs to determine its depletion kinetics was developed and validated. For sample pretreatment all samples were liquid-liquid extracted with citrate buffer (pH 5.0) and acetonitrile. Liquid chromatographic separation was carried out on a reversed phase C18 column employing a 0.5% formic acid/acetonitrile gradient system. The tylosin recovery in eggs at a concentration range from 1.0-400 microg/kg was >82% with relative standard deviations between 1.5 and 11.0%. In two experimental studies administrating tylosin via feed (final dosage: 1.5 g/kg) or drinking water (final dosage: 0.5 g/L), no residues above the MRL were found during and after treatment. Moreover, all samples were well below the actual MRL of 200 microg/kg. Therefore, our residue data suggest that a withholding period for eggs is not required when laying hens are treated with tylosin in recommended dosages via feed or drinking water. Tylosin; residue; depletion; laying hen; withholding period; mass spectrometry.

  5. Using Velocity Dispersion to Estimate Halo Mass: Is the Local Group in Tension with ΛCDM?

    Science.gov (United States)

    Elahi, Pascal J.; Power, Chris; Lagos, Claudia del P.; Poulton, Rhys; Robotham, Aaron S. G.

    2018-03-01

    Satellite galaxies are commonly used as tracers to measure the line-of-sight velocity dispersion (σLOS) of the dark matter halo associated with their central galaxy, and thereby to estimate the halo's mass. Recent observational dispersion estimates of the Local Group, including the Milky Way and M31, suggest σ ˜50 km/s, which is surprisingly low when compared to the theoretical expectation of σ ˜100s km/s for systems of their mass. Does this pose a problem for ΛCDM? We explore this tension using the SURFS suite of N-body simulations, containing over 10000 (sub)haloes with well tracked orbits. We test how well a central galaxy's host halo velocity dispersion can be recovered by sampling σLOS of subhaloes and surrounding haloes. Our results demonstrate that σLOS is biased mass proxy. We define an optimal window in vLOS and projected distance (Dp) - 0.5 ≲ Dp/Rvir ≲ 1.0 and vLOS ≲ 0.5Vesc, where Rvir is the virial radius and Vesc is the escape velocity - such that the scatter in LOS to halo dispersion is minimised - σLOS = (0.5 ± 0.1)σv, H. We argue that this window should be used to measure line-of-sight dispersions as a proxy for mass, as it minimises scatter in the σLOS - Mvir relation. This bias also naturally explains the results from McConnachie (2012), who used similar cuts when estimating σLOS, LG, producing a bias of σLG = (0.44 ± 0.14)σv, H. We conclude that the Local Group's velocity dispersion does not pose a problem for ΛCDM and has a mass of log M_{LG, vir}/M_⊙ =12.0^{+0.8}_{-2.0}.

  6. The chemical evolution of Kurnub Group paleowater in the Sinai-Negev province-a mass balance approach

    International Nuclear Information System (INIS)

    Rosenthal, E.; Jones, B.F.; Weinberger, G.

    1998-01-01

    The chemical evolution of the Kurnub Group paleowater was studied starting from rainwater in recharge areas of the Sinai and along groundwater flowpaths leading to the natural outlets of this regional aquifer. This was achieved by investigating the chemical composition of groundwater, ionic ratios, degrees of saturation with common mineral species, normative analysis of dissolved salts and by modeling of rock/water interaction and mixing processes occurring along groundwater flow paths. The initial groundwater composition used is from the Nakhel well in Sinai. It evolves from desert rainwater percolating through typical Kurnub Group lithology in Sinai. This rainwater dissolves mainly gypsum, halite and dolomite together with smaller amounts of marine aerosol and K-feldspar. At the same time it precipitates calcite, SiO 2 , smectite and degasses CO 2 . Between the area of Nakhel and the northern Negev the chemistry of Kurnub Group waters is influenced by dissolution of halite and lesser amounts of gypsum of surficial origin in recharge areas, small amounts of feldspars and of dolomite cement in sandstones eroded from the Arabo-Nubian igneous massif of Sinai and organic degradation-derived CO 2 . Concomitantly, there is precipitation of calcite, smectite, SiO 2 and probably analcime characteristic of sediments in continental closed basins. North of the Negev, the Kurnub Group fluids are diluted and altered by mixing with Judea Group aquifer groundwaters. On the E there is mixing with residual brines from the water body ancestral to the Dead Sea, prior to discharge into the Arava valley. Rock/water interaction indicated by NETPATH and PHREEQC modeling is in agreement with lithology and facies changes previously observed in the Kurnub Group sequence. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  7. [Risk groups in travel to tropical countries within the frame of mass tourism].

    Science.gov (United States)

    van der Linde, F; Steffen, R; Schwarzenbach, F H

    1977-01-01

    More than 10,000 tourists returning from tropical countries have been asked about health problems during their stay abroad. Preliminary results from the first 5,550 questionnaires indicate that 74,8% had complaints of any kind concerning their health and 13,6% can be considered as having been ill. The frequency of complaints and illness in relation to different variables is shown and the possibility of definition of high risk groups is being discussed.

  8. Categorizing Weapons of Mass Destruction Biological Agents into Postmortem Risk Groups

    Science.gov (United States)

    2012-12-20

    hypothesis, the authors made numerous underlying assumptions including staff immunization status, that embalming would not take place, compliance with...procedures, such as prosectors. • Embalmers are not included among the three groups of Mortuary Affairs (MA) personnel, as embalming is not a...and embalmers have experienced occupational exposure since 1988, (144) discriminating WMD bio agents against non-WMD bio agents may mitigate end

  9. Multi-dye residue analysis of triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish tissues by ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Reyns, Tim; Belpaire, Claude; Geeraerts, Caroline; Van Loco, Joris

    2014-03-15

    Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography-tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MS(n) operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin(-1). The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25-2ngg(-1)). Limit of quantification was 0.25ngg(-1) for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all dyes, the two rhodamine dyes could only be determined above 0.75ngg(-1). For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. [Determination of 21 plant growth regulator residues in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Huang, Hehe; Zhang, Jin; Xu, Dunming; Zhou, Yu; Luo, Jia; Li, Meiling; Chen, Shubin; Wang, Lianzhu

    2014-07-01

    A method for the simultaneous detection of 21 plant growth regulators in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The samples were initially extracted with acetonitrile containing 1% (v/v) acetic acid, followed by clean-up using the powder of magnesium sulfate and C18. The resulting samples were separated on a C18 column, and detected under positive and negative multiple reactions monitoring (MRM) mode through polarity switching between time segments. The matrix-matched external standard calibration curves were used for quantitative analysis. The linearities of chlormequat chloride, mepiquat chloride, choline chloride, cyclanilide, forchlorfenuron, thidiazuron, inabenfide, paclobutrazol, uniconazole and triapenthenol were in the concentration range of 0.1-500 microg/L, daminozide and 6-benzylaminopurine in the concentration range of 1.0-500 microg/L, 2,3,5-triiodobenzoic acid, 2,4-D, cloprop, 4-chlorophenoxyacetic acid (4-CPA) and trinexapac-ethyl in the concentration range of 2.0-1 000 microg/L, abscisic acid (ABA), gibberellic acid (GA3), 1-naphthaleneacetic acid (NAA) and indol-3-ylacetic acid (IAA) in the concentration range of 10-1000 microg/L, with the correlation coefficients higher than 0.990. The limits of detection and the limits of quantification of the method were 0.020-6.0 microg/kg and 0.10-15.0 microg/kg, respectively. For all the samples, the average spiked recoveries ranged from 73.0% to 111.0%, and the relative standard deviations (RSDs, n = 6) were in the range of 3.0% - 17.2%. The method is quick, easy, effective, sensitive and accurate, and can meet the requirements for the determination of the 21 plant growth regulator residues in fruits.

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

    Science.gov (United States)

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

    2016-11-04

    A rapid method to screen and quantify multi-class analytic targets in red wine has been developed by direct analysis in real time (DART) coupled with triple quadruple tandem mass spectrometry (QqQ-MS). A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for increasing analytical speed and reducing matrix effect, and the multiple reaction monitoring (MRM) in DART-MS/MS ensured accurate analysis. One bottle of wine containing 50 pesticides and 12 adulterants, i.e., preservatives, antioxidant, sweeteners, and azo dyes, could be totally determined less than 12min. This method exhibited proper linearity (R 2 ≥0.99) in the range of 1-1000ng/mL for pesticides and 10-5000ng/mL for adulterants. The limits of detection (LODs) were obtained in a 0.5-50ng/mL range for pesticides and 5-50ng/mL range for adulterants, and the limits of quantification (LOQs) were in a 1-100ng/mL range for pesticides and 10-250ng/mL range for adulterants. Three spiked levels for each analyte in wine were evaluated, and the recoveries were in a scope of 75-120%. The results demonstrated DART-MS/MS was a rapid and simple method, and could be applied to rapid analyze residual pesticides and illegal adulterants in a large quantities of red wine. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Food Safety is an Important Public Health Issue: Chloramphenicol Residues Determination by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) in honey.

    Science.gov (United States)

    Krivohlavek, Adela; Žuntar, Irena; Ivešić, Martina; Andačić, Ivana Mandić; Šikić, Sandra

    2014-12-01

    Honey is used for nutritional, medicinal and industrial purposes and antibiotic residues may harm its quality and constitute a danger to human health. The broad spectrum antibiotic chloramphenicol (CAP) was used for curative purposes in veterinary medicine, but is now forbidden in European Union (EU) because of its many serious side effects (e.g. aplastic anaemia, grey syndrome, severe bone marrow depression and hypersensitivity). The aim of this study was to facilitate analyses of the quality and safety of Croatian honey distributed to whole European Union market; an assessment that has not previously been made. CAP in honey was qualifying and quantifying by validated liquid chromatography tandem mass spectrometry with negative electrospray ionisation method (LC-MS/MS). The target antibiotic was separated on chromatographic column Zorbax SB C18 (150 mm x 2.1 mm, 3.5 μm) with a gradient elution using acetonitrile - 0.1% formic acid mobile phase at a flow rate of 0.3 mL/min, with column temperature 35°C for CAP and 5D-CAP as internal standard. Homogenised honey samples were diluted with acetate buffer solution and extracted on Oasis Hydrophilic-Lipophilic-Balanced (HLB) sorbents. The method was used to analyse 280 domestic honey samples collected throughout Croatia between 2005.-2013. Recoveries of the method for real (acacia, chestnut, linden and flower) honey samples were 102% with RSD 8.4%. The value CCα and CCβ were 0.09 and 0.12 μg/kg, respectively. Results showed only three subsequent positive detections (1.1%) of CAP in honey. Analysed honey samples from Croatia showed good quality and safety what is the one of the main objective in consumer health policy in EU.

  13. Development and comparison of two multi-residue methods for the analysis of select pesticides in honey bees, pollen, and wax by gas chromatography-quadrupole mass spectrometry.

    Science.gov (United States)

    Li, Yuanbo; Kelley, Rebecca A; Anderson, Troy D; Lydy, Michael J

    2015-08-01

    One of the hypotheses that may help explain the loss of honey bee colonies worldwide is the increasing potential for exposure of honey bees to complex mixtures of pesticides. To better understand this phenomenon, two multi-residue methods based on different extraction and cleanup procedures have been developed, and compared for the determination of 11 relevant pesticides in honey bees, pollen, and wax by gas chromatography-quadrupole mass spectrometry. Sample preparatory methods included solvent extraction followed by gel permeation chromatography (GPC) cleanup and cleanup using a dispersive solid-phase extraction with zirconium-based sorbents (Z-Sep). Matrix effects, method detection limits, recoveries, and reproducibility were evaluated and compared. Method detection limits (MDL) of the pesticides for the GPC method in honey bees, pollen, and wax ranged from 0.65 to 5.92 ng/g dw, 0.56 to 6.61 ng/g dw, and 0.40 to 8.30 ng/g dw, respectively, while MDLs for the Z-Sep method were from 0.33 to 4.47 ng/g dw, 0.42 to 5.37 ng/g dw, and 0.51 to 5.34 ng/g dw, respectively. The mean recoveries in all matrices and at three spiking concentrations ranged from 64.4% to 149.5% and 71.9% to 126.2% for the GPC and Z-Sep methods, with relative standard deviation between 1.5-25.3% and 1.3-15.9%, respectively. The results showed that the Z-Sep method was more suitable for the determination of the target pesticides, especially chlorothalonil, in bee hive samples. The Z-Sep method was then validated using a series of field-collected bee hive samples taken from honey bee colonies in Virginia. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Development of multi-residue analysis of herbicides in cereal grain by ultra-performance liquid chromatography-electrospray ionization-mass spectrometry.

    Science.gov (United States)

    Dong, Xinfeng; Liang, Shuxuan; Shi, Zhihong; Sun, Hanwen

    2016-02-01

    A rapid and sensitive method was developed for the determination of 50 herbicides in cereal grain by ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS). Using acetonitrile effectively extracted 22 kinds of triazine and other basic herbicides, and using 90:10 v/v acetonitrile-phosphate buffer (pH = 7.5) effectively extracted other 28 herbicides. Chromatographic separation was achieved using gradient elution with acetonitrile-water as a mobile phase for 22 triazine and phenylurea herbicides and with 5mM ammonium acetate aqueous solution containing 0.1% formic acid-acetonitrile as a mobile phase for other 28 herbicides. Using matrix-matched standard calibration curve effectively reduced the indirect matrix effects, ensured accurate quantification for these herbicides. The response was linear over two orders of magnitude with a correlation coefficients (r(2)) higher than 0.992. The limits of quantification for the herbicides varied from 0.2 to 25.6 μg kg(-1). The intra- and inter-day precisions (relative standard deviation, RSD) were 2.2-9.3% and 5.7-17.1%, respectively. The recovery varied from 61.6% to 110% with the RSD of 1.6-11.8%. Analyzing soybean, corn and wheat samples from 17 counties evaluated this method. The developed and validated method has high sensitivity, satisfactory recovery and precision, can ensure the multi-class multi-residue analysis at low μg kg(-1) level for the most herbicides in cereal grain. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Multi-residue method for trace level determination of pharmaceuticals in environmental samples using liquid chromatography coupled to triple quadrupole mass spectrometry.

    Science.gov (United States)

    Grabic, Roman; Fick, Jerker; Lindberg, Richard H; Fedorova, Ganna; Tysklind, Mats

    2012-10-15

    A multi-residue method for the simultaneous determination of more than 90 pharmaceuticals in water samples was developed and validated. The developed method utilizes a single liquid chromatography-tandem mass spectrometry (LC-MS/MS) run after sample enrichment using solid-phase extraction (SPE). The pharmaceuticals included in this method were chosen based on their potency (effect/concentration ratio) and potential to bioaccumulate in fish. Because the selection was based on ecotoxicological criteria and not on ease of detection, the pharmaceuticals have a wide range of physico-chemical properties and represent 27 distinct classes. No method for surface, waste water or similar matrices was previously described for 52 of the 100 target analytes. Four chromatographic columns were tested to optimize the separation prior to detection by mass spectrometry (MS). The resulting method utilizes a Hypersil Gold aQ column. Three different water matrices were tested during method validation: Milli-Q water, surface water (river water from the Umea River) and effluent from the Umea waste water treatment plant (WWTP). Four of the selected pharmaceuticals exhibited poor method efficiency in all matrices. Amiodarone, Dihydroergotamine, Perphenazine and Terbutalin were omitted from the final analytical method. In addition, five compounds were excluded from the method for surface water (Atorvastatin, Chloropromazin, Dipyridamol, Furosemid and Ranitidin) and three other pharmaceuticals (Glibenclamid, Glimepirid and Meclozine) from waste water method respectively. Absolute recoveries were above 70% for Milli-Q water, surface water, and sewage effluent for most pharmaceuticals. The limits of quantification (LOQs) ranged from 0.05 to 50 ng L(-1) (median 5 ng L(-1)). The use of matrix-matched standards led to the elimination of ionization enhancement or suppression. The recoveries of the method for real matrices were in the range of 23-134% for surface water (only three compounds were

  16. Acetylation and glycation of fibrinogen in vitro occur at specific lysine residues in a concentration dependent manner: A mass spectrometric and isotope labeling study

    Energy Technology Data Exchange (ETDEWEB)

    Svensson, Jan, E-mail: jan.svensson@ki.se [Department of Molecular Medicine and Surgery, Karolinska Institutet, Karolinska University Hospital (Solna), SE-171 76 Stockholm (Sweden); Karolinska Institutet, Department of Clinical Sciences, Danderyd Hospital, SE-182 88 Stockholm (Sweden); Bergman, Ann-Charlotte [Department of Molecular Medicine and Surgery, Karolinska Institutet, Karolinska University Hospital (Solna), SE-171 76 Stockholm (Sweden); Adamson, Ulf [Karolinska Institutet, Department of Clinical Sciences, Danderyd Hospital, SE-182 88 Stockholm (Sweden); Blombaeck, Margareta [Department of Molecular Medicine and Surgery, Karolinska Institutet, Karolinska University Hospital (Solna), SE-171 76 Stockholm (Sweden); Wallen, Hakan; Joerneskog, Gun [Karolinska Institutet, Department of Clinical Sciences, Danderyd Hospital, SE-182 88 Stockholm (Sweden)

    2012-05-04

    Highlights: Black-Right-Pointing-Pointer Fibrinogen was incubated in vitro with glucose or aspirin. Black-Right-Pointing-Pointer Acetylations and glycations were found at twelve lysine sites by mass spectrometry. Black-Right-Pointing-Pointer The labeling by aspirin and glucose occurred dose-dependently. Black-Right-Pointing-Pointer No competition between glucose and aspirin for binding to fibrinogen was found. -- Abstract: Aspirin may exert part of its antithrombotic effects through platelet-independent mechanisms. Diabetes is a condition in which the beneficial effects of aspirin are less prominent or absent - a phenomenon called 'aspirin resistance'. We investigated whether acetylation and glycation occur at specific sites in fibrinogen and if competition between glucose and aspirin in binding to fibrinogen occurs. Our hypothesis was that such competition might be one explanation to 'aspirin resistance' in diabetes. After incubation of fibrinogen in vitro with aspirin (0.8 mM, 24 h) or glucose (100 mM, 5-10 days), we found 12 modified sites with mass spectrometric techniques. Acetylations in the {alpha}-chain: {alpha}K191, {alpha}K208, {alpha}K224, {alpha}K429, {alpha}K457, {alpha}K539, {alpha}K562, in the {beta}-chain: {beta}K233, and in the {gamma}-chain: {gamma}K170 and {gamma}K273. Glycations were found at {beta}K133 and {gamma}K75, alternatively {gamma}K85. Notably, the lysine 539 is a site involved in FXIII-mediated cross-linking of fibrin. With isotope labeling in vitro, using [{sup 14}C-acetyl]salicylic acid and [{sup 14}C]glucose, a labeling of 0.013-0.084 and 0.12-0.5 mol of acetylated and glycated adduct/mol fibrinogen, respectively, was found for clinically (12.9-100 {mu}M aspirin) and physiologically (2-8 mM glucose) relevant plasma concentrations. No competition between acetylation and glycation could be demonstrated. Thus, fibrinogen is acetylated at several lysine residues, some of which are involved in the cross-linking of

  17. Acetylation and glycation of fibrinogen in vitro occur at specific lysine residues in a concentration dependent manner: A mass spectrometric and isotope labeling study

    International Nuclear Information System (INIS)

    Svensson, Jan; Bergman, Ann-Charlotte; Adamson, Ulf; Blombäck, Margareta; Wallén, Håkan; Jörneskog, Gun

    2012-01-01

    Highlights: ► Fibrinogen was incubated in vitro with glucose or aspirin. ► Acetylations and glycations were found at twelve lysine sites by mass spectrometry. ► The labeling by aspirin and glucose occurred dose-dependently. ► No competition between glucose and aspirin for binding to fibrinogen was found. -- Abstract: Aspirin may exert part of its antithrombotic effects through platelet-independent mechanisms. Diabetes is a condition in which the beneficial effects of aspirin are less prominent or absent – a phenomenon called “aspirin resistance”. We investigated whether acetylation and glycation occur at specific sites in fibrinogen and if competition between glucose and aspirin in binding to fibrinogen occurs. Our hypothesis was that such competition might be one explanation to “aspirin resistance” in diabetes. After incubation of fibrinogen in vitro with aspirin (0.8 mM, 24 h) or glucose (100 mM, 5–10 days), we found 12 modified sites with mass spectrometric techniques. Acetylations in the α-chain: αK191, αK208, αK224, αK429, αK457, αK539, αK562, in the β-chain: βK233, and in the γ-chain: γK170 and γK273. Glycations were found at βK133 and γK75, alternatively γK85. Notably, the lysine 539 is a site involved in FXIII-mediated cross-linking of fibrin. With isotope labeling in vitro, using [ 14 C-acetyl]salicylic acid and [ 14 C]glucose, a labeling of 0.013–0.084 and 0.12–0.5 mol of acetylated and glycated adduct/mol fibrinogen, respectively, was found for clinically (12.9–100 μM aspirin) and physiologically (2–8 mM glucose) relevant plasma concentrations. No competition between acetylation and glycation could be demonstrated. Thus, fibrinogen is acetylated at several lysine residues, some of which are involved in the cross-linking of fibrinogen. This may mechanistically explain why aspirin facilitates fibrin degradation. We find no support for the idea that glycation of fibrin(ogen) interferes with acetylation of

  18. S{sub 3} discrete group as a source of the quark mass and mixing pattern in 331 models

    Energy Technology Data Exchange (ETDEWEB)

    Carcamo Hernandez, A.E. [Universidad Tecnica Federico Santa Maria and Centro Cientifico-Tecnologico de Valparaiso, Valparaiso (Chile); Martinez, R.; Nisperuza, Jorge [Universidad Nacional de Colombia, Ciudad Universitaria, Departamento de Fisica, Bogota D.C. (Colombia)

    2015-02-01

    We propose a model based on the SU(3){sub C} x SU(3){sub L} x U(1){sub X} gauge symmetry with an extra S{sub 3} x Z{sub 2} x Z{sub 4} x Z{sub 12} discrete group, which successfully accounts for the SM quark mass and mixing pattern. The observed hierarchy of the SM quark masses and quark mixing matrix elements arises from the Z{sub 4} and Z{sub 12} symmetries, which are broken at a very high scale by the SU(3){sub L} scalar singlets (σ,ζ) and τ, charged under these symmetries, respectively. The Cabbibo mixing arises from the down-type quark sector whereas the up quark sector generates the remaining quark mixing angles. The obtained magnitudes of the CKM matrix elements, the CP violating phase, and the Jarlskog invariant are in agreement with the experimental data. (orig.)

  19. Enhanced Retention of Chelating Reagents in Octadecylsilyl Silica Phase by Interaction with Residual Silanol Groups in Solid Phase Extraction of Divalent Metal Ions.

    Science.gov (United States)

    Ohmuro, Satoshi; Fujii, Kan; Yasui, Takashi; Takada, Kazutake; Yuchi, Akio; Kokusen, Hisao

    2016-01-01

    Solid-phase extraction (SPE) of divalent metal ions with a lipophilic and potentially divalent hexadentate chelating reagent (H2L), with which octadecylsilyl silica (ODS), was impregnated with was studied to gain more insight into and develop the potential of this methodology. This is the first time to demonstrate that this reagent as well as other common nitrogen-containing reagents were retained both by adsorption due to hydrogen bonding between nitrogen atoms of the reagent and residual silanol groups in the ODS phase and by simple distribution into the hydrophobic space. An appreciably large amount of this reagent could be retained by the adsorption mechanism even with a relatively thin loading solution. The divalent metal ions of Mn(2+), Co(2+) and Zn(2+) were extracted as 1:1 neutral complexes ([ML]), while Ni(2+) and Cu(2+) as ion-pairs of 1:1 cationic complex ([MHL](+)) with anion in SPE with H2L. The extractability and selectivity were substantially the same as that in liquid-liquid extraction.

  20. Association of ABO Blood Group and Body Mass Index: A Cross-Sectional Study from a Ghanaian Population

    Directory of Open Access Journals (Sweden)

    Samuel Smith

    2018-01-01

    Full Text Available ABO blood group and body mass index (BMI have individually been appraised as risk factors for certain diseases. From statistical perspective, it may be important to examine the relationship between the ABO blood antigen and BMI. This cross-sectional study involved 412 participants aged 18 to 46 at the Kwame Nkrumah University of Science and Technology (KNUST, Kumasi. Weight and height of participants were measured for BMI calculation; blood group determination was done using antisera. Blood group O was the most prevalent (51.2%, while Rhesus-positive individuals constituted 90.3%. 6.3% of the participants were obese, while 18.7% were overweight. There was significant (p=0.006 higher prevalence of obesity in females (10.3% than in males (3.4%. The study did not observe any significant difference by association of ABO blood group with gender (p=0.973, BMI (p=0.307, or Rhesus status (p=0.723. Regarding gender (p=0.400 and BMI (p=0.197, no statistically significant difference was observed between Rhesus blood groups. The prevalence of overweight, obesity, blood type O, and rhesus positive observed among students in this study is largely similar to what has been reported in published studies in Ghana and from other countries. Overweight and obesity were not associated with ABO blood groups or Rhesus in this study.

  1. Relationship between body mass index, bone mineral density, and oral hygiene with periodontal disease in a Mexican elderly group.

    Directory of Open Access Journals (Sweden)

    José Francisco Murrieta

    2016-05-01

    Full Text Available The aim of this study was to evaluate the relationship of body mass index (BMI, bone mineral density (BMD, and oral hygiene with periodontal disease (PD in a group of elderly adults in Mexico City. Material and Methods: A cross-sectional study with a convenience sample of 151 elderly adults was conducted. Before applying the epidemiological survey, each subject was asked to sign an informed consent. Standardization for measuring Ramfjord’s Periodontal Disease Index (PDI, BMI, and Green and Vermilion’s OHI-S was carried out. Descriptive statistics and linear regression models were performed. Results: The 93.4% of the group had PD, 33.8% showed severe gingivitis and 20.5% mild gingivitis. A 28.5% five percent of the group had osteopenia and 18.5% had osteoporosis, being more common in people over 69 years. The 38.4% percent of the group was underweight and 53.0% had poor oral hygiene. Oral hygiene accounted for 63.1% of the PD variance (p=0.0001, figure that did not increase considerably by adding BMD and BMI variables to the regression model. Conclusion: The frequency of PD in this group of elderly adults was high and significantly associated with BMD, BMI, and mainly oral hygiene.

  2. A wide planetary-mass companion to a young M3 star of the AB Dor moving group

    Directory of Open Access Journals (Sweden)

    Lafrenière David

    2013-04-01

    Full Text Available We present a planetary-mass companion found 42′′ (2000 AU from a M3 star, candidate member of the young (50-120 Myr AB Doradus moving group. It was identified through an ongoing survey with GMOS at Gemini-South, via its distinctively red i-z color (>3.51. The comoving status of this object was confirmed by 2 epochs of WIRCam/CFHT J-band images. The NIR photometry and WISE colors suggest an early-to-mid T bound companion. A NIR spectrum, taken with GNIRS at Gemini-North, confirms a mid-T spectral type. With an estimated temperature between 900 K and 1200 K, models predict a mass between 7 and 12 MJup for this object. The benchmark character of this planetary-mass object lies in its relatively well-constrained age and in its very wide separation, that allows in-depth studies that can help validating models and understanding similar but closer-in companions such as the ones that will be uncovered by next-generation planet finders (e.g. GPI and SPHERE.

  3. Selective 'unlabeling' of amino acids in fractionally 13C labeled proteins: An approach for stereospecific NMR assignments of CH3 groups in Val and Leu residues

    Energy Technology Data Exchange (ETDEWEB)

    Atreya, H.S.; Chary, K.V.R. [Tata Institute of Fundamental Research, Department of Chemical Sciences (India)

    2001-03-15

    A novel methodology for stereospecific NMR assignments of methyl (CH{sub 3}) groups of Val and Leu residues in fractionally {sup 13}C-labeled proteins is presented. The approach is based on selective 'unlabeling' of specific amino acids in proteins while fractionally {sup 13}C-labeling the rest. A 2D [{sup 13}C-{sup 1}H] HSQC spectrum recorded on such a sample is devoid of peaks belonging to the 'unlabeled' amino acid residues. Such spectral simplification aids in unambiguous stereospecific assignment of diastereotopic CH{sub 3} groups in Val and Leu residues in large proteins. This methodology has been demonstrated on a 15 kDa calcium binding protein from Entamoeba histolytica (Eh-CaBP)

  4. Detection of pyridaben residue levels in hot pepper fruit and leaves by liquid chromatography-tandem mass spectrometry: effect of household processes.

    Science.gov (United States)

    Kim, Sung-Woo; Abd El-Aty, A M; Rahman, Md Musfiqur; Choi, Jeong-Heui; Choi, Ok-Ja; Rhee, Gyu-Seek; Chang, Moon-Ik; Kim, Heejung; Abid, Morad D N; Shin, Sung Chul; Shim, Jae-Han

    2015-07-01

    Following quick, easy, cheap, effective, rugged and safe (QuEChERS) and LC/MS/MS analysis, pyridaben residual levels were determined in unprocessed and processed hot pepper fruit and leaves. The linearities were satisfactory with determination coefficients (R(2)) in excess of 0.995 in processed and unprocessed pepper fruit and leaves. Recoveries at various concentrations were 79.9-105.1% with relative standard deviations ≤15%. The limits of quantitation of 0.003-0.012 mg/kg were very low compared with the maximum residue limits (2-5 mg/kg) set by the Ministry of Food and Drug Safety, Republic of Korea. The effects of various household processes, including washing, blanching, frying and drying under different conditions (water volume, blanching time and temperature) on residual concentrations were evaluated. Both washing and blanching (in combination with high water volume and time factor) significantly reduced residue levels in hot pepper fruit and leaves compared with other processes. In sum, the developed method was satisfactory and could be used to accurately detect residues in unprocessed and processed pepper fruit and leaves. It is recommended that pepper fruit/leaves be blanched after washing before being consumed to protect consumers from the negative health effects of detected pesticide residues. Copyright © 2014 John Wiley & Sons, Ltd.

  5. Distinguishing of Ile/Leu amino acid residues in the PP3 protein by (hot) electron capture dissociation in Fourier transform ion cyclotron resonance mass spectrometry

    DEFF Research Database (Denmark)

    Kjeldsen, Frank; Haselmann, Kim F; Sørensen, Esben Skipper

    2003-01-01

    In hot electron capture dissociation (HECD), multiply protonated polypeptides fragment upon capturing approximately 11-eV electrons. The excess of energy upon the primary c, z* cleavage induces secondary fragmentation in z* fragments. The resultant w ions allow one to distinguish between the isom......In hot electron capture dissociation (HECD), multiply protonated polypeptides fragment upon capturing approximately 11-eV electrons. The excess of energy upon the primary c, z* cleavage induces secondary fragmentation in z* fragments. The resultant w ions allow one to distinguish between...... the isomeric Ile and Leu residues. The analytical utility of HECD is evaluated using tryptic peptides from the bovine milk protein PP3 containing totally 135 amino acid residues. Using a formal procedure for Ile/Leu (Xle) residue assignment, the identities of 20 out of 25 Xle residues (80%) were determined....... The identity of an additional two residues could be correctly guessed from the absence of the alternative w ions, and only two residues, for which neither expected nor alternative w ions were observed, remained unassigned. Reinspection of conventional ECD spectra also revealed the presence of Xle w ions...

  6. Improvements in the analytical methodology for the residue determination of the herbicide glyphosate in soils by liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Botero-Coy, A M; Ibáñez, M; Sancho, J V; Hernández, F

    2013-05-31

    The determination of glyphosate (GLY) in soils is of great interest due to the widespread use of this herbicide and the need of assessing its impact on the soil/water environment. However, its residue determination is very problematic especially in soils with high organic matter content, where strong interferences are normally observed, and because of the particular physico-chemical characteristics of this polar/ionic herbicide. In the present work, we have improved previous LC-MS/MS analytical methodology reported for GLY and its main metabolite AMPA in order to be applied to "difficult" soils, like those commonly found in South-America, where this herbicide is extensively used in large areas devoted to soya or maize, among other crops. The method is based on derivatization with FMOC followed by LC-MS/MS analysis, using triple quadrupole. After extraction with potassium hydroxide, a combination of extract dilution, adjustment to appropriate pH, and solid phase extraction (SPE) clean-up was applied to minimize the strong interferences observed. Despite the clean-up performed, the use of isotope labelled glyphosate as internal standard (ILIS) was necessary for the correction of matrix effects and to compensate for any error occurring during sample processing. The analytical methodology was satisfactorily validated in four soils from Colombia and Argentina fortified at 0.5 and 5mg/kg. In contrast to most LC-MS/MS methods, where the acquisition of two transitions is recommended, monitoring all available transitions was required for confirmation of positive samples, as some of them were interfered by unknown soil components. This was observed not only for GLY and AMPA but also for the ILIS. Analysis by QTOF MS was useful to confirm the presence of interferent compounds that shared the same nominal mass of analytes as well as some of their main product ions. Therefore, the selection of specific transitions was crucial to avoid interferences. The methodology developed

  7. Determination of aminoglycoside residues in milk and muscle based on a simple and fast extraction procedure followed by liquid chromatography coupled to tandem mass spectrometry and time of flight mass spectrometry.

    Science.gov (United States)

    Arsand, Juliana Bazzan; Jank, Louíse; Martins, Magda Targa; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara; Sirtori, Carla

    2016-07-01

    Antibiotics are widely used in veterinary medicine mainly for treatment and prevention of diseases. The aminoglycosides are one of the antibiotics classes that have been extensively employed in animal husbandry for the treatment of bacterial infections, but also as growth promotion. The European Union has issued strict Maximum Residue Levels (MRLs) for aminoglycosides in several animal origin products including bovine milk, bovine, swine and poultry muscle. This paper describes a fast and simple analytical method for the determination of ten aminoglycosides (spectinomycin, tobramycin, gentamicin, kanamycin, hygromycin, apramycin, streptomycin, dihydrostreptomycin, amikacin and neomycin) in bovine milk and bovine, swine and poultry muscle. For sample preparation, an extraction method was developed using trichloroacetic acid and clean up with low temperature precipitation and C18 bulk. Liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) was used to carry out quantitative analysis and liquid chromatography-quadrupole-time of flight-mass spectrometry (LC-QTOF-MS) was used to screening purposes. Both methods were validated according to the European Union Commission Directive 2002/657/EC. Good performance characteristics were obtained for recovery, precision, calibration curve, specificity, decision limits (CCα) and detection capabilities (CCβ) in all matrices evaluated. The detection limit (LOD) and quantification limit (LOQ) were ranging from 5 to 100ngg(-1) and 12.5 to 250ngg(-1), respectively. Good linearity (r)-above 0.99-was achieved in concentrations ranging from 0.0 to 2.0×MRL. Recoveries ranged from 36.8% to 98.0% and the coefficient of variation from 0.9 to 20.2%, noting that all curves have been made into their own matrices in order to minimize the matrix effects. The CCβ values obtained in qualitative method were between 25 and 250ngg(-1). The proposed method showed to be simple, easy, and adequate for high-throughput analysis of a large

  8. New method to determine the total carbonyl functional group content in extractable particulate organic matter by tandem mass spectrometry.

    Science.gov (United States)

    Dron, J; Zheng, W; Marchand, N; Wortham, H

    2008-08-01

    A functional group analysis method was developed to determine the quantitative content of carbonyl functional groups in atmospheric particulate organic matter (POM) using constant neutral loss scanning-tandem mass spectrometry (CNLS-MS/MS). The neutral loss method consists in monitoring the loss of a neutral fragment produced by the fragmentation of a precursor ion in a collision cell. The only ions detected are the daughter ions resulting from the loss of the neutral fragment under study. Then, scanning the loss of a neutral fragment characteristic of a functional group enables the selective detection of the compounds bearing the chemical function under study within a complex mixture. The selective detection of carbonyl functional groups was achieved after derivatization with pentafluorophenylhydrazine (PFPH) by monitoring the neutral loss of C(6)F(5)N (181 amu), which was characteristic of a large panel of derivatized carbonyl compounds. The method was tested on 25 reference mixtures of different composition, all containing 24 carbonyl compounds at randomly determined concentrations. The repeatability and calibration tests were satisfying as they resulted in a relative standard deviation below 5% and a linear range between 0.01 and 0.65 mM with a calculated detection limit of 0.0035 mM. Also, the relative deviation induced by changing the composition of the mixture while keeping the total concentration of carbonyl functional groups constant was less than 20%. These reliability experiments demonstrate the high robustness of the developed procedure for accurate carbonyl functional group measurement, which was applied to atmospheric POM samples. Copyright (c) 2008 John Wiley & Sons, Ltd.

  9. Molecular detection of minimal residual disease is a strong predictive factor of relapse in childhood B-lineage acute lymphoblastic leukemia with medium risk features. A case control study of the International BFM study group

    NARCIS (Netherlands)

    Biondi, A; Valsecchi, MG; Seriu, T; D'Aniello, E; Willemse, MJ; Fasching, K; Pannunzio, A; Gadner, H; Schrappe, M; Kamps, WA; Bartram, CR; van Dongen, JJM; Panzer-Grumayer, ER

    2000-01-01

    The medium-risk B cell precursor acute lymphoblastic leukemia (ALL) accounts for 50-60% of total childhood ALL and comprises the largest number of relapses still unpredictable with diagnostic criteria. To evaluate the prognostic impact of minimal residual disease (MRD) in this specific group, a case

  10. Effect of Using Different Vehicle Weight Groups on the Estimated Relationship Between Mass Reduction and U.S. Societal Fatality Risk per Vehicle Miles of Travel

    Energy Technology Data Exchange (ETDEWEB)

    Wenzel, Tom P. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Environmental Technologies Area. Building Technology and Urban Systems Division

    2016-08-22

    This report recalculates the estimated relationship between vehicle mass and societal fatality risk, using alternative groupings by vehicle weight, to test whether the trend of decreasing fatality risk from mass reduction as case vehicle mass increases, holds over smaller increments of the range in case vehicle masses. The NHTSA baseline regression model estimates the relationship using for two weight groups for cars and light trucks; we re-estimated the mass reduction coefficients using four, six, and eight bins of vehicle mass. The estimated effect of mass reduction on societal fatality risk was not consistent over the range in vehicle masses in these weight bins. These results suggest that the relationship indicated by the NHTSA baseline model is a result of other, unmeasured attributes of the mix of vehicles in the lighter vs. heavier weight bins, and not necessarily the result of a correlation between mass reduction and societal fatality risk. An analysis of the average vehicle, driver, and crash characteristics across the various weight groupings did not reveal any strong trends that might explain the lack of a consistent trend of decreasing fatality risk from mass reduction in heavier vehicles.

  11. Consultants Group Meeting on Development of Cost-Effective Diets for Use in Mass Production of Tsetse Flies. Working Material

    International Nuclear Information System (INIS)

    2000-10-01

    The increasing demand for employing tsetse SIT for area-wide tsetse and trypanosomosis management programmes on mainland Africa has compelled the IAEA to concentrate on the development of semi-automated processes for standardising laborious and quality sensitive components of the sterile male mass production. The size of facilities required to produce the sterile males will continue to increase with time and demand. The current diet for tsetse is decontaminated vertebrate blood and it will need to be supplied to centres without access to a suitable local blood source. In view of the increasing demand for sterile male tsetse and uncertainty of obtaining high quality decontaminated blood locally, ways need to be explored to ensure availability of inexpensive, standard quality diets. Towards this goal a consultants group meeting on the development of cost-effective diets for tsetse was held at the IAEA headquarters in Vienna, Austria from 17 to 21 July 2000. The major objective of the consultants group meeting was to identify research that is needed to ensure the availability of large quantities of high quality diet for tsetse mass production. Seven papers were presented and discussed. A visit was made to the Entomology Unit, at the FAO/IAEA Agriculture and Biotechnology Laboratories, Seibersdorf to see the present tsetse rearing facility and the various steps of blood processing and quality assurance used in the evaluation of blood quality before use for colony feeding. The meeting noted that commercially available products are used to prepare standard diets for screwworm mass production. These products have not yet been adequately evaluated for tsetse. However, it is necessary to improve the current procedure applied to the use fresh blood. Possibilities of utilising commercially available dietary ingredients should also be explored. A three-step approach was proposed: Improvement and optimisation of the current blood collection, processing etc.; Use of additives

  12. Functional Groups and Structural Insights of Water-Soluble Organic Carbon using Ultrahigh Resolution FT-ICR Tandem Mass Spectrometry

    Science.gov (United States)

    Mazzoleni, L. R.; Habib, D.; Zhao, Y.; Dalbec, M.; Samburova, V.; Hallar, G.; Zielinska, B.; Lowenthal, D.

    2013-12-01

    Water-soluble organic carbon (WSOC) is a complex mixture of thousands of organic compounds which may have significant influence on the climate-relevant properties of atmospheric aerosols. An improved understanding of the molecular composition of WSOC is needed to evaluate the effect of aerosol composition upon aerosol physical properties. Products of gas phase, aqueous phase and particle phase reactions contribute to pre-existing aerosol organic mass or nucleate new aerosol particles. Thus, ambient aerosols carry a complex array of WSOC components with variable chemical signatures depending upon its origin and aerosol life-cycle processes. In this work, ultrahigh resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was used to characterize aerosol WSOC collected during the summer of 2010 at the Storm Peak Laboratory (3210 m a.s.l.) near Steamboat Springs, CO. Approximately 4000 molecular formulas were assigned in the mass range of m/z 100-800 after negative-ion electrospray ionization. The observed trends indicate significant non-oxidative accretion reaction pathways for the formation of high molecular weight WSOC components closely associated with terpene ozonolysis secondary organic aerosol (SOA). The aerosol WSOC was further characterized using ultrahigh resolution tandem MS analysis with infrared multiphoton dissociation to determine the functional groups and structural properties of 1700 WSOC species up to m/z 600. Due to the complex nature of the WSOC, multiple precursor ions were simultaneously fragmented. The exact mass measurements of the precursor and product ions facilitated molecular formula assignments and matching of neutral losses. The most important neutral losses are CO2, H2O, CH3OH, HNO3, CH3NO3, SO3 and SO4. The presence and frequency of these losses indicate the type of functional groups contained in the precursor structures. Consistent with the acidic nature of WSOC compounds, the most frequently observed losses

  13. Precursor ion scanning-mass spectrometry for the determination of nitro functional groups in atmospheric particulate organic matter.

    Science.gov (United States)

    Dron, Julien; Abidi, Ehgere; Haddad, Imad El; Marchand, Nicolas; Wortham, Henri

    2008-06-23

    An analytical method for the quantitative determination of the total nitro functional group (R-NO2) content in atmospheric particulate organic matter is developed. The method is based on the selectivity of NO2(-) (m/z 46) precursor ion scanning (PAR 46) by atmospheric pressure chemical ionization-tandem mass spectrometry (APCI-MS/MS). PAR 46 was experimented on 16 nitro compounds of different molecular structures and was compared with a neutral loss of NO (30 amu) technique in terms of sensitivity and efficiency to characterize the nitro functional groups. Covering a wider range of compounds, PAR 46 was preferred and applied to reference mixtures containing all the 16 compounds under study. Repeatability carried out using an original statistical approach, and calibration experiments were performed on the reference mixtures proven the suitability of the technique for quantitative measurements of nitro functional groups in samples of environmental interest with good accuracy. A linear range was obtained for concentrations ranging between 0.005 and 0.25 mM with a detection limit of 0.001 mM of nitro functional groups. Finally, the analytical error based on an original statistical approach applied to numerous reference mixtures was below 20%. Despite of potential artifacts related to nitro-alkanes and organonitrates, this new methodology offers a promising alternative to FT-IR measurements. The relevance of the method and its potentialities are demonstrated through its application to aerosols collected in the EUPHORE simulation chamber during o-xylene photooxidation experiments and in a suburban area of a French alpine valley during summer.

  14. Effect of Parasitoid: Host Ratio and Group Size on Fitness of Spathius galinae (Hymenoptera: Braconidae): Implications for Mass-Rearing.

    Science.gov (United States)

    Watt, Timothy J; Duan, Jian J; Tallamy, Douglas W; Hough-Goldstein, Judith

    2015-06-01

    Producing insect natural enemies in laboratories or insectaries for biological pest control is often expensive, and developing cost-effective rearing techniques is a goal of many biological control programs. Spathius galinae Belokobylskij and Strazenac (Hymenoptera: Braconidae), a newly described ectoparasitoid of emerald ash borer, Agrilus planipennis Fairmaire (Coleoptera: Buprestidae), is currently being evaluated for environmental introduction in the United States to provide biological control of this invasive pest. To improve mass-rearing outcomes for S. galinae, we investigated the effects of parasitoid: host ratio and parasitoid and host group size (density) on parasitoid fitness. Our results showed that when 1 emerald ash borer larva was exposed to 1, 2, 4, or 8 female parasitoids, parasitism rate was positively associated with increasing parasitoid: host ratio, while brood size, sex ratio, and fitness estimates of progeny were not affected. When a constant 1:1 parasitoid: host ratio was used, but group size varied from 1 female parasitoid and 1 host, 5 parasitoids and 5 hosts, 10 of each, and 20 of each in same size rearing cages, parasitism rates were highest when at least 5 females were exposed to 5 host larvae. Moreover, the number of progeny produced per female parasitoid was greatest when group size was 10 parasitoids and 10 hosts. These findings demonstrate that S. galinae may be reared most efficiently in moderately high-density groups (10 parasitoids and hosts) and with a 1:1 parasitoid: host ratio. © The Authors 2015. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  15. A multi-residue method for pesticides analysis in green coffee beans using gas chromatography-negative chemical ionization mass spectrometry in selective ion monitoring mode.

    Science.gov (United States)

    Pizzutti, Ionara R; de Kok, Andre; Dickow Cardoso, Carmem; Reichert, Bárbara; de Kroon, Marijke; Wind, Wouter; Weber Righi, Laís; Caiel da Silva, Rosselei

    2012-08-17

    In this study, a new gas chromatography-mass spectrometry (GC-MS) method, using the very selective negative chemical ionization (NCI) mode, was developed and applied in combination with a modified acetonitrile-based extraction method (QuEChERS) for the analysis of a large number of pesticide residues (51 pesticides, including isomers and degradation products) in green coffee beans. A previously developed integrated sample homogenization and extraction method for both pesticides and mycotoxins analysis was used. An homogeneous slurry of green milled coffee beans and water (ratio 1:4, w/w) was prepared and extracted with acetonitrile/acetic acid (1%), followed by magnesium sulfate addition for phase separation. Aliquots from this extract could be used directly for LC-MS/MS analysis of mycotoxins and LC-amenable pesticides. For GC-MS analysis, a further clean-up was necessary. C18- and PSA-bonded silica were tested as dispersive solid-phase extraction (d-SPE) sorbents, separate and as a mixture, and the best results were obtained using C18-bonded silica. For the optimal sensitivity and selectivity, GC-MS detection in the NCI-selected ion monitoring (SIM) mode had to be used to allow the fast analysis of the difficult coffee bean matrix. The validation was performed by analyzing recovery samples at three different spike concentrations, 10, 20 and 50 μg kg(-1), with 6 replicates (n=6) at each concentration. Linearity (r(2)) of calibration curves, estimated instrument and method limits of detection and limits of quantification (LOD(i), LOD(m), LOQ(i) and LOQ(m), respectively), accuracy (as recovery %), precision (as RSD%) and matrix effects (%) were determined for each individual pesticide. From the 51 analytes (42 parent pesticides, 4 isomers and 5 degradation products) determined by GC-MS (NCI-SIM), approximately 76% showed average recoveries between 70-120% and 75% and RSD ≤ 20% at the lowest spike concentration of 10 μg kg(-1), the target method LOQ. For the

  16. Low body mass index is an important risk factor for low bone mass and increased bone loss in early postmenopausal women. Early Postmenopausal Intervention Cohort (EPIC) study group

    DEFF Research Database (Denmark)

    Ravn, Pernille; Cizza, G; Bjarnason, N H

    1999-01-01

    Thinness (low percentage of body fat, low body mass index [BMI], or low body weight) was evaluated as a risk factor for low bone mineral density (BMD) or increased bone loss in a randomized trial of alendronate for prevention of osteoporosis in recently postmenopausal women with normal bone mass (n...... (r = -0.12 to -0.15, p mass parameters and response to alendronate treatment, which...... indicated that risk of low bone mass and increased bone loss caused by thinness could be compensated by alendronate treatment. In conclusion, thinness is an important risk factor for low bone mass and increased bone loss in postmenopausal women. Because the response to alendronate treatment is independent...

  17. Successful Therapy Reduction and Intensification for Childhood Acute Lymphoblastic Leukemia Based on Minimal Residual Disease Monitoring : Study ALL10 From the Dutch Childhood Oncology Group

    NARCIS (Netherlands)

    Pieters, Rob; de Groot-Kruseman, Hester; Van der Velden, Vincent; Fiocco, Marta; van den Berg, Henk; Bont, de Evelien; Egeler, R. Maarten; Hoogerbrugge, Peter; Kaspers, Gertjan; Van der Schoot, Ellen; De Haas, Valerie; Van Dongen, Jacques

    2016-01-01

    Purpose Outcome of childhood acute lymphoblastic leukemia (ALL) improved greatly by intensifying chemotherapy for all patients. Minimal residual disease (MRD) levels during the first months predict outcome and may select patients for therapy reduction or intensification. Methods Patients 1 to 18

  18. THE EFFECT OF ENVIRONMENT ON MILKY-WAY-MASS GALAXIES IN A CONSTRAINED SIMULATION OF THE LOCAL GROUP

    Energy Technology Data Exchange (ETDEWEB)

    Creasey, Peter; Scannapieco, Cecilia; Nuza, Sebastián E.; Gottlöber, Stefan; Steinmetz, Matthias [Leibniz-Institut für Astrophysik Potsdam (AIP), An der Sternwarte 16, D-14482, Potsdam (Germany); Yepes, Gustavo [Grupo de Astrofísica, Universidad Autónoma de Madrid, Madrid E-28049 (Spain)

    2015-02-10

    In this Letter, we present, for the first time, a study of star formation rate (SFR), gas fraction, and galaxy morphology of a constrained simulation of the Milky Way (MW) and Andromeda (M31) galaxies compared to other MW-mass galaxies. By combining with unconstrained simulations, we cover a sufficient volume to compare these galaxies’ environmental densities ranging from the field to that of the Local Group (LG). This is particularly relevant as it has been shown that, quite generally, galaxy properties depend intimately upon their environment, most prominently when galaxies in clusters are compared to those in the field. For galaxies in loose groups such as the LG, however, environmental effects have been less clear. We consider the galaxy’s environmental density in spheres of 1200 kpc (comoving) and find that while environment does not appear to directly affect morphology, there is a positive trend with SFRs. This enhancement in star formation occurs systematically for galaxies in higher density environments, regardless whether they are part of the LG or in filaments. Our simulations suggest that the richer environment at megaparsec scales may help replenish the star-forming gas, allowing higher specific SFRs in galaxies such as the MW.

  19. Analysis of organo-chlorine pesticides residue in raw coffee with a modified "quick easy cheap effective rugged and safe" extraction/clean up procedure for reducing the impact of caffeine on the gas chromatography-mass spectrometry measurement.

    Science.gov (United States)

    Bresin, Bruno; Piol, Maria; Fabbro, Denis; Mancini, Maria Antonietta; Casetta, Bruno; Del Bianco, Clorinda

    2015-01-09

    The control of pesticide residues on raw coffee is a task of great importance due to high consumption of this beverage in Italy and in many other countries. High caffeine content can hamper extraction and measurement of any pesticide residue. A tandem extraction protocol has been devised by exploiting the quick easy cheap effective rugged and safe (QuEChERS) scheme for extraction, coupled to a dispersive liquid-liquid micro-extraction (DLLME) in order to drastically reduce caffeine content in the final extract. Gas chromatography-mass spectrometry (GC-MS) has been used for quantification of organo-chlorine pesticides in single ion monitoring (SIM) mode. Method has been validated and performances meet the criteria prescribed by European Union regulations. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. BANYAN. II. Very low mass and substellar candidate members to nearby, young kinematic groups with previously known signs of youth

    International Nuclear Information System (INIS)

    Gagné, Jonathan; Lafrenière, David; Doyon, René; Malo, Lison; Artigau, Étienne

    2014-01-01

    We present Bayesian Analysis for Nearby Young AssociatioNs II (BANYAN II), a modified Bayesian analysis for assessing the membership of later-than-M5 objects to any of several Nearby Young Associations (NYAs). In addition to using kinematic information (from sky position and proper motion), this analysis exploits 2MASS-WISE color-magnitude diagrams in which old and young objects follow distinct sequences. As an improvement over our earlier work, the spatial and kinematic distributions for each association are now modeled as ellipsoids whose axes need not be aligned with the Galactic coordinate axes, and we use prior probabilities matching the expected populations of the NYAs considered versus field stars. We present an extensive contamination analysis to characterize the performance of our new method. We find that Bayesian probabilities are generally representative of contamination rates, except when a parallax measurement is considered. In this case contamination rates become significantly smaller and hence Bayesian probabilities for NYA memberships are pessimistic. We apply this new algorithm to a sample of 158 objects from the literature that are either known to display spectroscopic signs of youth or have unusually red near-infrared colors for their spectral type. Based on our analysis, we identify 25 objects as new highly probable candidates to NYAs, including a new M7.5 bona fide member to Tucana-Horologium, making it the latest-type member. In addition, we reveal that a known L2γ dwarf is co-moving with a bright M5 dwarf, and we show for the first time that two of the currently known ultra red L dwarfs are strong candidates to the AB Doradus moving group. Several objects identified here as highly probable members to NYAs could be free-floating planetary-mass objects if their membership is confirmed.

  1. BANYAN. II. Very low mass and substellar candidate members to nearby, young kinematic groups with previously known signs of youth

    Energy Technology Data Exchange (ETDEWEB)

    Gagné, Jonathan; Lafrenière, David; Doyon, René; Malo, Lison; Artigau, Étienne [Département de Physique and Observatoire du Mont-Mégantic, Université de Montréal, C.P. 6128 Succ. Centre-ville, Montréal, Qc H3C 3J7 (Canada)

    2014-03-10

    We present Bayesian Analysis for Nearby Young AssociatioNs II (BANYAN II), a modified Bayesian analysis for assessing the membership of later-than-M5 objects to any of several Nearby Young Associations (NYAs). In addition to using kinematic information (from sky position and proper motion), this analysis exploits 2MASS-WISE color-magnitude diagrams in which old and young objects follow distinct sequences. As an improvement over our earlier work, the spatial and kinematic distributions for each association are now modeled as ellipsoids whose axes need not be aligned with the Galactic coordinate axes, and we use prior probabilities matching the expected populations of the NYAs considered versus field stars. We present an extensive contamination analysis to characterize the performance of our new method. We find that Bayesian probabilities are generally representative of contamination rates, except when a parallax measurement is considered. In this case contamination rates become significantly smaller and hence Bayesian probabilities for NYA memberships are pessimistic. We apply this new algorithm to a sample of 158 objects from the literature that are either known to display spectroscopic signs of youth or have unusually red near-infrared colors for their spectral type. Based on our analysis, we identify 25 objects as new highly probable candidates to NYAs, including a new M7.5 bona fide member to Tucana-Horologium, making it the latest-type member. In addition, we reveal that a known L2γ dwarf is co-moving with a bright M5 dwarf, and we show for the first time that two of the currently known ultra red L dwarfs are strong candidates to the AB Doradus moving group. Several objects identified here as highly probable members to NYAs could be free-floating planetary-mass objects if their membership is confirmed.

  2. Residue processing

    Energy Technology Data Exchange (ETDEWEB)

    Gieg, W.; Rank, V.

    1942-10-15

    In the first stage of coal hydrogenation, the liquid phase, light and heavy oils were produced; the latter containing the nonliquefied parts of the coal, the coal ash, and the catalyst substances. It was the problem of residue processing to extract from these so-called let-down oils that which could be used as pasting oils for the coal. The object was to obtain a maximum oil extraction and a complete removal of the solids, because of the latter were returned to the process they would needlessly burden the reaction space. Separation of solids in residue processing could be accomplished by filtration, centrifugation, extraction, distillation, or low-temperature carbonization (L.T.C.). Filtration or centrifugation was most suitable since a maximum oil yield could be expected from it, since only a small portion of the let-down oil contained in the filtration or centrifugation residue had to be thermally treated. The most satisfactory centrifuge at this time was the Laval, which delivered liquid centrifuge residue and centrifuge oil continuously. By comparison, the semi-continuous centrifuges delivered plastic residues which were difficult to handle. Various apparatus such as the spiral screw kiln and the ball kiln were used for low-temperature carbonization of centrifuge residues. Both were based on the idea of carbonization in thin layers. Efforts were also being made to produce electrode carbon and briquette binder as by-products of the liquid coal phase.

  3. Analysis of class 1 residual solvents in pharmaceuticals using headspace-programmed temperature vaporization-fast gas chromatography-mass spectrometry.

    Science.gov (United States)

    Pérez Pavón, José Luis; Del Nogal Sánchez, Miguel; Fernández Laespada, M A Esther; García Pinto, Carmelo; Moreno Cordero, Bernardo

    2007-02-02

    A sensitive method is presented for the fast screening and determination of residual class 1 solvents (1,1-dichloroethene, 1,2-dichloroethane, 1,1,1-trichloroethane, carbon tetrachloride and benzene) in pharmaceutical products. The applicability of a headspace (HS) autosampler in combination with GC equipped with a programmed temperature vaporizer (PTV) and a MS detector is explored. Different injection techniques were compared. The benefits of using solvent vent injection instead of split or splitless-hot injection for the measurement of volatile compounds are shown: better peak shapes, better signal-to-noise ratios, and hence better detection limits. The proposed method is extremely sensitive. The limits of detection ranged from 4.9 ppt (benzene) to 7.9 ppt (1,2-dichloroethane) and precision (measured as the relative standard deviation) was equal to or lower than 12% in all cases. The method was applied to the determination of residual solvents in nine different pharmaceutical products. The analytical performance of the method shows that it is appropriate for the determination of residual class 1 solvents and has much lower detection limits than the concentration limits proposed by the International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use. The proposed method achieves a clear improvement in sensitivity with respect to conventional headspace methods due to the use of the PTV.

  4. Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Prados-Rosales, R C; Luque García, J L; Luque de Castro, M D

    2003-04-18

    A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency--namely microwave power, irradiation time, volume of extractant and number of cycles--were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

  5. Development of a Method for the Analysis of Multiclass Antibiotic Residues in Milk Using QuEChERS and Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Wang, Yuan-long; Liu, Zhen-min; Ren, Jing; Guo, Ben-heng

    2015-08-01

    A precise and simplified method of sample preparation for the simultaneous quantification of the antibiotics β-lactam, macrolide, tetracycline, sulfonamide, and quinolone in bovine milk was developed. The central composite design of response surface methodology was used to design and optimize the method for the determination of six different antibiotic residues in milk. The recovery of each antibiotic was studied using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Octadecylsilane (C18), primary secondary amine (PSA), and sodium acetate (Na acetate) were the main factors affecting the recovery of each antibiotic. After optimization, the maximum predicted recovery rate was 84.18% for erythromycin under the optimized conditions of 101.20 mg C18, 52.00 mg PSA, and 1.01 g Na acetate. The recovery rates of the five other antibiotic residues ranged from 86.09% to 115.99%. The results suggested that modified QuEChERS could effectively be implemented in the analysis of antibiotic residues in milk.

  6. On-line solid phase extraction-liquid chromatography-tandem mass spectrometry for insect repellent residue analysis in surface waters using atmospheric pressure photoionization.

    Science.gov (United States)

    Molins-Delgado, Daniel; García-Sillero, Daniel; Díaz-Cruz, M Silvia; Barceló, Damià

    2018-04-06

    Insect repellents (IRs) are a group of organic chemicals whose function is to prevent the ability of insects of landing in a surface. These compounds have been found in the environment and may pose a risk to non-target organisms. In this study, an on-line solid phase extraction - high performance liquid chromatography-tandem mass spectrometry multiresidue method was developed using an atmospheric photoionization source (SPE-HPLC-(APPI)-MS/MS). The use of the APPI as an alternative ionization technique to electrospray (ESI) and atmospheric pressure chemical ionization (APCI) allowed expanding the range of analytical techniques suitable for the analysis of IRs, so far relied in gas chromatography. High sensitivity and precision was reached with method limits of quantification between 0.2 and 4.6 ng l -1 and interday and intraday precision equal or below 15%. The validated method was applied to the study of surface water samples from three European river basins with different flow regime (Adige River in Italy, Sava River in the Balkans, and Evrotas River in Greece). The results showed that two IRs (DEET and Bayrepel) were ubiquitous in the Sava and Evrotas basins, reaching concentrations as high as 105 μg l -1 of Bayrepel in the Sava River, and 5 μg l -1 of DEET in the Evrotas River. Densely populated areas and effluent waste waters are pointed out as the responsible for this pollution. In the alpine river Adige, only three samples showed low levels of IRs (6.01-37.8 ng l -1 ). The concentrations measured were used to perform an environmental risk assessment based on the hazard quotients (HQs) estimation approach by using the chronic and acute eco-toxicity data available. The results revealed that despite the high frequency and eventually high concentrations of these IRs determined in the three basins, only few sites were at risk, with 1 < HQs < 3.3. Copyright © 2018 The Author(s). Published by Elsevier B.V. All rights reserved.

  7. Process combination of thermo pressure hydrolysis and fermentation for innovative processing of residual biogenous mass; Verfahrenskombination aus Thermodruckhydrolyse und Vergaerung zur innovativen Verwertung biogener Restmassen

    Energy Technology Data Exchange (ETDEWEB)

    Prechtl, S.; Merkl, M.; Schieder, D.; Schneider, R.; Bischof, F. [Applikations- und Technikzentrum fuer Energieverfahrens-, Umwelt- und Stroemungstechnik (ATZ-EVUS), Sulzbach-Rosenberg (Germany)

    1999-07-01

    The described processing technique consisting of topped thermal hydrolysis and downstream fermentation is particularly suitable for wet, low-structure organic waste. High turnover rates at short treatment times permit to minimize residues effectively, yield a fair amount of biogas and allow compact design because of low fermenter volumes, which has a positive impact on investment cost. (orig.) [German] Das vorgestellt Verwertungsverfahren bestehend aus vorgeschalteter thermischer Hydrolyse und nachgeschalteter Vergaerung eignet sich besonders fuer nasse, strukturarme organische Abfaelle. Hohe Umsatzraten bei kurzen Behandlungszeiten ermoeglichen eine gute Reststoffminimierung und Biogasausbeute sowie eine kompakte Bauweise durch kleine Fermentervolumina, was sich positiv auf die Investitionskosten auswirkt. (orig.)

  8. QuEChERS GC-MS validation and monitoring of pesticide residues in different foods in the tomato classification group.

    Science.gov (United States)

    Ramírez Restrepo, Andrés; Gallo Ortiz, Andrés Fernando; Hoyos Ossa, Duvan Esteban; Peñuela Mesa, Gustavo Antonio

    2014-09-01

    The objective of this study was to validate (SANCO/12495/2011 and NTC-ISO/IEC 17025) multi-residue multi-class methods using QuEChERS sample preparation and GC-MS for the analysis of regulated pesticides in tomatoes (Solanum lycopersicum), tamarillos (Solanum betaceum) and goldenberries (Physalis peruviana). These Latin American products are representative and widely produced in Antioquia (Colombia). Sample preparation followed the UNE-EN 15662 method (150 mg MgSO4, 25mg primary secondary amines and 25mg of octadecylsiloxane for cleanup; graphitized carbon black was added for tomatoes). Extracts were injected using a programmed temperature-vaporizing injector. The residues were validated over a range from 0.02 mg/kg to 0.20 mg/kg, with 24 analytes validated in tomatoes, 33 in tamarillos and 28 in goldenberries. An initial risk assessment was enabled by monitoring 24 samples in the municipalities of El Peñol, Marinilla and San Vicente Ferrer. Risks were found for tomatoes, but no significant risks were found for tamarillos or goldenberries. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Residual risk

    African Journals Online (AJOL)

    ing the residual risk of transmission of HIV by blood transfusion. An epidemiological approach assumed that all HIV infections detected serologically in first-time donors were pre-existing or prevalent infections, and that all infections detected in repeat blood donors were new or incident infections. During 1986 - 1987,0,012%.

  10. Dimerization Is Not a Determining Factor for Functional High Affinity Human Plasminogen Binding by the Group A Streptococcal Virulence Factor PAM and Is Mediated by Specific Residues within the PAM a1a2 Domain*

    Science.gov (United States)

    Bhattacharya, Sarbani; Liang, Zhong; Quek, Adam J.; Ploplis, Victoria A.; Law, Ruby; Castellino, Francis J.

    2014-01-01

    A emm53 subclass of Group A Streptococcus pyogenes (GAS) interacts tightly with human plasma plasminogen (hPg) and plasmin (hPm) via the kringle 2 (K2hPg) domain of hPg/hPm and the N-terminal a1a2 regions of a GAS coiled-coil M-like protein (PAM). Previous studies have shown that a monomeric PAM fragment, VEK30 (residues 97–125 + Tyr), interacted specifically with isolated K2hPg. However, the binding strength of VEK30 (KD = 56 nm) was ∼60-fold weaker than that of full-length dimeric PAM (KD = 1 nm). To assess whether this attenuated binding was due to the inability of VEK30 to dimerize, we defined the minimal length of PAM required to dimerize using a series of peptides with additional PAM residues placed at the NH2 and COOH termini of VEK30. VEK64 (PAM residues 83–145 + Tyr) was found to be the smallest peptide that adopted an α-helical dimer, and was bound to K2hPg with nearly the same affinity as PAM (KD = 1–2 nm). However, addition of two PAM residues (Arg126-His127) to the COOH terminus of VEK30 (VEK32) maintained a monomeric peptidic structure, but exhibited similar K2hPg binding affinity as full-length dimeric PAM. We identified five residues in a1a2 (Arg113, His114, Glu116, Arg126, His127), mutation of which reduced PAM binding affinity for K2hPg by ∼1000-fold. Replacement of these critical residues by Ala in the GAS genome resulted in reduced virulence, similar to the effects of inactivating the PAM gene entirely. We conclude that rather than dimerization of PAM, the five key residues in the binding domain of PAM are essential to mediate the high affinity interaction with hPg, leading to increased GAS virulence. PMID:24962580

  11. Dimerization is not a determining factor for functional high affinity human plasminogen binding by the group A streptococcal virulence factor PAM and is mediated by specific residues within the PAM a1a2 domain.

    Science.gov (United States)

    Bhattacharya, Sarbani; Liang, Zhong; Quek, Adam J; Ploplis, Victoria A; Law, Ruby; Castellino, Francis J

    2014-08-01

    A emm53 subclass of Group A Streptococcus pyogenes (GAS) interacts tightly with human plasma plasminogen (hPg) and plasmin (hPm) via the kringle 2 (K2hPg) domain of hPg/hPm and the N-terminal a1a2 regions of a GAS coiled-coil M-like protein (PAM). Previous studies have shown that a monomeric PAM fragment, VEK30 (residues 97-125 + Tyr), interacted specifically with isolated K2hPg. However, the binding strength of VEK30 (KD = 56 nm) was ∼60-fold weaker than that of full-length dimeric PAM (KD = 1 nm). To assess whether this attenuated binding was due to the inability of VEK30 to dimerize, we defined the minimal length of PAM required to dimerize using a series of peptides with additional PAM residues placed at the NH2 and COOH termini of VEK30. VEK64 (PAM residues 83-145 + Tyr) was found to be the smallest peptide that adopted an α-helical dimer, and was bound to K2hPg with nearly the same affinity as PAM (KD = 1-2 nm). However, addition of two PAM residues (Arg(126)-His(127)) to the COOH terminus of VEK30 (VEK32) maintained a monomeric peptidic structure, but exhibited similar K2hPg binding affinity as full-length dimeric PAM. We identified five residues in a1a2 (Arg(113), His(114), Glu(116), Arg(126), His(127)), mutation of which reduced PAM binding affinity for K2hPg by ∼ 1000-fold. Replacement of these critical residues by Ala in the GAS genome resulted in reduced virulence, similar to the effects of inactivating the PAM gene entirely. We conclude that rather than dimerization of PAM, the five key residues in the binding domain of PAM are essential to mediate the high affinity interaction with hPg, leading to increased GAS virulence. © 2014 by The American Society for Biochemistry and Molecular Biology, Inc.

  12. Atomic Mass and Nuclear Binding Energy for Y-90 (Yttrium)

    Science.gov (United States)

    Sukhoruchkin, S. I.; Soroko, Z. N.

    This document is part of the Supplement containing the complete sets of data of Subvolume A `Nuclei with Z = 1 - 54' of Volume 22 `Nuclear Binding Energies and Atomic Masses' of Landolt-Börnstein - Group I `Elementary Particles, Nuclei and Atoms'. It provides atomic mass, mass excess, nuclear binding energy, nucleon separation energies, Q-values, and nucleon residual interaction parameters for atomic nuclei of the isotope Y-90 (Yttrium, atomic number Z = 39, mass number A = 90).

  13. Multi-residue analysis of 90 emerging contaminants in liquid and solid environmental matrices by ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Petrie, Bruce; Youdan, Jane; Barden, Ruth; Kasprzyk-Hordern, Barbara

    2016-01-29

    Reported herein is new analytical methodology for the determination of 90 emerging contaminants (ECs) in liquid environmental matrices (crude wastewater, final effluent and river water). The application of a novel buffer, ammonium fluoride improved signal response for several ECs determined in negative ionisation mode. Most notably the sensitivity of steroid estrogens was improved by 4-5 times in environmental extracts. Method recoveries ranged from 40 to 152% in all matrices and method quantitation limits (MQLs) achieved were MQL in liquid environmental samples and digested sludge, respectively. To date, this is the most comprehensive multi-residue analytical method reported in the literature for the determination of ECs in both liquid and solid environmental matrices. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

  14. Multi-residue method for the determination of organochlorine pesticides in fish feed based on a cleanup approach followed by gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Nardelli, Valeria; dell'Oro, Daniela; Palermo, Carmen; Centonze, Diego

    2010-07-23

    A multi-residue method for the determination of organochlorine pesticides in fish feed samples was developed and optimized. The method is based on a cleanup step of the extracted fat, carried out by liquid-liquid extraction on diatomaceous earth cartridge with n-hexane/acetonitrile (80/20, v/v) followed by solid phase extraction (SPE) with silica gel-SCX cartridge, before the identification and quantification of the residues by gas chromatography-triple quadrupole tandem spectrometry (GC-MS/MS). Performance characteristics, such as accuracy, precision, linear range, limits of detection (LOD) and quantification (LOQ), for each pesticide were determined. Instrumental LODs ranged from 0.01 to 0.11 microg L(-1), LOQs were in the range of 0.02-0.35 microg L(-1), and calibration curves were linear (r2>0.999) in the whole range of explored concentrations (5-100 microg L(-1)). Repeatability values were in the range of 3-15%, evaluated from the relative standard deviation of six samples spiked at 100 microg kg(-1) of fat, and in compliance with that derived by the Horwitz's equation. No matrix effects or interfering substances were observed in fish feed analyses. The proposed method allowed high recoveries (92-116%) of spiked extracted fat samples at 100 microg kg(-1), and very low LODs (between 0.02 and 0.63 microg kg(-1)) and LOQs (between 0.05 and 2.09 microg kg(-1)) determined in fish feed samples. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  15. Residual basins

    International Nuclear Information System (INIS)

    D'Elboux, C.V.; Paiva, I.B.

    1980-01-01

    Exploration for uranium carried out over a major portion of the Rio Grande do Sul Shield has revealed a number of small residual basins developed along glacially eroded channels of pre-Permian age. Mineralization of uranium occurs in two distinct sedimentary units. The lower unit consists of rhythmites overlain by a sequence of black shales, siltstones and coal seams, while the upper one is dominated by sandstones of probable fluvial origin. (Author) [pt

  16. Development and validation of a multiclass method for the determination of antibiotic residues in honey using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    El Hawari, Khaled; Mokh, Samia; Doumyati, Samah; Al Iskandarani, Mohamad; Verdon, Eric

    2017-04-01

    A new, simple and fast method was developed for the determination of multi-class antibiotic residues in honey (sulfonamides, tetracyclines, macrolides, lincosamides and aminoglycosides). Separation and determination were carried out by LC-MS/MS. During sample preparation, various parameters affecting extraction efficiency were examined, including the type of solvent, pH, efficiencies of cleavage of N-glycosidic linkages by hydrochloric acid, ultrasonic extraction and its duration compared with shaking, along with dispersive SPE clean-up. Experiments with fortified samples demonstrated that 10 min of ultrasonic treatment with acidified methanol (HCl 2 M) followed by dispersive SPE clean-up with 50 mg PSA gave an effective sample preparation method for several classes of antibiotics in honey. Anhydroerythromycin A, erythromycin A enol ether and desmycosin were used as markers for the presence of erythromycin A and tylosin A in honey samples. The method was validated according to European Commission Decision (EC) No. 2002/657. The recoveries of analytes ranged from 85% to 111%. Repeatability and intra-laboratory reproducibility were honey test material 02270 through a FAPAS proficiency test (PT) for the determination of tetracyclines. PT results were obtained within a z-score range of ±2, proving that the validated method is suitable for routine analysis to ensure the quality of honey.

  17. Development and validation of multi-residue and multi-class method for antibacterial substances analysis in non-target feed by liquid chromatography - tandem mass spectrometry.

    Science.gov (United States)

    Patyra, Ewelina; Nebot, Carolina; Gavilán, Rosa Elvira; Cepeda, Alberto; Kwiatek, Krzysztof

    2018-03-01

    A confirmatory HPLC-MS/MS method for the determination of residues of 11 antibacterial substances from different therapeutic class (β-lactams, lincosamides, fluoroquinolones, macrolides, pleuromutilins and sulfonamides) in animal feeds has been developed. The sample preparation is based on extraction with 0.1% formic acid in acetonitrile. Separation of the analytes was performed on biphenyl column with a gradient of 0.1% formic acid in acetonitrile and 0.1% formic acid in Milli-Q water. The developed method was validated following the guidelines included in the European Union Commission Decision 2002/657/EC. Limits of detection ranging from 79.22 to 193.60 µg/kg; instrumental and analytical linearity coefficients were above 0.99 for matrix-match calibration; and relative recoveries ranging from 76.04% to 117.39%. Repeatability of the method was in the range of 2.41-19.76% (CV, %), whereas reproducibility ranged from 6.52 to 28.40% (CV %). The method shown to be efficient and precise for quantification of the 11 antibacterial substances in animal feed. The results demonstrate the feasibility of the method for routine use to monitor these substances in feed. The validated method was successfully applied to eight suspect feed samples collected from the Association of American Feed Control Officials (AFFCO) and feed manufactures from Galicia (Spain) in June and July 2017. Of these 8 non-target feeds, 5 were positive for the presence of tiamulin, tylosin and sulfadiazine.

  18. Development and validation of multi-residue analysis for tetracycline antibiotics in feed by high performance liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Patyra, Ewelina; Kwiatek, Krzysztof

    2017-09-01

    A new multi-residue method for the analysis of the tetracycline antibiotics oxytetracycline, tetracycline, chlortetracycline, and doxycycline was developed and validated for animal feed. After extraction with 0.1M Na 2 EDTA-McIlvaine buffer (pH 4), the samples were centrifuged, purified by SPE (Strata-X-CW cartridges) and analysed by HPLC-MS. Validation of the method was performed according to the guidelines indicated in European Commission Decision 2002/657/EC. The procedure was validated by spiking feed samples at three different levels (300, 1000, and 5000 µg/kg). Average recoveries for tetracyclines were in the range 79.70-98.8%, with RSD for repeatability and reproducibility in the ranges of 5.0-9.5% and 6.5-11.0%, respectively. The method was successfully validated and proved to be efficient, precise, and useful for quantification of tetracyclines in animal feed. The validated method was successfully applied to 65 suspect feed samples collected from different regions of Poland in 2015-16 and obtained from farms and feed manufactures. Of these 65 purportedly non-medicated feeds, eight (12.3%) were positive for the presence of doxycycline or chlortetracycline.

  19. Modification of Keap1 Cysteine Residues by Sulforaphane

    Science.gov (United States)

    Hu, Chenqi; Eggler, Aimee L.; Mesecar, Andrew D.; van Breemen, Richard B.

    2011-01-01

    Activation of the transcription factor NF-E2-related factor-2 (Nrf2) through modification of Kelch-like ECH-associated protein 1 (Keap1) cysteines, leading to up-regulation of the antioxidant response element (ARE), is an important mechanism of cellular defense against reactive oxygen species and xenobiotic electrophiles. Sulforaphane, occurring in cruciferous vegetables such as broccoli, is a potent natural ARE activator that functions by modifying Keap1 cysteine residues, but there are conflicting in vitro and in vivo data regarding which of these cysteine residues react. Although most biological data indicate that modification of C151 is essential for sulforaphane action, some recent studies using mass spectrometry have failed to identify C151 as a site of Keap1 sulforaphane reaction. We have reconciled these conflicting data using mass spectrometry with a revised sample preparation protocol and confirmed that C151 is indeed among the most readily modified cysteines of Keap1 by sulforaphane. Previous mass spectrometry-based studies used iodoacetamide during sample preparation to derivatize free cysteine sulfhydryl groups causing loss of sulforaphane from highly reactive and reversible cysteine residues on Keap1 including C151. By omitting iodoacetamide from the protocol and reducing sample preparation time, our mass spectrometry-based studies now confirm previous cell-based studies which showed that sulforaphane reacts with at least four cysteine residues of Keap1 including C151. PMID:21391649

  20. PhosProtect - a novel and superior compound to tag and protect phospho-groups during mass spectrometry based phospho-proteomics

    DEFF Research Database (Denmark)

    2012-01-01

    Value Proposition The PhosProtect compound alone (developed and tested, IP secured)* • protects phospho-groups during tandem mass spectrometry, thus reducing problematic neutral loss of phosphate. • provides unique phospho-tag by causing isotopic distribution patterns in MS and MS/MS data. The Phos...

  1. Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

    Science.gov (United States)

    Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

    2016-08-12

    A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Efeitos da Heterogeneidade de Variância Residual entre Grupos de Contemporâneos na Avaliação Genética de Bovinos de Corte Effects of Heterogeneity of Residual Variance among Contemporary Groups on Genetic Evaluation of Beef Cattle

    Directory of Open Access Journals (Sweden)

    Roberto Carvalheiro

    2002-07-01

    Full Text Available O objetivo deste estudo foi investigar, por meio de dados simulados, o efeito da heterogeneidade de variância residual entre grupos de contemporâneos (GC sobre as avaliações genéticas de bovinos de corte, e comparar o uso de uma avaliação genética ponderada (R¹Isigmae² em relação à avaliação que pressupõe homogeneidade de variância (R=Isigmae². A característica estudada foi ganho de peso pós-desmame corrigido para 345 dias, sendo esta simulada com variância fenotípica de 300 kg² e herdabilidade igual a 0,4. A estrutura de um conjunto real de dados foi utilizada para fornecer os GC e os pais referentes às observações de cada animal. Cinco níveis de heterogeneidade de variância residual foram considerados de forma que os componentes de variância fossem, na média, iguais aos da situação de homogeneidade de variância. Na medida em que níveis mais acentuados de heterogeneidade de variância residual foram considerados, os animais foram selecionados dos GC com maior variabilidade, especialmente com pressão de seleção intensa. Em relação à consistência de predição, os produtos e as vacas tiveram seus valores genéticos preditos mais afetados pela heterogeneidade de variância residual do que os touros. O fator de ponderação utilizado reduziu, mas não eliminou o efeito da heterogeneidade de variância. As avaliações genéticas ponderadas apresentaram resultados iguais ou superiores àqueles obtidos pelas avaliações que assumiram homogeneidade de variância. Mesmo quando não necessário, o uso de avaliações ponderadas produziu resultados não inferiores às avaliações que assumiram homogeneidade de variância.The objective of this study was to investigate, via simulated data, the effect of heterogeneity of residual variance among contemporary groups (CG on genetic evaluation of beef cattle, and to compare a weighted genetic evaluation procedure (R¹Isigmae² with one that assumes homogeneity of

  3. Artificial neural network modelling of pharmaceutical residue retention times in wastewater extracts using gradient liquid chromatography-high resolution mass spectrometry data.

    Science.gov (United States)

    Munro, Kelly; Miller, Thomas H; Martins, Claudia P B; Edge, Anthony M; Cowan, David A; Barron, Leon P

    2015-05-29

    The modelling and prediction of reversed-phase chromatographic retention time (tR) under gradient elution conditions for 166 pharmaceuticals in wastewater extracts is presented using artificial neural networks for the first time. Radial basis function, multilayer perceptron and generalised regression neural networks were investigated and a comparison of their predictive ability for model solutions discussed. For real world application, the effect of matrix complexity on tR measurements is presented. Measured tR for some compounds in influent wastewater varied by >1min in comparison to tR in model solutions. Similarly, matrix impact on artificial neural network predictive ability was addressed towards developing a more robust approach for routine screening applications. Overall, the best neural network had a predictive accuracy of <1.3min at the 75th percentile of all measured tR data in wastewater samples (<10% of the total runtime). Coefficients of determination for 30 blind test compounds in wastewater matrices lay at or above R(2)=0.92. Finally, the model was evaluated for application to the semi-targeted identification of pharmaceutical residues during a weeklong wastewater sampling campaign. The model successfully identified native compounds at a rate of 83±4% and 73±5% in influent and effluent extracts, respectively. The use of an HRMS database and the optimised ANN model was also applied to shortlisting of 37 additional compounds in wastewater. Ultimately, this research will potentially enable faster identification of emerging contaminants in the environment through more efficient post-acquisition data mining. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. CHARACTERIZATION OF A SYNTHETIC 37-RESIDUE FRAGMENT OF A MONOCLONAL-ANTIBODY AGAINST HERPES-VIRUS BY CAPILLARY ELECTROPHORESIS ELECTROSPRAY (IONSPRAY) MASS-SPECTROMETRY AND CF-252 PLASMA DESORPTION MASS-SPECTROMETRY

    NARCIS (Netherlands)

    KOSTIAINEN, R; LASONDER, E; BLOEMHOFF, W; VANVEELEN, PA; WELLING, GW; BRUINS, AP

    A peptide comprising 37 amino acids of the antigen binding site of a monoclonal antibody directed against glycoprotein D of herpes simplex virus was synthesized. The synthetic peptide and the impurities formed in the synthesis were characterized by capillary electrophoresis/ionspray mass

  5. Determination of Pesticide Residues in Honeybees using Modified QUEChERS Sample Work-Up and Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Żaneta Bargańska

    2014-03-01

    Full Text Available Increasing emissions of chemical compounds to the environment, especially of pesticides, is one of factors that may explain present honeybee colony losses. In this work, an analytical method employing liquid chromatography-tandem mass spectrometry (LC-MS/MS was optimized for the simultaneous screening of 19 pesticides which have not been yet determined in honeybee samples from northern Poland (Pomerania. The sample preparation, based on the QuEChERS method combining salting-out liquid-liquid extraction to acetonitrile and a dispersive-SPE clean-up, was adjusted to honeybee samples by adding a small amount of hexane to eliminate beeswax. The recovery of analytes ranged from 70% to 120% with relative standard deviation ≤20%. The limits of detection were in the range of 0.91–25 ng/g. A total of 19 samples of honeybees from suspected pesticide poisoning incidents were analyzed, in which 19 different pesticides were determined.

  6. Development and validation of a standardized method for the determination of morpholine residues in fruit commodities by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hengel, Matt J; Jordan, Rick; Maguire, Wesley

    2014-04-30

    An analytical method was developed for the determination of morpholine on apples and citrus. The method utilized acidified methanol extraction, centrifugation, and determination by hydrophilic interaction liquid chromatography with electrospray ionization and tandem mass spectrometry (HILIC-ESI-MS/MS). Validation of the method occurred at the Pacific Agricultural Laboratory (PAL, Portland, OR, USA) and the Trace Analytical Laboratory (TAL, UC Davis, CA, USA). Method validation recoveries from control apple, orange, lemon, and grapefruit samples ranged from 84 to 120% over three levels of fortification (0.01, 0.04, and 0.2 μg/g). The limit of quantitation (LOQ) for all commodities was 0.01 μg/g, and the calculated method detection limit (MDL) ranged from 0.0010 to 0.0040 μg/g.

  7. Label-free quantitative mass spectrometry for analysis of protein antigens in a meningococcal group B outer membrane vesicle vaccine.

    Science.gov (United States)

    Dick, Lawrence W; Mehl, John T; Loughney, John W; Mach, Anna; Rustandi, Richard R; Ha, Sha; Zhang, Lan; Przysiecki, Craig T; Dieter, Lance; Hoang, Van M

    2015-01-01

    The development of a multivalent outer membrane vesicle (OMV) vaccine where each strain contributes multiple key protein antigens presents numerous analytical challenges. One major difficulty is the ability to accurately and specifically quantitate each antigen, especially during early development and process optimization when immunoreagents are limited or unavailable. To overcome this problem, quantitative mass spectrometry methods can be used. In place of traditional mass assays such as enzyme-linked immunosorbent assays (ELISAs), quantitative LC-MS/MS using multiple reaction monitoring (MRM) can be used during early-phase process development to measure key protein components in complex vaccines in the absence of specific immunoreagents. Multiplexed, label-free quantitative mass spectrometry methods using protein extraction by either detergent or 2-phase solvent were developed to quantitate levels of several meningococcal serogroup B protein antigens in an OMV vaccine candidate. Precision was demonstrated to be less than 15% RSD for the 2-phase extraction and less than 10% RSD for the detergent extraction method. Accuracy was 70 to 130% for the method using a 2-phase extraction and 90-110% for detergent extraction. The viability of MS-based protein quantification as a vaccine characterization method was demonstrated and advantages over traditional quantitative methods were evaluated. Implementation of these MS-based quantification methods can help to decrease the development time for complex vaccines and can provide orthogonal confirmation of results from existing antigen quantification techniques.

  8. RESIDUAL RISK ASSESSMENTS - RESIDUAL RISK ...

    Science.gov (United States)

    This source category previously subjected to a technology-based standard will be examined to determine if health or ecological risks are significant enough to warrant further regulation for Coke Ovens. These assesments utilize existing models and data bases to examine the multi-media and multi-pollutant impacts of air toxics emissions on human health and the environment. Details on the assessment process and methodologies can be found in EPA's Residual Risk Report to Congress issued in March of 1999 (see web site). To assess the health risks imposed by air toxics emissions from Coke Ovens to determine if control technology standards previously established are adequately protecting public health.

  9. Microwave-assisted extraction and determination of cyanuric acid residue in pet food samples by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Han, Chao; Zhou, Yongfang; Xia, Biqi; Zhu, Zhenou; Liu, Cuiping; Shen, Yan

    2011-02-01

    Cyanuric acid (CYA) is attracting more attention due to its potential toxicity. In the present work, microwave-assisted extraction method in combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was proposed for the determination of CYA in pet food samples. Among different solvents, diethylamine-acetonitrile-water mixture (1:5:4, v/v) was found to be the best one as the extractant due to the strong polarity of CYA in the pet food. An internal standard, (13) C(3) -labeled CYA, was used in the extractions. The separation was performed on a MERCK ZIC HILIC column (150 mm × 2.1 mm id, 5 μm) with gradient elution of 20 mM ammonium acetate solution-acetonitrile. CYA was well retained (Rt = 5.10 min) and eluted with good peak shape. The method could respond linearly with CYA at concentrations from 1.0 to 50 ng/mL with a quantification limit of 0.25 mg/kg. The intra- and inter-day precision was less than 4.0% and the recovery of the assay was in the range of 90.4-108.1%. In the analysis of practical spiked pet food samples, the new method yielded satisfactory results. Due to its simplicity and accuracy the straightforward method is particularly suitable for routine CYA detection. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Application of high-performance liquid chromatography-tandem mass spectrometry with a quadrupole/linear ion trap instrument for the analysis of pesticide residues in olive oil.

    Science.gov (United States)

    Hernando, M D; Ferrer, C; Ulaszewska, M; García-Reyes, J F; Molina-Díaz, A; Fernández-Alba, A R

    2007-11-01

    This article describes the development of an enhanced liquid chromatography-mass spectrometry (LC-MS) method for the analysis of pesticides in olive oil. One hundred pesticides belonging to different classes and that are currently used in agriculture have been included in this method. The LC-MS method was developed using a hybrid quadrupole/linear ion trap (QqQ(LIT)) analyzer. Key features of this technique are the rapid scan acquisition times, high specificity and high sensitivity it enables when the multiple reaction monitoring (MRM) mode or the linear ion-trap operational mode is employed. The application of 5 ms dwell times using a linearly accelerating (LINAC) high-pressure collision cell enabled the analysis of a high number of pesticides, with enough data points acquired for optimal peak definition in MRM operation mode and for satisfactory quantitative determinations to be made. The method quantifies over a linear dynamic range of LOQs (0.03-10 microg kg(-1)) up to 500 microg kg(-1). Matrix effects were evaluated by comparing the slopes of matrix-matched and solvent-based calibration curves. Weak suppression or enhancement of signals was observed (ion (EPI) and MS3 were developed.

  11. Multi-residue analysis method for analysis of pharmaceuticals using liquid chromatography-time of flight/mass spectrometry (LC-TOF/MS) in water sample

    Science.gov (United States)

    Al-Qaim, Fouad Fadhil; Abdullah, Md Pauzi; Othman, Mohamed Rozali

    2013-11-01

    In this work, a developed method using solid - phase extraction (SPE) followed by liquid chromatography - time of flight mass spectrometry (LC-ESI-TOF/MS) was developed and validated for quantification and confirmation of eleven pharmaceuticals with different therapeutic classes in water samples, Malaysia. These compounds are caffeine (CAF), prazosin (PRZ), enalapril (ENL), carbamazepine (CBZ), nifedipine (NFD), levonorgestrel (LNG), simvastatin (SMV), hydrochlorothiazide (HYD), gliclazide (GLIC), diclofenac-Na (DIC-Na) and mefenamic acid (MEF). LC was performed on a Dionex Ultimate 3000/LC 09115047 (USA) system. Chromatography was performed on a Thermo Scientific C18 (250 mm × 2.1 mm, i.d.: 5μm) column. Several parameters were optimised such as; mobile phase, gradient elution, collision energy and solvent elution for extraction of compounds from water. The recoveries obtained ranged from 30-148 % in river water. Five pharmaceutical compounds were detected in the surface water samples: caffeine, prazosin, enalpril, diclofenac-Na and mefenamic acid. The developed method is precise and accepted recoveries were got. In addition, this method is suitable to identify and quantify trace concentrations of pharmaceuticals in surface water.

  12. Development of a multi-residue method for fast screening and confirmation of 20 prohibited veterinary drugs in feedstuffs by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Gui-Jun; Fang, Bing-Hu; Liu, Ya-Hong; Wang, Xu-Feng; Xu, Li-Xiao; Zhang, Ya-Ping; He, Li-Min

    2013-10-01

    A simple multiresidue method was developed for detecting and quantifying twenty analytes from 5 classes of prohibited veterinary drugs (β-agonists (9), anabolic hormones (4), quinoxalines (4), tranquilizers (1), cyproheptadine, and clonidine in animal feeds using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach. Feed samples were extracted by ultrasonic-assisted extraction with a mixture of methanol-acetonitrile (50:50, v/v), followed by a cleanup using a dispersive solid-phase extraction with PSA (primary secondary amine). Target compounds were separated and determined by a liquid chromatography tandem quadrupole mass spectrometer operating in positive electrospray ionization mode, using multiple reaction monitoring (MRM). The recoveries of these compounds were between 56.7% and 103% at three spiked levels. The repeatability was lower than 10%, whereas reproducibility was no more than 15% except for nandrolone (17% at 10μgkg(-1)) and diazepam (19% at 10μgkg(-1)). Decision limits (CCαs) and detection capabilities (CCβs) ranged from 0.42 to 5.74μgkg(-1) and 5.70-9.81μgkg(-1), respectively. The method was successfully applied to screening of real samples obtained from local feed markets and confirmation of the suspected target analytes. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Low-level Determination of Residual Methyl Methane Sulfonate and Ethyl Methane Sulfonate in Pharmaceuticals by Gas Chromatography with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    M. Sarat

    2010-01-01

    Full Text Available A capillary gas chromatographic method using mass spectrometric detection was developed and validated for the trace analysis (ppm level of methyl methane sulfonate and ethyl methane sulfonate in pharmaceutical drug substances. The method utilizes a capillary column (DB-624 with 6% cyanopropyl phenyl and 94% dimethyl polysiloxane stationary phase. A dissolve-and-injection approach was adopted for sample introduction in a split less mode. Mixture of (80:20 ratio of methanol and chloroform was used as a diluent or sample solvent. A limit of detection of about 0.17 μg/g (0.17 ppm for methyl methane sulfonate and 0.18 μg/g (0.18 ppm for ethyl methane sulfonate were achieved and limit of quantitation of 0.52 μg/g (0.52 ppm for methyl methane sulfonate and 0.54 μg/g (0.54 ppm for ethyl methane sulfonate were achieved for alkyl sulfonates in drug substance samples.

  14. Pesticides residues in water treatment plant sludge: validation of analytical methodology using liquid chromatography coupled to Tandem mass spectrometry (LC-MS/MS)

    International Nuclear Information System (INIS)

    Moracci, Luiz Fernando Soares

    2008-01-01

    The evolving scenario of Brazilian agriculture brings benefits to the population and demands technological advances to this field. Constantly, new pesticides are introduced encouraging scientific studies with the aim of determine and evaluate impacts on the population and on environment. In this work, the evaluated sample was the sludge resulted from water treatment plant located in the Vale do Ribeira, Sao Paulo, Brazil. The technique used was the reversed phase liquid chromatography coupled to electrospray ionization tandem mass spectrometry. Compounds were previously liquid extracted from the matrix. The development of the methodology demanded data processing in order to be transformed into reliable information. The processes involved concepts of validation of chemical analysis. The evaluated parameters were selectivity, linearity, range, sensitivity, accuracy, precision, limit of detection, limit of quantification and robustness. The obtained qualitative and quantitative results were statistically treated and presented. The developed and validated methodology is simple. As results, even exploring the sensitivity of the analytical technique, the work compounds were not detected in the sludge of the WTP. One can explain that these compounds can be present in a very low concentration, can be degraded under the conditions of the water treatment process or are not completely retained by the WTP. (author)

  15. Identification of ortho-Substituted Benzoic Acid/Ester Derivatives via the Gas-Phase Neighboring Group Participation Effect in (+)-ESI High Resolution Mass Spectrometry

    Science.gov (United States)

    Blincoe, William D.; Rodriguez-Granillo, Agustina; Saurí, Josep; Pierson, Nicholas A.; Joyce, Leo A.; Mangion, Ian; Sheng, Huaming

    2018-02-01

    Benzoic acid/ester/amide derivatives are common moieties in pharmaceutical compounds and present a challenge in positional isomer identification by traditional tandem mass spectrometric analysis. A method is presented for exploiting the gas-phase neighboring group participation (NGP) effect to differentiate ortho-substituted benzoic acid/ester derivatives with high resolution mass spectrometry (HRMS1). Significant water/alcohol loss (>30% abundance in MS1 spectra) was observed for ortho-substituted nucleophilic groups; these fragment peaks are not observable for the corresponding para and meta-substituted analogs. Experiments were also extended to the analysis of two intermediates in the synthesis of suvorexant (Belsomra) with additional analysis conducted with nuclear magnetic resonance (NMR), density functional theory (DFT), and ion mobility spectrometry-mass spectrometry (IMS-MS) studies. Significant water/alcohol loss was also observed for 1-substituted 1, 2, 3-triazoles but not for the isomeric 2-substituted 1, 2, 3-triazole analogs. IMS-MS, NMR, and DFT studies were conducted to show that the preferred orientation of the 2-substituted triazole rotamer was away from the electrophilic center of the reaction, whereas the 1-subtituted triazole was oriented in close proximity to the center. Abundance of NGP product was determined to be a product of three factors: (1) proton affinity of the nucleophilic group; (2) steric impact of the nucleophile; and (3) proximity of the nucleophile to carboxylic acid/ester functional groups. [Figure not available: see fulltext.

  16. Competition between counterions and active protein sites to bind bisquaternary ammonium groups. A combined mass spectrometry and quantum chemistry model study

    Science.gov (United States)

    Pashynska, V.; Boryak, O.; Kosevich, M. V.; Stepanian, S.; Adamowicz, L.

    2010-06-01

    A model study of the interaction between biologically active bisquaternary ammonium salts and their molecular targets in living systems is urgently needed to elucidate the molecular mechanisms involved in the interactions between these compounds. To address this need a combined experimental-computational study of the interaction of two tetramethylammonium cations (modeling two quaternary groups) with the chlorine anion and with the deprotonated 2,5-dihydroxybenzoic acid (modeling a carboxylic group and an aromatic ring of side radicals of proteins) has been performed. Fast atom bombardment mass spectrometry method and DFT/B3LYP/6-31++G** and MP2/6-31++G** calculations have been employed in the study. Stable noncovalent complexes with different ratios of the tetramethylammonium cations and chlorine anions or deprotonated 2,5-dihydroxybenzoic acid anions were registered in the mass spectra of tetramethylammonium chloride and 2,5-dihydroxybenzoic acid mixture. This finding shows that the organic and inorganic anions compete to bind tetramethylammonium in the studied system. The theoretically determined stabilities of the noncovalent complexes were compared with the relative stabilities evaluated from the mass spectrometric measurements. The results of the study allow us to elucidate the competing interactions that exist between quaternary groups with inorganic counterions or with active groups of molecular protein targets.

  17. Evaluation of Teaching Methods in Mass CPCR Training in Different Groups of the Society, an Observational Study.

    Science.gov (United States)

    Hasani, Hamed; Bahrami, Mojtaba; Malekpour, Abdorrasoul; Dehghani, Mohammadreza; Allahyary, Elaheh; Amini, Mitra; Abdorahimi, Mehdi; khani, Sara; Kalantari Meibodi, Mohammad; Kojuri, Javad

    2015-05-01

    To determine the efficacy of different methods of cardiopulmonary resuscitation (CPCR) training in 3 different groups of the society. In a prospective and observational study of 2000 individuals in 3 different groups including G1, G2, and G3 4 different protocols of CPCR training were applied and their efficacy was compared between the groups. Also, 12 months after the study course, 460 participants from 3 groups were asked to take apart in a theoretical and practical examination to evaluate the long-term efficacy of the 4 protocols. Among 2000 individuals took a parted in the study, 950 (47.5%) were G1, 600 (30%) were G2, and 450 (22.5%) were G3. G1 in 4 groups were 2.37 and 2.65 times more successful in pretest theoretical and 2.61 and 18.20 times more successful in practical examinations compared with G2 and G3 and gained highest improvement in CPCR skills. Other groups also showed significantly improved CPCR skills. Comparison of different methods of CPCR learning showed that the workshop using interactive lecture as well as human model, educational film, and reference CPCR book has the highest efficacy in all groups. This protocol of CPCR training showed more efficacy in long-term postdelayed evaluation. On the contrary, medical students had better long-term outcomes from the course. Although G1 and G2 obtained better results in learning CPCR skills, in G3 also the theoretical and practical knowledge were improved significantly. This course increased confidence for doing CPCR in all groups of the study. Considering that the most of the bystanders at emergency states are general population, training this group of the society and increasing their confidence about performing CPCR can be so effective and lifesaving at emergency states. (Clinical trial. Gov registration: NCT02120573).

  18. BANYAN. V. A SYSTEMATIC ALL-SKY SURVEY FOR NEW VERY LATE-TYPE LOW-MASS STARS AND BROWN DWARFS IN NEARBY YOUNG MOVING GROUPS

    Energy Technology Data Exchange (ETDEWEB)

    Gagné, Jonathan; Lafrenière, David; Doyon, René; Malo, Lison; Artigau, Étienne [Département de Physique, Université de Montréal, C.P. 6128 Succ. Centre-ville, Montréal, QC H3C 3J7 (Canada)

    2015-01-10

    We present the BANYAN All-Sky Survey (BASS) catalog, consisting of 228 new late-type (M4-L6) candidate members of nearby young moving groups (YMGs) with an expected false-positive rate of ∼13%. This sample includes 79 new candidate young brown dwarfs and 22 planetary-mass objects. These candidates were identified through the first systematic all-sky survey for late-type low-mass stars and brown dwarfs in YMGs. We cross-matched the Two Micron All Sky Survey and AllWISE catalogs outside of the galactic plane to build a sample of 98,970 potential ≥M5 dwarfs in the solar neighborhood and calculated their proper motions with typical precisions of 5-15 mas yr{sup –1}. We selected highly probable candidate members of several YMGs from this sample using the Bayesian Analysis for Nearby Young AssociatioNs II tool (BANYAN II). We used the most probable statistical distances inferred from BANYAN II to estimate the spectral type and mass of these candidate YMG members. We used this unique sample to show tentative signs of mass segregation in the AB Doradus moving group and the Tucana-Horologium and Columba associations. The BASS sample has already been successful in identifying several new young brown dwarfs in earlier publications, and will be of great interest in studying the initial mass function of YMGs and for the search of exoplanets by direct imaging; the input sample of potential close-by ≥M5 dwarfs will be useful to study the kinematics of low-mass stars and brown dwarfs and search for new proper motion pairs.

  19. Multi-residue analysis of eight anticoagulant rodenticides in animal plasma and liver using liquid chromatography combined with heated electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Vandenbroucke, Virginie; Desmet, Noël; De Backer, Patrick; Croubels, Siska

    2008-06-15

    A sensitive method for the simultaneous quantification of eight anticoagulant rodenticides (brodifacoum, bromadiolone, chlorophacinone, coumatetralyl, difenacoum, difethialone, flocoumafen and warfarin) in animal plasma and liver using liquid chromatography combined with heated electrospray ionization tandem mass spectrometry (LC-HESI-MS/MS) is described. The sample preparation includes a liquid-liquid extraction with acetone. The compound 7-acetoxy-6-(2,3-dibromopropyl)-4,8-dimethylcoumarin is used as an internal standard. Chromatographic separation was achieved using a Nucleodur C18 gravity column. Good linearity was observed up to 750 ng mL(-1) for chlorophacinone and up to 500 ng mL(-1) for the other compounds in plasma. In liver, good linearity was seen up to 500 ng g(-1) for brodifacoum, chlorophacinone, difenacoum and difethialone and up to 750 ng g(-1) for the other compounds. Depending on the compound, a level of 1 or 5 ng mL(-1) could be quantified fulfilling the criteria for accuracy and precision and was therefore set as limit of quantification of the method in plasma. In liver, the limit of quantification was set at 250 ng g(-1) for coumatetralyl and warfarin and at 100 ng g(-1) for the other compounds. In plasma, the limit of detection varied from 0.07 ng mL(-1) for flocoumafen to 3.21 ng mL(-1) for brodifacoum. In liver, the limit of detection varied from 0.37 ng g(-1) for warfarin to 4.64 ng g(-1) for chlorophacinone. The method was shown to be of use in a pharmacokinetic study after single oral administration to mice and in the confirmation of suspected poisoning cases in domestic animals.

  20. Validation of an ultra-high-performance liquid chromatography-tandem mass spectrometry method to quantify illicit drug and pharmaceutical residues in wastewater using accuracy profile approach.

    Science.gov (United States)

    Hubert, Cécile; Roosen, Martin; Levi, Yves; Karolak, Sara

    2017-06-02

    The analysis of biomarkers in wastewater has become a common approach to assess community behavior. This method is an interesting way to estimate illicit drug consumption in a given population: by using a back calculation method, it is therefore possible to quantify the amount of a specific drug used in a community and to assess the consumption variation at different times and locations. Such a method needs reliable analytical data since the determination of a concentration in the ngL -1 range in a complex matrix is difficult and not easily reproducible. The best analytical method is liquid chromatography - mass spectrometry coupling after solid-phase extraction or on-line pre-concentration. Quality criteria are not specially defined for this kind of determination. In this context, it was decided to develop an UHPLC-MS/MS method to analyze 10 illicit drugs and pharmaceuticals in wastewater treatment plant influent or effluent using a pre-concentration on-line system. A validation process was then carried out using the accuracy profile concept as an innovative tool to estimate the probability of getting prospective results within specified acceptance limits. Influent and effluent samples were spiked with known amounts of the 10 compounds and analyzed three times a day for three days in order to estimate intra-day and inter-day variations. The matrix effect was estimated for each compound. The developed method can provide at least 80% of results within ±25% limits except for compounds that are degraded in influent. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Targeted screening and safety evaluation of 276 agrochemical residues in raisins using buffered ethyl acetate extraction and liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Shabeer, T P Ahammed; Jadhav, Manjusha; Girame, Rushali; Hingmire, Sandip; Bhongale, Aarti; Pudale, Anjali; Banerjee, Kaushik

    2017-10-01

    A buffered ethyl acetate extraction method was optimized and validated in raisin matrix to monitor 276 pesticides by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The final method involved homogenization of raisinsalong with water 1:1 raisins: water followed by extraction using ethyl acetate (10 mL/10 g raisins homogenate in presence of 0.1 mL acetic acid, 0.5 g sodium acetate and 10 g sodium sulfate, and cleanup by dispersive solid phase extraction with primary secondary amine sorbent (25 mg/5 mL extract). 276 pesticides were estimated within 20 min of chromatographic run time by retention time dependent 'scheduled multiple reaction monitoring' (sMRM) by LC-MS/MS.The method was validated as per European guideline, DG-SANTE/11945/2015, at 2, 10, and 25 ng/g spiking levels where the method precision in terms of repeatability was <15% at 10 ng/g for 93.8% of the compounds. The Limit of quantification (LOQ) ranged between 0.01 and 10 ng/g with recoveries 70-120% with ≤20% RSD for 93.5% of compounds at regulatory default MRL of 10 ng/g. The matrix induced signal suppressions or enhancement were moderate (60-130% accuracy against solvent standard) for 85% compounds in white raisins and 67% compounds in black raisins. The method was successfully applied for screening of 94 market samples of raisins for the target analytes. The dietaryexposures calculated against the average concentrations detected were wellbelow the maximum permissible intake (MPI) values and the collected raisin samples were considered safe for human consumption without any acute toxicity hazard. Copyright © 2017 Elsevier Ltd. All rights reserved.

  2. Multi-residue analysis of legacy POPs and emerging organic contaminants in Singapore's coastal waters using gas chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Hui; Bayen, Stéphane; Kelly, Barry C

    2015-08-01

    A gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) based method was developed for determination of 86 hydrophobic organic compounds in seawater. Solid-phase extraction (SPE) was employed for sequestration of target analytes in the dissolved phase. Ultrasound assisted extraction (UAE) and florisil chromatography were utilized for determination of concentrations in suspended sediments (particulate phase). The target compounds included multi-class hydrophobic contaminants with a wide range of physical-chemical properties. This list includes several polycyclic and nitro-aromatic musks, brominated and chlorinated flame retardants, methyl triclosan, chlorobenzenes, organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs). Spiked MilliQ water and seawater samples were used to evaluate the method performance. Analyte recoveries were generally good, with the exception of some of the more volatile target analytes (chlorobenzenes and bromobenzenes). The method is very sensitive, with method detection limits typically in the low parts per quadrillion (ppq) range. Analysis of 51 field-collected seawater samples (dissolved and particulate-bound phases) from four distinct coastal sites around Singapore showed trace detection of several polychlorinated biphenyl congeners and other legacy POPs, as well as several current-use emerging organic contaminants (EOCs). Polycyclic and nitro-aromatic musks, bromobenzenes, dechlorane plus isomers (syn-DP, anti-DP) and methyl triclosan were frequently detected at appreciable levels (2-20,000pgL(-1)). The observed concentrations of the monitored contaminants in Singapore's marine environment were generally comparable to previously reported levels in other coastal marine systems. To our knowledge, these are the first measurements of these emerging contaminants of concern in Singapore or Southeast Asia. The developed method may prove beneficial for future environmental monitoring of hydrophobic organic contaminants

  3. Analyses of organochlorine pesticides residues in eels (Anguilla anguilla from Lake Garda using Gas chromatography coupled with Tandem Mass Spectrometry (GC-MS/MS.

    Directory of Open Access Journals (Sweden)

    Giuseppe Federico Labella

    2017-05-01

    Full Text Available Lake Garda is located in Insubria region, that is known for being the most populated and industrialized area of Italy (Camusso et al., 2001. Therefore, the Lake water, and also the fish species present, could be affected by environmental contamination.  European eel (Anguilla anguilla are considered as suitable matrix for biomonitoring environmental contaminants in European water (Belpaire et al., 2007, being widespread in many European waters and highly contaminated by lipophilic compounds, due to the high lipid content (up to 40% (Larsson et al., 1991. Moreover, eel is an edible species (its farming currently supplies approximately 45,000 tons/year (Nielsen et al., 2008, so it also represents a public health issue. Based on these considerations, the aim of this study was to evaluate the occurrence of fourteen organochlorine pesticides (OCs in forty-five eels (Anguilla anguilla from Lake Garda, using Accelerated Solvent Extraction (ASE procedure for the analytes extraction and Gas chromatography coupled with Tandem Mass Spectrometry (GC-MS/MS for the analysis of OCs. GC-MS/MS analysis was developed and validated according to the SANTE/11945/2015 guidelines.  Uncontaminated eel sample (previously checked for the presence of OCs and considered blank with a concentration of compounds < Limit of Detection were used for all procedure's optimization steps. For all the OCs analysed, satisfactory results were achieved. Regarding eel samples, several pesticides were detected, but DDTs (DDT and its metabolites were found with the highest prevalence (92 %. The concentration rage was from not detected (n.d. to 19000 ng g-1. Although DDTs levels in the environment are declining (Albaiges et al., 2011, they continue to bioaccumulate in tissues of human and animal and biomagnify in food chains.

  4. Gas chromatography and isotope ratio mass spectrometry of Pinot Noir wine volatile compounds (δ13C) and solid residues (δ13C, δ15N) for the reassessment of vineyard water-status.

    Science.gov (United States)

    Spangenberg, Jorge E; Vogiatzaki, Maria; Zufferey, Vivian

    2017-09-29

    This paper describes a novel approach to reassess the water status in vineyards based on compound-specific isotope analysis (CSIA) of wine volatile organic compounds (δ 13 C VOC/VPDB ) and bulk carbon and nitrogen isotopes, and the C/N molar ratios of the wine solid residues (δ 13 C SR/VPDB , δ 15 N SR/Air-N2 ). These analyses link gas chromatography/combustion and elemental analysis to isotope ratio mass spectrometry (GC/C/IRMS, EA/IRMS). Field-grown cultivars of Pinot Noir grapevines were exposed during six growing seasons (2009-2014) to controlled soil water availability, while maintaining identical the other environmental variables and agricultural techniques. Wines were produced from the grapes by the same oenological protocol. This permitted for the assessment of the effects in the biochemistry of wines solely induced by the changes in the plant-soil water status. This mimicked the more recurrent and prolonged periods of soil water deficiency due to climate changes. Water stress in grapevine was assessed by the measurement of the predawn leaf water potential (Ψ pd ) and the stable carbon isotope composition of the berry sugars during harvest (must sugars). For quantitation purposes and the normalization of the measured stable carbon isotope ratios of the VOCs, the wine samples were spiked with three standard compounds with known concentration and δ 13 C VPDB values. VOCs were extracted by liquid-liquid extraction and analyzed by gas chromatography/flame ionization detection (GC/FID), gas chromatography/mass spectrometry (GC/MS), and GC/C/IRMS. δ 13 C values were obtained for eighteen VOCs. The solid residues were obtained by freeze-drying wine aliquots and were analyzed for their C and N content and isotope composition by EA/IRMS. All the isotopic ratios (δ 13 C SR , δ 15 N SR , δ 13 C VOC ) are highly correlated with the Ψ pd values, indicating that the proposed gas chromatography and isotope ratio mass spectrometry approach is a useful tool to

  5. Quantification in mass units of group 1 grass allergens by a monoclonal antibody-based sandwich ELISA.

    Science.gov (United States)

    Arilla, M C; Ibarrola, I; Eraso, E; Aguirre, M; Martínez, A; Asturias, J A

    2001-08-01

    Grass pollen extracts currently used for allergy diagnosis and immunotherapy are a complex mixture of proteins of which only a few have allergenic activity. Lol p 1 is one of the most important allergens in grass pollen extracts. To develop a two-site enzyme-linked immunosorbent assay for the quantification of Lol p 1 and other group 1 allergens from grass species, and to assess its suitability for quantifying this group of allergens. Balb/c mice immunized with recombinant Lol p 1 were used for the production of monoclonal antibodies. Screening of hybridomas was performed by direct ELISA, and selected monoclonal antibodies were immobilized on ELISA plates and incubated with samples containing group 1 allergens. Bound allergens were detected by a combination of biotinylated Lol p 1-specific monoclonal antibody and peroxidase-streptavidin conjugate. The assay is based on three Lol p 1-specific monoclonal antibodies with different epitope specificities. The optimized ELISA measured Lol p 1 concentrations ranging from 125 to 1000 ng/mL and could quantify group 1 allergen from grass species belonging to the Pooidea subfamily. The assay does not depend on anti-sera production or availability of human sera and thus reactives can be produced in unlimited amounts. This sensitive and specific Lol p 1 assay will be helpful both for quantifying the group 1 allergen content of Pooideae pollen extracts intended for clinical use and for studying cross-reactivities among pollen extracts.

  6. Comparison of gait velocity and center of mass during square and semicircular turning gaits between groups of elderly people with differing visual acuity

    OpenAIRE

    Shin, Sun-shil; An, Duk-hyun; Yoo, Won-gyu

    2015-01-01

    [Purpose] The purpose of this study was to investigate gait velocity and center of mass (COM) during square and semicircular turning gaits between two groups of elderly people with differing visual acuity. [Subjects] Twenty elderly Korean women who could walk independently and who lived in the community were recruited. [Methods] We measured gait velocity and COM using an accelerometer during two different turning gaits. [Results] The velocity during square and semicircular turning gaits of pa...

  7. Fat-Free Mass and Fasting Glucose Values in Patients with and without Statin Therapy Assigned to Age Groups between 75 Years

    Directory of Open Access Journals (Sweden)

    Alexander Dzien

    2013-02-01

    Full Text Available Objective: The aging-associated changes in body composition result in an increased cardiometabolic risk. A tremendous reduction of cardiovascular morbidity and mortality can be obtained by statin therapy. Statins are well tolerated, with myopathy as the most serious negative side effect. Some recently published studies indicate that the incidence of type 2 diabetes might be increased during intensified statin therapy. The aim of our study was to investigate whether statin therapy has an influence on the aging-associated changes in fat-free mass (FFM. Methods: A total of 3,280 persons attending a medical outdoor center between January 2005 and July 2011 were assigned to 3 age groups from 75 years. Clinical data, body mass index (BMI, and body composition were evaluated in the different age groups in patients with and without statin therapy. To analyze the impact of statin use on FFM, we regressed a patient's FFM on an interaction term between statin use and age and other control variables. Results: Aging was associated with a decrease in BMI and FFM, while fat mass continuously increased up to the age of >75 years. This was paralleled by a continuous increase in fasting glucose levels in patients with and without statin therapy. The loss of FFM between the age group 75 years was more pronounced in statin-treated patients (10.88% than in non-statin users (8.47%. Creatine phosphokinase values revealed a decrease of 7.77 U/l between the age groups 75 years in non-statin users and of 14.75 U/l in statin users. Statistical analysis indicated that the effect of statin therapy on FFM is more pronounced in younger than in older patients. Conclusions: Patients under statin therapy seem to be more vulnerable to the aging-associated lowering of FFM. Diagnostic procedures and interventions to prevent a loss of muscle mass might be of particular advantage in elderly patients under statin therapy.

  8. Matrix-Assisted Laser Desorption Ionization Mass Spectrometry of Compounds Containing Carboxyl Groups Using CdTe and CuO Nanoparticles

    OpenAIRE

    Megumi Sakurai; Taro Sato; Jiawei Xu; Soichi Sato; Tatsuya Fujino

    2018-01-01

    Matrix-assisted laser desorption ionization mass spectrometry of compounds containing carboxyl groups was carried out by using semiconductor nanoparticles (CdTe and CuO) as the matrix. Salicylic acid (Sal), glucuronic acid (Glu), ibuprofen (Ibu), and tyrosine (Tyr) were ionized as deprotonated species (carboxylate anions) by using electrons ejected from CdTe after the photoexcitation. When CuO was used as the matrix, the peak intensity of Tyr became high compared with that obtained with CdTe....

  9. Intraoperative neuromuscular monitoring site and residual paralysis.

    Science.gov (United States)

    Thilen, Stephan R; Hansen, Bradley E; Ramaiah, Ramesh; Kent, Christopher D; Treggiari, Miriam M; Bhananker, Sanjay M

    2012-11-01

    Residual paralysis is common after general anesthesia involving administration of neuromuscular blocking drugs (NMBDs). Management of NMBDs and reversal is frequently guided by train-of-four (TOF) monitoring. We hypothesized that monitoring of eye muscles is associated with more frequent residual paralysis than monitoring at the adductor pollicis. This prospective cohort study enrolled 180 patients scheduled for elective surgery with anticipated use of NMBDs. Collected variables included monitoring site, age, gender, weight, body mass index, American Society of Anesthesiologists physical status class, type and duration of surgery, type of NMBDs, last and total dose administered, TOF count at time of reversal, dose of neostigmine, and time interval between last dose of NMBDs to quantitative measurement. Upon postanesthesia care unit admission, we measured TOF ratios by acceleromyography at the adductor pollicis. Residual paralysis was defined as a TOF ratio less than 90%. Multivariable logistic regression was used to account for unbalances between the two groups and to adjust for covariates. 150 patients received NMBDs and were included in the analysis. Patients with intraoperative TOF monitoring of eye muscles had significantly greater incidence of residual paralysis than patients monitored at the adductor pollicis (P paralysis was observed in 51/99 (52%) and 11/51 (22%) of patients, respectively. The crude odds ratio was 3.9 (95% CI: 1.8-8.4), and the adjusted odds ratio was 5.5 (95% CI: 2.1-14.5). Patients having qualitative TOF monitoring of eye muscles had a greater than 5-fold higher risk of postoperative residual paralysis than those monitored at the adductor pollicis.

  10. Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid-liquid extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Pirard, C; Widart, J; Nguyen, B K; Deleuze, C; Heudt, L; Haubruge, E; De Pauw, E; Focant, J-F

    2007-06-08

    We report on the development and validation under ISO 17025 criteria of a multi-residue confirmatory method to identify and quantify 17 widely chemically different pesticides (insecticides: Carbofuran, Methiocarb, Pirimicarb, Dimethoate, Fipronil, Imidacloprid; herbicides: Amidosulfuron, Rimsulfuron, Atrazine, Simazine, Chloroturon, Linuron, Isoxaflutole, Metosulam; fungicides: Diethofencarb) and 2 metabolites (Methiocarb sulfoxide and 2-Hydroxytertbutylazine) in honey. This method is based on an on-column liquid-liquid extraction (OCLLE) using diatomaceous earth as inert solid support and liquid chromatography (LC) coupled to mass spectrometry (MS) operating in tandem mode (MS/MS). Method specificity is ensured by checking retention time and theoretical ratio between two transitions from a single precursor ion. Linearity is demonstrated all along the range of concentration that was investigated, from 0.1 to 20 ng g(-1) raw honey, with correlation coefficients ranging from 0.921 to 0.999, depending on chemicals. Recovery rates obtained on home-made quality control samples are between 71 and 90%, well above the range defined by the EC/657/2002 document, but in the range we had fixed to ensure proper quantification, as levels found in real samples could not be corrected for recovery rates. Reproducibility is found to be between 8 and 27%. Calculated CCalpha and CCbeta (0.0002-0.943 ng g(-1) for CCalpha, and 0.0002-1.232 ng g(-1) for CCbeta) show the good sensitivity attained by this multi-residue analytical method. The robustness of the method has been tested in analyzing more than 100 raw honey samples collected from different areas in Belgium, as well as some wax and bee samples, with a slightly adapted procedure.

  11. Development of multi-residue method for the determination of pesticides in cereal matrices by isotopic dilution associated to liquid chromatography coupled to tandem mass spectrometry after pressurized liquid extraction

    International Nuclear Information System (INIS)

    El Mrabet, Khadija

    2008-01-01

    Pesticides are nowadays considered as toxic for human health. The maximal residues levels authorized in water and foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this thesis was to develop a multi-residue method for the determination of pesticides by isotopic dilution associated to liquid chromatography (LC) coupled with tandem mass spectrometry (MS 2 ) after pressurized liquid extraction. In a first step, an analysis method of phenyl-ureas and triazines in groundwater by isotopic dilution associated to LC/MS 2 after solid phase extraction has been developed. The method has been validated and evaluated by participating to an inter-laboratory study. Concerning cereals, an extraction method of pesticides associated to an analysis by LC/MS 2 has been developed for thirty-eight pesticides representative of twenty-six chemicals families and fourteen labeled compounds in wheat. The analysis has been carried out in reversed phase chromatography. Separation and detection conditions have been optimized. A global analytical protocol consisting of a pressurized liquid extraction step using acetonitrile at 100 deg. C and at 100 bars and followed by purification step of the resulting extract on a polymeric sorbent was developed. The developed method enables to extract thirty-eight pesticides and fourteen labeled compounds from wheat with recovery yield about 85% (RSD =4%, n=3). Moreover, the results show that the application of isotopic dilution can be complex. Although some improvements need to be added regarding experimentation of aged matrices or contaminated samples, the potential of the method has been demonstrated. (author) [fr

  12. Residue analysis of four diacylhydrazine insecticides in fruits and vegetables by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method using ultra-performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Liu, Xingang; Xu, Jun; Dong, Fengshou; Li, Yuanbo; Song, Wenchen; Zheng, Yongquan

    2011-08-01

    The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI-) for chromafenozide. The limits of detection were below 0.6 μg kg(-1), while the limit of quantification did not exceed 2 μg kg(-1) in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1 mg kg(-1)). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4-13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.

  13. Development of a multi-residue method for the determination of pesticides in cereals and dry animal feed using gas chromatography-tandem quadrupole mass spectrometry II. Improvement and extension to new analytes.

    Science.gov (United States)

    Walorczyk, Stanisław

    2008-10-24

    This paper describes the extension and re-validation of a previously published multi-residue method to currently 140 pesticides and 4 pesticide degradation products in cereals and feedingstuffs. The pesticides were extracted using buffered QuEChERS ("quick, easy, cheap, rugged, effective and safe") method and then cleaned up using dispersive solid-phase extraction with Bondesil PSA and C18 sorbents, and optionally by a freezing-out clean-up step. The final extracts were analyzed in a single injection gas chromatographic-tandem quadrupole mass spectrometric (GC-MS/MS) acquisition method. A high degree of confidence was achieved by entering two multiple reaction monitoring transitions per compound. In this way, quantification of analytical results and unequivocal identification of pesticide residues in compliance with the recent European Union criteria could be done in a single analysis. Thorough optimization of the GC-MS/MS acquisition conditions and application of an effective clean-up procedure has resulted in a remarkable enhancement of the validation parameters. The linearity of the calibration curves was excellent in matrix-matched standards, and yielded the coefficients of determination (R(2))> or =0.99 for approximately 96% of the target analytes. Average recoveries of the pesticides spiked at 0.01mgkg(-1) into a feed mixture and wheat grain were in the range 70-120% with associated RSD values feed mixtures and other samples such as malt, starch and dry vegetables have been analyzed. A total of 15 different pesticides have been detected, among which pirimiphos methyl (19 cases), deltamethrin (14 cases), tolylfluanid (5 cases), dichlofluanid (5 cases), and tebuconazole (4 cases) were the most frequently encountered ones.

  14. Simultaneous detection of forbidden chemical residues in milk using dual-label time-resolved reverse competitive chemiluminescent immunoassay based on amine group functionalized surface.

    Directory of Open Access Journals (Sweden)

    Dongdong Zhang

    Full Text Available In this study, a sensitive dual-label time-resolved reverse competitive chemiluminescent immunoassay was developed for simultaneous detection of chloramphenicol (CAP and clenbuterol (CLE in milk. The strategy was performed based on the distinction of the kinetic characteristics of horseradish peroxidase (HRP and alkaline phosphatase (ALP in chemiluminesecence (CL systems and different orders of magnitude in HRP CL value for CAP and ALP CL value for CLE in the chemiluminescent immunoassay. Capture antibodies were covalently bound to the amine group functionalized chemiluminescent microtiter plate (MTP for efficient binding of detection antibodies for the enzymes labeled CAP (HRP-CAP and CLE (ALP-CLE. The CL signals were recorded at different time points by the automatic luminometers with significant distinction in the dynamic curves. When we considered the ALP CL value (about 10(5 of CLE as background for HRP CL signal value (about 10(7 of CAP, there was no interaction from ALP CL background of CLE and the differentiation of CAP and CLE can be easily achieved. The 50% inhibition concentration (IC50 values of CAP and CLE in milk samples were 0.00501 µg L(-1 and 0.0128 µg L(-1, with the ranges from 0.0003 µg L(-1 to 0.0912 µg L(-1 and from 0.00385 µg L(-1 to 0.125 µg L(-1, respectively. The developed method is more sensitive and of less duration than the commercial ELISA kits, suitable for simultaneous screening of CAP and CLE.

  15. A new stem group echinoid from the Triassic of China leads to a revised macroevolutionary history of echinoids during the end-Permian mass extinction

    Science.gov (United States)

    Thompson, Jeffrey R.; Hu, Shi-xue; Zhang, Qi-Yue; Petsios, Elizabeth; Cotton, Laura J.; Huang, Jin-Yuan; Zhou, Chang-yong; Wen, Wen; Bottjer, David J.

    2018-01-01

    The Permian-Triassic bottleneck has long been thought to have drastically altered the course of echinoid evolution, with the extinction of the entire echinoid stem group having taken place during the end-Permian mass extinction. The Early Triassic fossil record of echinoids is, however, sparse, and new fossils are paving the way for a revised interpretation of the evolutionary history of echinoids during the Permian-Triassic crisis and Early Mesozoic. A new species of echinoid, Yunnanechinus luopingensis n. sp. recovered from the Middle Triassic (Anisian) Luoping Biota fossil Lagerstätte of South China, displays morphologies that are not characteristic of the echinoid crown group. We have used phylogenetic analyses to further demonstrate that Yunnanechinus is not a member of the echinoid crown group. Thus a clade of stem group echinoids survived into the Middle Triassic, enduring the global crisis that characterized the end-Permian and Early Triassic. Therefore, stem group echinoids did not go extinct during the Palaeozoic, as previously thought, and appear to have coexisted with the echinoid crown group for at least 23 million years. Stem group echinoids thus exhibited the Lazarus effect during the latest Permian and Early Triassic, while crown group echinoids did not.

  16. Analysis of Sunyaev-Zel'dovich effect mass-observable relations using South Pole Telescope observations of an X-ray selected sample of low-mass galaxy clusters and groups

    Energy Technology Data Exchange (ETDEWEB)

    Liu, J.; Mohr, J.; Saro, A.; Aird, K. A.; Ashby, M. L. N.; Bautz, M.; Bayliss, M.; Benson, B. A.; Bleem, L. E.; Bocquet, S.; Brodwin, M.; Carlstrom, J. E.; Chang, C. L.; Chiu, I.; Cho, H. M.; Clocchiatti, A.; Crawford, T. M.; Crites, A. T.; de Haan, T.; Desai, S.; Dietrich, J. P.; Dobbs, M. A.; Foley, R. J.; Gangkofner, D.; George, E. M.; Gladders, M. D.; Gonzalez, A. H.; Halverson, N. W.; Hennig, C.; Hlavacek-Larrondo, J.; Holder, G. P.; Holzapfel, W. L.; Hrubes, J. D.; Jones, C.; Keisler, R.; Lee, A. T.; Leitch, E. M.; Lueker, M.; Luong-Van, D.; McDonald, M.; McMahon, J. J.; Meyer, S. S.; Mocanu, L.; Murray, S. S.; Padin, S.; Pryke, C.; Reichardt, C. L.; Rest, A.; Ruel, J.; Ruhl, J. E.; Saliwanchik, B. R.; Sayre, J. T.; Schaffer, K. K.; Shirokoff, E.; Spieler, H. G.; Stalder, B.; Staniszewski, Z.; Stark, A. A.; Story, K.;  uhada, R.; Vanderlinde, K.; Vieira, J. D.; Vikhlinin, A.; Williamson, R.; Zahn, O.; Zenteno, A.

    2015-02-25

    We use microwave observations from the South Pole Telescope (SPT) to examine the Sunyaev–Zel'dovich effect (SZE) signatures of a sample of 46 X-ray selected groups and clusters drawn from ~6 deg2 of the XMM–Newton Blanco Cosmology Survey. These systems extend to redshift z = 1.02 and probe the SZE signal to the lowest X-ray luminosities (≥1042 erg s-1) yet; these sample characteristics make this analysis complementary to previous studies. We develop an analysis tool, using X-ray luminosity as a mass proxy, to extract selection-bias-corrected constraints on the SZE significance and Y_500 mass relations. The former is in good agreement with an extrapolation of the relation obtained from high-mass clusters. However, the latter, at low masses, while in good agreement with the extrapolation from the high-mass SPT clusters, is in tension at 2.8σ with the Planck constraints, indicating the low-mass systems exhibit lower SZE signatures in the SPT data. We also present an analysis of potential sources of contamination. For the radio galaxy point source population, we find 18 of our systems have 843 MHz Sydney University Molonglo Sky Survey sources within 2 arcmin of the X-ray centre, and three of these are also detected at significance >4 by SPT. Of these three, two are associated with the group brightest cluster galaxies, and the third is likely an unassociated quasar candidate. We examine the impact of these point sources on our SZE scaling relation analyses and find no evidence of biases. We also examine the impact of dusty galaxies using constraints from the 220 GHz data. The stacked sample provides 2.8σ significant evidence of dusty galaxy flux, which would correspond to an average underestimate of the SPT Y_500 signal that is (17 ± 9)per cent in this sample of low-mass systems. Finally, we explore the impact of future data from SPTpol and XMM-XXL, showing that it will lead to a factor of 4 to 5 tighter

  17. Selection of greenery plants' group tolerant to mineralized human wastes for their inclusion into intrasystem mass exchange of BTLSS

    Science.gov (United States)

    Tikhomirova, Natalia; Tikhomirov, Alexander A.; Kalacheva, Galina; Ushakova, Sofya; Trifonov, Sergey V.; Pavlova, Anastasiya

    2016-07-01

    A possible way solving the inclusion problem of the human liquid wastes containing sodium chloride into intrasystem mass exchange of bio-technical life support system (BTLSS) is selection of such species of greenery plants that can utilize sodium chloride, be edible for a human and have rather a high productivity. Our previous works showed that salt-accumulating halophyte Salicornia europaea L. was a promising candidate for sodium chloride inclusion into BTLSS mass exchange. However, with the aim of creation of more various human diet possibilities a set of greenery plants cultivated by the water culture method was estimated. Based on preliminary experiments the plants Brassica juncea L., Nasturtium officinale R. Br., Lepidium sativum angustifolia L. and Salicornia europaea L. were chosen as the investigation objects. The nutrient solution for greenery plant's cultivation was obtained after harvesting the wheat plants grown on the solution with mineralized human wastes' addition. The results of the first stage of the investigations carried out showed that plants of Brassica juncea and Lepidium sativum angustifolia are unpromising for their inclusion into BTLSS because of a set of physiological characteristics. On the next stage of investigations, an experimental model of closed ecosystem was created. For that purpose the plants of Salicornia europaea and Nasturtium officinale were introduced in the phototroph unit structure. It was determined that there was deficiency of main macronutrients for Salicornia europaea and Nasturtium officinale including sodium for Salicornia europaea. The deficiency had an effect on plants productivity and on carry-over of sodium from solution by Salicornia europaea. Thus in the future experiment it is necessary to carry out desalinization of solution by Salicornia europaea plants. Nasturtium officinale, that is rich in essential fatty acids and contributes into variety of human vegetable diet is planned to be cultivated by the

  18. Quantitative chemical derivatization technique in time-of-flight secondary ion mass spectrometry for surface amine groups on plasma-polymerized ethylenediamine film.

    Science.gov (United States)

    Kim, Jinmo; Shon, Hyun Kyong; Jung, Donggeun; Moon, Dae Won; Han, Sang Yun; Lee, Tae Geol

    2005-07-01

    A chemical derivatization technique in time-of-flight secondary ion mass spectrometry (TOF-SIMS) has been developed to quantify the surface density of amine groups of plasma-polymerized ethylenediamine thin film deposited on a glass surface by inductively coupled plasma chemical vapor deposition. Chemical tags of 4-nitrobenzaldehyde or pentafluorobenzaldehyde were hybridized with the surface amine groups and were detected in TOF-SIMS spectra as characteristic molecular secondary ions. The surface amine density was controlled in a reproducible manner as a function of deposition plasma power and was also quantified using UV-visible spectroscopy. A good linear correlation was observed between the results of TOF-SIMS and UV-visible measurements as a function of plasma power. This shows that the chemical derivatization technique in TOF-SIMS analysis would be useful in quantifying the surface density of specific functional groups that exist on the organic surface.

  19. Comparison of gait velocity and center of mass during square and semicircular turning gaits between groups of elderly people with differing visual acuity.

    Science.gov (United States)

    Shin, Sun-Shil; An, Duk-Hyun; Yoo, Won-Gyu

    2015-02-01

    [Purpose] The purpose of this study was to investigate gait velocity and center of mass (COM) during square and semicircular turning gaits between two groups of elderly people with differing visual acuity. [Subjects] Twenty elderly Korean women who could walk independently and who lived in the community were recruited. [Methods] We measured gait velocity and COM using an accelerometer during two different turning gaits. [Results] The velocity during square and semicircular turning gaits of participants with good binocular visual acuity (GBVA) was significantly higher than that of participants with poor binocular visual acuity (PBVA). The COM during square and semicircular turning gaits of the GBVA group was significantly decreased compared with that of the PBVA group. [Conclusion] These findings suggest that visual acuity affects velocity and COM during square and semicircular turning gaits of elderly people.

  20. Identifying Functional Cysteine Residues in the Mitochondria.

    Science.gov (United States)

    Bak, Daniel W; Pizzagalli, Mattia D; Weerapana, Eranthie

    2017-04-21

    The mitochondria are dynamic organelles that regulate oxidative metabolism and mediate cellular redox homeostasis. Proteins within the mitochondria are exposed to large fluxes in the surrounding redox environment. In particular, cysteine residues within mitochondrial proteins sense and respond to these redox changes through oxidative modifications of the cysteine thiol group. These oxidative modifications result in a loss in cysteine reactivity, which can be monitored using cysteine-reactive chemical probes and quantitative mass spectrometry (MS). Analysis of cell lysates treated with cysteine-reactive probes enable the identification of hundreds of cysteine residues, however, the mitochondrial proteome is poorly represented (proteins and suppression of mitochondrial peptide MS signals by highly abundant cytosolic peptides. Here, we apply a mitochondrial isolation and purification protocol to substantially increase coverage of the mitochondrial cysteine proteome. Over 1500 cysteine residues from ∼450 mitochondrial proteins were identified, thereby enabling interrogation of an unprecedented number of mitochondrial cysteines. Specifically, these mitochondrial cysteines were ranked by reactivity to identify hyper-reactive cysteines with potential catalytic and regulatory functional roles. Furthermore, analyses of mitochondria exposed to nitrosative stress revealed previously uncharacterized sites of protein S-nitrosation on mitochondrial proteins. Together, the mitochondrial cysteine enrichment strategy presented herein enables detailed characterization of protein modifications that occur within the mitochondria during (patho)physiological fluxes in the redox environment.

  1. Benefits of group living include increased feeding efficiency and lower mass loss during desiccation in the social and inbreeding spider Stegodyphus dumicola.

    Directory of Open Access Journals (Sweden)

    Bram eVanthournout

    2016-02-01

    Full Text Available Group living carries a price: it inherently entails increased competition for resources and reproduction, and may also be associated with mating among relatives, which carries costs of inbreeding. Nonetheless, group living and sociality is found in many animals, and understanding the direct and indirect benefits of cooperation that override the inherent costs remains a challenge in evolutionary ecology. Individuals in groups may benefit from more efficient management of energy or water reserves, for example in the form of reduced water or heat loss from groups of animals huddling, or through reduced energy demands afforded by shared participation in tasks. We investigated the putative benefits of group living in the permanently social spider Stegodyphus dumicola by comparing the effect of group size on standard metabolic rate, lipid/protein content as a body condition measure, feeding efficiency, per capita web investment and weight/water loss and survival during desiccation. Because energetic expenditure is temperature sensitive, some assays were performed under varying temperature conditions. We found that feeding efficiency increased with group size, and the rate of weight loss was higher in solitary individuals than in animals in groups of various sizes during desiccation. Interestingly, this was not translated into differences in survival or in standard metabolic rate. We did not detect any group size effects for other parameters, and group size effects did not co-vary with experimental temperature in a predictive manner. Both feeding efficiency and mass loss during desiccation are relevant ecological factors as the former results in lowered predator exposure time, and the latter benefits social spiders which occupy arid, hot environments.

  2. Novel and rapid method for determination of organophosphorus pesticide residues in edible fungus using direct gas purge microsyringe extraction coupled on-line with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Nan, Jingxi; Wang, Juan; Piao, Xiangfan; Yang, Cui; Wu, Xue; Quinto, Maurizio; Li, Donghao

    2015-09-01

    In this work a new analytical method for a rapid and simultaneous determination of 28 organophosphorus pesticides (OPPs) residues in edible fungus using gas purge microsyringe extraction (GP-MSE), coupled with on-line gas chromatography-mass spectrometry (GP-MSE-GC-MS) has been developed and optimized. GP-MSE, a novel gas flow liquid-phase microextraction technique, has been then fruitfully used as innovative and one-step extraction procedure, allowing a direct injection into the gas chromatograph coupled with a mass spectrometry detector (GC-MS) system without any further cleaning step. Once optimized, the GP-MSE-GC-MS analysis procedure showed reproducibility values, resolutions, linear responses, detection and quantification limits that allowed to consider this method suitable for the analysis of the 28 OPPs in real samples. Furthermore, OPP recoveries and the relative standard deviations (RSDs) ranged from 85.26% to 100.21%, and from 1.6% to 6.9%, respectively. This procedure was then used for the analysis of real samples and the obtained results were compared with those of ultrasonic extraction-solid phase extraction. Among the 28 OPPs, 14 of them were found in Lentinus edodes and Enoki mushrooms fungus samples, with a total concentrations of 112.7 and 210.7 μg kg(-1), respectively. This work demonstrated then that GP-MSE-GC-MS provided a highly efficient, solvent-saving, accurate and sensitive quantitative analysis method for a rapid determination of OPPs in edible fungus. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Buried Volume Analysis for Propene Polymerization Catalysis Promoted by Group 4 Metals: a Tool for Molecular Mass Prediction

    KAUST Repository

    Falivene, Laura

    2015-10-02

    A comparison of the steric properties of homogeneous single site catalysts for propene polymerization using the percentage of buried volume (%VBur) as molecular descriptor is reported. The %VBur calculated on the neutral precursors of the active species seems to be a reliable tool to explain several experimental data related to the propene insertion and to the monomer chain transfer. Interestingly, a linear correlation between the buried volume calculated for a large set of neutral precursors and the energetic difference between propagation and termination steps calculated by DFT methods is found for Group 4 metal catalysts. The “master curves” derived for Ti, Zr and Hf confirm not only that the %VBur is an appropriate molecular descriptor for the systems considered but also that it could be used as tool for a large computational screening of new ligands.

  4. Use of the extraction residue of emeralds in a formulation mass of ceramic tiles; Utilizacao do residuo da extracao de esmeraldas em uma formulacao de massa de revestimento ceramico

    Energy Technology Data Exchange (ETDEWEB)

    Cavalcante, R. F., E-mail: ronaldofcavalcante@gmail.com [Programa de Pos-Graduacao em Engenharia Mecanica - PPgEM - UFRN, Universidade Federal do Rio Grande do Norte, Lagoa Nova, RN (Brazil); Nascimento, R.M.; Paskocimas, C.A., E-mail: rmaribondo@ufrnet.br, E-mail: paskocimas_ca@hotmail.com [Departamento de Engenharia Materiais - DEMAT - Universidade Federal do Rio Grande do Norte, Lagoa Nova, RN (Brazil); Dutra, R.P.S., E-mail: ricardodutra@ct.ufpb.br [Departamento de Engenharia Materiais - DEMAT - UFPB - Universidade Federal de Pernambuco, Recife (Brazil)

    2012-04-15

    Companies involved in mining and beneficiation of emerald represent an important area of industrial development in Brazil, with a significant contribution to world production of this ore. As a result, large volumes of waste generated and emerald are constantly abandoned in the environment, contributing negatively to their preservation. On the other hand the interest in the use of mining waste as an additive in production of ceramic materials has grown among researchers in recent years. The ceramic industry is constantly seeking to expand the market for the sector and trying to improve product quality and increase the variety of applications. The technology of obtaining ceramic coating that uses waste from mining is still a largely unexplored market. Thus, the purpose of this study was to characterize the waste generated from mining emerald as well as to evaluate its potential use as raw material for production melting of ceramic tiles. Ceramic mixtures were prepared from raw materials characterized by X-ray fluorescence and X-ray diffraction. Five compositions were prepared using the waste codes of emeralds from 0%, 10%, 20%, 30% and 40%. Samples were prepared by pressing, sintered at 1000, 1100 and 1200 deg C and characterized to establish their mineralogical composition, water absorption, linear shrinkage and modulus of rupture. The results showed that the residue of emeralds studied can be embedded in the mass of ceramic tiles up to 20% in replacement of feldspar without compromising the end product properties. (author)

  5. Quantification of bupivacaine hydrochloride and isoflupredone acetate residues in porcine muscle, beef, milk, egg, shrimp, flatfish, and eel using a simplified extraction method coupled with liquid chromatography-triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Cho, Sang-Hyun; Park, Jin-A; Zheng, Weijia; Abd El-Aty, A M; Kim, Seong-Kwan; Choi, Jeong-Min; Yi, Hee; Cho, Soo-Min; Afifi, Nehal A; Shim, Jae-Han; Chang, Byung-Joon; Kim, Jin-Suk; Shin, Ho-Chul

    2017-10-15

    In this study, a simple analytical approach has been developed and validated for the determination of bupivacaine hydrochloride and isoflupredone acetate residues in porcine muscle, beef, milk, egg, shrimp, flatfish, and eel using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A 0.1% solution of acetic acid in acetonitrile combined with n-hexane was used for deproteinization and defatting of all tested matrices and the target drugs were well separated on a Waters Xbridge™ C18 analytical column using a mobile phase consisting of 0.1% acetic acid (A) and 0.1% solution of acetic acid in methanol (B). The linearity estimated from six-point matrix-matched calibrations was good, with coefficients of determination ≥0.9873. The limits of quantification (LOQs) for bupivacaine hydrochloride and isoflupredone acetate were 1 and 2ngg -1 , respectively. Recovery percentages in the ranges of 72.51-112.39% (bupivacaine hydrochloride) and 72.58-114.56% (isoflupredone acetate) were obtained from three different fortification concentrations with relative standard deviations (RSDs) of bupivacaine hydrochloride and isoflupredone acetate from porcine muscle, beef, milk, egg, shrimp, flatfish, and eel samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Multi-residue analysis of veterinary drugs, pesticides and mycotoxins in dairy products by liquid chromatography-tandem mass spectrometry using low-temperature cleanup and solid phase extraction.

    Science.gov (United States)

    Xie, Jie; Peng, Tao; Zhu, Ailing; He, Jianli; Chang, Qiaoying; Hu, Xueyan; Chen, Hui; Fan, Chunlin; Jiang, Wenxiao; Chen, Min; Li, Jiancheng; Ding, Shuangyang; Jiang, Haiyang

    2015-10-01

    A multi-class multi-residue analysis method for determination of veterinary drugs, pesticides and mycotoxins in dairy products by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been established. These 17 classes, a total of 40 kinds of target compounds were chosen because their administration to food-producing animals is banned or regulated in China and may be potentially abused or misused. Samples were extracted with acetonitrile-ethyl acetate-acetic acid (49.5+49.5+1, v/v/v). Most of lipids in the extract were removed by low-temperature cleanup, prior to solid phase extraction on HLB cartridges. The quantification and confirmation of the 40 analytes were performed by LC-MS/MS with electro-spray ionization (ESI) interface in multiple reaction monitoring (MRM) mode. The limits of detection (LODs) and limits of quantification (LOQs) were 0.006-0.3μg/kg and 0.02-1.0μg/kg, respectively. The spiked recoveries in milk, yogurt, milk powder and cheese samples were from 67.3% to 106.9%. The repeatability and the within-laboratory reproducibility were less than 12.7% and 13.9%. Applying this method, our results revealed the presences of chloramphenicol, cimeterol, and flunixin at the concentration of 0.027-0.452μg/kg in some samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid-liquid extraction technique and liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-MS/MS).

    Science.gov (United States)

    Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Campos Motta, Tanara Magalhães; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara

    2015-11-01

    A fast and simple method for residue analysis of the antibiotics classes of macrolides (erythromycin, azithromycin, tylosin, tilmicosin and spiramycin) and lincosamides (lincomycin and clindamycin) was developed and validated for cattle, swine and chicken muscle and for bovine milk. Sample preparation consists in a liquid-liquid extraction (LLE) with acetonitrile, followed by liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-ESI-MS/MS), without the need of any additional clean-up steps. Chromatographic separation was achieved using a C18 column and a mobile phase composed by acidified acetonitrile and water. The method was fully validated according the criteria of the Commission Decision 2002/657/EC. Validation parameters such as limit of detection, limit of quantification, linearity, accuracy, repeatability, specificity, reproducibility, decision limit (CCα) and detection capability (CCβ) were evaluated. All calculated values met the established criteria. Reproducibility values, expressed as coefficient of variation, were all lower than 19.1%. Recoveries range from 60% to 107%. Limits of detection were from 5 to 25 µg kg(-1).The present method is able to be applied in routine analysis, with adequate time of analysis, low cost and a simple sample preparation protocol. Copyright © 2015. Published by Elsevier B.V.

  8. Salmon Muscle Adherence to Polymer Coatings and Determination of Antibiotic Residues by Reversed-Phase High-Performance Liquid Chromatography Coupled to Selected Reaction Monitoring Mass Spectrometry, Atomic Force Microscopy, and Fourier Transform Infrared Spectroscopy

    Directory of Open Access Journals (Sweden)

    E. Zumelzu

    2015-01-01

    Full Text Available The persistent adhesion of salmon muscle to food container walls after treatment with urea solution was observed. This work evaluated the diffusion of antibiotics from the salmon muscle to the polyethylene terephthalate (PET coating protecting the electrolytic chromium coated steel (ECCS plates. New aquaculture production systems employ antibiotics such as florfenicol, florfenicol amine, oxytetracycline, and erythromycin to control diseases. The introduction of antibiotics is a matter of concern regarding the effects on human health and biodiversity. It is important to determine their impact on the adhesion of postmortem salmon muscle to can walls and the surface and structural changes affecting the functionality of multilayers. This work characterized the changes occurring in the multilayer PET polymer and steel of containers by electron microscopy, 3D atomic force microscopy (3D-AFM, X-ray photoelectron spectroscopy (XPS, and Fourier transform infrared spectroscopy (FT-IR analyses. A robust mass spectrometry methodology was employed to determine the presence of antibiotic residues. No evidence of antibiotics was observed on the protective coating in the range between 0.001 and 2.0 ng/mL; however, the presence of proteins, cholesterol, and alpha-carotene was detected. This in-depth profiling of the matrix-level elements is relevant for the use of adequate materials in the canning export industry.

  9. The last dinosaurs of Brazil: The Bauru Group and its implications for the end-Cretaceous mass extinction

    Directory of Open Access Journals (Sweden)

    STEPHEN L. BRUSATTE

    Full Text Available ABSTRACT The non-avian dinosaurs died out at the end of the Cretaceous, ~66 million years ago, after an asteroid impact. The prevailing hypothesis is that the effects of the impact suddenly killed the dinosaurs, but the poor fossil record of latest Cretaceous (Campanian-Maastrichtian dinosaurs from outside Laurasia (and even more particularly, North America makes it difficult to test specific extinction scenarios. Over the past few decades, a wealth of new discoveries from the Bauru Group of Brazil has revealed a unique window into the evolution of terminal Cretaceous dinosaurs from the southern continents. We review this record and demonstrate that there was a diversity of dinosaurs, of varying body sizes, diets, and ecological roles, that survived to the very end of the Cretaceous (Maastrichtian: 72-66 million years ago in Brazil, including a core fauna of titanosaurian sauropods and abelisaurid and carcharodontosaurid theropods, along with a variety of small-to-mid-sized theropods. We argue that this pattern best fits the hypothesis that southern dinosaurs, like their northern counterparts, were still diversifying and occupying prominent roles in their ecosystems before the asteroid suddenly caused their extinction. However, this hypothesis remains to be tested with more refined paleontological and geochronological data, and we give suggestions for future work.

  10. The last dinosaurs of Brazil: The Bauru Group and its implications for the end-Cretaceous mass extinction.

    Science.gov (United States)

    Brusatte, Stephen L; Candeiro, Carlos R A; Simbras, Felipe M

    2017-01-01

    The non-avian dinosaurs died out at the end of the Cretaceous, ~66 million years ago, after an asteroid impact. The prevailing hypothesis is that the effects of the impact suddenly killed the dinosaurs, but the poor fossil record of latest Cretaceous (Campanian-Maastrichtian) dinosaurs from outside Laurasia (and even more particularly, North America) makes it difficult to test specific extinction scenarios. Over the past few decades, a wealth of new discoveries from the Bauru Group of Brazil has revealed a unique window into the evolution of terminal Cretaceous dinosaurs from the southern continents. We review this record and demonstrate that there was a diversity of dinosaurs, of varying body sizes, diets, and ecological roles, that survived to the very end of the Cretaceous (Maastrichtian: 72-66 million years ago) in Brazil, including a core fauna of titanosaurian sauropods and abelisaurid and carcharodontosaurid theropods, along with a variety of small-to-mid-sized theropods. We argue that this pattern best fits the hypothesis that southern dinosaurs, like their northern counterparts, were still diversifying and occupying prominent roles in their ecosystems before the asteroid suddenly caused their extinction. However, this hypothesis remains to be tested with more refined paleontological and geochronological data, and we give suggestions for future work.

  11. Skin peptides from anurans of the Litoria rubella Group: sequence determination using electrospray mass spectrometry. Opioid activity of two major peptides.

    Science.gov (United States)

    Jackway, Rebecca J; Maselli, Vita M; Musgrave, Ian F; Maclean, Micheal J; Tyler, Michael J; Bowie, John H

    2009-04-01

    Many species of frogs of the genus Litoria secrete bioactive peptides from their skin glands. These peptides are normally host-defence compounds and may have one, or more of the following activities; smooth muscle contraction, analgesic, antimicrobial, antiviral, lymphocyte proliferator (immunomodulator) and neuronal nitric oxide synthase (nNOS) inactivation. Two frog species of the Litoria rubella Group that have been studied before, namely, Litoria electrica and Litoria rubella, are different from other species of the genus Litoria in that they produce small peptides that show neither membrane, lymphocyte nor nNOS activity. In this study we have used electrospray mass spectrometry together with Edman sequencing to identify eight skin peptides of the third member of this Group, Litoria dentata: surprisingly, none of these peptides show activity in our biological screening program. However, two major peptides (FPWL-NH(2) and FPWP-NH(2)) from L. electrica and L. rubella are opioids at the micromolar concentration.

  12. Determination of platinum group elements by inductively coupled plasma-mass spectrometry combined with nickel sulfide fire assay and tellurium coprecipitation

    Science.gov (United States)

    Sun, Yali; Guan, Xiyun; Du, Andao

    1998-09-01

    A method was developed for the determination of trace platinum group elements (PGEs) by nickel sulfide fire assay inductively coupled plasma-mass spectrometry (ICP-MS). With isotope dilution, the improved technique gives precise Os content data. Through the purification of the reagent nickel oxide, reagent blank was greatly reduced. Results obtained for the standard reference materials (SRM) GPt-1-GPt-7(GBW 07288-07294, China), DZ Σ-2 (GBW 07102, China) and Guilin Cu-Ni Ore are in good agreement with the recommended values for platinum group elements. The detection limits ranged from 0.01 to 0.39 ng/g. The relative standard deviations for Ru, Rh, Pd and Ir were less than 5%, for Os less than 1%, and Pt less than 8% for SRM GPt-6.

  13. Hydrazide and hydrazine reagents as reactive matrices for matrix-assisted laser desorption/ionization mass spectrometry to detect steroids with carbonyl groups.

    Science.gov (United States)

    Shigeri, Yasushi; Yasuda, Akikazu; Sakai, Masamichi; Ikeda, Shinya; Arakawa, Ryuichi; Sato, Hiroaki; Kinumi, Tomoya

    2015-01-01

    Fifty-one reagents (37 hydrazides and 14 hydrazines) were examined to determine if they could function as reactive matrices for the detection of steroids with carbonyl groups in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Among these reagents, 3-hydroxy-2-naphthoic acid hydrazide reacted most efficiently with steroids with carbonyl groups, allowing detection of them at the 1pmol level. Results from accurate mass measurement with a JMS-S3000 Spiral-TOF suggested that the ion peaks corresponding to the protonated fragment of a hydrazone were observed, in addition to the protonated molecular peaks of the resulting hydrazones ([M(D)+H](+)) and their sodium adduct ([M(D)+Na](+)). 3-Hydroxy-2-naphthoic acid hydrazide also could detect cortisol (1.93ng) spiked in a human serum certified reference material, as well as cortisone and cortisol in a human saliva sample collected in the morning. Using a combination of 3-hydroxy-2-naphthoic acid hydrazide and α- cyano-4-hydroxycinammic acid (CHCA) (3-hydroxy-2-naphthoic acid hydrazide:CHCA=4:1, v/v), even cortisone and cortisol in a human saliva sample collected in the afternoon, when levels are typically low, could be detected effectively.

  14. Monitoring the extraction of additives and additive degradation products from polymer packaging into solutions by multi-residue method including solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Pouech, Charlène; Lafay, Florent; Wiest, Laure; Baudot, Robert; Léonard, Didier; Cren-Olivé, Cécile

    2014-02-01

    The use of polymer materials in industry for product packaging is increasing. The presence of additives in the polymer matrix enables the modification or improvement of the properties and performance of the polymer, but these industries are concerned regarding the extractability of these additives. The quantification of these additives is particularly challenging because of the presence of these substances as contaminants in all the analytical equipment and the diversity of their physicochemical properties. In this context, a multi-residue analytical method was developed for the trace analysis of the twenty main additives (and their degradation products) authorized in plastic products such as pharmaceutical packaging (e.g., antioxidants, release agents, and light absorbers). This analytical method consisted of a solid phase extraction (SPE) followed by an analysis using ultra-high performance liquid chromatography coupled to a tandem mass spectrometer (UHPLC-MS/MS). A comparison of two ionization interfaces and the optimization of the extraction procedure were discussed. The influence of the quality of the solvent type (distilled versus not distilled) and the nature of the SPE cartridges (Polypropylene versus Teflon(®)) were demonstrated. The optimized method exhibited a quantification limit lower than 20 ng mL(-1) and recoveries between 70 % and 120 % for all compounds. Finally, the method was validated according to the ICH directive and was subsequently applied to the extraction of polymers under different pH conditions and storage temperatures. To the best of our knowledge, this study presents the first methodology allowing the simultaneous quantification of 24 additives at low ng mL(-1).

  15. Residues of sulfadiazine and doxycycline in broiler liver and muscle tissue due to cross-contamination of feed.

    Science.gov (United States)

    Vandenberge, V; Delezie, E; Huyghebaert, G; Delahaut, P; Daeseleire, E; Croubels, S

    2012-01-01

    Veterinary drugs, such as antimicrobial compounds, are widely used in poultry and may lead to the presence of residues in matrices of animal origin, such as muscle and liver tissue. In this study, broilers received an experimental feed containing sulfadiazine or doxycycline at cross-contamination levels of 2.5, 5 and 10% of the therapeutic dose in feed. Breast and thigh muscle and liver samples were collected during treatment and depletion period and analysed via liquid chromatography-tandem mass spectrometry (LC-MS/MS). Concentrations reached a plateau phase 3-5 days after the start of experimental feeding. A rapid depletion of residues was noted after withdrawal of the experimental feed. No significant differences in measured concentrations were observed between the various muscle types. Residue concentrations for some experimental groups; the 10% group of sulfadiazine and the 5 and 10% group of doxycycline, however, exceeded their corresponding maximum residue limits (MRLs).

  16. MassAI

    DEFF Research Database (Denmark)

    2011-01-01

    A software tool for general analysis and data-mining of mass-spectrometric datasets. The program features a strong emphasis on scan-by-scan identification and results-transparency. MassAI also accommodates residue level analysis of labelled runs, e.g. HDX.......A software tool for general analysis and data-mining of mass-spectrometric datasets. The program features a strong emphasis on scan-by-scan identification and results-transparency. MassAI also accommodates residue level analysis of labelled runs, e.g. HDX....

  17. Relationship between Body Mass Index (BMI) and body fat percentage, estimated by bioelectrical impedance, in a group of Sri Lankan adults: a cross sectional study.

    Science.gov (United States)

    Ranasinghe, Chathuranga; Gamage, Prasanna; Katulanda, Prasad; Andraweera, Nalinda; Thilakarathne, Sithira; Tharanga, Praveen

    2013-09-03

    Body Mass Index (BMI) is used as a useful population-level measure of overweight and obesity. It is used as the same for both sexes and for all ages of adults. The relationship between BMI and body fat percentage (BF %) has been studied in various ethnic groups to estimate the capacity of BMI to predict adiposity. We aimed to study the BMI-BF% relationship, in a group of South Asian adults who have a different body composition compared to presently studied ethnic groups. We examined the influence of age, gender in this relationship and assessed its' linearity or curvilinearity. A cross sectional study was conducted, where adults of 18-83 years were grouped into young (18-39 years) middle aged (40-59 years) and elderly (>60 years). BF% was estimated from bioelectrical impedance analysis. Pearsons' correlation coefficient(r) was calculated to see the relationship between BMI-BF% in the different age groups. Multiple regression analysis was performed to determine the effect of age and gender in the relationship and polynomial regression was carried out to see its' linearity. The relationships between age-BMI, age-BF % were separately assessed. Out of 1114 participants, 49.1% were males. The study sample represented a wide range of BMI values (14.8-41.1 kg/m2,Mean 23.8 ± 4.2 kg/m2). A significant positive correlation was observed between BMI-BF%, in males (r =0.75, p bioelectrical impedance, in this sub population of South Asian adults. This relationship was curvilinear in nature and was significantly influenced by age and gender. Our findings support the importance of taking age and gender in to consideration when using BMI to predict body fat percentage/obesity, in a population.

  18. Lysine 356 is a critical residue for binding the C-6 phospho group of fructose 2,6-bisphosphate to the fructose-2,6-bisphosphatase domain of rat liver 6-phosphofructo-2-kinase/fructose-2,6-bisphosphatase.

    Science.gov (United States)

    Li, L; Lin, K; Correia, J J; Pilkis, S J

    1992-08-15

    Lysine 356 has been implicated by protein modification studies as a fructose-2,6-bisphosphate binding site residue in the 6-phosphofructo-2-kinase domain of rat liver 6-phosphofructo-2-kinase/fructose-2,6-bisphosphatase (Kitajima, S., Thomas, H., and Uyeda, K. (1985) J. Biol. Chem. 260, 13995-14002). However, Lys-356 is found in the fructose-2,6-bisphosphatase domain (Bazan, F., Fletterick, R., and Pilkis, S. J. (1989) Proc. Natl. Acad. Sci. U.S.A. 86, 9642-9646). In order to ascertain whether Lys-356 is involved in fructose-2,6-bisphosphatase catalysis and/or domain/domain interactions of the bifunctional enzyme, Lys-356 was mutated to Ala, expressed in Escherichia coli, and then purified to homogeneity. Circular dichroism experiments indicated that the secondary structure of the Lys-356-Ala mutant was not significantly different from that of the wild-type enzyme. The Km for fructose 2,6-bisphosphate and the Ki for the noncompetitive inhibitor, fructose 6-phosphate, for the fructose-2,6-bisphosphatase of the Lys-356-Ala mutant were 2700- and 2200-fold higher, respectively, than those of the wild-type enzyme. However, the maximal velocity and the Ki for the competitive product inhibitor, inorganic phosphate, were unchanged compared to the corresponding values of the wild-type enzyme. Furthermore, in contrast to the wild-type enzyme, which exhibits substrate inhibition, there was no inhibition by substrate of the Lys-356-Ala mutant. In the presence of saturating substrate, inorganic phosphate, which acts by relieving fructose-6-phosphate and substrate inhibition, is an activator of the bisphosphatase. The Ka for inorganic phosphate of the Lys-356-Ala mutant was 1300-fold higher than that of the wild-type enzyme. The kinetic properties of the 6-phosphofructo-2-kinase of the Lys-356-Ala mutant were essentially identical with that of the wild-type enzyme. The results demonstrate that: 1) Lys-356 is a critical residue in fructose-2,6-bisphosphatase for binding the 6

  19. Grouping of Petroleum Substances as Example UVCBs by Ion Mobility-Mass Spectrometry to Enable Chemical Composition-Based Read-Across.

    Science.gov (United States)

    Grimm, Fabian A; Russell, William K; Luo, Yu-Syuan; Iwata, Yasuhiro; Chiu, Weihsueh A; Roy, Tim; Boogaard, Peter J; Ketelslegers, Hans B; Rusyn, Ivan

    2017-06-20

    Substances of Unknown or Variable composition, Complex reaction products, and Biological materials (UVCBs), including many refined petroleum products, present a major challenge in regulatory submissions under the EU Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) and US High Production Volume regulatory regimes. The inherent complexity of these substances, as well as variability in composition obfuscates detailed chemical characterization of each individual substance and their grouping for human and environmental health evaluation through read-across. In this study, we applied ion mobility mass spectrometry in conjunction with cheminformatics-based data integration and visualization to derive substance-specific signatures based on the distribution and abundance of various heteroatom classes. We used petroleum substances from four petroleum substance manufacturing streams and evaluated their chemical composition similarity based on high-dimensional substance-specific quantitative parameters including m/z distribution, drift time, carbon number range, and associated double bond equivalents and hydrogen-to-carbon ratios. Data integration and visualization revealed group-specific similarities for petroleum substances. Observed differences within a product group were indicative of batch- or manufacturer-dependent variation. We demonstrate how high-resolution analytical chemistry approaches can be used effectively to support categorization of UVCBs based on their heteroatom composition and how such data can be used in regulatory decision-making.

  20. Identificação de resíduos de disparos de armas de fogo por meio da técnica de espectrometria de massas de alta resolução com fonte de plasma indutivo Identification of gunshot residues by high resolution inductively coupled plasma mass spectrometry

    Directory of Open Access Journals (Sweden)

    Edson Luis Tocaia dos Reis

    2004-06-01

    Full Text Available The violence derived from crimes involving firearms represents one of the main concerns of society. For this reason modern techniques have emerged in forensic science to identify suspects at crime scenes. This work describes a methodology to identify residues present in the hands of suspect by using a high resolution inductively coupled plasma mass spectrometry and collection procedure based on ethylenediaminetetraacetic acid (EDTA solution as a complexing agent in moistened swabs. In order to distinguish real gunshot residues from others types of residues present in the hand of suspect, ternary ratio per cent diagrams were developed for antimony (Sb, barium (Ba and lead (Pb detected on the hands of volunteers, before and immediately after shooting tests, revealing a remarkable difference in both situations.

  1. Lie group analysis for the effect of viscosity and thermophoresis particle deposition on free convective heat and mass transfer in the presence of suction/injection

    Directory of Open Access Journals (Sweden)

    Sivagnana Prabhu K.K.

    2009-01-01

    Full Text Available An analysis has been carried out to study heat and mass transfer characteristics of an incompressible and Newtonian fluid having temperature-dependent fluid viscosity and thermophoresis particle deposition over a vertical stretching surface with variable stream condition. The Rosseland approximation is used to describe the radiative heat flux in the energy equation. The vertical surface is assumed to be permeable so as to allow for possible wall suction or injection. The governing differential equations are derived and transformed using Lie group analysis. The transformed equations are solved numerically by applying Runge-Kutta Gill scheme with shooting technique. Favorable comparisons with previously published work on various special cases of the problem are obtained. Numerical results for the velocity, temperature and concentration profiles for a prescribed temperature-dependent fluid viscosity and thermophoresis particle deposition parameters are presented graphically to elucidate the influence of the various physical parameters.

  2. Matrix-Assisted Laser Desorption Ionization Mass Spectrometry of Compounds Containing Carboxyl Groups Using CdTe and CuO Nanoparticles

    Directory of Open Access Journals (Sweden)

    Megumi Sakurai

    2018-03-01

    Full Text Available Matrix-assisted laser desorption ionization mass spectrometry of compounds containing carboxyl groups was carried out by using semiconductor nanoparticles (CdTe and CuO as the matrix. Salicylic acid (Sal, glucuronic acid (Glu, ibuprofen (Ibu, and tyrosine (Tyr were ionized as deprotonated species (carboxylate anions by using electrons ejected from CdTe after the photoexcitation. When CuO was used as the matrix, the peak intensity of Tyr became high compared with that obtained with CdTe. Measurements of model peptides, angiotensin II (AngII and substance P (SubP, were also carried out but the obtained peak intensities were very low. In order to explain this result, the interaction between CdTe and AngII was confirmed by diffuse reflectance spectroscopy. The results suggest that electrostatic binding between semiconductor nanoparticles and AngII prevented the efficient desorption of AngII into the gas phase.

  3. Atomic Mass and Nuclear Binding Energy for Cf-252 (Californium)

    Science.gov (United States)

    Sukhoruchkin, S. I.; Soroko, Z. N.

    This document is part of the Supplement containing the complete sets of data of Subvolume B `Nuclei with Z = 55 - 100' of Volume 22 `Nuclear Binding Energies and Atomic Masses' of Landolt-Börnstein - Group I `Elementary Particles, Nuclei and Atoms', and additionally including data for nuclei with Z = 101 - 130. It provides atomic mass, mass excess, nuclear binding energy, nucleon separation energies, Q-values, and nucleon residual interaction parameters for atomic nuclei of the isotope Cf-252 (Californium, atomic number Z = 98, mass number A = 252).

  4. Evaluation of two matrix-assisted laser desorption ionization-time of flight mass spectrometry systems for identification of viridans group streptococci.

    Science.gov (United States)

    Kärpänoja, P; Harju, I; Rantakokko-Jalava, K; Haanperä, M; Sarkkinen, H

    2014-05-01

    In this study, the performances of two matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) systems, MALDI Biotyper (Bruker Daltonics) and VITEK MS (bioMérieux), were evaluated in the identification of viridans group streptococci. Two collections of isolates were tested with both methods. From a panel of type collection strains (n = 54), MALDI Biotyper gave correct species-level identification for 51/54 (94 %) strains and 37/54 (69 %) strains for the VITEK MS in vitro diagnostic (IVD) method. Additionally, a collection of blood cultures isolates which had been characterized earlier with partial sequencing of 16S rRNA (n = 97) was analyzed. MALDI Biotyper classified 89 % and VITEK MS 93 % of these correctly to the group level. Comparison of species-level identification from the blood culture collection was possible for 36 strains. MALDI Biotyper identified 75 % and VITEK MS 97 % of these strains consistently. Among the clinical isolates, MALDI Biotyper misidentified 36 strains as Streptococcus pneumoniae. Nevertheless, our results suggest that the current MALDI-TOF methods are a good alternative for the identification of viridans streptococci and do perform as well as or better than commercial phenotypical methods.

  5. A generic approach for expanding homolog-targeted residue screening of sulfonamides using a fast matrix separation and class-specific fragmentation-dependent acquisition with a hybrid quadrupole-linear ion trap mass spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Huang Chunlin [Department of Biochemistry and Molecular Biology, School of Pharmacy and Life Science, University of South China, Hengyang 421001 (China); Guo Bin, E-mail: binnguo@126.com [Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China), Hunan Normal University, Changsha 410081 (China); Wang Xiaoying [Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China), Hunan Normal University, Changsha 410081 (China); Li Jie [Department of Biochemistry and Molecular Biology, School of Pharmacy and Life Science, University of South China, Hengyang 421001 (China); Zhu Weitao; Chen Bo [Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China), Hunan Normal University, Changsha 410081 (China); Ouyang Shan [Food Inspection and Quarantine Center, Shenzhen Entry-Exit Inspection and Quarantine Bureau of the People' s Republic of China, Shenzhen 518067 (China); Yao Shouzhuo [Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China), Hunan Normal University, Changsha 410081 (China)

    2012-08-06

    Highlights: Black-Right-Pointing-Pointer Generic homolog-targeted screening approach for multi-residual sulfonamide analogs. Black-Right-Pointing-Pointer Single-tube extraction/partitioning-multifunction adsorption cleanup for direct injection. Black-Right-Pointing-Pointer Class-specific fragmentation for expanding coverage of N{sup 4}-acetyl and N-OH metabolites. Black-Right-Pointing-Pointer PreS-IDA-EPI in LC-QqLIT for simultaneous screening and confirmation of real samples. - Abstract: A generic and efficient homolog-targeted approach was used to expand screening and detection of target class of sulfonamides and structural analogs, based on a fast single-tube extraction/partitioning-multifunction adsorption cleanup (SEP/MAC) for class-specific fragmentation-dependent acquisition with a liquid chromatography-hybrid triple-quadrupole linear ion trap mass spectrometer (LC-QqLIT). By combining the two-stage process conducted in a single tube as one-pot protocol, the straightforward SEP/MAC procedure was optimized to offer clean extracts with reasonable recovery (71-109% with RSDs < 20%) and decreased matrix interferences (-9 to 19%) of multiresidual sulfonamide extraction from different tissue samples. The novel use of neutral loss scan of 66 Da (NLS) or precursor ion scanning of m/z 108 (PreS) in positive ion mode was found to achieve more comprehensive coverage of protonated molecular ions of a wide array of sulfonamides including N{sup 4}-acetyl and hydroxylamine metabolites plus their possible dimers. Moreover, the PreS-triggered automatically enhanced product ion spectral acquisition enabled simultaneous screening, profiling and confirmation of an unlimited number of analytes belonging to the sulfonamide class within a single analysis. The validation and application results of the generic SEP/MAC-based LC-QqLIT strategy consistently demonstrated favorable performances with acceptable accuracy (67-116%), precision (RSDs < 25%), and sensitivity (LOQs {<=} 7.5 ng

  6. Multi-class, multi-residue analysis of pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenyl ethers and novel flame retardants in fish using fast, low-pressure gas chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sapozhnikova, Yelena, E-mail: yelena.sapozhnikova@ars.usda.gov [US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 193038 (United States); Lehotay, Steven J. [US Department of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 193038 (United States)

    2013-01-03

    Highlights: Black-Right-Pointing-Pointer A method for analysis of POPs and novel flame retardants in catfish was developed. Black-Right-Pointing-Pointer The method is based on a QuEChERS extraction, d-SPE clean-up and low pressure GC/MS-MS. Black-Right-Pointing-Pointer The method validation demonstrated good recoveries and low detection limits. Black-Right-Pointing-Pointer The method was successfully applied for analysis of catfish samples from the market. - Abstract: A multi-class, multi-residue method for the analysis of 13 novel flame retardants, 18 representative pesticides, 14 polychlorinated biphenyl (PCB) congeners, 16 polycyclic aromatic hydrocarbons (PAHs), and 7 polybrominated diphenyl ether (PBDE) congeners in catfish muscle was developed and evaluated using fast low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with acetonitrile and dispersive solid-phase extraction (d-SPE) clean-up with zirconium-based sorbent prior to LP-GC/MS-MS analysis. The developed method was evaluated at 4 spiking levels and further validated by analysis of NIST Standard Reference Materials (SRMs) 1974B and 1947. Sample preparation for a batch of 10 homogenized samples took about 1 h/analyst, and LP-GC/MS-MS analysis provided fast separation of multiple analytes within 9 min achieving high throughput. With the use of isotopically labeled internal standards, recoveries of all but one analyte were between 70 and 120% with relative standard deviations less than 20% (n = 5). The measured values for both SRMs agreed with certified/reference values (72-119% accuracy) for the majority of analytes. The detection limits were 0.1-0.5 ng g{sup -1} for PCBs, 0.5-10 ng g{sup -1} for PBDEs, 0.5-5 ng g{sup -1} for select pesticides and PAHs and 1-10 ng g{sup -1} for flame retardants. The developed method was successfully applied for analysis of catfish samples

  7. The effect of hydroxyl functional groups and molar mass on the viscosity of non-crystalline organic and organic–water particles

    Directory of Open Access Journals (Sweden)

    J. W. Grayson

    2017-07-01

    Full Text Available The viscosities of three polyols and three saccharides, all in the non-crystalline state, have been studied. Two of the polyols (2-methyl-1,4-butanediol and 1,2,3-butanetriol were studied under dry conditions, the third (1,2,3,4-butanetetrol was studied as a function of relative humidity (RH, including under dry conditions, and the saccharides (glucose, raffinose, and maltohexaose were studied as a function of RH. The mean viscosities of the polyols under dry conditions range from 1.5  ×  10−1 to 3.7  ×  101 Pa s, with the highest viscosity being that of the tetrol. Using a combination of data determined experimentally here and literature data for alkanes, alcohols, and polyols with a C3 to C6 carbon backbone, we show (1 there is a near-linear relationship between log10 (viscosity and the number of hydroxyl groups in the molecule, (2 that on average the addition of one OH group increases the viscosity by a factor of approximately 22 to 45, (3 the sensitivity of viscosity to the addition of one OH group is not a strong function of the number of OH functional groups already present in the molecule up to three OH groups, and (4 higher sensitivities are observed when the molecule has more than three OH groups. Viscosities reported here for 1,2,3,4-butanetetrol particles are lower than previously reported measurements using aerosol optical tweezers, and additional studies are required to resolve these discrepancies. For saccharide particles at 30 % RH, viscosity increases by approximately 2–5 orders of magnitude as molar mass increases from 180 to 342 g mol−1, and at 80 % RH, viscosity increases by approximately 4–5 orders of magnitude as molar mass increases from 180 to 991 g mol−1. These results suggest oligomerization of highly oxidized compounds in atmospheric secondary organic aerosol (SOA could lead to large increases in viscosity, and may be at least partially responsible for the high

  8. A personal memory of the history of the group of energy and mass transference; Una memoria personal de la historia del grupo de transferencia de energia y masa

    Energy Technology Data Exchange (ETDEWEB)

    Ramos, Eduardo [Centro de Investigacion en Energia (CIE) de la UNAM, Temixco, Morelos (Mexico)

    2010-07-01

    An object that is exposed to sunlight heats up. Based on the everyday experiences, this is a claim that the majority of us would agree. In a more technical note, this object increases its temperature and internal energy. Reflection for a moment, perhaps we would come to the conclusion that the energy captured by the object exposed to solar radiation could be used in a useful fashion. It would require a much longer time of reflection and analysis to imagine the method to convert the heat into useful energy. It is precisely this analysis that has been the objective of the group of energy and mass transference of the Center for Energy Research since its foundation, and probably will remain so while it can be identified as a group of scientific research. In the following pages we will feature briefly, from a personal stand point of view the history of the work, successes and failures of the group since its inception till the present. [Spanish] Un objeto que se expone a la luz solar se calienta. Basados en la experiencia cotidiana, esta es una aseveracion con la que la mayoria de nosotros estaria de acuerdo. Dicho de manera mas tecnica, este objeto aumenta su temperatura y su energia interna. Reflexionando un instante, quiza llegariamos a la conclusion que la energia capturada por el objeto expuesto a la radiacion solar podria ser usada de manera util. Se requeriria un tiempo mucho mas largo de reflexion y analisis para imaginar el metodo para convertir el calor en energia util. Precisamente este analisis ha sido el objetivo del grupo de Transferencia de Energia y Masa del Centro de Investigacion en Energia desde su fundacion, y probablemente lo seguira siendo mientras se le pueda identificar como un grupo de investigacion cientifica. En las paginas siguientes resenaremos brevemente desde un punto de vista personal la historia del trabajo, exitos y fracasos del grupo desde su inicio hasta el presente.

  9. BANYAN. III. Radial velocity, rotation, and X-ray emission of low-mass star candidates in nearby young kinematic groups

    Energy Technology Data Exchange (ETDEWEB)

    Malo, Lison; Artigau, Étienne; Doyon, René; Lafrenière, David; Albert, Loïc; Gagné, Jonathan, E-mail: malo@astro.umontreal.ca, E-mail: doyon@astro.umontreal.ca [Département de physique and Observatoire du Mont-Mégantic, Université de Montréal, Montréal, QC H3C 3J7 (Canada)

    2014-06-10

    Based on high-resolution spectra obtained with PHOENIX at Gemini-South, CRIRES at VLT-UT1, and ESPaDOnS at the Canada-France-Hawaii Telescope, we present new measurements of the radial and projected rotational velocities of 219 low-mass stars. The target likely membership was initially established using the Bayesian analysis tool recently presented in Malo et al., taking into account only the position, proper motion, and photometry of the stars to assess their membership probability. In the present study, we include radial velocity as an additional input to our analysis, and in doing so we confirm the high membership probability for 130 candidates: 27 in β Pictoris, 22 in Tucana-Horologium, 25 in Columba, 7 in Carina, 18 in Argus and 18 in AB Doradus, and 13 with an ambiguous membership. Our analysis also confirms the membership of 57 stars proposed in the literature. A subsample of 16 candidates was observed at 3 or more epochs, allowing us to discover 6 new spectroscopic binaries. The fraction of binaries in our sample is 25%, consistent with values in the literature. Of the stars in our sample, 20% show projected rotational velocities (vsin i) higher than 30 km s{sup –1} and therefore are considered as fast rotators. A parallax and other youth indicators are still needed to fully confirm the 130 highly probable candidates identified here as new bona fide members. Finally, based on the X-ray emission of bona fide and highly probable group members, we show that for low-mass stars in the 12-120 Myr age range, the X-ray luminosity is an excellent indicator of youth and better than the more traditionally used R {sub X} parameter, the ratio of X-ray to bolometric luminosity.

  10. Evaluation of residue-residue contact prediction in CASP10

    KAUST Repository

    Monastyrskyy, Bohdan

    2013-08-31

    We present the results of the assessment of the intramolecular residue-residue contact predictions from 26 prediction groups participating in the 10th round of the CASP experiment. The most recently developed direct coupling analysis methods did not take part in the experiment likely because they require a very deep sequence alignment not available for any of the 114 CASP10 targets. The performance of contact prediction methods was evaluated with the measures used in previous CASPs (i.e., prediction accuracy and the difference between the distribution of the predicted contacts and that of all pairs of residues in the target protein), as well as new measures, such as the Matthews correlation coefficient, the area under the precision-recall curve and the ranks of the first correctly and incorrectly predicted contact. We also evaluated the ability to detect interdomain contacts and tested whether the difficulty of predicting contacts depends upon the protein length and the depth of the family sequence alignment. The analyses were carried out on the target domains for which structural homologs did not exist or were difficult to identify. The evaluation was performed for all types of contacts (short, medium, and long-range), with emphasis placed on long-range contacts, i.e. those involving residues separated by at least 24 residues along the sequence. The assessment suggests that the best CASP10 contact prediction methods perform at approximately the same level, and comparably to those participating in CASP9.

  11. Identification and characterization of Clostridium botulinum group III field strains by matrix-assisted laser desorption-ionization time-of-flight mass spectrometry (MALDI-TOF MS).

    Science.gov (United States)

    Bano, Luca; Drigo, Ilenia; Tonon, Elena; Pascoletti, Simone; Puiatti, Cinzia; Anniballi, Fabrizio; Auricchio, Bruna; Lista, Florigio; Montecucco, Cesare; Agnoletti, Fabrizio

    2017-12-01

    Animal botulism is primarily due to botulinum neurotoxin (BoNT) types C, D or their chimeric variants C/D or D/C, produced by Clostridium botulinum group III, which appears to include the genetically indistinguishable Clostridium haemolyticum and Clostridium novyi. In the present study, we used matrix-assisted laser desorption-ionization time-of-flight mass spectrometry (MALDI TOF MS) to identify and characterize 81 BoNT-producing Clostridia isolated in 47 episodes of animal botulism. The instrument's default database, containing no entries for Clostridium botulinum, permitted reliable identification of 26 strains at the genus level. Although supplementation of the database with reference strains enhanced the instrument's ability to identify the neurotoxic strains at the genus level, resolution was not sufficient to recognize field strains at species level. Characterization by MALDI TOF confirmed the well-documented phenotypic and genetic differences between Clostridium botulinum strains of serotypes normally implicated in human botulism (A, B, E, F) and other Clostridium species able to produce BoNTs type C and D. The chimeric and non-chimeric field strains grouped separately. In particular, very low similarity was found between two non-chimeric type C field strains isolated in the same outbreak and the other field strains. This difference was comparable with the differences among the various Clostridia species included in the study. Characterization by MALDI TOF confirmed that BoNT-producing Clostridia isolated from animals are closely related and indistinguishable at the species level from Clostridium haemolyticum and Clostridium novyi reference strains. On the contrary, there seem to be substantial differences among chimeric and some non-chimeric type C strains. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Post-traumatic stress symptoms and childhood abuse categories in a national representative sample for a specific age group: associations to body mass index

    Directory of Open Access Journals (Sweden)

    Sidsel H. Karsberg

    2012-06-01

    Full Text Available Background: Studies of specific groups such as military veterans have found that posttraumatic stress disorder (PTSD is linked to adverse health outcomes including unhealthy weight. The aim of this study was to examine the relationship between PTSD symptoms, experiences of childhood trauma and weight in a community sample. Methods: A stratified random probability survey was conducted in Denmark by the Danish National Centre for Social Research between 2008 and 2009 with 2,981 participants born in 1984, achieving a response rate of 67%. The participants were interviewed with a structured interview with questions pertaining PTSD symptomatology, exposure to childhood abuse, exposure to potentially traumatizing events, height, and weight. Underweight was defined by a body mass index (BMI <18.5, overweight was defined by a BMI ≥25 and <30 and obesity was defined by a BMI ≥30. Results: PTSD symptomatology and childhood abuse were significantly associated with both underweight and overweight/obesity. Childhood emotional abuse was especially associated with underweight, whereas sexual abuse and overall abuse were particularly associated with overweight/obesity. Conclusion: These findings indicate that health care professionals may benefit from assessing PTSD and childhood abuse in the treatment of both overweight and underweight individuals.

  13. A single-step pesticide extraction and clean-up multi-residue analytical method by selective pressurized liquid extraction followed by on-line solid phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for complex matrices.

    Science.gov (United States)

    Rodrigues, Elsa Teresa; Pardal, Miguel Ângelo; Salgueiro-González, Noelia; Muniategui-Lorenzo, Soledad; Alpendurada, Maria Fátima

    2016-06-24

    Pesticides, a group of compounds linked to human activity, may, when in toxic levels, have a profound effect on water quality, and hence result in adverse consequences to aquatic life and ultimately to human health. Analytical challenges arise when successfully trying to determine these levels in environmental complex matrices. Therefore, fast, simple, sensitive and selective analytical methodologies for multi-residue determination of pesticides (atrazine, azoxystrobin, bentazon, λ-cyhalothrin, penoxsulam and terbuthylazine) in sediment, macrophytes (algae and aquatic plants) and aquatic animals were developed and validated. The established methods were matrix-dependent and were based on Selective Pressurized Liquid Extraction (SPLE) followed by on-line Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (on-line SPE-UPLC-ESI-MS/MS). This cutting-edge research methodology uses a small amount of sample, is time saving and reduces the use of organic solvents in compliance with Green Chemistry principles. The analytical features were adequate for all compounds in all studied matrices. The established methodology was applied on real marine samples and no pesticide concentrations above their respective method quantification limits were measured in sediments or aquatic plants. However, terbuthylazine was found in the macroalgae Ulva spp. (108ngg(-1)dw) and all the prospected pesticides were measured above their respective method quantification limits in the bivalve Scrobicularia plana (atrazine: 48ngg(-1)dw, azoxystrobin: 64ngg(-1)dw, bentazon: 33ngg(-1)dw, λ-cyhalothrin: 2531ngg(-1)dw, penoxsulam: 50ngg(-1)dw, and terbuthylazine: 44ngg(-1)dw). Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Simultaneous analysis of aminoglycosides with many other classes of drug residues in bovine tissues by ultrahigh-performance liquid chromatography-tandem mass spectrometry using an ion-pairing reagent added to final extracts

    Science.gov (United States)

    The way to maximize scope of analysis, sample throughput, and laboratory efficiency in the monitoring of veterinary drug residues in food animals is to determine as many analytes as possible as fast as possible in as few methods as possible. Capital and overhead expenses are also reduced by using f...

  15. Determination of six parabens residues in fresh-cut vegetables using QuEChERS with multi-walled carbon nanotubes and high performance liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    In this study, an optimized QuEChERS sample preparation method was developed to analyze residues of six parabens: methyl-, ethyl-, n-propyl-, isopropyl-, n-butyl-, and isobutyl-paraben in five fresh-cut vegetables (potato, broccoli, carrot, celery and cabbage) with high performance liquid chromatogr...

  16. Emissions of volatile organic compounds from maize residue open burning in the northern region of Thailand

    Science.gov (United States)

    Sirithian, Duanpen; Thepanondh, Sarawut; Sattler, Melanie L.; Laowagul, Wanna

    2018-03-01

    Emission factors for speciated volatile organic compounds (VOCs) from maize residue burning were determined in this study based on chamber experiments. Thirty-six VOC species were identified by Gas Chromatography/Mass Spectrometer (GC/MS). They were classified into six groups, including alkanes, alkenes, oxygenated VOCs, halogenated VOCs, aromatics and other. The emission factor for total VOCs was estimated as about 148 mg kg-1 dry mass burned. About 68.4% of the compounds were aromatics. Field samplings of maize residues were conducted to acquire the information of fuel characteristics including fuel loading, fraction of maize residues that were actually burned as well as proximate and elemental analysis of maize residues. The emission factors were then applied to estimate speciated VOC emissions from maize residue open burning at the provincial level in the upper-northern region of Thailand for the year 2014. Total burned area of maize covered an area of about 500,000 ha which was about 4.7% of the total area of upper-northern region of the country. It was found that total VOC emissions released during the burning season (January-April) was about 79.4 tons. Ethylbenzene, m,p-xylene, 1,2,4-trimethylbenzene, acetaldehyde and o-xylene were the major contributors, accounting for more than 65% of total speciated VOC emissions.

  17. Crop residues and agro-industrial by-products used in traditional ...

    African Journals Online (AJOL)

    The crop residues were grouped under cereal crop residues (3), root crop residues (5), legume crop residues (3), and fruit crop residues (3). All the sampled respondents kept livestock and depend on the natural pasture as the main source of feed for their animals. The mean stock number per farmer in this study was 14.0 ...

  18. MORTAR WITH UNSERVICEABLE TIRE RESIDUES

    Directory of Open Access Journals (Sweden)

    J. A. Canova

    2009-01-01

    Full Text Available This study analyzes the effects of unserviceable tire residues on rendering mortar using lime and washed sand at a volumetric proportion of 1:6. The ripened composite was dried in an oven and combined with both cement at a volumetric proportion of 1:1.5:9 and rubber powder in proportional aggregate volumes of 6, 8, 10, and 12%. Water exudation was evaluated in the plastic state. Water absorption by capillarity, fresh shrinkage and mass loss, restrained shrinkage and mass loss, void content, flexural strength, and deformation energy under compression were evaluated in the hardened state. There was an improvement in the water exudation and water absorption by capillarity and drying shrinkage, as well as a reduction of the void content and flexural strength. The product studied significantly aided the water exudation from mortar and, capillary elevation in rendering.

  19. MORTAR WITH UNSERVICEABLE TIRE RESIDUES

    Directory of Open Access Journals (Sweden)

    José Aparecido Canova

    2009-12-01

    Full Text Available This study analyzes the effects of unserviceable tire residues on rendering mortar using lime and washed sand at a volumetric proportion of 1:6. The ripened composite was dried in an oven and combined with both cement at a volumetric proportion of 1:1.5:9 and rubber powder in proportional aggregate volumes of 6, 8, 10, and 12%. Water exudation was evaluated in the plastic state. Water absorption by capillarity, fresh shrinkage and mass loss, restrained shrinkage and mass loss, void content, flexural strength, and deformation energy under compression were evaluated in the hardened state. There was an improvement in the water exudation and water absorption by capillarity and drying shrinkage, as well as a reduction of the void content and flexural strength. The product studied significantly aided the water exudation from mortar and, capillary elevation in rendering.

  20. Selection of basic data for numerical modeling of rock mass stress state at Mirny Mining and Processing Works, Alrosa Group of Companies

    Science.gov (United States)

    Bokiy, IB; Zoteev, OV; Pul, VV; Pul, EK

    2018-03-01

    The influence of structural features on the strength and elasticity modulus is studied in rock mass in the area of Mirny Mining and Processing Works. The authors make recommendations on the values of physical properties of rocks.

  1. The Pan-STARRS1 medium-deep survey: The role of galaxy group environment in the star formation rate versus stellar mass relation and quiescent fraction out to z ∼ 0.8

    International Nuclear Information System (INIS)

    Lin, Lihwai; Chen, Chin-Wei; Coupon, Jean; Hsieh, Bau-Ching; Jian, Hung-Yu; Foucaud, Sebastien; Norberg, Peder; Bower, R. G.; Cole, Shaun; Arnalte-Mur, Pablo; Draper, P.; Heinis, Sebastien; Phleps, Stefanie; Chen, Wen-Ping; Lee, Chien-Hsiu; Burgett, William; Chambers, K. C.; Denneau, L.; Flewelling, H.; Hodapp, K. W.

    2014-01-01

    Using a large optically selected sample of field and group galaxies drawn from the Pan-STARRS1 Medium-Deep Survey (PS1/MDS), we present a detailed analysis of the specific star formation rate (SSFR)—stellar mass (M * ) relation, as well as the quiescent fraction versus M * relation in different environments. While both the SSFR and the quiescent fraction depend strongly on stellar mass, the environment also plays an important role. Using this large galaxy sample, we confirm that the fraction of quiescent galaxies is strongly dependent on environment at a fixed stellar mass, but that the amplitude and the slope of the star-forming sequence is similar between the field and groups: in other words, the SSFR-density relation at a fixed stellar mass is primarily driven by the change in the star-forming and quiescent fractions between different environments rather than a global suppression in the star formation rate for the star-forming population. However, when we restrict our sample to the cluster-scale environments (M > 10 14 M ☉ ), we find a global reduction in the SSFR of the star-forming sequence of 17% at 4σ confidence as opposed to its field counterpart. After removing the stellar mass dependence of the quiescent fraction seen in field galaxies, the excess in the quiescent fraction due to the environment quenching in groups and clusters is found to increase with stellar mass, although deeper and larger data from the full PS1/MDS will be required to draw firm conclusions. We argue that these results are in favor of galaxy mergers to be the primary environment quenching mechanism operating in galaxy groups whereas strangulation is able to reproduce the observed trend in the environment quenching efficiency and stellar mass relation seen in clusters. Our results also suggest that the relative importance between mass quenching and environment quenching depends on stellar mass—the mass quenching plays a dominant role in producing quiescent galaxies for more

  2. Agricultural pesticide residues

    International Nuclear Information System (INIS)

    Fuehr, F.

    1984-01-01

    The utilization of tracer techniques in the study of agricultural pesticide residues is reviewed under the following headings: lysimeter experiments, micro-ecosystems, translocation in soil, degradation of pesticides in soil, biological availability of soil-applied substances, bound residues in the soil, use of macro- and microautography, double and triple labelling, use of tracer labelling in animal experiments. (U.K.)

  3. Role of mammography in evaluating residual cancer of locally advanced breast carcinoma after neo-adjuvant chemotherapy : compared with clinical examination

    International Nuclear Information System (INIS)

    Choi, Byoung Wook; Kim, Eun Kyung; Oh, Ki Keun; Cho, Jae Min; Chung, Hyun Cheol; Lee, Byung Chan; Lee, Kyong Sik; Lee, Yong Hee

    1997-01-01

    To compare the usefulness of mammography and clinical examination in the evaluation of residual cancer of locally-advanced breast carcinoma treated with neoadjuvant chemotherapy. Among 67 patients with locally advanced breast carcinoma who were treated with neoadjuvant chemotherapy, 18, aged 35-67 (mean, 48) years, underwent mammography before and after this therapy. The 18 sets of mammographs were analyzed retrospectively and compared with the results of clinical examination based on histologic diagnosis. On histologic examinations, 16 of 18 patients (89%) were found to have residual cancer, but in one of these 16, mammography did not show this same result. On mammography, residual cancer was found in 16 patients, but in one of this group, histologic examination did not reveal the same finding. Clinically, a complete response was shown by four patients, and a partial response by 11 ; three showed no response. On histolgogic examination, three of the four patients with complete clinical response were found to have residual cancer. Post-treatment mammographic findings showed that 11 patients had measurable mass ; all of these had residual cancer (positive predictive value : 100%). However, five of seven patients in whom no measurable mass was evident also had residual cancer. Seven of 8 patients in whom microcalcifications were seen on mammography were found to have residual cancer (positive predictive value : 88%). The sensitivity of mammography in predicting residual cancer was greater than that of clinical examination (94% vs 81%), even when microscopic residual cancer was considered as a complete response (92% vs 77%). The specificity of mammography was the same as that of clinical examination(50% vs 50%, 20% vs 20%). In evaluating residual cancer of locally-advanced breast carcinoma after neoadjuvant chemotheragy, mammography is more accurate and informative than clincal examination. In predicting residual cancer, however, it is not accurate enough to replace

  4. Improvement and extension to new analytes of a multi-residue method for the determination of pesticides in cereals and dry animal feed using gas chromatography-tandem quadrupole mass spectrometry revisited.

    Science.gov (United States)

    Walorczyk, Stanisław; Drożdżyński, Dariusz

    2012-08-17

    This article describes a substantially improved multi-residue method for the determination of a large number of pesticides in cereal samples (wheat, rye, barley, oats, maze, buckwheat etc.) and various animal feeds. The sample preparation method and the GC-MS/MS acquisition method were modified to accommodate new complex cereal and feed matrices and to extend the existing analytical scope to 167 pesticides. The co-extractives were reduced by the joint use of primary secondary amine (PSA) and octadecyl (C18), 75 mg and 50 mg/1 mL of acetonitrile extract, in the presence of MgSO(4), and thus the optimal recovery and analytical selectivity were obtained simultaneously. The new cleanup procedure was faster and easier to handle than our previously applied cleanup procedure. The overall recoveries of the pesticides from buckwheat and rye at the three spiking levels of 0.01, 0.05 and 0.25 mg kg(-1) were 96 ± 9% with relative standard deviations of 10 ± 4% on average. At the lowest spiking level of 0.01 mg kg(-1), 137 of 167 pesticide residues (82%) fulfilled the validation criteria with recoveries in the range of 70-120% and RSDs less or equal 20% whereas in the previous approach it was 93 out of 140 analytes (66%). The developed method was implemented in a routine analysis of approximately 900 real samples, providing an increased scope of the analysis, improved analytical performance parameters and improved ruggedness versus the previous approach. A total of 17% analyzed samples contained pesticide residues. There were 24 different compounds encountered in the samples, of which pirimiphos-methyl, tebuconazole, deltamethrin, and chlorpyrifos-methyl were the most frequent ones. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Handling of Solid Residues

    International Nuclear Information System (INIS)

    Medina Bermudez, Clara Ines

    1999-01-01

    The topic of solid residues is specifically of great interest and concern for the authorities, institutions and community that identify in them a true threat against the human health and the atmosphere in the related with the aesthetic deterioration of the urban centers and of the natural landscape; in the proliferation of vectorial transmitters of illnesses and the effect on the biodiversity. Inside the wide spectrum of topics that they keep relationship with the environmental protection, the inadequate handling of solid residues and residues dangerous squatter an important line in the definition of political and practical environmentally sustainable. The industrial development and the population's growth have originated a continuous increase in the production of solid residues; of equal it forms, their composition day after day is more heterogeneous. The base for the good handling includes the appropriate intervention of the different stages of an integral administration of residues, which include the separation in the source, the gathering, the handling, the use, treatment, final disposition and the institutional organization of the administration. The topic of the dangerous residues generates more expectation. These residues understand from those of pathogen type that are generated in the establishments of health that of hospital attention, until those of combustible, inflammable type, explosive, radio-active, volatile, corrosive, reagent or toxic, associated to numerous industrial processes, common in our countries in development

  6. On root class residuality of HNN-extensions

    International Nuclear Information System (INIS)

    Tieudjo, D.

    2004-08-01

    A sufficient condition or root-class residuality of HNN-extensions with root-class residual base group is proven; namely if G = -1 1Ht = K, φ> is the HNN-extension with base group A, stable letter t and associated subgroups H and K via the isomorphism φ, then G is root-class residual if group A is root-class residual and there exists a homomorphism σ of group G onto some group of a root-class such that σ is one-to-one on H. For the particular case when H = K and σ is the identical map, it is shown that G is root-class residual if and only if A is root-class residual and subgroup H of A is root-class separable. These results are generalized to multiple HNN-extensions. (author)

  7. Moxidectin residues in tissues of lambs submitted to three endoparasite control programs.

    Science.gov (United States)

    Fernandes, Maria Angela Machado; Gilaverte, Susana; Bianchi, Michele Dell; da Silva, Claudio José Araujo; Molento, Marcelo Beltrão; Reyes, Felix Guillermo Reyes; Monteiro, Alda Lucia Gomes

    2017-10-01

    The indiscriminate and continuous use of anthelmintic drugs has promoted the selection of resistant parasites population, the presence of drug residues in food products, and heavy environmental contamination. The aim of the present study was to determine the presence of antiparasitic drug residues in 42-days old lamb serum and tissues, submitted to three endoparasite control programs: preventive treatment (PT) using moxidectin (MOX) at every 28days; selective treatment (FEC) using MOX when fecal egg count was greater than or equal to 700; and selective treatment (FMC), using MOX when FAMACHA/FMC score was 3 and above. For this purpose, MOX residues were quantified in serum, muscle, fat, liver and kidney. Lambs were slaughtered when reaching 30kg of body weight, and after a 28-day MOX withdrawal period. Before slaughter, blood was collected to determine the concentration of MOX in serum. Tissues and organ samples were collected at slaughter. The quantitation of MOX residues was performed using liquid chromatography tandem mass spectrometry (LC-MS/MS). From the 756 tissue samples analyzed, only one sample of fat from the PT group showed residue levels (586.3μg/kg) above the maximum residue limit (MRL) of 500μg/kg. No treated lambs presented traces of MOX residues in fat and liver, suggesting possible environmental contamination. In conclusion, all weaned lambs, produced in continuous grazing and subjected to gastrointestinal parasite control programs via selective (FEC and FMC) or preventive (PT) treatment, displayed a low risk (residues above the MRL in muscle, fat, kidney, and liver. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Ammoniated maJze residue for the fattening of lambs

    African Journals Online (AJOL)

    of feed cost per kg carcass gain, a balanced diet containing untreated maize residue and 67,6t/a concentrate could be replaced by a balanced diet containing ammoniated maize residue and no energy concentrate. The increased dressing percentage and reduced ruminal digesta mass, pH and water volume owing to ...

  9. Compositional analysis of seasonal variation in Danish residual household waste

    DEFF Research Database (Denmark)

    Edjabou, Maklawe Essonanawe; Boldrin, Alessio; Astrup, Thomas Fruergaard

    2018-01-01

    . To assess differences between seasons and within individual households, we collected residual household waste from the same 101 households in summer, autumn and winter. The waste bags were sorted individually, and residual household waste data (mass and composition) were generated for each household...

  10. Analysis of hazardous organic residues from sodium hydrosulfite industry and utilization as raw materials in a novel solid lubricant production

    Energy Technology Data Exchange (ETDEWEB)

    Shang, Jiwu [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China); Zhang, Yihe, E-mail: zyh@cugb.edu.cn [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China); Department of Physics and Materials Science, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong (China); Zhou, Fengshan; Lv, Fengzhu; Han, Feng; Lu, Jinbo; Meng, Xianghai [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China); Chu, Paul K. [Department of Physics and Materials Science, City University of Hong Kong, Tat Chee Avenue, Kowloon, Hong Kong (China); Ye, Zhengfang [Department of Environmental Engineering, Key Laboratory of Water and Sediment Sciences of the Ministry of Education, Peking University, Beijing 100871 (China); Xing, Jing [State Key Laboratory of Geological Processes and Mineral Resources, National Laboratory of Mineral Materials, School of Materials Science and Technology, China University of Geosciences, Beijing 100083 (China)

    2011-12-30

    Highlights: Black-Right-Pointing-Pointer The hazardous organic residual wastes produced by the sodium hydrosulfite industry are analyzed and the main compounds are found to be thiodiglycol and 2,2 Prime -dithiodiethanol. Black-Right-Pointing-Pointer The lubricity of the organic residues is subsequently studied and the homemade solid lubricant is observed to have good lubricity. Black-Right-Pointing-Pointer The clean process is expected to not only have commercial impact but also help to reduce environmental pollution. - Abstract: The hazardous organic residual wastes produced by the sodium hydrosulfite industry are demonstrated to be convertible into a novel solid lubricant. Identification and isolation of the organic residues are achieved by Fourier transform infrared (FTIR) spectroscopy, gas chromatography-mass spectrometry (GC-MS), and nuclear magnetic resonance (NMR). FTIR and GC-MS provide important information about the residues and the two main components obtained by column chromatography are further analyzed by NMR. The main organic residues are found to be thiodiglycol and 2,2 Prime -dithiodiethanol which have potential applications in petroleum drilling because of their S-S and/or C-S functional groups. The lubricity of the organic residues is subsequently studied and the influence of different adsorbents on the lubricity is investigated and discussed. This homemade lubricant is observed to have good lubricity and by increasing the concentration of the commercial solid lubricant M, the lubricity diminishes. The process is expected to not only have commercial impact but also help to reduce environmental pollution.

  11. Environmental Activism Revisited: The Changing Nature of Communication through Organizational Public Relations, Special Interest Groups and the Mass Media. Monographs in Environmental Education and Environmental Studies, Volume V.

    Science.gov (United States)

    Grunig, Larissa A., Ed.

    The environmental movement of the 1960's and early 1970's resulted in unprecedented attention to environmental issues both in the mass media and in the scholarly literature. Interest has waned in recent years, with a concomitant erosion of coverage of what many consider enduring problems--particularly in water and air pollution and nuclear power.…

  12. [Residual neuromuscular blockade].

    Science.gov (United States)

    Fuchs-Buder, T; Schmartz, D

    2017-06-01

    Even small degrees of residual neuromuscular blockade, i. e. a train-of-four (TOF) ratio >0.6, may lead to clinically relevant consequences for the patient. Especially upper airway integrity and the ability to swallow may still be markedly impaired. Moreover, increasing evidence suggests that residual neuromuscular blockade may affect postoperative outcome of patients. The incidence of these small degrees of residual blockade is relatively high and may persist for more than 90 min after a single intubating dose of an intermediately acting neuromuscular blocking agent, such as rocuronium and atracurium. Both neuromuscular monitoring and pharmacological reversal are key elements for the prevention of postoperative residual blockade.

  13. TENORM: Wastewater Treatment Residuals

    Science.gov (United States)

    Water and wastes which have been discharged into municipal sewers are treated at wastewater treatment plants. These may contain trace amounts of both man-made and naturally occurring radionuclides which can accumulate in the treatment plant and residuals.

  14. Residuation in orthomodular lattices

    Directory of Open Access Journals (Sweden)

    Chajda Ivan

    2017-04-01

    Full Text Available We show that every idempotent weakly divisible residuated lattice satisfying the double negation law can be transformed into an orthomodular lattice. The converse holds if adjointness is replaced by conditional adjointness. Moreover, we show that every positive right residuated lattice satisfying the double negation law and two further simple identities can be converted into an orthomodular lattice. In this case, also the converse statement is true and the corresponence is nearly one-to-one.

  15. The Mass-Dimension Relationships in the Mussels Mytilus Galloprovincialis (Mollusca, Bivalvia from Different Phenotypical Groups in Periphyton Populations near Odessa Coast, the North-Western Part of Black Sea

    Directory of Open Access Journals (Sweden)

    Govorin I. A.

    2016-06-01

    Full Text Available The data of the size-mass indices in the mussels Mytilus galloprovincialis (Lamarck, 1819 from three phenotypic groups - brown, dark violet (black and “zebra” (brown with radial black stripes shells in the periphyton settlements on the concrete traverses near Odessa coast, the North-western part of Black Sea (Ukraine, in March-November 2014-2015 are presented. A comparative evaluation has been made on the relationships of total mass of the mollusks, wet and dry mass of their soft body and mass of the shells on the one hand, and the size of animals (length of its shells on the other hand, in the each of phenotypical groups from the five marine beach areas. It is shown, that in the marine areas with different degrees of isolation from the open sea by coast-protection engineering constructions, the mussels from different phenotypes have almost the same size-mass characteristics. Only the dry weight of soft animal body, which indicated to fatness of mollusk and therefore demonstrated his biological prosperity in specific hydrological conditions, can serve as a reliable criterion which can mark the shellfish habitats with different gradients of environmental factors.

  16. Characterization of Hospital Residuals

    International Nuclear Information System (INIS)

    Blanco Meza, A.; Bonilla Jimenez, S.

    1997-01-01

    The main objective of this investigation is the characterization of the solid residuals. A description of the handling of the liquid and gassy waste generated in hospitals is also given, identifying the source where they originate. To achieve the proposed objective the work was divided in three stages: The first one was the planning and the coordination with each hospital center, in this way, to determine the schedule of gathering of the waste can be possible. In the second stage a fieldwork was made; it consisted in gathering the quantitative and qualitative information of the general state of the handling of residuals. In the third and last stage, the information previously obtained was organized to express the results as the production rate per day by bed, generation of solid residuals for sampled services, type of solid residuals and density of the same ones. With the obtained results, approaches are settled down to either determine design parameters for final disposition whether for incineration, trituration, sanitary filler or recycling of some materials, and storage politics of the solid residuals that allow to determine the gathering frequency. The study concludes that it is necessary to improve the conditions of the residuals handling in some aspects, to provide the cleaning personnel of the equipment for gathering disposition and of security, minimum to carry out this work efficiently, and to maintain a control of all the dangerous waste, like sharp or polluted materials. In this way, an appreciable reduction is guaranteed in the impact on the atmosphere. (Author) [es

  17. Protein structure based prediction of catalytic residues

    Science.gov (United States)

    2013-01-01

    Background Worldwide structural genomics projects continue to release new protein structures at an unprecedented pace, so far nearly 6000, but only about 60% of these proteins have any sort of functional annotation. Results We explored a range of features that can be used for the prediction of functional residues given a known three-dimensional structure. These features include various centrality measures of nodes in graphs of interacting residues: closeness, betweenness and page-rank centrality. We also analyzed the distance of functional amino acids to the general center of mass (GCM) of the structure, relative solvent accessibility (RSA), and the use of relative entropy as a measure of sequence conservation. From the selected features, neural networks were trained to identify catalytic residues. We found that using distance to the GCM together with amino acid type provide a good discriminant function, when combined independently with sequence conservation. Using an independent test set of 29 annotated protein structures, the method returned 411 of the initial 9262 residues as the most likely to be involved in function. The output 411 residues contain 70 of the annotated 111 catalytic residues. This represents an approximately 14-fold enrichment of catalytic residues on the entire input set (corresponding to a sensitivity of 63% and a precision of 17%), a performance competitive with that of other state-of-the-art methods. Conclusions We found that several of the graph based measures utilize the same underlying feature of protein structures, which can be simply and more effectively captured with the distance to GCM definition. This also has the added the advantage of simplicity and easy implementation. Meanwhile sequence conservation remains by far the most influential feature in identifying functional residues. We also found that due the rapid changes in size and composition of sequence databases, conservation calculations must be recalibrated for specific

  18. Multi-residue method for the determination of over 400 priority and emerging pollutants in water and wastewater by solid-phase extraction and liquid chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Robles-Molina, José; Lara-Ortega, Felipe J; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

    2014-07-11

    This article describes the development and validation of a liquid chromatography high-resolution mass spectrometry method for the simultaneous determination of over 400 multi-class priority and emerging pollutants with different physicochemical properties in environmental waters (surface water and wastewater). The proposed approach is based on the use of a database consisting of retention time/exact mass (of selected ions) pairs implemented with specific software for data analysis. The targeted list comprises 430 contaminants belonging to different compound categories, including 105 multiclass pharmaceuticals (analgesics/anti-inflammatories, antibiotics, lipid regulators, β-blockers, antiepileptic/psychiatrics ulcer healings, diuretics, hormones and bronchodilatadors), life-style products (caffeine, nicotine), 21 drugs of abuse and their metabolites, 279 pesticides and some of their more relevant metabolites, nitrosamines, flame retardants, plasticizers and perfluorinated compounds. The proposed approach included a simple offline solid phase extraction (SPE) step using polymeric cartridges (Oasis HLB) with 200mL of water sample loaded, followed by analysis by rapid resolution liquid chromatography electrospray time-of-flight mass spectrometry (LC-TOFMS) in both positive and negative modes. The identification of the positive findings is accomplished with the data from accurate masses of the target ions along with retention time data and characteristic in-source fragment ions. The overall method performance was satisfactory with limits of quantification lower than 10ngL(-1) for the 44% of studied compounds. Recoveries between 50% and 130% were obtained for the 65% of the analytes (281 compounds). Matrix effects occurring with wastewater matrices were also assessed. The developed method was applied to the determination of target analytes in real surface water and wastewater samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Classification of crops grown in or imported into the European Union for pesticide residue assessment

    OpenAIRE

    Velde-Koerts T van der; Muller E; Ossendorp BHC; Plantenziektenkundige dienst; SIR; Plantenziektenkundige Dienst

    2003-01-01

    An important aspect of food safety is the control of pesticide residues on food. Pesticide residue assessments are conducted to establish legal limits, known as maximum residue limits (MRLs), for pesticide residues in plant and animal commodities. In the EC guidelines for pesticide residue assessment, the so-called Lundehn document, agricultural crops are classified into groups in which results are considered to be comparable. Within these groups, the results for one crop may be extrapolated,...

  20. Management of NORM Residues

    International Nuclear Information System (INIS)

    2013-06-01

    The IAEA attaches great importance to the dissemination of information that can assist Member States in the development, implementation, maintenance and continuous improvement of systems, programmes and activities that support the nuclear fuel cycle and nuclear applications, and that address the legacy of past practices and accidents. However, radioactive residues are found not only in nuclear fuel cycle activities, but also in a range of other industrial activities, including: - Mining and milling of metalliferous and non-metallic ores; - Production of non-nuclear fuels, including coal, oil and gas; - Extraction and purification of water (e.g. in the generation of geothermal energy, as drinking and industrial process water; in paper and pulp manufacturing processes); - Production of industrial minerals, including phosphate, clay and building materials; - Use of radionuclides, such as thorium, for properties other than their radioactivity. Naturally occurring radioactive material (NORM) may lead to exposures at some stage of these processes and in the use or reuse of products, residues or wastes. Several IAEA publications address NORM issues with a special focus on some of the more relevant industrial operations. This publication attempts to provide guidance on managing residues arising from different NORM type industries, and on pertinent residue management strategies and technologies, to help Member States gain perspectives on the management of NORM residues

  1. Determination of Pesticide Residues in Cannabis Smoke

    Directory of Open Access Journals (Sweden)

    Nicholas Sullivan

    2013-01-01

    Full Text Available The present study was conducted in order to quantify to what extent cannabis consumers may be exposed to pesticide and other chemical residues through inhaled mainstream cannabis smoke. Three different smoking devices were evaluated in order to provide a generalized data set representative of pesticide exposures possible for medical cannabis users. Three different pesticides, bifenthrin, diazinon, and permethrin, along with the plant growth regulator paclobutrazol, which are readily available to cultivators in commercial products, were investigated in the experiment. Smoke generated from the smoking devices was condensed in tandem chilled gas traps and analyzed with gas chromatography-mass spectrometry (GC-MS. Recoveries of residues were as high as 69.5% depending on the device used and the component investigated, suggesting that the potential of pesticide and chemical residue exposures to cannabis users is substantial and may pose a significant toxicological threat in the absence of adequate regulatory frameworks.

  2. Postinduction Minimal Residual Disease Predicts Outcome and Benefit From Allogeneic Stem Cell Transplantation in Acute Myeloid Leukemia With NPM1 Mutation: A Study by the Acute Leukemia French Association Group.

    Science.gov (United States)

    Balsat, Marie; Renneville, Aline; Thomas, Xavier; de Botton, Stéphane; Caillot, Denis; Marceau, Alice; Lemasle, Emilie; Marolleau, Jean-Pierre; Nibourel, Olivier; Berthon, Céline; Raffoux, Emmanuel; Pigneux, Arnaud; Rodriguez, Céline; Vey, Norbert; Cayuela, Jean-Michel; Hayette, Sandrine; Braun, Thorsten; Coudé, Marie Magdeleine; Terre, Christine; Celli-Lebras, Karine; Dombret, Hervé; Preudhomme, Claude; Boissel, Nicolas

    2017-01-10

    Purpose This study assessed the prognostic impact of postinduction NPM1-mutated ( NPM1m) minimal residual disease (MRD) in young adult patients (age, 18 to 60 years) with acute myeloid leukemia, and addressed the question of whether NPM1m MRD may be used as a predictive factor of allogeneic stem cell transplantation (ASCT) benefit. Patients and Methods Among 229 patients with NPM1m who were treated in the Acute Leukemia French Association 0702 (ALFA-0702) trial, MRD evaluation was available in 152 patients in first remission. Patients with nonfavorable AML according to the European LeukemiaNet (ELN) classification were eligible for ASCT in first remission. Results After induction therapy, patients who did not achieve a 4-log reduction in NPM1m peripheral blood-MRD (PB-MRD) had a higher cumulative incidence of relapse (subhazard ratio [SHR], 5.83; P benefit was not observed in those with a > 4-log reduction in PB-MRD, with a significant interaction between ASCT effect and PB-MRD response ( P = .024 and .027 for disease-free survival and OS, respectively). Conclusion Our study supports the strong prognostic significance of early NPM1m PB-MRD, independent of the cytogenetic and molecular context. Moreover, NPM1m PB-MRD may be used as a predictive factor for ASCT indication.

  3. Characterization of microwave liquefied bamboo residue and its potential use in the generation of nanofibrillated cellulosic fiber

    Science.gov (United States)

    Jiulong Xie; Chung Hse; Chunjie Li; Todd F. Shupe; Tingxing Hu; Jinqiu Qi; Cornelis F. De Hoop

    2016-01-01

    Bamboo raw feedstocks with large particle size (20−80 mesh) were subjected to a microwave liquefaction system, and the liquefied products were separated into biopolyols and liquefied residues. Biopolyols were first analyzed by gas chromatography mass spectrometry (GC−MS), and the main components were sugar derivatives with 2−4 hydroxyl groups and phenolic compounds...

  4. A simple multi-residue method for the determination of pesticides in fruits and vegetables using a methanolic extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry: optimization and extension of scope.

    Science.gov (United States)

    Hanot, V; Goscinny, S; Deridder, M

    2015-03-06

    In 2004, a new multi-residue pesticides method had been published using methanol as extraction solvent. Our goal for this study was to optimize the analytical scheme while extending the compound scope from 19 to 200 pesticides. The main changes from the original method take place at the sample extraction and processing with a special attention to make the overall method fit for routine analysis with minimal cost. Hence, after a quick Ultra-Turrax homogenization with a methanolic solution, the sample is simply diluted before the separation and detection by ultra-high-performance liquid chromatography and MS/MS detection for quantitative and confirmatory purposes. The performance of the method including limits of quantification (LOQs), linearity, matrix effect, precision was evaluated during validation in accordance with the European Union SANCO/12571/2013 regulatory guidelines. Two representative matrices, lettuce and orange, were selected and fortified at two concentration levels for these experiments. At the LOQ and ten times the LOQ, recoveries of the analytes were mostly within 70-120%, with coefficients of variation lower than 25% in intra-day repeatability conditions. In addition to being simple and fast, these results demonstrate the suitability of the optimized method for the analysis of large scope pesticides in routine laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Residual-stress measurements

    Energy Technology Data Exchange (ETDEWEB)

    Ezeilo, A.N.; Webster, G.A. [Imperial College, London (United Kingdom); Webster, P.J. [Salford Univ. (United Kingdom)

    1997-04-01

    Because neutrons can penetrate distances of up to 50 mm in most engineering materials, this makes them unique for establishing residual-stress distributions non-destructively. D1A is particularly suited for through-surface measurements as it does not suffer from instrumental surface aberrations commonly found on multidetector instruments, while D20 is best for fast internal-strain scanning. Two examples for residual-stress measurements in a shot-peened material, and in a weld are presented to demonstrate the attractive features of both instruments. (author).

  6. 40 CFR 180.627 - Fluopicolide; tolerances for residues.

    Science.gov (United States)

    2010-07-01

    ... combined residues of fluopicolide and its metabolite, 2,6-dichlorobenzamide (BAM). Commodity Parts per... brassica, group 4 25 Vegetable, leaves of root and tuber, group 2 15.0 Vegetable, root, subgroup 1A, except...

  7. Accumulation of clenbuterol residues in the hair of Chinese Simmental beef cattle during and after treatment.

    Science.gov (United States)

    Li, Lijun; Zhang, Junmin; Tang, Chaohua; Zhao, Qingyu

    2014-01-01

    The aim of this study was to evaluate the concentrations of clenbuterol residues in the red hair of Chinese Simmental beef cattle following exposure to two doses of clenbuterol for 21 days. This experiment was conducted in six male red pied Chinese Simmental beef cattle which were randomly divided into two groups (n = 3). Groups 1 and 2 were administered clenbuterol at a dose of 16 and 48 μg/kg body weight (BW)/day, respectively. Hair samples were collected on Days 7, 14 and 21 during treatment, and on Days 0, 14, 28, 42 and 70 after discontinuation of medication, using liquid chromatography tandem mass spectrometry (LC-MS-MS) method. About 500 mg hair samples spiked with 50 pg/mg D9-clenbuterol internal standard were analyzed with which the method recovery was from 88.6 to 116.9%. The results showed that clenbuterol was significantly accumulated in hair, with a concentration of 0.98 ± 0.56 pg/mg in Group 1 and 6.34 ± 3.21 pg/mg in Group 2 on Day 7 of treatment, and the residue concentrations increased as treatment proceeded. During the early withdrawal period, the residues increased from 13.52 ± 8.69 to 17.96 ± 6.94 pg/mg in Group 1 and from 55.15 ± 4.04 to 147.79 ± 15.35 pg/mg in Group 2. No significant differences were found in the later withdrawal period in both treatment groups. The results of the present study indicated that the red hair of Chinese Simmental beef cattle has high accumulation potential for clenbuterol residues. Hair, as a target matrix, even light-pigmented hair, can be used to monitor clenbuterol abuse over a long period.

  8. Structure and end-group analysis of complex hexanediol-neopentylglycol-adipic acid copolyesters by matrix-assisted laser desorption/ionization collision-induced dissociation tandem mass spectrometry.

    Science.gov (United States)

    Weidner, Steffen M; Falkenhagen, Jana; Knop, Karin; Thünemann, Andreas

    2009-09-01

    Sequences and end groups of complex copolyesters were determined by fragmentation analysis by means of matrix-assisted laser desorption/ionization collision-induced dissociation tandem mass spectrometry (MALDI CID MS/MS). The complexity of the crude copolyester mixture was reduced by a chromatographic separation followed by a MALDI time-of-flight (TOF) investigation of fractions. Due to overlapping compositional and end-group information a clear assignment of end groups was very difficult. However, the fragmentation of suitable precursor ions resulted in typical fragment ion patterns and, therefore, enabled a fast and unambiguous determination of the end groups and composition of this important class of polymers. Copyright (c) 2009 John Wiley & Sons, Ltd.

  9. Proceedings of the Annual Meeting of the Association for Education in Journalism and Mass Communication (83rd, Phoenix, Arizona, August 9-12, 2000). Graduate Education Interest Group.

    Science.gov (United States)

    Association for Education in Journalism and Mass Communication.

    The Graduate Education Interest Group section of the proceedings contains the following five papers: "The Press, President, and Presidential Popularity During Ronald Reagan's War on Drugs" (Hyo-Seong Lee); "Malaysia's Broadcasting Industry in Transition: Effect of New Competitions on Traditional Television Channels" (Tee-Tuan…

  10. A Higgs at 125.1 GeV and baryon mass spectra derived from a Common U(3) Lie group framework

    DEFF Research Database (Denmark)

    Trinhammer, Ole; Bohr, Henrik; Jensen, Mogens O Stibius

    2015-01-01

    Baryons are described by a Hamiltonian on an intrinsic U(3) Lie group configuration space with electroweak degrees of freedom originating in specific Bloch wave factors. By opening the Bloch degrees of freedom pairwise via a U(2) Higgs mechanism, the strong and electroweak energy scales become...

  11. Composition of carbonization residues

    Energy Technology Data Exchange (ETDEWEB)

    Hupfer; Leonhardt

    1943-11-27

    This report compared the composition of samples from Wesseling and Leuna. In each case the sample was a residue from carbonization of the residues from hydrogenation of the brown coal processed at the plant. The composition was given in terms of volatile components, fixed carbon, ash, water, carbon, hydrogen, oxygen, nitrogen, volatile sulfur, and total sulfur. The result of carbonization was given in terms of (ash and) coke, tar, water, gas and losses, and bitumen. The composition of the ash was given in terms of silicon dioxide, ferric oxide, aluminum oxide, calcium oxide, magnesium oxide, potassium and sodium oxides, sulfur trioxide, phosphorus pentoxide, chlorine, and titanium oxide. The most important difference between the properties of the two samples was that the residue from Wesseling only contained 4% oil, whereas that from Leuna had about 26% oil. Taking into account the total amount of residue processed yearly, the report noted that better carbonization at Leuna could save 20,000 metric tons/year of oil. Some other comparisons of data included about 33% volatiles at Leuna vs. about 22% at Wesseling, about 5 1/2% sulfur at Leuna vs. about 6 1/2% at Leuna, but about 57% ash for both. Composition of the ash differed quite a bit between the two. 1 table.

  12. Designing with residual materials

    NARCIS (Netherlands)

    Walhout, W.; Wever, R.; Blom, E.; Addink-Dölle, L.; Tempelman, E.

    2013-01-01

    Many entrepreneurial businesses have attempted to create value based on the residual material streams of third parties. Based on ‘waste’ materials they designed products, around which they built their company. Such activities have the potential to yield sustainable products. Many of such companies

  13. VizieR Online Data Catalog: Low-mass stars in 25 Ori group and Orion OB1a (Suarez+, 2017)

    Science.gov (United States)

    Suarez, G.; Downes, J. J.; Roman-Zuniga, C.; Covey, K. R.; Tapia, M.; Hernandez, J.; Petr-Gotzens, M. G.; Stassun, K. G.; Briceno, C.

    2017-09-01

    The V, R, and I photometry used in this work was obtained from the Centro de Investigaciones de Astronomia (CIDA) Deep Survey of Orion (CDSO) catalog (Downes et al. 2014, Cat. J/MNRAS/444/1793), which was constructed by coadding the multi-epoch optical observations from the CIDA Variability Survey of Orion (CVSO; Briceno et al. 2005, Cat. J/AJ/129/907). The sensitivity limits of the CDSO covers the Low-Mass Star (LMS) and Brown Dwarf (BD) population of 25 Ori and its surroundings within the region 79.7°Digital Sky Survey (SDSS) catalog (Finkbeiner et al. 2004AJ....128.2577F; Ahn et al. 2012, Cat. V/139). These values are listed in Table1. The Z, Y, J, H, and Ks near-infrared photometry used in this study was carried out by Petr-Gotzens et al. (2011Msngr.145...29P) as part of the Visible and Infrared Survey Telescope for Astronomy (VISTA) science verification surveys (Arnaboldi et al. 2010Msngr.139....6A). The 5σ limiting magnitudes of the VISTA survey of the Orion star-forming region are Z=22.5, Y=21.2, J=20.4, H=19.4, and Ks=18.6, which are enough to have VISTA photometry even for the faintest objects in our spectroscopic sample (J{approx}15.0). Additionally, we used near-infrared photometry from the 2MASS catalog (Cutri et al. 2003, Cat. II/246) and mid-infrared photometry from IRAC-Spitzer (Hernandez et al. 2007, Cat. J/ApJ/671/1784) and the AllWISE catalog (Cutri et al. 2013, Cat. II/328). This infrared photometry is listed in Table1. The spectra used in this paper were obtained as part of the Baryon Oscillation Spectroscopic Survey (BOSS; Dawson et al. 2013AJ....145...10D), which is one of the four main surveys of SDSS (York et al. 2000AJ....120.1579Y) in its third phase (SDSS-III; Eisenstein et al. 2011AJ....142...72E). The BOSS spectrograph has plates with 1000 fibers of 2'' diameter spanning a field of view of 3.0° in diameter and covering a wavelength range from 3560Å to 10400Å with a resolution of R=1560 at 3700Å and R=2650 at 9000Å (Gunn et al

  14. Determinação de resíduos de pesticidas em plasma bovino por cromatografia gasosa-espectrometria de massas Pesticides residue determination in cattle plasma by gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Daniele Fernanda Maffei

    2009-01-01

    Full Text Available An analytical method for the isolation based on matrix solid-phase dispersion technique and gas chromatographic determination of pesticides in cattle plasma is presented. It was fortified 0.25 g of plasma with pesticides and blended with 1 g each C18 and Na2SO4. The homogenized matter was transferred to a SPE cartridge, which contained 1 g of activated florisil with 5 mL acetonitrile. The analites were eluted under vaccum with 15 mL acetonitrile, the extract was analyzed by gas chromatography-mass spectrometry. The limit of quantification of the method was 0.04 mg L-1 for chlorphenvinfos and fipronil and 0.02 mg L-1 for cypermethrin..

  15. Residual Stresses in Thermoplastic Composites: A Review

    Directory of Open Access Journals (Sweden)

    M.M. Shokrieh

    2008-12-01

    Full Text Available Applications of thermoplastic composites have developed extensively. The thermoplastic composites in comparison with the thermoset composites have many advantages. Thermoplastic composites can be melted and remolded many times. The duration of manufacturing process of these composites is short, producing very tough material, and the welding ability and multiple recyclings are their further advantages. The lack of knowledge in this group of composites is the main obstacle in their development. In this review the research works in the field of residual stresses in thermoplastic composites is presented. First, a literature survey on the available research on residual stresses on thermoplastics and thermoplastic composites reinforced with short fibers is compiled. Moreover a review on the available research on residual stresses on thermoplastic composites reinforced with long fibers is presented as well. The effects of the residual stresses on these composites are discussed. Experimental techniques for the measurement of residual stresses in thermoplastic composites and the methods for reducing the existing residual stresses are studied.

  16. Galaxies in x-ray selected clusters and groups in Dark Energy Survey Data I: Stellar mass growth of bright central galaxies since Z similar to 1.2

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Y.; Miller, C.; McKay, T.; Rooney, P.; Evrard, A. E.; Romer, A. K.; Perfecto, R.; Song, J; Desai, S.; Mohr, J. J.; Vikram, V.

    2016-01-10

    Using the science verification data of the Dark Energy Survey for a new sample of 106 X-ray selected clusters and groups, we study the stellar mass growth of bright central galaxies (BCGs) since redshift z similar to 1.2. Compared with the expectation in a semi-analytical model applied to the Millennium Simulation, the observed BCGs become under-massive/under-luminous with decreasing redshift. We incorporate the uncertainties associated with cluster mass, redshift, and BCG stellar mass measurements into an analysis of a redshift-dependent BCG-cluster mass relation, m(*) proportional to (M-200/1.5 x 10(14)M(circle dot))(0.24 +/- 0.08)(1+z)(-0.19 +/- 0.34), and compare the observed relation to the model prediction. We estimate the average growth rate since z = 1.0 for BCGs hosted by clusters of M-200,M-z = 10(13.8)M(circle dot); at z = 1.0: m(*, BCG) appears to have grown by 0.13 +/- 0.11 dex, in tension at the similar to 2.5 sigma significance level with the 0.40 dex growth rate expected from the semi-analytic model. We show that the build-up of extended intracluster light after z = 1.0 may alleviate this tension in BCG growth rates.

  17. Residual stresses in material processing

    Science.gov (United States)

    Kozaczek, K. J.; Watkins, T. R.; Hubbard, C. R.; Wang, Xun-Li; Spooner, S.

    Material manufacturing processes often introduce residual stresses into the product. The residual stresses affect the properties of the material and often are detrimental. Therefore, the distribution and magnitude of residual stresses in the final product are usually an important factor in manufacturing process optimization or component life prediction. The present paper briefly discusses the causes of residual stresses. It then addresses the direct, nondestructive methods of residual stress measurement by X ray and neutron diffraction. Examples are presented to demonstrate the importance of residual stress measurement in machining and joining operations.

  18. Dietary exposure to tetracycline residues through milk consumption in Iran

    OpenAIRE

    Aalipour, Fathollah; Mirlohi, Maryam; Jalali, Mohammad; Azadbakht, Leila

    2015-01-01

    Background The abundant use of tetracycline antibiotics in veterinary medicine may result in the presence of their residues in milk at unsafe concentrations that can adversely affect public health. The aim of the current study was to evaluate the risk of tetracycline residue (TET) intake via milk consumption amongst different age groups of human consumers in Iran. Methods To quantify the drug residues, HPLC analysis was performed under isocratic conditions using UV detection at 355?nm. Milk c...

  19. Chemoselective synthesis of functional homocysteine residues in polypeptides and peptides.

    Science.gov (United States)

    Gharakhanian, Eric G; Deming, Timothy J

    2016-04-18

    A methodology was developed for efficient, chemoselective transformation of methionine residues into stable, functional homocysteine derivatives. Methionine residues can undergo highly chemoselective alkylation reactions at low pH to yield stable sulfonium ions, which could then be selectively demethylated to give stable alkyl homocysteine residues. This mild, two-step process is chemoselective, efficient, tolerates many functional groups, and provides a means for creation of new functional biopolymers, site-specific peptide tagging, and synthesis of biomimetic and structural analogs of peptides.

  20. Residual stresses analysis by X-ray and neutrons diffraction

    International Nuclear Information System (INIS)

    Lodini, A.; Perrin, M.

    1996-04-01

    This conference is composed of 17 papers grouped in 13 chapters which main themes are: advantages of neutrons and synchrotron radiation for material characterization; residual stress evaluation from micro-deformation measurements in polycrystalline materials; X-ray and neutron diffractometry; residual stress evaluation by X-ray diffraction in extreme surfaces; residual stress diffraction evaluation in monocrystalline nickel base alloys, in polyphasic materials, composite materials, thin films, multilayers and joints; application to thermonuclear reactor components

  1. Salting-out assisted liquid-liquid extraction coupled to ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of tetracycline residues in infant foods.

    Science.gov (United States)

    Moreno-González, David; García-Campaña, Ana M

    2017-04-15

    The use of salting-out assisted liquid-liquid extraction (SALLE) combined with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been evaluated for the determination of tetracyclines in infant foods based on meat and vegetables or in milk. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized. Analytical performances of the method were satisfactory, obtaining limits of quantification lower than 0.48μgkg -1 in all cases. The precision, expressed as relative standard deviation (%, RSD) was below 11.3%. The extraction efficiency for fortified samples ranged from 89.2 to 96.8%, with RSDs lower than 7.3%. Matrix effect was evaluated for all samples studied, being lower than |21|% in all cases. In relation to the low solvent consumption, the proposed methodology could be considered rapid, cheap and environmentally friendly. Its applicability has been successfully tested in a wide range of infant foods. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Processes of change in quality of life, weight self-stigma, body mass index and emotional eating after an acceptance-, mindfulness- and compassion-based group intervention (Kg-Free) for women with overweight and obesity.

    Science.gov (United States)

    Palmeira, Lara; Cunha, Marina; Pinto-Gouveia, José

    2017-01-01

    This study examined the effectiveness of Kg-Free: an acceptance-, mindfulness- and compassion-based group intervention for women with overweight and obesity at post-treatment and 3-month follow-up and explored the psychological processes that underlie changes in quality of life, weight self-stigma, body mass index and emotional eating at post-treatment. Overall, 53 women completed Kg-Free. At post-treatment and 3-month follow-up, participants reported increased quality of life, mindfulness and self-compassion abilities and decreased weight self-stigma, emotional eating, shame, weight-related experiential avoidance, self-criticism and body mass index. Shame and self-criticism reductions were important mediators of changes in health-related outcomes, whereas weight-related experiential avoidance, mindfulness and self-compassion mediated changes in weight and eating-related outcomes.

  3. SRC Residual fuel oils

    Science.gov (United States)

    Tewari, Krishna C.; Foster, Edward P.

    1985-01-01

    Coal solids (SRC) and distillate oils are combined to afford single-phase blends of residual oils which have utility as fuel oils substitutes. The components are combined on the basis of their respective polarities, that is, on the basis of their heteroatom content, to assure complete solubilization of SRC. The resulting composition is a fuel oil blend which retains its stability and homogeneity over the long term.

  4. Composition of carbonization residues

    Energy Technology Data Exchange (ETDEWEB)

    Hupfer; Leonhardt

    1943-11-30

    This report gave a record of the composition of several samples of residues from carbonization of various hydrogenation residue from processing some type of coal or tar in the Bergius process. These included Silesian bituminous coal processed at 600 atm. with iron catalyst, in one case to produce gasoline and middle oil and in another case to produce heavy oil excess, Scholven coal processed at 250 atm. with tin oxalate and chlorine catalyst, Bruex tar processed in a 10-liter oven using iron catalyst, and a pitch mixture from Welheim processed in a 10-liter over using iron catalyst. The values gathered were compared with a few corresponding values estimated for Boehlen tar and Gelsenberg coal based on several assumptions outlined in the report. The data recorded included percentage of ash in the dry residue and percentage of carbon, hydrogen, oxygen, nitrogen, chlorine, total sulfur, and volatile sulfur. The percentage of ash varied from 21.43% in the case of Bruex tar to 53.15% in the case of one of the Silesian coals. Percentage of carbon varied from 44.0% in the case of Scholven coal to 78.03% in the case of Bruex tar. Percentage of total sulfur varied from 2.28% for Bruex tar to a recorded 5.65% for one of the Silesian coals and an estimated 6% for Boehlen tar. 1 table.

  5. Monitoring antibiotic residues in honey

    Directory of Open Access Journals (Sweden)

    Monica Cristina Cara,

    2011-12-01

    Full Text Available Next to the beta-lactam antibiotics in veterinary medicine, streptomycin is one of the mostly used antibiotics. High concentration of streptomycin could lead to ototoxic and nephrotoxic effects. Low concentration – as found in food – may cause allergies, destroy the intestinal flora and favor immunity to some pathogenic microorganisms. In 1948 chlortetracycline was isolated by Duggan as a metabolite and this was the first antibiotic substance of the group of tetracyclines. In the present paper there are presented the monitoring of the antibiotic residues in honey from Timis County. The residues of tetracycline and streptomycin in honey were determined by the method ELISA – a quantitative method of detection. The microtitre wells are coated with tetracycline and anti-streptomycin antibodies. Free antibiotic and immobilized antibiotic compete with the added antibiotic antibody (competitive immunoassay reaction. Any unbound antibody is then removed in a washing step. Bound conjugate enzymes convert the colorless chromogen into a blue product. The addition ofthe stop reagent leads to a color change from blue to yellow. The measurement is made photometrically at 450 nm. The absorption is inversely proportional to the antibiotic concentration in the sample.

  6. Development of an analytical method for the targeted screening and multi-residue quantification of environmental contaminants in urine by liquid chromatography coupled to high resolution mass spectrometry for evaluation of human exposures.

    Science.gov (United States)

    Cortéjade, A; Kiss, A; Cren, C; Vulliet, E; Buleté, A

    2016-01-01

    The aim of this study was to develop an analytical method and contribute to the assessment of the Exposome. Thus, a targeted analysis of a wide range of contaminants in contact with humans on daily routines in urine was developed. The method focused on a list of 38 contaminants, including 12 pesticides, one metabolite of pesticide, seven veterinary drugs, five parabens, one UV filter, one plastic additive, two surfactants and nine substances found in different products present in the everyday human environment. These contaminants were analyzed by high performance liquid chromatography coupled to high resolution mass spectrometry (HPLC-HRMS) with a quadrupole-time-of-flight (QqToF) instrument from a raw urinary matrix. A validation according to the FDA guidelines was employed to evaluate the specificity, linear or quadratic curve fitting, inter- and intra-day precision, accuracy and limits of detection and quantification (LOQ). The developed analysis allows for the quantification of 23 contaminants in the urine samples, with the LOQs ranging between 4.3 ng.mL(-1) and 113.2 ng.mL(-1). This method was applied to 17 urine samples. Among the targeted contaminants, four compounds were detected in samples. One of the contaminants (tributyl phosphate) was detected below the LOQ. The three others (4-hydroxybenzoic acid, sodium dodecylbenzenesulfonate and O,O-diethyl thiophosphate potassium) were detected but did not fulfill the validation criteria for quantification. Among these four compounds, two of them were found in all samples: tributyl phosphate and the surfactant sodium dodecylbenzenesulfonate. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Optimization and application of fabric phase sorptive extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry for the determination of cytostatic drug residues in environmental waters.

    Science.gov (United States)

    Santana-Viera, Sergio; Guedes-Alonso, Rayco; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan; Kabir, Abuzar; Furton, Kenneth G

    2017-12-22

    Every year, hundreds of tons of organic pollutants reach the environment through effluents released from wastewater treatment plants worldwide, and many of these compounds have harmful effects on the aquatic ecosystem. A new class of emerging pollutants of high concern is cytostatic drugs, which are designed to treat different types of cancers by attacking cells. Environmental concentrations of cytostatic drugs are known to be in the range of ngL -1 , and for this reason, it is imperative to develop analytical methods of extraction and preconcentration to allow for subsequent instrumental analysis of these drugs. In this work, a rapid, simple and green method for the analysis of seven cytostatic drug compounds that are commonly used in anti-cancer therapies was developed using a novel extraction process based on a powerful miniaturized technique, fabric phase sorptive extraction (FPSE) coupled to ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The major parameters that affect the extraction process were optimized. The new method shows good linearity, with a relative standard deviation (RSD) of less than 12%. Relative recoveries higher than 40% were obtained for the studied compounds, and the detection limit of the method was within the values at which these compounds are usually found in environmental water (0.20ngL -1 to 80ngL -1 ). The Limit of Quantification ranged from 0.68 to 267ngL -1 . Significant suppression of the signal due to the matrix effect, a common shortcoming attributed to interference from the extraction process as well as the use of ionization mode, was not observed. Subsequently, the method was applied to real wastewater samples from an effluent obtained from a hospital area and three wastewater treatment plants located in Gran Canaria Island, Spain. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Mannosidase Production by Viridans Group Streptococci

    Science.gov (United States)

    Homer, K. A.; Roberts, G.; Byers, H. L.; Tarelli, E.; Whiley, R. A.; Philpott-Howard, J.; Beighton, D.

    2001-01-01

    The production of mannosidase activity by all currently recognized species of human viridans group streptococci was determined using an assay in which bacterial growth was dependent on the degradation of the high-mannose-type glycans of RNase B and subsequent utilization of released mannose. RNase B is an excellent substrate for the demonstration of mannosidase activity since it is a glycoprotein with a single glycosylation site which is occupied by high-mannose-type glycoforms containing five to nine mannose residues. Mannosidase activity was produced only by some members of the mitis group (Streptococcus mitis, Streptococcus oralis, Streptococcus gordonii, Streptococcus cristatus, Streptococcus infantis, Streptococcus parasanguinis, and Streptococcus pneumoniae) and Streptococcus intermedius of the anginosus group. None of the other species within the salivarius and mutans groups or Streptococcus peroris and Streptococcus sanguinis produced mannosidase activity. Using matrix-assisted laser desorption ionization time-of-flight mass spectrometry, it was demonstrated that the Man5 glycan alone was degraded while Man6 to Man9, which contain terminal α(1→2) mannose residues in addition to the α(1→3), α(1→6), and β(1→4) residues present in Man5, remained intact. Investigations on mannosidase production using synthetic (4-methylumbelliferone- or p-nitrophenol-linked) α- or β-mannosides as substrates indicated that there was no correlation between degradation of these substrates and degradation of the Man5 glycan of RNase B. No species degraded these α-linked mannosides, while degradation of the β-linked synthetic substrates was restricted to strains within the Streptococcus anginosus, S. gordonii, and S. intermedius species. The data generated using a native glycoprotein as the substrate demonstrate that mannosidase production within the viridans group streptococci is more widely distributed than had previously been considered. PMID:11230417

  9. Monitoring of Some Pesticides Residue in Consumed tea in Tehran Market

    Directory of Open Access Journals (Sweden)

    Maryam Amirahmadi

    2013-01-01

    Full Text Available Tea is an agricultural product of the leaves, leaf buds, and internodes of various cultivars and sub-varieties of the Camellia sinensis plant, processed and vulcanized using various methods. Tea is a main beverage in Iranian food basket so should be free from toxic elements such as pesticides residue. There is no data bank on the residue of pesticides in the consumed black tea in Iran. The present study is the first attempt for monitoring of 25 pesticide residues from different chemical groups in tea samples obtained from local markets in Tehran, I.R. Iran during the period 2011. A reliable and accurate method based on spiked calibration curve and QuEChERS sample preparation was developed for determination of pesticide residues in tea by gas chromatography--mass spectrometry (GC/MS. The using of spiked calibration standards for constructing the calibration curve substantially reduced adverse matrix-related effects and negative recovery affected by GCB on pesticides. The recovery of pesticides at 3 concentration levels (n = 3 was in range of 81.4 - 99.4%. The method was proved to be repeatable with RSDr lower than 20%. The limits of quantification for all pesticides were <=20 ng/g. 53 samples from 17 imported and manufactured brand were analyzed. Detectable pesticides residues were found in 28.3% (15 samples of the samples. All of the positive samples were contaminated with unregulated pesticides (Endosulfan Sulfate or Bifenthrin which are established by ISIRI. None of the samples had contamination higher than maximum residue limit set by EU and India.

  10. Monitoring of some pesticides residue in consumed tea in Tehran market

    Directory of Open Access Journals (Sweden)

    Hamedani Morteza Pirali

    2013-01-01

    Full Text Available Abstract Tea is an agricultural product of the leaves, leaf buds, and internodes of various cultivars and sub-varieties of the Camellia sinensis plant, processed and vulcanized using various methods. Tea is a main beverage in Iranian food basket so should be free from toxic elements such as pesticides residue. There is no data bank on the residue of pesticides in the consumed black tea in Iran. The present study is the first attempt for monitoring of 25 pesticide residues from different chemical groups in tea samples obtained from local markets in Tehran, I.R. Iran during the period 2011. A reliable and accurate method based on spiked calibration curve and QuEChERS sample preparation was developed for determination of pesticide residues in tea by gas chromatography–mass spectrometry (GC/MS. The using of spiked calibration standards for constructing the calibration curve substantially reduced adverse matrix-related effects and negative recovery affected by GCB on pesticides. The recovery of pesticides at 3 concentration levels (n = 3 was in range of 81.4 - 99.4%. The method was proved to be repeatable with RSDr lower than 20%. The limits of quantification for all pesticides were ≤20 ng/g. 53 samples from 17 imported and manufactured brand were analyzed. Detectable pesticides residues were found in 28.3% (15 samples of the samples. All of the positive samples were contaminated with unregulated pesticides (Endosulfan Sulfate or Bifenthrin which are established by ISIRI. None of the samples had contamination higher than maximum residue limit set by EU and India.

  11. Critical Mass

    CERN Multimedia

    AUTHOR|(CDS)2070299

    2017-01-01

    Critical Mass is a cycling event typically held on the last Friday of every month; its purpose is not usually formalized beyond the direct action of meeting at a set location and time and traveling as a group through city or town streets on bikes. The event originated in 1992 in San Francisco; by the end of 2003, the event was being held in over 300 cities around the world. At CERN it is held once a year in conjunction with the national Swiss campaing "Bike to work".

  12. Residual Wage Differences by Gender: Bounding the Estimates.

    Science.gov (United States)

    Sakellariou, Chris N.; Patrinos, Harry A.

    1996-01-01

    Uses data from the 1986 Canadian labor market activity survey file to derive estimates of residual gender wage gap differences. Investigates these estimates' dependence on experimental design and on assumptions about discrimination-free wage structures. Residual differences persist, even after restricting the sample to a group of highly motivated,…

  13. On the Structure of Finite Integral Commutative Residuated Chains

    Czech Academy of Sciences Publication Activity Database

    Horčík, Rostislav

    2011-01-01

    Roč. 21, č. 5 (2011), s. 717-728 ISSN 0955-792X Institutional research plan: CEZ:AV0Z10300504 Keywords : residuated lattice * ordered residuated monoid * nucleus * conucleus,Abelian lattice-ordered group * free commutative monoid Subject RIV: BA - General Mathematics Impact factor: 0.611, year: 2011

  14. Development of an NPP residual lifetime evaluation system

    International Nuclear Information System (INIS)

    Regano, M.; Ibanez, M.; Hevia, F.

    1993-01-01

    Various reasons have given rise to the need for residual life management of Spain's nuclear power plants which lead to the a project for the development of a residual lifetime evaluation system managed by UNESA and supported by the owner groups. This project is described. 1 fig

  15. Quadratic residues and non-residues selected topics

    CERN Document Server

    Wright, Steve

    2016-01-01

    This book offers an account of the classical theory of quadratic residues and non-residues with the goal of using that theory as a lens through which to view the development of some of the fundamental methods employed in modern elementary, algebraic, and analytic number theory. The first three chapters present some basic facts and the history of quadratic residues and non-residues and discuss various proofs of the Law of Quadratic Reciprosity in depth, with an emphasis on the six proofs that Gauss published. The remaining seven chapters explore some interesting applications of the Law of Quadratic Reciprocity, prove some results concerning the distribution and arithmetic structure of quadratic residues and non-residues, provide a detailed proof of Dirichlet’s Class-Number Formula, and discuss the question of whether quadratic residues are randomly distributed. The text is a valuable resource for graduate and advanced undergraduate students as well as for mathematicians interested in number theory.

  16. Evaluation of pesticide residues in fruits and vegetables from Algeria.

    Science.gov (United States)

    Mebdoua, Samira; Lazali, Mohamed; Ounane, Sidi Mohamed; Tellah, Sihem; Nabi, Fahima; Ounane, Ghania

    2017-06-01

    A total of 160 samples of 13 types of fresh fruits and vegetables from domestic production and import were analysed to detect the presence of pesticide residues. Analysis was performed by multi-residual extraction followed by gas chromatography-mass spectrometry. In 42.5% of the tested samples, no residues were found and 12.5% of samples contained pesticide residues above maximum residue limits. Risk assessment for long-term exposure was done for all pesticides detected in this study. Except chlorpyrifos and lambda-cyhalothrin, exposure to pesticides from vegetables and fruits was below 1% of the acceptable daily intake. Short-term exposure assessment revealed that in seven pesticide/commodity combinations, including three pesticides (chlorpyrifos, deltamethrin and lambda-cyhalothrin), the acute reference dose had been exceeded.

  17. Determination of residual ractopamine concentrations by enzyme immunoassay in treated pig's tissues on days after withdrawal.

    Science.gov (United States)

    Pleadin, Jelka; Perši, Nina; Vulić, Ana; Milić, Dinka; Vahčić, Nada

    2012-03-01

    The objective of this study was to measure residual ractopamine concentrations in tissues of pigs as experimental animals after treatment with dietary ractopamine for 28 consecutive days. Ractopamine was administered orally to the experimental group (n=9) in a dose of 0.1mg/kg body mass per day, whereas control animals (n=3) were left untreated. Treated pigs (60kg) were sacrificed on days 1, 3 and 8 of treatment discontinuation and residues were determined in kidney, liver, muscle, brain and heart tissues using previously validated enzyme-linked immunosorbent assay (ELISA) as a quantitative screening method. Validation showed good mean recoveries (approx. 70-90%) with acceptable inter- and intra-day relative standard deviations (RSDractopamine tissue concentrations. The highest ractopamine concentration on day 1 (24h) after the last exposure was recorded in the kidney (12.49±7.96ng/g), followed by the liver (7.21±2.73ng/g), heart (1.26±0.12ng/g) and brain (0.63±0.05ng/g); at this time of withdrawal, residues were not detected in the muscle. Ractopamine was depleted rapidly from all study tissues, with mostly no detectable residues on day 8 of withdrawal. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. Sharing Residual Liability

    DEFF Research Database (Denmark)

    Carbonara, Emanuela; Guerra, Alice; Parisi, Francesco

    2016-01-01

    Economic models of tort law evaluate the efficiency of liability rules in terms of care and activity levels. A liability regime is optimal when it creates incentives to maximize the value of risky activities net of accident and precaution costs. The allocation of primary and residual liability...... the virtues and limits of loss-sharing rules in generating optimal (second-best) incentives and allocations of risk. We find that loss sharing may be optimal in the presence of countervailing policy objectives, homogeneous risk avoiders, and subadditive risk, which potentially offers a valuable tool...

  19. Using of sawing quartzite fine residual for obtaining ceramic coating

    International Nuclear Information System (INIS)

    Nobrega, L.F.P.M.; Souza, M.M.

    2016-01-01

    Quartzite is a metamorphic rock that is consisting mainly of quartz. In Paraiba there is a mining activity of this rock, in the region of Varzea and Junco do Serido especially where many wastes are created, including the sawing residue. The objective is to use the waste cited as the ceramic component coating mass, thereby replacing the quartz. Initially, the raw materials samples were taken and the chemical analysis was done of them. This passed the comminution process to achieve the required minimum particle size. After this, a formulation which added the residue in ceramic mass was made. The specimens were subjected to sintering and it was later made physical tests according to NBR 13818. The results show that the residue can replace the quartz ceramic mass successfully, but not as good as the original raw material. (author)

  20. Bioenergy from sisal residues

    Energy Technology Data Exchange (ETDEWEB)

    Jungersen, G. [Dansk Teknologisk Inst. (Denmark); Kivaisi, A.; Rubindamayugi, M. [Univ. of Dar es Salaam (Tanzania, United Republic of)

    1998-05-01

    The main objectives of this report are: To analyse the bioenergy potential of the Tanzanian agro-industries, with special emphasis on the Sisal industry, the largest producer of agro-industrial residues in Tanzania; and to upgrade the human capacity and research potential of the Applied Microbiology Unit at the University of Dar es Salaam, in order to ensure a scientific and technological support for future operation and implementation of biogas facilities and anaerobic water treatment systems. The experimental work on sisal residues contains the following issues: Optimal reactor set-up and performance; Pre-treatment methods for treatment of fibre fraction in order to increase the methane yield; Evaluation of the requirement for nutrient addition; Evaluation of the potential for bioethanol production from sisal bulbs. The processing of sisal leaves into dry fibres (decortication) has traditionally been done by the wet processing method, which consumes considerable quantities of water and produces large quantities of waste water. The Tanzania Sisal Authority (TSA) is now developing a dry decortication method, which consumes less water and produces a waste product with 12-15% TS, which is feasible for treatment in CSTR systems (Continously Stirred Tank Reactors). (EG)

  1. Characterization of briquettes produced with agroforestry residues

    Directory of Open Access Journals (Sweden)

    Ananias Francisco Dias Júnior

    2014-09-01

    Full Text Available The objective of the present was to characterize the quality of briquettes produced with fines of vegetable coal and bamboo residues, under different formulations. Specific gravity density, bulk density mass, moisture content and speed or rate of thermic degradation were evaluated. Compressive strength and rotation test were applied to the briquettes. Superior and inferior calorific values from briquettes were estimate by adjusted equations. Briquettes produced with the highest percentages of vegetable coal fines presented higher specific gravity, bulk density, ash content and fixed carbon. It also presented resistance to fall and abrasion. Briquettes with higher bamboo residues content presented faster degradation, higher compressive strength, beyond higher volatile matters and calorific value.

  2. Analysis of hazardous organic residues from sodium hydrosulfite industry and utilization as raw materials in a novel solid lubricant production.

    Science.gov (United States)

    Shang, Jiwu; Zhang, Yihe; Zhou, Fengshan; Lv, Fengzhu; Han, Feng; Lu, Jinbo; Meng, Xianghai; Chu, Paul K; Ye, Zhengfang; Xing, Jing

    2011-12-30

    The hazardous organic residual wastes produced by the sodium hydrosulfite industry are demonstrated to be convertible into a novel solid lubricant. Identification and isolation of the organic residues are achieved by Fourier transform infrared (FTIR) spectroscopy, gas chromatography-mass spectrometry (GC-MS), and nuclear magnetic resonance (NMR). FTIR and GC-MS provide important information about the residues and the two main components obtained by column chromatography are further analyzed by NMR. The main organic residues are found to be thiodiglycol and 2,2'-dithiodiethanol which have potential applications in petroleum drilling because of their S-S and/or C-S functional groups. The lubricity of the organic residues is subsequently studied and the influence of different adsorbents on the lubricity is investigated and discussed. This homemade lubricant is observed to have good lubricity and by increasing the concentration of the commercial solid lubricant M, the lubricity diminishes. The process is expected to not only have commercial impact but also help to reduce environmental pollution. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Demographic, health-related, and work-related factors associated with body mass index and body fat percentage among workers at six Connecticut manufacturing companies across different age groups: a cohort study.

    Science.gov (United States)

    Garza, Jennifer L; Dugan, Alicia G; Faghri, Pouran D; Gorin, Amy A; Huedo-Medina, Tania B; Kenny, Anne M; Cherniack, Martin G; Cavallari, Jennifer M

    2015-01-01

    Effective workplace interventions that consider the multifactorial nature of obesity are needed to reduce and prevent obesity among adults. Furthermore, the factors associated with obesity may differ for workers across age groups. Therefore, the objective of this study was to identify demographic, health-related, and work-related factors associated with baseline and changes in body mass index (BMI) and body fat percentage (BFP) and among Connecticut manufacturing workers acrossage groups. BMI and BFPof 758 workers from six Connecticut manufacturing companies were objectively measuredat two time points approximately 36 months apart. Demographic, health-related, and work-related factors wereassessed via questionnaire. All variables were included in linear regression models to identify factors associated with baseline and changes in BMI and BFP for workers in 3 age groups: 55 years (28 %). There were differences in baseline and changes in BMI and BFP among manufacturing workers across age groups. Being interested in changing weight was significantly (p age categories. Other factors associated with higher baseline BMI and BFP differed by age group and included: male gender (BMI p = 0.04), female gender (BFP p age category, male gender (BMI p = 0.02), female gender (BFP p age category, and female gender (BFP p 55 year age category. Few factors were associated with change in BMI or BFP across any age category. Among manufacturing workers, we identified associations between individual, health-related, and work-related factors and baseline BMIand BFP that differed by age. Such results support the use of strategies tailored to the challenges faced by workers in specific age groups rather than adopting a one size fits all approach. Effective interventions should consider a full range of individual, health-related, and work-related factors. More work must be done to identify factors or strategies associated with changes in obesity over time.

  4. Protein Analysis by Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Cindic, M.

    2008-04-01

    Full Text Available Soft ionization techniques, electrospray (ESI and matrix-assisted laser desorption/ionization (MALDI make the analysis of biomolecules by mass spectrometry (MS possible. MS is used for determination of the molecular weight of peptides and protein, sequence analysis, characterization of protein-ligand interactions etc. The detection limit, resolution and mass accuracy depend on instrument used (Table 1. Impurities (buffers, salts, detergents can reduce the ion intensities or even totally suppress them, so a separation method (chromatography, 2D-gel electrophoresis must be used for purification of the sample.Molecular mass of intact protein can be determined by ESI or MALDI MS. Multiply charged ions are produced by ESI MS, while singly charged ions are predominant in MALDI spectra (Fig. 2.Sequence analysis of proteins by MS can be performed using peptide mass fingerprint. In this method, proteins are separated by 2-D gel electrophoresis and digested with specific protease (Table 2 or digested and then separated by two-dimensional chromatography (Fig. 1. The obtained peptide mixtures are analyzed by MS or MALDI-TOF technique. The masses determined by MS are compared with calculated masses from database entries. Different algorithms have been developed for protein identification. Example of posttranslational modifications (N- and O-glycosylation and protein sequence complex analysis after dual digestion (endoproteinase digestion followed by endoglycosidase digestion is shown in Fig. 3.It is known that detection of peptides by MS is influenced by intrinsic properties like amino acid composition, the basicity of the C-terminal amino acid, hydrophobicity, etc. Arginine-containing peptides dominate in MS spectra of tryptic digest, so the chemical derivatization of lysine terminal residue by O-methilisourea or 2-methoxy-4,5-1H-imidazole was suggested (Fig. 4.The peptide mass fingerprint method can be improved further by peptide fragmentation using tandem

  5. Screening the biosphere: the fungicolous fungus Trichoderma phellinicola, a prolific source of hypophellins, new 17-, 18-, 19-, and 20-residue peptaibiotics.

    Science.gov (United States)

    Röhrich, Christian René; Iversen, Anita; Jaklitsch, Walter Michael; Voglmayr, Hermann; Vilcinskas, Andreas; Nielsen, Kristian Fog; Thrane, Ulf; von Döhren, Hans; Brückner, Hans; Degenkolb, Thomas

    2013-05-01

    To investigate the significance of antibiotics for the producing organism(s) in the natural habitat, we screened a specimen of the fungicolous fungus Trichoderma phellinicola (syn. Hypocrea phellinicola) growing on its natural host Phellinus ferruginosus. Results revealed that a particular group of non-ribosomal antibiotic polypeptides, peptaibiotics, which contain the non-proteinogenic marker amino acid, α-aminoisobutyric acid, was biosynthesized in the natural habitat by the fungicolous producer and, consequently, released into the host. By means of liquid chromatography coupled to electrospray high-resolution time-of-flight mass spectrometry, we detected ten 20-residue peptaibols in the specimen. Sequences of peptaibiotics found in vivo were independently confirmed by analyzing the peptaibiome of an agar plate culture of T. phellinicola CBS 119283 (ex-type) grown under laboratory conditions. Notably, this strain could be identified as a potent producer of 39 new 17-, 18-, and 19-residue peptaibiotics, which display the same building scheme as the 20-residue peptaibols found in the specimen. Two of the 19-residue peptaibols are tentatively assigned to carry tyrosinol, a novel C-terminal residue, as deduced from high-resolution tandem mass-spectrometry data. For the new peptaibiotics produced by T. phellinicola, the name 'hypophellin(s)', based on the teleomorph name, is introduced. Copyright © 2013 Verlag Helvetica Chimica Acta AG, Zürich.

  6. Metabolomic study of plasma from female mink (Neovison vison) with low and high residual feed intake during restrictive and ad libitum feeding

    DEFF Research Database (Denmark)

    Hedemann, Mette Skou; Damgaard, Birthe Marie

    2012-01-01

    Metabolite profiling may elucidate changes in metabolic pathways under various physiological or nutritional conditions. In the present study two groups of female mink characterized as having a high (16 mink) or low (14 mink) residual feed intake were investigated during restrictive and ad libitum...... component analysis showed that there was no grouping of the data according to the residual feed intake. In contrast, data clearly grouped according to feeding level. Identification of the metabolites responsible for this grouping showed that the plasma level of metabolites related to mobilization of energy...... feeding. Blood samples were collected three times during the experimental period; during restrictive feeding, four days and three weeks after the change to ad libitum feeding. Plasma samples were subjected to liquid chromatography mass spectrometry non-targeted metabolomics. Subjecting data to principal...

  7. Leptonic Dirac CP violation predictions from residual discrete symmetries

    Directory of Open Access Journals (Sweden)

    I. Girardi

    2016-01-01

    Full Text Available Assuming that the observed pattern of 3-neutrino mixing is related to the existence of a (lepton flavour symmetry, corresponding to a non-Abelian discrete symmetry group Gf, and that Gf is broken to specific residual symmetries Ge and Gν of the charged lepton and neutrino mass terms, we derive sum rules for the cosine of the Dirac phase δ of the neutrino mixing matrix U. The residual symmetries considered are: i Ge=Z2 and Gν=Zn, n>2 or Zn×Zm, n,m≥2; ii Ge=Zn, n>2 or Zn×Zm, n,m≥2 and Gν=Z2; iii Ge=Z2 and Gν=Z2; iv Ge is fully broken and Gν=Zn, n>2 or Zn×Zm, n,m≥2; and v Ge=Zn, n>2 or Zn×Zm, n,m≥2 and Gν is fully broken. For given Ge and Gν, the sum rules for cos⁡δ thus derived are exact, within the approach employed, and are valid, in particular, for any Gf containing Ge and Gν as subgroups. We identify the cases when the value of cos⁡δ cannot be determined, or cannot be uniquely determined, without making additional assumptions on unconstrained parameters. In a large class of cases considered the value of cos⁡δ can be unambiguously predicted once the flavour symmetry Gf is fixed. We present predictions for cos⁡δ in these cases for the flavour symmetry groups Gf=S4, A4, T′ and A5, requiring that the measured values of the 3-neutrino mixing parameters sin2⁡θ12, sin2⁡θ13 and sin2⁡θ23, taking into account their respective 3σ uncertainties, are successfully reproduced.

  8. Marine Tar Residues: a Review

    OpenAIRE

    Warnock, April M.; Hagen, Scott C.; Passeri, Davina L.

    2015-01-01

    Marine tar residues originate from natural and anthropogenic oil releases into the ocean environment and are formed after liquid petroleum is transformed by weathering, sedimentation, and other processes. Tar balls, tar mats, and tar patties are common examples of marine tar residues and can range in size from millimeters in diameter (tar balls) to several meters in length and width (tar mats). These residues can remain in the ocean environment indefinitely, decomposing or becoming buried in ...

  9. Peptides containing internal residues of pyroglutamic acid: proton NMR characteristics

    International Nuclear Information System (INIS)

    Khan, S.A.

    1986-01-01

    The proton NMR characteristics of internal pyroglutamic acid (Glp; 5-oxoproline) residues in seven tripeptides of the general structure Boc-Xxx-Glp-Yyy-NH 2 were studied. In general, the chemical shifts of several diagnostic protons moved downfield on going from the Glu-containing peptides (Boc-Xxx-Glu-Yyy-NH 2 ) to the corresponding Glp-containing peptides. The C-2 proton of the Xxx residue was shifted by about 1.1 ppm. The N-2 proton of the Yyy residue was shifted by about 0.5 ppm. The C-2 proton of the Glx residue itself was shifted by about 0.5 ppm. One of the Glx C-3 protons was also shifted by about 0.5 ppm, but the other remained essentially unchanged. Finally, the Glx C-4 protons were shifted by about 0.3 ppm. Internal Glu residues are readily converted chemically into internal Glp residues. This conversion also occurs as a side reaction during HP cleavage of the protecting group from Glu(OBzl) residues. The spontaneous fragmentation of serum proteins C3, C4 and λ 2 -macroglobulin under denaturing conditions is probably due to regioselective hydrolysis of an internal Glp residue formed in each of these proteins upon denaturation. These proton NMR characteristics may be useful in establishing the presence of internal Glp residues in synthetic and natural peptides

  10. RESIDUAL LIMB VOLUME CHANGE: SYSTEMATIC REVIEW OF MEASUREMENT AND MANAGEMENT

    Science.gov (United States)

    Sanders, JE; Fatone, S

    2014-01-01

    Management of residual limb volume affects decisions regarding timing of fit of the first prosthesis, when a new prosthetic socket is needed, design of a prosthetic socket, and prescription of accommodation strategies for daily volume fluctuations. The purpose of this systematic review was to assess what is known about measurement and management of residual limb volume change in persons with lower-limb amputation. Publications that met inclusion criteria were grouped into three categories: (I) descriptions of residual limb volume measurement techniques; (II) studies on people with lower-limb amputation investigating the effect of residual limb volume change on clinical care; and (III) studies of residual limb volume management techniques or descriptions of techniques for accommodating or controlling residual limb volume. The review showed that many techniques for the measurement of residual limb volume have been described but clinical use is limited largely because current techniques lack adequate resolution and in-socket measurement capability. Overall, there is limited evidence regarding the management of residual limb volume, and the evidence available focuses primarily on adults with trans-tibial amputation in the early post-operative phase. While we can draw some insights from the available research about residual limb volume measurement and management, further research is required. PMID:22068373

  11. Complex scaling and residual flavour symmetry in the neutrino mass ...

    Indian Academy of Sciences (India)

    Probir Roy

    2017-10-09

    2 so that tan θ23 = k. −1 while θSRS. 23 is left undetermined (whereas other results change in an extension that we shall propose, the tan θ23 = k. −1 relation will be seen to survive). The earlier mentioned unitary matrix is now ...

  12. Recognition of Streptococcus pseudoporcinus Colonization in Women as a Consequence of Using Matrix-Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry for Group B Streptococcus Identification.

    Science.gov (United States)

    Suwantarat, Nuntra; Grundy, Maureen; Rubin, Mayer; Harris, Renee; Miller, Jo-Anne; Romagnoli, Mark; Hanlon, Ann; Tekle, Tsigereda; Ellis, Brandon C; Witter, Frank R; Carroll, Karen C

    2015-12-01

    During a 14-month period of using matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) for group B streptococcus (GBS) identification, we recovered 32 (1%) Streptococcus pseudoporcinus isolates from 3,276 GBS screening cultures from female genital sources (25 isolates from pregnant women and 7 from nonpregnant women). An additional two S. pseudoporcinus isolates were identified from a urine culture and a posthysterectomy wound culture. These isolates were found to cross-react with three different GBS antigen agglutination kits, PathoDx (Remel) (93%), Prolex (Pro-Lab Diagnostics) (38%), and Streptex (Remel) (53%). New approaches to bacterial identification in routine clinical microbiology laboratories may affect the prevalence of S. pseudoporcinus. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

  13. Evaluation of residue-residue contact predictions in CASP9

    KAUST Repository

    Monastyrskyy, Bohdan

    2011-01-01

    This work presents the results of the assessment of the intramolecular residue-residue contact predictions submitted to CASP9. The methodology for the assessment does not differ from that used in previous CASPs, with two basic evaluation measures being the precision in recognizing contacts and the difference between the distribution of distances in the subset of predicted contact pairs versus all pairs of residues in the structure. The emphasis is placed on the prediction of long-range contacts (i.e., contacts between residues separated by at least 24 residues along sequence) in target proteins that cannot be easily modeled by homology. Although there is considerable activity in the field, the current analysis reports no discernable progress since CASP8.

  14. Effect of routine preoperative fasting on residual gastric volume and ...

    African Journals Online (AJOL)

    Effect of routine preoperative fasting on residual gastric volume and acid in patients undergoing myomectomy. ... Placebo drink group (Group P, n = 30) received water in the same protocol as Group C. The Student's t‑test was used to analyze RGV and pH postoperative satisfaction and postoperative nausea and vomiting ...

  15. A comparative research on obesity hypertension by the comparisons and associations between waist circumference, body mass index with systolic and diastolic blood pressure, and the clinical laboratory data between four special Chinese adult groups.

    Science.gov (United States)

    Wu, Ou; Leng, Jian-Hang; Yang, Fen-Fang; Yang, Hai-Ming; Zhang, Hu; Li, Zeng-Fang; Zhang, Xing-Yu; Yuan, Cheng-Da; Li, Jia-Jia; Pan, Qi; Liu, Wei; Ren, Yan-Jun; Liu, Bing; Liu, Qing-Min; Cao, Cheng-Jian

    2018-01-01

    The obesity-hypertension pathogenesis is complex. From the phenotype to molecular mechanism, there is a long way to clarify the mechanism. To explore the association between obesity and hypertension, we correlate the phenotypes such as the waist circumference (WC), body mass index (BMI), systolic blood pressure (SB), and diastolic blood pressure (DB) with the clinical laboratory data between four specific Chinese adult physical examination groups (newly diagnosed untreated just-obesity group, newly diagnosed untreated obesity-hypertension group, newly diagnosed untreated just-hypertension group, and normal healthy group), and the results may show something. To explore the mechanisms from obesity to hypertension by analyzing the correlations and differences between WC, BMI, SB, DB, and other clinical laboratory data indices in four specific Chinese adult physical examination groups. This cross-sectional study was conducted from September 2012 to July 2014, and 153 adult subjects, 34 women and 119 men, from 21 to 69 years, were taken from four characteristic Chinese adult physical examination groups (newly diagnosed untreated just-obesity group, newly diagnosed untreated obesity-hypertension group, newly diagnosed untreated just-hypertension group, and normal healthy group). The study was approved by the ethics committee of Hangzhou Center for Disease Control and Prevention. WC, BMI, SB, DB, and other clinical laboratory data were collected and analyzed by SPSS. Serum levels of albumin (ALB),alanine aminotransferase (ALT), low density lipoprotein cholesterol (LDLC), triglyceride (TG), high density lipoprotein cholesterol (HDLC), alkaline phosphatase (ALP), uric acid (Ua), and TC/HDLC (odds ratio) were statistically significantly different between the four groups. WC statistically significantly positively correlated with BMI, ALT, Ua, and serum levels of glucose (GLU), and TC/HDLC, and negatively with ALB, HDLC, and serum levels of conjugated bilirubin (CB). BMI

  16. Alternatives in modeling of body mass index as a continuous response variable and relevance of residual analysis Alternativas para modelagem do índice de massa corporal como variável contínua e relevância da análise de resíduos

    Directory of Open Access Journals (Sweden)

    Maria de Jesus Mendes da Fonseca

    2008-02-01

    Full Text Available This article presents alternatives for modeling body mass index (BMI as a continuous variable and the role of residual analysis. We sought strategies for the application of generalized linear models with appropriate statistical adjustment and easy interpretation of results. The analysis included 2,060 participants in Phase 1 of a longitudinal study (Pró-Saúde Study with complete data on weight, height, age, race, family income, and schooling. In our study, the residual analysis of models estimated by maximum likelihood methods yielded inadequate adjustment. The transformed response variable resulted in a good fit but did not lead to estimates with straightforward interpretation. The best alternative was to apply quasi-likelihood as the estimation method, presenting a better adjustment and constant variance. In epidemiological data modeling, researchers should always take trade-offs into account between adequate statistical techniques and interpretability of results.Neste artigo, discutem-se alternativas de modelagem do índice de massa corporal (IMC, analisado como variável contínua, e a análise de resíduos. Buscaram-se estratégias de aplicação dos modelos lineares generalizados adequadas tanto do ponto de vista do ajuste estatístico quanto da facilidade de interpretação dos resultados. Nestas análises, foram incluídos dados relativos a 2.060 participantes da Fase 1 de estudo longitudinal (Estudo Pró-Saúde, com informação completa de peso, estatura, idade, raça/cor, renda familiar e escolaridade. Em nosso estudo, a análise de resíduos dos modelos estimados pelo método da máxima verossimilhança, amplamente utilizado, não possibilitou ajuste adequado dos modelos aos dados. A transformação da variável resposta, apesar de resultar em um bom ajuste, não conduziu a estimativas de fácil interpretação. Considerou-se como melhor alternativa a mudança do método de estimação para quase-verossimilhança. Assim, melhor

  17. A non-LEA sofic group

    Indian Academy of Sciences (India)

    We describe elementary examples of finitely presented sofic groups which are not residually amenable (and thus not initially subamenable or LEA, for short). We ask if an amalgam of two amenable groups over a finite subgroup is residually amenable and answer this positively for some special cases, including countable ...

  18. Effects of body mass index on the outcomes of percutaneous nephrolithotomy

    Directory of Open Access Journals (Sweden)

    Cemal Selcuk Isoglu

    Full Text Available ABSTRACT Objective To examine the the effect of body mass index (BMI on PNL results and complications with a large number of patients. Materials and Methods A total of 958 patients were included in the study, who underwent percutaneous nephrolithotomy in our clinic between 2008 and 2015. Patients were divided into 2 groups according to their body mass index. Patients with a BMI < 30 kg/m2 were classified as group 1 (n:676 and patients with a BMI ≥ 30 kg/m2 were classified as group 2 (n:282. Achieving stone-free status or having residual stones of ≤ 4 mm were considered as operational success. Results The mean age was 47.9 years for group 1 and 48.9 years for group 2 patients. At postoperative first month CT analysis, residual stone was not observed in 466 patients (69% of group 1 and 20 (72% patients of group 2. There was no significant difference between the groups in terms of stone-free status (p=0.348. There was no significant difference between two groups complications. Also, there was no difference between the groups for requiring additional intervention (p=0.924. No other complications were observed in the patients. Conclusions BMI does not affect the outcomes of percutaneous nephrolithotomy as well as complication rate.

  19. Mass drivers. 3: Engineering

    Science.gov (United States)

    Arnold, W.; Bowen, S.; Cohen, S.; Fine, K.; Kaplan, D.; Kolm, M.; Kolm, H.; Newman, J.; Oneill, G. K.; Snow, W.

    1979-01-01

    The last of a series of three papers by the Mass-Driver Group of the 1977 Ames Summer Study is presented. It develops the engineering principles required to implement the basic mass-driver. Optimum component mass trade-offs are derived from a set of four input parameters, and the program used to design a lunar launcher. The mass optimization procedures is then incorporated into a more comprehensive mission optimization program called OPT-4, which evaluates an optimized mass-driver reaction engine and its performance in a range of specified missions. Finally, this paper discusses, to the extent that time permitted, certain peripheral problems: heating effects in buckets due to magnetic field ripple; an approximate derivation of guide force profiles; the mechanics of inserting and releasing payloads; the reaction mass orbits; and a proposed research and development plan for implementing mass drivers.

  20. Graphic Three-Axes Presentation of Residual Gas Analyser Data

    Science.gov (United States)

    Johnson, Kenneth R.; Levi, Alejandro G.

    1996-01-01

    Residual gas analyzers (RGA) are commonly used to measure the composition of residual gases in thermal-vacuum test chambers. Measurements from RGAs are often used to identify and quantify outgassing contaminants from a test article during thermal-vacuum testing. RGA data is typically displayed as snapshots in time, showing instantaneous concentrations of ions from ionized residual gas molecules at different atomic masses. A method was devised by the authors to present RGA data in a three-axis format, plotting atomic mass unit (AMU), ion concentration as a function of AMU, and time, to provide a clear graphic visualization ot trends in gas concentration changes and to initiate a valuable analytical tool to interpret test article outgassing rates during thermal-vacuum testing.

  1. Landfilling of waste incineration residues

    DEFF Research Database (Denmark)

    Christensen, Thomas Højlund; Astrup, Thomas; Cai, Zuansi

    2002-01-01

    Residues from waste incineration are bottom ashes and air-pollution-control (APC) residues including fly ashes. The leaching of heavy metals and salts from the ashes is substantial and a wide spectrum of leaching tests and corresponding criteria have been introduced to regulate the landfilling...

  2. Statistical inference on residual life

    CERN Document Server

    Jeong, Jong-Hyeon

    2014-01-01

    This is a monograph on the concept of residual life, which is an alternative summary measure of time-to-event data, or survival data. The mean residual life has been used for many years under the name of life expectancy, so it is a natural concept for summarizing survival or reliability data. It is also more interpretable than the popular hazard function, especially for communications between patients and physicians regarding the efficacy of a new drug in the medical field. This book reviews existing statistical methods to infer the residual life distribution. The review and comparison includes existing inference methods for mean and median, or quantile, residual life analysis through medical data examples. The concept of the residual life is also extended to competing risks analysis. The targeted audience includes biostatisticians, graduate students, and PhD (bio)statisticians. Knowledge in survival analysis at an introductory graduate level is advisable prior to reading this book.

  3. MOBILIZATION OF AVIATION GASOLINE FROM A RESIDUAL SOURCE

    Science.gov (United States)

    A simple one-dimensional model describes the mobilization of 90 m3 of residual aviation gasoline from an 80-m diameter, O.3O6-m thick contaminated soil mass at the U.S. Coast Guard Air Station in Traverse City, Michigan. riginally deposited under a paved ground surface in Decembe...

  4. Automatic prediction of catalytic residues by modeling residue structural neighborhood

    Directory of Open Access Journals (Sweden)

    Passerini Andrea

    2010-03-01

    Full Text Available Abstract Background Prediction of catalytic residues is a major step in characterizing the function of enzymes. In its simpler formulation, the problem can be cast into a binary classification task at the residue level, by predicting whether the residue is directly involved in the catalytic process. The task is quite hard also when structural information is available, due to the rather wide range of roles a functional residue can play and to the large imbalance between the number of catalytic and non-catalytic residues. Results We developed an effective representation of structural information by modeling spherical regions around candidate residues, and extracting statistics on the properties of their content such as physico-chemical properties, atomic density, flexibility, presence of water molecules. We trained an SVM classifier combining our features with sequence-based information and previously developed 3D features, and compared its performance with the most recent state-of-the-art approaches on different benchmark datasets. We further analyzed the discriminant power of the information provided by the presence of heterogens in the residue neighborhood. Conclusions Our structure-based method achieves consistent improvements on all tested datasets over both sequence-based and structure-based state-of-the-art approaches. Structural neighborhood information is shown to be responsible for such results, and predicting the presence of nearby heterogens seems to be a promising direction for further improvements.

  5. Fermion masses and multiplicity

    International Nuclear Information System (INIS)

    Ramond, P.

    1986-01-01

    A general survey and analysis of fermion masses is presented in terms of both the known low energy gauge structure and of the simplest GUT structure. The replication of fermion families is discussed in the context of possible family group structures. Sample family gauge groups are presented in the cases of three and four chiral families, using ABJ and Witten anomalies to restrict the maximal gauged family group. The possible relevance of the family group to the fermion mass hierarchy is discussed in the context of various models. (author)

  6. Monitoring of Pesticide Residues in Commonly Used Fruits and Vegetables in Kuwait

    OpenAIRE

    Jallow, Mustapha F. A.; Awadh, Dawood G.; Albaho, Mohammed S.; Devi, Vimala Y.; Ahmad, Nisar

    2017-01-01

    The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers. The aim of this study was to assess the level of pesticide residues in commonly consumed fruits and vegetables in Kuwait. A total of 150 samples of different fresh vegetables and fruits were analyzed for the presence of 34 pesticides using the quick easy cheap effective rugged and safe (QuEChERS) multi-residue extraction, followed by gas chromatography-mass spectrometr...

  7. Impact of a nurse-directed, coordinated school health program to enhance physical activity behaviors and reduce body mass index among minority children: a parallel-group, randomized control trial.

    Science.gov (United States)

    Wright, Kynna; Giger, Joyce Newman; Norris, Keth; Suro, Zulma

    2013-06-01

    Underserved children, particularly girls and those in urban communities, do not meet the recommended physical activity guidelines (>60min of daily physical activity), and this behavior can lead to obesity. The school years are known to be a critical period in the life course for shaping attitudes and behaviors. Children look to schools for much of their access to physical activity. Thus, through the provision of appropriate physical activity programs, schools have the power to influence apt physical activity choices, especially for underserved children where disparities in obesity-related outcomes exist. To evaluate the impact of a nurse directed, coordinated, culturally sensitive, school-based, family-centered lifestyle program on activity behaviors and body mass index. This was a parallel group, randomized controlled trial utilizing a community-based participatory research approach, through a partnership with a University and 5 community schools. Participants included 251 children ages 8-12 from elementary schools in urban, low-income neighborhoods in Los Angeles, USA. The intervention included Kids N Fitness(©), a 6-week program which met weekly to provide 45min of structured physical activity and a 45min nutrition education class for parents and children. Intervention sites also participated in school-wide wellness activities, including health and counseling services, staff professional development in health promotion, parental education newsletters, and wellness policies for the provision of healthy foods at the school. The Child and Adolescent Trial for Cardiovascular Health School Physical Activity and Nutrition Student Questionnaire measured physical activity behavior, including: daily physical activity, participation in team sports, attending physical education class, and TV viewing/computer game playing. Anthropometric measures included height, weight, body mass index, resting blood pressure, and waist circumference. Measures were collected at baseline

  8. Residual stress by repair welds

    International Nuclear Information System (INIS)

    Mochizuki, Masahito; Toyoda, Masao

    2003-01-01

    Residual stress by repair welds is computed using the thermal elastic-plastic analysis with phase-transformation effect. Coupling phenomena of temperature, microstructure, and stress-strain fields are simulated in the finite-element analysis. Weld bond of a plate butt-welded joint is gouged and then deposited by weld metal in repair process. Heat source is synchronously moved with the deposition of the finite-element as the weld deposition. Microstructure is considered by using CCT diagram and the transformation behavior in the repair weld is also simulated. The effects of initial stress, heat input, and weld length on residual stress distribution are studied from the organic results of numerical analysis. Initial residual stress before repair weld has no influence on the residual stress after repair treatment near weld metal, because the initial stress near weld metal releases due to high temperature of repair weld and then stress by repair weld regenerates. Heat input has an effect for residual stress distribution, for not its magnitude but distribution zone. Weld length should be considered reducing the magnitude of residual stress in the edge of weld bead; short bead induces high tensile residual stress. (author)

  9. Lithic Residue Survival and Characterisation at Star Carr: a burial experiment

    Directory of Open Access Journals (Sweden)

    Shannon Croft

    2016-09-01

    Full Text Available A modern burial experiment was devised to test microscopic residue survival in acidic peat and slightly acidic clay soils at the Early Mesolithic site of Star Carr (North Yorkshire, UK, and at nearby control location. The experiment addresses concerns regarding the applicability of residue analysis in varied burial environments, and particularly in highly acidic archaeological conditions. Flint flakes (n= 78, including blank controls were used on twelve plant, animal, and mineral materials to create residues and then buried. The residues were examined 1 month and 11 months after burial. An unburied reference collection containing the same twelve residue types in a fresh state was compared to the buried residues to assess diagenesis. The residue types that survived across all burial conditions and time intervals were: softwood tissue, tree resin, bird feathers, squirrel hair, and red ochre. During microscopic analysis, it became clear that many residues lack diagnostic traits, and thus an assessment of the extent to which each residue can be identified was conducted. The degree to which residues were able to be identified was further investigated with a variable pressure scanning electron microscope (SEM. SEM images of the reference residues were compared to the reflected VLM micrographs of the same residues, which improved characterisation in some cases. Residues were grouped into three categories (diagnostic, distinctive, and non-distinctive within a visual characterisation guide. Our in situ microscopic analyses indicated that few residue types have diagnostic traits that allow them to be identified unambiguously, and thus further characterisation techniques are often required.

  10. The residue levels of narasin in eggs of laying hens fed with unmedicated and medicated feed.

    Science.gov (United States)

    Rokka, Mervi; Eerola, Susanna; Perttilä, Ulla; Rossow, Laila; Venäläinen, Eija; Valkonen, Eija; Valaja, Jarmo; Peltonen, Kimmo

    2005-01-01

    Laying hens were fed contaminated feed containing narasin 2.5 mg/kg for 21 days followed by a 7 day withdrawal period, hens in the control group were fed unmedicated feed. Eggs were collected during trial days 0, 3, 7, 14, 21 and after the withdrawal period of 7 days. The concentration of narasin in yolks and egg whites was analyzed by a liquid chromatography-mass spectrometry method. Narasin was found to accumulate in yolks, where the narasin concentration increased during the treatment. The concentration of narasin varied from 5.9 to 13.8 microg/kg (mean 10.6 microg/kg) in yolks after 21 day feeding periods. The concentrations of narasin ranged from residues were not found in egg whites of the laying hens fed contaminated feed nor in either yolks or egg whites of the laying hens fed unmedicated feed. The effect of cooking was also tested on the amount of narasin residues in eggs. Cooking for 10 min did not significantly influence the narasin residues in eggs. Traces of lasalocid were also found in the yolks. The traces of lasalocid are attributable to an accidental contamination of the feed during its manufacture.

  11. Leaching from municipal solid waste incineration residues

    Energy Technology Data Exchange (ETDEWEB)

    Hyks, J.

    2008-02-15

    Leaching of pollutants from Municipal Solid Waste Incineration (MSWI) residues has been investigated combining a range of laboratory leaching experiments with geochemical modeling. Special attention was paid to assessing the applicability of laboratory data for subsequent modeling with respect to presumed full-scale conditions; both sample pretreatment and actual influence of leaching conditions on the results of laboratory experiments were considered. It was shown that sample pretreatment may have large impact on leaching test data. In particular, a significant fraction of Pb was shown mobile during the washing of residues with water. In addition, drying of residues (i.e. slow oxidation) prior to leaching experiments increased the leaching of Cr significantly. Significant differences regarding the leaching behavior of individual elements with respect to (non)equilibrium conditions in column percolation experiments were observed in the study. As a result, three groups of elements were identified based on the predominant leaching control and the influence of (non)equilibrium on the results of the laboratory column experiments: I. Predominantly availability-controlled elements (e.g. Na, K, Cl) II. Solubility-controlled elements (e.g. Ca, S, Si, Al, Ba, and Zn) III. Complexation-controlled elements (e.g. Cu and Ni) With respect to the above groups it was suggested that results of laboratory column experiments can, with consideration, be used to estimate full-scale leaching of elements from Group I and II. However, in order to avoid large underestimations in the assessment of leaching from Group III, it is imperative to describe the time-dependent transport of dissolved organic carbon (DOC) in the tested system or to minimize the physical non-equilibrium during laboratory experiments (e.g. bigger column, slower flow velocity). Forward geochemical modeling was applied to simulate long-term release of elements from a MSWI air-pollution-control residue. Leaching of a

  12. Niclosamide residues in milk and organs of lactating goats

    International Nuclear Information System (INIS)

    El Hindi, A.M.; Sidra, M.S.

    1986-01-01

    14 C-Niclosamide was administered to two groups of lactating goats at levels of 2ppm for five consecutive days and 10ppm as a single dose. Residues of the molluscicide in milk, if at all present, did not exceed 0.001 ppm at any time. About 50% of the administered activity was excreted in faeces, while 30% excreted through urine in animals surviving 6 days after withdrawal. The unchanged molluscicide is present only in relatively trace amounts. The highest residues in organs were found in the liver of both groups (0.01-0.04 ppm). From the results it could be concluded that absorbed niclosamide is completely metabolised and rapidly eliminated through urine, leaving little or no residues of the unchanged molluscicide. Little or no residues were detected in lean muscles and milk which are consumed by humans. There is no preferential deposition of the molluscicide or its metabolites in fat

  13. Nominal Mass?

    Science.gov (United States)

    Attygalle, Athula B; Pavlov, Julius

    2017-08-01

    The current IUPAC-recommended definition of the term "nominal mass," based on the most abundant naturally occurring stable isotope of an element, is flawed. We propose that Nominal mass should be defined as the sum of integer masses of protons and neutrons in any chemical species. In this way, all isotopes and isotopologues can be assigned a definitive identifier. Graphical Abstract ᅟ.

  14. RESIDUAL RISK ASSESSMENT: ETHYLENE OXIDE ...

    Science.gov (United States)

    This document describes the residual risk assessment for the Ethylene Oxide Commercial Sterilization source category. For stationary sources, section 112 (f) of the Clean Air Act requires EPA to assess risks to human health and the environment following implementation of technology-based control standards. If these technology-based control standards do not provide an ample margin of safety, then EPA is required to promulgate addtional standards. This document describes the methodology and results of the residual risk assessment performed for the Ethylene Oxide Commercial Sterilization source category. The results of this analyiss will assist EPA in determining whether a residual risk rule for this source category is appropriate.

  15. Fungicide residue identification and discrimination using a conducting polymer electronic-nose

    Science.gov (United States)

    Alphus D. Wilson

    2013-01-01

    The identification of fungicide residues on crop foliage is necessary to make periodic pest management decisions. The determination of fungicide residue identities currently is difficult and time consuming using conventional chemical analysis methods such as gas chromatography-mass spectroscopy. Different fungicide types produce unique electronic aroma signature...

  16. Radiotracer studies of pesticide residues in stored products

    International Nuclear Information System (INIS)

    1987-01-01

    The current programme was initiated in 1983 and was designed to assist scientists of developing Member States to make safe and effective use of radiotracer techniques for studying pesticide residue problems in stored products. This report represents an appraisal of a group of studies with particular emphasis given to terminal residues at the time of human consumption. A separate abstract was prepared for each of the 12 papers

  17. Green coffee seed residue: A sustainable source of antioxidant compounds.

    Science.gov (United States)

    Castro, A C C M; Oda, F B; Almeida-Cincotto, M G J; Davanço, M G; Chiari-Andréo, B G; Cicarelli, R M B; Peccinini, R G; Zocolo, G J; Ribeiro, P R V; Corrêa, M A; Isaac, V L B; Santos, A G

    2018-04-25

    Oil extraction from green coffee seeds generates residual mass that is discarded by agribusiness and has not been previously studied. Bioactive secondary metabolites in coffee include antioxidant phenolic compounds, such as chlorogenic acids. Coffee seeds also contain caffeine, a pharmaceutically important methylxanthine. Here, we report the chemical profile, antioxidant activity, and cytotoxicity of hydroethanolic extracts of green Coffea arabica L. seed residue. The extracts of the green seeds and the residue have similar chemical profiles, containing the phenolic compounds chlorogenic acid and caffeine. Five monoacyl and three diacyl esters of trans-cinnamic acids and quinic acid were identified by ultra-performance liquid chromatography/electrospray ionization-quadruple time of flight mass spectrometry. The residue extract showed antioxidant potential in DPPH, ABTS, and pyranine assays and low cytotoxicity. Thus, coffee oil residue has great potential for use as a raw material in dietary supplements, cosmetic and pharmaceutical products, or as a source of bioactive compounds. Copyright © 2017. Published by Elsevier Ltd.

  18. Malignant lymphoma: MR tomographic findings of residual mediastinal space-occupying lesions

    International Nuclear Information System (INIS)

    Stroszczynski, C.; Hosten, N.; Oellinger, J.; Amthauer, H.; Bittner, R.C.; Hierholzer, J.; Felix, R.; Spahn, G.; Ludwig, W.D.

    1999-01-01

    Purpose: Evaluation of MR imaging in patients with Hodgkin's lymphoma and high grade non-Hodgkin's-lymphoma and mediastinal residual mass after first line chemotherapy. Materials and Methods: MR imaging (1.5 T) was performed in 36 patients (Hodgkin's lymphoma n=26, NHL n=10) after first line chemotherapy. Twenty patients had inactive residual mass, 16 patients had residual lymphoproliferative lesions. T 1 - and T 2 -weighted spin echo images were visually analysed by a score index (range 1-5) as well as quantification of enhancement by signal-intensity-ratios (SI max /SI plain ). Results: For the differentiation between residual lymphoproliferative activity and inactive residual mass, the highest accuracy was obtained for the signal intensity of residual mass on T 2 -w-SE compared to pectoralis muscle (94% sensitivity, 80% specificity, likelihood ratios: 4.0 [LR+]; 0.3 [LR-]). The cut-off value of the SI ratio was calculated retrospectively at 1.96 (p>0.05). Conclusions: Differentiation between inactive (fibrotic) and lymphoproliferative (active) residual mediastinal mass is possible by MR imaging using as parameter the size reduction after therapy and the signal intensity on T 2 -w-SE in comparison to pectoralis muscle. Thus, study suggests an additional value using the SI ratio for the differentiation. (orig.) [de

  19. Mass spectrometers

    International Nuclear Information System (INIS)

    Manojlov, V.E.; Nedelin, P.N.; Lukichev, A.N.; Sapozhkov, L.K.; Turubarov, V.I.

    1980-01-01

    Mass spectrometers of different types are suggested to use for qualitative and quantitative analyses of gas. The operation principles of static and dynamic mass spectrometer are studied. In static mass spectrometers mass separation of ions is performed by changing the value of accelerating voltage in the ion source when retaining the magnetic field intensity. Such devices are stationary. The device mass is conditioned by the magnet mass. Mass separation in dynamic mass spectrometers is dependent on the degree of energy increment of ions in HF-electric fields. Radio frequency mass spectrometers are used with advantage for studying upper layers of an atmosphere and are installed on radiosondes and satellites. The main technical characteristics of the MX-1330 mass spectrometer, the basis of which is the analyzer with 180 deg deviation of an ion beam in the field of permanent magnet, are presented. The device is intended for controlling the environment and permits to analyze gases with a molecular mass up to 450 using various systems of gas filling. The error of determination of molecular substance is not greater than +-3 %; the magnetic field intensity constitutes 4.8x10 5 A/m; the supply voltage is 380/220 V; the total power is 5.0 kVA [ru

  20. Cardiovascular group

    Science.gov (United States)

    Blomqvist, Gunnar

    1989-01-01

    As a starting point, the group defined a primary goal of maintaining in flight a level of systemic oxygen transport capacity comparable to each individual's preflight upright baseline. The goal of maintaining capacity at preflight levels would seem to be a reasonable objective for several different reasons, including the maintenance of good health in general and the preservation of sufficient cardiovascular reserve capacity to meet operational demands. It is also important not to introduce confounding variables in whatever other physiological studies are being performed. A change in the level of fitness is likely to be a significant confounding variable in the study of many organ systems. The principal component of the in-flight cardiovascular exercise program should be large-muscle activity such as treadmill exercise. It is desirable that at least one session per week be monitored to assure maintenance of proper functional levels and to provide guidance for any adjustments of the exercise prescription. Appropriate measurements include evaluation of the heart-rate/workload or the heart-rate/oxygen-uptake relationship. Respiratory gas analysis is helpful by providing better opportunities to document relative workload levels from analysis of the interrelationships among VO2, VCO2, and ventilation. The committee felt that there is no clear evidence that any particular in-flight exercise regimen is protective against orthostatic hypotension during the early readaptation phase. Some group members suggested that maintenance of the lower body muscle mass and muscle tone may be helpful. There is also evidence that late in-flight interventions to reexpand blood volume to preflight levels are helpful in preventing or minimizing postflight orthostatic hypotension.

  1. Nitrogen availability of biogas residues

    Energy Technology Data Exchange (ETDEWEB)

    El-Sayed Fouda, Sara

    2011-09-07

    The objectives of this study were to characterize biogas residues either unseparated or separated into a liquid and a solid phase from the fermentation of different substrates with respect to their N and C content. In addition, short and long term effects of the application of these biogas residues on the N availability and N utilization by ryegrass was investigated. It is concluded that unseparated or liquid separated biogas residues provide N at least corresponding to their ammonium content and that after the first fertilizer application the C{sub org}:N{sub org} ratio of the biogas residues was a crucial factor for the N availability. After long term application, the organic N accumulated in the soil leads to an increased release of N.

  2. Residual stress analysis: a review

    International Nuclear Information System (INIS)

    Finlayson, T.R.

    1983-01-01

    The techniques which are or could be employed to measure residual stresses are outlined. They include X-ray and neutron diffraction. Comments are made on the reliability and accuracy to be expected from particular techniques

  3. OECD Maximum Residue Limit Calculator

    Science.gov (United States)

    With the goal of harmonizing the calculation of maximum residue limits (MRLs) across the Organisation for Economic Cooperation and Development, the OECD has developed an MRL Calculator. View the calculator.

  4. The tyrosyl residues in creatine kinase. Modification by iodine.

    Science.gov (United States)

    Fattoum, A; Kassab, R; Pradel, L A

    1975-10-20

    The effect of the iodination of tyrosyl residues in creatine kinase from rabbit muscle has been investigated at alkaline pH after reversible masking of the reactive thiol groups. The conversion of 4-5 tyrosyl residues to monoiodotyrosines as measured by spectrotitration and by radioactive iodine labelling resulted in almost total loss of enzymic activity. The modified enzyme was unable to bind its nucleotide substrates but no significant conformational change was revealed by optical rotatory dispersion or Stokes radius measurements. However, change in the reactivity of some non-essential thiol groups, presumably those located near the active thiol groups, was observed.

  5. Observation of the hot GDR in neutron-deficient thorium evaporation residues

    International Nuclear Information System (INIS)

    Seitz, J.P.; Back, B.B.; Carpenter, M.P.; Dioszegi, I.; Eisenman, K.; Heckman, P.; Hofman, D.J.; Kelly, M.P.; Khoo, T.L.; Mitsuoka, S.; Nanal, V.; Pennington, T.; Siemssen, R.H.; Thoennessen, M.; Varner, R.L.

    2005-01-01

    The giant dipole resonance built on excited states was observed in very fissile nuclei in coincidence with evaporation residues. The reaction 48 Ca+ 176 Yb populated evaporation residues of mass A=213-220 with a cross section of ∼200 μb at 259 MeV. The extracted giant dipole resonance parameters are in agreement with theoretical predictions for this mass region

  6. Vesícula residual

    Directory of Open Access Journals (Sweden)

    Júlio C. U. Coelho

    Full Text Available Our objective is to report three patients with recurrent severe upper abdominal pain secondary to residual gallbladder. All patients had been subjected to cholecystectomy from 1 to 20 years before. The diagnosis was established after several episodes of severe upper abdominal pain by imaging exams: ultrasonography, tomography, or endoscopic retrograde cholangiography. Removal of the residual gallbladder led to complete resolution of symptoms. Partial removal of the gallbladder is a very rare cause of postcholecystectomy symptoms.

  7. Marine Tar Residues: a Review.

    Science.gov (United States)

    Warnock, April M; Hagen, Scott C; Passeri, Davina L

    Marine tar residues originate from natural and anthropogenic oil releases into the ocean environment and are formed after liquid petroleum is transformed by weathering, sedimentation, and other processes. Tar balls, tar mats, and tar patties are common examples of marine tar residues and can range in size from millimeters in diameter (tar balls) to several meters in length and width (tar mats). These residues can remain in the ocean environment indefinitely, decomposing or becoming buried in the sea floor. However, in many cases, they are transported ashore via currents and waves where they pose a concern to coastal recreation activities, the seafood industry and may have negative effects on wildlife. This review summarizes the current state of knowledge on marine tar residue formation, transport, degradation, and distribution. Methods of detection and removal of marine tar residues and their possible ecological effects are discussed, in addition to topics of marine tar research that warrant further investigation. Emphasis is placed on benthic tar residues, with a focus on the remnants of the Deepwater Horizon oil spill in particular, which are still affecting the northern Gulf of Mexico shores years after the leaking submarine well was capped.

  8. Identification of chemical signatures of gunshot residues in different fabrics

    International Nuclear Information System (INIS)

    Freitas, Joao Carlos Dias de

    2010-01-01

    The modern forensic science goes hand in hand with scientific research. The forensic scientists are faced every day with many cases requiring the analysis of residues from firing gun (gunshot residues). This works describes the development of a methodology to determine chemical signatures of shots from a firearm, by measuring the concentrations of Pb, Ba e Sb in the residues from these shots deposited near the entrance hole of bullets, based on the technique with high resolution inductively coupled plasma mass spectrometry (HRICP-MS). Shots were performed on five types of target-fabrics and collected testimonies from regions close to the entrance hole of projectiles. The results showed that the method enabled us to identify and distinguish the residues of the .38 caliber revolver and pistols .40 and 9mm caliber. The use of ternary graphs as a tool for data analysis helped to identify specific patterns of distribution of blank samples and gunshot residues deposited after firing revolvers and pistols. The methodology enabled the assignment of the origin of the shot through the confirmation of the residues collected also from the hands of shooters. As a result the methodology in police procedures and aims to add a valuable contribution to forensic investigations. (author)

  9. 40 CFR 180.103 - Captan; tolerances for residues.

    Science.gov (United States)

    2010-07-01

    ...: Commodity Parts per million Almond 0.25 Almond, hulls 75.0 Animal feed, nongrass, group 18 0.05 Apple 25.0... 4 0.05 Vegetable, leaves of root and tuber, group 2 0.05 Vegetable, legume, group 6 0.05 Vegetable, root and tuber, group 1 0.05 (2) Tolerances are established for the combined residues of the fungicide...

  10. Neutral Hydrogen in Local Group Dwarf Galaxies

    Science.gov (United States)

    Grcevich, Jana

    constant velocity and density wind which emulates relative motion of the dwarf and the host's hot halo. These simulations resolve instabilities which can contribute to gas loss, such as the effects of the Kelvin Helmholtz instability. The results of these simulations support the hypothesis that rapid gas loss occurs when the ram pressure stripping criterion is met, with complete stripping occurs with a timescale of about half a Gyr. This stripping would occur in less than an orbital period for ultra-faint like dwarfs. Models which do not meet the ram-pressure stripping criterion show slower but constant mass loss which does not depend on the residual dwarf's gas mass. Extrapolating the stripping timescales, we show low-mass dwarf galaxies can be stripped on timescales between 1.1 and 3.3 Gyrs. These simulations are a first step towards accurate ram-pressure and dynamical mass loss rates for low mass Local Group galaxies orbiting within a hot halo. They suggest that the lack of low mass galaxies within 250 kpc of the Milky Way can be explained via ram-pressure and dynamical interactions between the satellite galaxy's gas and the hot halo.

  11. In situ chemical composition measurement of individual cloud residue particles at a mountain site, southern China

    Science.gov (United States)

    Lin, Qinhao; Zhang, Guohua; Peng, Long; Bi, Xinhui; Wang, Xinming; Brechtel, Fred J.; Li, Mei; Chen, Duohong; Peng, Ping'an; Sheng, Guoying; Zhou, Zhen

    2017-07-01

    To investigate how atmospheric aerosol particles interact with chemical composition of cloud droplets, a ground-based counterflow virtual impactor (GCVI) coupled with a real-time single-particle aerosol mass spectrometer (SPAMS) was used to assess the chemical composition and mixing state of individual cloud residue particles in the Nanling Mountains (1690 m a. s. l. ), southern China, in January 2016. The cloud residues were classified into nine particle types: aged elemental carbon (EC), potassium-rich (K-rich), amine, dust, Pb, Fe, organic carbon (OC), sodium-rich (Na-rich) and Other. The largest fraction of the total cloud residues was the aged EC type (49.3 %), followed by the K-rich type (33.9 %). Abundant aged EC cloud residues that mixed internally with inorganic salts were found in air masses from northerly polluted areas. The number fraction (NF) of the K-rich cloud residues i