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Sample records for gas chromatography-time-of-flight mass

  1. Searching for anthropogenic contaminants in human breast adipose tissues using gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Hernández, Félix; Portolés, Tania; Pitarch, Elena; López, Francisco J

    2009-01-01

    The potential of gas chromatography-time-of-flight mass spectrometry (GC-TOF MS) for screening anthropogenic organic contaminants in human breast adipose tissues has been investigated. Initially a target screening was performed for a list of 125 compounds which included persistent halogen pollutants [organochlorine (OC) pesticides, polychlorinated biphenylss (PCBs), polybrominated diphenyl ethers (PBDEs)], polyaromatic hydrocarbons (PAHs), alkylphenols, and a notable number of pesticides from the different fungicide, herbicide and insecticide families. Searching for target pollutants was done by evaluating the presence of up to five representative ions for every analyte, all measured at accurate mass (20-mDa mass window). The experimental ion abundance ratios were then compared to those of reference standards for confirmation. Sample treatment consisted of an extraction with hexane and subsequent normal-phase (NP) High performance liquid chromatography (HPLC) or SPE cleanup. The fat-free LC fractions were then investigated by GC-TOF MS.Full-spectral acquisition and accurate mass data generated by GC-TOF MS also allowed the investigation of nontarget compounds using appropriate processing software to manage MS data. Identification was initially based on library fit using commercial nominal mass libraries. This was followed by comparing the experimental accurate masses of the most relevant ions with the theoretical exact masses with calculations made using the elemental composition calculator included in the software.The application of both target and nontarget approaches to around 40 real samples allowed the detection and confirmation of several target pollutants including p,p'-DDE, hexachlorobenzene (HCB), and some polychlorinated biphenyls (PCBs) and polyaromatic hydrocarbons (PAHs). Several nontarget compounds that could be considered anthropogenic pollutants were also detected. These included 3,5-di-tert-butyl-4-hydroxy-toluene (BHT) and its metabolite 3,5-di

  2. Gas chromatography x gas chromatography-time-of-flight mass spectrometry analysis and antibacterial activity of essential oil from Amomum xanthophlebium

    International Nuclear Information System (INIS)

    Masila, A.; Aminah, I.; Yaakob, W.A.; Nazlina, I.

    2011-01-01

    Essential oils of fresh leaves, stem, rhizomes and whole aromatic plants of Amomum xanthophlebium (Zingiberaceae) were obtained by hydro distillation. Percentage yields of the leaf, stem and whole plant oils were 0.0032, 0.0074 and 0.0021 % whereas the rhizome oil obtained was very little. Chemical components of each oil and their percentages were determined by Gas Chromatography x Gas Chromatography-Time-of-Flight Mass Spectrometry (GCxGC-TOFMS). Analysis of A. xanthophlebium oils showed that they were dominated by terpenes. Main components in the leaves were allo-aromadendrene (3.41 %), (±)-globulol (2.58 %) and rosifoliol (2.55 %); stem, α-terpineol (4.25 %), rosifoliol (2.41 %) and bingpian (2.27 %); rhizomes, viridiflorol (5.72 %), (±)-globulol (5.23 %) and α-cadinol (4.81 %); whole plants, eucalyptol (4.11 %), l-α-terpineol (2.88 %) and rosifoliol (2.82 %). The stem oil of A. xanthophlebium showed antibacterial activity against Gram-negative Escherichia coli and Gram-positive methicillin-resistant Staphylococcus aureus (MRSA) at the minimum inhibitory concentration of 80 mg/ ml. (author)

  3. Detection of an extended human volatome with comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Phillips, Michael; Cataneo, Renee N; Chaturvedi, Anirudh; Kaplan, Peter D; Libardoni, Mark; Mundada, Mayur; Patel, Urvish; Zhang, Xiang

    2013-01-01

    Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOF MS) has been proposed as a powerful new tool for multidimensional analysis of complex chemical mixtures. We investigated GCxGC-TOF MS as a new method for identifying volatile organic compounds (VOCs) in normal human breath. Samples of alveolar breath VOCs and ambient room air VOC were collected with a breath collection apparatus (BCA) onto separate sorbent traps from 34 normal healthy volunteers (mean age = 40 yr, SD = 17 yr, male/female = 19/15). VOCs were separated on two serial capillary columns separated by a cryogenic modulator, and detected with TOF MS. The first and second dimension columns were non-polar and polar respectively. BCA collection combined with GC×GC-TOF MS analysis identified approximately 2000 different VOCs in samples of human breath, many of which have not been previously reported. The 50 VOCs with the highest alveolar gradients (abundance in breath minus abundance in ambient room air) mostly comprised benzene derivatives, acetone, methylated derivatives of alkanes, and isoprene. Collection and analysis of breath VOCs with the BCA-GC×GC-TOF MS system extended the size of the detectable human volatile metabolome, the volatome, by an order of magnitude compared to previous reports employing one-dimensional GC-MS. The size of the human volatome has been under-estimated in the past due to coelution of VOCs in one-dimensional GC analytical systems.

  4. Detection of an extended human volatome with comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Michael Phillips

    Full Text Available BACKGROUND: Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GCxGC-TOF MS has been proposed as a powerful new tool for multidimensional analysis of complex chemical mixtures. We investigated GCxGC-TOF MS as a new method for identifying volatile organic compounds (VOCs in normal human breath. METHODS: Samples of alveolar breath VOCs and ambient room air VOC were collected with a breath collection apparatus (BCA onto separate sorbent traps from 34 normal healthy volunteers (mean age = 40 yr, SD = 17 yr, male/female = 19/15. VOCs were separated on two serial capillary columns separated by a cryogenic modulator, and detected with TOF MS. The first and second dimension columns were non-polar and polar respectively. RESULTS: BCA collection combined with GC×GC-TOF MS analysis identified approximately 2000 different VOCs in samples of human breath, many of which have not been previously reported. The 50 VOCs with the highest alveolar gradients (abundance in breath minus abundance in ambient room air mostly comprised benzene derivatives, acetone, methylated derivatives of alkanes, and isoprene. CONCLUSIONS: Collection and analysis of breath VOCs with the BCA-GC×GC-TOF MS system extended the size of the detectable human volatile metabolome, the volatome, by an order of magnitude compared to previous reports employing one-dimensional GC-MS. The size of the human volatome has been under-estimated in the past due to coelution of VOCs in one-dimensional GC analytical systems.

  5. Potential metabolomic biomarkers for reliable diagnosis of Behcet's disease using gas chromatography/ time-of-flight-mass spectrometry.

    Science.gov (United States)

    Ahn, Joong Kyong; Kim, Jungyeon; Hwang, Jiwon; Song, Juhwan; Kim, Kyoung Heon; Cha, Hoon-Suk

    2017-05-24

    Although many diagnostic criteria of Behcet's disease (BD) have been developed and revised by experts, diagnosing BD is still complicated and challenging. No metabolomic studies on serum have been attempted to improve the diagnosis and to identify potential biomarkers of BD. The purposes of this study were to investigate distinctive metabolic changes in serum samples of BD patients and to identify metabolic candidate biomarkers for reliable diagnosis of BD using the metabolomics platform. Metabolomic profiling of 90 serum samples from 45 BD patients and 45 healthy controls (HCs) were performed via gas chromatography with time-of-flight mass spectrometry (GC/TOF-MS) with multivariate statistical analyses. A total of 104 metabolites were identified from samples. The serum metabolite profiles obtained from GC/TOF-MS analysis can distinguish BD patients from HC group in discovery set. The variation values of the partial least squared-discrimination analysis (PLS-DA) model are R 2 X of 0.246, R 2 Y of 0.913 and Q 2 of 0.852, respectively, indicating strong explanation and prediction capabilities of the model. A panel of five metabolic biomarkers, namely, decanoic acid, fructose, tagatose, linoleic acid and oleic acid were selected and adequately validated as putative biomarkers of BD (sensitivity 100%, specificity 97.1%, area under the curve 0.998) in the discovery set and independent set. The PLS_DA model showed clear discrimination of BD and HC groups by the five metabolic biomarkers in independent set. This is the first report on characteristic metabolic profiles and potential metabolite biomarkers in serum for reliable diagnosis of BD using GC/TOF-MS. Copyright © 2017. Published by Elsevier SAS.

  6. MetPP: a computational platform for comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry-based metabolomics.

    Science.gov (United States)

    Wei, Xiaoli; Shi, Xue; Koo, Imhoi; Kim, Seongho; Schmidt, Robin H; Arteel, Gavin E; Watson, Walter H; McClain, Craig; Zhang, Xiang

    2013-07-15

    Due to the high complexity of metabolome, the comprehensive 2D gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) is considered as a powerful analytical platform for metabolomics study. However, the applications of GC×GC-TOF MS in metabolomics are not popular owing to the lack of bioinformatics system for data analysis. We developed a computational platform entitled metabolomics profiling pipeline (MetPP) for analysis of metabolomics data acquired on a GC×GC-TOF MS system. MetPP can process peak filtering and merging, retention index matching, peak list alignment, normalization, statistical significance tests and pattern recognition, using the peak lists deconvoluted from the instrument data as its input. The performance of MetPP software was tested with two sets of experimental data acquired in a spike-in experiment and a biomarker discovery experiment, respectively. MetPP not only correctly aligned the spiked-in metabolite standards from the experimental data, but also correctly recognized their concentration difference between sample groups. For analysis of the biomarker discovery data, 15 metabolites were recognized with significant concentration difference between the sample groups and these results agree with the literature results of histological analysis, demonstrating the effectiveness of applying MetPP software for disease biomarker discovery. The source code of MetPP is available at http://metaopen.sourceforge.net xiang.zhang@louisville.edu Supplementary data are available at Bioinformatics online.

  7. Chemometrics-assisted effect-directed analysis of crude and refined oil using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Radović, Jagoš R; Thomas, Kevin V; Parastar, Hadi; Díez, Sergi; Tauler, Romà; Bayona, Josep M

    2014-01-01

    An effect-directed analysis (EDA) of fresh and artificially weathered (evaporated, photooxidized) samples of North Sea crude oil and residual heavy fuel oil is presented. Aliphatic, aromatic, and polar oil fractions were tested for the presence of aryl hydrocarbon receptor (AhR) agonist and androgen receptor (AR) antagonist, demonstrating for the first time the AR antagonist effects in the aromatic and, to a lesser extent, polar fractions. An extension of the typical EDA strategy to include an N-way partial least-squares (N-PLS) model capable of relating the comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-TOFMS) data set to the bioassay data obtained from normal-phase LC fractions is proposed. The predicted AhR binding effects in the fresh and artificially weathered aromatic oil fractions facilitated the identification of alkyl-substituted three- and four-ring aromatic systems in the active fractions through the weighting of their contributions to the observed effects. A N-PLS chemometric model is demonstrated as a potentially useful strategy for future EDA studies that can streamline the compound identification process and provide additional reduction of samples' complexity. The AhR binding effects of the suspected compounds predicted by N-PLS and identified by GC × GC-TOFMS were confirmed using quantitative structure-activity relationship (QSAR) estimates.

  8. Urinary Metabolomic Profiling to Identify Potential Biomarkers for the Diagnosis of Behcet's Disease by Gas Chromatography/Time-of-Flight-Mass Spectrometry.

    Science.gov (United States)

    Ahn, Joong Kyong; Kim, Jungyeon; Hwang, Jiwon; Song, Juhwan; Kim, Kyoung Heon; Cha, Hoon-Suk

    2017-11-02

    Diagnosing Behcet's disease (BD) is challenging because of the lack of a diagnostic biomarker. The purposes of this study were to investigate distinctive metabolic changes in urine samples of BD patients and to identify urinary metabolic biomarkers for diagnosis of BD using gas chromatography/time-of-flight-mass spectrometry (GC/TOF-MS). Metabolomic profiling of urine samples from 44 BD patients and 41 healthy controls (HC) were assessed using GC/TOF-MS, in conjunction with multivariate statistical analysis. A total of 110 urinary metabolites were identified. The urine metabolite profiles obtained from GC/TOF-MS analysis could distinguish BD patients from the HC group in the discovery set. The parameter values of the orthogonal partial least squared-discrimination analysis (OPLS-DA) model were R ² X of 0.231, R ² Y of 0.804, and Q ² of 0.598. A biomarker panel composed of guanine, pyrrole-2-carboxylate, 3-hydroxypyridine, mannose, l-citrulline, galactonate, isothreonate, sedoheptuloses, hypoxanthine, and gluconic acid lactone were selected and adequately validated as putative biomarkers of BD (sensitivity 96.7%, specificity 93.3%, area under the curve 0.974). OPLS-DA showed clear discrimination of BD and HC groups by a biomarker panel of ten metabolites in the independent set (accuracy 88%). We demonstrated characteristic urinary metabolic profiles and potential urinary metabolite biomarkers that have clinical value in the diagnosis of BD using GC/TOF-MS.

  9. Gas chromatography time-of-flight mass spectrometry (GC-TOF-MS-based metabolomics for comparison of caffeinated and decaffeinated coffee and its implications for Alzheimer's disease.

    Directory of Open Access Journals (Sweden)

    Kai Lun Chang

    Full Text Available Findings from epidemiology, preclinical and clinical studies indicate that consumption of coffee could have beneficial effects against dementia and Alzheimer's disease (AD. The benefits appear to come from caffeinated coffee, but not decaffeinated coffee or pure caffeine itself. Therefore, the objective of this study was to use metabolomics approach to delineate the discriminant metabolites between caffeinated and decaffeinated coffee, which could have contributed to the observed therapeutic benefits. Gas chromatography time-of-flight mass spectrometry (GC-TOF-MS-based metabolomics approach was employed to characterize the metabolic differences between caffeinated and decaffeinated coffee. Orthogonal partial least squares discriminant analysis (OPLS-DA showed distinct separation between the two types of coffee (cumulative Q(2 = 0.998. A total of 69 discriminant metabolites were identified based on the OPLS-DA model, with 37 and 32 metabolites detected to be higher in caffeinated and decaffeinated coffee, respectively. These metabolites include several benzoate and cinnamate-derived phenolic compounds, organic acids, sugar, fatty acids, and amino acids. Our study successfully established GC-TOF-MS based metabolomics approach as a highly robust tool in discriminant analysis between caffeinated and decaffeinated coffee samples. Discriminant metabolites identified in this study are biologically relevant and provide valuable insights into therapeutic research of coffee against AD. Our data also hint at possible involvement of gut microbial metabolism to enhance therapeutic potential of coffee components, which represents an interesting area for future research.

  10. Comparison of two algorithmic data processing strategies for metabolic fingerprinting by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Almstetter, Martin F; Appel, Inka J; Dettmer, Katja; Gruber, Michael A; Oefner, Peter J

    2011-09-28

    The alignment algorithm Statistical Compare (SC) developed by LECO Corporation for the processing of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) data was validated and compared to the in-house developed retention time correction and data alignment tool INCA (Integrative Normalization and Comparative Analysis) by a spike-in experiment and the comparative metabolic fingerprinting of a wild type versus a double mutant strain of Escherichia coli (E. coli). Starting with the same peak lists generated by LECO's ChromaTOF software, the accuracy of peak alignment and detection of 1.1- to 4-fold changes in metabolite concentration was assessed by spiking 20 standard compounds into an aqueous methanol extract of E. coli. To provide the same quality input signals for both alignment routines, the universal m/z 73 trace of the trimethylsilyl (TMS) group was used as a quantitative measure for all features. The performance of data processing and alignment was evaluated and illustrated by ROC curves. Statistical Compare performed marginally better at the lower fold changes, while INCA did so at the higher fold changes. Using SC, quantitative precision could be improved substantially by exploiting the signal intensities of metabolite-specific unique (U) m/z ion traces rather than the universal m/z 73 trace. A list of 56 features that distinguished the two E. coli strains was obtained by the SC alignment using m/z U with an estimated false discovery rate (FDR) of <0.05. Ultimately, 23 metabolites could be identified, one additional and five less than with INCA due to the failure of SC to extract unitized m/z U's across all fingerprints with suitable spectral intensities for the latter metabolites. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. Non-Halal biomarkers identification based on Fourier Transform Infrared Spectroscopy (FTIR) and Gas Chromatography-Time of Flight Mass Spectroscopy (GC-TOF MS) techniques

    Science.gov (United States)

    Witjaksono, Gunawan; Saputra, Irwan; Latief, Marsad; Jaswir, Irwandi; Akmeliawati, Rini; Abdelkreem Saeed Rabih, Almur

    2017-11-01

    Consumption of meat from halal (lawful) sources is essential for Muslims. The identification of non-halal meat is one of the main issues that face consumers in meat markets, especially in non-Islamic countries. Pig is one of the non-halal sources of meat, and hence pig meat and its derivatives are forbidden for Muslims to consume. Although several studies have been conducted to identify the biomarkers for nonhalal meats like pig meat, these studies are still in their infancy stages, and as a result there is no universal biomarker which could be used for clear cut identification. The purpose of this paper is to use Fourier Transform Infrared Spectroscopy (FTIR) and Gas Chromatography-Time of Flight Mass Spectroscopy (GC-TOF MS) techniques to study fat of pig, cow, lamb and chicken to find possible biomarkers for pig fat (lard) identification. FTIR results showed that lard and chicken fat have unique peaks at wavenumbers 1159.6 cm-1, 1743.4 cm-1, 2853.1 cm-1 and 2922.5 cm-1 compared to lamb and beef fats which did not show peaks at these wavenumbers. On the other hand, GC/MS-TOF results showed that the concentration of 1,2,3-trimethyl-Benzene, Indane, and Undecane in lard are 250, 14.5 and 1.28 times higher than their concentrations in chicken fat, respectively, and 91.4, 2.3 and 1.24 times higher than their concentrations in cow fat, respectively. These initial results clearly indicate that there is a possibility to find biomarkers for non-halal identification.

  12. Characterization of olive oil volatiles by multi-step direct thermal desorption-comprehensive gas chromatography-time-of-flight mass spectrometry using a programmed temperature vaporizing injector

    NARCIS (Netherlands)

    de Koning, S.; Kaal, E.; Janssen, H.-G.; van Platerink, C.; Brinkman, U.A.Th.

    2008-01-01

    The feasibility of a versatile system for multi-step direct thermal desorption (DTD) coupled to comprehensive gas chromatography (GC × GC) with time-of-flight mass spectrometric (TOF-MS) detection is studied. As an application the system is used for the characterization of fresh versus aged olive

  13. Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Lima Gomes, Paulo C F; Barnes, Brian B; Santos-Neto, Álvaro J; Lancas, Fernando M; Snow, Nicholas H

    2013-07-19

    Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC-ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC-ToF/MS provided linear ranges from 0.6 to 1200μgL(-1) and limits of detection and quantitation from 0.02 to 100μgL(-1). A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC-ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Study of alkyl phosphates in industrial petroleum mixtures by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Harynuk, James J; Rossé, Aleisha D; McGarvey, G Bryce

    2011-11-01

    Dialkyl phosphate esters used as gellants in some oil well fracturing processes for conventional oil production can result in contamination of the collected crude. Though the exact mechanism is unclear, such compounds form volatile phosphorus that compromises refinery processes. Our initial research involved producing a comprehensive two-dimensional gas chromatographic method (GC × GC) for the detection and quantification of alkyl phosphate esters in petroleum samples, which surpassed the current method employed in sensitivity and speciation capabilities. However, selective detection is required for such analytes in petroleum matrices. This article describes the application of GC × GC with time-of-flight mass spectrometry for selective detection to the analysis of di- and tri-alkyl phosphates in petroleum samples. Features in the electron impact mass spectra of alkyl phosphates are discussed along with the GC × GC retention characteristics of the compounds. Based on these discussions, a preliminary classification and quantification of alkyl phosphate contamination in a suite of industrial samples is then presented.

  15. Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.

    Science.gov (United States)

    Zhang, Caixiang; Eganhouse, Robert P; Pontolillo, James; Cozzarelli, Isabelle M; Wang, Yanxin

    2012-03-23

    4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid-liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC×GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Determination of nonylphenol isomers in landfill leachate and municipal wastewater using steam distillation extraction coupled with comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry

    Science.gov (United States)

    Zhang, Caixiang; Eganhouse, Robert P.; Pontolillo, James; Cozzarelli, Isabelle M.; Wang, Yanxin

    2012-01-01

    4-Nonylphenols (4-NPs) are known endocrine disruptors and by-products of the microbial degradation of nonylphenol polyethoxylate surfactants. One of the challenges to understanding the toxic effects of nonylphenols is the large number of isomers that may exist in environmental samples. In order to attribute toxic effects to specific compounds, a method is needed for the separation and quantitation of individual nonylphenol isomers. The pre-concentration methods of solvent sublimation, solid-phase extraction or liquid–liquid extraction prior to chromatographic analysis can be problematic because of co-extraction of thousands of compounds typically found in complex matrices such as municipal wastewater or landfill leachate. In the present study, steam distillation extraction (SDE) was found to be an effective pre-concentration method for extraction of 4-NPs from leachate and wastewater, and comprehensive two-dimensional gas chromatography (GC × GC) coupled with fast mass spectral data acquisition by time-of-flight mass spectrometry (ToFMS) enhanced the resolution and identification of 4-NP isomers. Concentrations of eight 4-NP isomers were determined in leachate from landfill cells of different age and wastewater influent and effluent samples. 4-NP isomers were about 3 times more abundant in leachate from the younger cell than the older one, whereas concentrations in wastewater effluent were either below detection limits or <1% of influent concentrations. 4-NP isomer distribution patterns were found to have been altered following release to the environment. This is believed to reflect isomer-specific degradation and accumulation of 4-NPs in the aquatic environment.

  17. Tile-based Fisher-ratio software for improved feature selection analysis of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry data.

    Science.gov (United States)

    Marney, Luke C; Siegler, W Christopher; Parsons, Brendon A; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

    2013-10-15

    Comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a highly capable instrumental platform that produces complex and information-rich multi-dimensional chemical data. The data can be initially overwhelming, especially when many samples (of various sample classes) are analyzed with multiple injections for each sample. Thus, the data must be analyzed in such a way as to extract the most meaningful information. The pixel-based and peak table-based Fisher ratio algorithmic approaches have been used successfully in the past to reduce the multi-dimensional data down to those chemical compounds that are changing between the sample classes relative to those that are not changing (i.e., chemical feature selection). We report on the initial development of a computationally fast novel tile-based Fisher-ratio software that addresses the challenges due to 2D retention time misalignment without explicitly aligning the data, which is often a shortcoming for both pixel-based and peak table-based algorithmic approaches. Concurrently, the tile-based Fisher-ratio algorithm significantly improves the sensitivity contrast of true positives against a background of potential false positives and noise. In this study, eight compounds, plus one internal standard, were spiked into diesel at various concentrations. The tile-based F-ratio algorithmic approach was able to "discover" all spiked analytes, within the complex diesel sample matrix with thousands of potential false positives, in each possible concentration comparison, even at the lowest absolute spiked analyte concentration ratio of 1.06, the ratio between the concentrations in the spiked diesel sample to the native concentration in diesel. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Automating data analysis for two-dimensional gas chromatography/time-of-flight mass spectrometry non-targeted analysis of comparative samples.

    Science.gov (United States)

    Titaley, Ivan A; Ogba, O Maduka; Chibwe, Leah; Hoh, Eunha; Cheong, Paul H-Y; Simonich, Staci L Massey

    2018-03-16

    Non-targeted analysis of environmental samples, using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC/ToF-MS), poses significant data analysis challenges due to the large number of possible analytes. Non-targeted data analysis of complex mixtures is prone to human bias and is laborious, particularly for comparative environmental samples such as contaminated soil pre- and post-bioremediation. To address this research bottleneck, we developed OCTpy, a Python™ script that acts as a data reduction filter to automate GC × GC/ToF-MS data analysis from LECO ® ChromaTOF ® software and facilitates selection of analytes of interest based on peak area comparison between comparative samples. We used data from polycyclic aromatic hydrocarbon (PAH) contaminated soil, pre- and post-bioremediation, to assess the effectiveness of OCTpy in facilitating the selection of analytes that have formed or degraded following treatment. Using datasets from the soil extracts pre- and post-bioremediation, OCTpy selected, on average, 18% of the initial suggested analytes generated by the LECO ® ChromaTOF ® software Statistical Compare feature. Based on this list, 63-100% of the candidate analytes identified by a highly trained individual were also selected by OCTpy. This process was accomplished in several minutes per sample, whereas manual data analysis took several hours per sample. OCTpy automates the analysis of complex mixtures of comparative samples, reduces the potential for human error during heavy data handling and decreases data analysis time by at least tenfold. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Optimization of separation and detection conditions for the multiresidue analysis of pesticides in grapes by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Banerjee, Kaushik; Patil, Sangram H; Dasgupta, Soma; Oulkar, Dasharath P; Patil, Shubhangi B; Savant, Rahul; Adsule, Pandurang G

    2008-05-09

    A comprehensive GCxGC-TOFMS method was optimized for multiresidue analysis of pesticides using a combination of a non-polar (RTX-5MS, 10 m x 0.18 mm x 0.2 microm) and a polar capillary column (TR-50MS, 1 m x 0.1 mm x 0.1 microm), connected in series through a dual stage thermal modulator. The method resolved the co-elution problems as observed in full scan one-dimensional GC-MS analysis and allowed chromatographic separation of 51 pesticides within 24 min run time with library-searchable mass spectrometric confirmation. Four pesticides, viz. chlorpyrifos-methyl, vinclozoline, parathion-methyl and heptachlor could be baseline separated on GCxGC, which were otherwise closely eluting and interfering each other's detection in 1D GC-MS run. Similarly, it could be possible to separate myclobutanil, buprofezin, flusilazole and oxyfluorfen on GCxGC. Although in 1D GC-MS, these closely eluting compounds could be identified through deconvolution algorithm and 'peak-find' option of the Chromatof software but the spectral purity significantly improved on GCxGC analysis. Thorough optimization was accomplished for the oven temperature programming, ion source temperature and GCxGC parameters like modulation period, duration of hot pulses, modulation-offset temperature, acquisition rate, etc. to achieve best possible separation of the test compounds. The limit of detection significantly improved by 2-12 times on GCxGC-TOFMS against GC-TOFMS because of sharper and narrower peak shapes. The method was tested for grape matrix after preparing the samples using previously described method and recoveries of the entire test pesticides were within 70-110% at 10 ng/g level of fortification. GCxGC-TOFMS was found to be an excellent technique for library-based screening of pesticides with high accuracy and sensitivity.

  20. Characterisation of Stevia Rebaudiana by comprehensive two-dimensional liquid chromatography time-of-flight mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Pól, Jaroslav; Hohnová, B.; Hyötyläinen, T.

    2007-01-01

    Roč. 1150, 1-2 (2007), s. 85-92 ISSN 0021-9673 R&D Projects: GA AV ČR KJB4031405 Institutional research plan: CEZ:AV0Z40310501 Keywords : comprehensive two-dimensional liquid chromatography * time-of-flight mass spectrometry * Stevia rebaudiana Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.641, year: 2007

  1. Accurate mass error correction in liquid chromatography time-of-flight mass spectrometry based metabolomics

    NARCIS (Netherlands)

    Mihaleva, V.V.; Vorst, O.F.J.; Maliepaard, C.A.; Verhoeven, H.A.; Vos, de C.H.; Hall, R.D.; Ham, van R.C.H.J.

    2008-01-01

    Compound identification and annotation in (untargeted) metabolomics experiments based on accurate mass require the highest possible accuracy of the mass determination. Experimental LC/TOF-MS platforms equipped with a time-to-digital converter (TDC) give the best mass estimate for those mass signals

  2. Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Akoto, L.; Stellaard, F.; Irth, H.; Vreuls, R.J.J.; Pel, R.

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GC × GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

  3. Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Akoto, Lawrence; Stellaard, Frans; Irth, Hubertus; Vreuls, Rene J. J.; Pel, Roel

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GC x GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

  4. Atmospheric pressure gas chromatography-time-of-flight-mass spectrometry (APGC-ToF-MS) for the determination of regulated and emerging contaminants in aqueous samples after stir bar sorptive extraction (SBSE).

    Science.gov (United States)

    Pintado-Herrera, Marina G; González-Mazo, Eduardo; Lara-Martín, Pablo A

    2014-12-03

    This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50-100%) and limits of detection below 1ngL(-1) for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC-ToF-MS. To the best of our knowledge, this is the first time that this technique has been applied for the analysis of contaminants in aquatic systems. By employing lower energy than the more widely used electron impact ionization (EI), AGPC provides significant advantages over EI for those substances very susceptible to high fragmentation (e.g., fragrances, pyrethroids). Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Akoto, Lawrence; Stellaard, Frans; Irth, Hubertus; Vreuls, René J J; Pel, Roel

    2008-04-04

    Comprehensive two-dimensional gas chromatography (GC x GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix sp. strain MRI without any sample preparation steps. It is shown that the technique can be useful in the identification of lipid markers in food-web as well as environmental studies. For instance, new mono- and diunsaturated fatty acids were found in the C(16) and C(18) regions of the green algae S. acutus and the filamentous cyanobacterium Limnothrix sp. strain MRI samples. These fatty acids have not, to our knowledge, been detected in the conventional one-dimensional (1D) GC analysis of these species due to either co-elution and/or their presence in low amounts in the sample matrix. In GC x GC, all congeners of the fatty acids in these microorganisms could be detected and identified due to the increased analyte detectability and ordered structures in the two-dimensional separation space. The combination of direct thermal desorption (DTD)-GC x GC-time-of-flight mass spectrometry (ToF-MS) promises to be an excellent tool for a more accurate profiling of biological samples and can therefore be very useful in lipid biomarker research as well as food-web and ecological studies.

  6. Tile-based Fisher ratio analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) data using a null distribution approach.

    Science.gov (United States)

    Parsons, Brendon A; Marney, Luke C; Siegler, W Christopher; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

    2015-04-07

    Comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a versatile instrumental platform capable of collecting highly informative, yet highly complex, chemical data for a variety of samples. Fisher-ratio (F-ratio) analysis applied to the supervised comparison of sample classes algorithmically reduces complex GC × GC-TOFMS data sets to find class distinguishing chemical features. F-ratio analysis, using a tile-based algorithm, significantly reduces the adverse effects of chromatographic misalignment and spurious covariance of the detected signal, enhancing the discovery of true positives while simultaneously reducing the likelihood of detecting false positives. Herein, we report a study using tile-based F-ratio analysis whereby four non-native analytes were spiked into diesel fuel at several concentrations ranging from 0 to 100 ppm. Spike level comparisons were performed in two regimes: comparing the spiked samples to the nonspiked fuel matrix and to each other at relative concentration factors of two. Redundant hits were algorithmically removed by refocusing the tiled results onto the original high resolution pixel level data. To objectively limit the tile-based F-ratio results to only features which are statistically likely to be true positives, we developed a combinatorial technique using null class comparisons, called null distribution analysis, by which we determined a statistically defensible F-ratio cutoff for the analysis of the hit list. After applying null distribution analysis, spiked analytes were reliably discovered at ∼1 to ∼10 ppm (∼5 to ∼50 pg using a 200:1 split), depending upon the degree of mass spectral selectivity and 2D chromatographic resolution, with minimal occurrence of false positives. To place the relevance of this work among other methods in this field, results are compared to those for pixel and peak table-based approaches.

  7. Part-per-trillion determination of pharmaceuticals, pesticides, and related organic contaminants in river water by solid-phase extraction followed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Matamoros, Víctor; Jover, Eric; Bayona, Josep M

    2010-01-15

    An analytical procedure based on comprehensive two-dimensional gas chromatography (GC x GC) coupled with time-of-flight mass spectrometry (TOF-MS) for the simultaneous determination of 97 organic contaminants at trace concentration in river water is presented. The target analytes included 13 pharmaceuticals, 18 plasticizers, 8 personal care products, 9 acid herbicides, 8 triazines, 10 organophosphorous compounds, 5 phenylureas, 12 organochlorine biocides, 9 polycyclic aromatic hydrocarbons (PAHs), and 5 benzothiazoles and benzotriazoles. The best resolution of the target analytes in the contour plots was obtained when a nonpolar stationary phase was used in the first dimension and polar one in the second. However, in the opposite configuration, polar-nonpolar, the retention time in the second dimension exhibited a strong correlation with the log Kow (p identification criteria. The developed methodology is based on a polymeric solid-phase extraction followed by in GC-port methylation and GC x GC/TOF-MS determination. Moreover, limits of detection (LODs) and quantification (LOQs) ranged from 0.5 to 100 ng/L and from 2 to 185 ng/L, respectively. Repeatability was always lower than 20%. Finally, the developed method has been successfully applied to the determination of incurred target analytes in four river waters subjected to a different anthropogenic pressure.

  8. Fast and robust direct immersion solid phase microextraction coupled with gas chromatography-time-of-flight mass spectrometry method employing a matrix compatible fiber for determination of triazole fungicides in fruits.

    Science.gov (United States)

    Silva, Érica A Souza; Lopez-Avila, Viorica; Pawliszyn, Janusz

    2013-10-25

    A fast and robust method was developed for the determination of ten triazole fungicides in fruit samples using direct immersion solid-phase microextraction coupled to gas chromatography with time-of-flight mass spectrometry detection (DI-SPME-GC-ToFMS). In this work, a newly developed concept of solid-phase microextraction (SPME) sorbent, which allows for direct immersion extraction in complex food matrices, has been applied in the analysis of 10 triazole fungicides in grapes and strawberries pulps. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction temperature, sample pH, and ionic strength, agitation speed, extraction and desorption times. Under optimized conditions, the method was linear for over 4 orders of magnitude in concentration, with linear regression coefficients (R(2)) greater than 0.99 for all test compounds in both matrices. Method reproducibility, as determined by analysis of spiked grapes and strawberries, was better than ±20%. The limits of quantitation objective (LOQs) ranged from 0.25 to 5 ng g(-1) for both matrices, well below the maximum residues levels allowed for those compounds in both matrices. The method was successfully applied in the analysis of commercial samples of grapes and strawberries. Finally, the new SPME method was compared to a modified version of t QuEChERS AOAC method: the limits of quantitation reached by SPME were at least one order of magnitude lower than those achieved by the QuEChERS method, whereas precision and accuracy were comparable for both methods. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Separation of VX, RVX and GB Enantiomers Using Liquid ChromatographyTime-of-Flight Mass Spectrometry

    Science.gov (United States)

    2016-02-01

    and GB Enantiomers Using Liquid Chromatography– Time-of-Flight Mass Spectrometry 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT...used for liquid chromatography–time-of-flight mass spectrometry analysis. For large-scale separation and quantitation, the UV absorbance at 210 nm (with...RVX, AND GB ENANTIOMERS USING LIQUID CHROMATOGRAPHY–TIME-OF-FLIGHT MASS SPECTROMETRY 1. INTRODUCTION Tetra-coordinate pentavalent

  10. Analysis of sucralose and other sweeteners in water and beverage samples by liquid chromatography/time-of-flight mass spectrometry.

    Science.gov (United States)

    Ferrer, Imma; Thurman, E Michael

    2010-06-18

    A methodology for the chromatographic separation and analysis of three of the most popular artificial sweeteners (aspartame, saccharin, and sucralose) in water and beverage samples was developed using liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS). The sweeteners were extracted from water samples using solid-phase extraction (SPE) cartridges. Furthermore, several beverages were analyzed by a rapid and simple method without SPE, and the presence of the sweeteners was confirmed by accurate mass measurements below 2-ppm error. The unambiguous confirmation of the compounds was based on accurate mass measurements of the protonated molecules [M+H](+), their sodium adducts and their main fragment ions. Quantitation was carried out using matrix-matched standard calibration and linearity of response over 2 orders of magnitude was demonstrated (r>0.99). A detailed fragmentation study for sucralose was carried out by time-of-flight and a characteristic spectrum fingerprint pattern was obtained for the presence of this compound in water samples. Finally, the analysis of several wastewater, surface water and groundwater samples from the US showed that sucralose can be found in the aquatic environment at concentrations up to 2.4microg/L, thus providing a good indication of wastewater input from beverage sources. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  11. Qualitative and Quantitative Analysis of Andrographis paniculata by Rapid Resolution Liquid Chromatography/Time-of-Flight Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jian-Fei Qin

    2013-09-01

    Full Text Available A rapid resolution liquid chromatography/time-of-flight tandem mass spectrometry (RRLC-TOF/MS method was developed for qualitative and quantitative analysis of the major chemical constituents in Andrographis paniculata. Fifteen compounds, including flavonoids and diterpenoid lactones, were unambiguously or tentatively identified in 10 min by comparing their retention times and accurate masses with standards or literature data. The characteristic fragmentation patterns of flavonoids and diterpenoid lactones were summarized, and the structures of the unknown compounds were predicted. Andrographolide, dehydroandrographolide and neoandrographolide were further quantified as marker substances. It was found that the calibration curves for all analytes showed good linearity (R2 > 0.9995 within the test ranges. The overall limits of detection (LODs and limits of quantification (LOQs were 0.02 μg/mL to 0.06 μg/mL and 0.06 μg/mL to 0.2 μg/mL, respectively. The relative standard deviations (RSDs for intra- and inter-day precisions were below 3.3% and 4.2%, respectively. The mean recovery rates ranged from 96.7% to 104.5% with the relative standard deviations (RSDs less than 2.72%. It is concluded that RRLC-TOF/MS is powerful and practical in qualitative and quantitative analysis of complex plant samples due to time savings, sensitivity, precision, accuracy and lowering solvent consumption.

  12. An ultra performance liquid chromatography-time-of-flight-mass spectrometric method for fast analysis of ginsenosides in Panax ginseng root

    NARCIS (Netherlands)

    Hu, C.; Kong, H.; Zhu, C.; Wei, H.; Hankemeier, T.; Greef, J. van der; Wang, M.; Xu, G.

    2011-01-01

    A method for fast analysis of ginsenosides in Panax ginseng roots was developed using ultra performance liquid chromatography-time-of-flight-mass spectrometry (UPLC-TOF-MS). The column used was HSS T3 (100 mm × 2.1 mm, 1.8 µm). The mobile phase consisted of 15 mmol/L ammonium formate and

  13. Determination of Prazosin and Simvastatin in Landfill Leachate using Liquid Chromatography-Time of Flight-Mass Spectrometry

    International Nuclear Information System (INIS)

    Zainab Haider Mussa; Zainab Haider Mussa; Fouad Fadhil Al-Qaim; Fouad Fadhil Al-Qaim; Md Pauzi Abdullah; Mohamed Rozali Othman

    2016-01-01

    Human pharmaceuticals have been shown to occur in considerably high amounts in sewage treatment plant (STP) effluents and surface waters. So far there is no data available on the occurrence of prazosin and simvastatin in leachate sample in Malaysia. Thus, this study is the first report to analysis of prazosin and simvastatin in leachate samples by using solid phase extraction-liquid chromatography-time of flight-mass spectrometry (SPE-LC-TOF-MS). The proposed method included isolation and reconstitute procedure. The linearity range was achieved at 1.5-3000 μg/ L and 0.8-125 μg/ L for prazosin and simvstatin, respectively with a determination coefficient (R 2 ) > 0.99. The limit of quantification (LOQ) for prazosin and simvastatin was calculated at 2.1 and 0.5 ng/ L in deionised water (DIW), meanwhile it was recorded at 3.5 and 2.4 ng/ L for prazosin and simvastatin in effluent sample, respectively. Two pharmaceutical compounds were detected in the leachate samples: prazosin and simvastatin at concentrations levels of 3850 and 415 ng/ L, respectively. (author)

  14. Investigation of storage time-dependent alterations of enantioselective amino acid profiles in kimchi using liquid chromatography-time of flight mass spectrometry.

    Science.gov (United States)

    Taniguchi, Moyu; Konya, Yutaka; Nakano, Yosuke; Fukusaki, Eiichiro

    2017-10-01

    Although naturally abundant amino acids are represented mainly by l-enantiomers, fermented foods are known to contain various d-amino acids. Enantiospecific profiles of food products can vary due to fermentation by bacteria, and such alterations may contribute to changes in food properties that would not be dependent exclusively on l-amino acids. Therefore, more attention should be paid to the study of temporal alterations of d-amino acid profiles during fermentation process. However, there have been very few studies reporting time-dependent profiling of d-amino acids because enantioseparation of widely targeted d-amino acids is technically difficult. This study aimed to achieve high throughput profiling of amino acids enantiomers. Enantioselective profiling of amino acids using CROWNPAK CR-I(+) column, liquid chromatography, time of flight mass spectrometry, and principle component analysis was performed to investigate time-dependent alterations in concentrations of free d- and l-amino acids in kimchi stored at 4°C or 25°C. We demonstrated significant changes in d- and l-amino acid profiles in kimchi stored at 25°C. In particular, concentrations of the amino acids d-Ala, d-Ser, d-allo-Ile, d-Leu, d-Asp, d-Glu, and d-Met became higher in kimchi with storage time. This is the first report of time-dependent alterations of d- and l-amino acid contents in kimchi. This study showed that our analytical method of enantioselective detection of amino acids using liquid chromatography time-of-flight mass spectrometry (LC-TOFMS) with CROWNPAK CR-I(+) enables high throughput food screening and can be recommended for advanced studies of the relationship between d-amino acid content and food properties. Copyright © 2017 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  15. A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kolmonen, Marjo [Forensic Toxicology Division, Department of Forensic Medicine, University of Helsinki (Finland) and Doping Control Laboratory, United Laboratories Ltd., Helsinki (Finland)]. E-mail: marjo.kolmonen@helsinki.fi; Leinonen, Antti [Doping Control Laboratory, United Laboratories Ltd., Helsinki (Finland); Pelander, Anna [Forensic Toxicology Division, Department of Forensic Medicine, University of Helsinki (Finland); Ojanperae, Ilkka [Forensic Toxicology Division, Department of Forensic Medicine, University of Helsinki (Finland)

    2007-02-28

    A general screening method based on solid phase extraction (SPE) and liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) was developed and investigated with 124 different doping agents, including stimulants, {beta}-blockers, narcotics, {beta}{sub 2}-adrenergic agonists, agents with anti-estrogenic activity, diuretics and cannabinoids. Mixed mode cation exchange/C8 cartridges were applied to SPE, and chromatography was based on gradient elution on a C18 column. Ionization of the analytes was achieved with electrospray ionization in the positive mode. Identification by LC/TOFMS was based on retention time, accurate mass and isotopic pattern. Validation of the method consisted of analysis of specificity, analytical recovery, limit of detection and repeatability. The minimum required performance limit (MRPL), established by World Anti-Doping Agency (WADA), was attained to 97 doping agents. The extraction recoveries varied between 33 and 98% and the median was 58%. Mass accuracy was always better than 5 ppm, corresponding to a maximum mass error of 0.7 mDa. The repeatability of the method for spiked urine samples, expressed as median of relative standard deviations (RSD%) at concentrations of MRPL and 10 times MRPL, were 14% and 9%, respectively. The suitability of the LC/TOFMS method for doping control was demonstrated with authentic urine samples.

  16. A pre-processing strategy for liquid chromatography time-of-flight mass spectrometry metabolic fingerprinting data

    DEFF Research Database (Denmark)

    Nielsen, Nikoline Juul; Tomasi, Giorgio; Frandsen, Rasmus John Normand

    2010-01-01

    A series of simple and robust operations for handling large chromatographic time-of-flight mass spectrometry fingerprinting data has been established and applied to data from extracts of Fusarium graminearum genotypes modified in a non-ribosomal peptide synthase gene by over-expression and deleti...

  17. Detection and identification of diterpenoid alkaloids, isoflavonoids and saponins in Qifu decoction and rat plasma by liquid chromatography-time-of-flight mass spectrometry.

    Science.gov (United States)

    Tan, Guangguo; Jing, Jing; Zhu, Zhenyu; Lou, Ziyang; Li, Wuhong; Zhao, Liang; Zhang, Guoqing; Chai, Yifeng

    2012-02-01

    A liquid chromatography-time-of-flight mass spectrometric (LC-TOFMS) method has been developed for analysis of components in Qifu decoction (QFD), a traditional Chinese medical formula consisting of Radix Astragali and Acontium carmichaeli, and in rat plasma after oral administration. Based on accurate mass measurements within 3 ppm error for each molecular ion and subsequent fragment ions of TOFMS, as well as matching of empirical molecular formulae with those of published components in the in-house chemical library, a total of 44 major components including 21 diterpenoid alkaloids, 12 flavonoids and 11 saponins were identified in QFD. After oral administration of QFD, 22 components in rat plasma were detected and identified by comparing and contrasting the constituents measured in QFD with those in the plasma samples. The results provided valuable chemical information for further pharmacology and active mechanism research on QFD. LC-TOFMS was also applied for the comparison of relative peak area of major active components between QFD and the single herb extracts. The concentration ratios of major saponins detected in the crude herb Radix Astragali were found to be different from those in QFD. The experimental data indicated that the decocting process could result in differences in the amounts of active components. Copyright © 2011 John Wiley & Sons, Ltd.

  18. Liquid chromatography time of flight mass spectrometry based environmental metabolomics for the analysis of Pseudomonas putida Bacteria in potable water.

    Science.gov (United States)

    Kouremenos, Konstantinos A; Beale, David J; Antti, Henrik; Palombo, Enzo A

    2014-09-01

    Water supply biofilms have the potential to harbour waterborne diseases, accelerate corrosion, and contribute to the formation of tuberculation in metallic pipes. One particular species of bacteria known to be found in the water supply networks is Pseudomonas sp., with the presence of Pseudomonas putida being isolated to iron pipe tubercles. Current methods for detecting and analysis pipe biofilms are time consuming and expensive. The application of metabolomics techniques could provide an alternative method for assessing biofilm risk more efficiently based on bacterial activity. As such, this paper investigates the application of metabolomic techniques and provides a proof-of-concept application using liquid chromatography coupled with time-of-flight mass spectrometry (LC-ToF-MS) to three biologically independent P. putida samples, across five different growth conditions exposed to solid and soluble iron (Fe). Analysis of the samples in +ESI and -ESI mode yielded 887 and 1789 metabolite features, respectively. Chemometric analysis of the +ESI and -ESI data identified 34 and 39 significant metabolite features, respectively, where features were considered significant if the fold change was greater than 2 and obtained a p-value less than 0.05. Metabolite features were subsequently identified according to the Metabolomics Standard Initiative (MSI) Chemical Analysis Workgroup using analytical standards and standard online LC-MS databases. Possible markers for P. putida growth, with and without being exposed to solid and soluble Fe, were identified from a diverse range of different chemical classes of metabolites including nucleobases, nucleosides, dipeptides, tripeptides, amino acids, fatty acids, sugars, and phospholipids. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. An Ultrahigh-Performance Liquid Chromatography-Time-of-Flight Mass Spectrometry Metabolomic Approach to Studying the Impact of Moderate Red-Wine Consumption on Urinary Metabolome.

    Science.gov (United States)

    Esteban-Fernández, Adelaida; Ibañez, Clara; Simó, Carolina; Bartolomé, Begoña; Moreno-Arribas, M Victoria

    2018-04-06

    Moderate red-wine consumption has been widely described to exert several benefits in human health. This is mainly due to its unique content of bioactive polyphenols, which suffer several modifications along their pass through the digestive system, including microbial transformation in the colon and phase-II metabolism, until they are finally excreted in urine and feces. To determine the impact of moderate wine consumption in the overall urinary metabolome of healthy volunteers ( n = 41), samples from a red-wine interventional study (250 mL/day, 28 days) were investigated. Urine (24 h) was collected before and after intervention and analyzed by an untargeted ultrahigh-performance liquid chromatography-time-of-flight mass spectrometry metabolomics approach. 94 compounds linked to wine consumption, including specific wine components (tartaric acid), microbial-derived phenolic metabolites (5-(dihydroxyphenyl)-γ-valerolactones and 4-hydroxyl-5-(phenyl)-valeric acids), and endogenous compounds were identified. Also, some relationships between parallel fecal and urinary metabolomes are discussed.

  20. 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.

  1. Improved fatty acid detection in micro-algae and aquatic meiofauna species using a direct thermal desorption interface combined with comprehensive gas chromatography-time-of-flight spectrometry.

    NARCIS (Netherlands)

    Akoto, L.; Stellaard, F.; Irth, H.; Vreuls, R.J.J.; Pel, R.

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GC × GC) with time-of-flight mass spectrometry detection is used to profile the fatty acid composition of whole/intact aquatic microorganisms such as the common fresh water green algae Scenedesmus acutus and the filamentous cyanobacterium Limnothrix

  2. New drostanolone metabolites in human urine by liquid chromatography time-of-flight tandem mass spectrometry and their application for doping control.

    Science.gov (United States)

    Liu, Yang; Lu, Jianghai; Yang, Sheng; Zhang, Qingying; Xu, Youxuan

    2016-04-01

    Drostanolone is one of the most frequently detected anabolic androgenic steroids in doping control analysis. Here, we studied drostanolone urinary metabolic profiles using liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. The drug was administered to one healthy male volunteer and liquid-liquid extraction along with direct-injection were used to analyze urine samples. Chromatographic peaks for potential metabolites were identified with the theoretical [M-H](-) as a target ion in a full scan experiment and actual deprotonated ions were analyzed in targeted MS/MS mode. Eleven metabolites including five new sulfates, five glucuronide conjugates, and one free metabolite were confirmed for drostanolone. Due to the absence of useful fragment ions to illustrate the steroid ring structure of drostanolone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was used to obtain structural details of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and a potential structure was proposed using a combined MS approach. Metabolite detection times were recorded and S4 (2α-methyl-5α-androstan-17-one-6β-ol-3α-sulfate) and G1 (2α-methyl-5α-androstan-17-one-3α-glucuronide) were thought to be new potential biomarkers for drostanolone misuse which can be detected up to 24days by liquid-liquid extraction and 7days by direct-injection analysis after intramuscular injection. S4 and G1 were also detected in two drostanolone-positive routine urine samples. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. Towards Surface Plasmon Resonance biosensing combined with bioaffinity-assisted nano HILIC Liquid Chromatography / Time-of-flight Mass Spectrometry identification of Paralytic Shellfish Poisons

    NARCIS (Netherlands)

    Marchesini, G.R.; Hooijerink, H.; Haasnoot, W.; Buijs, J.; Campbell, K.; Elliott, C.T.; Nielen, M.W.F.

    2009-01-01

    The potential for coupling technologies to deliver new, improved forms of bioanalysis is still in its infancy. We review a number of examples in which coupling has been successful, with special emphasis on combining surface-plasmon-resonance biosensors with mass spectrometry. We give an overview of

  4. Identification of pesticide transformation products in food by liquid chromatography/time-of-flight mass spectrometry via "fragmentation-degradation" relationships.

    Science.gov (United States)

    García-Reyes, Juan F; Molina-Díaz, Antonio; Fernandez-Alba, Amadeo R

    2007-01-01

    The identification of transformation products of pesticides in foodstuffs is a crucial task difficult to tackle, due to the lack of standards and scarce information available. In this work, we describe a methodology for the identification and structural elucidation of pesticide transformation products in food. The proposed strategy is based on the use of liquid chromatography electrospray time-of-flight mass spectrometry (LC/TOFMS): accurate mass measurements of (molecule and fragment) ions of interest are used in order to establish relationships between fragmentation of the parent pesticides in the instrument (in-source CID fragmentation) and possible degradation products of these pesticides in food. Examples of this strategy showing the potential of LC/TOFMS to determine unknown pesticides in food are described in two different real samples, suggesting that pesticides often are transformed into degradation products in the same fashion that they are fragmented in the instrument. Using the proposed approach and without using standards a priori, based solely on accurate mass measurements of ions and "fragmentation-degradation" relationships, we have identified two parent pesticides (amitraz and malathion) along with six degradation products, m/z 253 (N,N'-bisdimethylphenylformamidine), 163 (N-2,4-dimethylphenyl-N-methyl formamidine), 150 (2,4-dimethylformamidine), and 122 (2,4-dimethylaniline) from amitraz, and m/z 317 and 303, due to ether hydrolysis of methyl and ethyl groups from malathion. Structures for these species were proposed, and the potential of the proposed approach was critically discussed.

  5. Toward unraveling grape tannin composition: application of online hydrophilic interaction chromatography × reversed-phase liquid chromatography-time-of-flight mass spectrometry for grape seed analysis.

    Science.gov (United States)

    Kalili, Kathithileni M; Vestner, Jochen; Stander, Maria A; de Villiers, André

    2013-10-01

    Despite the significant importance of tannins in viticulture and enology, relatively little is known about the detailed chemical composition of these molecules. This is due to challenges associated with the accurate analytical determination of the highly structurally diverse proanthocyanidins which comprise tannins. In this contribution, we address this limitation by demonstrating how online comprehensive two-dimensional liquid chromatography (LC × LC) coupled to high resolution mass spectrometry (HR-MS) can be exploited as a powerful analytical approach for the detailed characterization of grape seed tannins. Hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RP-LC) were employed in the two dimensions to provide complementary information in terms of separation according to hydrophilicity and hydrophobicity, respectively. Online coupling of HILIC × RP-LC with fluorescence detection and electrospray ionization MS delivered high resolution analysis in a practical analysis time, while allowing selective detection and facilitating compound identification. Time-of-flight (TOF) MS provided high acquisition rates and sensitivity coupled to accurate mass information, which allowed detection of procyanidins up to a degree of polymerization (DP) of 16 and a degree of galloylation up to 8 in a red grape seed extract. This analytical methodology promises to shed new light on these important grape constituents and potentially on their evolution during wine production.

  6. Accelerated benzene polycarboxylic acid analysis by liquid chromatography-time-of-flight-mass spectrometry for the determination of petrogenic and pyrogenic carbon.

    Science.gov (United States)

    Hindersmann, Benjamin; Achten, Christine

    2017-08-11

    Pyrogenic carbon species are of particular interest due to their ubiquitous occurrence in the environment and their high sorption capacities for nonpolar organic compounds. It has recently been shown that the analysis of the molecular markers for complex aromatic carbon structures, benzene polycarboxylic acids (BPCA), has a high potential for aid in the identification of different carbon sources. In this study, the first LC method using mass spectrometry (MS) for reliable and accelerated (carbon by BPCA analysis has been developed. The main advantage of LC-MS compared to previous methods is the higher sensitivity, which is important if only small sample amounts are available. Sample pre-treatment could be reduced to a minimum. Deuterated phthalic acid was introduced as internal standard due to its structural similarity to BPCA and its lack of occurrence in the environment. Linear quantification with r 2 ≥0997 was accomplished for all BPCA. Method validation showed an excellent quantification reproducibility (mean CVcarbon, large amounts of petrogenic carbon species can also be present in urban soils and river sediments, especially in mining regions. They also to a large degree consist of aromatic carbon structures and therefore have an impact on source identification by BPCA analysis. Comparison of petrogenic and pyrogenic carbon samples shows similarities in the BPCA concentrations and patterns, in their aromaticity and degree of aromatic condensation. Thus, a differentiation between petrogenic and pyrogenic carbon only by BPCA analysis of samples with unknown carbon sources is not possible. For reliable source identification of the carbon species, the combination with other methods, such as e. g. analysis of polycyclic aromatic hydrocarbons may be successful. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Fingerprint analysis and quality consistency evaluation of flavonoid compounds for fermented Guava leaf by combining high-performance liquid chromatography time-of-flight electrospray ionization mass spectrometry and chemometric methods.

    Science.gov (United States)

    Wang, Lu; Tian, Xiaofei; Wei, Wenhao; Chen, Gong; Wu, Zhenqiang

    2016-10-01

    Guava leaves are used in traditional herbal teas as antidiabetic therapies. Flavonoids are the main active of Guava leaves and have many physiological functions. However, the flavonoid compositions and activities of Guava leaves could change due to microbial fermentation. A high-performance liquid chromatography time-of-flight electrospray ionization mass spectrometry method was applied to identify the varieties of the flavonoids in Guava leaves before and after fermentation. High-performance liquid chromatography, hierarchical cluster analysis and principal component analysis were used to quantitatively determine the changes in flavonoid compositions and evaluate the consistency and quality of Guava leaves. Monascus anka Saccharomyces cerevisiae fermented Guava leaves contained 2.32- and 4.06-fold more total flavonoids and quercetin, respectively, than natural Guava leaves. The flavonoid compounds of the natural Guava leaves had similarities ranging from 0.837 to 0.927. The flavonoid compounds from the Monascus anka S. cerevisiae fermented Guava leaves had similarities higher than 0.993. This indicated that the quality consistency of the fermented Guava leaves was better than that of the natural Guava leaves. High-performance liquid chromatography fingerprinting and chemometric analysis are promising methods for evaluating the degree of fermentation of Guava leaves based on quality consistency, which could be used in assessing flavonoid compounds for the production of fermented Guava leaves. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A fast and sensitive method for the simultaneous analysis of a wide range of per- and polyfluoroalkyl substances in indoor dust using on-line solid phase extraction-ultrahigh performance liquid chromatography-time-of-flight-mass spectrometry.

    Science.gov (United States)

    Padilla-Sánchez, Juan Antonio; Haug, Line Småstuen

    2016-05-06

    A fast and sensitive method for simultaneous determination of 18 traditional and 6 alternative per- and polyfluoroalkyl substances (PFASs) using solid-liquid extraction (SLE), off-line clean-up using activated carbon and on-line solid phase extraction-ultrahigh performance liquid chromatography-time-of-flight-mass spectrometry (on-line SPE-UHPLC-TOF-MS) was developed. The extraction efficiency was studied and recoveries in range the 58-114% were obtained. Extraction and injection volumes were also optimized to 2mL and 400μL, respectively. The method was validated by spiking dust from a vacuum cleaner bag that had been found to contain low levels of the PFASs in focus. Low method detection limits (MDLs) and method quantification limits (MQLs) in the range 0.008-0.846ngg(-1) and 0.027-2.820ngg(-1) were obtained, respectively. For most of the PFASs, the accuracies were between 70 and 125% in the range from 2 to100ngg(-1) dust. Intra-day and inter-day precisions were in general well below 30%. Analysis of a Standard Reference Material (SRM 2585) showed high accordance with results obtained by other laboratories. Finally, the method was applied to seven indoor dust samples, and PFAS concentrations in the range 0.02-132ngg(-1) were found. The highest median concentrations were observed for some of the alternative PFASs, such as 6:2-diPAP (25ngg(-1)), 8:2-diPAP (49ngg(-1)), and PFOPA (23ngg(-1)), illustrating the importance of inclusion of new PFASs in the analytical methods. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. 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.

  10. Screening and analysis of potential anti-tumor components from the stipe of Ganoderma sinense using high-performance liquid chromatography/time-of-flight mass spectrometry with multivariate statistical tool.

    Science.gov (United States)

    Chan, Kar-Man; Yue, Grace Gar-Lee; Li, Ping; Wong, Eric Chun-Wai; Lee, Julia Kin-Ming; Kennelly, Edward J; Lau, Clara Bik-San

    2017-03-03

    According to Chinese Pharmacopoeia 2015 edition, Ganoderma (Lingzhi) is a species complex that comprise of Ganoderma lucidum and Ganoderma sinense. The bioactivity and chemical composition of G. lucidium had been studied extensively, and it was shown to possess antitumor activities in pharmacological studies. In contrast, G. sinense has not been studied in great detail. Our previous studies found that the stipe of G. sinense exhibited more potent antitumor activity than the pileus. To identify the antitumor compounds in the stipe of G. sinense, we studied its chemical components by merging the bioactivity results with liquid chromatography-mass spectrometry-based chemometrics. The stipe of G. sinense was extracted with water, followed by ethanol precipitation and liquid-liquid partition. The resulting residue was fractionated using column chromatography. The antitumor activity of these fractions were analysed using MTT assay in murine breast tumor 4T1 cells, and their chemical components were studied using the LC-QTOF-MS with multivariate statistical tools. The chemometric and MS/MS analysis correlated bioactivity with five known cytotoxic compounds, 4-hyroxyphenylacetate, 9-oxo-(10E,12E)-octadecadienoic acid, 3-phenyl-2-propenoic acid, 13-oxo-(9E,11E)-octadecadienoic acid and lingzhine C, from the stipe of G. sinense. To the best of our knowledge, 4-hyroxyphenylacetate, 3-phenyl-2-propenoic acid and lingzhine C are firstly reported to be found in G. sinense. These five compounds will be investigated for their antitumor activities in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Non-target evaluation of contaminants in honey bees and pollen samples by gas chromatography time-of-flight mass spectrometry.

    Science.gov (United States)

    Hakme, E; Lozano, A; Gómez-Ramos, M M; Hernando, M D; Fernández-Alba, A R

    2017-10-01

    This work presents a non-targeted screening approach for the detection and quantitation of contaminants in bees and pollen, collected from the same hive, by GC-EI-ToF-MS. It consists of a spectral library datasets search using a compound database followed by a manual investigation and analytical standard confirmation together with semi-quantitation purposes. Over 20% of the compounds found automatically by the library search could not be confirmed manually. This number of false positive detections was mainly a consequence of an inadequate ion ratio criterion (±30%), not considered in the automatic searching procedure. Eight compounds were detected in bees and pollen. They include insecticides/acaricides (chlorpyrifos, coumaphos, fluvalinate-tau, chlorfenvinphos, pyridaben, and propyl cresol) at a concentration range of 1-1207 μg kg -1 , herbicides (oxyfluorfen) at a concentration range of 212-1773 μg kg -1 and a growth regulator hormone (methoprene). Some compounds were detected only in pollen; such as herbicides (clomazone), insecticides/acaricides and fungicides used to control Varroa mites as benzylbenzoate, bufencarb, allethrin, permethrin, eugenol and cyprodinil. Additional compounds were detected only in bees: flamprop-methyl, 2-methylphenol (2-49 μg kg -1 ) and naphthalene (1-23 μg kg -1 ). The proposed method presents important advantages as it can avoid the use of an unachievable number of analytical standards considered target compounds "a priori" but not present in the analyzed samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Investigation of the Antifatigue Effects of Korean Ginseng on Professional Athletes by Gas Chromatography-Time-of-Flight-Mass Spectrometry-Based Metabolomics.

    Science.gov (United States)

    Yan, Bei; Liu, Yao; Shi, Aixin; Wang, Zhihong; Aa, Jiye; Huang, Xiaoping; Liu, Yi

    2017-09-19

    Ginseng is usually used for alleviating fatigue. The purpose of this paper was to evaluate the regulatory effect of Korean ginseng on the metabolic pattern in professional athletes, and, further, to explore the underlying mechanism of the antifatigue effect of Korean ginseng. GC-time-of-flight-MS was used to profile serum samples from professional athletes before training and after 15 and 30 day training, and professional athletes administered with Korean ginseng in the meanwhile. Biochemical parameters of all athletes were also analyzed. For the athlete control group, strength–endurance training resulted in an elevation of creatine kinase (CK) and blood urea nitrogen (BUN), and a reduction in blood hemoglobin, and a dynamic trajectory of the metabolomic profile which were related to fatigue. Korean ginseng treatment not only lead to a marked reduction in CK and blood urea nitrogen (BUN) in serum, but also showed regulatory effects on the serum metabolic profile and restored scores plots close to normal, suggesting that the change in metabolic profiling could reflect the antifatigue effect of Korean ginseng. Furthermore, perturbed levels of 11 endogenous metabolites were regulated by Korean ginseng significantly, which might be primarily involved in lipid metabolism, energy balance, and chemical signaling. These findings suggest that metabolomics is a potential tool for the evaluation of the antifatigue effect of Korean ginseng and for the elucidation of its pharmacological mechanism.

  13. Qualitative analyses of less-volatile organic molecules from female skin scents by comprehensive two dimensional gas chromatography-time of flight mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Doležal, P.; Kyjaková, Pavlína; Valterová, Irena; Urban, Š.

    2017-01-01

    Roč. 1505, Jul 7 (2017), s. 77-86 ISSN 0021-9673. [International Symposium on Capillary Chromatography /40./ and GCxGC Symposium /13./. Riva del Garda, 29.05.2016-03.06.2016] Institutional support: RVO:61388963 Keywords : human scent analysis * molecular composition of human scent * forensic chemistry * human scent signature * GCxGC-TOFMS Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.981, year: 2016

  14. Extraction Methodological Contributions Toward Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry: Quantification of Free GB from Various Food Matrices

    Science.gov (United States)

    2016-02-01

    Validation for Determination of 128 Pesticides in Bananas by Modified QuEChERS and UHPLC–MS/MS Analysis. Food Control 2013, 33, 413–423. 23. Sinha...30. Kolakowski, B.M.; DʼAgostino, P.A.; Chenier, C.; Mester, Z. Analysis of Chemical Warfare Agents in Food Products by Atmospheric Pressure...SPECTROMETRY: QUANTIFICATION OF FREE GB FROM VARIOUS FOOD MATRICES ECBC-TR-1351 Sue Y. Bae Mark D. Winemiller RESEARCH AND TECHNOLOGY DIRECTORATE

  15. Quantification of VX Nerve Agent in Various Food Matrices by Solid-Phase Extraction Ultra-Performance Liquid ChromatographyTime-of-Flight Mass Spectrometry

    Science.gov (United States)

    2016-04-01

    Validation for Determination of 128 Pesticides in Bananas by Modified QuEChERS and UHPLC–MS/MS Analysis. Food Control 2013, 33, 413–423. 23. Sinha, S.N...213. 30. Kolakowski, B.M.; DʼAgostino, P.A.; Chenier, C.; Mester, Z. Analysis of Chemical Warfare Agents in Food Products by Atmospheric Pressure...QUANTIFICATION OF VX NERVE AGENT IN VARIOUS FOOD MATRICES BY SOLID-PHASE EXTRACTION ULTRA-PERFORMANCE

  16. Generic sample preparation combined with high-resolution liquid chromatography- time-of-flight mass spectrometry for unification of urine screening in doping-control laboratories

    NARCIS (Netherlands)

    Peters, R.J.B.; Oosterink, J.E.; Stolker, A.A.M.; Georgakopoulos, C.G.; Nielen, M.W.F.

    2010-01-01

    A unification of doping-control screening procedures of prohibited small molecule substances—including stimulants, narcotics, steroids, ß2-agonists and diuretics—is highly urgent in order to free resources for new classes such as banned proteins. Conceptually this may be achieved by the use of a

  17. Investigating the causes of low detectability of pesticides in fruits and vegetables analysed by high-performance liquid chromatography - Time-of-flight.

    Science.gov (United States)

    Muehlwald, S; Buchner, N; Kroh, L W

    2018-03-23

    Because of the high number of possible pesticide residues and their chemical complexity, it is necessary to develop methods which cover a broad range of pesticides. In this work, a qualitative multi-screening method for pesticides was developed by use of HPLC-ESI-Q-TOF. 110 pesticides were chosen for the creation of a personal compound database and library (PCDL). The MassHunter Qualitative Analysis software from Agilent Technologies was used to identify the analytes. The software parameter settings were optimised to produce a low number of false positive as well as false negative results. The method was validated for 78 selected pesticides. However, the validation criteria were not fulfilled for 45 analytes. Due to this result, investigations were started to elucidate reasons for the low detectability. It could be demonstrated that the three main causes of the signal suppression were the co-eluting matrix (matrix effect), the low sensitivity of the analyte in standard solution and the fragmentation of the analyte in the ion source (in-source collision-induced dissociation). In this paper different examples are discussed showing that the impact of these three causes is different for each analyte. For example, it is possible that an analyte with low signal intensity and an intense fragmentation in the ion source is detectable in a difficult matrix, whereas an analyte with a high sensitivity and a low fragmentation is not detectable in a simple matrix. Additionally, it could be shown that in-source fragments are a helpful tool for an unambiguous identification. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. An empirical Bayes model using a competition score for metabolite identification in gas chromatography mass spectrometry

    Directory of Open Access Journals (Sweden)

    Kim Seongho

    2011-10-01

    Full Text Available Abstract Background Mass spectrometry (MS based metabolite profiling has been increasingly popular for scientific and biomedical studies, primarily due to recent technological development such as comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GCxGC/TOF-MS. Nevertheless, the identifications of metabolites from complex samples are subject to errors. Statistical/computational approaches to improve the accuracy of the identifications and false positive estimate are in great need. We propose an empirical Bayes model which accounts for a competing score in addition to the similarity score to tackle this problem. The competition score characterizes the propensity of a candidate metabolite of being matched to some spectrum based on the metabolite's similarity score with other spectra in the library searched against. The competition score allows the model to properly assess the evidence on the presence/absence status of a metabolite based on whether or not the metabolite is matched to some sample spectrum. Results With a mixture of metabolite standards, we demonstrated that our method has better identification accuracy than other four existing methods. Moreover, our method has reliable false discovery rate estimate. We also applied our method to the data collected from the plasma of a rat and identified some metabolites from the plasma under the control of false discovery rate. Conclusions We developed an empirical Bayes model for metabolite identification and validated the method through a mixture of metabolite standards and rat plasma. The results show that our hierarchical model improves identification accuracy as compared with methods that do not structurally model the involved variables. The improvement in identification accuracy is likely to facilitate downstream analysis such as peak alignment and biomarker identification. Raw data and result matrices can be found at http

  19. Screening for anabolic steroids and related compounds in illegal cocktails by liquid chromatography/time-of-flight mass spectrometry and liquid chromatography/quadrupole time-of-flight tandem mass spectrometry with accurate mass measurement

    NARCIS (Netherlands)

    Nielen, M.W.F.; Vissers, J.P.C.; Fuchs, R.E.M.; Velde, van J.W.; Lommen, A.

    2001-01-01

    Findings of illegal hormone preparations such as syringes, bottles, cocktails, and so on, are an important information source for the nature of the current abuse of anabolic steroids and related compounds as growth-promoting agents in cattle. A new screening method for steroids in cocktails is

  20. Gas chromatography: mass selective detector

    International Nuclear Information System (INIS)

    Lapinskas, R.

    1988-01-01

    The mechanism of mass spectrometry technique directed for detecting molecular structures is described, with some considerations about its operational features. This mass spectrometer is used as a gas chromatography detector. (author)

  1. Global metabolomic profiling of human serum from obese individuals by liquid chromatography-time-of-flight/mass spectrometry to evaluate the intake of breakfasts prepared with heated edible oils.

    Science.gov (United States)

    Ferreiro-Vera, Carlos; Priego-Capote, Feliciano; Calderón-Santiago, Mónica; Luque de Castro, María D

    2013-12-01

    The metabolic profile of human serum after intake of breakfasts prepared with different heated vegetable oils has been studied. Four oils (olive and sunflower oils, pure and enriched with natural and artificial oxidation inhibitors) were subjected to a simulated heated process prior to breakfast preparation. A metabolomics global profiling approach performed on post-basal serum samples revealed statistical differences among individuals based on breakfast intake, and identified compounds responsible for such differences. Serum samples obtained in basal state (control samples) and 2 and 4h after programmed intakes were analyzed by LC-TOF/MS. The resulting fingerprints were compared and differences between basal and post-basal states evaluated, observing that the intake of different breakfasts altered the metabolic signature of serum. Analysis models based on PLS algorithms were developed to discriminate individuals in post-basal state for each intervention breakfast. Then, Volcano tests enabled to detect significant molecular entities explaining the variability associated to each breakfast. It is worth emphasizing the importance of fatty acids, their derivatives and phospholipids for tentative identification. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Method for analysis of psychopharmaceuticals in real industrial wastewater and groundwater with suspended organic particulate matter using solid phase extraction disks extraction and ultra-high performance liquid chromatography/time-of-flight mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Křesinová, Zdena; Linhartová, Lucie; Petrů, Klára; Krejčová, L.; Šrédlová, Kamila; Lhotský, O.; Kameník, Zdeněk; Cajthaml, Tomáš

    2016-01-01

    Roč. 1440, APR 1 (2016), s. 15-22 ISSN 0021-9673 R&D Projects: GA TA ČR TE01020218 Institutional support: RVO:61388971 Keywords : Pharmaceuticals * SPE disks * Whole-water Subject RIV: EE - Microbiology, Virology Impact factor: 3.981, year: 2016

  3. Extraction and Analysis of V-Type Agents (VX, RVX, CVX, and VM) from Various Food Matrices by Ultra-Performance Liquid Chromatography-Time-Of-Flight Mass Spectrometry

    Science.gov (United States)

    2015-12-01

    nuggets, and turkey deli meat (99% fat free). The total percent recoveries (and percent relative standard deviations) for VX, RVX, CVX, and VM in...Egg Whites and Tomato Sauce .....................................................3 2.3.3 Group 3: Hot Dogs, Chicken Nuggets, Turkey Deli Meat ...Apple juice, orange juice, whole milk, 2% reduced fat milk, Egg Beaters processed egg whites, tomato sauce, precooked turkey deli meat (99% fat free

  4. Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine.

    Science.gov (United States)

    Perestrelo, Rosa; Petronilho, Sílvia; Câmara, José S; Rocha, Sílvia M

    2010-05-14

    An analytical methodology based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC x GC-ToFMS) was developed for the identification and quantification of the toxic contaminant ethyl carbamate (EC) directly in fortified wines. The method performance was assessed for dry/medium dry and sweet/medium sweet model wines, and for quantification purposes, calibration plots were performed for both matrices using the ion extraction chromatography (IEC) mode (m/z 62). Good linearity was obtained with a regression coefficient (r(2)) higher than 0.981. A good precision was attained (R.S.D. wines. The quantification limits (LOQ) and recovery for dry wines were 14.38 microg/L and 88.6%, whereas for sweet wines were 9.16 microg/L and 99.4%, respectively. The higher performance was attained with sweet model wine, as increasing of glucose content improves the volatile compound in headspace, and a better linearity, recovery and precision were achieved. The analytical methodology was applied to analyse 20 fortified Madeira wines including different types of wine (dry, medium dry, sweet, and medium sweet) obtained from several harvests in Madeira Island (Portugal). The EC levels ranged from 54.1 microg/L (medium dry) to 162.5 microg/L (medium sweet). 2010 Elsevier B.V. All rights reserved.

  5. Impurity profiling of a chemical weapon precursor for possible forensic signatures by comprehensive two-dimensional gas chromatography/mass spectrometry and chemometrics.

    Science.gov (United States)

    Hoggard, Jamin C; Wahl, Jon H; Synovec, Robert E; Mong, Gary M; Fraga, Carlos G

    2010-01-15

    In this report we present the feasibility of using analytical and chemometric methodologies to reveal and exploit the chemical impurity profiles from commercial dimethyl methylphosphonate (DMMP) samples to illustrate the type of forensic information that may be obtained from chemical-attack evidence. Using DMMP as a model compound of a toxicant that may be used in a chemical attack, we used comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GC x GC/TOF-MS) to detect and identify trace organic impurities in six samples of commercially acquired DMMP. The GC x GC/TOF-MS data was analyzed to produce impurity profiles for all six DMMP samples using 29 analyte impurities. The use of PARAFAC for the mathematical resolution of overlapped GC x GC peaks ensured clean spectra for the identification of many of the detected analytes by spectral library matching. The use of statistical pairwise comparison revealed that there were trace impurities that were quantitatively similar and different among five of the six DMMP samples. Two of the DMMP samples were revealed to have identical impurity profiles by this approach. The use of nonnegative matrix factorization indicated that there were five distinct DMMP sample types as illustrated by the clustering of the multiple DMMP analyses into five distinct clusters in the scores plots. The two indistinguishable DMMP samples were confirmed by their chemical supplier to be from the same bulk source. Sample information from the other chemical suppliers supported the idea that the other four DMMP samples were likely from different bulk sources. These results demonstrate that the matching of synthesized products from the same source is possible using impurity profiling. In addition, the identified impurities common to all six DMMP samples provide strong evidence that basic route information can be obtained from impurity profiles. Finally, impurities that may be unique to the sole bulk manufacturer of DMMP were

  6. Preventive doping control screening analysis of prohibited substances in human urine using rapid-resolution liquid chromatography/high-resolution time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Vonaparti, A.; Lyris, E.; Angelis, Y.S.; Panderi, I.; Koupparis, M.; Tsantili- Kakoulidou, A.; Peters, R.J.B.; Nielen, M.W.F.; Georgakopoulos, C.G.

    2010-01-01

    Unification of the screening protocols for a wide range of doping agents has become an important issue for doping control laboratories. This study presents the development and validation of a generic liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) screening method of 241 small

  7. Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee

    International Nuclear Information System (INIS)

    Risticevic, Sanja; Carasek, Eduardo; Pawliszyn, Janusz

    2008-01-01

    Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 deg. C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 μm metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C 8 -C 40 alkanes and the mass spectral library search was utilized for the

  8. Portable gas chromatograph-mass spectrometer

    Science.gov (United States)

    Andresen, B.D.; Eckels, J.D.; Kimmons, J.F.; Myers, D.W.

    1996-06-11

    A gas chromatograph-mass spectrometer (GC-MS) is described for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units. 4 figs.

  9. Comprehensive two-dimensional liquid chromatography–time-of-flight mass spectrometry in the analysis of acidic compounds in atmospheric aerosols

    Czech Academy of Sciences Publication Activity Database

    Pól, Jaroslav; Hohnová, B.; Jussila, M.; Hyötyläinen, T.

    2006-01-01

    Roč. 1130, č. 1 (2006), s. 64-71 ISSN 0021-9673. [International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers /9./. York, 08.02.2006-10.02.2006] Institutional research plan: CEZ:AV0Z40310501 Keywords : comprehensive two-dimensional liquid chromatography * time-of-flight mass spectrometry * atmospheric aerosol analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.554, year: 2006

  10. Identification of organic xenobiotics in urban aquatic environments using time-of-flight mass spectrometry.

    Science.gov (United States)

    Jernberg, Joonas; Pellinen, Jukka; Rantalainen, Anna-Lea

    2013-04-15

    Qualitative non-target and post-target analysis methods using gas chromatography-time-of-flight mass spectrometry were applied for analysing neutral and acidic organic xenobiotics in urban and suburban water samples. Ten water samples representing wastewater, stormwater and surface water matrices were collected and concentrated using solid phase extraction. Compound identification was performed using a spectral deconvolution program, accurate mass measurements and comparisons with library spectra. The non-target and post-target analyses identified 36 and 18 compounds, respectively. The identification of 10 compounds was afterwards confirmed with standard compounds. Organophosphate esters were the most abundant compound group detected. The combination of non-target and post-target analyses proved a useful tool in the tentative identification of xenobiotics in water samples. Post-target analysis can complement non-target analysis results at low analyte concentrations. Results showed that several organic xenobiotics originate in urban areas and accumulate in the environment. The wastewater sample produced the highest number of identified compounds, but most of these compounds were also found in stormwater samples from the city centre. Nearly all the compounds present in wastewater were additionally detected in the surface water sample taken 3 km downstream from the wastewater effluent discharge point. Only a few xenobiotics were otherwise detected in the surface water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Mass transfer in gas-liquid slurry reactors

    NARCIS (Netherlands)

    Beenackers, A.A.C.M.; van Swaaij, Willibrordus Petrus Maria

    1993-01-01

    A critical review is presented on the mass transfer characteristics of gas¿liquid slurry reactors. The recent findings on the influence of the presence of solid particles on the following mass transfer parameters in slurry reactors are discussed: volumetric gas¿liquid mass transfer coefficients

  12. Forensic profiling of sassafras oils based on comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Schäffer, M; Gröger, T; Pütz, M; Zimmermann, R

    2013-06-10

    Safrole, the main compound in the essential oil of several plants of the Laurel family (Lauraceae), and its secondary product piperonylmethylketone are the predominantly used precursors for the illicit synthesis of 3,4-methylenedioxymethamphetamine (MDMA) which is, in turn, the most common active ingredient in Ecstasy tablets. Analytical methods with adequate capacity to identify links and origin of precursors, such as safrole, provide valuable information for drug-related police intelligence. Authentic sassafras oil samples from police seizures were subjected to comparative analysis based on their chemical profiles obtained by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS). The enhanced separation power and increased sensitivity of GC × GC allowed for the detection of minor compounds present in the essential oils which were of particular interest in case of very pure samples whose impurity profiles were not very pronounced. Discrimination of such samples was still possible even in the absence of characteristic main compounds. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  13. Study on the calculating the second dimension retention index in comprehensive two-dimensional gas chromatography spectrometry

    International Nuclear Information System (INIS)

    Zhao Yaping; Zhang Jun; Wang Bing; Fang Aiqin; Zhang Xiang; Kim, Seong Ho; Bogdanov, Bogdan; McClain, Craig

    2012-01-01

    A method was developed to calculate the second dimension retention index of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC/TOF MS) data using n-alkanes as reference compounds. The retention times of the C 7 -C 31 alkanes acquired during 24 isothermal experiments cover the 0-6 s retention time area in the second dimension retention time space, which makes it possible to calculate the retention indices of target compounds from the corresponding retention time values without the extension of the retention space of the reference compounds. An empirical function was proposed to show the relationship among the second dimension retention time. the temperature of the second dimension column, and the carbon number of the n-alkanes. The proposed function is able to extend the second dimension retention time beyond the reference n-alkanes by increasing the carbon number. The extension of carbon numbers in reference n-alkanes up to two more carbon atoms introduces less than 10 retention index units (iu) of deviation. The effectiveness of using the proposed method was demonstrated by analyzing a mixture of compound standards in temperature programmed experiments using 6 different initial column temperatures. The standard deviation of the calculated retention index values of the compound standards fluctuated from 1 to 12 iu with a mean standard deviation of 5 iu. (authors)

  14. Comprehensive two-dimensional gas chromatographic profiling and chemometric interpretation of the volatile profiles of sweat in knit fabrics.

    Science.gov (United States)

    de la Mata, A Paulina; McQueen, Rachel H; Nam, Seo Lin; Harynuk, James J

    2017-03-01

    Human axillary sweat is a poorly explored biofluid within the context of metabolomics when compared to other fluids such as blood and urine. In this paper, we explore the volatile organic compounds emitted from two different types of fabric samples (cotton and polyester) which had been worn repeatedly during exercise by participants. Headspace solid-phase microextraction (SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) were employed to profile the (semi)volatile compounds on the fabric. Principal component analysis models were applied to the data to aid in visualizing differences between types of fabrics, wash treatment, and the gender of the subject who had worn the fabric. Statistical tools included with commercial chromatography software (ChromaTOF) and a simple Fisher ratio threshold-based feature selection for model optimization are compared with a custom-written algorithm that uses cluster resolution as an objective function to maximize in a hybrid backward-elimination forward-selection approach for optimizing the chemometric models in an effort to identify some compounds that correlate to differences between fabric types. The custom algorithm is shown to generate better models than the simple Fisher ratio approach. Graphical Abstract A route from samples and questions to data and then answers.

  15. Analysis of sulphur compounds in underground reservoirs of natural gas and town gas by gas chromatography and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Triska, J.; Kuras, M.; Zachar, P.; Vodicka, L. (Institute of Chemical Technology, Prague (Czechoslovakia). Lab. of Synthetic Fuels)

    1990-09-01

    This paper deals with mass spectrometry and gas chromatography of the sulphur compounds in waste waters from the natural gas underground reservoirs, in extracts of activated charcoal used for purification of town gas, and in the oils from compressors of natural gas. (orig.).

  16. MAVEN Neutral Gas and Ion Mass Spectrometer Data

    Data.gov (United States)

    National Aeronautics and Space Administration — This bundle contains the data collected by the Neutral Gas and Ion Mass Spectrometer (NGIMS) instrument aboard the Mars Atmosphere and Volatile EvolutioN (MAVEN)...

  17. Microbial metabolomics with gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Koek, M.M.; Muilwijk, B.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    An analytical method was set up suitable for the analysis of microbial metabolomes, consisting of an oximation and silylation derivatization reaction and subsequent analysis by gas chromatography coupled to mass spectrometry. Microbial matrixes contain many compounds that potentially interfere with

  18. Prediction of Mass Flow Rate in Supersonic Natural Gas Processing

    Directory of Open Access Journals (Sweden)

    Wen Chuang

    2015-11-01

    Full Text Available The mass flow rate of natural gas through the supersonic separator was numerically calculated by various cubic equations of state. The numerical results show that the compressibility factor and specific heat ratio for ideal gas law diverge remarkably from real gas models at a high inlet pressure. Simultaneously, the deviation of mass flow calculated by the ideal and real gas models reaches over 10 %. The difference increases with the lower of the inlet temperature regardless of the inlet pressure. A higher back pressure results in an earlier location of the shock wave. The pressure ratio of 0.72 is the first threshold to get the separator work normally. The second threshold is 0.95, in which case the whole flow is subsonic and cannot reach the choked state. The shock position moves upstream with the real gas model compared to the ideal gas law in the cyclonic separation section.

  19. Pyrolysis - gas chromatography - mass spectrometry of lignins

    Energy Technology Data Exchange (ETDEWEB)

    Martin, F.; Saiz-Jimenez, C.; Gonzalez-Vila, F.J.

    1979-01-01

    Milled wood lignins from spruce, beech and bamboo were pyrolysed. The high-boiling products of pyrolysis were studied by GLC and mass spectrometry. The forty-three products identified provide information on the structural units of lignin.

  20. The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

    Science.gov (United States)

    Pfennig, Brian W.; Schaefer, Amy K.

    2011-01-01

    A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

  1. Isotopic mass-dependence of noble gas diffusion coefficients inwater

    Energy Technology Data Exchange (ETDEWEB)

    Bourg, I.C.; Sposito, G.

    2007-06-25

    Noble gas isotopes are used extensively as tracers inhydrologic and paleoclimatic studies. These applications requireknowledge of the isotopic mass (m) dependence of noble gas diffusioncoefficients in water (D), which has not been measured but is estimatedusing experimental D-values for the major isotopes along with an untestedrelationship from kinetic theory, D prop m-0.5. We applied moleculardynamics methods to determine the mass dependence of D for four noblegases at 298 K, finding that D prop m-beta with beta<0.2, whichrefutes the kinetic theory model underlying all currentapplications.

  2. Thermogravimetry-evolved gas analysis–mass spectrometry system ...

    Indian Academy of Sciences (India)

    Unknown

    ried out to optimize the interface conditions and to obtain ideal operating parameters to achieve best possible results with minimum time delay, better resolution and sensiti- vity (Kaisersberger and Post 1997). The operating para- meters like heating rate, sample mass and carrier flow gas were systematically varied to study ...

  3. Gas Chromatographic-Mass Spectrometric Analysis of Essential Oil ...

    African Journals Online (AJOL)

    Purpose: To analyze the essential oil composition of the flower of Jasminum officinale L. var. grandifloroum L. (Jasminum grandiflorum) by gas chromatography-mass spectrometry (GC-MS). Methods: The optimum GC-MS conditions used for the analysis were 250 oC inlet temperature, 150 oC MSD detector temperature, ...

  4. Analysis of essential oils by gas chromatography and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Masada, Y.

    1976-01-01

    The book is in two parts: first part Essential Oil includes compositae; labiatae; verbenaceae; oleaceae; umbelliferae; myrtaceae; euphorbiaceae; rutaceae; geraniaceae; rosaceae; lauraceae; myristicaceae; anonaceae; santalaceae; moraceae; piperaceae; zingiberaceae; araceae; gramineae; and cupressaceae written in English and Japanese. Part two includes essential oil; gas chromatography, and mass spectrometry written in Japanese. (DP)

  5. Gas chromatography mass spectrometry : key technology in metabolomics

    NARCIS (Netherlands)

    Koek, Maud Marijtje

    2009-01-01

    Metabolomics involves the unbiased quantitative and qualitative analysis of the complete set of metabolites present in cells, body fluids and tissues. Gas chromatography coupled to mass spectrometry (GC-MS) is very suitable for metabolomics analysis, as it combines high separation power with

  6. Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

    African Journals Online (AJOL)

    Prof. Ogunji

    Key words: Quassia undulata, GC MS, Biodiesel, Gbur, seed oil, Gas Chromatography, Mass. Spectrometry. Correspondence: waneniko@yahoo.co.uk ... these triglycerides and their applications depend on the fatty acid constituents .... injector temperature of 250°C and ion source temperature of 200°C and a split ratio of ...

  7. Gas-liquid mass transfer coefficient in stirred tank reactors

    NARCIS (Netherlands)

    Yawalkar, Archis A.; Heesink, Albertus B.M.; Versteeg, Geert; Pangarkar, Vishwas G.

    2003-01-01

    Volumetric gas—liquid mass transfer coefficient (kLa) data available in the literature for larger tanks (T = 0.39 m to 2.7 m) have been analyzed on the basis of relative dispersion parameter, N/Ncd. It was observed that at a given superficial gas velocity (VG), kLa values were approximately the same

  8. Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

    African Journals Online (AJOL)

    chromatography (GC) and gas chromaotography-mass spectrometry (GC-MS). The nematicidal activity of the essential oil and its major constituents was determined against second stage juveniles of H. avenae. Results: A total of 33 components of the essential oil were identified. The major constituents were bornyl acetate ...

  9. Specialized Gas Chromatography--Mass Spectrometry Systems for Clinical Chemistry.

    Science.gov (United States)

    Gochman, Nathan; And Others

    1979-01-01

    A discussion of the basic design and characteristics of gas chromatography-mass spectrometry systems used in clinical chemistry. A comparison of three specific systems: the Vitek Olfax IIA, Hewlett-Packard HP5992, and Du Pont DP-102 are included. (BB)

  10. Fluid dynamics and mass transfer in a gas centrifuge

    International Nuclear Information System (INIS)

    Conlisk, A.T.; Foster, M.R.; Walker, J.D.A.

    1982-01-01

    The fluid motion, temperature distribution and the mass-transfer problem of a binary gas mixture in a rapidly rotating centrifuge are investigated. Solutions for the velocity, temperature and mass-fraction fields within the centrifuge are obtained for mechanically or thermally driven centrifuges. For the mass-transfer problem, a detailed analysis of the fluid-mechanical boundary layers is required, and, in particular, mass fluxes within the boundary layers are obtained for a wide range of source-sink geometries. Solutions to the mass-transfer problem are obtained for moderately and strongly forced flows in the container; the dependence of the separation (or enrichment) factor on centrifuge configuration, rotational speed and fraction of the volumetric flow rate extracted at the product port (the cut) are predicted. (author)

  11. Catalytic Upgrading of Biomass Pyrolysis Oxygenates with Vacuum Gas Oil Using a Davison Circulating Riser Reactor

    Energy Technology Data Exchange (ETDEWEB)

    Jarvis, Mark W. [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Olstad, Jessica [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Parent, Yves [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Deutch, Steve [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Iisa, Kristiina [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Christensen, Earl [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Ben, Haoxi [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Black, Stuart [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Nimlos, Mark [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States; Magrini, Kim [National Bioenergy Center, National Renewable Energy Laboratory, 15523 Denver West Parkway, Golden, Colorado 80401, United States

    2018-01-22

    We investigate and quantitate the changes in hydrocarbon product composition while evaluating the performance and operability of the National Renewable Energy Laboratory's Davison Circulating Riser (DCR) reactor system when biomass model compounds are cofed with traditional fluid catalyst cracking (FCC) feeds and catalyst: vacuum gas oil (VGO) and equilibrium zeolite catalyst (E-Cat). Three compounds (acetic acid, guaiacol, and sorbitan monooleate) were selected to represent the major classes of oxygenates present in biomass pyrolysis vapors. These vapors can contain 30-50% oxygen as oxygenates, which create conversion complications (increased reactivity and coking) when integrating biomass vapors and liquids into fuel and chemical processes long dominated by petroleum feedstocks. We used these model compounds to determine the appropriate conditions for coprocessing with petroleum and ultimately pure pyrolysis vapors only as compared with standard baseline conditions obtained with VGO and E-Cat only in the DCR. Model compound addition decreased the DCR catalyst circulation rate, which controls reactor temperature and measures reaction heat demand, while increasing catalyst coking rates. Liquid product analyses included 2-dimensional gas chromatography time-of-flight mass spectroscopy (2D GCxGC TOFS), simulated distillation (SIM DIST), 13C NMR, and carbonyl content. Aggregated results indicated that the model compounds were converted during reaction, and despite functional group differences, product distributions for each model compound were very similar. In addition, we determined that adding model compounds to the VGO feed did not significantly affect the DCR's operability or performance. Future work will assess catalytic upgrading of biomass pyrolysis vapor to fungible hydrocarbon products using upgrading catalysts currently being developed at NREL and at Johnson Matthey.

  12. Chemical discrimination in turbulent gas mixtures with MOX sensors validated by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fonollosa, Jordi; Rodríguez-Luján, Irene; Trincavelli, Marco; Vergara, Alexander; Huerta, Ramón

    2014-10-16

    Chemical detection systems based on chemo-resistive sensors usually include a gas chamber to control the sample air flow and to minimize turbulence. However, such a kind of experimental setup does not reproduce the gas concentration fluctuations observed in natural environments and destroys the spatio-temporal information contained in gas plumes. Aiming at reproducing more realistic environments, we utilize a wind tunnel with two independent gas sources that get naturally mixed along a turbulent flow. For the first time, chemo-resistive gas sensors are exposed to dynamic gas mixtures generated with several concentration levels at the sources. Moreover, the ground truth of gas concentrations at the sensor location was estimated by means of gas chromatography-mass spectrometry. We used a support vector machine as a tool to show that chemo-resistive transduction can be utilized to reliably identify chemical components in dynamic turbulent mixtures, as long as sufficient gas concentration coverage is used. We show that in open sampling systems, training the classifiers only on high concentrations of gases produces less effective classification and that it is important to calibrate the classification method with data at low gas concentrations to achieve optimal performance.

  13. Discovery of safety biomarkers for atorvastatin in rat urine using mass spectrometry based metabolomics combined with global and targeted approach

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Bhowmik Salil [Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology, P.O. Box 131, Cheongryang, Seoul 130-650 (Korea, Republic of); University of Science and Technology, (305-333) 113 Gwahangno, Yuseong-gu, Daejeon (Korea, Republic of); Lee, Young-Joo; Yi, Hong Jae [College of Pharmacy, Kyung Hee University, Hoegi-dong, Dongdaemun-gu, Seoul 130-791 (Korea, Republic of); Chung, Bong Chul [Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology, P.O. Box 131, Cheongryang, Seoul 130-650 (Korea, Republic of); Jung, Byung Hwa, E-mail: jbhluck@kist.re.kr [Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology, P.O. Box 131, Cheongryang, Seoul 130-650 (Korea, Republic of); University of Science and Technology, (305-333) 113 Gwahangno, Yuseong-gu, Daejeon (Korea, Republic of)

    2010-02-19

    In order to develop a safety biomarker for atorvastatin, this drug was orally administrated to hyperlipidemic rats, and a metabolomic study was performed. Atorvastatin was given in doses of either 70 mg kg{sup -1} day{sup -1} or 250 mg kg{sup -1} day{sup -1} for a period of 7 days (n = 4 for each group). To evaluate any abnormal effects of the drug, physiological and plasma biochemical parameters were measured and histopathological tests were carried out. Safety biomarkers were derived by comparing these parameters and using both global and targeted metabolic profiling. Global metabolic profiling was performed using liquid chromatography/time of flight/mass spectrometry (LC/TOF/MS) with multivariate data analysis. Several safety biomarker candidates that included various steroids and amino acids were discovered as a result of global metabolic profiling, and they were also confirmed by targeted metabolic profiling using gas chromatography/mass spectrometry (GC/MS) and capillary electrophoresis/mass spectrometry (CE/MS). Serum biochemical and histopathological tests were used to detect abnormal drug reactions in the liver after repeating oral administration of atorvastatin. The metabolic differences between control and the drug-treated groups were compared using PLS-DA score plots. These results were compared with the physiological and plasma biochemical parameters and the results of a histopathological test. Estrone, cortisone, proline, cystine, 3-ureidopropionic acid and histidine were proposed as potential safety biomarkers related with the liver toxicity of atorvastatin. These results indicate that the combined application of global and targeted metabolic profiling could be a useful tool for the discovery of drug safety biomarkers.

  14. Discovery of safety biomarkers for atorvastatin in rat urine using mass spectrometry based metabolomics combined with global and targeted approach

    International Nuclear Information System (INIS)

    Kumar, Bhowmik Salil; Lee, Young-Joo; Yi, Hong Jae; Chung, Bong Chul; Jung, Byung Hwa

    2010-01-01

    In order to develop a safety biomarker for atorvastatin, this drug was orally administrated to hyperlipidemic rats, and a metabolomic study was performed. Atorvastatin was given in doses of either 70 mg kg -1 day -1 or 250 mg kg -1 day -1 for a period of 7 days (n = 4 for each group). To evaluate any abnormal effects of the drug, physiological and plasma biochemical parameters were measured and histopathological tests were carried out. Safety biomarkers were derived by comparing these parameters and using both global and targeted metabolic profiling. Global metabolic profiling was performed using liquid chromatography/time of flight/mass spectrometry (LC/TOF/MS) with multivariate data analysis. Several safety biomarker candidates that included various steroids and amino acids were discovered as a result of global metabolic profiling, and they were also confirmed by targeted metabolic profiling using gas chromatography/mass spectrometry (GC/MS) and capillary electrophoresis/mass spectrometry (CE/MS). Serum biochemical and histopathological tests were used to detect abnormal drug reactions in the liver after repeating oral administration of atorvastatin. The metabolic differences between control and the drug-treated groups were compared using PLS-DA score plots. These results were compared with the physiological and plasma biochemical parameters and the results of a histopathological test. Estrone, cortisone, proline, cystine, 3-ureidopropionic acid and histidine were proposed as potential safety biomarkers related with the liver toxicity of atorvastatin. These results indicate that the combined application of global and targeted metabolic profiling could be a useful tool for the discovery of drug safety biomarkers.

  15. Solid-Gas Coupling Model for Coal-Rock Mass Deformation and Pressure Relief Gas Flow in Protection Layer Mining

    OpenAIRE

    Zhu, Zhuohui; Feng, Tao; Yuan, Zhigang; Xie, Donghai; Chen, Wei

    2018-01-01

    The solid-gas coupling model for mining coal-rock mass deformation and pressure relief gas flow in protection layer mining is the key to determine deformation of coal-rock mass and migration law of pressure relief gas of protection layer mining in outburst coal seams. Based on the physical coupling process between coal-rock mass deformation and pressure-relief gas migration, the coupling variable of mining coal-rock mass, a part of governing equations of gas seepage field and deformation fiel...

  16. Clinical applications of gas chromatography and gas chromatography-mass spectrometry of steroids

    NARCIS (Netherlands)

    Wolthers, BG; Kraan, GPB

    1999-01-01

    This review article underlines the importance of gas chromatography-mass spectrometry (GC-MS) for determination of steroids in man. The use of steroids labelled with stable isotopes as internal standard and subsequent analysis by GC-MS yields up to now the only reliable measurement of steroids in

  17. Mass casualties from acute inhalation of chlorine gas.

    Science.gov (United States)

    Cevik, Yunsur; Onay, Meral; Akmaz, Ibrahim; Sezigen, Sermet

    2009-12-01

    Chlorine gas is a potent pulmonary irritant that affects the mucous membranes and induces severe disturbances of pulmonary gas exchange within minutes of inhalation. The present study evaluated an extraordinary type of mass inhalational exposure. Clinical reports of 25 soldiers who were admitted to the emergency department of Maresal Cakmak Military Hospital, Erzurum were retrospectively evaluated. All patients were exposed to chlorine gas as a result of mixing sodium hypochlorite with hydrochloric acid during cleaning activities. All patients were male and the mean age of patients was 22.04+/-2.98 years. The main symptoms were coughing and dyspnea in 18 patients (72%). Forced expiratory volume in 1 second (FEV1) and FEV1/forced volume capacity (FVC) ratio were found to be normal in all patients but FVC and peak expiratory flow (PEF) were below the normal range (80%) in 9 patients (36%). All patients received warmed humidified oxygen combined with nebulized salbutamol. Inhaled budesonide and nebulized sodium bicarbonate were ordered additionally for 19 patients (76%). Thirteen patients (52%) were discharged from the emergency department and 12 patients (48%) were hospitalized. No mortality was observed. Chlorine gas is a potent pulmonary irritant that causes acute damage in both the upper and lower respiratory tract. We suggest that inhaled steroids combined with nebulized sodium bicarbonate could be a safe and effective alternative for the treatment of symptomatic patients. Education of the public about the dangers of mixing of hypochlorite bleach with acidic cleaning agents is also very important.

  18. Diesel characterization by high-resolution mass spectrometry - gas chromatography

    International Nuclear Information System (INIS)

    Baldrich, C.A

    1998-01-01

    High-resolution mass spectrometry-gas chromatography is combined with the HC22 method in order to obtain detailed information about the chemical composition of diesel and the distribution of different compound types in terms of its final boiling temperature from a single analysis. The total time elapsed from sample injection and signal processing to obtain final results is 90 minutes. This fact makes this methodology a new and very important tool for the decision making process concerning the most suitable final boiling temperature and the type of treatment of the product in order to obtain diesel that fulfills the international standards. The consistency and repeatability of the experimental results are demonstrated

  19. Identification of inorganic anions by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Sakayanagi, Masataka; Yamada, Yaeko; Sakabe, Chikako; Watanabe, Kunio; Harigaya, Yoshihiro

    2006-03-10

    Inorganic anions were identified by using gas chromatography/mass spectrometry (GC/MS). Derivatization of the anions was achieved with pentafluorobenzyl p-toluenesulphonate (PFB-Tos) as the reaction reagent and a crown ether as a phase transfer catalyst. When PFB-Br was used as the reaction reagent, the retention time of it was close to those of the derivatized inorganic anions and interfered with the analysis. In contrast, the retention time of PFB-Tos differed greatly from the PFB derivatives of the inorganic anions and the compounds of interest could be detected without interference. Although the PFB derivatives of SO4, S2O3, CO3, ClO4, and ClO3 could not be detected, the derivatives of F, Cl, Br, I, CN, OCN, SCN, N3, NO3, and NO2 were detected using PFB-Tos as the derivatizing reagent. The inorganic anions were detectable within 30 ng approximately, which is of sufficient sensitivity for use in forensic chemistry. Accurate mass number was measured for each PFB derivative by high-resolution mass spectrometry (HRMS) within a measurement error of 2 millimass units (mmu), which allowed determination of the compositional formula from the mass number. In addition, actual analysis was performed successively by our method using trial samples of matrix.

  20. An inverse gas chromatographic methodology for studying gas-liquid mass transfer.

    Science.gov (United States)

    Paloglou, A; Martakidis, K; Gavril, D

    2017-01-13

    A novel methodology of reversed flow inverse gas chromatography (RF-IGC) is presented. It permits the simultaneous determination of mass transfer coefficients across the gas liquid interface as well as the respective solubility parameters and thermodynamic functions of dissolution of gases into liquids. The standard deviation of the experimentally determined parameters is estimated for first time, which combined with the successful comparison of the values of the present parameters with other literature ones ascertain the reliability of the methodology. Another novelty of the present work is that the chromatographic sampling of the physicochemical phenomena is done without performing the usual flow reversals procedure. Vinyl chloride monomer's (VCM) interaction with various composition liquid foods: orange juice, milk and olive oil was used as model system. The present transfer rates are controlled by the gas film at lower temperatures, but at higher temperatures the resistances in both films tend to become equal. The found liquid diffusivity values express the total mass transfer from the gas phase into the liquid's bulk and they decrease with rising temperature, as the solubilities of gases in liquids do. Solubility, expressed by Henry's law constant and the mean values of interfacial thickness are of the same order of magnitude to literature ones. From the thermodynamic point of view, VCM dissolution in all liquids is accompanied by significant heat release and it is a slightly non-spontaneous process, near equilibrium, while the entropy change values are negative. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. MEMS device for mass market gas and chemical sensors

    Science.gov (United States)

    Kinkade, Brian R.; Daly, James T.; Johnson, Edward A.

    2000-08-01

    Gas and chemical sensors are used in many applications. Industrial health and safety monitors allow companies to meet OSHA requirements by detecting harmful levels of toxic or combustible gases. Vehicle emissions are tested during annual inspections. Blood alcohol breathalizers are used by law enforcement. Refrigerant leak detection ensures that the Earth's ozone layer is not being compromised. Industrial combustion emissions are also monitored to minimize pollution. Heating and ventilation systems watch for high levels of carbon dioxide (CO2) to trigger an increase in fresh air exchange. Carbon monoxide detectors are used in homes to prevent poisoning from poor combustion ventilation. Anesthesia gases are monitored during a patients operation. The current economic reality is that two groups of gas sensor technologies are competing in two distinct existing market segments - affordable (less reliable) chemical reaction sensors for consumer markets and reliable (expensive) infrared (IR) spectroscopic sensors for industrial, laboratory, and medical instrumentation markets. Presently high volume mass-market applications are limited to CO detectros and on-board automotive emissions sensors. Due to reliability problems with electrochemical sensor-based CO detectors there is a hesitancy to apply these sensors in other high volume applications. Applications such as: natural gas leak detection, non-invasive blood glucose monitoring, home indoor air quality, personal/portable air quality monitors, home fire/burnt cooking detector, and home food spoilage detectors need a sensor that is a small, efficient, accurate, sensitive, reliable, and inexpensive. Connecting an array of these next generation gas sensors to wireless networks that are starting to proliferate today creates many other applications. Asthmatics could preview the air quality of their destinations as they venture out into the day. HVAC systems could determine if fresh air intake was actually better than the air

  2. Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

    Science.gov (United States)

    MacAskill, John A.; Tsikata, Edem

    2014-01-01

    We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

  3. Low thermal mass gas chromatography: principles and applications.

    Science.gov (United States)

    Luong, Jim; Gras, Ronda; Mustacich, Robert; Cortes, Hernan

    2006-01-01

    In gas chromatography (GC), temperature programming is often considered to be the second most important parameter to control, the first being column selectivity. A radically new GC technology to achieve ultrafast temperature programming with an unprecedented cool down time and low power consumption has recently become available. This technology is referred to as low thermal mass GC (LTMGC). Though the technology has its roots in resistive heating, which forms the basis of principle and design concept, the approach taken to achieve ultrafast heating and cool down time by LTMGC represents a significant break-through in GC. Despite some rectifiable shortcomings, LTMGC has proven to be an ideal methodology to deliver near/real time GC data, high precision, and high throughput applications. It is a new approach for modern high-speed GC. This paper documents the fundamental design principles behind LTMGC, performance data, and examples of applications investigated.

  4. THE GAS PHASE MASS METALLICITY RELATION FOR DWARF GALAXIES: DEPENDENCE ON STAR FORMATION RATE AND HI GAS MASS

    Energy Technology Data Exchange (ETDEWEB)

    Jimmy; Tran, Kim-Vy [George P. and Cynthia W. Mitchell Institute for Fundamental Physics and Astronomy, Department of Physics and Astronomy, Texas A and M University, College Station, TX 77843 (United States); Saintonge, Amélie; Accurso, Gioacchino [Department of Physics and Astronomy, University College London, Gower Place, London WC1E 6BT (United Kingdom); Brough, Sarah; Oliva-Altamirano, Paola [Australian Astronomical Observatory, P.O. Box 915, North Ryde, NSW 1670 (Australia)

    2015-10-20

    Using a sample of dwarf galaxies observed using the VIMOS IFU on the Very Large Telescope, we investigate the mass–metallicity relation (MZR) as a function of star formation rate (FMR{sub SFR}) as well as HI-gas mass (FMR{sub HI}). We combine our IFU data with a subsample of galaxies from the ALFALFA HI survey crossmatched to the Sloan Digital Sky Survey (SDSS) to study the FMR{sub SFR} and FMR{sub HI} across the stellar mass range 10{sup 6.6}–10{sup 8.8} M{sub ⊙}, with metallicities as low as 12 + log(O/H) = 7.67. We find the 1σ mean scatter in the MZR to be 0.05 dex. The 1σ mean scatter in the FMR{sub SFR} (0.02 dex) is significantly lower than that of the MZR. The FMR{sub SFR} is not consistent between the IFU observed galaxies and the ALFALFA/SDSS galaxies for SFRs lower than 10{sup −2.4} M{sub ⊙} yr{sup −1}, however, this could be the result of limitations of our measurements in that regime. The lowest mean scatter (0.01 dex) is found in the FMR{sub HI}. We also find that the FMR{sub HI} is consistent between the IFU observed dwarf galaxies and the ALFALFA/SDSS crossmatched sample. We introduce the fundamental metallicity luminosity counterpart to the FMR, again characterized in terms of SFR (FML{sub SFR}) and HI-gas mass (FML{sub HI}). We find that the FML{sub HI} relation is consistent between the IFU observed dwarf galaxy sample and the larger ALFALFA/SDSS sample. However, the 1σ scatter for the FML{sub HI} relation is not improved over the FMR{sub HI} scenario. This leads us to conclude that the FMR{sub HI} is the best candidate for a physically motivated fundamental metallicity relation.

  5. Determination of anabolic steroids with gas chromatography-ion trap mass spectrometry using hydrogen as carrier gas.

    Science.gov (United States)

    Impens, S; De Wasch, K; De Brabander, H

    2001-01-01

    Helium is considered to be the ideal carrier gas for gas chromatography/mass spectrometry (GC/MS) in general, and for use with an ion trap in particular. Helium is an inert gas, can be used without special precautions for security and, moreover, it is needed as a damping gas in the trap. A disadvantage of helium is the high viscosity resulting in long GC run times. In this work hydrogen was tested as an alternative carrier gas for GC in performing GC/MS analyses. A hydrogen generator was used as a safe source of hydrogen gas. It is demonstrated that hydrogen can be used as a carrier gas for the gas chromatograph in combination with helium as make-up gas for the trap. The analysis time was thus shortened and the chromatographic performance was optimized. Although hydrogen has proven useful as a carrier gas in gas chromatography coupled to standard detectors such as ECD or FID, its use is not mentioned extensively in the literature concerning gas chromatography-ion trap mass spectrometry. However, it is worth considering as a possibility because of its chromatographic advantages and its advantageous price when using a hydrogen generator. Copyright 2001 John Wiley & Sons, Ltd.

  6. Molecular Communication over Gas Stream Channels using Portable Mass Spectrometry

    Science.gov (United States)

    Giannoukos, Stamatios; Marshall, Alan; Taylor, Stephen; Smith, Jeremy

    2017-07-01

    The synthetic generation/coding and transmission of olfactory information over a gas stream or an odor network is a new and unexplored field. Application areas vary from the entertainment or advertisement industry to security and telemedicine. However, current technological limitations frustrate the accurate reproduction of decoded and transmitted olfactory data. This study describes the development, testing, and characterization of a novel odor emitter (OE) that is used to investigate the generation-encoding of gaseous standards with odorous characteristics with a regulatable way, for scent transmission purposes. The calibration and the responses of a developed OE were examined using a portable quadrupole mass spectrometer (MS). Experiments were undertaken for a range of volatile organic compounds (VOCs) at different temperatures and flow rates. Individual compounds and mixtures were tested to investigate periodic and dynamic transmission characteristics within two different size tubular containers for distances up to 3 m. Olfactory information transmission is demonstrated using MS as the main molecular sensor for odor detection and monitoring and for the first time spatial encryption of olfactory information is shown.

  7. A low thermal mass fast gas chromatograph and its implementation in fast gas chromatography mass spectrometry with supersonic molecular beams.

    Science.gov (United States)

    Fialkov, Alexander B; Moragn, Mati; Amirav, Aviv

    2011-12-30

    A new type of low thermal mass (LTM) fast gas chromatograph (GC) was designed and operated in combination with gas chromatography mass spectrometry (GC-MS) with supersonic molecular beams (SMB), including GC-MS-MS with SMB, thereby providing a novel combination with unique capabilities. The LTM fast GC is based on a short capillary column inserted inside a stainless steel tube that is resistively heated. It is located and mounted outside the standard GC oven on its available top detector port, while the capillary column is connected as usual to the standard GC injector and supersonic molecular beam interface transfer line. This new type of fast GC-MS with SMB enables less than 1 min full range temperature programming and cooling down analysis cycle time. The operation of the fast GC-MS with SMB was explored and 1 min full analysis cycle time of a mixture of 16 hydrocarbons in the C(10)H(22) up to C(44)H(90) range was achieved. The use of 35 mL/min high column flow rate enabled the elution of C(44)H(90) in less than 45 s while the SMB interface enabled splitless acceptance of this high flow rate and the provision of dominant molecular ions. A novel compound 9-benzylazidanthracene was analyzed for its purity and a synthetic chemistry process was monitored for the optimization of the chemical reaction yield. Biodiesel was analyzed in jet fuel (by both GC-MS and GC-MS-MS) in under 1 min as 5 ppm fatty acid methyl esters. Authentic iprodion and cypermethrin pesticides were analyzed in grapes extract in both full scan mode and fast GC-MS-MS mode in under 1 min cycle time and explosive mixture including TATP, TNT and RDX was analyzed in under 1 min combined with exhibiting dominant molecular ion for TATP. Fast GC-MS with SMB is based on trading GC separation for speed of analysis while enhancing the separation power of the MS via the enhancement of the molecular ion in the electron ionization of cold molecules in the SMB. This paper further discusses several features of

  8. Thermally modulated nano-trampoline material as smart skin for gas molecular mass detection

    Science.gov (United States)

    Xia, Hua

    2012-06-01

    Conventional multi-component gas analysis is based either on laser spectroscopy, laser and photoacoustic absorption at specific wavelengths, or on gas chromatography by separating the components of a gas mixture primarily due to boiling point (or vapor pressure) differences. This paper will present a new gas molecular mass detection method based on thermally modulated nano-trampoline material as smart skin for gas molecular mass detection by fiber Bragg grating-based gas sensors. Such a nanomaterial and fiber Bragg grating integrated sensing device has been designed to be operated either at high-energy level (highly thermal strained status) or at low-energy level (low thermal strained status). Thermal energy absorption of gas molecular trigs the sensing device transition from high-thermal-energy status to low-thermal- energy status. Experiment has shown that thermal energy variation due to gas molecular thermal energy absorption is dependent upon the gas molecular mass, and can be detected by fiber Bragg resonant wavelength shift with a linear function from 17 kg/kmol to 32 kg/kmol and a sensitivity of 0.025 kg/kmol for a 5 micron-thick nano-trampoline structure and fiber Bragg grating integrated gas sensing device. The laboratory and field validation data have further demonstrated its fast response characteristics and reliability to be online gas analysis instrument for measuring effective gas molecular mass from single-component gas, binary-component gas mixture, and multi-gas mixture. The potential industrial applications include fouling and surge control for gas charge centrifugal compressor ethylene production, gas purity for hydrogen-cooled generator, gasification for syngas production, gasoline/diesel and natural gas fuel quality monitoring for consumer market.

  9. Gas Chromatography-Mass Spectroscopic (GC-MS) Analysis of n ...

    African Journals Online (AJOL)

    tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC-. MS) techniques. Methods: The n-hexane extract of the sclerotia ... Soxhlet extraction and analysed using gas chromatography-mass spectroscopic (MS) techniques. ..... Phytochemical composition of Pleurotus tuber regium.

  10. Comparison of radioimmunoassay and gas chromatographic mass spectrometric assay for d-amphetamine

    International Nuclear Information System (INIS)

    Powers, K.H.; Ebert, M.H.

    1979-01-01

    Quantification of low levels of psychotropic drugs (10 -7 to 10 -9 g ml -1 ) in small volumes of plasma requires sensitive and accurate methods. Validation of these methods is best achieved by comparing results obtained using several techniques. In this study, amphetamine levels in plasma were measured using gas chromatography mass spectrometry and radioimmunoassay. Correlation of the results obtained by the two methods was found to be positive and high (R = 0.9822). The average coefficient of variation between assays for gas chromatography mass spectrometry was 5.8% and for radioimmunoassay was 12.3%, while the average coefficient of variation within assays for gas chromatography mass spectrometry was 4.9% and for radioimmunoassay 6.9%. Although gas chromatography mass spectrometry was 1.9 times more sensitive than radioimmunoassay, for most purposes, the convenience of the radioimmunoassay method outweighs the technical superiority of gas chromatography mass spectrometry. (author)

  11. Recent applications of gas chromatography with high-resolution mass spectrometry.

    Science.gov (United States)

    Špánik, Ivan; Machyňáková, Andrea

    2018-01-01

    Gas chromatography coupled to high-resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high-resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi-volatile organic compounds. Gas chromatography with high-resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high-resolution time-of-flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi-target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high-resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high-resolution mass spectrometry for non-target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high-resolution mass spectrometry over the currently used methods is expected, will be discussed as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Mass Spectral Studies of 1-(2-Chloroethoxy)-2-[(2-chloroethyl)thio] Ethane and Related Compounds Using Gas ChromatographyMass Spectrometry and Gas ChromatographyTriple-Quadrupole Mass Spectrometry

    Science.gov (United States)

    2016-02-01

    characteristic ions. 15. SUBJECT TERMS Sulfur mustard Degradation product Tandem mass spectrometry (MS-MS) Fragmentation Gas chromatography (GC...MacIver, B.K.; Rohrbaugh, D.K.; Yang, Y.C. Thermal Degradation of Bis (2-Chloroethyl) Sulfide ( Mustard Gas ). Phosphorus Sulfur Silicon Relat. Elem...MASS SPECTRAL STUDIES OF 1-(2-CHLOROETHOXY)-2-[(2-CHLOROETHYL)THIO] ETHANE AND RELATED COMPOUNDS USING GAS

  13. Advancement and application of gas chromatography isotope ratio mass spectrometry techniques for atmospheric trace gas analysis

    Science.gov (United States)

    Giebel, Brian M.

    2011-12-01

    The use of gas chromatography isotope ratio mass spectrometry (GC-IRMS) for compound specific stable isotope analysis is an underutilized technique because of the complexity of the instrumentation and high analytical costs. However stable isotopic data, when coupled with concentration measurements, can provide additional information on a compounds production, transformation, loss, and cycling within the biosphere and atmosphere. A GC-IRMS system was developed to accurately and precisely measure delta13C values for numerous oxygenated volatile organic compounds having natural and anthropogenic sources. The OVOCs include methanol, ethanol, acetone, methyl ethyl ketone, 2-pentanone, and 3-pentanone. Guided by the requirements for analysis of trace components in air, the GC-IRMS system was developed with the goals of increasing sensitivity, reducing dead-volume and peak band broadening, optimizing combustion and water removal, and decreasing the split ratio to the IRMS. The technique relied on a two-stage preconcentration system, a low-volume capillary reactor and water trap, and a balanced reference gas delivery system. Measurements were performed on samples collected from two distinct sources (i.e. biogenic and vehicle emissions) and ambient air collected from downtown Miami and Everglades National Park. However, the instrumentation and the method have the capability to analyze a variety of source and ambient samples. The measured isotopic signatures that were obtained from source and ambient samples provide a new isotopic constraint for atmospheric chemists and can serve as a new way to evaluate their models and budgets for many OVOCs. In almost all cases, OVOCs emitted from fuel combustion were enriched in 13C when compared to the natural emissions of plants. This was particularly true for ethanol gas emitted in vehicle exhaust, which was observed to have a uniquely enriched isotopic signature that was attributed to ethanol's corn origin and use as an alternative

  14. Quantification of carbonate by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Tsikas, Dimitrios; Chobanyan-Jürgens, Kristine

    2010-10-01

    Carbon dioxide and carbonates are widely distributed in nature, are constituents of inorganic and organic matter, and are essential in vegetable and animal organisms. CO(2) is the principal greenhouse gas in the atmosphere. In human blood, CO(2)/HCO(3)(-) is an important buffering system. Quantification of bicarbonate and carbonate in inorganic and organic matter and in biological fluids such as blood or blood plasma by means of the GC-MS technology has been impossible so far, presumably because of the lack of suitable derivatization reactions to produce volatile and thermally stable derivatives. Here, a novel derivatization reaction is described for carbonate that allows for its quantification in aqueous alkaline solutions and alkalinized plasma and urine. Carbonate in acetonic solutions of these matrices (1:4 v/v) and added (13)C-labeled carbonate for use as the internal standard were heated in the presence of the derivatization agent pentafluorobenzyl (PFB) bromide for 60 min and 50 °C. Investigations with (12)CO(3)(2-), (13)CO(3)(2-), (CH(3))(2)CO, and (CD(3))(2)CO in alkaline solutions and GC-MS and GC-MS/MS analyses under negative-ion chemical ionization (NICI) or electron ionization (EI) conditions of toluene extracts of the reactants revealed formation of two minor [i.e., PFB-OCOOH and O=CO(2)-(PFB)(2)] and two major [i.e., CH(3)COCH(2)-C(OH)(OPFB)(2) and CH(3)COCH=C(OPFB)(2)] carbonate derivatives. The latter have different retention times (7.9 and 7.5 min, respectively) but virtually identical EI and NICI mass spectra. It is assumed that CH(3)COCH(2)-C(OH)(OPFB)(2) is formed from the reaction of the carbonate dianion with two molecules of PFB bromide to form the diPFB ester of carbonic acid, which further reacts with one molecule of acetone. Subsequent loss of water finally generates the major derivative CH(3)COCH=C(OPFB)(2). This derivatization reaction was utilized to quantify total CO(2)/HCO(3)(-)/CO(3)(2-) (tCO(2)) in human plasma and urine by GC

  15. [Diagnosis of inborn errors of metabolism using tandem mass spectrometry and gas chromatography mass spectrometry].

    Science.gov (United States)

    Han, Lian-Shu; Ye, Jun; Qiu, Wen-Juan; Gao, Xiao-Lan; Wang, Yu; Jin, Jing; Gu, Xue-Fan

    2008-08-05

    To investigate the effects of tandem mass spectrometry (MS/MS) combined with gas chromatography mass spectrometry (GC-MS) in the diagnosis of inborn errors of metabolism in children. Amino acids and acylcarnitines in the dry blood filter papers were tested by MS/MS, and the organic acid profiles in urea were tested by GC-MS among 4981 children suspected to be with inborn errors of metabolism from more than 100 hospitals in China. A few pediatric patients underwent analysis of activity of enzyme and gene mutation analysis too. 319 of the 4981 children (6.4%) were diagnosed as with 24 kinds of diseases: 155 of the 319 cases (48.6%) with 8 kinds of amino acid diseases (97 with hyperphenylalaninemia, 14 with maple syrup urine disease 13 with ornithine transcarbamylase deficiency, 13 with citrullinemia type II, 10 with tyrosinemia type I, 5 with citrullinemia type I, 2 with homocystinuria, and 1 with arginasemia); 150 of the 319 cases (47.0%) were diagnosed as with 10 kinds of organic acidemias (81 with methylmalonic acidemia, 17 with propionic acidemia, 17 with multiple CoA carboxylase deficiency, 11 with glutaric acidemia type II, 8 with isovaleric acidemia, 6 with beta-keto thiolase deficiency, 5 with 3-methylcrotonyl-CoA carboxylase deficiency, and 3 with 3-hydroxy-3-methylglutaryl-CoA lyase deficiency); 14 cases (4.4%) were diagnosed as with 6 kinds of fatty acid disorders (5 with medium chain acyl-CoA dehydrogenase deficiency, 3 with very long chain acyl CoA dehydrogenase deficiency, 2 with short chain acyl-CoA dehydrogenase deficiency, 2 with multiple acyl-CoA dehydrogenase deficiency, 1 with carnitine palmitoyl transferase type II, and 1 with carnitine palmitoyl transferase type I). MS/MS is specific for amino acid diseases and fatty acid disorders. GC-MS is specific for detect organic acidemias. And the diagnoses of part of amino acid diseases need the combination of both methods.

  16. Thermogravimetry-evolved gas analysis–mass spectrometry system ...

    Indian Academy of Sciences (India)

    Unknown

    Metallurgy and Materials Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102, India. MS received 13 May 2002. Abstract. ... This paper essentially describes design features involved in coupling the existing .... pressure and (iv) for qualitative and quantitative analysis of unknown gas mixture (Dash et al ...

  17. Thermogravimetry-evolved gas analysis–mass spectrometry system ...

    Indian Academy of Sciences (India)

    This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for. temperature programmed decomposition (TPD),; synthesis of nanocrystalline materials,; gas–solid interactions and; analysis of gas mixtures. The TPD of various inorganic oxyanion solids ...

  18. Hybrid recoil mass analyzer at IUAC – First results using gas-filled ...

    Indian Academy of Sciences (India)

    2. — journal of. August 2010 physics pp. 317–331. Hybrid recoil mass analyzer at IUAC – First results using gas-filled mode and future plans. N MADHAVAN1,∗, S NATH1, .... with lighter projectiles by the choice of gas-filled mode operation of its first stage .... This slit system is designed and fabricated so that multiple slits for.

  19. Mass transfer processes across the Capillary Fringe: Quantification of gas-water interface and bubble mediated mass transfer

    Science.gov (United States)

    Geistlinger, Helmut; Mohammadian, Sadjad; Schlüter, Steffen; Karimzadeh, Lotfollah; Vogel, Hans-Jörg

    2013-04-01

    The Capillary Fringe (CF) is a highly dynamic zone at the interface between the water-saturated aquifer and the vadose zone, where steep biogeochemical gradients and thus high bioactivities are expected. Mass transfer processes between the unsaturated zone and the atmosphere, like Greenhouse gas emissions and evaporation, are controlled by the highly temporal and spatial variable gas-water interface across the capillary fringe. Due to water table fluctuations, gas phase may be entrapped or released at/from the CF, which extremely affects the hydraulic properties of the porous medium as well as the mass transfer processes in the partially saturated zone. Most of these processes (gas entrapment and bubble mediated mass transfer (BMT)) are governed by the interactions between the interfaces of gas, water and soil phases. Quantification of these parameters requires a pore-scale approach, which can determine the phase volumes and interfaces with high accuracy. For the understanding and prediction of the involved processes, experiments and modeling at the pore scale are the necessary prerequisites for upscaled, effective modeling approaches. To achieve this aim, we conducted a set of column experiments using X-Ray Computed Tomography (CT). Using this technique, we are able to quantitatively analyze the desired variables in 3D inside the actual bulk volume of the porous media. Water table (WT) elevation was raised at different velocities in the column filled with 1mm-glass beads. After each rise, the column was scanned with CT. We used an intelligent multi-phase segmentation method, considering grey value frequency and voxel neighboring, to separate gas, water, and solid phases in the CT images. The saturation of the gas phase, distribution of the trapped gas bubbles and clusters, and their size, shape, and area are quantified and analyzed at pore-scale. We developed a new segmentation algorithm to distinguish the gas/water interface from the gas/solid interface. Only the

  20. Low-mass spiral galaxies with little molecular gas and prodigious star formation

    International Nuclear Information System (INIS)

    Kenney, J.D.; Young, J.S.

    1988-01-01

    A comparison of CO and H I properties is used here to demonstrate that many CO-poor low-mass Virgo spiral galaxies are rich in atomic gas, which implies that the lack of CO emission from them is due, at least partly, to a lack of molecular gas. Despite the paucity of molecular gas, these H I-rich, CO-poor, low-mass spiral galaxies are undergoing extensive massive star formation. A column density of 10 to the 21st nuclei/sq cm is a necessary but insufficient condition for the creation of an H 2 -dominated interstellar medium. 40 references

  1. Microporous hollow fibre membrane modules as gas-liquid contactors. Part 1: Physical mass transfer processes. A specific application: mass transfer in highly viscous liquids

    NARCIS (Netherlands)

    Kreulen, H.; Kreulen, H.; Versteeg, Geert; Smolders, C.A.; Smolders, C.A.; van Swaaij, Willibrordus Petrus Maria

    1993-01-01

    Gas-liquid mass transfer has been studied in a membrane module with non-wetted microporous fibres in the laminar flow regime. This new type of gas/liquid contactor can be operated stabily over a large range of gas and liquid flows because gas and liquid phase do not influence each other directly.

  2. Kinetic energy and added mass of hydrodynamically interacting gas bubbles in liquid

    NARCIS (Netherlands)

    Kok, Jacobus B.W.

    1988-01-01

    By averaging the basic equations on microscale, expressions are derived for the effective added mass density and the kinetic energy density of a mixture of liquid and gas bubbles. Due to hydrodynamic interaction between the bubbles there appears to be a difference between the effective added mass

  3. Origin of the hot gas in low-mass protostars

    DEFF Research Database (Denmark)

    Van Kempen, T. A.; Kristensen, L. E.; Herczeg, G. J.

    2010-01-01

    Aims. "Water In Star-forming regions with Herschel" (WISH) is a Herschel key programme aimed at understanding the physical and chemical structure of young stellar objects (YSOs) with a focus on water and related species. Methods. The low-mass protostar HH 46 was observed with the Photodetector...

  4. Modelling of interactions between variable mass and density solid particles and swirling gas stream

    International Nuclear Information System (INIS)

    Wardach-Święcicka, I; Kardaś, D; Pozorski, J

    2011-01-01

    The aim of this work is to investigate the solid particles - gas interactions. For this purpose, numerical modelling was carried out by means of a commercial code for simulations of two-phase dispersed flows with the in-house models accounting for mass and density change of solid phase. In the studied case the particles are treated as spherical moving grains carried by a swirling stream of hot gases. Due to the heat and mass transfer between gas and solid phase, the particles are losing their mass and they are changing their volume. Numerical simulations were performed for turbulent regime, using two methods for turbulence modelling: RANS and LES.

  5. Viscous slip coefficients for binary gas mixtures measured from mass flow rates through a single microtube

    OpenAIRE

    Yamaguchi, H.; Takamori, K.; Perrier, P.; Graur, I.; Matsuda, Y.; Niimi, T.

    2016-01-01

    The viscous slip coefficient for helium-argon binary gas mixture is extracted from the experimental values of the mass flow rate through a microtube. The mass flow rate is measured by the constant-volume method. The viscous slip coefficient was obtained by identifying the measured mass flow rate through a microtube with the corresponding analytical expression, which is a function of the Knudsen number. The measurements were carried out in the slip flow regime where the first-order slip bounda...

  6. Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Wong, April S Y; Leung, Gary N W; Leung, David K K; Wan, Terence S M

    2017-09-01

    Anabolic steroids are banned substances in equine sports. Gas chromatography-mass spectrometry (GC-MS) has been the traditional technique for doping control analysis of anabolic steroids in biological samples. Although liquid chromatography-mass spectrometry (LC/MS) has become an important technique in doping control, the detection of saturated hydroxysteroids by LC-MS remains a problem due to their low ionization efficiency under electrospray. The recent development in fast-scanning gas-chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) has provided a better alternative with a significant reduction in chemical noise by means of selective reaction monitoring. Herein, we present a sensitive and selective method for the screening of over 50 anabolic steroids in equine urine using gas chromatography-tandem mass spectrometry (GC-MS/MS). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  7. Liquid-gas mass transfer at drop structures

    DEFF Research Database (Denmark)

    Matias, Natércia; Nielsen, Asbjørn Haaning; Vollertsen, Jes

    2017-01-01

    established. Then, by applying the two-film theory with two-reference substances, the relation to hydrogen sulfide release was defined. The experiments confirmed that the choice of the type of drop structure is critical to determine the uptake/emission rates. By quantifying the air-water mass transfer rates...... between free-fall and backdrop types of drop, the latter resulted in considerably lower oxygen uptake rates....

  8. Modelling mass transfer during venting/soil vapour extraction: Non-aqueous phase liquid/gas mass transfer coefficient estimation

    Science.gov (United States)

    Esrael, D.; Kacem, M.; Benadda, B.

    2017-07-01

    We investigate how the simulation of the venting/soil vapour extraction (SVE) process is affected by the mass transfer coefficient, using a model comprising five partial differential equations describing gas flow and mass conservation of phases and including an expression accounting for soil saturation conditions. In doing so, we test five previously reported quations for estimating the non-aqueous phase liquid (NAPL)/gas initial mass transfer coefficient and evaluate an expression that uses a reference NAPL saturation. Four venting/SVE experiments utilizing a sand column are performed with dry and non-saturated sand at low and high flow rates, and the obtained experimental results are subsequently simulated, revealing that hydrodynamic dispersion cannot be neglected in the estimation of the mass transfer coefficient, particularly in the case of low velocities. Among the tested models, only the analytical solution of a convection-dispersion equation and the equation proposed herein are suitable for correctly modelling the experimental results, with the developed model representing the best choice for correctly simulating the experimental results and the tailing part of the extracted gas concentration curve.

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

    Directory of Open Access Journals (Sweden)

    Sumandeep Rana

    2014-09-01

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

  10. Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

    Science.gov (United States)

    Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

    2016-01-01

    Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. A black-hole mass measurement from molecular gas kinematics in NGC4526.

    Science.gov (United States)

    Davis, Timothy A; Bureau, Martin; Cappellari, Michele; Sarzi, Marc; Blitz, Leo

    2013-02-21

    The masses of the supermassive black holes found in galaxy bulges are correlated with a multitude of galaxy properties, leading to suggestions that galaxies and black holes may evolve together. The number of reliably measured black-hole masses is small, and the number of methods for measuring them is limited, holding back attempts to understand this co-evolution. Directly measuring black-hole masses is currently possible with stellar kinematics (in early-type galaxies), ionized-gas kinematics (in some spiral and early-type galaxies) and in rare objects that have central maser emission. Here we report that by modelling the effect of a black hole on the kinematics of molecular gas it is possible to fit interferometric observations of CO emission and thereby accurately estimate black-hole masses. We study the dynamics of the gas in the early-type galaxy NGC 4526, and obtain a best fit that requires the presence of a central dark object of 4.5(+4.2)(-3.1) × 10(8) solar masses (3σ confidence limit). With the next-generation millimetre-wavelength interferometers these observations could be reproduced in galaxies out to 75 megaparsecs in less than 5 hours of observing time. The use of molecular gas as a kinematic tracer should thus allow one to estimate black-hole masses in hundreds of galaxies in the local Universe, many more than are accessible with current techniques.

  12. The effect of nuclear gas distribution on the mass determination of supermassive black holes

    Science.gov (United States)

    Mejía-Restrepo, J. E.; Lira, P.; Netzer, H.; Trakhtenbrot, B.; Capellupo, D. M.

    2018-01-01

    Supermassive black holes reside in the nuclei of most galaxies. During their active episodes, black holes are powered by accretion discs where gravitational energy is converted into radiation1. Accurately determining black hole masses is key to understand how the population evolves over time and how the black holes relate to their host galaxies2-4. Beyond the local universe, z ≳ 0.2, the mass is commonly estimated assuming a virialized motion of gas in the close vicinity of the active black holes, traced through broad emission lines5,6. However, this procedure has uncertainties associated with the unknown distribution of the gas clouds. Here, we show that the black hole masses derived from the properties of the accretion disk and virial mass estimates differ by a factor that is inversely proportional to the width of the broad emission lines. This leads to virial mass misestimations up to a factor of six. Our results suggest that a planar gas distribution that is inclined with respect to the line of sight may account for this effect. However, radiation pressure effects on the distribution of gas can also reproduce our results. Regardless of the physical origin, our findings contribute to mitigating the uncertainties in current black hole mass estimations and, in turn, will help us to better understand the evolution of distant supermassive black holes and their host galaxies.

  13. Determination of gas phase triacetone triperoxide with aspiration ion mobility spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Räsänen, Riikka-Marjaana; Nousiainen, Marjaana; Peräkorpi, Kaleva; Sillanpää, Mika; Polari, Lauri; Anttalainen, Osmo; Utriainen, Mikko

    2008-08-08

    Aspiration ion mobility spectrometry (IMS) has been used for the first time to screen 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexaoxacyclononane explosive, the most commonly known as triacetone triperoxide (TATP). Gaseous TATP was generated from synthesized solid compound, sublimed and directed to a portable chemical detection system comprised of an aspiration-type IMS detector and six semiconductor sensors. Different unknown TATP gas phase concentrations were produced and corresponding IMS and semiconductor responses were measured. The experimental concentrations were determined by gas chromatography-mass spectrometry (GC-MS). The results evidenced that the monitored compound in the gas phase was TATP. In addition, the determined TATP concentrations and corresponding IMS intensities showed that the IMS response values were proportional to the measured TATP concentrations.

  14. Gas phase ion/molecule reactions as studied by Fourier Transform Ion Cyclotron Resonance mass spectrometry

    International Nuclear Information System (INIS)

    Joergensen, S.I.

    1985-01-01

    The subject of this thesis is gas phase ion/molecule reactions as studied by Fourier Transform Ion Cyclotron Resonance (FT-ICR) mass spectrometry (chapter 2 contains a short description of this method). Three chapters are mainly concerned with mechanistic aspects of gas phase ion/molecule reactions. An equally important aspect of the thesis is the stability and reactivity of α-thio carbanions, dipole stabilized carbanions and homoenolate anions, dealt with in the other four chapters. (Auth.)

  15. Cosmological Evolution of the Universe Neutral Gas Mass Measured by Quasar Absorption Systems

    OpenAIRE

    Peroux, Celine; McMahon, Richard G.; Irwin, Mike; Storrie-Lombardi, Lisa J.

    2001-01-01

    The cosmological evolution of neutral hydrogen is an efficient way of tracing structure formation with redshift. It indicates the rate of evolution of gas into stars and hence the gas consumption and rate star formation history of the Universe. In measuring HI, quasar absorbers have proven to be an ideal tool and we use observations from a recent survey for high-redshift quasar absorption systems together with data gathered from the literature to measure the cosmological comoving mass density...

  16. Microporous hollow fibre membrane modules as gas-liquid contactors. Part 1. Physical mass transfer processes : A specific application

    NARCIS (Netherlands)

    Kreulen, H.; Versteeg, G.F.; Swaaij, W.P.M. van

    1993-01-01

    Gas-liquid mass transfer has been studied in a membrane module with non-wetted microporous fibres in the laminar flow regime. This new type of gas/liquid contactor can be operated stabily over a large range of gas and liquid flows because gas and liquid phase do not influence each other directly.

  17. Global mass conservation method for dual-continuum gas reservoir simulation

    KAUST Repository

    Wang, Yi

    2018-03-17

    In this paper, we find that the numerical simulation of gas flow in dual-continuum porous media may generate unphysical or non-robust results using regular finite difference method. The reason is the unphysical mass loss caused by the gas compressibility and the non-diagonal dominance of the discretized equations caused by the non-linear well term. The well term contains the product of density and pressure. For oil flow, density is independent of pressure so that the well term is linear. For gas flow, density is related to pressure by the gas law so that the well term is non-linear. To avoid these two problems, numerical methods are proposed using the mass balance relation and the local linearization of the non-linear source term to ensure the global mass conservation and the diagonal dominance of discretized equations in the computation. The proposed numerical methods are successfully applied to dual-continuum gas reservoir simulation. Mass conservation is satisfied while the computation becomes robust. Numerical results show that the location of the production well relative to the large-permeability region is very sensitive to the production efficiency. It decreases apparently when the production well is moved from the large-permeability region to the small-permeability region, even though the well is very close to the interface of the two regions. The production well is suggested to be placed inside the large-permeability region regardless of the specific position.

  18. Gas chromatography - mass spectrometry data processing made easy.

    Science.gov (United States)

    Johnsen, Lea G; Skou, Peter B; Khakimov, Bekzod; Bro, Rasmus

    2017-06-23

    Evaluation of GC-MS data may be challenging due to the high complexity of data including overlapped, embedded, retention time shifted and low S/N ratio peaks. In this work, we demonstrate a new approach, PARAFAC2 based Deconvolution and Identification System (PARADISe), for processing raw GC-MS data. PARADISe is a computer platform independent freely available software incorporating a number of newly developed algorithms in a coherent framework. It offers a solution for analysts dealing with complex chromatographic data. It allows extraction of chemical/metabolite information directly from the raw data. Using PARADISe requires only few inputs from the analyst to process GC-MS data and subsequently converts raw netCDF data files into a compiled peak table. Furthermore, the method is generally robust towards minor variations in the input parameters. The method automatically performs peak identification based on deconvoluted mass spectra using integrated NIST search engine and generates an identification report. In this paper, we compare PARADISe with AMDIS and ChromaTOF in terms of peak quantification and show that PARADISe is more robust to user-defined settings and that these are easier (and much fewer) to set. PARADISe is based on non-proprietary scientifically evaluated approaches and we here show that PARADISe can handle more overlapping signals, lower signal-to-noise peaks and do so in a manner that requires only about an hours worth of work regardless of the number of samples. We also show that there are no non-detects in PARADISe, meaning that all compounds are detected in all samples. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

  19. The influence of polymeric membrane gas spargers on hydrodynamics and mass transfer in bubble column bioreactors

    DEFF Research Database (Denmark)

    Tirunehe, Gossay; Norddahl, B.

    2016-01-01

    Gas sparging performances of a flat sheet and tubular polymeric membranes were investigated in 3.1 m bubble column bioreactor operated in a semi batch mode. Air–water and air–CMC (Carboxymethyl cellulose) solutions of 0.5, 0.75 and 1.0 % w/w were used as interacting gas–liquid mediums. CMC...... solutions were employed in the study to simulate rheological properties of bioreactor broth. Gas holdup, bubble size distribution, interfacial area and gas–liquid mass transfer were studied in the homogeneous bubbly flow hydrodynamic regime with superficial gas velocity (UG) range of 0.0004–0.0025 m...

  20. Numerical simulation study of gas-liquid reactive mass transfer along corrugated sheets with interface tracking

    International Nuclear Information System (INIS)

    Haroun, Y.

    2008-11-01

    This work is done within the framework of gas treatment and CO 2 capture process development. The main objective of the present work is to fill the gap between classical experiments and industrial conditions by the use of Computational Fluid Dynamics (CFD). The physical problem considered corresponds to the liquid film flow down a corrugate surface under gravity in present of a gas phase. The chemical species in the gas phase absorb in the liquid phase and react. Numerical calculations are carried out in order to determine the impact of physical and geometrical properties on reactive mass transfer in industrial operating conditions. (author)

  1. Simulation of rarefied gas flows in atmospheric pressure interfaces for mass spectrometry systems.

    Science.gov (United States)

    Garimella, Sandilya; Zhou, Xiaoyu; Ouyang, Zheng

    2013-12-01

    The understanding of the gas dynamics of the atmospheric pressure interface is very important for the development of mass spectrometry systems with high sensitivity. While the gas flows at high pressure (>1 Torr) and low pressure (pressure stage (1 to 10(-3) Torr) remains challenging. In this study, we used the direct simulation Monte Carlo (DMSC) method to develop the gas dynamic simulations for the continuous and discontinuous atmospheric pressure interfaces (API), with different focuses on the ion transfer by gas flows through a skimmer or directly from the atmospheric pressure to a vacuum stage, respectively. The impacts by the skimmer location in the continuous API and the temporal evolvement of the gas flow with a discontinuous API were characterized, which provide a solid base for the instrument design and performance improvement.

  2. Qualitative gas chromatography-mass spectrometry analyses using amines as chemical ionization reagent gases.

    Science.gov (United States)

    Little, James L; Howard, Adam S

    2013-12-01

    Ammonia is a very useful chemical ionization (CI) reagent gas for the qualitative analyses of compounds by positive ion gas chromatography-mass spectrometry (GCMS). The gas is readily available, inexpensive, and leaves no carbon contamination in the MS source. Compounds of interest to our laboratory typically yield abundant protonated or ammoniated species, which are indicative of a compound's molecular weight. Nevertheless, some labile compounds fragment extensively by substitution and elimination reactions and yield no molecular weight information. In these cases, a CI reagent gas mixture of methylamine in methane prepared dynamically was found to be very useful in obtaining molecular weight data. Likewise, deuterated ammonia and deuterated methylamine are useful CI reagent gases for determining the exchangeable protons in organic compounds. Deuterated methylamine CI reagent gas is conveniently prepared by dynamically mixing small amounts of methylamine with excess deuterated ammonia.

  3. Coriolis Mass-Flowmeter for aerostatic gas amount determination in zero pressure stratosperic balloons.

    Science.gov (United States)

    Behar, Jean-Baptiste

    2016-07-01

    The CNES ballooning community regularly operates zero pressure balloons in many countries around the world (recently in France, Sweden, Canada and soon, Australia in 2017). An important operational flight parameter is the aerostatic gas mass injected into the balloon (currently helium and hydrogen in the study). Besides the lifting force, it determines mainly the ascent rate from which the adiabatic expansion depends directly. A too high ascent velocity in very cold air temperature profiles could result in a gas temperature drop which if too great, might induce brittleness of the envelope. A precise gas mass determination is therefore critical for performance as well as for mission safety. The various gas supply tanks in various countries all have different characteristics with possible uncertainties with regard to their volumes. This makes the currently used gas mass determination method based on supply tank pressure measurements unreliable. This method also relies on tank temperature, another source of inaccuracy in the gas amount determination. CNES has therefore prospected for alternative methods to reduce inaccuracies and perhaps also ease the operational procedures during balloon inflation. Coriolis mass-flowmeters which have reached industrial maturity, offer the great advantage over other flowmeters to be able to directly measure the mass of the transferred fluid, and not deducing it from other parameters as other types of flowmeters would do. An industrial contractor has been therefore assigned to integrate this solution into the CNES operational setup. This new system is to be tested in February 2016. The presentation will briefly explain the Coriolis flowmeter's principle and display the February 2016 performance tests' results. The expected incidence on zero pressure balloons' trajectories will also be discussed based on simulations ran on a balloon flight simulator software.

  4. Multiple inert gas elimination technique by micropore membrane inlet mass spectrometry--a comparison with reference gas chromatography.

    Science.gov (United States)

    Kretzschmar, Moritz; Schilling, Thomas; Vogt, Andreas; Rothen, Hans Ulrich; Borges, João Batista; Hachenberg, Thomas; Larsson, Anders; Baumgardner, James E; Hedenstierna, Göran

    2013-10-15

    The mismatching of alveolar ventilation and perfusion (VA/Q) is the major determinant of impaired gas exchange. The gold standard for measuring VA/Q distributions is based on measurements of the elimination and retention of infused inert gases. Conventional multiple inert gas elimination technique (MIGET) uses gas chromatography (GC) to measure the inert gas partial pressures, which requires tonometry of blood samples with a gas that can then be injected into the chromatograph. The method is laborious and requires meticulous care. A new technique based on micropore membrane inlet mass spectrometry (MMIMS) facilitates the handling of blood and gas samples and provides nearly real-time analysis. In this study we compared MIGET by GC and MMIMS in 10 piglets: 1) 3 with healthy lungs; 2) 4 with oleic acid injury; and 3) 3 with isolated left lower lobe ventilation. The different protocols ensured a large range of normal and abnormal VA/Q distributions. Eight inert gases (SF6, krypton, ethane, cyclopropane, desflurane, enflurane, diethyl ether, and acetone) were infused; six of these gases were measured with MMIMS, and six were measured with GC. We found close agreement of retention and excretion of the gases and the constructed VA/Q distributions between GC and MMIMS, and predicted PaO2 from both methods compared well with measured PaO2. VA/Q by GC produced more widely dispersed modes than MMIMS, explained in part by differences in the algorithms used to calculate VA/Q distributions. In conclusion, MMIMS enables faster measurement of VA/Q, is less demanding than GC, and produces comparable results.

  5. Black hole mass measurement using molecular gas kinematics: what ALMA can do

    Science.gov (United States)

    Yoon, Ilsang

    2017-04-01

    We study the limits of the spatial and velocity resolution of radio interferometry to infer the mass of supermassive black holes (SMBHs) in galactic centres using the kinematics of circum-nuclear molecular gas, by considering the shapes of the galaxy surface brightness profile, signal-to-noise ratios (S/Ns) of the position-velocity diagram (PVD) and systematic errors due to the spatial and velocity structure of the molecular gas. We argue that for fixed galaxy stellar mass and SMBH mass, the spatial and velocity scales that need to be resolved increase and decrease, respectively, with decreasing Sérsic index of the galaxy surface brightness profile. We validate our arguments using simulated PVDs for varying beam size and velocity channel width. Furthermore, we consider the systematic effects on the inference of the SMBH mass by simulating PVDs including the spatial and velocity structure of the molecular gas, which demonstrates that their impacts are not significant for a PVD with good S/N unless the spatial and velocity scale associated with the systematic effects are comparable to or larger than the angular resolution and velocity channel width of the PVD from pure circular motion. Also, we caution that a bias in a galaxy surface brightness profile owing to the poor resolution of a galaxy photometric image can largely bias the SMBH mass by an order of magnitude. This study shows the promise and the limits of ALMA observations for measuring SMBH mass using molecular gas kinematics and provides a useful technical justification for an ALMA proposal with the science goal of measuring SMBH mass.

  6. Fault Detection of Inline Reciprocating Diesel Engine: A Mass and Gas-Torque Approach

    Directory of Open Access Journals (Sweden)

    S. H. Gawande

    2012-01-01

    Full Text Available Early fault detection and diagnosis for medium-speed diesel engines are important to ensure reliable operation throughout the course of their service. This work presents an investigation of the diesel engine combustion-related fault detection capability of crankshaft torsional vibrations. Proposed methodology state the way of early fault detection in the operating six-cylinder diesel engine. The model of six cylinders DI Diesel engine is developed appropriately. As per the earlier work by the same author the torsional vibration amplitudes are used to superimpose the mass and gas torque. Further mass and gas torque analysis is used to detect fault in the operating engine. The DFT of the measured crankshaft’s speed, under steady-state operating conditions at constant load shows significant variation of the amplitude of the lowest major harmonic order. This is valid both for uniform operating and faulty conditions and the lowest harmonic orders may be used to correlate its amplitude to the gas pressure torque and mass torque for a given engine. The amplitudes of the lowest harmonic orders (0.5, 1, and 1.5 of the gas pressure torque and mass torque are used to map the fault. A method capable to detect faulty cylinder of operating Kirloskar diesel engine of SL90 Engine-SL8800TA type is developed, based on the phases of the lowest three harmonic orders.

  7. [Structure determination of alkyd resins by simultaneous pyrolysis methylation gas chromatography-mass spectometry].

    Science.gov (United States)

    Cao, J Y; Fu, D H; Zhang, F; Liang, D

    2000-09-01

    Several types of alkyd resins have been analyzed by simultaneous pyrolysis methylation gas chromatography mass spectrometry (SPM-GC-MS). The samples were mixed with tetramethylammonium hydroxide, and the process included simultaneous pyrolysis derivatization and mass spectrometry determination. SPM-GC-MS conditions: a vertical microfurnace-type pyrolyzer was directly attached to a gas chromatograph-mass spectrometer. About 20 ug of the mixed alkyd resin sample was introduced into the center of the pyrolyzer at 450 degrees C under the flow of helium carrier gas. The inlet mode was split with an injection interval of 10 s and the inlet pressure was 82.7 kPa. The gas chromatograph was fitted with a fused-silica capillary column ( SE-54 30 m x0.25 mm i.d. x 0.25 um). Temperature program settings were: initial temperature, 40 degrees C, hold 2 min; increase at 6 degrees C min 1 to 220 degrees C, hold 14 min; increase at 10 degrees C min 1 to 280 degrees C, hold 8 min. All pyrolysis products referred to were identified by mass spectrometry. The temperature of the ion source was 210 degrees C and that of the transfer line was 250 degrees C. The technique could give additional information about the composition of the dibasic acids, polyols, six types of drying oils, and modified alkyd resins. The method is sensitive, accurate, convenient, and involves minimal sample manipulation.

  8. Incorporation of Gas Chromatography-Mass Spectrometry into the Undergraduate Organic Chemistry Laboratory Curriculum

    Science.gov (United States)

    Giarikos, Dimitrios G.; Patel, Sagir; Lister, Andrew; Razeghifard, Reza

    2013-01-01

    Gas chromatography-mass spectrometry (GC-MS) is a powerful analytical tool for detection, identification, and quantification of many volatile organic compounds. However, many colleges and universities have not fully incorporated this technique into undergraduate teaching laboratories despite its wide application and ease of use in organic…

  9. Gas Chromatography/mass Spectrometry Analysis of Exhaled Leukotrienes in Asthmatic Patients

    Czech Academy of Sciences Publication Activity Database

    Čáp, P.; Chládek, J.; Pehal, F.; Malý, Marek; Petrů, V.; Barnes, P.J.; Montuschi, P.

    2004-01-01

    Roč. 59, č. 6 (2004), s. 465-470 ISSN 0040-6376 Source of funding: V - iné verejné zdroje Keywords : asthma * breath condensate * gas chromatography/mass spectrometry * leukotrienes Subject RIV: BB - Applied Statistics, Operational Research Impact factor: 5.040, year: 2004

  10. Gas chromatography-mass spectrometry (GC-MS) analysis of extractives of naturally durable wood

    Science.gov (United States)

    G.T. Kirker; A.B. Blodgett; S.T. Lebow; C.A. Clausen

    2011-01-01

    A preliminary study to evaluate naturally durable wood species in an above ground field trial using Gas Chromatography-Mass Spectrometry (GC-MS) detected differences in fatty acid extractives between species and within the same species over time. Fatty acids were extracted with chloroform: methanol mixture then methylated with sodium methoxide and fractionated using...

  11. Ion counting method and it's operational characteristics in gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Fujii, Toshihiro

    1976-01-01

    Ion counting method with continuous channel electron multiplier which affords the direct detection of very small ion currents and it's operational characteristics were studied in gas chromatography-mass spectrometry. Then this method was applied to the single ion detection technique of GC-MS. A detection limit was measured, using various standard samples of low level concentration. (auth.)

  12. The Significance of Gas-Phase Mass Transport in Assessment of kchem and Dchem

    DEFF Research Database (Denmark)

    Lohne, Ørjan Fossmark; Søgaard, Martin; Wiik, Kjell

    2013-01-01

    In this work, the validity of electrical conductivity relaxation (ECR) as a method for the assessment of chemical surface exchange, kchem, and bulk diffusion, Dchem, coefficients is investigated with respect to mass transport limitations in the gas phase. A model encompassing both the oxygen...

  13. Identification of Synthetic Polymers and Copolymers by Analytical Pyrolysis-Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

    An experiment for the identification of synthetic polymers and copolymers by analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was developed and performed in the polymer analysis courses for third-year undergraduate students of chemistry with material sciences, and for first-year postgraduate students of polymer sciences. In…

  14. Mass transfer accompanied with complete reversible chemical reactions in gas-liquid systems: an overview

    NARCIS (Netherlands)

    van Swaaij, Willibrordus Petrus Maria; Versteeg, Geert

    1992-01-01

    In many processes in the chemical industry mass transfer accompanied with reversible, complex chemical reactions in gas-liquid systems are frequently encountered. In point of view of design purposes it is very important that the absorption rates of the transferred reactants can estimated

  15. Molecular theory of mass transfer kinetics and dynamics at gas-water interface

    International Nuclear Information System (INIS)

    Morita, Akihiro; Garrett, Bruce C

    2008-01-01

    The mass transfer mechanism across gas-water interface is studied with molecular dynamics (MD) simulation. The MD results provide a robust and qualitatively consistent picture to previous studies about microscopic aspects of mass transfer, including interface structure, free energy profiles for the uptake, scattering dynamics and energy relaxation of impinging molecules. These MD results are quantitatively compared with experimental uptake measurements, and we find that the apparent inconsistency between MD and experiment could be partly resolved by precise decomposition of the observed kinetics into elemental steps. Remaining issues and future perspectives toward constructing a comprehensive multi-scale description of interfacial mass transfer are summarized.

  16. Gas-liquid mass transfer coefficient of methane in bubble column reactor

    International Nuclear Information System (INIS)

    Lee, Jaewon; Ha, Kyoung-Su; Lee, Jinwon; Kim, Choongik; Yasin, Muhammad; Park, Shinyoung; Chang, In Seop; Lee, Eun Yeol

    2015-01-01

    Biological conversion of methane gas has been attracting considerable recent interest. However, methanotropic bioreactor is limited by low solubility of methane gas in aqueous solution. Although a large mass transfer coefficient of methane in water could possibly overcome this limitation, no dissolved methane probe in aqueous environment is commercially available. We have developed a reactor enabling the measurement of aqueous phase methane concentration and mass transfer coefficient (k L a). The feasibility of the new reactor was demonstrated by measuring k L a values as a function of spinning rate of impeller and flow rate of methane gas. Especially, at spinning rate of 300 rpm and flow rate of 3.0 L/min, a large k L a value of 102.9 h -1 was obtained

  17. Time resolved mass flow measurements for a fast gas delivery system

    International Nuclear Information System (INIS)

    Ruden, E.L.; Degnan, J.H.; Hussey, T.W.; Scott, M.C.; Graham, J.D.; Coffey, S.K.

    1992-01-01

    A technique is demonstrated whereby the delivered mass and flow rate vs. time of a short rise time gas delivery system may be accurately determined. The gas mass M which flows past a point in a gas delivery system by an arbitrary time t may be accurately measured if that point is sealed off within a time interval short compared to the mass flow time scale. If the ejected mass is allowed to equilibrate in a known volume after being cut off from its source, a conventional static pressure measurement before and after injection, and application of the ideal gas law suffices. Assuming reproducibility, a time history M(t) may be generated, allowing the flow rate vs. time dM(t)/dt to be determined. Mass flow measurements are presented for a fast delivery system in which the flow of argon through a 3.2 mm I.D., 0.76 mm thick copper tube is cut off by imploding (θ pinching) the tube using a single turn tungsten magnetic field coil. Pinch discharge parameters are 44 μf, 20 kV, 47 nH, 3.5 mΩ, 584 kA, and 8.63 ps current period. Optical measurements of the tube's internal area vs. time indicate that the tube is sealed 2 ps from the time the tube is still 90% open (7 μs from the start of pinch current). The pinch delay is varied from 500--1,500 ps from the valve trigger (0--1,000 ps from the start of gas flow). The mass injected into the test volume is ∼ 100 μg during this interval. The leak rate of the sealed tube results in a mass increase of only ∼ 0.1 μg by the time the pressure gauge stabilizes (6 s). Results are correlated with piezoelectric probe measurements of the gas flow and 2-D axisymmetric numerical simulations of the θ pinch process. Simulations of a θ pinch suitable for characterizing an annular supersonic nozzle typical of those used in gas puff z pinches are discussed

  18. Graphitized carbon in gas-liquid-solid chromatography and gas chromatography/mass spectrometric analysis of high boiling hydrocarbon mixtures

    International Nuclear Information System (INIS)

    Ciccioli, P.; Hayes, J.M.; Rinaldi, G.; Denson, K.B.; Meinschein, W.G.

    1979-01-01

    Gas--liquid--solid chromatography (GLSC) employing a poly(phenyl ether) (PPE 20) liquid phase on graphitized carbon black (GCB) is applicable to the analyses of crude oils and distillates of sedimentary rocks. The elution of C 4 to C 40 hydrocarbons which consist of n-alkanes, isoprenoid-type alkanes, steranes, olefins, and aromatic hydrocarbons can be handled in a single GC run. A GLSC column in tandem with a mass spectrometer provides an excellent means for the identification of geochemically significant organic compounds in complex natural mixtures. 8 figures, 4 tables

  19. CI as a Tracer of Gas Mass in Star Forming Galaxies

    Science.gov (United States)

    Bourne, Nathan

    2018-01-01

    Research in galaxy evolution aims to understand the cosmic industry of converting gas into stars. While SFR and stellar mass evolution are well constrained by current data, our knowledge of gas in galaxies throughout cosmic time is comparatively lacking. Almost all high-redshift gas measurements to date rely on CO as a tracer, but this is subject to systematic uncertainties due to optically thick emission and poorly constrained dependences on gas density, distribution and metallicity. Recently, some attention has been given to dust continuum as an alternative gas tracer, which shows promise for large samples but still requires accurate calibration on a direct gas tracer at high redshift. The [CI] 492GHz emission line could overcome much of the systematic uncertainty, as it is optically thin and has similar excitation conditions to CO(1-0), but observational limitations have so far restricted CI measurements to very small samples. I will presen t some new data from ALMA, for the first time testing the CI/dust correlation in a representative sample of star-forming galaxies at z=1, and discuss how future observations could be designed to more widely exploit this independent gas tracer.

  20. Gas chromatography/mass spectrometry and pyrolysis-gas chromatography/mass spectrometry for the chemical characterisation of modern and archaeological figs (Ficus carica).

    Science.gov (United States)

    Ribechini, Erika; Pérez-Arantegui, Josefina; Colombini, Maria Perla

    2011-06-24

    Gas chromatography/mass spectrometry (GC/MS) after alkaline hydrolysis, solvent extraction and trimethylsilylation, and analytical pyrolysis using hexamethyldisilazane (HMDS) for in situ derivatisation followed by gas chromatographic/mass spectrometric analysis (Pyrolysis-silylation-GC/MS) were used to investigate the hydrolysable and soluble constituents, and the polymerised macromolecules of an archaeological fig (Ficus carica) recovered in Zaragoza (Spain), as well as of modern figs. The main aim was to study the compositional alterations undergone by the fig tissues in a particular archaeological environment: the fig was in a vessel and covered by a layer of a mixture of orpiment and gypsum. A comparison between the GC/MS results from modern and archaeological figs revealed that degradative reactions took place, leading to the disappearance/depletion of reactive (unsaturated fatty acids) and sensitive compounds (phytosterols and triterpenes). Py-silylation-GC/MS data provided evidence of a significant degradation of the saccharide and lipid components of the fig tissue, which left a residue enriched in polyphenols and polyesters. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Pozo, Oscar J; Van Thuyne, Wim; Deventer, Koen; Van Eenoo, Peter; Delbeke, Frans T

    2008-03-01

    The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MS(n) experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples. Copyright (c) 2008 John Wiley & Sons, Ltd.

  2. Quantitation of dissolved gas content in emulsions and in blood using mass spectrometric detection

    Science.gov (United States)

    Grimley, Everett; Turner, Nicole; Newell, Clayton; Simpkins, Cuthbert; Rodriguez, Juan

    2011-01-01

    Quantitation of dissolved gases in blood or in other biological media is essential for understanding the dynamics of metabolic processes. Current detection techniques, while enabling rapid and convenient assessment of dissolved gases, provide only direct information on the partial pressure of gases dissolved in the aqueous fraction of the fluid. The more relevant quantity known as gas content, which refers to the total amount of the gas in all fractions of the sample, can be inferred from those partial pressures, but only indirectly through mathematical modeling. Here we describe a simple mass spectrometric technique for rapid and direct quantitation of gas content for a wide range of gases. The technique is based on a mass spectrometer detector that continuously monitors gases that are rapidly extracted from samples injected into a purge vessel. The accuracy and sample processing speed of the system is demonstrated with experiments that reproduce within minutes literature values for the solubility of various gases in water. The capability of the technique is further demonstrated through accurate determination of O2 content in a lipid emulsion and in whole blood, using as little as 20 μL of sample. The approach to gas content quantitation described here should greatly expand the range of animals and conditions that may be used in studies of metabolic gas exchange, and facilitate the development of artificial oxygen carriers and resuscitation fluids. PMID:21497566

  3. A compact apparatus for mass selective resonance ionization spectroscopy in a buffer gas cell

    Science.gov (United States)

    Backe, H.; Eberhardt, K.; Feldmann, R.; Hies, M.; Kunz, H.; Lauth, W.; Martin, R.; Schöpe, H.; Schwamb, P.; Sewtz, M.; Thörle, P.; Trautmann, N.; Zauner, S.

    An ultra-sensitive laser spectroscopic method for the investigation of transuranium nuclides has been developed based on resonance ionization in an argon buffer gas cell. This method has been combined with ion-guide extraction and mass selective direct detection of the resonantly ionized atoms. Using argon as a buffer gas, recoils of fusion reactions can be thermalized even at low pressure. The differential pumping system consists of only one roots pump and two turbo molecular pumps. The set-up has been tested with 243Am evaporated from a filament located inside the optical gas cell. Resonance ionization is performed using a two-step excitation with an excimer-dye-laser combination. The ions are transported by a suitable electrical field to the nozzle, and are ejected with the ion-guide gas jet into an electrostatic lens system followed by a quadrupole mass spectrometer and a channeltron detector. The total sensitivity has been measured to be 1.0 × 10 -4. The extraction time for ions based on electric field guidance amounts to 1.5 ms, which is two orders of magnitude faster than the ion-guide gas exchange time of this set-up.

  4. Gas Kinematics and the Black Hole Mass at the Center of the Radio Galaxy NGC 4335

    Science.gov (United States)

    Verdoes Kleijn, Gijs A.; van der Marel, Roeland P.; de Zeeuw, P. Tim; Noel-Storr, Jacob; Baum, Stefi A.

    2002-11-01

    We investigate the kinematics of the central gas disk of the radio-loud elliptical galaxy NGC 4335, derived from Hubble Space Telescope (HST) long-slit spectroscopic observations of Hα+[N II] along three parallel slit positions. The observed mean velocities are consistent with a rotating thin disk. We model the gas disk in the customary way, taking into account the combined potential of the galaxy and a putative black hole with mass M•, as well as the influence on the observed kinematics of the point-spread function and finite slit width. This sets a 3 σ upper limit of 108 Msolar on M•. The velocity dispersion at rintegral model of the stellar dynamics yields M•>~3×109 Msolar. However, there is reason to believe that this model overestimates M•. Reported correlations between black hole mass and inner stellar velocity dispersion σ predict M• to be >=5.4×108 Msolar in NGC 4335. If our standard thin disk modeling of the gas kinematics is valid, then NGC 4335 has an unusually low M• for its velocity dispersion. If, on the other hand, this approach is flawed and provides an underestimate of M•, then black hole masses for other galaxies derived from HST gas kinematics with the same assumptions should be treated with caution. In general, a precise determination of the M•-σ relation and its scatter will benefit from (1) joint measurements of M• from gas and stellar kinematics in the same galaxies and (2) a better understanding of the physical origin of the excess velocity dispersion commonly observed in nuclear gas disks of elliptical galaxies. Based on observations made with the NASA/ESA Hubble Space Telescope, obtained at the Space Telescope Science Institute, which is operated by the Association of Universities for Research in Astronomy, Inc., under NASA contract NAS 5-26555.

  5. Determination of interfering triazine degradation products by gas chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Magnuson, M L; Speth, T F; Kelty, C A

    2000-01-28

    Deethylatrazine (DEA), an atrazine degradation product, has been added to the US Environmental Protection Agency's Drinking Water Contaminant Candidate List (CCL). In its gas chromatographic analysis, DEA can coelute with deisopropylatrazine (DIA), another degradation product. The present work demonstrates that the coelution of DEA and DIA can induce a significant (up to approximately 50%) positive bias in the DEA determination, when using an ion-trap mass spectrometer as the detector. The DIA determination is unaffected by the coelution within experimental error. This may be explained in terms of gas-phase ion fragment populations. A correction factor to the observed DEA concentration may be developed based on the measured DIA concentration.

  6. Complex double-mass dynamic model of rotor on thrust foil gas dynamic bearings

    Science.gov (United States)

    Sytin, A.; Babin, A.; Vasin, S.

    2017-08-01

    The present paper considers simulation of a rotor’s dynamics behaviour on thrust foil gas dynamic bearings based on simultaneous solution of gas dynamics differential equations, equations of theory of elasticity, motion equations and some additional equations. A double-mass dynamic system was considered during the rotor’s motion simulation which allows not only evaluation of rotor’s dynamic behaviour, but also to evaluate the influence of operational and load parameters on the dynamics of the rotor-bearing system.

  7. Characterization of Volatile Compounds from Ethnic Agave Alcoholic Beverages by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Pilar Escalante-Minakata

    2008-01-01

    Full Text Available Ethnic Agave alcoholic beverages such as raicilla, sisal, tequila, mezcal, bacanora, sotol and pulque have been analyzed by gas chromatography and headspace solid-phase microextraction- gas chromatography-mass spectrometry (HS-SPME-GC-MS. There were 105 compounds identified, eleven were classified as major compounds and the others were classified as minor compounds. Seventeen minor compounds could be used as authenticity markers since they were beverage specific. Cluster analysis (CA showed that Agave alcoholic beverages could be distinguished by multivariate analysis of major compounds; however, the analysis of minor compounds provided a better fingerprinting.

  8. Microporous hollow fibre membrane modules as gas-liquid contactors. Part 1: Physical mass transfer processes. A specific application: mass transfer in highly viscous liquids

    OpenAIRE

    Kreulen, H.; Kreulen, H.; Versteeg, Geert; Smolders, C.A.; Smolders, C.A.; van Swaaij, Willibrordus Petrus Maria

    1993-01-01

    Gas-liquid mass transfer has been studied in a membrane module with non-wetted microporous fibres in the laminar flow regime. This new type of gas/liquid contactor can be operated stabily over a large range of gas and liquid flows because gas and liquid phase do not influence each other directly. Therefore foam is not formed in the module, gas bubbles are not entrained in the liquid flowing out of the reactor and the separation of both phases can be achieved very easily. These phenomena often...

  9. Gas-phase ion-molecule reactions and high-pressure mass spectrometer, 1

    International Nuclear Information System (INIS)

    Hiraoka, Kenzo

    1977-01-01

    The reasons for the fact that the research in gas-phase ion-molecule reactions, to which wide interest is shown, have greatly contributed to the physical and chemical fields are that, first it is essential in understanding general phenomena concerning ions, second, it can furnish many unique informations in the dynamics of chemical reactions, and third, usefulness of '' chemical ionization'' methods has been established as its application to chemical analysis. In this review, the history and trend of studies and equipments in gas-phase ion-molecule reactions are surveyed. The survey includes the chemical ionization mass spectrometer for simultaneously measuring the positive and negative ions utilizing a quadrupole mass spectrometer presented by Hunt and others, flowing afterglow method derived from the flowing method which traces neutral chemical species mainly optically, ion cyclotron resonance mass spectrometer, trapped ion mass spectrometer and others. Number of reports referred to ion-molecule reactions issued during the last one year well exceeds the total number of reports concerning mass spectrometers presented before 1955. This truly shows how active the research and development are in this field. (Wakatsuki, Y.)

  10. Gas chromatography/mass spectrometry characterization of historical varnishes of ancient Italian lutes and violin.

    Science.gov (United States)

    Echard, J P; Benoit, C; Peris-Vicente, J; Malecki, V; Gimeno-Adelantado, J V; Vaiedelich, S

    2007-02-12

    The organic constituents of historical vanishes from two ancient Italian lutes and a Stradivari violin, kept in the Musée de la musique in Paris, have been characterized using gas chromatography-mass spectrometry. Results have been compared with the chromatograms and mass spectra of recent as well as old naturally aged reference materials. The three historical varnishes analyzed have been shown to be oil varnishes, probably mixtures of linseed oil with resins. Identification of diterpenoids and triterpenoids compounds, and of the resins that may have been ingredients of the varnishes, are discussed in this paper.

  11. Cooling system having reduced mass pin fins for components in a gas turbine engine

    Science.gov (United States)

    Lee, Ching-Pang; Jiang, Nan; Marra, John J

    2014-03-11

    A cooling system having one or more pin fins with reduced mass for a gas turbine engine is disclosed. The cooling system may include one or more first surfaces defining at least a portion of the cooling system. The pin fin may extend from the surface defining the cooling system and may have a noncircular cross-section taken generally parallel to the surface and at least part of an outer surface of the cross-section forms at least a quartercircle. A downstream side of the pin fin may have a cavity to reduce mass, thereby creating a more efficient turbine airfoil.

  12. Determination of Alkyl Methanesulfonates in Doxazosin Mesylate by Gas Chromatography-mass Spectrometer.

    Science.gov (United States)

    Sitaram, C; Rupakula, R B; Reddy, B N; Sastry, C S P

    2011-01-01

    High sensitive rapid gas chromatography-mass spectrometry method for the determination of four carcinogenic alkyl methanesulfonates viz. methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate in doxazosin mesylate has been presented by using selective ion monitoring mode. The optimum separation was achieved between methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate on a DB-5 (30 m×0.32 mm×1.0 μm) capillary column under programming temperature. Acetonitrile, water and ammonia (90:9:1 v/v/v) mixture was used as diluent. Various factors involved in the gas chromatography-mass spectrometry method development are also presented. This method was validated as per International Conference on Harmonization guidelines. The limit of quantitation of methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate is 6 ppm with respect to 30 mg/ml of doxazosin mesylate.

  13. Mass-independent oxygen isotopic partitioning during gas-phase SiO2 formation.

    Science.gov (United States)

    Chakraborty, Subrata; Yanchulova, Petia; Thiemens, Mark H

    2013-10-25

    Meteorites contain a wide range of oxygen isotopic compositions that are interpreted as heterogeneity in solar nebula. The anomalous oxygen isotopic compositions of refractory mineral phases may reflect a chemical fractionation process in the nebula, but there are no experiments to demonstrate this isotope effect during particle formation through gas-phase reactions. We report experimental results of gas-to-particle conversion during oxidation of silicon monoxide that define a mass-independent line (slope one) in oxygen three-isotope space of (18)O/(16)O versus (17)O/(16)O. This mass-independent chemical reaction is a potentially initiating step in nebular meteorite formation, which would be capable of producing silicate reservoirs with anomalous oxygen isotopic compositions.

  14. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which was quant......A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... from 98 to 107%, demonstrating the suitability of the method for measuring ketone bodies over a wide concentration range. The method has been applied to cases in which ketoacidosis was suspected as the cause of death in diabetics or chronic alcoholics, as well as to cases in which another cause...

  15. Total molecular gas masses of Planck - Herschel selected strongly lensed hyper luminous infrared galaxies

    Science.gov (United States)

    Harrington, K. C.; Yun, M. S.; Magnelli, B.; Frayer, D. T.; Karim, A.; Weiß, A.; Riechers, D.; Jiménez-Andrade, E. F.; Berman, D.; Lowenthal, J.; Bertoldi, F.

    2018-03-01

    We report the detection of CO(1-0) line emission from seven Planck and Herschel selected hyper luminous ({L_{IR (8-1000{μ m})} > 10^{13} L_{⊙}) infrared galaxies with the Green Bank Telescope (GBT). CO(1-0) measurements are a vital tool to trace the bulk molecular gas mass across all redshifts. Our results place tight constraints on the total gas content of these most apparently luminous high-z star-forming galaxies (apparent IR luminosities of LIR > 1013 - 14 L⊙), while we confirm their predetermined redshifts measured using the Large Millimeter Telescope, LMT (zCO = 1.33-3.26). The CO(1-0) lines show similar profiles as compared to Jup = 2-4 transitions previously observed with the LMT. We report enhanced infrared to CO line luminosity ratios of = 110 ± 22 L_{⊙} (K km s^{-1} pc^{-2})^{-1} compared to normal star-forming galaxies, yet similar to those of well-studied IR-luminous galaxies at high-z. We find average brightness temperature ratios of 〈 r21〉 = 0.93 (2 sources), 〈 r31〉 = 0.34 (5 sources), and 〈 r41〉 = 0.18 (1 source). The r31 and r41 values are roughly half the average values for SMGs. We estimate the total gas mass content as {μ M_{H2} = (0.9-27.2) × 10^{11} (α _CO/0.8) M_{⊙}, where μ is the magnification factor and αCO is the CO line luminosity to molecular hydrogen gas mass conversion factor. The rapid gas depletion times, = 80} Myr, reveal vigorous starburst activity, and contrast the Gyr depletion time-scales observed in local, normal star-forming galaxies.

  16. Photoluminescence Spectroscopy of Mass-Selected Electrosprayed Ions Embedded in Cryogenic Rare-Gas Matrixes.

    Science.gov (United States)

    Kern, Bastian; Greisch, Jean-François; Strelnikov, Dmitry; Weis, Patrick; Böttcher, Artur; Ruben, Mario; Schäfer, Bernhard; Schooss, Detlef; Kappes, Manfred M

    2015-12-01

    An apparatus is presented which combines nanoelectrospray ionization for isolation of large molecular ions from solution, mass-to-charge ratio selection in gas-phase, low-energy-ion-beam deposition into a (co-condensed) inert gas matrix and UV laser-induced visible-region photoluminescence (PL) of the matrix isolated ions. Performance is tested by depositing three different types of lanthanoid diketonate cations including also a dissociation product species not directly accessible by chemical synthesis. For these strongly photoluminescent ions, accumulation of some femto- to picomoles in a neon matrix (over a time scale of tens of minutes to several hours) is sufficient to obtain well-resolved dispersed emission spectra. We have ruled out contributions to these spectra due to charge neutralization or fragmentation during deposition by also acquiring photoluminescence spectra of the same ionic species in the gas phase.

  17. Chemotaxonomic Characterization of Microorganisms by Capillary Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    1988-06-01

    indirectly detecting differences in carbohydrate composition ( Lancefield grouping ). The group B-specific polysaccharide consists of a backbcne of...carbohydrate pyrolysis product generated from the glucitol moiety. We have further used pattern recognition to differentiate several Lancefield groups of... Group A and Group B Streptococci by Pyrolysis Gas Chromatography- Mass Spectrometry," A- alytical Chemistry, 59, 1410-1413 (1987). S. L. Morgan, M. D

  18. Carbohydrate analysis of hemicelluloses by gas chromatography-mass spectrometry of acteylated methyl glycosides

    DEFF Research Database (Denmark)

    Sárossy, Zsuzsa; Plackett, David; Egsgaard, Helge

    2012-01-01

    A method based on gas chromatography–mass spectrometry analysis of acetylated methyl glycosides was developed in order to analyze monosaccharides obtained from various hemicelluloses. The derivatives of monosaccharide standards, arabinose, glucose, and xylose were studied in detail and 13C-labele......-labeled analogues were used for identification and quantitative analysis. Excellent chromatographic separation of the monosaccharide derivatives was found and identification of the anomeric configuration was feasible through a prepared and identified pure methyl 2,3,4,6-tetra...

  19. Determination of Alkyl Methanesulfonates in Doxazosin Mesylate by Gas Chromatography-mass Spectrometer

    OpenAIRE

    Sitaram, C.; Rupakula, R. B.; Reddy, B. N.; Sastry, C. S. P

    2011-01-01

    High sensitive rapid gas chromatography-mass spectrometry method for the determination of four carcinogenic alkyl methanesulfonates viz. methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate in doxazosin mesylate has been presented by using selective ion monitoring mode. The optimum separation was achieved between methyl methanesulfonate, ethyl methanesulfonate, isopropyl methanesulfonate and n-butyl methanesulfonate on a DB-5 (30 m×0.32 mm×1...

  20. Determination of Carboxypeptidase Activity in Clinical Pathogens by Gas Chromatography?Mass Spectrometry

    OpenAIRE

    Lough, Fraser; Perry, John D.; Stanforth, Stephen P.; Dean, John R.

    2016-01-01

    ABSTRACT A novel method for the determination of benzoic acid has been employed to identify carboxypeptidase activities in clinically relevant pathogens. Benzoic acid was determined after chemical derivatization by gas chromatography?mass spectrometry (GC?MS). N-Benzoyl amino acid substrates were evaluated for the detection of carboxypeptidase activities in a number of clinical pathogens. Upon enzymatic hydrolysis of these substrates, benzoic acid was produced which was detected by extraction...

  1. Weighing Galaxy Clusters with Gas. I. On the Methods of Computing Hydrostatic Mass Bias

    OpenAIRE

    Lau, Erwin T.; Nagai, Daisuke; Nelson, Kaylea

    2013-01-01

    Mass estimates of galaxy clusters from X-ray and Sunyeav-Zel'dovich observations assume the intracluster gas is in hydrostatic equilibrium with their gravitational potential. However, since galaxy clusters are dynamically active objects whose dynamical states can deviate significantly from the equilibrium configuration, the departure from the hydrostatic equilibrium assumption is one of the largest sources of systematic uncertainties in cluster cosmology. In the literature there has been two ...

  2. Identification of bound alcohols in soil humic acids by gas chromatography-mass spectrometry

    OpenAIRE

    Berthier , Gersende; Dou , Sen; Peakman , Torren; Lichtfouse , Eric

    2000-01-01

    International audience; Humic acids are complex, partly macromolecular, yellow-brownish substances occurring in soils, waters and sediments. In order to shed some light on their molecular structure, crop humic acids were cleaved by alkaline hydrolysis (KOH). The products were fractionated by thin layer chromatography to give mono-alcohols which were analysed as acetate derivatives by gas chromatography coupled to mass spectrometry. Linear alcohols, sterols, stanols and plant-derived triterpen...

  3. Humidity independent mass spectrometry for gas phase chemical analysis via ambient proton transfer reaction.

    Science.gov (United States)

    Zhu, Hongying; Huang, Guangming

    2015-03-31

    In this work, a humidity independent mass spectrometric method was developed for rapid analysis of gas phase chemicals. This method is based upon ambient proton transfer reaction between gas phase chemicals and charged water droplets, in a reaction chamber with nearly saturate humidity under atmospheric pressure. The humidity independent nature enables direct and rapid analysis of raw gas phase samples, avoiding time- and sample-consuming sample pretreatments in conventional mass spectrometry methods to control sample humidity. Acetone, benzene, toluene, ethylbenzene and meta-xylene were used to evaluate the analytical performance of present method. The limits of detection for benzene, toluene, ethylbenzene and meta-xylene are in the range of ∼0.1 to ∼0.3 ppbV; that of benzene is well below the present European Union permissible exposure limit for benzene vapor (5 μg m(-3), ∼1.44 ppbV), with linear ranges of approximately two orders of magnitude. The majority of the homemade device contains a stainless steel tube as reaction chamber and an ultrasonic humidifier as the source of charged water droplets, which makes this cheap device easy to assemble and facile to operate. In addition, potential application of this method was illustrated by the real time identification of raw gas phase chemicals released from plants at different physiological stages. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Theoretical studies on membrane-based gas separation using computational fluid dynamics (CFD) of mass transfer

    International Nuclear Information System (INIS)

    Sohrabi, M.R.; Marjani, A.; Davallo, M.; Moradi, S.; Shirazian, S.

    2011-01-01

    A 2D mass transfer model was developed to study carbon dioxide removal by absorption in membrane contactors. The model predicts the steady state absorbent and carbon dioxide concentrations in the membrane by solving the conservation equations. The continuity equations for three sub domains of the membrane contactor involving the tube; membrane and shell were obtained and solved by finite element method (FEM). The model was based on 'non-wetted mode' in which the gas phase filled the membrane pores. Laminar parabolic velocity profile was used for the liquid flow in the tube side; whereas, the gas flow in the shell side was characterized by Happel's free surface model. Axial and radial diffusion transport inside the shell, through the membrane, and within the tube side of the contactor was considered in the mass transfer model. The predictions of percent CO/sub 2/ removal obtained by modeling were compared with the experimental values obtained from literature. They were the experimental results for CO/sub 2/ removal from CO/sub 2//N/sub 2/ gas mixture with amines aqueous solutions as the liquid solvent using polypropylene membrane contactor. The modeling predictions were in good agreement with the experimental values for different values of gas and liquid flow rates. (author)

  5. Chemometrics comparison of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry Daphnia magna metabolic profiles exposed to salinity.

    Science.gov (United States)

    Parastar, Hadi; Garreta-Lara, Elba; Campos, Bruno; Barata, Carlos; Lacorte, Silvia; Tauler, Roma

    2018-02-27

    The performances of gas chromatography with mass spectrometry and of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry are examined through the comparison of Daphnia magna metabolic profiles. Gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with mass spectrometry were used to compare the concentration changes of metabolites under saline conditions. In this regard, a chemometric strategy based on wavelet compression and multivariate curve resolution-alternating least squares is used to compare the performances of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry for the untargeted metabolic profiling of Daphnia magna in control and salinity-exposed samples. Examination of the results confirmed the outperformance of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry over gas chromatography with mass spectrometry for the detection of metabolites in D. magna samples. The peak areas of multivariate curve resolution-alternating least squares resolved elution profiles in every sample analyzed by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry were arranged in a new data matrix that was then modeled by partial least squares discriminant analysis. The control and salt-exposed daphnids samples were discriminated and the most relevant metabolites were estimated using variable importance in projection and selectivity ratio values. Salinity de-regulated 18 metabolites from metabolic pathways involved in protein translation, transmembrane cell transport, carbon metabolism, secondary metabolism, glycolysis, and osmoregulation. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. The gas-liquid mass transfer coefficient (k(L)a) in the gas-liquid Multi-stage Agitated Contactor (MAC)

    NARCIS (Netherlands)

    Breman, B.B; Beenackers, A.A C M; Bouma, M.J; VanderWerf, M.H.

    1996-01-01

    Data on the volumetric liquid-side gas-liquid mass transfer coefficient, k(L)a, in a Multi-stage Agitated Contractor (MAC) are reported for three gas-liquid systems (air-water, helium-n-octane, and air-Monoethylene Glycol (MEG)). k(L)a (s(-1)) was determined using a dynamic method with moderately

  7. Mass flow discharge and total temperature characterisation of a pyrotechnic gas generator formulation for airbag systems

    Energy Technology Data Exchange (ETDEWEB)

    Neutz, Jochen; Koenig, Andreas [Fraunhofer Institut fuer Chemische Technologie ICT, Pfinztal (Germany); Knauss, Helmut; Jordan, Sebastian; Roediger, Tim; Smorodsky, Boris [Universitaet Stuttgart (Germany). Institut fuer Aerodynamik und Gasdynamik; Bluemcke, Erich Walter [AUDI AG, Department I/EK-523, Ingolstadt (Germany)

    2009-06-15

    The mass flow characteristics of gas generators for airbag applications have to comply with a number of requirements for an optimal deployment of the airbag itself. Up to now, the mass flow was determined from pressure time histories of so-called can tests. This procedure suffers from the missing knowledge on the temperature of the generated gas entering the can. A new test setup described in this paper could overcome this problem by providing highly time resolved information on the gas's total temperature and the mass flow of the generator. The test setup consisted of a combustion chamber with a specially designed Laval nozzle in combination with a temperature sensor of high time resolution. The results showed a high time resolved temperature signal, which was disturbed by the formation of a slag layer on the sensor. Plausibility considerations with experimentally and thermodynamically determined combustion temperatures led to satisfying results for the overall temperature as characteristic parameter of airbag inflating gases flows from pyrotechnics. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  8. Gravitational fragmentation in turbulent primordial gas and the initial mass function of Population III stars

    Energy Technology Data Exchange (ETDEWEB)

    Clark, Paul C.; /ZAH, Heidelberg; Glover, Simon C.O.; /ZAH, Heidelberg; Klessen, Ralf S.; /ZAH, Heidelberg /KIPAC, Menlo Park; Bromm, Volker; /Texas U., Astron. Dept.

    2010-08-25

    We report results from numerical simulations of star formation in the early universe that focus on the dynamical behavior of metal-free gas under different initial and environmental conditions. In particular we investigate the role of turbulence, which is thought to ubiquitously accompany the collapse of high-redshift halos. We distinguish between two main cases: the birth of Population III.1 stars - those which form in the pristine halos unaffected by prior star formation - and the formation of Population III.2 stars - those forming in halos where the gas is still metal free but has an increased ionization fraction. This latter case can arise either from exposure to the intense UV radiation of stellar sources in neighboring halos, or from the high virial temperatures associated with the formation of massive halos, that is, those with masses greater than {approx} 10{sup 8} M{sub {circle_dot}}. We find that turbulent primordial gas is highly susceptible to fragmentation in both cases, even for turbulence in the subsonic regime, i.e. for rms velocity dispersions as low as 20 % of the sound speed. Contrary to our original expectations, fragmentation is more vigorous and more widespread in pristine halos compared to pre-ionized ones. We therefore predict Pop III.1 stars to be on average of somewhat lower mass, and form in larger groups, than Pop III.2 stars. We find that fragment masses cover over two orders of magnitude, indicating that the resulting Population III initial mass function was significantly extended in mass as well. Our results suggest that the details of the fragmentation process depend on the local properties of the turbulent velocity field and hence we expect considerable variations in the resulting stellar mass spectrum in different halos. In particular, the lowest-mass objects in our sample should have survived to the present day and could potentially provide a unique record of the physical conditions of stellar birth in the primordial universe

  9. WEIGHING GALAXY CLUSTERS WITH GAS. I. ON THE METHODS OF COMPUTING HYDROSTATIC MASS BIAS

    Energy Technology Data Exchange (ETDEWEB)

    Lau, Erwin T.; Nagai, Daisuke [Department of Physics, Yale University, New Haven, CT 06520 (United States); Nelson, Kaylea, E-mail: erwin.lau@yale.edu [Department of Astronomy, Yale University, New Haven, CT 06520 (United States)

    2013-11-10

    Mass estimates of galaxy clusters from X-ray and Sunyeav-Zel'dovich observations assume the intracluster gas is in hydrostatic equilibrium with their gravitational potential. However, since galaxy clusters are dynamically active objects whose dynamical states can deviate significantly from the equilibrium configuration, the departure from the hydrostatic equilibrium assumption is one of the largest sources of systematic uncertainties in cluster cosmology. In the literature there have been two methods for computing the hydrostatic mass bias based on the Euler and the modified Jeans equations, respectively, and there has been some confusion about the validity of these two methods. The word 'Jeans' was a misnomer, which incorrectly implies that the gas is collisionless. To avoid further confusion, we instead refer these methods as 'summation' and 'averaging' methods respectively. In this work, we show that these two methods for computing the hydrostatic mass bias are equivalent by demonstrating that the equation used in the second method can be derived from taking spatial averages of the Euler equation. Specifically, we identify the correspondences of individual terms in these two methods mathematically and show that these correspondences are valid to within a few percent level using hydrodynamical simulations of galaxy cluster formation. In addition, we compute the mass bias associated with the acceleration of gas and show that its contribution is small in the virialized regions in the interior of galaxy clusters, but becomes non-negligible in the outskirts of massive galaxy clusters. We discuss future prospects of understanding and characterizing biases in the mass estimate of galaxy clusters using both hydrodynamical simulations and observations and their implications for cluster cosmology.

  10. Weighing galaxy clusters with gas. II. On the origin of hydrostatic mass bias in ΛCDM galaxy clusters

    Energy Technology Data Exchange (ETDEWEB)

    Nelson, Kaylea; Nagai, Daisuke; Yu, Liang [Department of Astronomy, Yale University, New Haven, CT 06520 (United States); Lau, Erwin T.; Rudd, Douglas H., E-mail: kaylea.nelson@yale.edu [Department of Physics, Yale University, New Haven, CT 06520 (United States)

    2014-02-20

    The use of galaxy clusters as cosmological probes hinges on our ability to measure their masses accurately and with high precision. Hydrostatic mass is one of the most common methods for estimating the masses of individual galaxy clusters, which suffer from biases due to departures from hydrostatic equilibrium. Using a large, mass-limited sample of massive galaxy clusters from a high-resolution hydrodynamical cosmological simulation, in this work we show that in addition to turbulent and bulk gas velocities, acceleration of gas introduces biases in the hydrostatic mass estimate of galaxy clusters. In unrelaxed clusters, the acceleration bias is comparable to the bias due to non-thermal pressure associated with merger-induced turbulent and bulk gas motions. In relaxed clusters, the mean mass bias due to acceleration is small (≲ 3%), but the scatter in the mass bias can be reduced by accounting for gas acceleration. Additionally, this acceleration bias is greater in the outskirts of higher redshift clusters where mergers are more frequent and clusters are accreting more rapidly. Since gas acceleration cannot be observed directly, it introduces an irreducible bias for hydrostatic mass estimates. This acceleration bias places limits on how well we can recover cluster masses from future X-ray and microwave observations. We discuss implications for cluster mass estimates based on X-ray, Sunyaev-Zel'dovich effect, and gravitational lensing observations and their impact on cluster cosmology.

  11. Linking high resolution mass spectrometry data with exposure ...

    Science.gov (United States)

    There is a growing need in the field of exposure science for monitoring methods that rapidly screen environmental media for suspect contaminants. Measurement and analysis platforms, based on high resolution mass spectrometry (HRMS), now exist to meet this need. Here we describe results of a study that links HRMS data with exposure predictions from the U.S. EPA's ExpoCast™ program and in vitro bioassay data from the U.S. interagency Tox21 consortium. Vacuum dust samples were collected from 56 households across the U.S. as part of the American Healthy Homes Survey (AHHS). Sample extracts were analyzed using liquid chromatography time-of-flight mass spectrometry (LC–TOF/MS) with electrospray ionization. On average, approximately 2000 molecular features were identified per sample (based on accurate mass) in negative ion mode, and 3000 in positive ion mode. Exact mass, isotope distribution, and isotope spacing were used to match molecular features with a unique listing of chemical formulas extracted from EPA's Distributed Structure-Searchable Toxicity (DSSTox) database. A total of 978 DSSTox formulas were consistent with the dust LC–TOF/molecular feature data (match score ≥ 90); these formulas mapped to 3228 possible chemicals in the database. Correct assignment of a unique chemical to a given formula required additional validation steps. Each suspect chemical was prioritized for follow-up confirmation using abundance and detection frequency results, along wi

  12. Large-scale correlations in gas traced by Mg II absorbers around low-mass galaxies

    Science.gov (United States)

    Kauffmann, Guinevere

    2018-03-01

    The physical origin of the large-scale conformity in the colours and specific star formation rates of isolated low-mass central galaxies and their neighbours on scales in excess of 1 Mpc is still under debate. One possible scenario is that gas is heated over large scales by feedback from active galactic nuclei (AGNs), leading to coherent modulation of cooling and star formation between well-separated galaxies. In this Letter, the metal line absorption catalogue of Zhu & Ménard is used to probe gas out to large projected radii around a sample of a million galaxies with stellar masses ˜1010M⊙ and photometric redshifts in the range 0.4 effective volume of 2.2 Gpc3. A statistically significant excess of Mg II absorbers is present around the red-low-mass galaxies compared to their blue counterparts out to projected radii of 10 Mpc. In addition, the equivalent width distribution function of Mg II absorbers around low-mass galaxies is shown to be strongly affected by the presence of a nearby (Rp < 2 Mpc) radio-loud AGNs out to projected radii of 5 Mpc.

  13. Development of gas analyzer to aim for speed and high sensitivity and shaping of mass spectrum

    International Nuclear Information System (INIS)

    Hatano, Toshihisa; Hiratsuka, Hajime; Abe, Tetsuya

    2011-01-01

    The gas analysis system with EI-QMS (Electron Ionization-Quadrupole Mass Spectrometer) developed by Japan Atomic Energy Agency (JAEA) is commercially available from a private company through a technology transfer. The system has already been used to a medical field such as breath analysis, a quality control of automobile casting parts made of recycled aluminum, and a measurement of food aromatic elements emitting from vegetable and sake. A pulse gas sampling and a continuous evacuation were integrated to the system that aimed at obtaining high sensitive and stable mass spectrum and accomplishing fast measurement prepared for 100% inspection of industrial parts and various foods. As a result, the system achieved a background pressure of 10 -7 Pa and a background ion current of 10 -13 A in the normal condition. An intensity of the mass spectrum decreased linearly with decreasing the pressure by the continuous evacuation, therefore, the intensity of the mass spectrum was corrected by the pump down curve, which is a new mathematical approach equivalent to a constant pressure curve. It was confirmed that the system had the sensing performance of 100 ppb. (author)

  14. Characterization of the fermentation process by gas chromatography Lasiodiplodia theobromae and gas chromatography coupled with mass spectrometry

    International Nuclear Information System (INIS)

    Castillo Portela, Grolamys; Eng Sanchez, Felipe; Nogueiras Lima, Clara

    2014-01-01

    Lasiodiplodia theobromae is a fungus, which has been reported by some authors as a high yield producer of the phytohormone jasmonic acid (JA). An indigenous strain of this fungus has been used for producing a fermentation broth with a high JA concentration by the Cuban Research Institute for Sugar Cane Derivatives (ICIDCA), registered as BIOJAS. The broth has been applied to some agricultural crops and demonstrated its economic feasibility as plant growth regulator and biological control of various phytopathogenic microorganisms and pests. Both fermentation broth and biomass from this fungus contain some other metabolites having bioactive properties, for instance, fatty acids. This paper shows the composition and quantification of fatty acids in the biomass using Gas Chromatography (GC) and the identification of substances profile in fermentation broth by Gas Chromatography coupled to Mass Spectrometry (GC-MS). The most fatty acids in the biomass are palmitic, stearic, oleic, linoleic and linolenic acids, being oleic acid the major component. On the other hand, 2,32 % of fatty acid esters; 2,47 % of alkenes; 14,40 % of alcohols; 30,15 % of aldehydes and 21,73 % of paraffins were detected in the composition of fermentation broth

  15. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

  16. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  17. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  18. Pebble-isolation mass: Scaling law and implications for the formation of super-Earths and gas giants

    Science.gov (United States)

    Bitsch, Bertram; Morbidelli, Alessandro; Johansen, Anders; Lega, Elena; Lambrechts, Michiel; Crida, Aurélien

    2018-04-01

    The growth of a planetary core by pebble accretion stops at the so-called pebble isolation mass, when the core generates a pressure bump that traps drifting pebbles outside its orbit. The value of the pebble isolation mass is crucial in determining the final planet mass. If the isolation mass is very low, gas accretion is protracted and the planet remains at a few Earth masses with a mainly solid composition. For higher values of the pebble isolation mass, the planet might be able to accrete gas from the protoplanetary disc and grow into a gas giant. Previous works have determined a scaling of the pebble isolation mass with cube of the disc aspect ratio. Here, we expand on previous measurements and explore the dependency of the pebble isolation mass on all relevant parameters of the protoplanetary disc. We use 3D hydrodynamical simulations to measure the pebble isolation mass and derive a simple scaling law that captures the dependence on the local disc structure and the turbulent viscosity parameter α. We find that small pebbles, coupled to the gas, with Stokes number τf < 0.005 can drift through the partial gap at pebble isolation mass. However, as the planetary mass increases, particles must be decreasingly smaller to penetrate the pressure bump. Turbulent diffusion of particles, however, can lead to an increase of the pebble isolation mass by a factor of two, depending on the strength of the background viscosity and on the pebble size. We finally explore the implications of the new scaling law of the pebble isolation mass on the formation of planetary systems by numerically integrating the growth and migration pathways of planets in evolving protoplanetary discs. Compared to models neglecting the dependence of the pebble isolation mass on the α-viscosity, our models including this effect result in higher core masses for giant planets. These higher core masses are more similar to the core masses of the giant planets in the solar system.

  19. [Feasibility investigation of hydrogen instead of helium as carrier gas in the determination of five organophosphorus pesticides by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Liu, Zhenxue; Zhou, Shixue

    2015-01-01

    Helium is almost the only choosable carrier gas used in gas chromatography-mass spectrometry (GC-MS). A mixed standard solution of five organophosphorus pesticides was analyzed by using GC-MS, and hydrogen or helium as carrier gas, so as to study the feasibility of hydrogen instead of helium as carrier gas for the determination of organophosphorus pesticides. Combining a mass spectrum database built by ourselves, the results were deconvolved and identified by Automated Mass Spectral Deconvolution & Identification System (AMDIS32), a software belonging to the workstation of the instrument. Then, the statistical software, IBM SPSS Statistics 19.0 was used for the clustering analysis of the data. The results indicated that when hydrogen was used as carrier gas, the peaks of the pesticides detected were slightly earlier than those when helium used as carrier gas, but the resolutions of the chromatographic peaks were lower, and the fraction good indices (Frac. Good) were lower, too. When hydrogen was used as carrier gas, the signals of the pesticides were unstable, the measuring accuracies of the pesticides were reduced too, and even more, some compounds were undetectable. Therefore, considering the measuring accuracy, the signal stability, and the safety, etc., hydrogen should be cautiously used as carrier gas in the determination of organophosphorus pesticides by GC-MS.

  20. Determination of gas & liquid two-phase flow regime transitions in wellbore annulus by virtual mass force coefficient when gas cut

    Science.gov (United States)

    Qu, Junbo; Yan, Tie; Sun, Xiaofeng; Chen, Ye; Pan, Yi

    2017-10-01

    With the development of drilling technology to deeper stratum, overflowing especially gas cut occurs frequently, and then flow regime in wellbore annulus is from the original drilling fluid single-phase flow into gas & liquid two-phase flow. By using averaged two-fluid model equations and the basic principle of fluid mechanics to establish the continuity equations and momentum conservation equations of gas phase & liquid phase respectively. Relationship between pressure and density of gas & liquid was introduced to obtain hyperbolic equation, and get the expression of the dimensionless eigenvalue of the equation by using the characteristic line method, and analyze wellbore flow regime to get the critical gas content under different virtual mass force coefficients. Results show that the range of equation eigenvalues is getting smaller and smaller with the increase of gas content. When gas content reaches the critical point, the dimensionless eigenvalue of equation has no real solution, and the wellbore flow regime changed from bubble flow to bomb flow. When virtual mass force coefficients are 0.50, 0.60, 0.70 and 0.80 respectively, the critical gas contents are 0.32, 0.34, 0.37 and 0.39 respectively. The higher the coefficient of virtual mass force, the higher gas content in wellbore corresponding to the critical point of transition flow regime, which is in good agreement with previous experimental results. Therefore, it is possible to determine whether there is a real solution of the dimensionless eigenvalue of equation by virtual mass force coefficient and wellbore gas content, from which we can obtain the critical condition of wellbore flow regime transformation. It can provide theoretical support for the accurate judgment of the annular flow regime.

  1. The ratio of CO to total gas mass in high-redshift galaxies

    Science.gov (United States)

    Mashian, Natalie; Sternberg, Amiel; Loeb, Abraham

    2013-11-01

    Walter et al. have recently identified the J = 6 - 5, 5 - 4, and 2 - 1 CO rotational emission lines, and [C II] fine-structure emission line from the star-forming interstellar medium (ISM) in the high-redshift submillimetre source HDF 850.1, at z = 5.183. We employ large velocity gradient (LVG) modelling to analyse the spectra of this source assuming the [C II] and CO emissions originate from (i) separate virialized regions, (ii) separate unvirialized regions, (iii) uniformly mixed virialized regions and (iv) uniformly mixed unvirialized regions. We present the best-fitting set of parameters, including for each case the ratio α between the total hydrogen/helium gas mass and the CO(1-0) line luminosity. We also present computations of the ratio of H2 mass to [C II] line luminosity for optically thin conditions, for a range of gas temperatures and densities, for direct conversion of [C II] line luminosities to `CO-dark' H2 masses. For HDF 850.1 we find that a model in which the CO and C+ are uniformly mixed in gas that is shielded from ultraviolet radiation requires a cosmic ray or X-ray ionization rate of ζ ≈ 3 × 10-14 s-1, plausibly consistent with the large star formation rate (˜103 M⊙ yr-1) observed in this source. Enforcing the cosmological constraint posed by the abundance of dark matter haloes in the standard Λ cold dark matter (ΛCDM) cosmology and taking into account other possible contributions to the total gas mass, we find that the two models in which the virialization condition is enforced can be ruled out at the ≳2σ level, while the model assuming mixed unvirialized regions is less likely. We conclude that modelling HDF 850.1's ISM as a collection of unvirialized molecular clouds with distinct CO and C+ layers, for which α = 1.2 M⊙ (K km s-1 pc2)-1 for the CO to H2 mass-to-luminosity ratio (similar to the standard ultraluminous infrared galaxy value), is most consistent with the ΛCDM cosmology.

  2. Microporous hollow fibre membrane modules as gas-liquid contactors. Part 1. Physical mass transfer processes: A specific application

    OpenAIRE

    Kreulen, H.; Versteeg, G.F.; Swaaij, W.P.M. van

    1993-01-01

    Gas-liquid mass transfer has been studied in a membrane module with non-wetted microporous fibres in the laminar flow regime. This new type of gas/liquid contactor can be operated stabily over a large range of gas and liquid flows because gas and liquid phase do not influence each other directly. Therefore foam is not formed in the module, gas bubbles are not entrained in the liquid flowing out of the reactor and the separation of both phases can be achieved very easily. These phenomena often...

  3. Differentiation of endogenous and exogenous steroids by gas chromatography-combustion-mass spectrometry isotope ratio

    International Nuclear Information System (INIS)

    Montes de Oca Porto, Rodny; Rosado Perez, Aristides; Correa Vidal, Margarita Teresa

    2007-01-01

    Urinary steroids profiles are used to control the misuse of endogenous steroids such as testosterone and dihydrotestosterone. The testosterone/epistestosterone ratio, measured by Gas Chromatography-Mass Spectrometry, is used to control testosterone administration. When T/E ratio is higher than 4, consumption of testosterone or its precursors is suspected. Recent researches have demonstrated the effectiveness of Carbon Isotope Ratio Mass Spectrometry to detect and confirm endogenous steroids administration. The ratio of the two stable carbon isotopes 1 3 C and 1 2 C allows the differentiation of natural and synthetic steroids because synthetic steroids have lower 1 3 C abundance. In fact, the carbon isotope ratios can be used to determine endogenous steroids administration even when testosterone/epistestosterone ratio is at its normal value. In the current work, some of the most important aspects related to differentiation of endogenous and exogenous steroids by means of Gas Chromatography-Combustion-Isotope Ratio Mass Spectrometry are discussed. Also, this article provides a review about the purification and sample preparation previous to the analysis, and diet effects on carbon isotope ratio of endogenous anabolics steroids is presented too

  4. Light-induced heat and mass transfer in a single-component gas in a capillary

    International Nuclear Information System (INIS)

    Chermyaninov, I. V.; Chernyak, V. G.; Vilisova, E. A.

    2007-01-01

    A theoretical analysis is presented of light-induced heat and mass transfer in a single-component gas in a capillary tube at arbitrary Knudsen numbers. Surface and collisional mechanisms of transfer are analyzed, due to differences in accommodation coefficient and collision cross section between excited-and ground-state particles, respectively. Analytical expressions for kinetic coefficients characterizing the gas drift and heat transfer in a capillary tube are obtained in the limits of low and high Knudsen numbers. Numerical computations are performed for intermediate Knudsen numbers. Both drift and heat fluxes are determined as functions of the light beam frequency. In the case of an inhomogeneously broadened absorption line, the light-induced fluxes are found to depend not only on the sign, but also on the amount, of light beam detuning from the absorption line center frequency

  5. Ring positional differentiation of isomeric N-alkylated fluorocathinones by gas chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Westphal, Folker; Junge, Thomas

    2012-11-30

    In analogy to our previously published procedure for the differentiation of regioisomeric fluoroamphetamines a method was developed, to differentiate ring positional isomeric fluorocathinones by product ion spectrometry of ions generated by chemical ionization (CI) under GC-MS conditions using methane as reagent gas. N-alkylated ortho-, meta- and para-fluorocathinones could be unequivocally differentiated by product ion spectrometry of the hydrogen fluoride loss ions [M+H-HF](+) using a triple quadrupole mass spectrometer with argon as collision gas under normalized collision conditions. This method enables the differentiation of ring positional isomers of fluorocathinones even in complex mixtures and low concentrations. The applicability of the method was shown by the analysis of synthesized N-alkylated ortho-, meta- and para-fluorocathinones and seized designer drug mixtures. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  6. Compound-specific chlorine isotope analysis: a comparison of gas chromatography/isotope ratio mass spectrometry and gas chromatography/quadrupole mass spectrometry methods in an interlaboratory study.

    Science.gov (United States)

    Bernstein, Anat; Shouakar-Stash, Orfan; Ebert, Karin; Laskov, Christine; Hunkeler, Daniel; Jeannottat, Simon; Sakaguchi-Söder, Kaori; Laaks, Jens; Jochmann, Maik A; Cretnik, Stefan; Jager, Johannes; Haderlein, Stefan B; Schmidt, Torsten C; Aravena, Ramon; Elsner, Martin

    2011-10-15

    Chlorine isotope analysis of chlorinated hydrocarbons like trichloroethylene (TCE) is of emerging demand because these species are important environmental pollutants. Continuous flow analysis of noncombusted TCE molecules, either by gas chromatography/isotope ratio mass spectrometry (GC/IRMS) or by GC/quadrupole mass spectrometry (GC/qMS), was recently brought forward as innovative analytical solution. Despite early implementations, a benchmark for routine applications has been missing. This study systematically compared the performance of GC/qMS versus GC/IRMS in six laboratories involving eight different instruments (GC/IRMS, Isoprime and Thermo MAT-253; GC/qMS, Agilent 5973N, two Agilent 5975C, two Thermo DSQII, and one Thermo DSQI). Calibrations of (37)Cl/(35)Cl instrument data against the international SMOC scale (Standard Mean Ocean Chloride) deviated between instruments and over time. Therefore, at least two calibration standards are required to obtain true differences between samples. Amount dependency of δ(37)Cl was pronounced for some instruments, but could be eliminated by corrections, or by adjusting amplitudes of standards and samples. Precision decreased in the order GC/IRMS (1σ ≈ 0.1‰), to GC/qMS (1σ ≈ 0.2-0.5‰ for Agilent GC/qMS and 1σ ≈ 0.2-0.9‰ for Thermo GC/qMS). Nonetheless, δ(37)Cl values between laboratories showed good agreement when the same external standards were used. These results lend confidence to the methods and may serve as a benchmark for future applications. © 2011 American Chemical Society

  7. Gas-liquid mass transfer in a cross-flow hollow fiber module : Analytical model and experimental validation

    NARCIS (Netherlands)

    Dindore, V. Y.; Versteeg, G. F.

    2005-01-01

    The cross-flow operation of hollow fiber membrane contactors offers many advantages and is preferred over the parallel-flow contactors for gas-liquid mass transfer operations. However, the analysis of such a cross-flow membrane gas-liquid contactor is complicated due to the change in concentrations

  8. A243 Comparison between Theoretical and Experimental Mass Flow Rate regarding Release of High-Pressure Hydrogen Gas

    OpenAIRE

    河野, 慎吾; 坂田, 展康; 岡林, 一木; 河内, 昭紀; 千歳, 敬子; Shingo, Kawano; Nobuyasu, Sakata; Kazuki, OKABAYASHI; Akinori, KOUCHI; Keiko, CHITOSE; 三菱重工; 三菱重工; 三菱重工; 三菱重工; 三菱重工

    2004-01-01

    Experiments of the leak of the hydrogen from high pressure tank has been conducted to investigate the safety of the hydrogen station. In the experiments, it was confirmed that the mass flow rate of the hydrogen gas released from the nozzle was lower than the theoretical value that was derived from the assumption that the hydrogen was ideal gas and expanded isentropically. From the one-dimensional analysis including the real gas effect and numerical simulation that reproduced the shape of the ...

  9. Determination of polar pharmaceuticals in sewage water of Greece by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Koutsouba, V; Heberer, Th; Fuhrmann, B; Schmidt-Baumler, K; Tsipi, D; Hiskia, A

    2003-04-01

    Sewage influents and effluents of different urban areas of Greece, were analyzed for polar pharmaceutical residues, used in human medicine. Drugs investigated were the anti-inflammatory drugs diclofenac and ibuprofen, the metabolite of the drugs clofibrates used as blood lipid regulators, clofibric acid and the analgesics phenazone and propyphenazone. Analysis was carried out using capillary gas chromatography-mass spectrometry with selected ion monitoring. The method used was involved solid phase extraction (C(18)) and derivatization with pentafluorobenzyl bromide. Diclofenac was detected in every sewage effluent sample.

  10. [Quantitative determination of strychnine in blood and urine by gas chromatography with mass-selective detector].

    Science.gov (United States)

    Kataev, S S; Krylova, E A

    2010-01-01

    A method for the quantitative determination of strychnine in biological fluids by gas chromatography--mass spectrometry is proposed. The preparation of samples for the analysis included extraction of strychnine from blood and urine with the use of AccuBond(II) EVIDEX cartridges for solid-phase extraction and SPEC MP3 disks respectively. The efficiency of extraction was estimated at 0.05 mg/l for blood and 0.02 mg/l for urine. The detection limit was 0.10 mg/l in blood and 0.05 mg/l in urine.

  11. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... was quantified by the use of headspace GC-MS using acetone-(13)C(3) as an internal standard. The developed method was found to have intra- and total interday relative standard deviations acetone+acetoacetate levels (~25 to 8300 µM) and D-ß-hydroxybutyrate levels (~30 to 16500 µM). Recovery values varied...

  12. Chemical characterization using gas chromatography/mass spectrometry of two extracts from Phyllanthus orbicularis HBK

    International Nuclear Information System (INIS)

    Gutierrez Gaiten, Yamilet Irene; Miranda Martinez, Migdalia; Bello Alarcon, Adonis

    2011-01-01

    The objective of this paper was the chemical characterization of two extracts from Phyllanthus orbicularis HBK through gas chromatography/mass spectrometry. To this end, maceration with N-hexane and ethyl acetate was used to obtain the respective extracts. The study of the hexane extract identified 17 components in which hydrocarbonate structures prevailed, mainly cyclooctacosane. In the ethyl acetate extract, 19 compounds were detected, being the terpenoids the predominant, although the most abundant was sterol g-sitosterol. For the first time, the identified compounds are reported for this species

  13. Analysis of the anthraquinones aloe-emodin and aloin by gas chromatography/mass spectrometry.

    Science.gov (United States)

    ElSohly, Mahmoud A; Gul, Waseem; Murphy, Timothy P

    2004-12-20

    A procedure was developed for the determination of low levels of the anthraquinones aloe-emodin and aloin A (barbalin) in aloe products based on gas chromatography/mass spectrometry (GC/MS) of the trimethyl silyl (TMS) derivatives of these analytes in the presence of Chrysophanol used as internal standard. The method was used to analyze several aloe based commercial products (liquids, gels and solids). Wide variation in the level of these anthraquinones was observed among the different products. The method had a sensitivity of 0.005 ppm of aloe-emodin and 0.05 ppm of aloin.

  14. Gas chromatographic-mass spectrometric determination of levodropropizine plasma levels in healthy volunteers.

    Science.gov (United States)

    Zaratin, P; De Angelis, L; Cattabeni, F

    1988-08-01

    A gas chromatographic-mass spectrometric method for the qualitative and quantitative analysis of levodropropizine (S(-)-3-(4-phenyl-piperazin-1-yl)-propane-1,2-diol, DF 526) in plasma is described. The method proved to be highly selective and sensitive. Drug concentrations as low as 5 ng/ml could be measured. Levodropropizine plasma levels were measured in 6 healthy volunteers after administration of an acute 60 mg dose. Peak concentrations were reached between 40 and 60 min and measurable amounts of drug were present till 8 h after administration.

  15. Determination of cocaine in brazilian paper currency by capillary gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Enrico Di Donato

    2007-01-01

    Full Text Available The presence of illicit drugs such as cocaine and marijuana in US paper currency is very well demonstrated. However, there is no published study describing the presence of cocaine and/or other illicit drugs in Brazilian paper currency. In this study, Brazilian banknotes were collected from nine cities, extracted and analyzed by capillary gas chromatography/mass spectrometry, in order to investigate the presence of cocaine. Bills were extracted with deionized water followed by ethyl acetate. Results showed that 93% of the bills presented cocaine in a concentration range of 2.38-275.10 µg/bill.

  16. Gas chromatographic-mass spectrometric analysis of creosotes extracted from wooden sleepers installed in playgrounds

    Energy Technology Data Exchange (ETDEWEB)

    Rotard, W.; Mailahn, W.

    1987-01-01

    In order to evaluate their hygienic risk, wood samples from sleepers (railroad cross ties) impregnated with coal tar creosote were taken from playgrounds and investigated for hazardous compounds. The samples were extracted with ether, and acid-base-neutral separations were made on the creosote extracts. Water-soluble compounds were also isolated. All the fractions were investigated by capillary gas chromatography-mass spectrometry. Besides phenols in the acidic fractions and N-heterocyclic polynuclear aromatic hydrocarbons (PAH) in the basic fractions, high amounts of neutral PAH and also, in several samples high levels of carcinogenic and cocarcinogenic PAH were determined.

  17. 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.

  18. Determination of d-limonene in adipose tissue by gas chromatography-mass spectrometry

    Science.gov (United States)

    Miller, Jessica A.; Hakim, Iman A.; Thomson, Cynthia; Thompson, Patricia; Chow, H-H. Sherry

    2008-01-01

    We developed a novel method for analyzing d-limonene levels in adipose tissue. Fat samples were subjected to saponification followed by solvent extraction. d-Limonene in the sample extract was analyzed using gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring. Linear calibration curves were established over the mass range of 79.0-2,529 ng d-limonene per 0.1 grams of adipose tissue. Satisfactory within day precision (RSD 6.7 to 9.6%) and accuracy (% difference of −2.7 to 3.8%) and between day precision (RSD 6.0 to 10.7%) and accuracy (% difference of 1.8 to 2.6%) were achieved. The assay was successfully applied to human fat biopsy samples from a d-limonene feeding trial. PMID:18571481

  19. Compressibility, zero sound, and effective mass of a fermionic dipolar gas at finite temperature

    International Nuclear Information System (INIS)

    Kestner, J. P.; Das Sarma, S.

    2010-01-01

    The compressibility, zero-sound dispersion, and effective mass of a gas of fermionic dipolar molecules is calculated at finite temperature for one-, two-, and three-dimensional uniform systems, and in a multilayer quasi-two-dimensional system. The compressibility is nonmonotonic in the reduced temperature, T/T F , exhibiting a maximum at finite temperature. This effect might be visible in a quasi-low-dimensional experiment, providing a clear signature of the onset of many-body quantum degeneracy effects. The collective mode dispersion and effective mass show similar nontrivial temperature and density dependence. In a quasi-low-dimensional system, the zero-sound mode may propagate at experimentally attainable temperatures.

  20. Gas-phase metalloprotein complexes interrogated by ion mobility-mass spectrometry

    Science.gov (United States)

    Faull, Peter A.; Korkeila, Karoliina E.; Kalapothakis, Jason M.; Gray, Andrew; McCullough, Bryan J.; Barran, Perdita E.

    2009-06-01

    Gas-phase biomolecular structure may be explored through a number of analytical techniques. Ion mobility-mass spectrometry (IM-MS) continues to prove itself as a sensitive and reliable bioanalytical tool for gas-phase structure determination due to intense study and development over the past 15 years. A vast amount of research interest, especially in protein and peptide conformational studies has generated a wealth of structural information for biological systems from small peptides to megadalton-sized biomolecules. In this work, linear low field IM-MS has been used to study gas-phase conformations and determine rotationally averaged collision cross-sections of three metalloproteins--cytochrome c, haemoglobin and calmodulin. Measurements have been performed on the MoQToF, a modified QToF 1 instrument (Micromass UK Ltd., Manchester, UK) modified in house. Gas-phase conformations and cross-sections of multimeric cytochrome c ions of the form [xM + nH+]n+ for x = 1-3 (monomer to trimer) have been successfully characterised and measured. We believe these to be the first reported collision cross-sections of higher order multimeric cytochrome c. Haemoglobin is investigated to obtain structural information on the associative mechanism of tetramer formation. Haemoglobin molecules, comprising apo- and holo-monomer chains, dimer and tetramer are transferred to the gas phase under a range of solution conditions. Structural information on the proposed critical intermediate, semi-haemoglobin, is reported. Cross-sections of the calcium binding protein calmodulin have been obtained under a range of calcium-bound conditions. Metalloprotein collision cross-sections from ion mobility measurements are compared with computationally derived values from published NMR and X-ray crystallography structural data. Finally we consider the change in the density of the experimentally measured rotationally averaged collision cross-section for compact geometries of the electrosprayed proteins.

  1. Portable Dew Point Mass Spectrometry System for Real-Time Gas and Moisture Analysis

    Science.gov (United States)

    Arkin, C.; Gillespie, Stacey; Ratzel, Christopher

    2010-01-01

    A portable instrument incorporates both mass spectrometry and dew point measurement to provide real-time, quantitative gas measurements of helium, nitrogen, oxygen, argon, and carbon dioxide, along with real-time, quantitative moisture analysis. The Portable Dew Point Mass Spectrometry (PDP-MS) system comprises a single quadrupole mass spectrometer and a high vacuum system consisting of a turbopump and a diaphragm-backing pump. A capacitive membrane dew point sensor was placed upstream of the MS, but still within the pressure-flow control pneumatic region. Pressure-flow control was achieved with an upstream precision metering valve, a capacitance diaphragm gauge, and a downstream mass flow controller. User configurable LabVIEW software was developed to provide real-time concentration data for the MS, dew point monitor, and sample delivery system pressure control, pressure and flow monitoring, and recording. The system has been designed to include in situ, NIST-traceable calibration. Certain sample tubing retains sufficient water that even if the sample is dry, the sample tube will desorb water to an amount resulting in moisture concentration errors up to 500 ppm for as long as 10 minutes. It was determined that Bev-A-Line IV was the best sample line to use. As a result of this issue, it is prudent to add a high-level humidity sensor to PDP-MS so such events can be prevented in the future.

  2. The dependence of bar frequency on galaxy mass, colour, and gas content - and angular resolution - in the local universe

    Science.gov (United States)

    Erwin, Peter

    2018-03-01

    I use distance- and mass-limited subsamples of the Spitzer Survey of Stellar Structure in Galaxies (S4G) to investigate how the presence of bars in spiral galaxies depends on mass, colour, and gas content and whether large, Sloan Digital Sky Survey (SDSS)-based investigations of bar frequencies agree with local data. Bar frequency reaches a maximum of fbar ≈ 0.70 at M⋆ ˜ 109.7M⊙, declining to both lower and higher masses. It is roughly constant over a wide range of colours (g - r ≈ 0.1-0.8) and atomic gas fractions (log (M_{H I}/ M_{\\star }) ≈ -2.5 to 1). Bars are thus as common in blue, gas-rich galaxies are they are in red, gas-poor galaxies. This is in sharp contrast to many SDSS-based studies of z ˜ 0.01-0.1 galaxies, which report fbar increasing strongly to higher masses (from M⋆ ˜ 1010 to 1011M⊙), redder colours, and lower gas fractions. The contradiction can be explained if SDSS-based studies preferentially miss bars in, and underestimate the bar fraction for, lower mass (bluer, gas-rich) galaxies due to poor spatial resolution and the correlation between bar size and stellar mass. Simulations of SDSS-style observations using the S4G galaxies as a parent sample, and assuming that bars below a threshold angular size of twice the point spread function full width at half-maximum cannot be identified, successfully reproduce typical SDSS fbar trends for stellar mass and gas mass ratio. Similar considerations may affect high-redshift studies, especially if bars grow in length over cosmic time; simulations suggest that high-redshift bar fractions may thus be systematically underestimated.

  3. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  4. Integrated gas and liquid chromatography tandem mass spectrometry for forensic engine lubricating oil identification

    International Nuclear Information System (INIS)

    Shang, D.; McPherson, B.

    2009-01-01

    This paper presented a method for rapid chemical characterization of engine lubricating oils. Motor oils typically contain up to 5 per cent additives, such as detergent, antifoamant, dispersant, emulsifier, antioxidant, friction modifier, colour stabilizer and corrosion inhibitors. Different lube oil products usually have either different additives in various concentrations. As such, the formulation of additives in lube oil products should provide fingerprint information for forensic oil identification. The characterization method used in this study was based on a newly developed fast solvent liquid-liquid sample extraction procedure that combined the use of both liquid chromatography tandem mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) simultaneously together with gas chromatography flame ionization detection (GC-FID). The method was used on a blind sample testing of commercially available engine lubricating products. The sample extraction procedure involved extraction of additives into acidified acetonitrile, two hexane washes of hydrophobic components of lube oil, filtration, and dilution with solvents for GC and LC analysis. The new method proved to be rapid and easy to use. It enabled the identification of unknown additives and hydrocarbons in many different types of fresh lube oils. Further tests will be needed to determine if this method can be used on real-world weathered samples. The method is part of an ongoing effort to deal with mysterious chemical spills, an important aspect of environmental protection and emergency preparedness. 8 refs., 7 figs

  5. Effect of dimethylamine on the gas phase sulfuric acid concentration measured by Chemical Ionization Mass Spectrometry

    CERN Document Server

    Rondo, L.; Kürten, A.; Adamov, A.; Bianchi, F.; Breitenlechner, M.; Duplissy, J.; Franchin, A.; Dommen, J.; Donahue, N. M.; Dunne, E. M.; Flagan, R. C.; Hakala, J.; Hansel, A.; Keskinen, H.; Kim, J.; Jokinen, T.; Lehtipalo, K.; Leiminger, M.; Praplan, A.; Riccobono, F.; Rissanen, M. P.; Sarnela, N.; Schobesberger, S.; Simon, M.; Sipilä, M.; Smith, J. N.; Tomé, A.; Tröstl, J.; Tsagkogeorgas, G.; Vaattovaara, P.; Winkler, P. M.; Williamson, C.; Wimmer, D.; Baltensperger, U.; Kirkby, J.; Kulmala, M.; Petäjä, T.; Worsnop, D. R.; Curtius, J.

    2016-01-01

    Sulfuric acid is widely recognized as a very important substance driving atmospheric aerosolnucleation. Based on quantum chemical calculations it has been suggested that the quantitative detectionof gas phase sulfuric acid (H2SO4) by use of Chemical Ionization Mass Spectrometry (CIMS) could be biased inthe presence of gas phase amines such as dimethylamine (DMA). An experiment (CLOUD7 campaign) was setup at the CLOUD (Cosmics Leaving OUtdoor Droplets) chamber to investigate the quantitative detection ofH2SO4in the presence of dimethylamine by CIMS at atmospherically relevant concentrations. For the first time inthe CLOUD experiment, the monomer sulfuric acid concentration was measured by a CIMS and by two CI-APi-TOF(Chemical Ionization-Atmospheric Pressure interface-Time Of Flight) mass spectrometers. In addition, neutralsulfuric acid clusters were measured with the CI-APi-TOFs. The CLOUD7 measurements show that in the presenceof dimethylamine (<5 to 70 pptv) the sulfuric acid monomer measured by the CIMS...

  6. Effect of dimethylamine on the gas phase sulfuric acid concentration measured by Chemical Ionization Mass Spectrometry

    Science.gov (United States)

    Rondo, L.; Ehrhart, S.; Kürten, A.; Adamov, A.; Bianchi, F.; Breitenlechner, M.; Duplissy, J.; Franchin, A.; Dommen, J.; Donahue, N. M.; Dunne, E. M.; Flagan, R. C.; Hakala, J.; Hansel, A.; Keskinen, H.; Kim, J.; Jokinen, T.; Lehtipalo, K.; Leiminger, M.; Praplan, A.; Riccobono, F.; Rissanen, M. P.; Sarnela, N.; Schobesberger, S.; Simon, M.; Sipilä, M.; Smith, J. N.; Tomé, A.; Tröstl, J.; Tsagkogeorgas, G.; Vaattovaara, P.; Winkler, P. M.; Williamson, C.; Wimmer, D.; Baltensperger, U.; Kirkby, J.; Kulmala, M.; Petäjä, T.; Worsnop, D. R.; Curtius, J.

    2016-03-01

    Sulfuric acid is widely recognized as a very important substance driving atmospheric aerosol nucleation. Based on quantum chemical calculations it has been suggested that the quantitative detection of gas phase sulfuric acid (H2SO4) by use of Chemical Ionization Mass Spectrometry (CIMS) could be biased in the presence of gas phase amines such as dimethylamine (DMA). An experiment (CLOUD7 campaign) was set up at the CLOUD (Cosmics Leaving OUtdoor Droplets) chamber to investigate the quantitative detection of H2SO4 in the presence of dimethylamine by CIMS at atmospherically relevant concentrations. For the first time in the CLOUD experiment, the monomer sulfuric acid concentration was measured by a CIMS and by two CI-APi-TOF (Chemical Ionization-Atmospheric Pressure interface-Time Of Flight) mass spectrometers. In addition, neutral sulfuric acid clusters were measured with the CI-APi-TOFs. The CLOUD7 measurements show that in the presence of dimethylamine (growth. Although it was found that the addition of dimethylamine dramatically changes the H2SO4 cluster distribution compared to binary (H2SO4-H2O) conditions, the CIMS detection efficiency does not seem to depend substantially on whether an individual H2SO4 monomer is clustered with a DMA molecule. The experimental observations are supported by numerical simulations based on A Self-contained Atmospheric chemistry coDe coupled with a molecular process model (Sulfuric Acid Water NUCleation) operated in the kinetic limit.

  7. A Low Mass for Mars from Jupiter's Early Gas-Driven Migration

    Science.gov (United States)

    Walsh, Kevin J.; Morbidelli, Alessandro; Raymond, Sean N.; O'Brien, David P.; Mandell, Avi M.

    2011-01-01

    Jupiter and Saturn formed in a few million years from a gas-dominated protoplanetary disk, and were susceptible to gas-driven migration of their orbits on timescales of only approximately 100,000 years. Hydrodynamic simulations show that these giant planets can undergo a two-stage, inward-then-outward, migration. The terrestrial planets finished accreting much later and their characteristics, including Mars' small mass, are best reproduced by starting from a planetesimal disk with an outer edge at about one astronomical unit from the Sun (1 AU is the Earth-Sun distance). Here we report simulations of the early Solar System that show how the inward migration of Jupiter to 1.5 AU, and its subsequent outward migration, lead to a planetesimal disk truncated at 1 AU; the terrestrial planets then form from this disk over the next 30-50 million years, with an Earth/Mars mass ratio consistent with observations. Scattering by Jupiter initially empties but then repopulates the asteroid belt, with inner-belt bodies originating between 1 and 3 AU and outer-belt bodies originating between and beyond the giant planets. This explains the significant compositional differences across the asteroid belt. The key aspect missing from previous models of terrestrial planet formation is the substantial radial migration of the giant planets, which suggests that their behaviour is more similar to that inferred for extrasolar planets than previously thought.

  8. 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.

  9. observations of hot molecular gas emission from embedded low-mass protostars

    DEFF Research Database (Denmark)

    Visser, R.; Kristensen, L. E.; Bruderer, S.

    2012-01-01

    the observations quantitatively, to investigate the origin of the emission, and to use the lines as probes of the various heating mechanisms. Methods. The model consists of a spherical envelope with a power-law density structure and a bipolar outflow cavity. Three heating mechanisms are considered: passive heating...... such as luminosity and envelope mass. Results. The bulk of the gas in the envelope, heated by the protostellar luminosity, accounts for 3–10% of the CO luminosity summed over all rotational lines up to J = 40–39; it is best probed by low-J CO isotopologue lines such as C18O 2–1 and 3–2. The UV-heated gas and the C......-type shocks, probed by 12CO 10–9 and higher-J lines, contribute 20–80% each. The model fits show a tentative evolutionary trend: the CO emission is dominated by shocks in the youngest source and by UV-heated gas in the oldest one. This trend is mainly driven by the lower envelope density in more evolved...

  10. The effect of gas double-dynamic on mass distribution in solid-state fermentation.

    Science.gov (United States)

    Chen, Hong-Zhang; Zhao, Zhi-Min; Li, Hong-Qiang

    2014-05-10

    The mass distribution regularity in substrate of solid-state fermentation (SSF) has rarely been reported due to the heterogeneity of solid medium and the lack of suitable instrument and method, which limited the comprehensive analysis and enhancement of the SSF performance. In this work, the distributions of water, biomass, and fermentation product in different medium depths of SSF were determined using near-infrared spectroscopy (NIRS) and the developed models. Based on the mass distribution regularity, the effects of gas double-dynamic on heat transfer, microbial growth and metabolism, and product distribution gradient were systematically investigated. Results indicated that the maximum temperature of substrate and the maximum carbon dioxide evolution rate (CER) were 39.5°C and 2.48mg/(hg) under static aeration solid-state fermentation (SASSF) and 33.9°C and 5.38mg/(hg) under gas double-dynamic solid-state fermentation (GDSSF), respectively, with the environmental temperature for fermentation of 30±1°C. The fermentation production (cellulase activity) ratios of the upper, middle, and lower levels were 1:0.90:0.78 at seventh day under SASSF and 1:0.95:0.89 at fifth day under GDSSF. Therefore, combined with NIRS analysis, gas double-dynamic could effectively strengthen the solid-state fermentation performance due to the enhancement of heat transfer, the stimulation of microbial metabolism and the increase of the homogeneity of fermentation products. Copyright © 2014 Elsevier Inc. All rights reserved.

  11. On-line mass spectrometry measurement of fission gas release from nuclear fuel submitted to thermal transients

    International Nuclear Information System (INIS)

    Guigues, E.; Janulyte, A.; Zerega, Y.; Pontillon, Y.

    2013-06-01

    The work presented in this paper has been performed in the framework of a joint research program between Aix-Marseille University and CEA Cadarache. The aim is to develop a mass spectrometer (MS) device for the MERARG facility. MERARG is devoted to the study of fission gas release measurement, from nuclear fuels submitted to annealing tests in high activity laboratory such as LECA-STAR, thanks to gamma spectrometry. The mass spectrometer will then extend the measurement capability from the γ-emitters gases to all the gases involved in the release in order to have a better understanding of the fission gas release dynamics from fuel during thermal transients. Furthermore, the mass spectrometer instrument combines the capabilities and performances of both on-line (for release kinetic) and off-line implementations (for delayed accurate analysis of capacities containing total release gas). The paper deals with two main axes: (1) the modelling of gas sampling inlet device and its performance and (2) the first MS qualification/calibration results. The inlet device samples the gas and also adapts the pressure between MERARG sweeping line at 1.2 bar and mass spectrometer chamber at high vacuum. It is a two-stage device comprising a capillary at inlet, an intermediate vacuum chamber, a molecular leak inlet and a two-stage pumping device. Pressure drops, conductance and throughputs are estimated both for mass spectrometer operation and for exhaust gas recovery. Possible gas segregation is also estimated and device modification is proposed to attain a more accurate calibration. First experimental results obtained from a standard gas bottle show that the quantitative analysis at a few ppm level can be achieved for all isotopes of Kr and Xe, as well as masses 2 and 4 u. (authors)

  12. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Isotope Ratio Mass Spectrometry and Shale Gas - What Is Possible with Current Technology?

    Science.gov (United States)

    Barrie, C. D.; Kasson, A.

    2014-12-01

    With ever increasing exploration and exploitation of 'unconventional' hydrocarbon resources, the drive to understand the origins, history and importance of these resources and their effects on the surrounding environment (i.e. ground waters) has never been more important. High-throughput, high-precision isotopic measurements are therefore a key tool in this industry to both understand the gas generated and monitor the development and stability of wells through time. With the advent of cavity ringdown spectroscopy (CRDS) instrumentation, there has been a push in some applications - environmental & atmospheric - to gather more and more data directly at the location of collection or at dedicated field stations. Furthermore, CRDS has resulted in users seeking greater autonomy of instrumentation and so-called black box technology. Traditionally IRMS technology has not met any of these demands, requiring very specific and extensive footprint, power and environmental requirements. This has meant that the 'Oil & Gas' sector, which for natural gases measurements requires GC-IRMS technology - not possible via CRDS - loses time, money and manpower as samples get sent to central facility or contract labs with potentially long lee times. However, recent developments in technology mean that IRMS systems exist which are benchtop, have much lower power requirements, standard power connections and as long as housed in a temperature controlled field stations can be deployed anywhere. Furthermore, with advances in electronics and software IRMS systems are approaching the black box level of newer instrumentation while maintaining the flexibility and abilities of isotope ratio mass spectrometry. This presentation will outline changes in IRMS technology applicable to the Oil & Gas industry, discuss the feasibility of true 'field' deployability and present results from a range of Oil & Gas samples.

  14. Comparison Study on Empirical Correlation for Mass Transfer Coefficient with Gas Hold-up and Input Power of Aeration Process

    Energy Technology Data Exchange (ETDEWEB)

    Park, Sang Kyoo; Yang, Hei Cheon [Chonnam Nat’l Univ., Gwangju (Korea, Republic of)

    2017-06-15

    As stricter environmental regulation have led to an increase in the water treatment cost, it is necessary to quantitatively study the input power of the aeration process to improve the energy efficiency of the water treatment processes. The objective of this study is to propose the empirical correlations for the mass transfer coefficient with the gas hold-up and input power in order to investigate the mass transfer characteristics of the aeration process. It was found that as the input power increases, the mass transfer coefficient increases because of the decrease of gas hold-up and increase of Reynolds number, the penetration length, and dispersion of mixed flow. The correlations for the volumetric mass transfer coefficients with gas hold-up and input power were consistent with the experimental data, with the maximum deviation less than approximately ±10.0%.

  15. Community air monitoring for pesticides-part 2: multiresidue determination of pesticides in air by gas chromatography, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hengel, Matt; Lee, P

    2014-03-01

    Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography-mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37-104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70-170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air.

  16. The mass-metallicity relations for gas and stars in star-forming galaxies: strong outflow versus variable IMF

    Science.gov (United States)

    Lian, Jianhui; Thomas, Daniel; Maraston, Claudia; Goddard, Daniel; Comparat, Johan; Gonzalez-Perez, Violeta; Ventura, Paolo

    2018-02-01

    We investigate the mass-metallicity relations for the gaseous (MZRgas) and stellar components (MZRstar) of local star-forming galaxies based on a representative sample from Sloan Digital Sky Survey Data Release 12. The mass-weighted average stellar metallicities are systematically lower than the gas metallicities. This difference in metallicity increases towards galaxies with lower masses and reaches 0.4-0.8 dex at 109 M⊙ (depending on the gas metallicity calibration). As a result, the MZRstar is much steeper than the MZRgas. The much lower metallicities in stars compared to the gas in low-mass galaxies imply dramatic metallicity evolution with suppressed metal enrichment at early times. The aim of this paper is to explain the observed large difference in gas and stellar metallicity and to infer the origin of the mass-metallicity relations. To this end we develop a galactic chemical evolution model accounting for star formation, gas inflow and outflow. By combining the observed mass-metallicity relation for both gas and stellar components to constrain the models, we find that only two scenarios are able to reproduce the observations. Either strong metal outflow or a steep initial mass function (IMF) slope at early epochs of galaxy evolution is needed. Based on these two scenarios, for the first time we successfully reproduce the observed MZRgas and MZRstar simultaneously, together with other independent observational constraints in the local Universe. Our model also naturally reproduces the flattening of the MZRgas at the high-mass end leaving the MZRstar intact, as seen in observational data.

  17. Measuring deuterium enrichment of glucose hydrogen atoms by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Antoniewicz, Maciek R; Kelleher, Joanne K; Stephanopoulos, Gregory

    2011-04-15

    We developed a simple and accurate method for determining deuterium enrichment of glucose hydrogen atoms by electron impact gas chromatography mass spectrometry (GC/MS). First, we prepared 18 derivatives of glucose and screened over 200 glucose fragments to evaluate the accuracy and precision of mass isotopomer data for each fragment. We identified three glucose derivatives that gave six analytically useful ions: (1) glucose aldonitrile pentapropionate (m/z 173 derived from C4-C5 bond cleavage; m/z 259 from C3-C4 cleavage; m/z 284 from C4-C5 cleavage; and m/z 370 from C5-C6 cleavage); (2) glucose 1,2,5,6-di-isopropylidene propionate (m/z 301, no cleavage of glucose carbon atoms); and (3) glucose methyloxime pentapropionate (m/z 145 from C2-C3 cleavage). Deuterium enrichment at each carbon position of glucose was determined by least-squares regression of mass isotopomer distributions. The validity of the approach was tested using labeled glucose standards and carefully prepared mixtures of standards. Our method determines deuterium enrichment of glucose hydrogen atoms with an accuracy of 0.3 mol %, or better, without the use of any calibration curves or correction factors. The analysis requires only 20 μL of plasma, which makes the method applicable for studying gluconeogenesis using deuterated water in cell culture and animal experiments. © 2011 American Chemical Society

  18. CAST search for sub-eV mass solar axions with $^{3}$He buffer gas

    CERN Document Server

    Aune, S; Belov, A; Borghi, S; Brauninger, H; Cantatore, G; Carmona, J M; Cetin, S A; Collar, J I; Dafni, T; Davenport, M; Eleftheriadis, C; Elias, N; Ezer, C; Fanourakis, G; Ferrer-Ribas, E; Friedrich, P; Galan, J; Garcia, J A; Gardikiotis, A; Gazis, E N; Geralis, T; Giomataris, I; Gninenko, S; Gomez, H; Gruber, E; Guthorl, T; Hartmann, R; Haug, F; Hasinoff, M D; Hoffmann, D H H; Iguaz, F J; Irastorza, I G; Jacoby, J; Jakovcic, K; Karuza, M; Konigsmann, K; Kotthaus, R; Krcmar, M; Kuster, M; Lakic, B; Laurent, J M; Liolios, A; Ljubicic, A; Lozza, V; Lutz, G; Luzon, G; Morales, J; Niinikoski, T; Nordt, A; Papaevangelou, T; Pivovaroff, M J; Raffelt, G; Rashba, T; Riege, H; Rodriguez, A; Rosu, M; Ruz, J; Savvidis, I; Silva, P S; Solanki, S.K; Stewart, L; Tomas, A; Tsagri, M; van Bibber, K; Vafeiadis, T; Villar, J A; Vogel, J K; Yildiz, S C; Zioutas, K

    2011-01-01

    The CERN Axion Solar Telescope (CAST) has extended its search for solar axions by using 3He as a buffer gas. At T=1.8 K this allows for larger pressure settings and hence sensitivity to higher axion masses than our previous measurements with 4He. With about 1 h of data taking at each of 252 different pressure settings we have scanned the axion mass range 0.39 eV < m_a < 0.64 eV. From the absence of excess X-rays when the magnet was pointing to the Sun we set a typical upper limit on the axion-photon coupling of g_ag < 2.3 x 10^{-10} GeV^{-1} at 95% CL, the exact value depending on the pressure setting. KSVZ axions are excluded at the upper end of our mass range, the first time ever for any solar axion search. In future we will extend our search to m_a < 1.15 eV, comfortably overlapping with cosmological hot dark matter bounds.

  19. Application of gas chromatography-surface ionization organic mass spectrometry to forensic toxicology.

    Science.gov (United States)

    Ishii, Akira; Watanabe-Suzuki, Kanako; Seno, Hiroshi; Suzuki, Osamu; Katsumata, Yoshinao

    2002-08-25

    Surface ionization (SI), which consists in the formation of positive and negative ions along the course of thermal desorption of particles from a solid surface, was first applied as a detector for gas chromatography (GC), GC-surface ionization detection (SID); we developed many new sensitive methods for the determination of abused and other drugs by GC-SID. Recently, Fujii has devised a combination of SI and a quadrupole mass spectrometer and named this system a surface ionization organic mass spectrometer (SIOMS), which is highly selective and sensitive for organic compounds containing tertiary amino groups. We have tried to apply this mass spectrometer to forensic toxicological study; so far we have succeeded in determining important drugs-of-abuse and toxic compounds, such as phencyclidine (PCP), pethidine, pentazocine, MPTP and its derivatives from human body fluids with high sensitivity and selectivity. In this review, we describe our recent studies on the application of GC-SIOMS to forensic toxicology. Copyright 2002 Elsevier Science B.V.

  20. [Combined use of tandem mass spectrometry with urine gas chromatography/mass spectrometry is useful for diagnosis of inborn errors of metabolism in children].

    Science.gov (United States)

    Xie, Li-Juan; Zhu, Jian-Xing; Zhu, Xiao-Dong; Li, Hua-Jun; Han, Lian-Shu; Gu, Xue-Fan

    2008-02-01

    Many inborn errors of metabolism have similar presenting clinical manifestations, making early diagnosis difficult. We report our experience with tandem mass spectrometry combined with urine gas chromatography/mass spectrometry as a means of definitively diagnosing inborn errors of metabolism. One hundred and thirty-two children with suspected inborn errors of metabolism but without specific clinical manifestations, admitted to the Xinhua Hospital Affiliated to Shanghai Jiaotong University School of Medicine between June 1, 2003 and September 30, 2006, were studied. Children received routine biochemical examinations, as well as mass spectrometry and gas chromatography-mass spectrometry. Fifteen cases (11.5%) were confirmed as having inborn errors of metabolism, including 6 cases of methylmalonic acidemia, 2 of propionic academia, 2 of Type II citrullinemia, 1 of biotinidase deficiency, 1 of tyrosinemia, 1 of maple syrup urine disease, 1 of omithine transcarbamylase deficiency and 1 of very long chain Acyl CoA dehydrogenase deficiency. The combined use of tandem mass spectrometry with urine gas chromatography mass spectrometry is useful for early diagnosis of inborn errors of metabolism in children with suspected inborn errors of metabolism but without specific clinical manifestations.

  1. Investigation of the Flow Rate Effect Upstream of the Constant-Geometry Throttle on the Gas Mass Flow

    Directory of Open Access Journals (Sweden)

    Yu. M. Timofeev

    2016-01-01

    Full Text Available The turbulent-flow throttles are used in pneumatic systems and gas-supply ones to restrict or measure gas mass flow. It is customary to install the throttles in joints of pipelines (in teejoints and cross tees or in joints of pipelines with pneumatic automation devices Presently, in designing the pneumatic systems and gas-supply ones a gas mass flow through a throttle is calculated by a known equation derived from the Saint-Venant-Vantсel formula for the adiabatic flow of ideal gas through a nozzle from an unrestrictedly high capacity tank. Neglect of gas velocity at the throttle inlet is one of the assumptions taken in the development of the above equation. As may be seen in practice, in actual systems the diameters of the throttle and the pipe wherein it is mounted can be commensurable. Neglect of the inlet velocity therewith can result in an error when determining the required throttle diameter in design calculation and a flow rate in checking calculation, as well as when measuring a flow rate in the course of the test. The theoretical study has revealed that the flow velocity at the throttle inlet is responsible for two parameter values: the outlet flow velocity and the critical pressure ratio, which in turn determine the gas mass flow value. To calculate the gas mass flow, the dependencies are given in the paper, which allow taking into account the flow rate at the throttle inlet. The analysis of obtained dependencies has revealed that the degree of influence of inlet flow rate upon the mass flow is defined by two parameters: pressure ratio at the throttle and open area ratio of the throttle and the pipe wherein it is mounted. An analytical investigation has been pursued to evaluate the extent to which the gas mass flow through the throttle is affected by the inlet flow rate. The findings of the investigation and the indications for using the present dependencies are given in this paper. By and large the investigation allowed the

  2. Gas-liquid mass transfer and flow phenomena in the Peirce-Smith converter: a water model study

    Science.gov (United States)

    Zhao, Xing; Zhao, Hong-liang; Zhang, Li-feng; Yang, Li-qiang

    2018-01-01

    A water model with a geometric similarity ratio of 1:5 was developed to investigate the gas-liquid mass transfer and flow characteristics in a Peirce-Smith converter. A gas mixture of CO2 and Ar was injected into a NaOH solution bath. The flow field, volumetric mass transfer coefficient per unit volume ( Ak/V; where A is the contact area between phases, V is the volume, and k is the mass transfer coefficient), and gas utilization ratio ( η) were then measured at different gas flow rates and blow angles. The results showed that the flow field could be divided into five regions, i.e., injection, strong loop, weak loop, splashing, and dead zone. Whereas the Ak/V of the bath increased and then decreased with increasing gas flow rate, and η steadily increased. When the converter was rotated clockwise, both Ak/V and η increased. However, the flow condition deteriorated when the gas flow rate and blow angle were drastically increased. Therefore, these parameters must be controlled to optimal conditions. In the proposed model, the optimal gas flow rate and blow angle were 7.5 m3·h-1 and 10°, respectively.

  3. Gas dispersion and bubble-to-emulsion phase mass exchange in a gas-solid bubbling fluidized bed: a computational and experimental study

    NARCIS (Netherlands)

    Patil, D.J.; van Sint Annaland, M.; Kuipers, J.A.M.

    2003-01-01

    Knowledge of gas dispersion and mass exchange between the bubble and the emulsion phases is essential for a correct prediction of the performance of fluidized beds, particularly when catalytic reactions take place. Test cases of single rising bubble and a bubbling fluidized bed operated with a jet

  4. Pyrolysis-gas chromatography-mass spectrometry of isolated, synthetic and degraded lignins

    Energy Technology Data Exchange (ETDEWEB)

    Saiz-Jimenez, C.; De Leeuw, J.W.

    1984-01-01

    Curie-point pyrolysis-gas chromatography-mass spectrometry was applied to study the chemical structure of sound and fungus degraded, industrial and synthetic lignins. Pyrolysis products reflected in some detail the structural units present in the lignin polymer. Thus, sound spruce lignin yielded trans-isoeugenol coniferaldehyde and trans-coniferyl alcohol as major pyrolysis products. Biodegraded lignin yielded oxidized units, including vanillin, acetoguaiacone, methyl vanillate, propioguaiacone, vanilloyl methyl ketone and vanillic acid as major products. Kraft lignin also showed evidence of oxidation, although not as much as the biodegraded lignin. Major products from this industrial lignin were guaiacol, methylguaiacol, vinylguaiacol and homovanillic acid. Results indicated that synthetic lignin duplicates fairly well the structure of natural lignin. However, coniferylaldehyde and trans-coniferyl alcohol were the dominant products only from the synthetic lignin, indicating the presence of large amounts of coniferyl alcohol and coniferylaldehyde end groups. 21 references.

  5. Verification of chemical composition of commercially available propolis extracts by gas chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Czyżewska, Urszula; Konończuk, Joanna; Teul, Joanna; Drągowski, Paweł; Pawlak-Morka, Renata; Surażyński, Arkadiusz; Miltyk, Wojciech

    2015-05-01

    Propolis is a resin that is collected by honeybees from various plant sources. Due to its pharmacological properties, it is used in commercial production of nutritional supplements in pharmaceutical industry. In this study, gas chromatography-mass spectrometry was applied for quality control analysis of the three commercial specimens containing aqueous-alcoholic extracts of bee propolis. More than 230 constituents were detected in analyzed products, including flavonoids, chalcones, cinnamic acids and their esters, phenylpropenoid glycerides, and phenylpropenoid sesquiterpenoids. An allergenic benzyl cinnamate ester was also identified in all tested samples. This analytical method allows to evaluate biological activity and potential allergenic components of bee glue simultaneously. Studies on chemical composition of propolis samples may provide new approach to quality and safety control analysis in production of propolis supplementary specimens.

  6. Gas chromatography-mass spectrometry identification of photoproducts of hexahydroquinoline derivatives: potential calcium channel antagonists.

    Science.gov (United States)

    Mielcarek, Jadwiga; Matłoka, Agnieszka

    2005-05-05

    Photodegradation products of hexahydroquinoline derivatives (HHQ) have been analysed with gas chromatography-mass spectrometry (GC-MS). The photodegradation was carried out under the conditions recommended in the first version of the document issued by the International Conference on Harmonization (ICH), currently in force in the studies of photochemical stability of drugs and therapeutic substances. The study was performed on the compounds having two chlorine atoms at different positions of the phenyl ring. Photodegradation of dichlorophenyl derivatives of HHQ resulted in formation of one or three photoproducts. The main product of their decomposition was aromatic compound formed as a result of dehydrogenation of the dihydropyridine ring. The most often observed fragmentation pathway of the photoproducts formed was elimination of methyl and methoxy radicals from the ester groups. The fragmentation of the photoproducts containing one chlorine atom at the ortho-position of the phenyl ring occurred through elimination of chlorine radical.

  7. Multiresidue determination of pesticides in fruit and vegetables by gas chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Gamón, M; Lleó, C; Ten, A; Mocholí, F

    2001-01-01

    Pesticide residues in fruit and vegetables were determined by gas chromatography/tandem mass spectrometry (GC/MS/MS). Electron impact (EI)/MS/MS and chemical ionization (CI)/MS/MS were developed for 80 compounds, including organochlorine, organophosphorus, organonitrogen, and pyrethroids, providing unambiguous spectral confirmation for these complex matrixes. Residues were extracted from samples with acetone followed by a mixture of dichloromethane-petroleum ether. Two injections per sample were required for analysis of the entire pesticide list by EI/MS/MS and CI/MS/MS. Initial steps involving cleanup and concentration of extracts were eliminated. The excellent selectivity and good linearity allowed quantification and identification of low levels of pesticides in the most difficult matrixes. The method has been used for routine analysis of many vegetables.

  8. Profiling of plasma metabolites in canine oral melanoma using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kawabe, Mifumi; Baba, Yuta; Tamai, Reo; Yamamoto, Ryohei; Komori, Masayuki; Mori, Takashi; Takenaka, Shigeo

    2015-08-01

    Malignant melanoma is one of the most common and aggressive tumors in the oral cavity of dog. The tumor has a poor prognosis, and methods for diagnosis and prediction of prognosis after treatment are required. Here, we examined metabolite profiling using gas chromatography-mass spectrometry (GC-MS) for development of a discriminant model for evaluation of prognosis. Metabolite profiles were evaluated in healthy and melanoma plasma samples using orthogonal projection to latent structure using discriminant analysis (OPLS-DA). Cases that were predicted to be healthy using the OPLS discriminant model had no advanced lesions after radiation therapy. These results indicate that metabolite profiling may be useful in diagnosis and prediction of prognosis of canine malignant melanoma.

  9. Gas chromatography-mass spectrometric identification of iodine species arising from photo-chemical vapor generation

    Energy Technology Data Exchange (ETDEWEB)

    Grinberg, Patricia; Mester, Zoltan [Institute for National Measurements Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6 (Canada); D' Ulivo, Alessandro [Institute for Chemical and Physical Processes, National Research Council, Via G. Moruzzi 1, Pisa, 56124 (Italy); Sturgeon, Ralph E. [Institute for National Measurements Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6 (Canada)], E-mail: ralph.sturgeon@nrc.ca

    2009-07-15

    Ultraviolet irradiation of aqueous solutions of iodide/iodate ion containing low molecular weight organic acids generates volatile iodine species that are amenable to detection by atomic spectrometry. In the presence of formic, acetic or propionic acids, photo-chemical generation results in the formation of HI, methyl- and ethyl-iodide respectively, the latter two products being directly identified by gas chromatography-mass spectrometry. Deuterium and {sup 13}C-labeled reagents were employed to elucidate the provenance of the alkyl group. Use of {sup 13}CH{sub 3}-COOH produced {sup 13}CH{sub 3}-I; deuterated acetic acid (D{sub 3}C-COOD) resulted in the formation of CD{sub 3}-I. These observations indicate direct transfer of the alkyl group from the carboxylic acid to iodide, consistent with the suggestion that the mechanism of synthesis involves radical induced reactions.

  10. Gas chromatography-mass spectrometric identification of iodine species arising from photo-chemical vapor generation

    Science.gov (United States)

    Grinberg, Patricia; Mester, Zoltan; D'Ulivo, Alessandro; Sturgeon, Ralph E.

    2009-07-01

    Ultraviolet irradiation of aqueous solutions of iodide/iodate ion containing low molecular weight organic acids generates volatile iodine species that are amenable to detection by atomic spectrometry. In the presence of formic, acetic or propionic acids, photo-chemical generation results in the formation of HI, methyl- and ethyl-iodide respectively, the latter two products being directly identified by gas chromatography-mass spectrometry. Deuterium and 13C-labeled reagents were employed to elucidate the provenance of the alkyl group. Use of 13CH 3-COOH produced 13CH 3-I; deuterated acetic acid (D 3C-COOD) resulted in the formation of CD 3-I. These observations indicate direct transfer of the alkyl group from the carboxylic acid to iodide, consistent with the suggestion that the mechanism of synthesis involves radical induced reactions.

  11. Detecting naphthenic acids in waters by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Merlin, Mireya; Guigard, Selma E; Fedorak, Phillip M

    2007-01-26

    Naphthenic acids (general formula C(n)H(2n+Z)O(2)) are water-soluble, toxic compounds found in petroleum and bitumen. Some of the current methods for detecting these acids in waters depend on measuring the presence of the carboxylic acid functional group, and therefore many of these methods also detect naturally occurring carboxylic acids that are not naphthenic acids. We report a procedure that includes liquid-liquid extraction, cleanup, and derivatization to form t-butyldimethylsilyl esters prior to gas chromatography-mass spectrometry (GC-MS) analysis. Using low- and high-resolution MS to detect the ion C(15)H(27)O(2)Si(+) (nominal m/z=267) is an excellent indicator of the presence of naphthenic acids at concentrations > or =10microgL(-1).

  12. A mass spectrometric investigation of the exchange of deuterium with tetraborane(10) in the gas phase

    International Nuclear Information System (INIS)

    Greatrex, R.; Greenwood, N.N.; Potter, C.D.

    1984-01-01

    Mass spectrometry has been used to establish direct exchange between dideuterium (D 2 ) and B 4 H 10 in the gas phase. In a mixture of stoicheiometry B 4 H 10 :3D 2 at 42 deg C, ca. 7% of the hydrogen atoms were replaced by deuterium in 130 min. The possibility that the exchange might be occurring by an indirect or autocatalytic mechanism was eliminated by a series of experiments in which the rate of exchange was shown to be independent of small admixtures of the decomposition products. The present work resolves a troublesome inconsistency in the literature and strengthens the view that the equilibrium B 4 H 10 brace B 4 H 8 brace + H 2 plays a key role in borane interconversion reactions. (author)

  13. Determination of Chlorpyrifos in Human Blood by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Xinhua Dai

    2017-01-01

    Full Text Available Gas chromatography-mass spectrometry method was developed for the qualitative and quantitative analyses of chlorpyrifos in human blood samples. The chlorpyrifos and parathion (internal standard in human blood were extracted with a mixed solvent of hexane and acetonitrile. Chlorpyrifos was well separated from the internal standard. The linear range of chlorpyrifos was 0.01–2 μg/ml in blood. The limit of detection and limit of quantification were estimated at 0.002 and 0.01 μg/ml, respectively. The inter- and intra-day precisions, accuracy, and recovery were assessed to verify this method. The results showed that the developed method is rapid, sensitive, and reliable. It is suitable for the determination of chlorpyrifos in forensic toxicological analysis and clinical diagnosis.

  14. Quantitative analysis of abused drugs in physiological fluids by gas chromatography/chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Foltz, R.L.

    1978-01-01

    Methods have been developed for quantitative analysis of commonly abused drugs in physiological fluids using gas chromatography/chemical ionization mass spectrometry. The methods are being evaluated in volunteer analytical and toxicological laboratories, and analytical manuals describing the methods are being prepared. The specific drug and metabolites included in this program are: Δ 9 -tetrahydrocannabinol, methadone, phencyclidine, methaqualone, morphine, amphetamine, methamphetamine, mescaline, 2,5-dimethoxy-4-methyl amphetamine, cocaine, benzoylecgonine, diazepam, and N-desmethyldiazepam. The current analytical methods utilize relatively conventional instrumentation and procedures, and are capable of measuring drug concentrations as low as 1 ng/ml. Various newer techniques such as sample clean-up by high performance liquid chromatography, separation by glass capillary chromatography, and ionization by negative ion chemical ionization are being investigated with respect to their potential for achieving higher sensitivity and specificity, as well as their ability to facilitate simultaneous analysis of more than one drug and metabolite. (Auth.)

  15. The Neutral Gas and Ion Mass Spectrometer on the Mars Atmosphere and Volatile Evolution Mission

    Science.gov (United States)

    Mahaffy, Paul R.; Benna, Mehdi; King, Todd; Harpold, Daniel N.; Arvey, Robert; Barciniak, Michael; Bendt, Mirl; Carrigan, Daniel; Errigo, Therese; Holmes, Vincent; Johnson, Christopher S.; Kellogg, James; Kimvilakani, Patrick; Lefavor, Matthew; Hengemihle, Jerome; Jaeger, Ferzan; Lyness, Eric; Maurer, John; Melak, Anthony; Noreiga, Felix; Noriega, Marvin; Patel, Kiran; Prats, Benito; Raaen, Eric; Tan, Florence; Weidner, Edwin; Gundersen, Cynthia; Battel, Steven; Block, Bruce P.; Arnett, Ken; Miller, Ryan; Cooper, Curt; Edmonson, Charles; Nolan, J. Thomas

    2015-12-01

    The Neutral Gas and Ion Mass Spectrometer (NGIMS) of the Mars Atmosphere and Volatile Evolution Mission (MAVEN) is designed to measure the composition, structure, and variability of the upper atmosphere of Mars. The NGIMS complements two other instrument packages on the MAVEN spacecraft designed to characterize the neutral upper atmosphere and ionosphere of Mars and the solar wind input to this region of the atmosphere. The combined measurement set is designed to quantify atmosphere escape rates and provide input to models of the evolution of the martian atmosphere. The NGIMS is designed to measure both surface reactive and inert neutral species and ambient ions along the spacecraft track over the 125-500 km altitude region utilizing a dual ion source and a quadrupole analyzer.

  16. Gas-Phase Reactions of Dimethyl Disulfide with Aliphatic Carbanions - A Mass Spectrometry and Computational Study

    Science.gov (United States)

    Franczuk, Barbara; Danikiewicz, Witold

    2018-03-01

    Ion-molecule reactions of Me2S2 with a wide range of aliphatic carbanions differing by structure and proton affinity values have been studied in the gas phase using mass spectrometry techniques and DFT calculations. The analysis of the spectra shows a variety of product ions formed via different reaction mechanisms, depending on the structure and proton affinity of the carbanion. Product ions of thiophilic reaction ( m/z 47), SN2 ( m/z 79), and E2 elimination - addition sequence of reactions ( m/z 93) can be observed. Primary products of thiophilic reaction can undergo subsequent SN2 and proton transfer reactions. Gibbs free energy profiles calculated for experimentally observed reactions using PBE0/6-311+G(2d,p) method show good agreement with experimental results.

  17. Determination of long-chain fatty acids in serum by gas chromatography coupled to mass spectrometry

    International Nuclear Information System (INIS)

    Nuevas Paz, Lauro; Camayd Viera, Ivette

    2014-01-01

    The quantification of long-chain fatty acids is fundamental for the diagnosis of several peroxisome disorders, particularly those in which the β-oxidation peroxisome of fatty acids is affected. In this work the implementation of an analytical method for the determination of these markers in serum by gas chromatography coupled to mass spectrometry is described. Besides, samples from patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome were analyzed. The necessary experimental conditions were achieved for the separation and quantification of C22:0, C24:0 and C26:0 fatty acids in serum, which are biochemical markers of various peroxisome diseases. The application of this method allowed confirming the diagnosis of three patients with a diagnostic impression of adrenoleukodystrophy linked to the X chromosome. The application of the method in daily practice will allow the Cuban medical system to count on a new laboratory parameter for the diagnosis of peroxisome disorders

  18. Improvements in bis(cyclopentadienyl)magnesium purity as determined with gas chromatography-mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    BARTRAM,MICHAEL E.

    2000-03-08

    Bis(cyclopentadienyl)magnesium (MgCp2) is used commonly as a source for doping nitride materials with magnesium. Increased oxygen incorporation known to accompany the use of MgCp2 makes the purity of this precursor an important consideration in nitride CVD. Gas chromatography-mass spectroscopy (GCMS) methods have now been developed for the identification of volatile impurities in MgCp2. Diethylether, an oxygen containing organic compound (CH{sub 3}CH{sub 2}OCH{sub 2}CH{sub 3}), and additional organic impurities were found in the MgCp2 supplied by three manufacturers. Subsequent refinements in the synthetic processes by these companies have resulted in the availability of MgCp2 free of ether and other organic impurities as determined by GCMS.

  19. Fast methods for screening of trichothecenes in fungal cultures using gas chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Kristian Fog; Thrane, Ulf

    2001-01-01

    The paper presents a fast method for trichothecene profiling and chemotaxonomic studies in species of Fusarium, Stachybotrys, Trichoderma and Memnoniella. Micro scale extracted crude Fusarium extracts were derivatised using pentafluoropropionic anhydride and analysed by gas chromatography......-acetoxyscirpentriol, nivalenol, fusarenon-X, deoxynivalenol, 15-acetyl- deoxynivalenol and 3-acetyl-deoxynivalenol possible during a 23-min GC run. A slightly modified method could detect trichothecenes produced by Stachybotrys, Memnoniella and Trichoderma, by hydrolysing crude extracts prior to derivatisation...... with heptafluorobuturyl imidazole. All types of derivatised extracts could be reanalysed using negative ion chemical ionisation (NICI) GC-MS for molecular mass determination and verification purposes. A retention time index could be used for correction in retention time drifts between sequences and worked both in EI...

  20. Ionizing radiation effects in Acai oil analysed by gas chromatography coupled to mass spectrometry technique

    International Nuclear Information System (INIS)

    Valli, Felipe; Fernandes, Carlos Eduardo; Moura, Sergio; Machado, Ana Carolina; Furasawa, Helio Akira; Pires, Maria Aparecida Faustino; Bustillos, Oscar Vega

    2007-01-01

    The Acai fruit is a well know Brazilian seed plant used in large scale as a source of feed stock, specially in the Brazilian North-east region. The Acai oil is use in many purposes from fuel sources to medicine. The scope of this paper is to analyzed the chemical structures modification of the acai oil after the ionizing radiation. The radiation were set in the range of 10 to 25 kGy in the extracted Acai oil. The analyses were made by gas chromatography coupled to mass spectrometry techniques. A GC/MS Shimatzu QP-5000 equipped with 30 meters DB-5 capillary column with internal diameter of 0.25 mm and 0.25 μm film thickness was used. Helium was used as carried gas and gave a column head pressure of 12 p.s.i. (1 p.s.i. = 6894.76 Pa) and an average flux of 1 ml/min. The temperature program for the GC column consisted of a 4-minutes hold at 75 deg C, a 15 deg C /min ramp to 200 deg C, 8 minutes isothermal. 20 deg C/min ramp to 250 deg C, 2 minutes isothermal. The extraction of the fatty acids was based on liquid-liquid method using chloroform as solvent. The chromatograms resulted shows the presences of the oleic acid and others fatty acids identify by the mass spectra library (NIST-92). The ionization radiation deplete the fatty acids presents in the Acai oil. Details on the chemical qualitative analytical is present as well in this work. (author)

  1. Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

    2011-09-09

    Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

  2. Effect of dimethylamine on the gas phase sulfuric acid concentration measured by Chemical Ionization Mass Spectrometry.

    Science.gov (United States)

    Rondo, L; Ehrhart, S; Kürten, A; Adamov, A; Bianchi, F; Breitenlechner, M; Duplissy, J; Franchin, A; Dommen, J; Donahue, N M; Dunne, E M; Flagan, R C; Hakala, J; Hansel, A; Keskinen, H; Kim, J; Jokinen, T; Lehtipalo, K; Leiminger, M; Praplan, A; Riccobono, F; Rissanen, M P; Sarnela, N; Schobesberger, S; Simon, M; Sipilä, M; Smith, J N; Tomé, A; Tröstl, J; Tsagkogeorgas, G; Vaattovaara, P; Winkler, P M; Williamson, C; Wimmer, D; Baltensperger, U; Kirkby, J; Kulmala, M; Petäjä, T; Worsnop, D R; Curtius, J

    2016-03-27

    Sulfuric acid is widely recognized as a very important substance driving atmospheric aerosol nucleation. Based on quantum chemical calculations it has been suggested that the quantitative detection of gas phase sulfuric acid (H 2 SO 4 ) by use of Chemical Ionization Mass Spectrometry (CIMS) could be biased in the presence of gas phase amines such as dimethylamine (DMA). An experiment (CLOUD7 campaign) was set up at the CLOUD (Cosmics Leaving OUtdoor Droplets) chamber to investigate the quantitative detection of H 2 SO 4 in the presence of dimethylamine by CIMS at atmospherically relevant concentrations. For the first time in the CLOUD experiment, the monomer sulfuric acid concentration was measured by a CIMS and by two CI-APi-TOF (Chemical Ionization-Atmospheric Pressure interface-Time Of Flight) mass spectrometers. In addition, neutral sulfuric acid clusters were measured with the CI-APi-TOFs. The CLOUD7 measurements show that in the presence of dimethylamine (sulfuric acid monomer measured by the CIMS represents only a fraction of the total H 2 SO 4 , contained in the monomer and the clusters that is available for particle growth. Although it was found that the addition of dimethylamine dramatically changes the H 2 SO 4 cluster distribution compared to binary (H 2 SO 4 -H 2 O) conditions, the CIMS detection efficiency does not seem to depend substantially on whether an individual H 2 SO 4 monomer is clustered with a DMA molecule. The experimental observations are supported by numerical simulations based on A Self-contained Atmospheric chemistry coDe coupled with a molecular process model (Sulfuric Acid Water NUCleation) operated in the kinetic limit.

  3. Development of a technique for mercury speciation and quantification using gas chromatography/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Barshick, S.A.; Barshick, C.M.; Britt, P.F.; Vance, M.A.; Duckworth, D.C.

    1997-07-01

    One element of concern to DOE is mercury. Mercury was used extensively at the DOE facilities in Oak Ridge, Tennessee from 1950 to 1963 in the process of making lithium deuteride, a component of nuclear weapons. Although both the inorganic and organometallic forms of mercury are toxic to humans, the organic compounds are often more toxic. Since the toxicity of mercury is a function of its chemical form, an understanding of the interactions between commercially discharged mercury, naturally occurring mercury, and the environment in which they are present is vital. In this report, the authors have been investigating gas chromatography/mass spectrometry (GC/MS) for the analysis of both the organometallic and inorganic forms of mercury in the same environmental sample (e.g., solutions, soils, and sludges). Although gas chromatography is the classical technique for analyzing organic molecules, (e.g., organometallic compounds) little has been done on the analysis of inorganic compounds. In a previous publication, the authors described how a solid phase microextraction (SPME) fiber could be used to sample organomercurials from aqueous samples. An alkylation reaction was then carried out to transform chemically mercury nitrate into dimethylmercury; subsequent GC/MS analysis of this compound permitted quantification of the inorganic constituent. Subsequently, several different alkylation reagents have been synthesized that methylate any inorganic mercury compound to methylmercury iodide. Here, the authors report results on alkylation reaction time and the effect of pH on the population of the product.

  4. Oxysterols in cosmetics-Determination by planar solid phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Schrack, S; Hohl, C; Schwack, W

    2016-11-18

    Sterol oxidation products (SOPs) are linked to several toxicological effects. Therefore, investigation of potential dietary uptake sources particularly food of animal origin has been a key issue for these compounds. For the simultaneous determination of oxysterols from cholesterol, phytosterols, dihydrolanosterol and lanosterol in complex cosmetic matrices, planar solid phase extraction (pSPE) was applied as clean-up tool. SOPs were first separated from more non-polar and polar matrix constituents by normal phase thin-layer chromatography and then focussed into one target zone. Zone extraction was performed with the TLC-MS interface, followed by gas chromatography-mass spectrometry analysis. pSPE showed to be effective for cleaning up cosmetic samples as sample extracts were free of interferences, and gas chromatographic columns did not show any signs of overloading. Recoveries were between 86 and 113% with relative standard deviations of below 10% (n=6). Results of our market survey in 2016 showed that some cosmetics with ingredients of plant origin contained phytosterol oxidation products (POPs) in the low ppm range and therefore in line with levels reported for food. In lanolin containing products, total SOPs levels (cholesterol oxidation products (COPs), lanosterol oxidation products (LOPs), dihydrolanosterol oxidation products (DOPs)) being in the low percent range exceeded reported levels for food by several orders of magnitudes. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Mantle rare gas relative abundances in a steady-state mass transport model

    Science.gov (United States)

    Porcelli, D.; Wasserburg, G. J.

    1994-01-01

    A model for He and Xe was presented previously which incorporates mass transfer of rare gases from an undegassed lower mantle (P) and the atmosphere into a degassed upper mantle (D). We extend the model to include Ne and Ar. Model constraints on rare gas relative abundances within P are derived. Discussions of terrestrial volatile acquisition have focused on the rare gas abundance pattern of the atmosphere relative to meteoritic components, and the pattern of rare gases still trapped in the Ear,th is important in identifying volatile capture and loss processes operating during Earth formation. The assumptions and principles of the model are discussed in Wasserburg and Porcelli (this volume). For P, the concentrations in P of the decay/nuclear products 4 He, 21 Ne, 40 Ar, and 136 Xe can be calculated from the concentrations of the parent elements U, Th, K, and Pu. The total concentration of the daughter element in P is proportional to the isotopic shifts in P. For Ar, ((40)Ar/(36)Ar)p - ((40)Ar/(36)Ar)o =Delta (exp 40) p= 40 Cp/(exp 36)C where(i)C(sub j) the concentration of isotope i in j. In D, isotope compositions are the result of mixing rare gases from P, decay/nuclear products generated in the upper mantle, and subducted rare gases (for Ar and Xe).

  6. [Determination of olive oil content in olive blend oil by headspace gas chromatography-mass spectrometry].

    Science.gov (United States)

    Jiang, Wanfeng; Zhang, Ning; Zhang, Fengyan; Yang, Zhao

    2017-07-08

    A method for the determination of the content of olive oil in olive blend oil by headspace gas chromatography-mass spectrometry (SH-GC/MS) was established. The amount of the sample, the heating temperature, the heating time, the amount of injection, the injection mode and the chromatographic column were optimized. The characteristic compounds of olive oil were found by chemometric method. A sample of 1.0 g was placed in a 20 mL headspace flask, and heated at 180℃ for 2700 s. Then, 1.0 mL headspace gas was taken into the instrument. An HP-88 chromatographic column was used for the separation and the analysis was performed by GC/MS. The results showed that the linear range was 0-100%(olive oil content). The linear correlation coefficient ( r 2 ) was more than 0.995, and the limits of detection were 1.26%-2.13%. The deviations of olive oil contents in the olive blend oil were from -0.65% to 1.02%, with the relative deviations from -1.3% to 6.8% and the relative standard deviations from 1.18% to 4.26% ( n =6). The method is simple, rapid, environment friendly, sensitive and accurate. It is suitable for the determination of the content of olive oil in olive blend oil.

  7. Gas Chromatography-Mass Spectroscopy Study of tert-Butylarsine Stability and Purification

    Energy Technology Data Exchange (ETDEWEB)

    Bartram, M.E.; Breiland, W.G.; Bruskas, L.A.; Killeen, K.P.

    1999-07-20

    TBA (tert-butylarsine, H{sub 2}AsC(CH{sub 3}){sub 3}) has been demonstrated to be an effective arsenic precursor for the deposition of compound semiconductors such as GaAs by MOCVD (metal organic chemical vapor deposition). TBA is used as a liquid (bubbler) source in MOCVD and is a less toxic alternative to the more commonly used gaseous arsine (AsH{sub 3}). Materials and device performance using TBA have in many cases equaled or surpassed those using arsine. This includes the first observation of fractional quantum Hall behavior in a two dimensional electron gas structure grown by MOCVD. Despite the beneficial characteristics, the use of TBA in our laboratories has revealed some inconsistent behavior. Small pressure rises have been observed in the TBA bubbler sources when left unused over a period of many days. Measurements of the TBA partial pressure using UV absorption revealed that new absorption peaks could be observed after storage. The features of the absorption profile were insufficient to ascribe to a specific chemical species. Attempts to remove the gaseous impurities with liquid nitrogen freeze-pump-thaw techniques had limited success. Unfortunately, there is no published information on the room temperature decomposition of TBA. In this paper, we present a series of GCMS (gas chromatography-mass spectroscopy) analyses designed to determine the stability of TBA and identify its decomposition products in storage containers. The GCMS is also used to evaluate several methods for in-situ purification of TBA.

  8. Gas-phase pesticide measurement using iodide ionization time-of-flight mass spectrometry

    Science.gov (United States)

    Murschell, Trey; Fulgham, S. Ryan; Farmer, Delphine K.

    2017-06-01

    Volatilization and subsequent processing in the atmosphere are an important environmental pathway for the transport and chemical fate of pesticides. However, these processes remain a particularly poorly understood component of pesticide lifecycles due to analytical challenges in measuring pesticides in the atmosphere. Most pesticide measurements require long (hours to days) sampling times coupled with offline analysis, inhibiting observation of meteorologically driven events or investigation of rapid oxidation chemistry. Here, we present chemical ionization time-of-flight mass spectrometry with iodide reagent ions as a fast and sensitive measurement of four current-use pesticides. These semi-volatile pesticides were calibrated with injections of solutions onto a filter and subsequently volatilized to generate gas-phase analytes. Trifluralin and atrazine are detected as iodide-molecule adducts, while permethrin and metolachlor are detected as adducts between iodide and fragments of the parent analyte molecule. Limits of detection (1 s) are 0.37, 0.67, 0.56, and 1.1 µg m-3 for gas-phase trifluralin, metolachlor, atrazine, and permethrin, respectively. The sensitivities of trifluralin and metolachlor depend on relative humidity, changing as much as 70 and 59, respectively, as relative humidity of the sample air varies from 0 to 80 %. This measurement approach is thus appropriate for laboratory experiments and potentially near-source field measurements.

  9. Gas-phase pesticide measurement using iodide ionization time-of-flight mass spectrometry

    Directory of Open Access Journals (Sweden)

    T. Murschell

    2017-06-01

    Full Text Available Volatilization and subsequent processing in the atmosphere are an important environmental pathway for the transport and chemical fate of pesticides. However, these processes remain a particularly poorly understood component of pesticide lifecycles due to analytical challenges in measuring pesticides in the atmosphere. Most pesticide measurements require long (hours to days sampling times coupled with offline analysis, inhibiting observation of meteorologically driven events or investigation of rapid oxidation chemistry. Here, we present chemical ionization time-of-flight mass spectrometry with iodide reagent ions as a fast and sensitive measurement of four current-use pesticides. These semi-volatile pesticides were calibrated with injections of solutions onto a filter and subsequently volatilized to generate gas-phase analytes. Trifluralin and atrazine are detected as iodide–molecule adducts, while permethrin and metolachlor are detected as adducts between iodide and fragments of the parent analyte molecule. Limits of detection (1 s are 0.37, 0.67, 0.56, and 1.1 µg m−3 for gas-phase trifluralin, metolachlor, atrazine, and permethrin, respectively. The sensitivities of trifluralin and metolachlor depend on relative humidity, changing as much as 70 and 59, respectively, as relative humidity of the sample air varies from 0 to 80 %. This measurement approach is thus appropriate for laboratory experiments and potentially near-source field measurements.

  10. Comparative study of radio gas-chromatography and gas chromatography - mass spectrometry coupling in the identification of metabolites of estrogens and progesterone

    International Nuclear Information System (INIS)

    Adessi, G.; Nhuan, T.Q.; Jayle, M.F.

    1978-01-01

    Radio-gas chromatography (RGC) and gas chromatography-mass spectrometry (GC-MS) were used to identify estrogen and progesterone metabolites. The RGC enables the identification of metabolites of labelled precursors ( 3 H)-estradiol-17β and ( 14 C)-progesterone were used as precursors. The GC-MS analytical technique with mass fragmentography, offers the interest of using unlabelled precursors at physiological levels. The identification of metabolites was based on obtaining the mass spectrum or the compiled fragmentogram on the basis of the most characteristic fragment ions. More over, several metabolites can be quantified on the same fragmentogram. Results on the metabolism of estradiol-17β and progesterone by the hepatic tissue of guinea pigs are given. (Auth.)

  11. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics.

    Science.gov (United States)

    Pacáková, V; Leclercq, P A

    1991-08-30

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the products.

  12. The Low Mass of Mars: First Evidence of Early Gas-Driven Migration by Jupiter

    Science.gov (United States)

    Walsh, K. J.; Morbidelli, A.; Raymond, S. N.; O'Brien, D. P.; Mandell, A. M.

    2010-12-01

    Numerical simulations of planetary accretion have succeeded in matching most of the physical and orbital properties of the terrestrial planets with one glaring exception: they categorically form Mars analogs that are roughly an order of magnitude too massive (Raymond et al. 2009). The initial conditions that best reproduce the mass of Mars require that the inner planetesimal disk had an outer edge at 1 Astronomical Unit (AU) (Hansen 2009). To date, no mechanism has been shown to create this edge and remain compatible with the current-day solar system, in particular the existence of the asteroid belt. Here we show that a substantial gas-driven radial migration of the giant planets is the needed mechanism. Hydrodynamical simulations show that the evolution of Jupiter and Saturn in a gas-disk generically leads to a two-stage, inward-then-outward, migration where the extent of each stage of migration depends on a priori unconstrained disk parameters (Masset & Snellgrove 2001, Morbidelli et al. 2007, Pierens & Nelson 2008). We demonstrate with numerical simulations that, if Jupiter migrated inwards to 1.5 AU before migrating out towards its current location, its gravitational influence would truncate the inner planetesimal disk at 1 AU. The resulting disk naturally reproduces all the terrestrial planets including Mars. During the giant planets' migration, the asteroid belt is emptied and later re-populated from two distinct parent populations. This provides the first dynamical explanation for the current dichotomy of physical properties of the main asteroid belt, with anhydrous asteroids (S-type) in the inner part and primitive asteroids (C-type) in the outer part (Gradie & Tedesco 1982). Our model links the origin of the inner solar system -- explaining the mass of Mars and the properties of the asteroid belt -- to a realistic evolution of the giant planets. Thus Mars and the asteroid belt provide the first evidence for an early solar system evolution characterized by

  13. [Determination of fenfluramine, diethylpropion and mazindol in slimming foods by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Feng, Jiali; Pan, Zhenqiu; Cao, Huajuan; Wang, Chun'e

    2004-05-01

    A gas chromatography-mass spectrometry (GC/MS) analytical method for three anorectics drugs, fenfluramine, diethylpropion and mazindol, illegally adulterated in slimming foods has been developed. They can be simultaneously identified and quantified. The samples were extracted with chloroform, and then separated by GC with an HP-5MS GC capillary column. The temperature programming was started at 70 degrees C. The temperature was held at this temperature for 2 min and then increased at 10 degrees C/min to 280 degrees C. The completely separated peaks were identified by MS with a quadrupole mass filter and quantitated in selected ion monitoring mode. Compared with the NIST98 library, the matching qualities of the drugs in foods were all over 90%. The calibration curves of the drugs were excellent with correlation coefficients between 0.9991 and 0.9999, and relative standard deviations between 1.6% and 2.2%. The recoveries were between 96.0% and 102.4%. The results demonstrated that this method is suitable for the identification and quantitation of these anorectics drugs in slimming foods.

  14. Gas chromatographic-mass spectrometric urinary metabolome analysis to study mutations of inborn errors of metabolism.

    Science.gov (United States)

    Kuhara, Tomiko

    2005-01-01

    Urine contains numerous metabolites, and can provide evidence for the screening or molecular diagnosis of many inborn errors of metabolism (IEMs). The metabolomic analysis of urine by the combined use of urease pretreatment, stable-isotope dilution, and capillary gas chromatography/mass spectrometry offers reliable and quantitative data for the simultaneous screening or molecular diagnosis of more than 130 IEMs. Those IEMs include hyperammonemias and lactic acidemias, and the IEMs of amino acids, pyrimidines, purines, carbohydrates, and others including primary hyperoxalurias, hereditary fructose intolerance, propionic acidemia, and methylmalonic acidemia. Metabolite analysis is comprehensive for mutant genotypes. Enzyme dysfunction-either by the abnormal structure of an enzyme/apoenzyme, the reduced quantity of a normal enzyme/apoenzyme, or the lack of a coenzyme-is involved. Enzyme dysfunction-either by an abnormal regulatory gene, abnormal sub-cellular localization, or by abnormal post-transcriptional or post-translational modification-is included. Mutations-either known or unknown, common or uncommon-are involved. If the urine metabolome approach can accurately observe quantitative abnormality for hundreds of metabolites, reflecting 100 different disease-causing reactions in a body, then it is possible to simultaneously detect different mutant genotypes of far more than tens of thousands. (c) 2004 Wiley Periodicals, Inc., Mass Spec Rev 24:814-827, 2005.

  15. Analysis of galanthamine-type alkaloids by capillary gas chromatography-mass spectrometry in plants.

    Science.gov (United States)

    Berkov, Strahil; Bastida, Jaume; Viladomat, Francesc; Codina, Carles

    2008-01-01

    Galanthamine, an acetylcholinesterase inhibitor used for the treatment of Alzheimer's disease, and galanthamine-type alkaloids are synthesised in different plants of the family Amaryllidaceae. A capillary gas chromatographic-mass spectroscopic (CGC-MS) method for the separation of 7 galanthamine type alkaloids, including galanthamine and epigalanthamine, is described in the present paper. A simple method for the routine quantification of galanthamine in plants was developed using pre-packed columns with diatomaceous earth (Isolute HM-N), allowing simultaneous preparation of a large number of samples. Galanthamine showed excellent linearity in the range from 50 to 1000 microg/mL and the limit of quantification was 5 microg/mL in total ion current mode and 1.6 ng/mL in selected ion monitoring mode. The recovery of galanthamine was more than 90%. Interday reproducibility (RSD) of the extraction was 2.74%. A method to find and to microextract Amaryllidaceae alkaloids in low-mass plant samples is also described.

  16. Importance of enhanced mass resolution in removing interferences when measuring volatile organic compounds in human blood by using purge-and-trap gas chromatography/mass spectrometry.

    Science.gov (United States)

    Bonin, M A; Ashley, D L; Cardinali, F L; McGraw, J M; Patterson, D G

    1992-11-01

    The number of volatile organic compounds (VOCs) that can be purged from human blood is so great that they cannot be separated completely by capillary gas chromatography. As a result, the single-mass chromatograms used for quantitating the target compounds by mass spectrometry have many interferences at nominal (integer) mass resolution of a quadrupole mass spectrometer. The results of these interferences range from small errors in quantitation to completely erroneous results for the target VOCs. By using a magnetic sector mass spectrometer, these interferences at nominal mass can be removed at higher resolution by lowering the ion chromatogram windows around the masses of interest. At 3000 resolution (10% valley definition), unique single-ion chromatograms can be made for the quantitation ions of the target VOCs. Full-scan mass data are required to allow the identification of unknown compounds purged from the blood. By using isotope-dilution mass spectrometry, most target VOCs can be detected in the low parts per trillion range for a 10-mL quantity of blood from which the VOCs have been removed by a purge-and-trap method.

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

    Directory of Open Access Journals (Sweden)

    Amol B Tayade

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

  18. Analysis of small carbohydrates in several bioactive botanicals by gas chromatography with mass spectrometry and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

    2015-11-01

    Bioactive botanicals contain natural compounds with specific biological activity, such as antibacterial, antioxidant, immune stimulating, and taste improving. A full characterization of the chemical composition of these botanicals is frequently necessary. A study of small carbohydrates from the plant materials of 18 bioactive botanicals is further described. The study presents the identification of the carbohydrate using a gas chromatographic-mass spectrometric analysis that allows detection of molecules as large as maltotetraose, after changing them into trimethylsilyl derivatives. A number of carbohydrates in the plant (fructose, glucose, mannose, sucrose, maltose, xylose, sorbitol, and myo-, chiro-, and scyllo-inositols) were quantitated using a novel liquid chromatography with tandem mass spectrometric technique. Both techniques involved new method developments. The gas chromatography with mass spectrometric analysis involved derivatization and separation on a Rxi(®)-5Sil MS column with H2 as a carrier gas. The liquid chromatographic separation was obtained using a hydrophilic interaction type column, YMC-PAC Polyamine II. The tandem mass spectrometer used an electrospray ionization source in multiple reaction monitoring positive ion mode with the detection of the adducts of the carbohydrates with Cs(+) ions. The validated quantitative procedure showed excellent precision and accuracy allowing the analysis in a wide range of concentrations of the analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. A new time of flight mass spectrometer for absolute dissociative electron attachment cross-section measurements in gas phase

    Science.gov (United States)

    Chakraborty, Dipayan; Nag, Pamir; Nandi, Dhananjay

    2018-02-01

    A new time of flight mass spectrometer (TOFMS) has been developed to study the absolute dissociative electron attachment (DEA) cross section using a relative flow technique of a wide variety of molecules in gas phase, ranging from simple diatomic to complex biomolecules. Unlike the Wiley-McLaren type TOFMS, here the total ion collection condition has been achieved without compromising the mass resolution by introducing a field free drift region after the lensing arrangement. The field free interaction region is provided for low energy electron molecule collision studies. The spectrometer can be used to study a wide range of masses (H- ion to few hundreds atomic mass unit). The mass resolution capability of the spectrometer has been checked experimentally by measuring the mass spectra of fragment anions arising from DEA to methanol. Overall performance of the spectrometer has been tested by measuring the absolute DEA cross section of the ground state SO2 molecule, and the results are satisfactory.

  20. A new time of flight mass spectrometer for absolute dissociative electron attachment cross-section measurements in gas phase.

    Science.gov (United States)

    Chakraborty, Dipayan; Nag, Pamir; Nandi, Dhananjay

    2018-02-01

    A new time of flight mass spectrometer (TOFMS) has been developed to study the absolute dissociative electron attachment (DEA) cross section using a relative flow technique of a wide variety of molecules in gas phase, ranging from simple diatomic to complex biomolecules. Unlike the Wiley-McLaren type TOFMS, here the total ion collection condition has been achieved without compromising the mass resolution by introducing a field free drift region after the lensing arrangement. The field free interaction region is provided for low energy electron molecule collision studies. The spectrometer can be used to study a wide range of masses (H - ion to few hundreds atomic mass unit). The mass resolution capability of the spectrometer has been checked experimentally by measuring the mass spectra of fragment anions arising from DEA to methanol. Overall performance of the spectrometer has been tested by measuring the absolute DEA cross section of the ground state SO 2 molecule, and the results are satisfactory.

  1. Quantitative assay of plasma homocysteine thiolactone by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Daneshvar, Parham; Yazdanpanah, Mehrdad; Cuthbert, Carla; Cole, David E C

    2003-01-01

    Enzymatic cyclization of homocysteine forms a reactive thiolactone that may play an important role in its cardiovascular toxicity, but reliable quantitation of the free thiolactone metabolite in physiological fluids has not been reported. We have therefore used a highly selective gas chromatography/mass spectrometry (GC/MS) technique combined with the sensitivity of negative chemical ionization (NCI) to develop a quantitative method for the detection of homocysteine thiolactone (HcyTL) in plasma. To improve accuracy the deuterated isomer d(4)-HcyTL was synthesized and added to plasma as internal standard. The plasma was then treated with silica solid-phase extraction and derivatized with heptafluorobutyric anhydride. The derivative was analyzed by GC/MS in NCI mode with methane as the reagent gas and quantified by analyzing for the HcyTL ion [M(-)[bond]HF] and its d(4)-HcyTL counterpart in single-ion monitoring mode. The calibration curve showed a dynamic linear range up to 40 nmol/L. Within-day precision (n = 20, nominal concentration 5.2 nmol/L) was 0.96% and between-day precision was 3.9%, with a detection limit of 1.7 nmol/L and quantification limit of 5.2 nmol/L. Two human plasma samples had HcyTL concentrations of 18 and 25 nmol/L. This facile method for quantitation of homocysteine thiolactone opens the way for more detailed clinical studies of its potential role in homocysteine-induced arteriosclerosis and vaso-occlusive disease. Copyright 2003 John Wiley & Sons, Ltd.

  2. Gas chromatography–triple quadrupole mass spectrometry for the determination of atmospheric polychlorinated naphthalenes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Fang [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Jin, Jing [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Sun, Xiaoli [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Wang, Xueli; Li, Yun; Shah, Syed Mazhar [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023 (China)

    2014-09-15

    Highlights: • Atmospheric PCNs were detected by isotope-dilution GC–MS/MS. • The pollution levels of PCNs covering from mono- to octa-CNs were investigated comprehensively in air samples. • The dioxin-like toxicity and human exposure levels of PCNs in air samples were estimated. - Abstract: Atmospheric polychlorinated naphthalenes (PCNs) ranging from mono-CNs to octa-CNs were detected using isotope-dilution gas chromatography coupled with triple quadrupole mass spectrometry (GC–MS/MS). The developed instrumental method was successfully applied to the determination of PCNs in technical products. It was observed that there were significant differences in concentrations, homologue profiles, chlorinated contents and total toxic equivalents (∑TEQs) of PCNs for four Halowax products. Subsequently, the validation of the analytical method was evaluated for the determination of PCNs in air samples in terms of method detection limit (MDL), recovery and matrix effect. The results demonstrated that this method could provide satisfactory sensitivity and adequate selectivity with lower cost. It was conducted to comprehensively evaluate the levels, composition patterns, ∑TEQs, and daily intake exposure of PCNs in indoor and outdoor air samples. Concentrations and ∑TEQs of PCNs in air samples ranged 47.7–832.7 pg m{sup −3} and 1.31–5.99 fg m{sup −3}, respectively, and the predominant homologues were di- and tri-CNs in the gas phase. The results indicated that this analytical method was useful for the accurate and specific evaluation of dioxin-like toxicity and human exposure levels of PCNs in the atmosphere.

  3. Detection of nerve agents using proton transfer reaction mass spectrometry with ammonia as reagent gas.

    Science.gov (United States)

    Ringer, Joachim M

    2013-01-01

    The chemical warfare agents (CWA) Sarin, Soman, Cyclosarin and Tabun were characterised by proton transfer mass spectrometry (PTRMS). It was found that PTRMS is a suitable technique to detect nerve agents highly sensitively, highly selectively and in near real-time. Methods were found to suppress molecule fragmentation which is significant under PTRMS hollow cathode ionisation conditions. In this context, the drift voltage (as one of the most important system parameters) was varied and ammonia was introduced as an additional chemical reagent gas. Auxiliary chemicals such as ammonia affect ionisation processes and are quite common in context with detectors for CWAs based on ion mobility spectrometry (IMS). With both, variation of drift voltage and ammonia as the reagent gas, fragmentation can be suppressed effectively. Suppression of fragmentation is crucial particularly concerning the implementation of an algorithm for automated agent identification in field applications. On the other hand, appearance of particular fragments might deliver additional information. Degradation and rearrangement products of nerve agents are not distinctive for the particular agent but for the chemical class they belong to. It was found that switching between ammonia doped and ordinary water ionisation chemistry can easily be performed within a few seconds. Making use of this effect it is possible to switch between fragment and molecular ion peak spectra. Thus, targeted fragmentation can be used to confirm identification based only on single peak detection. PTRMS turned out to be a promising technique for future CWA detectors. In terms of sensitivity, response time and selectivity (or confidence of identification, respectively) PTRMS performs as a bridging technique between IMS and GC-MS.

  4. TRACING MOLECULAR GAS MASS IN EXTREME EXTRAGALACTIC ENVIRONMENTS: AN OBSERVATIONAL STUDY

    International Nuclear Information System (INIS)

    Zhu Ming; Papadopoulos, Padeli P.; Xilouris, Emmanuel M.; Kuno, Nario; Lisenfeld, Ute

    2009-01-01

    We present a new observational study of the 12 CO(1-0) line emission as an H 2 gas mass tracer under extreme conditions in extragalactic environments. Our approach is to study the full neutral interstellar medium (H 2 , H I, and dust) of two galaxies whose bulk interstellar medium (ISM) resides in environments that mark (and bracket) the excitation extremes of the ISM conditions found in infrared luminous galaxies, the starburst NGC 3310, and the quiescent spiral NGC 157. Our study maintains a robust statistical notion of the so-called X = N(H 2 )/I CO factor (i.e., a large ensemble of clouds is involved) while exploring its dependence on the very different average ISM conditions prevailing within these two systems. These are constrained by fully sampled 12 CO(3-2) and 12 CO(1-0) observations, at a matched beam resolution of half-power beam width ∼15'', obtained with the James Clerk Maxwell Telescope (JCMT) on Mauna Kea (Hawaii) and the 45 m telescope of the Nobeyama Radio Observatory in Japan, combined with sensitive 850 μm and 450 μm dust emission and H I interferometric images which allow a complete view of all the neutral ISM components. Complementary 12 CO(2-1) observations were obtained with the JCMT toward the center of the two galaxies. We found an X factor varying by a factor of 5 within the spiral galaxy NGC 157 and about two times lower than the Galactic value in NGC 3310. In addition, the dust emission spectrum in NGC 3310 shows a pronounced submillimeter 'excess'. We tried to fit this excess by a cold dust component but very low temperatures were required (T C ∼ 5-11 K) with a correspondingly low gas-to-dust mass ratio of ∼5-43. We furthermore show that it is not possible to maintain the large quantities of dust required at these low temperatures in this starburst galaxy. Instead, we conclude that the dust properties need to be different from Galactic dust in order to fit the submillimeter 'excess'. We show that the dust spectral energy

  5. Determination of glycerol concentrations and glycerol isotopic enrichments in human plasma by gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Ackermans, M. T.; Ruiter, A. F.; Endert, E.

    1998-01-01

    An analytical method is presented to determine glycerol concentrations and stable isotope tracer enrichments in human plasma after intravenous tracer infusion in a single analytical run, using gas chromatography coupled to mass spectrometry. The method uses an internal standard, which is also a

  6. ANALYSIS OF ARTEMISININ AND RELATED SESQUITERPENOIDS FROM ARTEMISIA-ANNUA L BY COMBINED GAS-CHROMATOGRAPHY MASS-SPECTROMETRY

    NARCIS (Netherlands)

    WOERDENBAG, HJ; PRAS, N; BOS, R; VISSER, JF; HENDRIKS, H; MALINGRE, TM

    1991-01-01

    The sesquiterpenoid artemisinin (3) and its biosynthetic precursors arteannuic acid (1), arteannuin B (2) and artemisitene (4) can be separated and identified by combined gas chromatography/mass spectrometry both as a mixture of reference standards as well as in extracts of Artemisia annua L. From

  7. Determination of polychlorinated terphenyls in aquatic biota and sediment with gas chromatography/mass spectrometry using negative chemical ionization.

    NARCIS (Netherlands)

    Wester, P.G.; de Boer, J.; Brinkman, U.A.T.

    1996-01-01

    Polychlorinated terphenyls (PCTs) have been determined in aquatic biota and sediments by gas chromatography/mass spectrometry using negative chemical ionization. The use of various methods of calculation is discussed. Total PCT concentrations expressed as A (Aroclor) 5442 equivalents ranged from

  8. Determination of ifosfamide, 2-and 3-dechloroethyifosfamide using gas chromatography with nitrogen-phosphorus or mass spectrometry detection

    NARCIS (Netherlands)

    Kerbusch, T; Jeuken, MJ; Derraz, J; van Putten, JWG; Huitema, ADR; Beijnen, JH

    2000-01-01

    A comparison was made between methods for determining ifosfamide (IF), 2- (2DCE) and 3-dechloroethylifosfamide (3DCE) using gas chromatography with nitrogen-phosphorus detection (GC-NPD) versus positive ion electron-impact ion-trap mass spectrometry (GC-MS'). Sample pretreatment involved

  9. Application of the penetration theory for gas - Liquid mass transfer without liquid bulk : Differences with system with a bulk

    NARCIS (Netherlands)

    van Elk, E. P.; Knaap, M. C.; Versteeg, G. F.

    2007-01-01

    Frequently applied micro models for gas-liquid mass transfer all assume the presence of a liquid bulk. However, some systems are characterized by the absence of a liquid bulk, a very thin layer of liquid flows over a solid surface. An example of such a process is absorption in a column equipped with

  10. c2d Spitzer IRS spectra of embedded low-mass young stars : gas-phase emission lines

    NARCIS (Netherlands)

    Lahuis, F.; van Dishoeck, E. F.; Jorgensen, J. K.; Blake, G. A.; Evans, N. J.

    Context. A survey of mid-infrared gas-phase emission lines of H(2), H(2)O and various atoms toward a sample of 43 embedded low-mass young stars in nearby star-forming regions is presented. The sources are selected from the Spitzer "Cores to Disks" (c2d) legacy program. Aims. The environment of

  11. Interfacing a gas proportional counter with a mass spectrometer: Simultaneous display of GC/MS and radiocarbon data

    International Nuclear Information System (INIS)

    Peterson, G.S.; Laemmerhirt, D.F.; Weaver, A.

    1985-01-01

    To facilitate the location of pesticides and monitor their metabolism in environmental and biological systems, carbon-14 labelling of the parent compound is used. Detection of the radiolabel is achieved using a gas proportional counter, while identification of the labelled components is most easily accomplished with mass spectrometry. However, when these two operations are performed separately, correlation of the information is awkward, at best. Since each is a destructive detector, simultaneous monitoring of the outposts requires an effluent splitter. The complete system consists of a variable splitter, which allows control of the ratio of the GC effluent to the two instruments, and signal processing circuitry for simultaneous recording and storage of radiocarbon and mass spectral data. Modifications to a Finnigan GC/MS and Gas Proportional Counter included a high temperature GC effluent splitter with glass-lined connecting tubing, and a data interface, including analog to digital and serial to parallel conversions with optical isolation between the gas proportional counter and the computer. The splitter restricted the flow to the mass spectrometer, preventing flow completely in the closed position. The split was adjusted to maximize flow to the mass spectrometer using the vacuum as a rough guide (1.0 x 10 -5 torr in EI, 7.5 x 10 -5 torr in CI). A heated transfer line between the transfer oven and gas proportional counter prevented condensation of eluting components prior to radiocarbon detection

  12. Advantages of Atmospheric Pressure Chemical Ionization in Gas Chromatography Tandem Mass Spectrometry: Pyrethroid Insecticides as a Case Study

    NARCIS (Netherlands)

    Portolés, T.; Mol, J.G.J.; Sancho, J.V.; Hernández, F.

    2012-01-01

    Gas chromatography coupled to mass spectrometry (GC/MS) has been extensively applied for determination of volatile, nonpolar, compounds in many applied fields like food safety, environment, or toxicology. The wide majority of methods reported use electron ionization (EI), which may result in

  13. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  14. Simultaneous determination of the intermediates of the citric acid cycle by gas chromatography--mass fragmentography using deuterated internal standards

    International Nuclear Information System (INIS)

    Lee, C.R.; Pollitt, R.J.

    1977-01-01

    Current developments in the use of gas chromatography and mass spectroscopy in studying the intermediates in the Krebs tricarboxylic acid cycle are outlined. The methods developed make use of deuterated internal standards and multiple-ion monitoring to obtain sensitivity comparable to that of the better fluorimetric enzymatic assays. The problems still remaining are indicated

  15. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  16. Gas chromatography-mass spectrometry analysis of effects of dietary fish oil on total fatty acid composition in mouse skin

    OpenAIRE

    Peiru Wang; Min Sun; Jianwei Ren; Zora Djuric; Gary J. Fisher; Xiuli Wang; Yong Li

    2017-01-01

    Altering the fatty acid (FA) composition in the skin by dietary fish oil could provide therapeutic benefits. Although it has been shown that fish oil supplementation enhances EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid) abundance in the skin, comprehensive skin FA profiling is needed. We established a gas chromatography-mass spectrometry method, which allows precise quantification of FA profile using small (

  17. Preventive doping control analysis: Liquid and gas chromatography time-to-flight mass spectrometry for detection of designer steriods

    NARCIS (Netherlands)

    Georgakopoulos, C.G.; Vonaparti, A.; Stamou, M.; Kiousi, P.; Lyris, E.; Angelis, Y.S.; Tsoupras, G.; Wuest, B.; Nielen, M.W.F.; Panderi, I.; Koupparis, M.

    2007-01-01

    A new combined doping control screening method for the analysis of anabolic steroids in human urine using liquid chromatography/electrospray ionization orthogonal acceleration time-of-flight mass spectrometry (LCoaTOFMS) and gas chromatography/electron ionization orthogonal acceleration

  18. Molecular analysis of intact preen waxes of Calidris canutus (Aves : Scolopacidae) by gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Dekker, MHA; Piersma, T; Damste, JSS; Dekker, Marlèn H.A.; Sinninghe Damsté, Jaap S.

    The intact preen wax esters of the red knot Calidris canutus were studied with gas chromatography/mass spectrometry (GC/MS) and GC/MS/MS. In this latter technique, transitions from the molecular ion to fragment ions representing the fatty acid moiety of the wax esters were measured, providing

  19. Characterization of lipids in complex samples using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry

    NARCIS (Netherlands)

    Jover, E.; Adahchour, M.; Bayona, J.M.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2005-01-01

    Most lipids are a complex mixture of classes of compounds such as fatty acids, fatty alcohols, diols, sterols and hydroxy acids. In this study, the suitability of comprehensive two-dimensional gas chromatography coupled to a time-of-light mass spectrometer is studied for lipid characterization in

  20. Introducing Students to Gas Chromatography-Mass Spectrometry Analysis and Determination of Kerosene Components in a Complex Mixture

    Science.gov (United States)

    Pacot, Giselle Mae M.; Lee, Lyn May; Chin, Sung-Tong; Marriott, Philip J.

    2016-01-01

    Gas chromatography-mass spectrometry (GC-MS) and GC-tandem MS (GC-MS/MS) are useful in many separation and characterization procedures. GC-MS is now a common tool in industry and research, and increasingly, GC-MS/MS is applied to the measurement of trace components in complex mixtures. This report describes an upper-level undergraduate experiment…

  1. An Advanced Analytical Chemistry Experiment Using Gas Chromatography-Mass Spectrometry, MATLAB, and Chemometrics to Predict Biodiesel Blend Percent Composition

    Science.gov (United States)

    Pierce, Karisa M.; Schale, Stephen P.; Le, Trang M.; Larson, Joel C.

    2011-01-01

    We present a laboratory experiment for an advanced analytical chemistry course where we first focus on the chemometric technique partial least-squares (PLS) analysis applied to one-dimensional (1D) total-ion-current gas chromatography-mass spectrometry (GC-TIC) separations of biodiesel blends. Then, we focus on n-way PLS (n-PLS) applied to…

  2. Mass transfer with complex chemical reaction in gas-liquid systems - I. Consecutive reversible reactions with equal diffusivities

    NARCIS (Netherlands)

    Vas bhat, R.D.; van Swaaij, Willibrordus Petrus Maria; Kuipers, J.A.M.; Versteeg, Geert

    1999-01-01

    A fundamental description of gas¿liquid mass transfer with reversible consecutive reaction has been derived. The Higbie penetration theory has been used and numerical simulations were carried out for isothermal absorption. Although the model can be adapted to reactions of general stoichiometric and

  3. Determining the Probability of Achieving a Successful Quantitative Analysis for Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Pinkerton, David K; Reaser, Brooke C; Berrier, Kelsey L; Synovec, Robert E

    2017-09-19

    A new approach is presented to determine the probability of achieving a successful quantitative analysis for gas chromatography coupled with mass spectrometry (GC-MS). The proposed theory is based upon a probabilistic description of peak overlap in GC-MS separations to determine the probability of obtaining a successful quantitative analysis, which has its lower limit of chromatographic resolution R s at some minimum chemometric resolution, R s *; that is to say, successful quantitative analysis can be achieved when R s ≥ R s *. The value of R s * must be experimentally determined and is dependent on the chemometric method to be applied. The approach presented makes use of the assumption that analyte peaks are independent and randomly distributed across the separation space or are at least locally random, namely, that each analyte represents an independent Bernoulli random variable, which is then used to predict the binomial probability of successful quantitative analysis. The theoretical framework is based on the chromatographic-saturation factor and chemometric-enhanced peak capacity. For a given separation, the probability of quantitative success can be improved via two pathways, a chromatographic-efficiency pathway that reduces the saturation of the sample and a chemometric pathway that reduces R s * and improves the chemometric-enhanced peak capacity. This theory is demonstrated through a simulation-based study to approximate the resolution limit, R s *, of multivariate curve resolution-alternating least-squares (MCR-ALS). For this study, R s * was determined to be ∼0.3, and depending on the analytical expectations for the quantitative bias and the obtained mass-spectral match value, a lower value of R s * ∼ 0.2 may be achievable.

  4. The Morphologies and Alignments of Gas, Mass, and the Central Galaxies of CLASH Clusters of Galaxies

    Science.gov (United States)

    Donahue, Megan; Ettori, Stefano; Rasia, Elena; Sayers, Jack; Zitrin, Adi; Meneghetti, Massimo; Voit, G. Mark; Golwala, Sunil; Czakon, Nicole; Yepes, Gustavo; Baldi, Alessandro; Koekemoer, Anton; Postman, Marc

    2016-03-01

    Morphology is often used to infer the state of relaxation of galaxy clusters. The regularity, symmetry, and degree to which a cluster is centrally concentrated inform quantitative measures of cluster morphology. The Cluster Lensing and Supernova survey with Hubble Space Telescope (CLASH) used weak and strong lensing to measure the distribution of matter within a sample of 25 clusters, 20 of which were deemed to be “relaxed” based on their X-ray morphology and alignment of the X-ray emission with the Brightest Cluster Galaxy. Toward a quantitative characterization of this important sample of clusters, we present uniformly estimated X-ray morphological statistics for all 25 CLASH clusters. We compare X-ray morphologies of CLASH clusters with those identically measured for a large sample of simulated clusters from the MUSIC-2 simulations, selected by mass. We confirm a threshold in X-ray surface brightness concentration of C ≳ 0.4 for cool-core clusters, where C is the ratio of X-ray emission inside 100 h70-1 kpc compared to inside 500 {h}70-1 kpc. We report and compare morphologies of these clusters inferred from Sunyaev-Zeldovich Effect (SZE) maps of the hot gas and in from projected mass maps based on strong and weak lensing. We find a strong agreement in alignments of the orientation of major axes for the lensing, X-ray, and SZE maps of nearly all of the CLASH clusters at radii of 500 kpc (approximately 1/2 R500 for these clusters). We also find a striking alignment of clusters shapes at the 500 kpc scale, as measured with X-ray, SZE, and lensing, with that of the near-infrared stellar light at 10 kpc scales for the 20 “relaxed” clusters. This strong alignment indicates a powerful coupling between the cluster- and galaxy-scale galaxy formation processes.

  5. Stable chlorine isotope analysis of chlorinated acetic acids using gas chromatography/quadrupole mass spectrometry.

    Science.gov (United States)

    Miska, Milena E; Shouakar-Stash, Orfan; Holmstrand, Henry

    2015-12-30

    The environmental occurrence of chlorinated acetic acids (CAAs) has been extensively studied, but the sources and transport are still not yet fully understood. A promising approach for source apportionment and process studies is the isotopic characterization of target compounds. We present the first on-line stable chlorine isotope analysis of CAAs by use of gas chromatography/quadrupole mass spectrometry (GC/qMS). Following approved procedures for concentration analysis, CAAs extracted into MTBE were methylated to GC-amenable methyl esters (mCAAs). These mCAAs were then analyzed by GC/qMS for their stable chlorine isotope composition using a sample/standard-bracketing approach (CAA standards in the range δ(37) Cl -6.3 to -0.2 ‰, Standard Mean Ocean Chloride). Cross-calibration of the herein presented method with off-line reference methods (thermal ionization and continuous-flow GC isotope ratio mass spectrometry; TI-MS and CF-GC/IRMS, respectively) shows good agreement between the methods (regression slope for GC/qMS vs reference method data sets: 0.92 ± 0.29). Sample amounts as small as 10 pmol Cl can herewith be analyzed with a precision of 0.1 to 0.4 ‰. This method should be useful for environmental studies of CAAs at ambient concentrations in precipitations (<0.06 to 100 nmol L(-1) ), surface waters (<0.2 to 5 nmol L(-1) ) and soil (<0.6 to 2000 nmol kg(-1) dry soil) where conventional off-line methods cannot be applied. Copyright © 2015 John Wiley & Sons, Ltd.

  6. Assessment of a combined gas chromatography mass spectrometer sensor system for detecting biologically relevant volatile compounds.

    Science.gov (United States)

    Gould, Oliver; Wieczorek, Tom; de Lacy Costello, Ben; Persad, Raj; Ratcliffe, Norman

    2017-12-06

    There have been a number of studies in which metal oxide sensors (MOS) have replaced conventional analytical detectors in gas chromatography systems. However, despite the use of these instruments in a range of applications including breath research the sensor responses (i.e. resistance changes w.r.t. concentration of VCs) remain largely unreported. This paper addresses that issue by comparing the response of a metal oxide sensor directly with a mass spectrometer (MS), whereby both detectors are interfaced to the same GC column using an s-swafer. It was demonstrated that the sensitivity of an in-house fabricated ZnO/SnO 2 thick film MOS was superior to a modern MS for the detection of a wide range of volatile compounds (VCs) of different functionalities and masses. Better techniques for detection and quantification of these VCs is valuable, as many of these compounds are commonly reported throughout the scientific literature. This is also the first published report of a combined GC-MS sensor system. These two different detector technologies when combined, should enhance discriminatory abilities to aid disease diagnoses using volatiles from e.g. breath, and bodily fluids. Twenty-nine chemical standards have been tested using solid phase micro-extraction; 25 of these compounds are found on human breath. In all but two instances the sensor exhibited the same or superior limit of detection compared to the MS. Twelve stool samples from healthy participants were analysed; the sensor detected, on average 1.6 peaks more per sample than the MS. Similarly, analysing the headspace of E. coli broth cultures the sensor detected 6.9 more peaks per sample versus the MS. This greater sensitivity is primarily a function of the superior limits of detection of the metal oxide sensor. This shows that systems based on the combination of chromatography systems with solid state sensors shows promise for a range of applications.

  7. A simple method to reconstruct the molar mass signal of respiratory gas to assess small airways with a double-tracer gas single-breath washout.

    Science.gov (United States)

    Port, Johannes; Tao, Ziran; Junger, Annika; Joppek, Christoph; Tempel, Philipp; Husemann, Kim; Singer, Florian; Latzin, Philipp; Yammine, Sophie; Nagel, Joachim H; Kohlhäufl, Martin

    2017-11-01

    For the assessment of small airway diseases, a noninvasive double-tracer gas single-breath washout (DTG-SBW) with sulfur hexafluoride (SF 6 ) and helium (He) as tracer components has been proposed. It is assumed that small airway diseases may produce typical ventilation inhomogeneities which can be detected within one single tidal breath, when using two tracer components. Characteristic parameters calculated from a relative molar mass (MM) signal of the airflow during the washout expiration phase are analyzed. The DTG-SBW signal is acquired by subtracting a reconstructed MM signal without tracer gas from the signal measured with an ultrasonic sensor during in- and exhalation of the double-tracer gas for one tidal breath. In this paper, a simple method to determine the reconstructed MM signal is presented. Measurements on subjects with and without obstructive lung diseases including the small airways have shown high reliability and reproducibility of this method.

  8. ATLASGAL - Kinematic distances and the dense gas mass distribution of the inner Galaxy

    Science.gov (United States)

    Wienen, M.; Wyrowski, F.; Menten, K. M.; Urquhart, J. S.; Csengeri, T.; Walmsley, C. M.; Bontemps, S.; Russeil, D.; Bronfman, L.; Koribalski, B. S.; Schuller, F.

    2015-07-01

    Context. The formation of high mass stars and clusters occurs in giant molecular clouds. Objects in evolved stages of massive star formation such as protostars, hot molecular cores, and ultracompact HII regions have been studied in more detail than earlier, colder objects. Further progress thus requires the analysis of the time before massive protostellar objects can be probed by their infrared emission. With this in mind, the APEX Telescope Large Area Survey of the whole inner Galactic plane at 870 μm (ATLASGAL) has been carried out to provide a global view of cold dust and star formation at submillimetre wavelengths. Aims: We derive kinematic distances to a large sample of massive cold dust clumps from their measured line velocities. We estimate masses and sizes of ATLASGAL sources, for which the kinematic distance ambiguity is resolved. Methods: The ATLASGAL sample is divided into groups of sources, which are located close together, mostly within a radius of 2 pc, and have velocities in a similar range with a median velocity dispersion of ~1 km s-1. We use NH3, N2H+, and CS velocities to calculate near and far kinematic distances to those groups. Results: We obtain 296 groups of ATLASGAL sources in the first quadrant and 393 groups in the fourth quadrant, which are coherent in space and velocity. We analyse HI self-absorption and HI absorption to resolve the kinematic distance ambiguity to 689 complexes of submm clumps. They are associated with 12CO emission probing large-scale structure and 13CO (1-0) line as well as the 870 μm dust continuum on a smaller scale. We obtain a scale height of ~28 ± 2 pc and displacement below the Galactic midplane of ~-7 ± 1 pc. Within distances from 2 to 18 kpc ATLASGAL clumps have a broad range of gas masses with a median of 1050 M⊙ as well as a wide distribution of radii with a median of 0.4 pc. Their distribution in galactocentric radii is correlated with spiral arms. Conclusions: Using a statistically significant

  9. Gas Chromatography-Mass Spectrometry Method to Quantify Benzo[a]Pyrene in Tobacco Products.

    Science.gov (United States)

    Wagner, Karl A; Huang, Chorng B; Melvin, Matt S; Ballentine, Regina; Meruva, Naren K; Flora, Jason W

    2017-08-01

    The USA Food and Drug Administration (FDA) established benzo[a]pyrene (B[a]P) as a harmful and potentially harmful constituent (HPHC) found in tobacco products. Tobacco manufacturers are required to report HPHC quantities to the FDA; however, there is currently no standardized method for determination of B[a]P in smokeless tobacco products (STPs). This work details a sensitive, selective and rapid method for the determination of B[a]P in STPs, cigarette filler and tobacco. Tobacco is extracted using methanol followed by solid-phase extraction and concentration prior to analysis by gas chromatography/mass spectrometry in the selected ion monitoring mode. Cooperation Centre for Scientific Research Relative to Tobacco reference products and 3R4F Kentucky reference cigarette filler were used for method validation. All method validation requirements were met including linearity, accuracy, precision, robustness, limit of detection (LOD) and limit of quantitation (LOQ), and stability. Calibration range of 0.5-125 ng mL-1 was achieved with the coefficient of determination (R2) greater than 0.995. The method LOQ and LOD were 0.729 and 0.216 ng/g, respectively. Using standardized methods for the measurement of HPHCs in tobacco products will reduce variability and ensure accurate data for regulatory reporting. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  10. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  11. Differentiation of essential oils in Atractylodes lancea and Atractylodes koreana by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Liu, Qiutao; Zhang, Shanshan; Yang, Xihui; Wang, Ruilin; Guo, Weiying; Kong, Weijun; Yang, Meihua

    2016-12-01

    Atractylodes rhizome is a valuable traditional Chinese medicinal herb that comprises complex several species whose essential oils are the primary pharmacologically active component. Essential oils of Atractylodes lancea and Atractylodes koreana were extracted by hydrodistillation, and the yield was determined. The average yield of essential oil obtained from A. lancea (2.91%) was higher than that from A. koreana (2.42%). The volatile components of the essential oils were then identified by a gas chromatography with mass spectrometry method that demonstrated good precision. The method showed clear differences in the numbers and contents of volatile components between the two species. 41 and 45 volatile components were identified in A. lancea and A. koreana, respectively. Atractylon (48.68%) was the primary volatile component in A. lancea, while eudesma-4(14)-en-11-ol (11.81%) was major in A. koreana. However, the most significant difference between A. lancea and A. koreana was the major component of atractylon and atractydin. Principal component analysis was utilized to reveal the correlation between volatile components and species, and the analysis was used to successfully discriminate between A. lancea and A. koreana samples. These results suggest that different species of Atractylodes rhizome may yield essential oils that differ significantly in content and composition. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Determination of Selected Phthalates by Gas Chromatography-Mass Spectrometry in Personal Perfumes.

    Science.gov (United States)

    Orecchio, Santino; Indelicato, Roberta; Barreca, Salvatore

    2015-01-01

    A simple and fast method is proposed to analyze commercial personal perfumes. Our method includes measurement of phthalates, known to be major sources of endocrine disruptor chemicals (EDC), which originate from the less volatile fraction of perfumes. The quantification of phthalates were carried out directly with no sample preparation required on 30 samples of commercial products using gas chromatography and mass spectrometry (GC-MS) as a detector. The total concentrations of 15 investigated compounds ranged from 17 to 9650 mg/L with an average of 2643 mg/L. The highest total concentration was found in cologne. Diethyl phthalate (DEP), diisobutyl phthalate (DiBP), di(2-ethylhexyl) phthalate (DEHP), and di-n-butyl phthalate (DBP) were detected in appreciable concentrations. Further, it was found that the composition of counterfeit samples varied widely from that of authentic products. The composition of old products was different from that of recent perfumes, which contain less harmful chemicals, attributed to the ban on some phthalates in Europe due their toxicity. It should be noted that older and contaminated products are not equivalent to authentic products when considering quality, safety, and probably effectiveness. Older and nonapproved perfumes contain chemicals that are not allowed for commercial use and may contain toxic impurities.

  13. The analysis of common metabolites of organophosphorus pesticides in urine by gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Park, Seong Soo; Pyo, Hee Soo; Lee, Kang Jin; Park, Song Ja; Park, Taek Kyu

    1998-01-01

    Most organophosphorus pesticides may be metabolized to yield some common phosphates in human or in animals, and these metabolites may be used as the exposure biomarkers to pesticides. In this study, we developed the extraction method of four phosphate metabolites from the spiked human urine in high recovery by the solid phase extraction with a reverse-phase cartridge (cyclohexyl silica) followed by the elution with methanol. The extracted urinary metabolites were derivatized with hexamethyldisilazane/trimethyl-chlorosilane/pyridine (2:1:10, v/v/v) and identified by gas chromatography/mass spectrometry. Calibration curve obtained from each metabolite standard using by GC/MS/SIM has shown good linearity and detection limits of metabolites were the range of 0.05-0.1 μg/ml in urine. Phenthoate, one of the organophosphorus pesticides, was orally administrated to rats. Four metabolites were detected in the rat urine. The results of this study may be applied to development of exposure biomarkers for monitoring of environmental pollutants

  14. Postmortem interval estimation: a novel approach utilizing gas chromatography/mass spectrometry-based biochemical profiling.

    Science.gov (United States)

    Kaszynski, Richard H; Nishiumi, Shin; Azuma, Takeshi; Yoshida, Masaru; Kondo, Takeshi; Takahashi, Motonori; Asano, Migiwa; Ueno, Yasuhiro

    2016-05-01

    While the molecular mechanisms underlying postmortem change have been exhaustively investigated, the establishment of an objective and reliable means for estimating postmortem interval (PMI) remains an elusive feat. In the present study, we exploit low molecular weight metabolites to estimate postmortem interval in mice. After sacrifice, serum and muscle samples were procured from C57BL/6J mice (n = 52) at seven predetermined postmortem intervals (0, 1, 3, 6, 12, 24, and 48 h). After extraction and isolation, low molecular weight metabolites were measured via gas chromatography/mass spectrometry (GC/MS) and examined via semi-quantification studies. Then, PMI prediction models were generated for each of the 175 and 163 metabolites identified in muscle and serum, respectively, using a non-linear least squares curve fitting program. A PMI estimation panel for muscle and serum was then erected which consisted of 17 (9.7%) and 14 (8.5%) of the best PMI biomarkers identified in muscle and serum profiles demonstrating statistically significant correlations between metabolite quantity and PMI. Using a single-blinded assessment, we carried out validation studies on the PMI estimation panels. Mean ± standard deviation for accuracy of muscle and serum PMI prediction panels was -0.27 ± 2.88 and -0.89 ± 2.31 h, respectively. Ultimately, these studies elucidate the utility of metabolomic profiling in PMI estimation and pave the path toward biochemical profiling studies involving human samples.

  15. Integration of Gas Chromatography Mass Spectrometry Methods for Differentiating Ricin Preparation Methods

    Energy Technology Data Exchange (ETDEWEB)

    Wunschel, David S.; Melville, Angela M.; Ehrhardt, Christopher J.; Colburn, Heather A.; Victry, Kristin D.; Antolick, Kathryn C.; Wahl, Jon H.; Wahl, Karen L.

    2012-05-17

    The investigation of crimes involving chemical or biological agents is infrequent, but presents unique analytical challenges. The protein toxin ricin is encountered more frequently than other agents and is found in the seeds of the castor plant Ricinus communis. Typically, the toxin is extracted from castor seeds utilizing a variety of different recipes that result in varying purity of the toxin. Moreover, these various purification steps can also leave or differentially remove a variety of exogenous and endogenous residual components with the toxin that may indicate the type and number of purification steps involved. We have applied three gas chromatographic - mass spectrometric (GC-MS) based analytical methods to measure the variation in seed carbohydrates and castor oil ricinoleic acid as well as the presence of solvents used for purification. These methods were applied to the same samples prepared using four previously identified toxin preparation methods starting from four varieties of castor seeds. The individual data sets for seed carbohydrate profiles, ricinoleic acid or acetone amount each provided information capable of differentiating different types of toxin preparations across seed types. However, the integration of the data sets using multivariate factor analysis provided a clear distinction of all samples based on the preparation method and independent of the seed source. In particular the abundance of mannose, arabinose, fucose, ricinoleic acid and acetone were shown to be important differentiating factors. These complementary tools provide a more confident determination of the method of toxin preparation.

  16. Characterisation of varnishes used in violins by pyrolysis-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Chiavari, Giuseppe; Montalbani, Simona; Otero, Vanessa

    2008-12-01

    The correct characterisation and a detailed knowledge of the materials originally used in violin varnishes, like natural resins, is crucial for the conservation in museums and for a suitable restoration technique. The study presented here reports on the potential of pyrolysis (Py) coupled with gas chromatography (GC) and mass spectrometry (MS) for the identification of chemical markers of each resin; this technique is very sensitive and selective, it needs a small quantity of sample and does not require chemical treatments. To improve the chromatographic behaviour of polar compounds the derivatising agent tetramethylammonium hydroxide (TMAH) in combination with pyrolysis has been used, in the so-called TMAH thermochemolysis or thermally assisted hydrolysis and methylation (THM), or more simply pyrolysis-methylation. The natural resins studied were colophony, sandarac, manila copal, elemi, amber and benzoin, mainly composed of terpenic compounds, with the exception of the latter, composed of aromatic compounds. Many compounds were identified; in particular, methyl esters of resinous acids that, individually or in a group, can be used as chemical markers. However, through this technique it was not possible to distinguish between the sandarac and manila copal resins because their chromatographic behaviour is very similar. Finally, the procedure applied has been employed in the characterisation of original varnish samples.

  17. Trash-to-Gas: Using Waste Products to Minimize Logistical Mass During Long Duration Space Missions

    Science.gov (United States)

    Hintze, Paul. E.; Caraccio, Anne J.; Anthony, Stephen M.; Tsoras, Alexandra N.; Nur, Monoita; Devor, Robert; Captain, James G.

    2013-01-01

    Just as waste-to-energy processes utilizing municipal landftll and biomass wastes are finding increased terrestrial uses, the Trash-to-Gas (TtG) project seeks to convert waste generated during spaceflight into high value commodities. These include methane for propulsion and water for life support in addition to a variety of other gasses. TtG is part of the Logistic Reduction and Repurposing (LRR) project under the NASA Advanced Exploration Systems Program. The LRR project will enable a largely mission-independent approach to minimize logistics contributions to total mission architecture mass. LRR includes technologies that reduce the amount of consumables that need to be sent to space, repurpose items sent to space, or convert wastes to commodities. Currently, waste generated on the International Space Station is stored inside a logistic module which is de-orbited into Earth's atmosphere for destruction. The waste consists of food packaging, food, clothing and other items. This paper will discuss current results on incineration as a waste processing method. Incineration is part of a two step process to produce methane from waste: first the waste is converted to carbon oxides; second, the carbon oxides are fed to a Sabatier reactor where they are converted to methane. The quantities of carbon dioxide, carbon monoxide, methane and water were measured under the different thermal degradation conditions. The overall carbon conversion efficiency and water recovery are discussed.

  18. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    Science.gov (United States)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

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

    Science.gov (United States)

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

    2017-01-01

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

  20. Exploring the Metabolomic Responses of Bacillus licheniformis to Temperature Stress by Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Dong, Zixing; Chen, Xiaoling; Cai, Ke; Chen, Zhixin; Wang, Hongbin; Jin, Peng; Liu, Xiaoguang; Permaul, Kugenthiren; Singh, Suren; Wang, Zhengxiang

    2018-03-28

    Owing to its high protein secretion capacity, simple nutritional requirements, and GRAS (generally regarded as safe) status, Bacillus licheniformis is widely used as a host for the industrial production of enzymes, antibiotics, and peptides. However, as compared with its close relative Bacillus subtilis , little is known about the physiology and stress responses of B. licheniformis . To explore its temperature-stress metabolome, B. licheniformis strains ATCC 14580 and B186, with respective optimal growth temperatures of 42°C and 50°C, were cultured at 42°C, 50°C, and 60°C and their corresponding metabolic profiles were determined by gas chromatography/mass spectrometry and multivariate statistical analyses. It was found that with increased growth temperatures, the two B. licheniformis strains displayed elevated cellular levels of proline, glutamate, lysine, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and octadecanoic acid, and decreased levels of glutamine and octadecenoic acid. Regulation of amino acid and fatty acid metabolism is likely to be associated with the evolution of protective biochemical mechanisms of B. licheniformis . Our results will help to optimize the industrial use of B. licheniformis and other important Bacillus species.

  1. Identification of floral scent in chrysanthemum cultivars and wild relatives by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sun, Hainan; Zhang, Ting; Fan, Qingqing; Qi, Xiangyu; Zhang, Fei; Fang, Weimin; Jiang, Jiafu; Chen, Fadi; Chen, Sumei

    2015-03-25

    The objective of this study was to identify the major volatile compounds and their relative concentrations in flowers of different chrysanthemum cultivars and their wild relatives. The volatile organic components of fresh flowers were analyzed using a headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry. In total, 193 volatile organic components were detected; the major scent components were monoterpenoids and oxygenated monoterpenoids, which accounted for 68.59%-99.93% of the total volatiles in all tested materials except for Chrysanthemum indicum collected from Huangshan, in which they accounted for only 37.45% of total volatiles. The major volatile compounds were camphor, α-pinene, chrysanthenone, safranal, myrcene, eucalyptol, 2,4,5,6,7,7ab-hexahydro-1H-indene, verbenone, β-phellandrene and camphene. In a hierarchical cluster analysis, 39 accessions of Chrysanthemum and its relatives formed six clusters based on their floral volatile compounds. In a principal component analysis, only spider type flowers were located closely on the score plot. The results of this study provide a basis for breeding chrysanthemum cultivars which desirable floral scents.

  2. [Simultaneous determination of ten organotin compounds in polyvinyl chloride plastics using gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Ying; Li, Bin; Liu, Li; Zhang, Chen; Wu, Jingwu; Liu, Zhihong; Li, Xintian

    2009-01-01

    A rapid and effective gas chromatography coupled with mass spectrometry method has been developed systematically and studied for the simultaneous determination of 10 organotin compounds, dibutyltin-dichloride (DBT), n-butyltin-trichloride (MBT), triethyltinchloride (TET), fentin-chloride (TPhT), chlorotributylstannane (TBT), tri-n-propyltinchloride (TPrT), diphenyltin-dichloride (DPhT), tetrabutyltin (TeBT), di-n-octyltin-dichloride (DOT), phenyltin trichloride (MPhT)), in polyvinyl chloride (PVC) plastics. The PVC sample was dissolved with tetrahydrofuran and the polymer in the sample was precipitated with methanol, and then the target compounds were derivatized with sodium tetraethylborate and extracted with hexane under ultrasonication. The qualitative and quantitative analysis were carried out by GC-MS and the total ion chromatogram and selected ion chromatogram were obtained. The derivatization and extraction conditions, such as the derivatization time, derivatization pH value, dosages of derivatization reagent and precipitation reagent were optimized. The good linearities, recoveries and precisions were obtained. The linearity ranges were 0.5 - 50 mg/L. The linearity correlation coefficients of 10 organotin compounds were between 0.997 8 and 0.999 7. The average recoveries were 84.23% - 109.1% with relative standard deviations of 4.24% - 10.75%. The established method has been successfully applied to the determination of organotin compounds in PVC plastics.

  3. Multiresidue Analysis of 86 Pesticides Using Gas Chromatography Mass Spectrometry: II-Nonleafy Vegetables

    Directory of Open Access Journals (Sweden)

    M. H. EL-Saeid

    2013-01-01

    Full Text Available A total of 1057 samples of fresh vegetables from import and domestic production were analyzed (cold pepper, egg plant, carrot, cucumber, potato, hot pepper, cultivation tomato, squash, beans, okra, onions, cauliflower, and green house tomato. The aim of this study was to investigate pesticide residues in market foods in Riyadh, which have been collected from Riyadh Development Company (Al-Tamer Vegetables Market. Pesticide residues were determined by gas chromatography with mass selective detector (GC-MSD. A multiresidue method was developed and described for simultaneous determination of 86 pesticides commonly used in crop protection. This method used to determine 86 pesticide residues with a broad range of physicochemical properties in fresh vegetables related to organophosphorus (OPP, organochlorines (OCP, pyrethroids, and carbamates mainly used in agriculture. Sample extract was cleaned up by using AOAC method. Pesticide residues above the maximum residue limits (MRL were detected in 15.89% of the total samples (168 from 1057 samples, but 83.90% of the total samples (887 from 1057 samples has no residues or contained pesticide residues at or below MRL. The detected and most frequently found pesticide residues were permethrin (45 times and endosulfan (34 times followed by deltamethrin (27 times. The findings of this study pointed to the following recommendations: the need for a monitoring program for pesticide residues in imported food crops.

  4. Gas chromatographic/mass spectrometric characterization of dromostanolone metabolites in human urine

    International Nuclear Information System (INIS)

    Kim, Tae Wook; Choi, Man Ho; Jung, Byung Hwa; Chung, Bong Chul

    1998-01-01

    The metabolism of dromostanolone (2α-methyl-5α-androstan-17β-ol-3-one) was studied in three adult volunteers after oral dose of 20 mg. Solvent extracts of urine obtained after enzyme hydrolysis were derivatized with MSTFA/TMCS and MSTFA/TMIS. The structures of intact drug and its metabolites were determined by gas chromatography/mass spectrometry (GC/MS) in electron impact (EI) mode. The major metabolite (2α-methyl-5α-androstan-3α-ol-17-one), its 3β-epimer, parent compound, and several hydroxylated metabolites including intact drug were detected by comparing total ion chromatograms of control urine with that of the administered sample. Two epimers of 2α-methyl-5α-androstan-3, 17β-diol were detected using selected ion monitoring. The maximum excretion of dromostanolone and 2α-methyl-5α-androstan-3α-ol-17-one was reached in 6.2-15 hr. The half-life of intact dromostanolone was 5.3 hr. About 3.0% of the administered amount was found to be excreted within 95 hr as unchanged form

  5. Metabolic Profiling and Quantification of Neurotransmitters in Mouse Brain by Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Jäger, Christian; Hiller, Karsten; Buttini, Manuel

    2016-09-01

    Metabolites are key mediators of cellular functions, and have emerged as important modulators in a variety of diseases. Recent developments in translational biomedicine have highlighted the importance of not looking at just one disease marker or disease inducing molecule, but at populations thereof to gain a global understanding of cellular function in health and disease. The goal of metabolomics is the systematic identification and quantification of metabolite populations. One of the most pressing issues of our times is the understanding of normal and diseased nervous tissue functions. To ensure high quality data, proper sample processing is crucial. Here, we present a method for the extraction of metabolites from brain tissue, their subsequent preparation for non-targeted gas chromatography-mass spectrometry (GC-MS) measurement, as well as giving some guidelines for processing of raw data. In addition, we present a sensitive screening method for neurotransmitters based on GC-MS in selected ion monitoring mode. The precise multi-analyte detection and quantification of amino acid and monoamine neurotransmitters can be used for further studies such as metabolic modeling. Our protocol can be applied to shed light on nervous tissue function in health, as well as neurodegenerative disease mechanisms and the effect of experimental therapeutics at the metabolic level. © 2016 by John Wiley & Sons, Inc. Copyright © 2016 John Wiley & Sons, Inc.

  6. A gas chromatography-mass spectrometry method for the quantitation of clobenzorex.

    Science.gov (United States)

    Cody, J T; Valtier, S

    1999-01-01

    Drugs metabolized to amphetamine or methamphetamine are potentially significant concerns in the interpretation of amphetamine-positive urine drug-testing results. One of these compounds, clobenzorex, is an anorectic drug that is available in many countries. Clobenzorex (2-chlorobenzylamphetamine) is metabolized to amphetamine by the body and excreted in the urine. Following administration, the parent compound was detectable for a shorter time than the metabolite amphetamine, which could be detected for days. Because of the potential complication posed to the interpretation of amphetamin-positive drug tests following administration of this drug, the viability of a current amphetamine procedure using liquid-liquid extraction and conversion to the heptafluorobutyryl derivative followed by gas chromatography-mass spectrometry (GC-MS) analysis was evaluated for identification and quantitation of clobenzorex. Qualitative identification of the drug was relatively straightforward. Quantitative analysis proved to be a far more challenging process. Several compounds were evaluated for use as the internal standard in this method, including methamphetamine-d11, fenfluramine, benzphetamine, and diphenylamine. Results using these compounds proved to be less than satisfactory because of poor reproducibility of the quantitative values. Because of its similar chromatographic properties to the parent drug, the compound 3-chlorobenzylamphetamine (3-Cl-clobenzorex) was evaluated in this study as the internal standard for the quantitation of clobenzorex. Precision studies showed 3-Cl-clobenzorex to produce accurate and reliable quantitative results (within-run relative standard deviations [RSDs] clobenzorex.

  7. Structural investigations of neuromelanin by pyrolysis-gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Dzierzega-Lecznar, A.; Kurkiewicz, S.; Stepien, K.; Chodurek, E.; Riederer, P.; Gerlach, M.

    2006-01-01

    Pyrolysis combined with gas chromatography and mass spectrometry (Py-GC/MS) was applied for structural investigations of the human substantia nigra neuromelanin. Using synthetic neuromelanins, we have demonstrated that Py-GC/MS is suitable for identification and differentiation of both eumelanin (dopamine-derived) and pheomelanin (cysteinyldopamine-derived) component of the pigment. Structural information on melanin monomers was inferred from their pyrolytic markers. When the human neuromelanin was subjected to pyrolysis, none of the heterocyclic, sulfur-containing markers of pheomelanin component was detected among the thermal degradation products. We have concluded that nigral pigment isolated from normal brain tissue does not contain benzothiazine-type monomers, and that cysteinyldopamine-originated units may be incorporated into the polymer in uncyclized form. The most abundant pyrolysis product was identified as limonene, which indicates that nigral pigment is tightly associated with an isoprenoid-type compound. Pyrolysis in the presence of the methylating reagent allowed identification of high levels of saturated and monounsaturated straight-chain C14-C18 fatty acid species chemically bound to the pigment macromolecule. (author)

  8. Analysis of fatty acid composition of Withania coagulans fruits by gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    A. Ali

    2017-10-01

    Full Text Available Background and objectives: Withania coagulans Dunal (Solanaceae fruits are recommended to treat asthma, dyspepsia, biliousness, flatulent colic, liver complaints, intestinal infections, strangury, wounds and as diuretic, emetic and sedative agent in Indian traditional system of medicine. The objective of this study was to describe the systematic fatty acid composition of the petroleum ether extract of W. coagulans fruits. Methods: Petroleum ether extract of W. coagulans fruits was prepared by maceration. Components of the W. coagulans petroleum ether extract were identified by gas chromatography-mass spectrometry and their concentrations were determined. Results: The fixed oil of W. coagulans fruits constituted of twenty nine components including unsaturated (52.36% and saturated (22.15% fatty acids, alkenes (5.65%, phytosterols (4.39%, fatty alcohols (4.14%, aromatic acid (3.56%, monoterpenes (3.22%, triterpenoids (1.83% and alkanes (2.7%. Most of the saturated and unsaturated fatty acids were identified as their methyl esters. Conclusions: Palmitoleic and 11-eicosenoic acids have been reported for the first time in petroleum ether extract of the W. coagulans fruits. The present study has illustrated the chemical nature of W. coagulans fruit and described its fatty acids composition.

  9. 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.

  10. Gas chromatography/mass spectrometry analysis of triacetone triperoxide (TATP) degradation products.

    Science.gov (United States)

    Armitt, David; Zimmermann, Peter; Ellis-Steinborner, Simon

    2008-04-01

    Interest in the analysis and detection of triacetone triperoxide (TATP) and other organic peroxides has increased in recent years. Also of interest is the degradation and decomposition of the peroxides, not only to gain more detailed chemical information from organic peroxide samples, but also to investigate possible new procedures or mechanisms for chemical neutralisation. This report investigates the chemical degradation products of TATP after it has been treated with different acids within a sealed system over a period of 14 days. The samples were collected and analysed by solid-phase microextraction (SPME) and direct liquid injection gas chromatography/mass spectrometry (GC/MS). The results of the experiments indicate that the rate of chemical degradation of TATP and the products formed are dependent on the type of acid. The observed differences enables the type of acid used in the degradation process to be determined, provide complementary information to identify the presence of TATP, and possibly indicate new pathways that may be used to chemically neutralise TATP. (c) 2008 Commonwealth of Australia. Published by John Wiley & Sons, Ltd.

  11. Identification of Floral Scent in Chrysanthemum Cultivars and Wild Relatives by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Hainan Sun

    2015-03-01

    Full Text Available The objective of this study was to identify the major volatile compounds and their relative concentrations in flowers of different chrysanthemum cultivars and their wild relatives. The volatile organic components of fresh flowers were analyzed using a headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry. In total, 193 volatile organic components were detected; the major scent components were monoterpenoids and oxygenated monoterpenoids, which accounted for 68.59%–99.93% of the total volatiles in all tested materials except for Chrysanthemum indicum collected from Huangshan, in which they accounted for only 37.45% of total volatiles. The major volatile compounds were camphor, α-pinene, chrysanthenone, safranal, myrcene, eucalyptol, 2,4,5,6,7,7ab-hexahydro-1H-indene, verbenone, β-phellandrene and camphene. In a hierarchical cluster analysis, 39 accessions of Chrysanthemum and its relatives formed six clusters based on their floral volatile compounds. In a principal component analysis, only spider type flowers were located closely on the score plot. The results of this study provide a basis for breeding chrysanthemum cultivars which desirable floral scents.

  12. Determination of pyrrolizidine alkaloids in selected feed materials with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kowalczyk, Ewelina; Kwiatek, Krzysztof

    2017-05-01

    1,2-Dehydropyrrolizidine alkaloids are known to be toxic to many animals and humans. To provide safety of feeds a method based on gas chromatography-mass spectrometry enabling the determination of a content of 1,2-unsaturated PAs in feed materials was developed. After extraction with aqueous solution of HCl and purification of the extract, 1,2-unsaturated alkaloids are reduced to their common backbone structures and subsequently derivatised with heptafluorobutyric anhydride (HFBA). The method was validated according to SANTE/11945/2015. All received parameters are consistent with the document requirements as recovery of a final compound retronecine derivative was from 81.8% to 94.4% when retrosine was used for spiking and from 72.7% to 85.5% when retrorsine N-oxide was spiked. The repeatability was calculated as relative standards deviation and ranged from 7.5% to 14.4%, for N-oxide was from 7.9% to 15.4%. The reproducibility was in the range from 14.2% to 16.3% and from 17.0% to 18.1% for free base and N-oxide respectively. The limit of quantification was determined as 10 µg kg - 1 . Good linearity of the method was obtained with coefficient of determination R 2  > 0.99. The method was applied to 35 silage and two hay samples analysis.

  13. Thermal desorption gas chromatography with mass spectrometry study of outgassing from polymethacrylimide foam (Rohacell®).

    Science.gov (United States)

    Carrasco-Correa, Enrique J; Herrero-Martínez, José M; Consuegra, Lina; Ramis-Ramos, Guillermo; Sanz, Rafael Mata; Martínez, Benito Gimeno; Esbert, Vicente E Boria; García-Baquero, David Raboso

    2015-09-01

    Polymethacrylimide foams are used as light structural materials in outer-space devices; however, the foam closed cells contain volatile compounds that are outgassed even at low temperatures. These compounds ignite as plasmas under outer-space radiation and the intense radio-frequency fields used in communications. Since plasmas may cause spacecraft fatal events, the conditions in which they are ignited should be investigated. Therefore, qualitative and quantitative knowledge about polymethacrylimide foam outgassing should be established. Using thermogravimetric analysis, weight losses reached 3% at ca. 200°C. Thermal desorption gas chromatography with mass spectrometry detection was used to study the offgassed compounds. Using successive 4 min heating cycles at 125°C, each one corresponding to an injection, significant amounts of nitrogen (25.3%), water (2.6%), isobutylene (11.3%), tert-butanol (2.9%), 1-propanol (11.9%), hexane (25.3%), propyl methacrylate (1.4%), higher hydrocarbons (11.3%), fatty acids (2.2%) and their esters (1.3%), and other compounds were outgassed. Other compounds were observed during the main stage of thermal destruction (220-280°C). A similar study at 175°C revealed the extreme difficulty in fully outgassing polar compounds from polymethacrylimide foams by baking and showed the different compositions of the offgassed atmosphere that can be expected in the long term. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Hydrocarbon phenotyping of algal species using pyrolysis-gas chromatography mass spectrometry

    Directory of Open Access Journals (Sweden)

    Kothari Shankar L

    2010-05-01

    Full Text Available Abstract Background Biofuels derived from algae biomass and algae lipids might reduce dependence on fossil fuels. Existing analytical techniques need to facilitate rapid characterization of algal species by phenotyping hydrocarbon-related constituents. Results In this study, we compared the hydrocarbon rich algae Botryococcus braunii against the photoautotrophic model algae Chlamydomonas reinhardtii using pyrolysis-gas chromatography quadrupole mass spectrometry (pyGC-MS. Sequences of up to 48 dried samples can be analyzed using pyGC-MS in an automated manner without any sample preparation. Chromatograms of 30-min run times are sufficient to profile pyrolysis products from C8 to C40 carbon chain length. The freely available software tools AMDIS and SpectConnect enables straightforward data processing. In Botryococcus samples, we identified fatty acids, vitamins, sterols and fatty acid esters and several long chain hydrocarbons. The algae species C. reinhardtii, B. braunii race A and B. braunii race B were readily discriminated using their hydrocarbon phenotypes. Substructure annotation and spectral clustering yielded network graphs of similar components for visual overviews of abundant and minor constituents. Conclusion Pyrolysis-GC-MS facilitates large scale screening of hydrocarbon phenotypes for comparisons of strain differences in algae or impact of altered growth and nutrient conditions.

  15. Metabolomic study of aging in mouse plasma by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Seo, Chan; Hwang, Yun-Ho; Kim, Youngbae; Joo, Bo Sun; Yee, Sung-Tae; Kim, Cheol Min; Paik, Man-Jeong

    2016-07-01

    Metabolomic analysis of aging was performed in plasma samples of young (8 weeks) and old (72 weeks) mice as ethoxycarbonyl/methoxime/tert-butyldimethylsilyl derivatives by gas chromatography-mass spectrometry (GC-MS). As new approaches, study of altered metabolism from aging was attempted by simultaneous profiling analysis of amino acids (AAs), organic acids (OAs) and fatty acids (FAs) by GC-MS in a single run combined with pattern analysis. As a result, 27 amino acids (AAs), 17 organic acids (OAs) and 24 fatty acids (FAs) were positively screened with large variations in plasma samples. Among altered metabolites, levels of six AAs (proline, methionine, 4-hydroxyproline, pipecolic acid, glutamic acid, α-aminoadipic acid) as neurotransmetters and nutrients, five OAs (2-hydroxybutyric acid, 2-hydroxyglutaric acid, cis-aconitic acid citric acid, isocitric acid) including intermediate metabolites in the TCA cycle, and three n-3 polyunsaturated FAs (PUFAs) of α-octadecatrienoic acid, eicosapentaenoic acid and docosahexaenoic acid as potential biomarkers were significantly different between young and old groups. Their levels were normalized to the corresponding mean values of the young group and then plotted into star symbol patterns, which were clearly distinct compared with numerical data and readily distinguishable for young and old groups. Thus, the present metabolomic screening and the star pattern recognition method might be useful for understanding the complexity of biochemical events in aging. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Analysis of volatile compounds of Malaysian Tualang (Koompassia excelsa) honey using gas chromatography mass spectrometry.

    Science.gov (United States)

    Nurul Syazana, M S; Gan, S H; Halim, A S; Shah, Nurul Syazana Mohamad; Gan, Siew Hua; Sukari, Halim Ahmad

    2013-01-01

    The constituents of honey's volatile compounds depend on the nectar source and differ depending on the place of origin. To date, the volatile constituents of Tualang honey have never been investigated. The objective of this study was to analyze the volatile compounds in local Malaysian Tualang honey. A continuous extraction of Tualang honey using five organic solvents was carried out starting from non-polar to polar solvents and the extracted samples were analysed using gas chromatography-mass spectrometry (GC-MS). Overall, 35 volatile compounds were detected. Hydrocarbons constitute 58.5% of the composition of Tualang honey. Other classes of chemical compounds detected included acids, aldehydes, alcohols, ketones, terpenes, furans and a miscellaneous group. Methanol yielded the highest number of extracted compounds such as acids and 5-(Hydroxymethyl) furfural (HMF). This is the first study to describe the volatile compounds in Tualang honey. The use of a simple one tube, stepwise, non-thermal liquid-liquid extraction of honey is a advantageous as it prevents sample loss. Further research to test the clinical benefits of these volatile compounds is recommended.

  17. Characterization by Gas Chromatography-Mass Spectrometry of Commercially Available Thinner in the City of Cartagena

    Directory of Open Access Journals (Sweden)

    Jesus Olivero

    2013-09-01

    Full Text Available Thinner is a widely used product in the industry of paints, lubricants and adhesives. Its composition varies according to its use and quality. However, its chronic exposure is a concern, because it can affect major organs such as lungs, liver, kidney and the adrenal glands. This study characterizes the composition of several thinner samples commercially available in the city of Cartagena. Twelve samples were collected in different stores, these were then analyzed through gas chromatography coupled to mass spectrometry (GC/MS. The results showed that not only the composition but also the relative distribution of the components present in the samples are variable. Thirty two compounds were detected: toluene, o-xylene, p-xylene and ethylbenzene —among others— with occurrence frequencies of 91.7, 66.7, 75, and 66.7 %, respectively. The lack of knowledge regarding the risk of poisoning, produced when handling this type of mixtures, may be the cause of many health problems in people exposed to thinner, both in workplace and domestic activities. A data mining showed the potential association between thinner components and clinical manifestations, which include kidney and liver damage, hair loss, haematological disorders, dermatitis, anxiety and balance problems, among others. In conclusion, thinner has large variability, both in terms of components and of their relative composition. The adverse health effects of direct or indirect exposure to these components have been widely described in the literature.

  18. Headspace gas chromatography-mass spectrometry of volatile compounds in murici (Byrsonima crassifolia l. Rich).

    Science.gov (United States)

    Alves, G L; Franco, M R B

    2003-01-24

    Northern and Northeastern Brazil have a natural diversity of fruits, many of which are considered exotic, presenting different flavors and aromas. The enormous diversity of fruits represents a promising area for research on aromas. There is also a great potential for the manufacture of juices, desserts or other processed products. Murici is a typical fruit from these regions presenting a different flavor, reminiscent of that of cheese. This fruit is consumed mainly as juice, ice cream or as liquor, greatly appreciated by the local population. Headspace volatile compounds of three lots of the fruit from Ceará (Fortaleza) were collected by suction on Porapak Q for 2 h and desorbed with 300 microl of acetone. The isolated volatile compounds were separated by high resolution GC. Forty-six volatile compounds were detected, of which 41 were identified by gas chromatography-mass spectrometry and Kovats indices. The most abundant compounds were ethanol (28.3%) and ethyl hexanoate (25.1%). Butanoic acid (5.1%), hexanoic acid (5.1%) and methyl butyrate (2.8%) were also detected in the headspace of the fruit and confirm its unusual cheese aroma.

  19. Analysis of ergosterol in single kernel and ground grain by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dong, Yanhong; Steffenson, Brian J; Mirocha, Chester J

    2006-06-14

    A method for analyzing ergosterol in a single kernel and ground barley and wheat was developed using gas chromatography-mass spectrometry (GC-MS). Samples were saponified in methanolic KOH. Ergosterol was extracted by "one step" hexane extraction and subsequently silylated by N-trimethylsilylimidazole/trimethylchlorosilane (TMSI/TMCS) reagent at room temperature. The recoveries of ergosterol from ground barley were 96.6, 97.1, 97.1, 88.5, and 90.3% at the levels of 0.2, 1, 5, 10, and 20 microg/g (ppm), respectively. The recoveries from a single kernel were between 93.0 and 95.9%. The precision (coefficient of variance) of the method was in the range 0.8-12.3%. The method detection limit (MDL) and the method quantification limit (MQL) were 18.5 and 55.6 ng/g (ppb), respectively. The ergosterol analysis method developed can be used to handle 80 samples daily by one person, making it suitable for screening cereal cultivars for resistance to fungal infection. The ability for detecting low levels of ergosterol in a single kernel provides a tool to investigate early fungal invasion and to study mechanisms of resistance to fungal diseases.

  20. Using Gas Phase Reactions of Hexamethylene Triperoxide Diamine (HMTD) to Improve Detection in Mass Spectrometry

    Science.gov (United States)

    Colizza, Kevin; Yevdokimov, Alexander; McLennan, Lindsay; Smith, James L.; Oxley, Jimmie C.

    2018-01-01

    Our efforts to lower the detection limits of hexamethylene triperoxide diamine (HMTD) have uncovered previously unreported gas-phase reactions of primary and secondary amines with one of the six methylene carbons. The reaction occurs primarily in the atmospheric pressure chemical ionization (APCI) source and is similar to the behavior of alcohols with HMTD [1]. However, unlike alcohols, the amine reaction conserves the hydrogen peroxide on the intact product. Furthermore, with or without amines, HMTD is oxidized to tetramethylene diperoxide diamine dialdehyde (TMDDD) in a temperature-dependent fashion in the APCI source. Synthesized TMDDD forms very strong adducts (not products) to ammonium and amine ions in the electrospray ionization (ESI) source. Attempts to improve HMTD detection by generating TMDDD in the APCI source with post-column addition of amines were not successful. Signal intensity of the solvent related HMTD product in methanol, [HMTD+MeOH2-H2O2]+ (m/z 207.0975), was understandably related to the amount of methanol in the HMTD environment as it elutes into the source. With conditions optimized for this product, the detection of 100 pg on column was accomplished with a robust analysis of 300 pg (1.44 pmol) routinely performed on the Orbitrap mass spectrometers. [Figure not available: see fulltext.

  1. Acceleration of Gas Flow Simulations in Dual-Continuum Porous Media Based on the Mass-Conservation POD Method

    KAUST Repository

    Wang, Yi

    2017-09-12

    Reduced-order modeling approaches for gas flow in dual-porosity dual-permeability porous media are studied based on the proper orthogonal decomposition (POD) method combined with Galerkin projection. The typical modeling approach for non-porous-medium liquid flow problems is not appropriate for this compressible gas flow in a dual-continuum porous media. The reason is that non-zero mass transfer for the dual-continuum system can be generated artificially via the typical POD projection, violating the mass-conservation nature and causing the failure of the POD modeling. A new POD modeling approach is proposed considering the mass conservation of the whole matrix fracture system. Computation can be accelerated as much as 720 times with high precision (reconstruction errors as slow as 7.69 × 10−4%~3.87% for the matrix and 8.27 × 10−4%~2.84% for the fracture).

  2. Probing the Binding Interfaces of Protein Complexes Using Gas-Phase H/D Exchange Mass Spectrometry

    DEFF Research Database (Denmark)

    Mistarz, Ulrik H; Brown, Jeffery M; Haselmann, Kim F

    2016-01-01

    Fast gas-phase hydrogen/deuterium exchange mediated by ND3 gas and measured by mass spectrometry (gas-phase HDX-MS) is a largely unharnessed, fast, and sensitive method for probing primary- and higher-order polypeptide structure. Labeling of heteroatom-bound non-amide hydrogens in a sub...... conditions. Lysozyme ions bound by an oligosaccharide incorporated less deuterium than the unbound ion. Similarly, trypsin ions showed reduced deuterium uptake when bound by the peptide ligand vasopressin. Our results are in good agreement with crystal structures of the native protein complexes......, and illustrate that gas-phase HDX-MS can provide a sensitive and simple approach to measure the number of heteroatom-bound non-amide side-chain hydrogens involved in the binding interface of biologically relevant protein complexes....

  3. Method for detection of trace metal and metalloid contaminants in coal-generated fuel gas using gas chromatography/ion trap mass spectrometry.

    Science.gov (United States)

    Rupp, Erik C; Granite, Evan J; Stanko, Dennis C

    2010-07-15

    There exists an increasing need to develop a reliable method to detect trace contaminants in fuel gas derived from coal gasification. While Hg is subject to current and future regulations, As, Se, and P emissions may eventually be regulated. Sorbents are the most promising technology for the removal of contaminants from coal-derived fuel gas, and it will be important to develop a rapid analytical detection method to ensure complete removal and determine the ideal time for sorbent replacement/regeneration in order to reduce costs. This technical note explores the use of a commercial gas chromatography/ion trap mass spectrometry system for the detection of four gaseous trace contaminants in a simulated fuel gas. Quantitative, repeatable detection with limits at ppbv to ppmv levels were obtained for arsine (AsH(3)), phosphine (PH(3)), and hydrogen selenide (H(2)Se), while qualitative detection was observed for mercury. Decreased accuracy and response caused by the primary components of fuel gas were observed.

  4. Specialists' meeting on heat and mass transfer in the reactor cover gas, Harwell, England, 8-10 October 1985

    International Nuclear Information System (INIS)

    1986-07-01

    The specialists' meeting on ''Heat and Mass Transfer in the Reactor Cover Gas'' was held at Harwell, the United Kingdom, on 8-10 October 1985. It was attended by 24 participants from all IWGFR member-countries: France, the Federal Republic of Germany, India, Italy, Japan, the Union of Soviet Socialist Republics, the United Kingdom and the United States. The meeting was presided over by Dr K. Eickhoff of the United Kingdom. The following topical areas were reviewed and discussed during the meeting: 1. National review presentations on the status of activities on heat and mass transfer in the reactor cover gas - 2 papers; 2. Aerosol dynamics - 4 papers; 3. Aerosol trapping - 2 papers; 4. Heat and mass transfer through cover gas in annuli - 3 papers; 5. Radiative properties - 4 papers; 6. Modelling of cover gas - 4 papers. A separate abstract was prepared for each of these papers. On the basis of papers presented and discussed by participants, session summaries and conclusions were drafted on the above topical areas. These summaries, as well as general conclusions and recommendations of the meeting were reviewed and agreed upon by consensus at the end of the meeting

  5. Estimation of air-water gas exchange coefficient in a shallow lagoon based on 222Rn mass balance.

    Science.gov (United States)

    Cockenpot, S; Claude, C; Radakovitch, O

    2015-05-01

    The radon-222 mass balance is now commonly used to quantify water fluxes due to Submarine Groundwater Discharge (SGD) in coastal areas. One of the main loss terms of this mass balance, the radon evasion to the atmosphere, is based on empirical equations. This term is generally estimated using one among the many empirical equations describing the gas transfer velocity as a function of wind speed that have been proposed in the literature. These equations were, however, mainly obtained from areas of deep water and may be less appropriate for shallow areas. Here, we calculate the radon mass balance for a windy shallow coastal lagoon (mean depth of 6m and surface area of 1.55*10(8) m(2)) and use these data to estimate the radon loss to the atmosphere and the corresponding gas transfer velocity. We present new equations, adapted to our shallow water body, to express the gas transfer velocity as a function of wind speed at 10 m height (wind range from 2 to 12.5 m/s). When compared with those from the literature, these equations fit particularly well with the one of Kremer et al. (2003). Finally, we emphasize that some gas transfer exchange may always occur, even for conditions without wind. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. 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.

  7. The use of multivariate curve resolution methods to improve the analysis of muramic acid as bacterial marker using gas chromatography-mass spectrometry: an alternative method to gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Moazeni-Pourasil, Roudabeh Sadat; Piri, Farhad; Ghassempour, Alireza; Jalali-Heravi, Mehdi

    2014-02-15

    In analysis of muramic acid (MA) as bacterial marker, two dominant disturbing factors lead the researchers to use gas chromatography-tandem mass spectrometry (GC-MS/MS) technique instead of gas chromatography-mass spectrometry (GC-MS). These factors are the trace concentration of MA and fundamental disturbance of base line mass channels in GC-MS technique. This study aimed to utilize multivariate curve resolution (MCR) methods combined with GC-MS to improve the analysis of MA. First, the background and noise in GC-MS analysis were corrected and reduced using MCR methods. In addition, the MA overlapped peaks were resolved to its pure chromatographic and mass spectral profiles. Then the two-way response of each component was reconstructed by the outer product of the pure chromatographic and mass spectral profiles. The overall volume integration (OVI) method was used for quantitative determination. The MA peak area was decreased dramatically after the background correction and noise reduction. The findings severely ratify the appropriateness of using MCR techniques combined with GC-MS analysis as a simple, fast and inexpensive method for the analysis of MA in complex mixtures. The proposed method may be considered as an alternative method to GC-MS/MS for thorough analysis of the bacterial marker. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Experimental investigation on distribution of mass flux and gas/liquid mixture ratio of airblast coaxial atomizers

    Science.gov (United States)

    Wu, Jinxiang; Liu, Weidong; Zhuang, Fengchen

    1993-06-01

    Airblast coaxial atomizers are widely used in combustion chambers of liquid rocket engines, and the distributions of mass flux and gas/liquid mixture ratio in the downstream of the atomizers are one of the important parameters which influence the performance of combustion. A two-phase impact probe designed by the authors was employed to measure these parameters in a type of airblast coaxial atomizer. Graphs from experimental results show the details of the distribution in the downstream of the atomizers and the influences of the configuration parameters on distribution. The results provides important references for understanding the structure of gas/liquid flow fields and for designing and improving such atomizers.

  9. ANALYSIS OF CHEMICAL COMPOUNDS OF AGARWOOD OIL FROM DIFFERENT SPECIES BY GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS

    Directory of Open Access Journals (Sweden)

    Yumi Zuhanis Has-Yun Hashim

    2014-05-01

    Full Text Available ABSTRACT: Agarwood oil is a highly prized type of oil due to its unique aroma. The oil is extracted from the fragrant resin found in the agarwood tree (trunk.  The unique aroma and quality of agarwood resin and oil are contributed by the presence of certain chemical compounds. In this work, analysis and comparison of the chemical compounds of agarwood oil from A. malaccensis, A. sub-integra and a mixture of both were conducted.  The essential oils were diluted in hexane (5% prior to gas chromatography mass spectrometry (GCMS analysis performed using Agilent GCMS 7890A coupled with MSD quadrupole detector 5975 C.  Separation of analytes by gas chromatography was carried out using a Hewlett Packard HP-5MS silica capillary column (30 m X 0.25 mm X 0.25 mm. A total of 107 compounds were identified from the three samples of agarwood oils. Fifty-five (55 components were identified in A. malaccensis sample which contributes to the largest portion of the total compounds. About 20% of the compounds identified were aromatic and sesquiterpenes which have been revealed to be the main active compounds of agarwood oils which also give the aroma and pleasant odour of agarwood. Different compositions or profile of chemical components were found in agarwood oils from the two different species. Two compounds were commonly identified in all three samples namely 3-phenyl-2-butanone and alpha-cubebene.  Further studies are needed to refine the results which later can be used to assist detection and authentication of agarwood as well as its scientific-based grading. ABSTRAK: Minyak gaharu merupakan sejenis minyak beraroma unik yang mendapat permintaan tinggi dan mahal. Minyak ini diekstrak daripada resin beraroma yang terbentuk di dalam batang pokok gaharu. Keunikan aroma dan kualiti resin dan minyak gaharu ini bergantung kepada kehadiran bahan kimia tertentu. Penyelidikan ini menjurus kepada analisis dan perbandingan bahan-bahan kimia yang terdapat dalam minyak

  10. Serum metabolic profiling of human gastric cancer based on gas chromatography/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Song, Hu; Peng, Jun-Sheng [Department of Gastrointestinal Surgery, the Sixth Affiliated Hospital (Gastrointestinal and Anal Hospital), Sun Yat-sen University, Guangzhou, Guangdong (China); Yao, Dong-Sheng [National Engineering Research Center of Genetic Medicine,Ji Nan University, Guangzhou, Guangdong (China); Yang, Zu-Li [Department of Gastrointestinal Surgery, the Sixth Affiliated Hospital (Gastrointestinal and Anal Hospital), Sun Yat-sen University, Guangzhou, Guangdong (China); Liu, Huan-Liang [Institute of Gastroenterology,Sun Yat-sen University, Guangzhou, Guangdong (China); Zeng, Yi-Ke [Department of Gastrointestinal Surgery, the Sixth Affiliated Hospital (Gastrointestinal and Anal Hospital), Sun Yat-sen University, Guangzhou, Guangdong (China); Shi, Xian-Ping; Lu, Bi-Yan [Institute of Gastroenterology,Sun Yat-sen University, Guangzhou, Guangdong (China)

    2011-11-25

    Research on molecular mechanisms of carcinogenesis plays an important role in diagnosing and treating gastric cancer. Metabolic profiling may offer the opportunity to understand the molecular mechanism of carcinogenesis and help to non-invasively identify the potential biomarkers for the early diagnosis of human gastric cancer. The aims of this study were to explore the underlying metabolic mechanisms of gastric cancer and to identify biomarkers associated with morbidity. Gas chromatography/mass spectrometry (GC/MS) was used to analyze the serum metabolites of 30 Chinese gastric cancer patients and 30 healthy controls. Diagnostic models for gastric cancer were constructed using orthogonal partial least squares discriminant analysis (OPLS-DA). Acquired metabolomic data were analyzed by the nonparametric Wilcoxon test to find serum metabolic biomarkers for gastric cancer. The OPLS-DA model showed adequate discrimination between cancer and non-cancer cohorts while the model failed to discriminate different pathological stages (I-IV) of gastric cancer patients. A total of 44 endogenous metabolites such as amino acids, organic acids, carbohydrates, fatty acids, and steroids were detected, of which 18 differential metabolites were identified with significant differences. A total of 13 variables were obtained for their greatest contribution in the discriminating OPLS-DA model [variable importance in the projection (VIP) value >1.0], among which 11 metabolites were identified using both VIP values (VIP >1) and the Wilcoxon test. These metabolites potentially revealed perturbations of glycolysis and of amino acid, fatty acid, cholesterol, and nucleotide metabolism of gastric cancer patients. These results suggest that gastric cancer serum metabolic profiling has great potential in detecting this disease and helping to understand its metabolic mechanisms.

  11. Extraction of pure components from overlapped signals in gas chromatography-mass spectrometry (GC-MS

    Directory of Open Access Journals (Sweden)

    Likić Vladimir A

    2009-10-01

    Full Text Available Abstract Gas chromatography-mass spectrometry (GC-MS is a widely used analytical technique for the identification and quantification of trace chemicals in complex mixtures. When complex samples are analyzed by GC-MS it is common to observe co-elution of two or more components, resulting in an overlap of signal peaks observed in the total ion chromatogram. In such situations manual signal analysis is often the most reliable means for the extraction of pure component signals; however, a systematic manual analysis over a number of samples is both tedious and prone to error. In the past 30 years a number of computational approaches were proposed to assist in the process of the extraction of pure signals from co-eluting GC-MS components. This includes empirical methods, comparison with library spectra, eigenvalue analysis, regression and others. However, to date no approach has been recognized as best, nor accepted as standard. This situation hampers general GC-MS capabilities, and in particular has implications for the development of robust, high-throughput GC-MS analytical protocols required in metabolic profiling and biomarker discovery. Here we first discuss the nature of GC-MS data, and then review some of the approaches proposed for the extraction of pure signals from co-eluting components. We summarize and classify different approaches to this problem, and examine why so many approaches proposed in the past have failed to live up to their full promise. Finally, we give some thoughts on the future developments in this field, and suggest that the progress in general computing capabilities attained in the past two decades has opened new horizons for tackling this important problem.

  12. Automated thermochemolysis reactor for detection of Bacillus anthracis endospores by gas chromatography–mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Dan [Department of Chemistry and Biochemistry, Brigham Young University, Provo, UT 84602 (United States); Rands, Anthony D.; Losee, Scott C. [Torion Technologies, American Fork, UT 84003 (United States); Holt, Brian C. [Department of Statistics, Brigham Young University, Provo, UT 84602 (United States); Williams, John R. [Department of Chemistry and Biochemistry, Brigham Young University, Provo, UT 84602 (United States); Lammert, Stephen A. [Torion Technologies, American Fork, UT 84003 (United States); Robison, Richard A. [Department of Microbiology and Molecular Biology, Brigham Young University, Provo, UT 84602 (United States); Tolley, H. Dennis [Department of Statistics, Brigham Young University, Provo, UT 84602 (United States); Lee, Milton L., E-mail: milton_lee@byu.edu [Department of Chemistry and Biochemistry, Brigham Young University, Provo, UT 84602 (United States)

    2013-05-02

    Graphical abstract: -- Highlights: •An automated sample preparation system for Bacillus anthracis endospores was developed. •A thermochemolysis method was applied to produce and derivatize biomarkers for Bacillus anthracis detection. •The autoreactor controlled the precise delivery of reagents, and TCM reaction times and temperatures. •Solid phase microextraction was used to extract biomarkers, and GC–MS was used for final identification. •This autoreactor was successfully applied to the identification of Bacillus anthracis endospores. -- Abstract: An automated sample preparation system was developed and tested for the rapid detection of Bacillus anthracis endospores by gas chromatography–mass spectrometry (GC–MS) for eventual use in the field. This reactor is capable of automatically processing suspected bio-threat agents to release and derivatize unique chemical biomarkers by thermochemolysis (TCM). The system automatically controls the movement of sample vials from one position to another, crimping of septum caps onto the vials, precise delivery of reagents, and TCM reaction times and temperatures. The specific operations of introduction of sample vials, solid phase microextraction (SPME) sampling, injection into the GC–MS system, and ejection of used vials from the system were performed manually in this study, although they can be integrated into the automated system. Manual SPME sampling is performed by following visual and audible signal prompts for inserting the fiber into and retracting it from the sampling port. A rotating carousel design allows for simultaneous sample collection, reaction, biomarker extraction and analysis of sequential samples. Dipicolinic acid methyl ester (DPAME), 3-methyl-2-butenoic acid methyl ester (a fragment of anthrose) and two methylated sugars were used to compare the performance of the autoreactor with manual TCM. Statistical algorithms were used to construct reliable bacterial endospore signatures, and 24

  13. Serum metabolic profiling of human gastric cancer based on gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Song, Hu; Peng, Jun-Sheng; Yao, Dong-Sheng; Yang, Zu-Li; Liu, Huan-Liang; Zeng, Yi-Ke; Shi, Xian-Ping; Lu, Bi-Yan

    2011-01-01

    Research on molecular mechanisms of carcinogenesis plays an important role in diagnosing and treating gastric cancer. Metabolic profiling may offer the opportunity to understand the molecular mechanism of carcinogenesis and help to non-invasively identify the potential biomarkers for the early diagnosis of human gastric cancer. The aims of this study were to explore the underlying metabolic mechanisms of gastric cancer and to identify biomarkers associated with morbidity. Gas chromatography/mass spectrometry (GC/MS) was used to analyze the serum metabolites of 30 Chinese gastric cancer patients and 30 healthy controls. Diagnostic models for gastric cancer were constructed using orthogonal partial least squares discriminant analysis (OPLS-DA). Acquired metabolomic data were analyzed by the nonparametric Wilcoxon test to find serum metabolic biomarkers for gastric cancer. The OPLS-DA model showed adequate discrimination between cancer and non-cancer cohorts while the model failed to discriminate different pathological stages (I-IV) of gastric cancer patients. A total of 44 endogenous metabolites such as amino acids, organic acids, carbohydrates, fatty acids, and steroids were detected, of which 18 differential metabolites were identified with significant differences. A total of 13 variables were obtained for their greatest contribution in the discriminating OPLS-DA model [variable importance in the projection (VIP) value >1.0], among which 11 metabolites were identified using both VIP values (VIP >1) and the Wilcoxon test. These metabolites potentially revealed perturbations of glycolysis and of amino acid, fatty acid, cholesterol, and nucleotide metabolism of gastric cancer patients. These results suggest that gastric cancer serum metabolic profiling has great potential in detecting this disease and helping to understand its metabolic mechanisms

  14. Automated thermochemolysis reactor for detection of Bacillus anthracis endospores by gas chromatography–mass spectrometry

    International Nuclear Information System (INIS)

    Li, Dan; Rands, Anthony D.; Losee, Scott C.; Holt, Brian C.; Williams, John R.; Lammert, Stephen A.; Robison, Richard A.; Tolley, H. Dennis; Lee, Milton L.

    2013-01-01

    Graphical abstract: -- Highlights: •An automated sample preparation system for Bacillus anthracis endospores was developed. •A thermochemolysis method was applied to produce and derivatize biomarkers for Bacillus anthracis detection. •The autoreactor controlled the precise delivery of reagents, and TCM reaction times and temperatures. •Solid phase microextraction was used to extract biomarkers, and GC–MS was used for final identification. •This autoreactor was successfully applied to the identification of Bacillus anthracis endospores. -- Abstract: An automated sample preparation system was developed and tested for the rapid detection of Bacillus anthracis endospores by gas chromatography–mass spectrometry (GC–MS) for eventual use in the field. This reactor is capable of automatically processing suspected bio-threat agents to release and derivatize unique chemical biomarkers by thermochemolysis (TCM). The system automatically controls the movement of sample vials from one position to another, crimping of septum caps onto the vials, precise delivery of reagents, and TCM reaction times and temperatures. The specific operations of introduction of sample vials, solid phase microextraction (SPME) sampling, injection into the GC–MS system, and ejection of used vials from the system were performed manually in this study, although they can be integrated into the automated system. Manual SPME sampling is performed by following visual and audible signal prompts for inserting the fiber into and retracting it from the sampling port. A rotating carousel design allows for simultaneous sample collection, reaction, biomarker extraction and analysis of sequential samples. Dipicolinic acid methyl ester (DPAME), 3-methyl-2-butenoic acid methyl ester (a fragment of anthrose) and two methylated sugars were used to compare the performance of the autoreactor with manual TCM. Statistical algorithms were used to construct reliable bacterial endospore signatures, and 24

  15. Onsite well screening with a transportable gas chromatography/mass spectrometer system

    International Nuclear Information System (INIS)

    Rossabi, J.; Eckenrode, B.A.; Owens, B.

    1992-01-01

    The number of hazardous waste site operations continue to multiply. The requirements for efficient chemical assessment and monitoring of these sites become more stringent daily. As more samples are required, the time required for cleanup operations also increases and may make analytical costs prohibitive. Thus improvements in operation efficiency and reduction of cost in evaluating specific sites to minimize or eliminate their toxic effects on the surrounding environment are critical. For many years a formal policy did not exist for the disposal of waste solvents and other chemicals, thus many of these compounds were disposed of ensite. So long as these materials were contained onsite they were not considered to pose a threat to the surrounding environment. We have since determined that many of these compounds found their way into the groundwater. Contaminants such as trichloroethylene and perchloroethylene, which were heavily used for cleaning and degreasing purposes, must be monitored. Groundwater wells can be used to define the location and extent of the migration of any contaminant plume and aid in the determination of required cleanup. The major problem is that monitoring of hundreds of wells may be necessary, requiring several hundred samples on a quarterly basis to characterize the degree and extent of any contamination. Onsite analysis of monitoring wells for this characterization of waste operations could provide time savings and significant cost reduction. Field analyses can provide the required analytical results quickly and at a reduced cost without compromising either sample integrity or data quality. By using onsite analytical instrumentation, such as a field-transportable gas chromatograph/mass spectrometer (GC/MS), screening analyses can be performed to eliminate retturning to the laboratory with meaningless samples. Onsite GC/MS will provide qualitative or semi-quantitative information that can significantly simplify subsequent laboratory analyses

  16. Analysis of essential oil of eaglewood tree (Aquilaria agallocha Roxb. by gas chromatography mass spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Nazrul Islam Bhuiyan

    2009-06-01

    Full Text Available The study was carried out to find out the differences in composition of oils obtained from healthy, naturally infected and artificially screws wounds eaglewood (Aquilaria agallocha Roxb. using gas chromatography mass spectrometry (GC-MS analysis. Natural healthy plants agar contained octacosane (19.83%, naphthalene, 1,2,3,5,6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methylethenyl-, [1R-(1.alpha.,7.beta.,8a.alpha.]- (12.67%, 5-isobutyramido-2-methyl pyrimidine (13.52%, caryophyllene oxide (11.25% and (.+-.-cadinene (5.46%. Natural infected plants agar (super agar contained cycloheptane, 4-methylene-1-methyl-2-(2-methyl-1-propen-1-yl-1-vinyl- (46.17%, caryophyllene oxide (33.00% and 7-Isopropenyl-4a-methyl-1-methylenedecahydronaphthalene (20.83%. Artificially screw injected plants agar contained diisooctyl phthalate (71.97%, 1H-Cycloprop[e]azulen-4-ol, decahydro-1,1,4,7-tetramethyl-, [1ar-(1a.alpha.,4.beta.,4a.beta., 7.alpha., 7a.beta., 7b.alpha.]- (9.16%, hexadecanoic acid (7.05%, naphthalene, 1,2,3,5,6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methylethenyl-, [1R-(1.alpha.,7.beta.,8a.alpha.]- (6.45% and aristolene (5.36%. This study showed a marked difference in the oil compositions among the treatments with regards to their quality.

  17. Analysis of essential oil of eaglewood tree (Aquilaria agallocha Roxb. by gas chromatography mass spectrometry

    Directory of Open Access Journals (Sweden)

    Mohammad Nazrul Islam Bhuiyan

    2009-03-01

    Full Text Available The study was carried out to find out the differences in composition of oils obtained from healthy, naturally infected and artificially screws wounds eaglewood (Aquilaria agallocha Roxb. using gas chromatography mass spectrometry (GC-MS analysis. Natural healthy plants agar contained octacosane (19.83%, naphthalene, 1,2,3,5,6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methylethenyl-, [1R-(1.alpha.,7.beta.,8a.alpha.]- (12.67%, 5-isobutyramido-2-methyl pyrimidine (13.52%, caryophyllene oxide (11.25% and (.+-.-cadinene (5.46%. Natural infected plants agar (super agar contained cycloheptane, 4-methylene-1-methyl-2-(2-methyl-1-propen-1-yl-1-vinyl- (46.17%, caryophyllene oxide (33.00% and 7-Isopropenyl-4a-methyl-1-methylenedecahydronaphthalene (20.83%. Artificially screw injected plants agar contained diisooctyl phthalate (71.97%, 1H-Cycloprop[e]azulen-4-ol, decahydro-1,1,4,7-tetramethyl-, [1ar-(1a.alpha.,4.beta.,4a.beta., 7.alpha., 7a.beta., 7b.alpha.]- (9.16%, hexadecanoic acid (7.05%, naphthalene, 1,2,3,5,6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methylethenyl-, [1R-(1.alpha.,7.beta.,8a.alpha.]- (6.45% and aristolene (5.36%. This study showed a marked difference in the oil compositions among the treatments with regards to their quality.

  18. Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

    International Nuclear Information System (INIS)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Higgins, C.E.; Jenkins, R.A.

    1994-05-01

    A thermal desorption/ps chromatography/mass spectrometry (TD/GC/MS) has been evaluated for the determination of volatile organic compounds (VOCS) in vapor phase samples using Carbosieve S-III/Carbotrap/Carotrap C triple sorbent traps (TST) similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an inhouse manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from twenty six compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitrites, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative, standard deviation of 0.55 to 24.3 % was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTS, minimal loss (10 to 22%) was observed after storing the spiked in, a 4 degree C refrigerator for 29 days. The only chromatographable artifact observed was a 5% conversion of isopropanol to acetone. The validated method been successfully applied, to the determination of VOCs collected from various emission sources in a diversified concentration range

  19. Surface-sampling and analysis of TATP by swabbing and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Romolo, Francesco Saverio; Cassioli, Luigi; Grossi, Silvana; Cinelli, Giuseppe; Russo, Mario Vincenzo

    2013-01-10

    The method of sample recovery for trace detection and identification of explosives plays a critical role in several criminal investigations. After bombing, there can be difficulties in sending big objects to a laboratory for analysis. Traces can also be searched for on large surfaces, on hands of suspects or on surfaces where the explosive was placed during preparatory phases (e.g. places where an IED was assembled, vehicles used for transportation, etc.). In this work, triacetone triperoxide (TATP) was synthesized from commercial precursors following reported methods. Several portions of about 6mg of TATP were then spread on different surfaces (e.g. floors, tables, etc.) or used in handling tests. Three different swabbing systems were used: a commercial swab, pre-wetted with propan-2-ol (isopropanol) and water (7:3), dry paper swabs, and cotton swabs wetted with propan-2-ol. Paper and commercial swabs were also used to sample a metal plate, where a small charge of about 4g of TATP was detonated. Swabs were sealed in small glass jars with screw caps and Parafilm(®) M and sent to the laboratory for analysis. Swabs were extracted and analysed several weeks later by gas chromatography/mass spectrometry. All the three systems gave positive results, but wetted swabs collected higher amounts of TATP. The developed procedure showed its suitability for use in real cases, allowing TATP detection in several simulations, including a situation in which people wash their hands after handling the explosive. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  20. Triple sorbent thermal desorption/gas chromatography/mass spectrometry determination of vapor phase organic contaminants

    Energy Technology Data Exchange (ETDEWEB)

    Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Higgins, C.E.; Jenkins, R.A.

    1994-05-01

    A thermal desorption/ps chromatography/mass spectrometry (TD/GC/MS) has been evaluated for the determination of volatile organic compounds (VOCS) in vapor phase samples using Carbosieve S-III/Carbotrap/Carotrap C triple sorbent traps (TST) similar to those available from a commercial source. The analysis was carried out with a Hewlett-Packard 5985A or 5995 GC/MS system with a modified injector to adapt an inhouse manufactured short-path desorber for transferring desorbate directly onto a cryofocusing loop for subsequent GC/MS analysis. Vapor phase standards generated from twenty six compounds were used for method validation, including alkanes, alkyl alcohols, alkyl ketones, and alkyl nitrites, a group of representative compounds that have previously been identified in a target airborne matrix. The method was validated based on the satisfactory results in terms of reproducibility, recovery rate, stability, and linearity. A relative, standard deviation of 0.55 to 24.3 % was obtained for the entire TD process (generation of gas phase standards, spiking the standards on and desorbing from TST) over a concentration range of 20 to 500 ng/trap. Linear correlation coefficients for the calibration curves as determined ranged from 0.81 to 0.99 and limits of detection ranged from 3 to 76 ng. For a majority of standards, recoveries of greater than 90% were observed. For three selected standards spiked on TSTS, minimal loss (10 to 22%) was observed after storing the spiked in, a 4{degree}C refrigerator for 29 days. The only chromatographable artifact observed was a 5% conversion of isopropanol to acetone. The validated method been successfully applied, to the determination of VOCs collected from various emission sources in a diversified concentration range.

  1. A gas chromatography-tandem quadrupole mass spectrometric analysis of policosanols in commercial vegetable oils.

    Science.gov (United States)

    Jung, Dong Min; Lee, Mi Jin; Yoon, Suk Hoo; Jung, Mun Yhung

    2011-08-01

    Reportedly policosanols (PCs) have various beneficial functionalities on health. A gas chromatography-tandem mass spectrometry (GC-MS/MS) with a low limit of detection (LOD), and high specificity, recovery, and precision was successfully established for the PC analysis in vegetable oils. The LODs for the PCs were in the range of 0.002 to 0.016 μg/mL. The relative standard deviation (RSD) for the repeated analysis of PCs was less than 3.356%. The mean recoveries for spiked heptacosanol and octacosanol in vegetable oil were 102.3% and 106.3%, respectively. The total PC contents in the vegetable oils varied from 3.01 to 427.83 mg/kg oil. Perilla seed, grape seed, and rice bran oils were found to be highly rich sources of PCs, containing 427.83, 245.15, and 171.17 mg PCs/kg oil, respectively. Corn, sesame, and soybean oils contained only a negligible quantity of PCs. The PC composition in vegetable oils was greatly source dependent. In perilla seed oil, octacosanol was the single most predominant component, representing 55.93% of the total PC. In grape seed oil, however, hexacosanol is the most abundant PC, followed by octacosanol, tetracosanol, and triacontanol in a decreasing order. The major PCs in rice bran oil were triacontanol, octacosanol, hexacosanol, and tetracosanol, which constituted over 87.3% of the total PC. This represents the 1st report on the composition and contents of PC in most vegetable oils analyzed here. The information might be used for the development of vegetable oil products with beneficial functionality. © 2011 Institute of Food Technologists®

  2. Gas-phase dissociation study of erythrinian alkaloids by electrospray ionization mass spectrometry and computational methods.

    Science.gov (United States)

    Guaratini, T; Feitosa, L G P; Silva, D B; Lopes, N P; Lopes, J L C; Vessecchi, R

    2017-09-01

    Alkaloids from plants of the genus Erythrina display important biological activities, including anxiolytic action. Characterization of these alkaloids by mass spectrometry (MS) has contributed to the construction of a spectral library, has improved understanding of their structures and has supported the proposal of fragmentation mechanisms in light of density functional calculations. In this study, we have used low-resolution and high-resolution MS n analyses to investigate the fragmentation patterns of erythrinian alkaloids; we have employed the B3LYP/6-31+G(d,p) model to obtain their reactive sites. To suggest the fragmentation mechanism of these alkaloids, we have studied their protonation sites by density functional calculation, and we have obtained their molecular electrostatic potential map and their gas-phase basicity values. These analyses have indicated the most basic sites on the basis of the proton affinities of the nitrogen and oxygen atoms. The protonated molecules were generated by two major fragmentations, namely, neutral loss of CH 3 OH followed by elimination of H 2 O. High-resolution analysis confirmed elimination of NH 3 by comparison with the losses of H 2 and •CH 3 . NH 3 was eliminated from compounds that did not bear a substituent on ring C. The benzylic carbocation initiated the dissociation mechanism, and the first reaction involved charge transfer from a lone pair of electrons in the oxygen atoms. The second reaction consisted of ring contraction with loss of a CO molecule. The presence of hydroxy and epoxy groups could change the intensity or the occurrence of the fragmentation pathways. Given that erythrinian alkaloids are applied in therapeutics and are promising leads for the development of new drugs, the present results could aid identification of several analogues of these alkaloids in biological samples and advance pharmacokinetic studies of new plant derivatives based on MS n and MS/MS analyses. Copyright © 2017 John Wiley

  3. Technical advance: simultaneous analysis of metabolites in potato tuber by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Roessner, U; Wagner, C; Kopka, J; Trethewey, R N; Willmitzer, L

    2000-07-01

    A new method is presented in which gas chromatography coupled to mass spectrometry (GC-MS) allows the quantitative and qualitative detection of more than 150 compounds within a potato tuber, in a highly sensitive and specific manner. In contrast to other methods developed for metabolite analysis in plant systems, this method represents an unbiased and open approach that allows the detection of unexpected changes in metabolite levels. Although the method represents a compromise for a wide range of metabolites in terms of extraction, chemical modification and GC-MS analysis, for 25 metabolites analysed in detail the recoveries were found to be within the generally accepted range of 70-140%. Further, the reproducibility of the method was high: the error occurring in the analysis procedures was found to be less than 6% for 30 out of 33 compounds tested. Biological variability exceeded the systematic error of the analysis by a factor of up to 10. The method is also suited for upscaling, potentially allowing the simultaneous analysis of a large number of samples. As a first example this method has been applied to soil- and in vitro-grown tubers. Due to the simultaneous analysis of a wide range of metabolites it was immediately apparent that these systems differ significantly in their metabolism. Furthermore, the parallel insight into many pathways allows some conclusions to be drawn about the underlying physiological differences between both tuber systems. As a second example, transgenic lines modified in sucrose catabolism or starch synthesis were analysed. This example illustrates the power of an unbiased approach to detecting unexpected changes in transgenic lines.

  4. Planck/SDSS Cluster Mass and Gas Scaling Relations for a Volume-Complete redMaPPer Sample

    Science.gov (United States)

    Jimeno, Pablo; Diego, Jose M.; Broadhurst, Tom; De Martino, I.; Lazkoz, Ruth

    2018-04-01

    Using Planck satellite data, we construct Sunyaev-Zel'dovich (SZ) gas pressure profiles for a large, volume-complete sample of optically selected clusters. We have defined a sample of over 8,000 redMaPPer clusters from the Sloan Digital Sky Survey (SDSS), within the volume-complete redshift region 0.100 Dividing the sample into richness bins we simultaneously solve for the mean cluster mass in each bin together with the corresponding radial pressure profile parameters, employing an MCMC analysis. These profiles are well detected over a much wider range of cluster mass and radius than previous work, showing a clear trend towards larger break radius with increasing cluster mass. Our SZ-based masses fall ˜16% below the mass-richness relations from weak lensing, in a similar fashion as the "hydrostatic bias" related with X-ray derived masses. Finally, we derive a tight Y500-M500 relation over a wide range of cluster mass, with a power law slope equal to 1.70 ± 0.07, that agrees well with the independent slope obtained by the Planck team with an SZ-selected cluster sample, but extends to lower masses with higher precision.

  5. Spontaneous Separation in Trapped Fermi Gas with p-Wave Interactions: Due to the Mass-Imbalance

    Science.gov (United States)

    Kang, Yanshuang; Sun, Zongli; Kang, Yanmei; Li, Yushan; Tan, Shanshan

    2018-03-01

    Based on density functional theory, the spontaneous separation in the mass-imbalanced Fermi-Fermi mixture is studied. The ground-state energy density functional is constructed with the effective contact interaction, with which the ground-state density profiles of the mixture are calculated under different conditions of mass-imbalance and coupling strength. The influence of mass-imbalance on the separation and the cloud size is analyzed. In addition, the system with both mass- and population-imbalance is also calculated and studied. Despite our rough treatment in the Thomas-Fermi approximation, it is hoped that the results may provide new clues to understand the nature of phase separation of a trapped ultracold gas in both theoretical and experimental researches in the future.

  6. Innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard

    International Nuclear Information System (INIS)

    Varlet, V.; Smith, F.; Froidmont, S. de; Dominguez, A.; Rinaldi, A.; Augsburger, M.; Mangin, P.; Grabherr, S.

    2013-01-01

    Graphical abstract: -- Highlights: •We developed a method for CO 2 analysis in cardiac samples and quantification by 13 CO 2 . •This method was fully validated by accuracy profile. •We have applied this method to perform CO 2 precise quantification for forensic applications. •Context of the death could be documented following CO 2 concentrations. -- Abstract: A novel approach to measure carbon dioxide (CO 2 ) in gaseous samples, based on a precise and accurate quantification by 13 CO 2 internal standard generated in situ is presented. The main goal of this study was to provide an innovative headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable in the routine determination of CO 2 . The main drawback of the GC methods discussed in the literature for CO 2 measurement is the lack of a specific internal standard necessary to perform quantification. CO 2 measurement is still quantified by external calibration without taking into account analytical problems which can often occur considering gaseous samples. To avoid the manipulation of a stable isotope-labeled gas, we have chosen to generate in situ an internal labeled standard gas ( 13 CO 2 ) on the basis of the stoichiometric formation of CO 2 by the reaction of hydrochloric acid (HCl) with sodium hydrogen carbonate (NaH 13 CO 3 ). This method allows a precise measurement of CO 2 concentration and was validated on various human postmortem gas samples in order to study its efficiency

  7. The effect of microbubbles on gas-liquid mass transfer coefficient and degradation rate of COD in wastewater treatment.

    Science.gov (United States)

    Yao, Kangning; Chi, Yong; Wang, Fei; Yan, Jianhua; Ni, Mingjiang; Cen, Kefa

    2016-01-01

    A commonly used aeration device at present has the disadvantages of low mass transfer rate because the generated bubbles are several millimeters in diameter which are much bigger than microbubbles. Therefore, the effect of a microbubble on gas-liquid mass transfer and wastewater treatment process was investigated. To evaluate the effect of each bubble type, the volumetric mass transfer coefficients for microbubbles and conventional bubbles were determined. The volumetric mass transfer coefficient was 0.02905 s(-1) and 0.02191 s(-1) at a gas flow rate of 0.67 L min(-1) in tap water for microbubbles and conventional bubbles, respectively. The degradation rate of simulated municipal wastewater was also investigated, using aerobic activated sludge and ozone. Compared with the conventional bubble generator, the chemical oxygen demand (COD) removal rate was 2.04, 5.9, 3.26 times higher than those of the conventional bubble contactor at the same initial COD concentration of COD 200 mg L(-1), 400 mg L(-1), and 600 mg L(-1), while aerobic activated sludge was used. For the ozonation process, the rate of COD removal using microbubble generator was 2.38, 2.51, 2.89 times of those of the conventional bubble generator. Based on the results, the effect of initial COD concentration on the specific COD degradation rate were discussed in different systems. Thus, the results revealed that microbubbles could enhance mass transfer in wastewater treatment and be an effective method to improve the degradation of wastewater.

  8. [Specific detection of urinary sympathomimetic amines for control of anti-doping by gas chromatography-mass spectroscopy].

    Science.gov (United States)

    Franceschini, A; Duthel, J M; Vallon, J J

    1991-03-22

    A specific, sensitive and reliable gas chromatography-mass spectrometry (GC-MS) technique for detection of sympathomimetic amines following urinary extraction is proposed. Amphetamine, phentermine, ephedrine, mephenorex, methylphenidate, benzphetamine, clobenzorex and internal standard (fenfluramine) are extracted from urines at pH 7.0 using elution by chloroform-isopropanol on C18 cartridges. Derivatization followed by GC-MS analysis allows identification of these drugs founded on relative retention times and mass spectra. The quantitation limit for derivatizable drugs was found to be 200 ng/ml and 500 ng/ml for underivatizable drugs.

  9. Characterization of odor-active compounds of various Chrysanthemum essential oils by gas chromatography-olfactometry, gas chromatography-mass spectrometry and their correlation with sensory attributes.

    Science.gov (United States)

    Xiao, Zuobing; Fan, Binbin; Niu, Yunwei; Wu, Minling; Liu, Junhua; Ma, Shengtao

    2016-01-15

    Volatiles of five kinds of Chrysanthemum essential oils with different manufactures were characterized by descriptive sensory analysis, gas chromatography-olfactometry (GC-O), gas chromatography-mass spectrometry (GC-MS) and statistics analysis. Six sensory attributes (floral, woody, grassy, fruity, sour and minty) were selected to assess Chrysanthemum essential oils. A total of 38 volatile compounds were detected and quantified using standard substances by GC-O and GC-MS. Terpenes constituted the largest chemical group among the volatiles of the essential oils. Then partial least squares regression (PLSR) was used to elucidate the relationship between sensory attributes and aroma compounds. The result showed that α-pinene, β-thujene, α-terpinolen, β-cubebene, caryophyllene, (Z)β-farnesene, (-)-spathulenol, linalool, camphor, camphene, 4-terpineol, Z-citral and 4-isopropyltoluene were typical aroma compounds covaried with characteristic aroma of Chrysanthemum essential oils. Copyright © 2015. Published by Elsevier B.V.

  10. Method development and validation for determining 1,3-butadiene in human blood by gas chromatography-mass spectrometry and head-space gas chromatography.

    Science.gov (United States)

    Zhang, Su-Jing; Shen, Bao-Hua; Zhuo, Xian-Yi

    2013-04-01

    To develop a simple, validated method for identifying and quantifying 1,3-butadiene (BD) in human blood by gas chromatography-mass spectrometry (GC-MS) and head-space gas chromatography (HS-GC). BD was identified by GC-MS and HS-GC, and quantified by HS-GC. The method showed that BD had a good linearity from 50 to 500 microg/mL (r > 0.99). The limits of detection and quantification were 10 microg/mL and 50 microg/mL, respectively. Both the intra-day precision and inter-day precision were < 6.08%, and the accuracy was 96.98%-103.81%. The method was applied to an actual case, and the concentration of BD in the case was 242 microg/mL in human blood. This simple method is found to be useful for the routine forensic analysis of acute exposure to BD.

  11. Identification of organic acids as potential biomarkers in the urine of autistic children using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Żurawicz, Ewa; Struck, Wiktoria; Markuszewski, Michał

    2014-09-01

    There is a need to identify metabolic phenotypes in autism as they might each require unique approaches to prevention. Biological markers can help define autism subtypes and reveal potential therapeutic targets. The aim of the study was to identify alterations of small molecular weight compounds and to find potential biomarkers. Gas chromatography/mass spectrometry was employed to evaluate major metabolic changes in low molecular weight urine metabolites of 14 children with autism spectrum disorders vs. 10 non-autistic subjects. The results prove the usefulness of an identified set of 21 endogenous compounds (including 14 organic acids), whose levels are changed in diseased children. Gas chromatography/mass spectrometry method combined with multivariate statistical analysis techniques provide an efficient way of depicting metabolic perturbations of diseases, and may potentially be applicable as a novel strategy for the noninvasive diagnosis and treatment of autism. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Whole Microorganisms Studied by Pyrolysis-Gas Chromatography-Mass Spectrometry: Significance for Extraterrestrial Life Detection Experiments 1

    Science.gov (United States)

    Simmonds, Peter G.

    1970-01-01

    Pyrolysis-gas chromatography-mass spectrometric studies of two microorganisms, Micrococcus luteus and Bacillus subtilis var. niger, indicate that the majority of thermal fragments originate from the principal classes of bio-organic matter found in living systems such as protein and carbohydrate. Furthermore, there is a close qualitative similarity between the type of pyrolysis products found in microorganisms and the pyrolysates of other biological materials. Conversely, there is very little correlation between microbial pyrolysates and comparable pyrolysis studies of meteoritic and fossil organic matter. These observations will aid in the interpretation of a soil organic analysis experiment to be performed on the surface of Mars in 1975. The science payload of this landed mission will include a combined pyrolysis-gas chromatography-mass spectrometry instrument as well as several “direct biology experiments” which are designed to search for extraterrestrial life. PMID:16349890

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

    Directory of Open Access Journals (Sweden)

    Swati SONAWANE

    2015-12-01

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

  14. Comprehensive multidimensional gas chromatography coupled to low resolution quadrupole mass spectrometry for the analysis of PCDDs, PCDFs and PCBs

    Energy Technology Data Exchange (ETDEWEB)

    Costa, J.P. [Universitat de Barcelona (Spain). Facultat de Quimica, Dept. de Quimica Analitica; Korytar, P.; Boer, J. de [Netherlands Institutes for Fisheries Research, Ijmuiden (Netherlands); Leonards, P. [Instituto Quimico de Sarria, Barcelona (Spain)

    2004-09-15

    Because of the high persistency and extreme toxicity of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) and so-called dioxin-like polychlorinated biphenyls (PCBs), their trace level determination is a topic of much interest. The typical concentrations of this compounds, sub-ng/kg, makes that they have to be clearly separated from other, less toxic, congeners present in the samples and from the matrix and the use of sensitive techniques is required for the quantification. The analyses of the compounds are usually done by high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC-HRMS). Recently, alternative novel techniques have been developed which are improving the chromatographic separation, e.g. comprehensive multidimensional gas chromatography (GC x GC), for the analysis of the compounds. The aim of this work is to evaluate GC x GC coupled to a low resolution quadrupole mass spectrometer for the quantification of PCDDs, PCDFs and dioxin like PCBs.

  15. A continuous flow isotope ratio mass spectrometry method for high precision determination of dissolved gas ratios and isotopic composition

    DEFF Research Database (Denmark)

    Charoenpong, C. N.; Bristow, L. A.; Altabet, M. A.

    2014-01-01

    Dissolved gas ratios and isotopic compositions provide essential information about the biological and physical mechanisms influencing N-2, O-2, and Ar in aquatic systems. Current methods available are either limited by overall cost, labor-intensive sample collection and analysis, or insufficient...... ratio mass spectrometer (IRMS). A continuous flow of He carrier gas completely degasses the sample, and passes through the preparation and purification system before entering the IRMS for analysis. The use of this continuous He carrier permits short analysis times (less than 8 min per sample......) as compared with current high-precision methods. In addition to reference gases, calibration is achieved using air-equilibrated water standards of known temperature and salinity. Assessment of reference gas injections, air equilibrated standards, as well as samples collected in the field shows the accuracy...

  16. Gas

    International Nuclear Information System (INIS)

    1996-01-01

    The French government has decided to modify the conditions of extension of local natural gas authorities to neighbouring districts. The European Union is studying the conditions of internal gas market with the objective of more open markets although considering public service requirements

  17. Experimental and analytical studies of iodine mass transfer from xenon-iodine mixed gas bubble to liquid sodium pool

    International Nuclear Information System (INIS)

    Miyahara, S.; Sagawa, N.; Shimoyama, K.

    1996-01-01

    In the fuel pin failure accident of a liquid metal fast reactor, volatile fission products play an important role in the assessment of radiological consequences. Especially the radioisotopes of elemental iodine are important because of their high volatility and of the low permissible dose to human thyroid. The released iodines are known to be retained in the coolant sodium as sodium iodide due to the chemical affinity between alkali metals and halogens. However, the xenon and krypton released with iodines into the sodium pool as bubbles may influence the reaction rate of iodine with sodium during the bubble rising. So far, the only few experimental results have been available concerning the decontamination factor (DF: the ratio of the initial iodine mass in the mixed gas bubble to the released mass into the cover gas) of iodine in this phenomenon. Therefore, experimental and analytical studies were carried out to study the mass transfer of iodine from a xenon-iodine mixed gas bubble to the liquid sodium pool. In the experiments, the bubble was generated in the sodium pool by cracking a quartz ball which contains the xenon-iodine mixed gas and then, the mixed gas released into the argon cover gas was collected to determine the transferred iodine mass into the pool. A rising velocity of the bubble was measured by Chen-type void sensors arranged vertically in the pool. From the measured rising velocity and another observation of bubble behavior in simulated water experiments, it is found that the generated bubble breaks up into several smaller bubbles of spherical cap type during the rising period. Transferred iodine mass per unit initial bubble volume from the bubble to the sodium pool shows increases with increasing time and the initial iodine concentration. A mass transfer rate obtained by differentiating the transferred iodine mass with respect to the time indicates a rapid decrease just after the bubble generation and a slow decrease for the successive period

  18. Mass spectral identification and gas-liquid chromatographic determination of methyl 4-chloroindolyl-3-acetate in canned and frozen peas.

    Science.gov (United States)

    Heikes, D L

    1980-11-01

    Methyl 4-chloroindolyl-3-acetate (MCIA), a naturally occurring auxin, has been identified in canned and frozen peas by gas-liquid chromatography (GLC)/mass spectrometry. Eight samples were analyzed for MCIA using slightly modified official AOAC multiple pesticide residue procedures employing GLC with microcoulometric detection. Levels of MCIA averaged 0.20 ppm for canned peas and 0.16 ppm for frozen peas. Recovery of MCIA from a fortified sample was 40%.

  19. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    OpenAIRE

    Suriyavathana Muthukrishnan; Subha Palanisamy; Senthilkumar Subramanian; Sumathi Selvaraj; Kavitha Rani Mari; Ramalingam Kuppulingam

    2016-01-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. Th...

  20. Identification of Guest-Host Inclusion Complexes in the Gas Phase by Electrospray Ionization-Mass Spectrometry

    Science.gov (United States)

    Mendes, De´bora C.; Ramamurthy, Vaidhyanathan; Da Silva, Jose´ P.

    2015-01-01

    In this laboratory experiment, students follow a step-by-step procedure to prepare and study guest-host complexes in the gas phase using electrospray ionization-mass spectrometry (ESI-MS). Model systems are the complexes of hosts cucurbit[7]uril (CB7) and cucurbit[8]uril (CB8) with the guest 4-styrylpyridine (SP). Aqueous solutions of CB7 or CB8…

  1. [Analysis of aromatic hydrocarbons in cracking products of jet fuel by comprehensive two-dimensional gas chromatography-mass spectrometry].

    Science.gov (United States)

    Li, Haijing; Zhang, Xiangwen

    2017-08-08

    As coking precursors, aromatic hydrocarbons have an effect on the cracking stability of fuels. A method for identifying and quantitating aromatics in the supercritical cracking products of jet fuel was established by comprehensive two-dimensional gas chromatography coupled with mass spectrometry (GC×GC-MS). The effects of main chromatographic conditions such as initial oven temperature and modulation period on the separation of supercritical cracking products were studied. The method has good separation ability for polycyclic aromatic hydrocarbons (PAH) isomers. A total of 27 aromatics, including monocyclic aromatic hydrocarbons, bicyclic aromatic hydrocarbons, tricyclic aromatic hydrocarbons, tetracyclic aromatic hydrocarbons, etc., were identified based on standard mass spectra, the retention times of standards and literature reports. Moreover, the corresponding quantitative determination was achieved by external standard method of GC×GC-FID. The results showed that the contents of aromatics increased with the increase of gas yield. When gas yield reached 22%, the bicyclic aromatic hydrocarbons began to produce, and their contents increased exponentially with the increase of gas yield. Compared with the traditional GC-MS, the method has better separation and qualitative ability, and can be applied to the separation of complex samples and qualitative and quantitative analyses of cracking products.

  2. Development of an on-line low gas pressure cell for laser ablation-ICP-mass spectrometry

    International Nuclear Information System (INIS)

    Hirata, Takafumi

    2007-01-01

    An on-line low gas pressure cell device has been developed for elemental analysis using laser ablation-ICP-mass spectrometry (LA-ICPMS). Ambient gas in the sample cell was evacuated by a constant-flow diaphragm pump, and the pressure of the sample cell was controlled by changing the flow rate of He-inlet gas. The degree of sample re-deposition around the ablation pit could be reduced when the pressure of the ambient gas was lower than 50 kPa. Produced sample aerosol was drawn and taken from the outlet of the diaphragm pump, and directly introduced into the ICP ion source. The flow rate of He gas controls not only the gas pressure in the sample cell, but also the transport efficiency of the sample particles from the cell to the ICP, and the gas flow rate must be optimized to maximize the signal intensity of the analytes. The flow rates of the He carrier and Ar makeup gas were tuned to maximize the signal intensity of the analytes, and in the case of 238 U from the NIST SRM610 glass material, the signal intensity could be maximized with gas flow rates of 0.4 L/min for He and 1.2 L/min for Ar. The resulting gas pressure in the cell was 30-35 kPa. Using the low gas pressure cell device, the stability in the signal intensities and the resulting precision in isotopic ratio measurements were evaluated. The signal intensity profile of 63 Cu obtained by laser ablation from a metallic sample (NIST SRM976) demonstrated that typical spikes in the transient signal, which can become a large source of analytical error, were no longer found. The resulting precision in the 65 Cu/ 63 Cu ratio measurements was 2-3% (n=10, 2SD), which was half on the level obtained by laser ablation under atmospheric pressure (6-10%). The newly developed low-pressure cell device provides easier optimization of the operational conditions, together with smaller degrees of sample re-deposition and better stability in the signal intensity, even from a metallic sample. (author)

  3. Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena, E-mail: lorena.vidal@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Ahmadi, Mazaher [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Fernández, Elena [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Madrakian, Tayyebeh [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Canals, Antonio, E-mail: a.canals@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain)

    2017-06-08

    This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L{sup −1} for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L{sup −1} for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L{sup −1} for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L{sup −1} and 50 ng L{sup −1} spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L{sup −1}. Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. - Highlights: • A new extraction technique named Magnetic Headspace Adsorptive Extraction is presented. • Graphene oxide/iron oxide composite deposited on a neodymiun magnet as sorbent. • Sorbent of low cost, rapid and simple synthesis, easy manipulation and portability options. • Fast and efficient extraction and sensitive determination of chlorobenzenes in water samples.

  4. Analysis of chemical profiles of insect adhesion secretions by gas chromatography–mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reitz, Manuela [Institute of Organic Chemistry, University of Tübingen, Auf der Morgenstelle 8, 72076 Tübingen (Germany); Gerhardt, Heike [Institute of Pharmaceutical Sciences, University of Tübingen, Auf der Morgenstelle 8, 72076 Tübingen (Germany); Schmitt, Christian; Betz, Oliver [Institute of Evolution and Ecology, University of Tübingen, Auf der Morgenstelle 28, 72076 Tübingen (Germany); Albert, Klaus, E-mail: klaus.albert@uni-tuebingen.de [Institute of Organic Chemistry, University of Tübingen, Auf der Morgenstelle 8, 72076 Tübingen (Germany); Lämmerhofer, Michael, E-mail: michael.laemmerhofer@uni-tuebingen.de [Institute of Pharmaceutical Sciences, University of Tübingen, Auf der Morgenstelle 8, 72076 Tübingen (Germany)

    2015-01-07

    Highlights: • Adhesion secretions of desert locust analyzed by GC–MS. • Insect secretions are composed of apolar and polar constituents. • Sampling simplified with contact SPME as compared to solvent sampling. • Thin-film SPME-GC–MS revealed complex alkane patterns for insect secretions. • Differences in tarsal (feet) secretions and samples from tibiae (upper legs) identified. - Abstract: This article reports on the chemical analysis of molecular profiles of tarsal secretions of the desert locust Schistocerca gregaria (Forsskål, 1775) by gas chromatography hyphenated with quadrupol mass spectrometry (GC–MS) as well as {sup 1}H-nuclear magnetic resonance ({sup 1}H NMR) spectroscopy. Special focus of this study was to elaborate on sampling methods which enable selective microscale extraction of insect secretions in a spatially controlled manner, in particular tarsal adhesive secretions and secretions located on cuticle surfaces at the tibia. Various solvent sampling procedures and contact solid-phase microextraction (SPME) methods were compared in terms of comprehensiveness and extraction efficiencies as measured by signal intensities in GC–MS. Solvent sampling with water as extraction solvent gave access to the elucidation of chemical profiles of polar compound classes such as amino acids and carbohydrates, but is extremely tedious. Contact SPME on the other hand can be regarded as a simplified and more elegant alternative, in particular for the lipophilic compound fraction. Many proteinogenic amino acids and ornithine as well as carbohydrate monomers arabinose, xylose, glucose, and galactose were detected in tarsal secretions after acid hydrolysis of aqueous extracts. Qualitatively similar but quantitatively significantly different molecular profiles were found for the lipid fraction which contained mainly n-alkanes and internally branched monomethyl-, dimethyl-, and trimethyl-alkanes in the C23–C49 range as well as long chain fatty acids and

  5. Plasma metabolomic profiling of dairy cows affected with ketosis using gas chromatography/mass spectrometry.

    Science.gov (United States)

    Zhang, Hongyou; Wu, Ling; Xu, Chuang; Xia, Cheng; Sun, Lingwei; Shu, Shi

    2013-09-26

    Ketosis is an important problem for dairy cows` production performance. However, it is still little known about plasma metabolomics details of dairy ketosis. A gas chromatography/mass spectrometry (GC/MS) technique was used to investigate plasma metabolic differences in cows that had clinical ketosis (CK, n=22), subclinical ketosis (SK, n=32), or were clinically normal controls (NC, n=22). The endogenous plasma metabolome was measured by chemical derivatization followed by GC/MS, which led to the detection of 267 variables. A two-sample t-test of 30, 32, and 13 metabolites showed statistically significant differences between SK and NC, CK and NC, and CK and SK, respectively. Orthogonal signal correction-partial least-square discriminant analysis (OPLS-DA) revealed that the metabolic patterns of both CK and SK were mostly similar, with the exception of a few differences. The development of CK and SK involved disturbances in many metabolic pathways, mainly including fatty acid metabolism, amino acid metabolism, glycolysis, gluconeogenesis, and the pentose phosphate pathway. A diagnostic model arbitrary two groups was constructed using OPLS-DA and receiver-operator characteristic curves (ROC). Multivariate statistical diagnostics yielded the 19 potential biomarkers for SK and NC, 31 for CK and NC, and 8 for CK and SK with area under the curve (AUC) values. Our results showed the potential biomarkers from CK, SK, and NC, including carbohydrates, fatty acids, amino acids, even sitosterol and vitamin E isomers, etc. 2-piperidinecarboxylic acid and cis-9-hexadecenoic acid were closely associated with metabolic perturbations in ketosis as Glc, BHBA and NEFA for dealing with metabolic disturbances of ketosis in clinical practice. However, further research is needed to explain changes of 2,3,4-trihydroxybutyric acid, 3,4-dihydroxybutyric acid, α-aminobutyric acid, methylmalonic acid, sitosterol and α-tocopherol in CK and SK, and to reveal differences between CK and SK. Our

  6. Analysis of naphthenic acid mixtures as pentafluorobenzyl derivatives by gas chromatography-electron impact mass spectrometry.

    Science.gov (United States)

    Gutierrez-Villagomez, Juan Manuel; Vázquez-Martínez, Juan; Ramírez-Chávez, Enrique; Molina-Torres, Jorge; Trudeau, Vance L

    2017-01-01

    In this study, we report for the first time the efficiency of pentafluorobenzyl bromide (PFBBr) for naphthenic acid (NA) mixtures derivatization, and the comparison in the optimal conditions to the most common NAs derivatization reagents, BF 3 /MeOH and N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Naphthenic acids are carboxylic acid mixtures of petrochemical origin. These compounds are important for the oil industry because of their corrosive properties, which can damage oil distillation infrastructure. Moreover, NAs are commercially used in a wide range of products such as paint and ink driers, wood and fabric preservatives, fuel additives, emulsifiers, and surfactants. Naphthenic acids have also been found in sediments after major oils spills in the United States and South Korea. Furthermore, the toxicity of the oil sands process-affected water (OSPW), product of the oil sands extraction activities in Canada's oil sands, has largely been attributed to NAs. One of the main challenges for the chromatographic analysis of these mixtures is the resolution of the components. The derivatization optimization was achieved using surface response analysis with molar ratio and time as factors for derivatization signal yield. After gas chromatography-electron impact mass spectrometry (GC/EIMS) analysis of a mixture of NA standards, it was found that the signal produced by PFB-derivatives was 2.3 and 1.4 times higher than the signal produced by methylated and MTBS-derivatives, respectively. The pentafluorobenzyl derivatives have a characteristic fragment ion at 181m/z that is diagnostic for the differentiation of carboxylic and non-carboxylic acid components within mixtures. In the analysis of a Sigma and a Merichem derivatized oil extract NA mixtures, it was found that some peaks lack the characteristic fragment ion; therefore they are not carboxylic acids. Open column chromatography was used to obtain a hexane and a methanol fraction of the Sigma and

  7. Stabilization of gas-phase uranyl complexes enables rapid speciation using electrospray ionization and ion mobility-mass spectrometry.

    Science.gov (United States)

    Davis, Austen L; Clowers, Brian H

    2018-01-01

    Significant challenges exist when characterizing f-element complexes in solution using traditional approaches such as electrochemical and spectroscopic techniques as they do not always capture information for lower abundance species. However, provided a metal-complex with sufficient stability, soft ionization techniques such as electrospray offer a means to quantify and probe the characteristics of such systems using mass spectrometry. Unfortunately, the gas-phase species observed in ESI-MS systems do not always reflect the solution phase distributions due to the inherent electrochemical mechanism of the electrospray process, ion transfer from ambient to low pressures conditions, and other factors that are related to droplet evaporation. Even for simple systems (e.g. hydrated cations), it is not always clear whether the distribution observed reflects the solution phase populations or whether it is simply a result of the ionization process. This complexity is further compounded in mixed solvent systems and when multiply charged species are present. Despite these challenges, the benefits of mass spectrometry with respect to speed, sensitivity, and the ability to resolve isotopes continue to drive efforts to develop techniques for the speciation of metal complexes. Using an electrospray ionization atmospheric pressure ion mobility mass spectrometer (ESI-apIMS-MS), we demonstrate an approach to stabilize simple uranyl complexes during the ionization process and mobility separation to aid speciation and isotope profile analysis. Specifically, we outline and demonstrate the capacity of ESI-apIMS-MS methods to measure mobilities of different uranyl species, in simple mixtures, by promoting stable gas phase conformations with the addition of sulfoxides (i.e. dimethyl sulfoxide (DMSO), dibutyl sulfoxide (DBSO), and methyl phenyl sulfoxide (MPSO)). Addition of these sulfoxides, as observed in the mass spectrum and mobility domain, produce stable gas-phase conformations that

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

    Science.gov (United States)

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

    2015-12-15

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

  9. Evaluation of quantitative sulfur speciation in gas oils by Fourier transform ion cyclotron resonance mass spectrometry: validation by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Muller, Hendrik; Adam, Frederick M; Panda, Saroj K; Al-Jawad, Hanadi H; Al-Hajji, Adnan A

    2012-05-01

    Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) has been applied for the quantitative speciation of sulfur containing compounds in gas oil (GO). For this purpose, ionization and mass spectrometric parameters have been studied and optimized with a set of standard compounds and GO samples. Comprehensive two-dimensional gas chromatography (GCxGC) was used as the reference method. To allow a quantitative comparison between FT-ICR MS and GCxGC results for GO samples, FT-ICR MS parameters were optimized and data obtained by both techniques were standardized. Response factors were established for two ionization modes: atmospheric pressure photo ionization (APPI) and electrospray after selective derivatization of sulfur compounds (MeESI). To test the validity of the developed MS methods, a third GO was analyzed and response factors were applied. Comparison with GCxGC results showed good agreement for sulfur families (deviation within 5% and 15% for MeESI and APPI data, respectively). Abundances of individual isomer groups match within 40% in most cases. These results principally demonstrate the suitability of FT-ICR MS for a quantitative analysis of sulfur compounds (by DBE and carbon number distribution pattern) in petroleum middle distillates. This approach has the potential to be extended to higher- and non-boiling petroleum fractions where quantitative speciation is presently not available.

  10. Influence of the atomic mass of the background gas on laser ablation plume propagation

    DEFF Research Database (Denmark)

    Amoruso, Salvatore; Schou, Jørgen; Lunney, James G.

    2008-01-01

    A combination of time-of-flight ion probe measurements and gas dynamical modeling has been used to investigate the propagation of a laser ablation plume in gases of different atomic/molecular weight. The pressure variation of the ion time-of-flight was found to be well described by the gas...... dynamical model of Predtechensky and Mayorov (Appl. Supercond. 1:2011, 1993). In particular, the model describes how the pressure required to stop the plume in a given distance depends on the atomic/molecular weight of the gas, which is a feature that cannot be explained by standard point......-blast-wave descriptions of laser ablation plume expansion in gas....

  11. Mass transfer and chemical reaction in gas-liquid-liquid systems

    NARCIS (Netherlands)

    Brilman, Derk Willem Frederik

    1998-01-01

    Gas-liquid-liquid reaction systems may be encountered in several important fields of application as e.g. hydroformylation, alkylation, carboxylation, polymerisation, hydrometallurgy, biochemical processes and fine chemicals manufacturing. However, the reaction engineering aspects of these systems

  12. NGVS. Challenges for the Japanese gas industry to open the door for their mass introduction

    International Nuclear Information System (INIS)

    Akimoto, Minoru; Kawamoto, Hiroshi; Suzuki, Tatsuya; Yamaguchi, Eiji

    1997-01-01

    There have been a number of restraints in Japan delaying the introduction of natural gas vehicles (NGVs), which is a new comer in car industry. The Japanese gas industry, with support from government agencies, has conducted feasibility studies and clarified necessary technical and safety standards and regulations. These efforts have contributed to the government's drive for deregulation. Concurrently, the gas industry worked out its own scenarios for the promotion of NGVs in Japan, which helped the government in laying down necessary regulations and establishing clear market objectives for the vehicles as government policies. Such activities have yielded model introduction by the national and local governments and government-sponsored incentives for NGV promotion. For auto manufacturers, the gas industry proposed joint development projects and clarified potential market for NGVs. Consequently, many manufactures are now involved in their own NGV development projects. (au)

  13. Continuous Measurements of Dissolved Ne, Ar, Kr, and Xe Ratios with a Field-Deployable Gas Equilibration Mass Spectrometer.

    Science.gov (United States)

    Manning, Cara C; Stanley, Rachel H R; Lott, Dempsey E

    2016-03-15

    Noble gases dissolved in natural waters are useful tracers for quantifying physical processes. Here, we describe a field-deployable gas equilibration mass spectrometer (GEMS) that provides continuous, real-time measurements of Ne, Ar, Kr, and Xe mole ratios in natural waters. Gas is equilibrated with a membrane contactor cartridge and measured with a quadrupole mass spectrometer, after in-line purification with reactive metal alloy getters. We use an electron energy of 35 V for Ne to eliminate isobaric interferences, and a higher electron energy for the other gases to improve sensitivity. The precision is 0.7% or better and 1.0% or better for all mole ratios when the instrument is installed in a temperature-controlled environment and a variable-temperature environment, respectively. In the lab, the accuracy is 0.9% or better for all gas ratios using air as the only calibration standard. In the field (and/or at greater levels of disequilbrium), the accuracy is 0.7% or better for Ne/Kr, Ne/Ar, and Ar/Kr, and 2.5% or better for Ne/Xe, Ar/Xe, and Kr/Xe using air as the only calibration standard. The field accuracy improves to 0.6% or better for Ne/Xe, Ar/Xe, and Kr/Xe when the data is calibrated using discrete water samples run on a laboratory-based mass spectrometer. The e-folding response time is 90-410 s. This instrument enables the collection of a large number of continuous, high-precision and accuracy noble gas measurements at substantially reduced cost and labor compared to traditional methods.

  14. Monitoring the mass of UF6 gas and uranium deposits in aluminium pipes using X-ray fluorescence and X-ray transmission gauges

    International Nuclear Information System (INIS)

    Packer, T.W.; Smith, S.M.

    1984-12-01

    In order to determine the enrichment of UF 6 gas in centrifuge plant pipework it is necessary to measure the mass of the gas (pressure) and the mass per unit area of any uranium deposited on the pipe. This paper shows that it is possible to determine the pressure of the UF 6 gas in pipes 120 mm in diameter using an energy-dispersive X-ray fluorescence spectrometer. Results are also given of transmission measurements made using a low power X-ray generator operated at two different applied voltages. A method of using the two measurements to determine the mass per unit area of deposited uranium is described. (author)

  15. Methane mass balance at three landfill sites: What is the efficiency of capture by gas collection systems?

    International Nuclear Information System (INIS)

    Spokas, K.; Bogner, J.; Chanton, J.P.; Morcet, M.; Aran, C.; Graff, C.; Golvan, Y. Moreau-Le; Hebe, I.

    2006-01-01

    Many developed countries have targeted landfill methane recovery among greenhouse gas mitigation strategies, since methane is the second most important greenhouse gas after carbon dioxide. Major questions remain with respect to actual methane production rates in field settings and the relative mass of methane that is recovered, emitted, oxidized by methanotrophic bacteria, laterally migrated, or temporarily stored within the landfill volume. This paper presents the results of extensive field campaigns at three landfill sites to elucidate the total methane balance and provide field measurements to quantify these pathways. We assessed the overall methane mass balance in field cells with a variety of designs, cover materials, and gas management strategies. Sites included different cell configurations, including temporary clay cover, final clay cover, geosynthetic clay liners, and geomembrane composite covers, and cells with and without gas collection systems. Methane emission rates ranged from -2.2 to >10,000 mg CH 4 m -2 d -1 . Total methane oxidation rates ranged from 4% to 50% of the methane flux through the cover at sites with positive emissions. Oxidation of atmospheric methane was occurring in vegetated soils above a geomembrane. The results of these studies were used as the basis for guidelines by the French environment agency (ADEME) for default values for percent recovery: 35% for an operating cell with an active landfill gas (LFG) recovery system, 65% for a temporary covered cell with an active LFG recovery system, 85% for a cell with clay final cover and active LFG recovery, and 90% for a cell with a geomembrane final cover and active LFG recovery

  16. Eruption mass estimation using infrasound waveform inversion and ash and gas measurements: Evaluation at Sakurajima Volcano, Japan

    Science.gov (United States)

    Fee, David; Izbekov, Pavel; Kim, Keehoon; Yokoo, Akihiko; Lopez, Taryn; Prata, Fred; Kazahaya, Ryunosuke; Nakamichi, Haruhisa; Iguchi, Masato

    2017-12-01

    Eruption mass and mass flow rate are critical parameters for determining the aerial extent and hazard of volcanic emissions. Infrasound waveform inversion is a promising technique to quantify volcanic emissions. Although topography may substantially alter the infrasound waveform as it propagates, advances in wave propagation modeling and station coverage permit robust inversion of infrasound data from volcanic explosions. The inversion can estimate eruption mass flow rate and total eruption mass if the flow density is known. However, infrasound-based eruption flow rates and mass estimates have yet to be validated against independent measurements, and numerical modeling has only recently been applied to the inversion technique. Here we present a robust full-waveform acoustic inversion method, and use it to calculate eruption flow rates and masses from 49 explosions from Sakurajima Volcano, Japan. Six infrasound stations deployed from 12-20 February 2015 recorded the explosions. We compute numerical Green's functions using 3-D Finite Difference Time Domain modeling and a high-resolution digital elevation model. The inversion, assuming a simple acoustic monopole source, provides realistic eruption masses and excellent fit to the data for the majority of the explosions. The inversion results are compared to independent eruption masses derived from ground-based ash collection and volcanic gas measurements. Assuming realistic flow densities, our infrasound-derived eruption masses for ash-rich eruptions compare favorably to the ground-based estimates, with agreement ranging from within a factor of two to one order of magnitude. Uncertainties in the time-dependent flow density and acoustic propagation likely contribute to the mismatch between the methods. Our results suggest that realistic and accurate infrasound-based eruption mass and mass flow rate estimates can be computed using the method employed here. If accurate volcanic flow parameters are known, application of

  17. Calibration strategy for semi-quantitative direct gas analysis using inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Gerdes, Kirk; Carter, Kimberly E.

    2011-01-01

    A process is described by which an ICP-MS equipped with an Octopole Reaction System (ORS) is calibrated using liquid phase standards to facilitate direct analysis of gas phase samples. The instrument response to liquid phase standards is analyzed to produce empirical factors relating ion generation and transmission efficiencies to standard operating parameters. Empirical factors generated for liquid phase samples are then used to produce semi-quantitative analysis of both mixed liquid/gas samples and pure gas samples. The method developed is similar to the semi-quantitative analysis algorithms in the commercial software, which have here been expanded to include gas phase elements such as Xe and Kr. Equations for prediction of relative ionization efficiencies and isotopic transmission are developed for several combinations of plasma operating conditions, which allows adjustment of limited parameters between liquid and gas injection modes. In particular, the plasma temperature and electron density are calculated from comparison of experimental results to the predictions of the Saha equation. Comparisons between operating configurations are made to determine the robustness of the analysis to plasma conditions and instrument operating parameters. Using the methods described in this research, the elemental concentrations in a liquid standard containing 45 analytes and treated as an unknown sample were quantified accurately to ± 50% for most elements using 133 Cs as a single internal reference. The method is used to predict liquid phase mercury within 12% of the actual concentration and gas phase mercury within 28% of the actual concentration. The results verify that the calibration method facilitates accurate semi-quantitative, gas phase analysis of metal species with sufficient sensitivity to quantify metal concentrations lower than 1 ppb for many metallic analytes.

  18. Suspected-target pesticide screening using gas chromatography-quadrupole time-of-flight mass spectrometry with high resolution deconvolution and retention index/mass spectrum library.

    Science.gov (United States)

    Zhang, Fang; Wang, Haoyang; Zhang, Li; Zhang, Jing; Fan, Ruojing; Yu, Chongtian; Wang, Wenwen; Guo, Yinlong

    2014-10-01

    A strategy for suspected-target screening of pesticide residues in complicated matrices was exploited using gas chromatography in combination with hybrid quadrupole time-of-flight mass spectrometry (GC-QTOF MS). The screening workflow followed three key steps of, initial detection, preliminary identification, and final confirmation. The initial detection of components in a matrix was done by a high resolution mass spectrum deconvolution; the preliminary identification of suspected pesticides was based on a special retention index/mass spectrum (RI/MS) library that contained both the first-stage mass spectra (MS(1) spectra) and retention indices; and the final confirmation was accomplished by accurate mass measurements of representative ions with their response ratios from the MS(1) spectra or representative product ions from the second-stage mass spectra (MS(2) spectra). To evaluate the applicability of the workflow in real samples, three matrices of apple, spinach, and scallion, each spiked with 165 test pesticides in a set of concentrations, were selected as the models. The results showed that the use of high-resolution TOF enabled effective extractions of spectra from noisy chromatograms, which was based on a narrow mass window (5 mDa) and suspected-target compounds identified by the similarity match of deconvoluted full mass spectra and filtering of linear RIs. On average, over 74% of pesticides at 50 ng/mL could be identified using deconvolution and the RI/MS library. Over 80% of pesticides at 5 ng/mL or lower concentrations could be confirmed in each matrix using at least two representative ions with their response ratios from the MS(1) spectra. In addition, the application of product ion spectra was capable of confirming suspected pesticides with specificity for some pesticides in complicated matrices. In conclusion, GC-QTOF MS combined with the RI/MS library seems to be one of the most efficient tools for the analysis of suspected-target pesticide residues

  19. A fast, comprehensive screening method for doping agents in urine by gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Van Eenoo, Peter; Van Gansbeke, Wim; De Brabanter, Nik; Deventer, Koen; Delbeke, Frans T

    2011-05-27

    The use of performance enhancing drugs in sports is prohibited. For the detection of misuse of such substances gas chromatography or liquid chromatography coupled to mass spectrometry are the most frequently used detection techniques. In this work the development and validation of a fast gas chromatography tandem mass spectrometric method for the detection of a wide range of doping agents is described. The method can determine 13 endogenous steroids (the steroid profile), 19-norandrosterone, salbutamol and 11-nor-Δ9-tetrahydrocannabinol.9carboxylic acid in the applicable ranges and to detect qualitatively over 140 substances in accordance with the minimum required performance levels of the World Anti-Doping Agency in 1ml of urine. The classes of substances included in the method are anabolic steroids, β2-agonists, stimulants, narcotics, hormone antagonists and modulators and beta-blockers. Moreover, using a short capillary column and hydrogen as a carrier gas the run time of the method is less than 8min. Copyright © 2010 Elsevier B.V. All rights reserved.

  20. MASS ACCRETION AND ITS EFFECTS ON THE SELF-SIMILARITY OF GAS PROFILES IN THE OUTSKIRTS OF GALAXY CLUSTERS

    Energy Technology Data Exchange (ETDEWEB)

    Lau, Erwin T.; Nagai, Daisuke; Avestruz, Camille [Department of Physics, Yale University, New Haven, CT 06520 (United States); Nelson, Kaylea [Yale Center for Astronomy and Astrophysics, Yale University, New Haven, CT 06520 (United States); Vikhlinin, Alexey, E-mail: erwin.lau@yale.edu [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge, MA 02138 (United States)

    2015-06-10

    Galaxy clusters exhibit remarkable self-similar behavior which allows us to establish simple scaling relationships between observable quantities and cluster masses, making galaxy clusters useful cosmological probes. Recent X-ray observations suggested that self-similarity may be broken in the outskirts of galaxy clusters. In this work, we analyze a mass-limited sample of massive galaxy clusters from the Omega500 cosmological hydrodynamic simulation to investigate the self-similarity of the diffuse X-ray emitting intracluster medium (ICM) in the outskirts of galaxy clusters. We find that the self-similarity of the outer ICM profiles is better preserved if they are normalized with respect to the mean density of the universe, while the inner profiles are more self-similar when normalized using the critical density. However, the outer ICM profiles as well as the location of accretion shock around clusters are sensitive to their mass accretion rate, which causes the apparent breaking of self-similarity in cluster outskirts. We also find that the collisional gas does not follow the distribution of collisionless dark matter (DM) perfectly in the infall regions of galaxy clusters, leading to 10% departures in the gas-to-DM density ratio from the cosmic mean value. Our results have a number implications for interpreting observations of galaxy clusters in X-ray and through the Sunyaev–Zel’dovich effect, and their applications to cosmology.

  1. Microstructural analysis of mass transport phenomena in gas diffusion media for high current density operation in PEM fuel cells

    Science.gov (United States)

    Kotaka, Toshikazu; Tabuchi, Yuichiro; Mukherjee, Partha P.

    2015-04-01

    Cost reduction is a key issue for commercialization of fuel cell electric vehicles (FCEV). High current density operation is a solution pathway. In order to realize high current density operation, it is necessary to reduce mass transport resistance in the gas diffusion media commonly consisted of gas diffusion layer (GDL) and micro porous layer (MPL). However, fundamental understanding of the underlying mass transport phenomena in the porous components is not only critical but also not fully understood yet due to the inherent microstructural complexity. In this study, a comprehensive analysis of electron and oxygen transport in the GDL and MPL is conducted experimentally and numerically with three-dimensional (3D) microstructural data to reveal the structure-transport relationship. The results reveal that the mass transport in the GDL is strongly dependent on the local microstructural variations, such as local pore/solid volume fractions and connectivity. However, especially in the case of the electrical conductivity of MPL, the contact resistance between carbon particles is the dominant factor. This suggests that reducing the contact resistance between carbon particles and/or the number of contact points along the transport pathway can improve the electrical conductivity of MPL.

  2. Analysis of selective androgen receptor modulators by gas chromatography-microchip atmospheric pressure photoionization-mass spectrometry.

    Science.gov (United States)

    Luosujärvi, Laura; Haapala, Markus; Thevis, Mario; Saarela, Ville; Franssila, Sami; Ketola, Raimo A; Kostiainen, Risto; Kotiaho, Tapio

    2010-02-01

    A gas chromatography-microchip atmospheric pressure photoionization-mass spectrometric (GC-microAPPI-MS) method was developed and used for the analysis of three 2-quinolinone-derived selective androgen receptor modulators (SARMs). SARMs were analyzed from spiked urine samples, which were hydrolyzed and derivatized with N-methyl-N-(trimethylsilyl)trifluoroacetamide before analysis. Trimethylsilyl derivatives of SARMs formed both radical cations (M(+*)) and protonated molecules ([M + H](+)) in photoionization. Better signal-to-noise ratios (S/N) were obtained in MS/MS analysis using the M(+*) ions as precursor ions than using the [M + H](+) ions, and therefore the M(+*) ions were selected for the precursor ions in selected reaction monitoring (SRM) analysis. Limits of detection (LODs) with the method ranged from 0.01 to 1 ng/mL, which correspond to instrumental LODs of 0.2-20 pg. Limits of quantitation ranged from 0.03 to 3 ng/mL. The mass spectrometric response to the analytes was linear (R > or = 0.995) from the LOQ concentration level up to 100 ng/mL concentration, and intra-day repeatabilities were 5%-9%. In addition to the GC-microAPPI-MS study, the proof-of-principle of gas chromatography-microchip atmospheric pressure chemical ionization-Orbitrap MS (GC-microAPCI-Orbitrap MS) was demonstrated. 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

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

    Data.gov (United States)

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

  4. Gas Chromatography and Mass Spectrometry Measurements and Protocols for Database and Library Development Relating to Organic Species in Support of the Mars Science Laboratory

    Science.gov (United States)

    Misra, P.; Garcia, R.; Mahaffy, P. R.

    2010-04-01

    An organic contaminant database and library has been developed for use with the Sample Analysis at Mars (SAM) instrumentation utilizing laboratory-based Gas Chromatography-Mass Spectrometry measurements of pyrolyzed and baked material samples.

  5. Domestic Preparedness Program: Evaluation of the Agilent Gas Chromatograph - Flame Photometric Detector/Mass Selective Detector (GC-FPD/MSD) System Against Chemical Warfare Agents Summary Report

    National Research Council Canada - National Science Library

    Longworth, Terri

    2003-01-01

    This report characterizes the chemical warfare agent (CWA) detection potential of the commercially available Agilent gas chromatograph-flame photometric detector/mass selective detector (GC-FPD/MSD...

  6. Studies of gas phase ion/molecule reactions by Fourier transform ion cyclotron resonance mass spectrometry

    International Nuclear Information System (INIS)

    Kleingeld, J.C.

    1984-01-01

    An important field in which Fourier-transform ion cyclotron resonance has useful applications is that of gas phase ion chemistry, the subject of this thesis. First, the general picture of ion-molecule reactions in the gas phase is discussed. Next, some positive ion-molecule reactions are described, whereas the remaining chapters deal with negative ion-molecule reactions. Most of these studies have been performed using the FT-ICR method. Reactions involving H 3 O - and NH 4 - ions are described whereas the other chapters deal with larger organic complexes. (Auth.)

  7. Determination of cholesterol and four phytosterols in foods without derivatization by gas chromatography-tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Yan-Zong Chen

    2015-12-01

    Full Text Available In this study, a method for determination of cholesterol and four phytosterols by gas chromatography coupled with electron impact ionization mode–tandem mass spectrometry without derivatization in general food was developed. The sample was saponified with 7.5% KOH in methanol. After heating on hot plate and reflux for 60 minutes, the saponified portion was extracted with n-hexane/petroleum ether (50:50, v/v. The extracts were evaporated with rotary evaporator and then redissolved with tetrahydrofuran. The tetrahydrofuran layer was transferred into an injection vial and analyzed by gas chromatography on a 30 m VF-5 column. Limit of quantification was 2 mg/kg. Recoveries of cholesterol and four phytosterols from general food were between 91% and 100%.

  8. Exposure Assessment of Acetamide in Milk, Beef, and Coffee Using Xanthydrol Derivatization and Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Vismeh, Ramin; Haddad, Diane; Moore, Janette; Nielson, Chandra; Bals, Bryan; Campbell, Tim; Julian, Allen; Teymouri, Farzaneh; Jones, A Daniel; Bringi, Venkataraman

    2018-01-10

    Acetamide has been classified as a possible human carcinogen, but uncertainties exist about its levels in foods. This report presents evidence that thermal decomposition of N-acetylated sugars and amino acids in heated gas chromatograph injectors contributes to artifactual acetamide in milk and beef. An alternative gas chromatography/mass spectrometry protocol based on derivatization of acetamide with 9-xanthydrol was optimized and shown to be free of artifactual acetamide formation. The protocol was validated using a surrogate analyte approach based on d 3 -acetamide and applied to analyze 23 pasteurized whole milk, 44 raw sirloin beef, and raw milk samples from 14 different cows, and yielded levels about 10-fold lower than those obtained by direct injection without derivatization. The xanthydrol derivatization procedure detected acetamide in every food sample tested at 390 ± 60 ppb in milk, 400 ± 80 ppb in beef, and 39 000 ± 9000 ppb in roasted coffee beans.

  9. 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.

  10. Solid-phase microcolumn extraction and gas chromatography-mass spectrometry identification of volatile organic compounds emitted by paper.

    Science.gov (United States)

    Hrivnák, Ján; Tölgyessy, Peter; Figedyová, Sona; Katuscák, Svetozár

    2009-11-15

    A rapid non-destructive sampling technique for the analysis of volatile organic compounds (VOCs) emitted by paper sheets is described. A capillary, which is connected to a microcolumn packed with Tenax TA, is inserted between two sheets at the centre of a paper stack encapsulated inside a PET/Al/PE composite foil. The other end of the microcolumn is connected to a gas-tight syringe and an appropriate volume of gaseous phase is aspirated. The microcolumn is then thermally desorbed in a modified GC inlet (modification is presented) and analysed by gas chromatography-mass spectrometry (GC-MS). In the chromatogram from the analysis of artificially aged paper sample 21 compounds were identified. Advantages of the method including the short sampling time (1 min), simplicity and economic aspect are discussed.

  11. Gas-phase fragmentation of peptides to increase the spatial resolution of the Hydrogen Exchange Mass Spectrometry experiment

    DEFF Research Database (Denmark)

    Jensen, Pernille Foged; Rand, Kasper Dyrberg

    2016-01-01

    are produced after precursor ion selection and thus do not add complexity to the LC-MS analysis. The key to obtaining optimal spatial resolution in a hydrogen exchange mass spectrometry (HX-MS) experiment is the fragmentation efficiency. This chapter discusses common fragmentation techniques like collision......-induced dissociation (CID) occur with complete Hydrogen-deuterium (H/D) scrambling, while other techniques that induce dissociation on a faster timescale through radical-based fragmentation channels, like electron-capture dissociation (ECD) and electron-transfer dissociation (ETD), occur inherently without H......Generation of overlapping peptides in solution via multiple proteases requires a very high peak capacity for the LC-MS analysis to minimize signal overlap. An inherent advantage of a gas-phase fragmentation step is that the additional gas-phase fragment ions used to sublocalize deuterium...

  12. Gas chromatographic-mass spectroscopic determination of benzene in indoor air during the use of biomass fuels in cooking time.

    Science.gov (United States)

    Sinha, Sukesh Narayan; Kulkarni, P K; Desai, N M; Shah, S H; Patel, G M; Mansuri, M M; Parikh, D J; Saiyed, H N

    2005-02-18

    A gas chromatography-mass spectroscopic method in electron ionization (EI) mode with MS/MS ion preparation using helium at flow rate 1 ml min(-1) as carrier gas on DB-5 capillary column (30 m x 0.25 mm i.d. film thickness 0.25 microm) has been developed for the determination of benzene in indoor air. The detection limit for benzene was 0.002 microg ml(-1) with S/N: 4 (S: 66, N: 14). The benzene concentration for cooks during cooking time in indoor kitchen using dung fuel was 114.1 microg m(-3) while it was 6.6 microg m(-3) for open type kitchen. The benzene concentration was significantly higher (p analytical chemist dealing with GC-MS in confirmation and quantification of benzene in environmental samples with health risk exposure assessment.

  13. The use of stable isotopes and gas chromatography/mass spectrometry in the identification of steroid metabolites in the equine

    International Nuclear Information System (INIS)

    Houghton, E.; Dumasia, M.C.; Teale, P.; Smith, S.J.; Cox, J.; Marshall, D.; Gower, D.B.

    1990-01-01

    Stable isotope gas chromatography/mass spectrometry has been used successfully in the elucidation of structures of urinary steroid metabolites in the horse and in the identification of metabolites isolated from in vivo perfusion and in vitro incubation studies using equine tissue preparations. Deuterium-labeled steroids, testosterone, dehydroepiandrosterone, and 5-androstene-3 beta,17 beta-diol have been synthesized by base-catalyzed isotope exchange methods and the products characterized by gas chromatography/mass spectrometry. [16,16(-2)H2]Dehydroepiandrosterone (plus radiolabeled dehydroepiandrosterone) was perfused into a testicular artery of a pony stallion and was shown to be metabolized into 2H2-labeled testosterone, 4-androstenedione, isomers of 5-androstene-3,17-diol, 19-hydroxytestosterone, and 19-hydroxy-4-androstenedione. In further studies, equine testicular minces have been incubated with 2H2-labeled and radiolabeled dehydroepiandrosterone and 5-androstene-3 beta, 17 beta-diol. The metabolites, whose identity was confirmed by stable isotope gas chromatography/mass spectrometry, proved the interconversion of the two substrates, as well as formation of testosterone and 4-androstenedione. The aromatization of dehydroepiandrosterone was also confirmed, together with the formation of an isomer of 5(10)-estrene-3,17-diol from both substrates showing 19-demethylation without concomitant aromatization. In studies of the feto-placental unit, the allantochorion was shown to aromatize [2H5]testosterone to [2H4]estradiol, the loss of one 2H from the substrate being consistent with aromatization of the A ring. The formation of 6-hydroxyestradiol was also confirmed in this study. The same technique has been valuable in determining the structure of two metabolites of nandrolone isolated from horse urine

  14. Hybrid recoil mass analyzer at IUAC – First results using gas-filled ...

    Indian Academy of Sciences (India)

    the positive and negative power supplies for safety, similar to HIRA, our earlier spectrometer. The second ... purity is expected to be less as only momentum analysis is possible in the first stage of HYRA. The gas-filled mode ... Multiple scattering effects on the efficiency reduction are ignored in this preliminary simulation.

  15. Method Development for the Determination of Fluorotelomer Alcohols in Soils by Gas Chromatography Mass Spectrometry

    Science.gov (United States)

    Fluorotelomer alcohols (FTOHs) have been widely studied as precursors to perfluorocarboxylates, e.g. 8:2 FTOH degrades to perfluorooctanoic acid (PFOA). This presentation describes an analytical method for the extraction and analysis of 6:2, 8:2, and 10:2 FTOHs. Gas chromatograph...

  16. Molecular analysis of sulphur-rich brown coals by flash pyrolysis-gas chromatography-mass spectrometry: The type III-S kerogen

    NARCIS (Netherlands)

    Sinninghe Damsté, J.S.; Las Heras, F.X.C. de; Leeuw, J.W. de

    1992-01-01

    The molecular composition of five brown coals from three different basins (Maestrazgo, Mequinenza and Rubielos) in Spain was investigated by flash pyrolysis-gas chromatography and flash pyrolysis-gas chromatography-mass spectrometry. In these techniques, the macromolecular material is thermally

  17. Gas chromatographic-mass spectrometric determination of aromatic hydrocarbon metabolites from livers of fish exposed to fuel oil.

    Science.gov (United States)

    Krahn, M M; Malins, D C

    1982-10-15

    Metabolites of several two- and three-ring aromatic hydrocarbons (AHs) have been found in livers of English sole exposed to No. 2 fuel oil. Four metabolites of the C2H5-naphthalenes, six of the C3H7-naphthalenes and one each of fluorene, phenanthrene and anthracene have been partially characterized and their concentrations, which ranged from 50 to 1100 ng/g, were determined. Metabolites were separated from the liver matrix using an automated extractor/concentrator. The resulting extract was then purified by high-performance liquid chromatography, and the metabolites were characterized and quantitated by gas chromatography-mass spectrometry.

  18. Rapid determination of polysaccharides in BianTi Soft Extract by spectrophotometry coupled with gas chromatography-mass spectrometry

    OpenAIRE

    Zheng, Minxia; Shen, Jie; Yang, Kai; Qian, Songxiang; Feng, Sujuan

    2010-01-01

    A simple approach for the rapid determination of polysaccharides in BianTi Soft Extract using spectrophotometry coupled with gas chromatography-mass spectrometry (GC-MS) was developed. The mixed standard solution composed of D-glucose, D-mannose, galactose and D-xylose in different proportions (1.00: 1.01: 0.12: 0.05) was prepared according to the monosaccharide composition analysis of the polysaccharides by GC-MS. The determination of polysaccharides by UV-Vis spectrophotometer was performed...

  19. Comparison of Gas Chromatography-Mass Spectrometry and Gas Chromatography-Tandem Mass Spectrometry with Electron Ionization and Negative-Ion Chemical Ionization for Analyses of Pesticides at Trace Levels in Atmospheric Samples

    Directory of Open Access Journals (Sweden)

    Renata Raina

    2008-01-01

    Full Text Available A comparison of detection limits of gas chromatography-mass spectrometry (GC-MS in selected ion monitoring (SIM with gas chromatography-tandem mass spectrometry (GC-MS/MS in selected reaction monitoring (SRM mode with both electron ionization (EI and negative-ion chemical ionization (NCI are presented for over 50 pesticides ranging from organochlorines (OCs, organophosphorus pesticides (OPs and pre-emergent herbicides used in the Canadian prairies (triallate, trifluralin, ethalfluralin. The developed GC-EI/SIM, GC-NCI/SIM, and GC-NCI/SRM are suitable for the determination of pesticides in air sample extracts at concentrations <100 pg µL−1 (<100 pg m−3 in air. No one method could be used to analyze the range of pre-emergent herbicides, OPs, and OCs investigated. In general GC-NCI/SIM provided the lowest method detection limits (MDLs commonly 2.5–10 pg µL−1 along with best confirmation (<25% RSD of ion ratio, while GC-NCI/SRM is recommended for use where added selectivity or confirmation is required (such as parathion-ethyl, tokuthion, carbofenothion. GC-EI/SRM at concentration <100 pg µL−1 was not suitable for most pesticides. GC-EI/SIM was more prone to interference issues than NCI methods, but gave good sensitivity (MDLs 1–10 pg µL−1 for pesticides with poor NCI response (OPs: sulfotep, phorate, aspon, ethion, and OCs: alachlor, aldrin, perthane, and DDE, DDD, DDT.

  20. Comparison of gas chromatography-mass spectrometry and gas chromatography-tandem mass spectrometry with electron ionization and negative-ion chemical ionization for analyses of pesticides at trace levels in atmospheric samples.

    Science.gov (United States)

    Raina, Renata; Hall, Patricia

    2008-09-09

    A comparison of detection limits of gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) with gas chromatography-tandem mass spectrometry (GC-MS/MS) in selected reaction monitoring (SRM) mode with both electron ionization (EI) and negative-ion chemical ionization (NCI) are presented for over 50 pesticides ranging from organochlorines (OCs), organophosphorus pesticides (OPs) and pre-emergent herbicides used in the Canadian prairies (triallate, trifluralin, ethalfluralin). The developed GC-EI/SIM, GC-NCI/SIM, and GC-NCI/SRM are suitable for the determination of pesticides in air sample extracts at concentrations air). No one method could be used to analyze the range of pre-emergent herbicides, OPs, and OCs investigated. In general GC-NCI/SIM provided the lowest method detection limits (MDLs commonly 2.5-10 pg microL(-1)) along with best confirmation (pesticides. GC-EI/SIM was more prone to interference issues than NCI methods, but gave good sensitivity (MDLs 1-10 pg microL(-1)) for pesticides with poor NCI response (OPs: sulfotep, phorate, aspon, ethion, and OCs: alachlor, aldrin, perthane, and DDE, DDD, DDT).

  1. A comparative study of the number and mass of fine particles emitted with diesel fuel and marine gas oil (MGO)

    Science.gov (United States)

    Nabi, Md. Nurun; Brown, Richard J.; Ristovski, Zoran; Hustad, Johan Einar

    2012-09-01

    The current investigation reports on diesel particulate matter emissions, with special interest in fine particles from the combustion of two base fuels. The base fuels selected were diesel fuel and marine gas oil (MGO). The experiments were conducted with a four-stroke, six-cylinder, direct injection diesel engine. The results showed that the fine particle number emissions measured by both SMPS and ELPI were higher with MGO compared to diesel fuel. It was observed that the fine particle number emissions with the two base fuels were quantitatively different but qualitatively similar. The gravimetric (mass basis) measurement also showed higher total particulate matter (TPM) emissions with the MGO. The smoke emissions, which were part of TPM, were also higher for the MGO. No significant changes in the mass flow rate of fuel and the brake-specific fuel consumption (BSFC) were observed between the two base fuels.

  2. Selective 3,4-Dihydroxyphenylalanine Analysis in Human Urine as Ethoxycarbonyltert- butyldimethylsilyl Derivatives by Gas Chromatography-Mass Spectrometry

    International Nuclear Information System (INIS)

    Paik, Man Jeong; Nguyen, Duc Toan; Cho, In Seon; Kim, Kyoung Rae; Cho, Ki Hong; Choi, Sang Dun; Lee, Gwang; Yoon, Jae Hwan; Shim, Woo Young

    2011-01-01

    A new analytical method for measurement of 3,4-dihydroxyphenylalanine (DOPA) in human urine was developed. DOPA from an aqueous solution was converted into an ethoxycarbonyl (EOC) derivative. A tertbutyldimethylsilyl (TBDMS) reaction under anhydrous conditions was then attempted for analysis by gas chromatography-mass spectrometry in selected ion monitoring mode. A new mass spectral data on DOPA as a tri-EOC/mono-TBDMS derivative was built. This method showed good linearity (r ≥ 0.999), precision (% relative standard deviation = 3.1-9.2), and accuracy (% relative error = .7.2-8.8), with a detection limit of 0.05 ng/mL. This selective and accurate method of DOPA analysis will be useful for biochemical monitoring of various neurological disorders including Parkinson's disease in biological fluids

  3. The effects of geometry and operational conditions on gas holdup, liquid circulation and mass transfer in an airlift reactor

    Directory of Open Access Journals (Sweden)

    Gouveia E.R.

    2003-01-01

    Full Text Available In airlift reactors transport phenomena are achieved by pneumatic agitation and circulation occurs in a defined cyclic pattern through a loop. In the present work, the effect of geometrical relations on gas holdup and liquid velocity, and consequently on the gas-liquid mass transfer coefficient, was studied in a 6-liter airlift bioreactor with A D/A R = 0.63; A D, downcomer cross-sectional area, and A R, riser cross-sectional area. Measurements of the volumetric oxygen transfer coefficient (kLa were taken in a water-air system using a modified sulfite oxidation method. Different conditions were examined by varying parameters such as superficial air velocity in the riser (U GR, bottom clearance (d1 and top clearance (d2. It was observed from the experimental results that d1 and d2 have a remarkable effect on kLa values. The effect is due to their influence on gas holdup and liquid velocity, consequently affecting kLa. Superficial air velocity in the riser (U GR ranged from 0.0126 to 0.0440 m.s-1 and kLa varied between 40 to 250 h-1, whereas gas holdup (e reached values up to 0.2. The volumetric oxygen transfer coefficient (kLa, gas holdup in the riser (eR and downcomer (eD and superficial liquid velocity in the riser (U LR for all the geometrical relations were successfully correlated with dimensionless numbers, namely, the Sherwood number (Sh and the Froude number (Fr as well as with geometrical relations such as the bottom space ratio (B = d1/D D and top space ratio (T = (d2 + D D/D D.

  4. Optimization of plasma sampling depth and aerosol gas flow rates for single particle inductively coupled plasma mass spectrometry analysis.

    Science.gov (United States)

    Kálomista, Ildikó; Kéri, Albert; Galbács, Gábor

    2017-09-01

    We performed experiments to assess the separate and also the combined effect of the sampling depth and the aerosol gas flow rates on the signal formation in single particle inductively coupled plasma mass spectrometry (spICP-MS) measurements by using dispersions containing Ag and Au NPs. It was found that the NP signal can significantly be improved by the optimization of the sampling depth. With respect to the "robust" setting, a signal improvement of nearly 100% could be achieved, which translates into a 25-30% improvement in size detection limits. It was also found that the shape of the spICP-MS signal histograms also change with the change of the plasma sampling depth. It was demonstrated that nanoparticle peak separation can also be significantly enhanced by using sampling depth optimization. The effect of the aerosol dilution gas flow, now standard in most ICP-MS instruments, on the spICP-MS signal formation was also studied for the first time in the literature, as this flow was hoped to make spICP-MS measurements more practical and faster via the on-line dilution of the aerosol generated from nano-dispersions. Our experimental results revealed that the dilution gas flow can only be used for a moderate aerosol dilution in spICP-MS measurements, if the gas flow going to the pneumatic nebulizer is proportionally lowered at the same time. This however was found to cause a significant worsening in the operation of the sample introduction system, which gives rise to a strong NP signal loss. Thus it was concluded that the use of the aerosol dilution gas flow, in its present form, can not be suggested for spICP-MS analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Identification of key aromatic compounds in Congou black tea by PLSR with variable importance of projection scores and gas chromatography-mass spectrometry/gas chromatography-olfactometry.

    Science.gov (United States)

    Mao, Shihong; Lu, Changqi; Li, Meifeng; Ye, Yulong; Wei, Xu; Tong, Huarong

    2018-04-13

    Gas chromatography-olfactometry (GC-O) is the most frequently used method to estimate the sensory contribution of single odorant, but disregards the interactions between volatiles. In order to select the key volatiles responsible for the aroma attributes of Congou black tea (Camellia sinensis), instrumental, sensory and multivariate statistical approaches were applied. By sensory analysis, nine panelists developed 8 descriptors, namely, floral, sweet, fruity, green, roasted, oil, spicy, and off-odor. Linalool, (E)-furan linalool oxide, (Z)-pyran linalool oxide, methyl salicylate, β-myrcene, phenylethyl alcohol which identified from the most representative samples by GC-O procedure, were the essential aroma-active compounds in the formation of basic Congou black tea aroma. In addition, 136 volatiles were identified by gas chromatography-mass spectrometry (GC-MS), among which 55 compounds were determined as the key factors for the six sensory attributes by partial least-square regression (PLSR) with variable importance of projection (VIP) scores. Our results demonstrated that HS-SPME/GC-MS/GC-O was a fast approach for isolation and quantification aroma-active compounds. PLSR method was also considered to be a useful tool in selecting important variables for sensory attributes. These two strategies allowed us to comprehensively evaluate the sensorial contribution of single volatile from different perspectives, can be applied to related products for comprehensive quality control. This article is protected by copyright. All rights reserved.

  6. Odour-active compounds of Citrus deliciosa Tenore var. Caí essential oils detected by gas chromatography-mass spectrometry and gas chromatography-olfactometry

    Directory of Open Access Journals (Sweden)

    Manuel A. Minteguiaga

    2017-11-01

    Full Text Available Context: Mandarins are a complex taxonomic group including different species, cultivars and hybrids growing around the world being fruits greatly appreciated by the consumers. Citrus deliciosa Tenore var. Caí originates from Rio Grande do Sul State (Brazil and the fruit is characterised by its pleasant properties, especially its aroma. Aims: To evaluate the C. deliciosa cold-pressed essential oils, classified as “green”, “yellow” and “red” according to fruit maturity, and the one produced by distillation by gas chromatography-mass spectrometry (GC-MS and gas chromatography-olfactometry (GC-O. Methods: The essential oils aromatic quality was evaluated by GC-O through a panel of trained judges. The identification of the volatile compounds was performed by GC-MS and their quantification by GC-FID. Results: The chemical composition of the three types of cold-pressed essential oils was very similar. However, the distilled oil presented a higher concentration of oxygenated monoterpenes (mainly α-terpineol, 4-terpineol and sabinene hydrates. Herbaceous and floral aromatic notes were able to describe the “green” oil, while for the distilled oil wood and unpleasant notes were perceived. Conclusions: The cold-pressed oils did not show nor chemical, or aromatic differences, by the fruit maturity. The distilled oil was characterized by aromatic nuances making the oil less appreciated (inferior quality than the cold-pressed oil. Probably as consequence of artifacts formation during the distillation process.

  7. Comparison of aroma volatiles in commercial Merlot and Cabernet Sauvignon wines using gas chromatography-olfactometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gürbüz, Ozan; Rouseff, June M; Rouseff, Russell L

    2006-05-31

    Seventy-four aroma active compounds were observed in Merlot and Cabernet Sauvignon wines produced in California and Australia. Volatiles were sampled using solid phase microextraction and analyzed using time-intensity gas chromatography-olfactometry and gas chromatography-mass spectrometry (GC-MS). The most intense odorants were 3-methyl-1-butanol, 3-hydroxy-2-butanone, octanal, ethyl hexanoate, ethyl 2-methylbutanoate, beta-damascenone, 2-methoxyphenol, 4-ethenyl-2-methoxy-phenol, ethyl 3-methylbutanoate, acetic acid, and 2-phenylethanol. Aroma compounds were classified according to their aroma descriptor similarity and summed into nine distinct categories consisting of fruity, sulfury, caramel/cooked, spicy/peppery, floral, earthy, pungent/chemical, woody, and green/vegetative/fatty. Both Merlot and Cabernet Sauvignon wines were characterized by high fruity, caramel, green, and earthy aroma totals. Although there were distinct quantitative differences between Merlot and Cabernet wines, the relative aroma category profiles of the four wines were similar. Of the 66 volatiles identified by GC-MS, 28 were esters and 19 were minor alcohols. Between 81 and 88% of the total MS total ion chromatogram peak areas from each wine type were produced from only eight compounds: ethanol, ethyl octanoate, ethyl decanoate, ethyl acetate, 3-methyl-1-butanol, ethyl hexanoate, diethyl succinate, and 2-phenylethanol. Merlot wines from both Australia and California contained 4-5 times more ethyl octanoate than Cabernet Sauvignon wines from the same sources.

  8. Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.

    Science.gov (United States)

    Varlet, Vincent; Giuliani, Nicole; Palmiere, Cristian; Maujean, Géraldine; Augsburger, Marc

    2015-01-01

    The aim of our study was to present a new headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable to the routine determination of hydrogen sulfide (H(2)S) concentrations in biological and gaseous samples. The primary analytical drawback of the GC/MS methods for H(2)S measurement discussed in the literature was the absence of a specific H(2)S internal standard required to perform quantification. Although a deuterated hydrogen sulfide (D(2)S) standard is currently available, this standard is not often used because this standard is expensive and is only available in the gas phase. As an alternative approach, D(2)S can be generated in situ by reacting deuterated chloride with sodium sulfide; however, this technique can lead to low recovery yield and potential isotopic fractionation. Therefore, N(2)O was chosen for use as an internal standard. This method allows precise measurements of H(2)S concentrations in biological and gaseous samples. Therefore, a full validation using accuracy profile based on the β-expectation tolerance interval is presented. Finally, this method was applied to quantify H(2)S in an actual case of H(2)S fatal intoxication. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Impact of gas chromatography and mass spectrometry combined with gas chromatography and olfactometry for the sex differentiation of Baccharis articulata by the analysis of volatile compounds.

    Science.gov (United States)

    Minteguiaga, Manuel; Umpiérrez, Noelia; Fariña, Laura; Falcão, Manuel A; Xavier, Vanessa B; Cassel, Eduardo; Dellacassa, Eduardo

    2015-09-01

    The Baccharis genus has more than 400 species of aromatic plants. However, only approximately 50 species have been studied in oil composition to date. From these studies, very few take into consideration differences between male and female plants, which is a significant and distinctive factor in Baccharis in the Asteraceae family. Baccharis articulata is a common shrub that grows wild in south Brazil, northern and central Argentina, Bolivia, Paraguay and Uruguay. It is considered to be a medicinal plant and is employed in traditional medicine. We report B. articulata male and female volatile composition obtained by simultaneous distillation-extraction technique and analyzed by gas chromatography with mass spectrometry. Also, an assessment of aromatic differences between volatile extracts was evaluated by gas chromatography with olfactometry. The results show a very similar chemical composition between male and female extracts, with a high proportion of terpene compounds of which β-pinene, limonene and germacrene D are the main components. Despite the chemical similarity, great differences in aromatic profile were found: male plant samples exhibited the strongest odorants in number and intensity of aromatic attributes. These differences explain field observations which indicate differences between male and female flower aroma, and might be of ecological significance in the attraction of pollinating insects. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Gas-Phase Fragmentation Behavior of Oxidized Prenyl Peptides by CID and ETD Tandem Mass Spectrometry

    Science.gov (United States)

    Bhawal, Ruchika P.; Shahinuzzaman, A. D. A.; Chowdhury, Saiful M.

    2017-04-01

    Farnesylation and geranylgeranylation are the two types of prenyl modification of proteins. Prenylated peptides are highly hydrophobic and their abundances in biological samples are low. In this report, we studied the oxidized prenylated peptides by electrospray ionization mass spectrometry and identified them by collision-induced dissociation (CID) and electron-transfer dissociation (ETD) tandem mass spectrometry. Modified prenyl peptides were generated utilizing strong and low strength oxidizing agents to selectively oxidize and epoxidize cysteine sulfur and prenyl side chain. We selected three peptides with prenyl motifs and synthesized their prenylated versions. The detailed characteristic fragmentations of oxidized and epoxidized farnesylated and geranylgeranylated peptides were studied side by side with two popular fragmentation techniques. CID and ETD mass spectrometry clearly distinguished the modified version of these peptides. ETD mass spectrometry provided sequence information of the highly labile modified prenyl peptides and showed different characteristic fragmentations compared with CID. A detailed fragmentation of modified geranylgeranylated peptides was compared by CID and ETD mass spectrometry for the first time.

  11. Analysis of Fission Gas Release Kinetics by On-Line Mass Spectrometry

    Science.gov (United States)

    Zerega, Yves; Reynard-Carette, Christelle; Parrat, Daniel; Carette, Michel; Brkic, Boris; Lyoussi, Abdallah; Bignan, Gill; Janulyte, Aurika; Andre, Jacques; Pontillon, Yves; Ducros, Gerard; Taylor, Steve

    2012-08-01

    The release of fission gases (Xe and Kr) and helium out of nuclear fuel materials in normal operation of a nuclear power reactor can constitute a serious limitation of the fuel lifetime. Moreover, radioactive isotopes of Xe and Kr contribute significantly to the global radiological source term released in the primary coolant circuit in case of accidental situations accompanied by loss of fuel rod integrity. As a consequence, fission gas release investigation is of prime importance for the nuclear fuel cycle economy, and is the driving force for numerous R&D programs. In this domain, for understanding current fuel behavior issues, preparing the development of new fuels (e.g., for Gen IV power systems) and for improving modeling prediction capability, there is a marked need for innovations in the instrumentation field, mainly for: Quantification of very low fission gas concentrations, released from fuel sample and routed in sweeping lines,

  12. Selected ion flow tube mass spectrometry (sift-MS) for on-line trace gas analysis

    Czech Academy of Sciences Publication Activity Database

    Smith, D.; Španěl, Patrik

    2005-01-01

    Roč. 24, č. 5 (2005), s. 661-700 ISSN 0277-7037 R&D Projects: GA ČR(CZ) GA202/03/0827; GA ČR(CZ) GA203/02/0737 Institutional research plan: CEZ:AV0Z40400503 Keywords : SIFT-MS * chemical ionization * trace gas analysis * breath analysis * urine headspace analysis Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 13.273, year: 2005

  13. Analysis of Bacterial Vaginosis-Related Amines in Vaginal Fluid by Gas Chromatography and Mass Spectrometry

    OpenAIRE

    Wolrath, Helen; Forsum, Urban; Larsson, P. G.; Borén, Hans

    2001-01-01

    The presence of various amines in vaginal fluid from women with malodorous vaginal discharge has been reported before. The investigations have used several techniques to identify the amines. However, an optimized quantification, together with a sensitive analysis method in connection with a diagnostic procedure for vaginal discharge, including the syndrome of bacterial vaginosis, as defined by the accepted “gold standard,” has not been done before. We now report a sensitive gas chromatographi...

  14. Phytochemical analyses of Ziziphus jujuba Mill. var. spinosa seed by ultrahigh performance liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Bao; Yang, Hongshun; Chen, Feng; Hua, Yanglin; Jiang, Yueming

    2013-11-21

    Ziziphus jujuba Mill. var. spinosa (Z. jujuba) seeds have attracted much attention within the field of medicine due to their significant effects against disturbances of the central nervous system. Secondary metabolites composition is key to the influence of the pharmaceutical and commercial qualities of this plant. In this work, the phytochemical profile of Z. jujuba seeds was analysed by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS). The UPLC-MS/MS information identified the main secondary metabolites in Z. jujuba seeds, including flavonoid C-glycosides, triterpene acids and unsaturated fatty acids. The leading chemical identified by UPLC-MS/MS was betulinic acid, and oleic acid was the leading volatile from the GC-MS results. All the samples tested showed similar phytochemical profiles, but levels of the chemical compounds varied. Principal component analysis revealed the principal secondary metabolites that could define the differences in quality. It was confirmed that the combination of UPLC-MS/MS and GC-MS was an effective technique to demonstrate the pharmaceutical quality of Z. jujuba seeds.

  15. Metabolic profiling of yeast culture using gas chromatography coupled with orthogonal acceleration accurate mass time-of-flight mass spectrometry: application to biomarker discovery.

    Science.gov (United States)

    Kondo, Elsuida; Marriott, Philip J; Parker, Rhiannon M; Kouremenos, Konstantinos A; Morrison, Paul; Adams, Mike

    2014-01-07

    Yeast and yeast cultures are frequently used as additives in diets of dairy cows. Beneficial effects from the inclusion of yeast culture in diets for dairy mammals have been reported, and the aim of this study was to develop a comprehensive analytical method for the accurate mass identification of the 'global' metabolites in order to differentiate a variety of yeasts at varying growth stages (Diamond V XP, Yea-Sacc and Levucell). Microwave-assisted derivatization for metabolic profiling is demonstrated through the analysis of differing yeast samples developed for cattle feed, which include a wide range of metabolites of interest covering a large range of compound classes. Accurate identification of the components was undertaken using GC-oa-ToFMS (gas chromatography-orthogonal acceleration-time-of-flight mass spectrometry), followed by principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) for data reduction and biomarker discovery. Semi-quantification (fold changes in relative peak areas) was reported for metabolites identified as possible discriminative biomarkers (p-value 2), including D-ribose (four fold decrease), myo-inositol (five fold increase), L-phenylalanine (three fold increase), glucopyranoside (two fold increase), fructose (three fold increase) and threitol (three fold increase) respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Owens, J; Hok, S; Alcaraz, A; Koester, C

    2008-11-13

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  17. Gas chromatography-mass spectrometry/mass spectrometry analysis to determine natural and post-administration levels of oestrogens in bovine serum and urine

    Energy Technology Data Exchange (ETDEWEB)

    Biddle, S. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom)]. E-mail: sbiddle@hfl.co.uk; Teale, P. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom); Robinson, A. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom); Bowman, J. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom); Houghton, E. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom)

    2007-03-14

    A novel analytical approach has been developed and shown to be capable of detecting the isomers of oestradiol in the low ppt (pg mL{sup -1}) range in bovine serum and urine. Following extractive derivatisation the analytes were detected as their 3-pentafluorobenzoyl 17-trimethylsilyl ether derivatives by gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS), using electron capture negative ion chemical ionisation. The isomers of oestradiol were quantified in both blank and post-administration urine and serum samples, with a view to setting action/threshold levels for these compounds, to allow discrimination between normal samples and samples from animals treated with growth promoting ear implants. A non-parametric statistical assessment of the data resulted in proposed action levels (with a false positive probability of 1 in 1000) of 1.6 and 2.7 ng mL{sup -1} for 17{alpha}-oestradiol, in male and female urine, respectively, and 40 and 44 pg mL{sup -1} for 17{beta}-oestradiol, in male and female urine, respectively. An action level of 20 pg mL{sup -1} was proposed for 17{alpha}- and 17{beta}-oestradiol in male serum. In female serum the proposed action levels were 40 and 20 pg mL{sup -1} for 17{alpha}- and 17{beta}-oestradiol, respectively.

  18. Gas chromatography-mass spectrometry/mass spectrometry analysis to determine natural and post-administration levels of oestrogens in bovine serum and urine

    International Nuclear Information System (INIS)

    Biddle, S.; Teale, P.; Robinson, A.; Bowman, J.; Houghton, E.

    2007-01-01

    A novel analytical approach has been developed and shown to be capable of detecting the isomers of oestradiol in the low ppt (pg mL -1 ) range in bovine serum and urine. Following extractive derivatisation the analytes were detected as their 3-pentafluorobenzoyl 17-trimethylsilyl ether derivatives by gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS), using electron capture negative ion chemical ionisation. The isomers of oestradiol were quantified in both blank and post-administration urine and serum samples, with a view to setting action/threshold levels for these compounds, to allow discrimination between normal samples and samples from animals treated with growth promoting ear implants. A non-parametric statistical assessment of the data resulted in proposed action levels (with a false positive probability of 1 in 1000) of 1.6 and 2.7 ng mL -1 for 17α-oestradiol, in male and female urine, respectively, and 40 and 44 pg mL -1 for 17β-oestradiol, in male and female urine, respectively. An action level of 20 pg mL -1 was proposed for 17α- and 17β-oestradiol in male serum. In female serum the proposed action levels were 40 and 20 pg mL -1 for 17α- and 17β-oestradiol, respectively

  19. Urinary metabonomics study in a rat model in response to protein-energy malnutrition by using gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Wu, Zeming; Li, Min; Zhao, Chunxia; Zhou, Jia; Chang, Yuwei; Li, Xiang; Gao, Peng; Lu, Xin; Li, Yousheng; Xu, Guowang

    2010-11-01

    Systematic studies were performed on the biological perturbations in metabolic phenotype responding to protein-energy malnutrition through global metabolic profiling analysis, in combination with pattern recognition. The malnutrition rat model was established through five weeks of strict diet restriction, and the metabonome data obtained from gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) were integrated to approximate the comprehensive metabolic signature. Principal component analysis and orthogonal projection to latent structure analysis were used for the classification of metabolic phenotypes and discovery of differentiating metabolites. The perturbations in the urine profiles of malnourished rats were marked by higher levels of creatine, threitol, pyroglutamic acid, gluconic acid and kynurenic acid, as well as decreased levels of succinic acid, cis-aconitic acid, citric acid, isocitric acid, threonic acid, trimethylglycine, N-methylnicotinic acid and uric acid. The alterations in these metabolites were associated with perturbations in energy metabolism, carbohydrate, amino acid, and fatty acid metabolism, purine metabolism, cofactor and vitamin metabolism, in response to protein and energy malnutrition. Our findings show the integration of GC-MS and LC-MS techniques for untargeted metabolic profiling analysis was promising for nutriology.

  20. Quantitative Analysis of Tetramethylenedisulfotetramine ('Tetramine') Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    International Nuclear Information System (INIS)

    Owens, J.; Hok, S.; Alcaraz, A.; Koester, C.

    2008-01-01

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 50 = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 (micro)g/mL by LC/MS/MS versus 0.15 (micro)g/mL for GC/MS. Fortifications of the beverages at 2.5 (micro)g/mL and 0.25 (micro)g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  1. The screening of inborn errors of metabolism in sick Chinese infants by tandem mass spectrometry and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Sun, Weihua; Wang, Yi; Yang, Yi; Wang, Jianshe; Cao, Yun; Luo, Feihong; Lu, Wei; Peng, Yongmei; Yao, Haili; Qiu, Penglin

    2011-06-11

    Analyses of amino acid/acylcarnitines in dried blood spots (DBS) and organic acids in urine are the primary tests for inborn errors of metabolism (IEMs). Automated tandem mass spectrometry (MS/MS) and gas chromatography/mass spectrometry (GC/MS) can rapidly and simultaneously detect numerous metabolic compounds with high precision and sensitivity. Three thousand four hundred and twenty-nine DBSs and 2781 urine samples were collected from our hospital patients with suspected IEMs, and analyzed for amino acid/acylcarnitines and organic acids by MS/MS and GC/MS, respectively. The results were used in a coincidental survey to determine the efficacy of these methods for the diagnosis of IEMs. Nineteen different types of IEMs were detected in 121 affected cases (1.95% of 6210 samples). There were 66.12% amino acid disorders, 29.75% organic acid disorders and 4.13% with fatty acid oxidation disorders. the sick infants tested in this study had high prevalence rates of neonatal intrahepatic cholestasis, methylmalonic acidemia, hyperphenylalaninemia, tyrosinemia type I, and urea cycle disorders. The combined use of MS/MS and GC/MS is an appropriate tool for screening of IEMs in sick infants. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Sensitive determination of fluoride in biological samples by gas chromatography-mass spectrometry after derivatization with 2-(bromomethyl)naphthalene.

    Science.gov (United States)

    Kwon, Sun-Myung; Shin, Ho-Sang

    2014-12-10

    A gas chromatography-mass spectrometric method was developed in this study in order to determine fluoride in plasma and urine after derivatization with 2-(bromomethyl)naphthalene. 2-Fluoronaphthalene was chosen as the internal standard. The derivatization of fluoride was performed in the biological sample and the best reaction conditions (10.0 mg mL(-1) of 2-(bromomethyl)naphthalene, 1.0 mg mL(-1) of 15-crown-5-ether as a phase transfer catalyst, pH of 7.0, reaction temperature of 70°C, and heating time of 70 min) were established. The organic derivative was extracted with dichloromethane and then measured by a gas chromatography-mass spectrometry. Under the established condition, the detection limits were 11 μg L(-1) and 7 μg L(-1) by using 0.2 mL of plasma or urine, respectively. The accuracy was in a range of 100.8-107.6%, and the precision of the assay was less than 4.3% in plasma or urine. Fluoride was detected in a concentration range of 0.12-0.53 mg L(-1) in six urine samples after intake of natural mineral water containing 0.7 mg L(-1) of fluoride. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Gas chromatography interfaced with atmospheric pressure ionization-quadrupole time-of-flight-mass spectrometry by low-temperature plasma ionization

    DEFF Research Database (Denmark)

    Norgaard, Asger W.; Kofoed-Sorensen, Vivi; Svensmark, Bo

    2013-01-01

    A low temperature plasma (LTP) ionization interface between a gas chromatograph (GC) and an atmospheric pressure inlet mass spectrometer, was constructed. This enabled time-of-flight mass spectrometric detection of GC-eluting compounds. The performance of the setup was evaluated by injection...

  4. Mass transfer with complex chemical reactions in gas-liquid systems: two-step reversible reactions with unit stoichiometric and kinetic orders

    NARCIS (Netherlands)

    Vas bhat, R.D.; Kuipers, J.A.M.; Versteeg, Geert

    2000-01-01

    An absorption model to study gas¿liquid mass transfer accompanied by reversible two-step reactions in the liquid phase has been presented. This model has been used to determine mass transfer rates, enhancement factors and concentration profiles over a wide range of process conditions. Although

  5. Ion Mobility Spectrometry-Mass Spectrometry Coupled with Gas-Phase Hydrogen/Deuterium Exchange for Metabolomics Analyses

    Science.gov (United States)

    Maleki, Hossein; Karanji, Ahmad K.; Majuta, Sandra; Maurer, Megan M.; Valentine, Stephen J.

    2018-02-01

    Ion mobility spectrometry-mass spectrometry (IMS-MS) in combination with gas-phase hydrogen/deuterium exchange (HDX) and collision-induced dissociation (CID) is evaluated as an analytical method for small-molecule standard and mixture characterization. Experiments show that compound ions exhibit unique HDX reactivities that can be used to distinguish different species. Additionally, it is shown that gas-phase HDX kinetics can be exploited to provide even further distinguishing capabilities by using different partial pressures of reagent gas. The relative HDX reactivity of a wide variety of molecules is discussed in light of the various molecular structures. Additionally, hydrogen accessibility scoring (HAS) and HDX kinetics modeling of candidate ( in silico) ion structures is utilized to estimate the relative ion conformer populations giving rise to specific HDX behavior. These data interpretation methods are discussed with a focus on developing predictive tools for HDX behavior. Finally, an example is provided in which ion mobility information is supplemented with HDX reactivity data to aid identification efforts of compounds in a metabolite extract.

  6. An improved, automated whole air sampler and gas chromatography mass spectrometry analysis system for volatile organic compounds in the atmosphere

    Science.gov (United States)

    Lerner, Brian M.; Gilman, Jessica B.; Aikin, Kenneth C.; Atlas, Elliot L.; Goldan, Paul D.; Graus, Martin; Hendershot, Roger; Isaacman-VanWertz, Gabriel A.; Koss, Abigail; Kuster, William C.; Lueb, Richard A.; McLaughlin, Richard J.; Peischl, Jeff; Sueper, Donna; Ryerson, Thomas B.; Tokarek, Travis W.; Warneke, Carsten; Yuan, Bin; de Gouw, Joost A.

    2017-01-01

    Volatile organic compounds were quantified during two aircraft-based field campaigns using highly automated, whole air samplers with expedited post-flight analysis via a new custom-built, field-deployable gas chromatography-mass spectrometry instrument. During flight, air samples were pressurized with a stainless steel bellows compressor into electropolished stainless steel canisters. The air samples were analyzed using a novel gas chromatograph system designed specifically for field use which eliminates the need for liquid nitrogen. Instead, a Stirling cooler is used for cryogenic sample pre-concentration at temperatures as low as -165 °C. The analysis system was fully automated on a 20 min cycle to allow for unattended processing of an entire flight of 72 sample canisters within 30 h, thereby reducing typical sample residence times in the canisters to less than 3 days. The new analytical system is capable of quantifying a wide suite of C2 to C10 organic compounds at part-per-trillion sensitivity. This paper describes the sampling and analysis systems, along with the data analysis procedures which include a new peak-fitting software package for rapid chromatographic data reduction. Instrument sensitivities, uncertainties and system artifacts are presented for 35 trace gas species in canister samples. Comparisons of reported mixing ratios from each field campaign with measurements from other instruments are also presented.

  7. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates.

    Science.gov (United States)

    Moerdijk-Poortvliet, Tanja C W; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J; Boschker, Henricus T S

    2015-07-15

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although LC/IRMS is expected to be more accurate and precise, no direct comparison has been reported. GC/IRMS with the aldonitrile penta-acetate (ANPA) derivatisation method was compared with LC/IRMS without derivatisation. A large number of glucose standards and a variety of natural samples were analysed for five neutral carbohydrates at natural abundance as well as at (13)C-enriched levels. Gas chromatography/chemical ionisation mass spectrometry (GC/CIMS) was applied to check for incomplete derivatisation of the carbohydrate, which would impair the accuracy of the GC/IRMS method. The LC/IRMS technique provided excellent precision (±0.08‰ and ±3.1‰ at natural abundance and enrichment levels, respectively) for the glucose standards and this technique proved to be superior to GC/IRMS (±0.62‰ and ±19.8‰ at natural abundance and enrichment levels, respectively). For GC/IRMS measurements the derivatisation correction and the conversion of carbohydrates into CO2 had a considerable effect on the measured δ(13)C values. However, we did not find any significant differences in the accuracy of the two techniques over the full range of natural δ(13)C abundances and (13)C-labelled glucose. The difference in the performance of GC/IRMS and LC/IRMS diminished when the δ(13)C values were measured in natural samples, because the chromatographic performance and background correction became critical factors, particularly for LC/IRMS. The derivatisation of carbohydrates for the GC/IRMS method was complete. Although both LC/IRMS and GC/IRMS are reliable techniques for compound-specific stable carbon isotope analysis of carbohydrates (provided that derivatisation is complete and the

  8. Galaxy And Mass Assembly (GAMA): Gas Fuelling of Spiral Galaxies in the Local Universe II. - Direct Measurement of the Dependencies on Redshift and Host Halo Mass of Stellar Mass Growth in Central Disk Galaxies

    Science.gov (United States)

    Grootes, M. W.; Dvornik, A.; Laureijs, R. J.; Tuffs, R. J.; Popescu, C. C.; Robotham, A. S. G.; Liske, J.; Brown, M. J. I.; Holwerda, B. W.; Wang, L.

    2018-03-01

    We present a detailed analysis of the specific star formation rate - stellar mass (sSFR - M*) of z ≤ 0.13 disk central galaxies using a morphologically selected mass-complete sample (M* ≥ 109.5M⊙). Considering samples of grouped and ungrouped galaxies, we find the sSFR - M* relations of disk-dominated central galaxies to have no detectable dependence on host dark-matter halo (DMH) mass, even where weak-lensing measurements indicate a difference in halo mass of a factor ≳ 5. We further detect a gradual evolution of the sSFR - M* relation of non-grouped (field) central disk galaxies with redshift, even over a Δz ≈ 0.04 (≈5 . 108yr) interval, while the scatter remains constant. This evolution is consistent with extrapolation of the "main-sequence-of-star-forming-galaxies" from previous literature that uses larger redshift baselines and coarser sampling. Taken together, our results present new constraints on the paradigm under which the SFR of galaxies is determined by a self-regulated balance between gas inflows and outflows, and consumption of gas by star-formation in disks, with the inflow being determined by the product of the cosmological accretion rate and a fuelling-efficiency - \\dot{M}_{b,halo}ζ. In particular, maintaining the paradigm requires \\dot{M}_{b,halo}ζ to be independent of the mass Mhalo of the host DMH. Furthermore, it requires the fuelling-efficiency ζ to have a strong redshift dependence (∝(1 + z)2.7 for M* = 1010.3M⊙ over z = 0 - 0.13), even though no morphological transformation to spheroids can be invoked to explain this in our disk-dominated sample. The physical mechanisms capable of giving rise to such dependencies of ζ on Mhalo and z for disks are unclear.

  9. Correlation of Mass Spectrometry Identified Bacterial Biomarkers From a Fielded Pyrolysis-Gas Chromatography-Ion Mobility Spectrometry Biodetector With the Microbiological Gram Stain Classification Scheme

    Science.gov (United States)

    2005-09-01

    REPORT TYPE 3. DATES COVERED (From - TO) XX-09-2005 Final Oct 2002 - Dec 2003 4. TITLE- AND SUBTITLE 5a. CONTRACT NUMBER Correlation of Mass ...M.M.; Wick, C.H. Novel Biomarkers for Gram-Type Differentiation of Bacteria by Pyrolysis-Gas Chromatography- Mass Spectometry . J. Anal. Appl...EDGEWOOD CHEMICAL BIOLOGICAL CENTER U.S. ARMY RESEARCH, DEVELOPMENT AND ENGINEERING COMMAND ECBC-TR-415 CORRELATION OF MASS SPECTROMETRY IDENTIFIED

  10. Ion mobility spectrometry-mass spectrometry (IMS-MS) for on- and offline analysis of atmospheric gas and aerosol species

    Science.gov (United States)

    Krechmer, Jordan E.; Groessl, Michael; Zhang, Xuan; Junninen, Heikki; Massoli, Paola; Lambe, Andrew T.; Kimmel, Joel R.; Cubison, Michael J.; Graf, Stephan; Lin, Ying-Hsuan; Budisulistiorini, Sri H.; Zhang, Haofei; Surratt, Jason D.; Knochenmuss, Richard; Jayne, John T.; Worsnop, Douglas R.; Jimenez, Jose-Luis; Canagaratna, Manjula R.

    2016-07-01

    Measurement techniques that provide molecular-level information are needed to elucidate the multiphase processes that produce secondary organic aerosol (SOA) species in the atmosphere. Here we demonstrate the application of ion mobility spectrometry-mass spectrometry (IMS-MS) to the simultaneous characterization of the elemental composition and molecular structures of organic species in the gas and particulate phases. Molecular ions of gas-phase organic species are measured online with IMS-MS after ionization with a custom-built nitrate chemical ionization (CI) source. This CI-IMS-MS technique is used to obtain time-resolved measurements (5 min) of highly oxidized organic molecules during the 2013 Southern Oxidant and Aerosol Study (SOAS) ambient field campaign in the forested SE US. The ambient IMS-MS signals are consistent with laboratory IMS-MS spectra obtained from single-component carboxylic acids and multicomponent mixtures of isoprene and monoterpene oxidation products. Mass-mobility correlations in the 2-D IMS-MS space provide a means of identifying ions with similar molecular structures within complex mass spectra and are used to separate and identify monoterpene oxidation products in the ambient data that are produced from different chemical pathways. Water-soluble organic carbon (WSOC) constituents of fine aerosol particles that are not resolvable with standard analytical separation methods, such as liquid chromatography (LC), are shown to be separable with IMS-MS coupled to an electrospray ionization (ESI) source. The capability to use ion mobility to differentiate between isomers is demonstrated for organosulfates derived from the reactive uptake of isomers of isoprene epoxydiols (IEPOX) onto wet acidic sulfate aerosol. Controlled fragmentation of precursor ions by collisionally induced dissociation (CID) in the transfer region between the IMS and the MS is used to validate MS peak assignments, elucidate structures of oligomers, and confirm the

  11. Improving quantitative gas chromatography-electron ionization mass spectrometry results using a modified ion source: demonstration for a pharmaceutical application.

    Science.gov (United States)

    D'Autry, Ward; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Van Schepdael, Ann

    2011-07-01

    Gas chromatography-mass spectrometry is a well established analytical technique. However, mass spectrometers with electron ionization sources may suffer from signal drifts, hereby negatively influencing quantitative performance. To demonstrate this phenomenon for a real application, a static headspace-gas chromatography method in combination with electron ionization-quadrupole mass spectrometry was optimized for the determination of residual dichloromethane in coronary stent coatings. Validating the method, the quantitative performance of an original stainless steel ion source was compared to that of a modified ion source. Ion source modification included the application of a gold coating on the repeller and exit plate. Several validation aspects such as limit of detection, limit of quantification, linearity and precision were evaluated using both ion sources. It was found that, as expected, the stainless steel ion source suffered from signal drift. As a consequence, non-linearity and high RSD values for repeated analyses were obtained. An additional experiment was performed to check whether an internal standard compound would lead to better results. It was found that the signal drift patterns of the analyte and internal standard were different, consequently leading to high RSD values for the response factor. With the modified ion source however, a more stable signal was observed resulting in acceptable linearity and precision. Moreover, it was also found that sensitivity improved compared to the stainless steel ion source. Finally, the optimized method with the modified ion source was applied to determine residual dichloromethane in the coating of coronary stents. The solvent was detected but found to be below the limit of quantification. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Detection of clenbuterol at trace levels in doping analysis using different gas chromatographic-mass spectrometric techniques.

    Science.gov (United States)

    Yang, Sheng; Liu, Xin; Xing, Yanyi; Zhang, Dapeng; Wang, Shan; Wang, Xiaobing; Xu, Youxuan; Wu, Moutian; He, Zhenwen; Zhao, Jian

    2013-01-01

    This study demonstrates the development of a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS-MS) assay to detect clenbuterol in human urine and the comparison of this method with GC-MS techniques and gas chromatography-high resolution mass spectrometry (GC-HRMS) techniques. Urine samples were hydrolyzed with β-glucuronidase, extracted with methyl tert-butyl ether and dried under nitrogen. The derivative reagent was N-methyl-N-(trimethylsilyl)-trifluoroacetamide with NH4I and was analyzed by GC-MS, GC-MS-MS and GC-HRMS. A validation study was conducted by GC-MS-MS. The analyses of clenbuterol using different mass spectrometric techniques were compared. The limit of detection (LOD) for clenbuterol in human urine was 2 ng/mL by GC-MS (selected ion monitoring mode: SIM mode), 0.06 ng/mL by GC-HRMS and 0.03 ng/mL by GC-MS-MS, respectively, while the LOD by GC-HRMS was 0.06. With GC-MS-MS, the intra-assay and inter-assay precisions were less than 15%, the recoveries were 86 to 112% and the linear range was 0.06 to 8.0 ng/mL. The GC-MS under SIM mode can be used as a screening tool to detect clenbuterol at trace levels in human urine. The GC-MS-MS and GC-HRMS methods can confirm clenbuterol when its concentration is below 2 ng/mL. The results demonstrate that the GC-MS-MS method is quite sensitive, specific and reliable for the detection of clenbuterol in doping analysis.

  13. Can Electrospray Mass Spectrometry Probe Speciation? Hydrolysis of Uranyl Nitrate Studied by Gas-Phase Methods

    Czech Academy of Sciences Publication Activity Database

    Tsierkezos, Nikos; Roithová, Jana; Schröder, Detlef; Ončák, Milan; Slavíček, Petr

    2009-01-01

    Roč. 48, č. 13 (2009), s. 6287-6296 ISSN 0020-1669 R&D Projects: GA ČR GA203/08/1487 Grant - others:GA ČR(CZ) GP203/07/P449 Institutional research plan: CEZ:AV0Z40550506; CEZ:AV0Z40400503 Keywords : collision-induced dissociation * electrodpray ionization * ion association * mass spectrometry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.657, year: 2009

  14. Simulating gas-liquid mass transfer in a spin filter bioreactor

    OpenAIRE

    Niño López, Lilibeth Caridad; Gelves Zambrano, Germán Ricardo

    2015-01-01

    Computational fluid dynamics (CFD) and population balance model (PBM) model have been used to simulate hydrodynamics and mass transfer in a 0.014 m3 Spin Filter Bioreactor. The operating conditions chosen were defined by typical settings used for culturing plant cells. Turbulence, rotating flow, bubbles breakage and coalescence were simulated by using the k-e, MRF (Multiple Reference Frame) and PBM approaches, respectively. The numerical results from different operational conditions are compa...

  15. Theoretical approach for enhanced mass transfer effects in-duct flue gas desulfurization processes

    Energy Technology Data Exchange (ETDEWEB)

    1990-10-24

    During the reporting of July 1 to September 30, 1990, bench- and pilot-scale experiments were conducted to measure mass transfer and kinetic rates under simulated duct-injection conditions. This report describes the results of stirred-tank modelling experiments; experiments with moist solids in a short-time differential reactor in order to study and compare SO{sub 2} conversions; an investigation of the agglomeration of damp Ca(OH)-based solids; and evaluation of speciality sorbents.

  16. Gas hold-up and oxygen mass transfer in three pneumatic bioreactors operating with sugarcane bagasse suspensions.

    Science.gov (United States)

    Esperança, M N; Cunha, F M; Cerri, M O; Zangirolami, T C; Farinas, C S; Badino, A C

    2014-05-01

    Sugarcane bagasse is a low-cost and abundant by-product generated by the bioethanol industry, and is a potential substrate for cellulolytic enzyme production. The aim of this work was to evaluate the effects of air flow rate (QAIR), solids loading (%S), sugarcane bagasse type, and particle size on the gas hold-up (εG) and volumetric oxygen transfer coefficient (kLa) in three different pneumatic bioreactors, using response surface methodology. Concentric tube airlift (CTA), split-cylinder airlift (SCA), and bubble column (BC) bioreactor types were tested. QAIR and %S affected oxygen mass transfer positively and negatively, respectively, while sugarcane bagasse type and particle size (within the range studied) did not influence kLa. Using large particles of untreated sugarcane bagasse, the loop-type bioreactors (CTA and SCA) exhibited higher mass transfer, compared to the BC reactor. At higher %S, SCA presented a higher kLa value (0.0448 s−1) than CTA, and the best operational conditions in terms of oxygen mass transfer were achieved for %S 27.0 L min−1. These results demonstrated that pneumatic bioreactors can provide elevated oxygen transfer in the presence of vegetal biomass, making them an excellent option for use in three-phase systems for cellulolytic enzyme production by filamentous fungi.

  17. Application of a Gas Chromatography/Mass Spectrometric Method for the Determination of Butyltin Compounds in Sediment

    International Nuclear Information System (INIS)

    Chung, Min Young; Kim, Byung Joo; Yim, Yong Heon; So, Hun Young; Won, Yong Il; Jung, Pyong Gil; Kim, Yong Seong

    2004-01-01

    A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry

  18. Standard test method for isotopic analysis of uranium hexafluoride by double standard single-collector gas mass spectrometer method

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This is a quantitative test method applicable to determining the mass percent of uranium isotopes in uranium hexafluoride (UF6) samples with 235U concentrations between 0.1 and 5.0 mass %. 1.2 This test method may be applicable for the entire range of 235U concentrations for which adequate standards are available. 1.3 This test method is for analysis by a gas magnetic sector mass spectrometer with a single collector using interpolation to determine the isotopic concentration of an unknown sample between two characterized UF6 standards. 1.4 This test method is to replace the existing test method currently published in Test Methods C761 and is used in the nuclear fuel cycle for UF6 isotopic analyses. 1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appro...

  19. Improved Resolution of Hydrocarbon Structures and Constitutional Isomers in Complex Mixtures Using Gas Chromatography-Vacuum Ultraviolet-Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Isaacman, Gabriel [Univ. of California, Berkeley, CA (United States); Wilson, Kevin R. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Chan, Arthur W. H. [Univ. of California, Berkeley, CA (United States); Worton, David R. [Univ. of California, Berkeley, CA (United States). Aerosol Dynamics Inc., Berkeley, CA (United States); Kimmel, Joel R. [Aerodyne Research, Inc., Billerica, MA (United States); Univ. of Colorado, Boulder, CO (United States). Tofwerk AG, Thun (Switzerland); Nah, Theodora [Univ. of California, Berkeley, CA (United States); Hohaus, Thorsten [Aerodyne Research, Inc., Billerica, MA (United States); Gonin, Marc [Tofwerk AG, Thun (Switzerland); Kroll, Jesse H. [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States); Worsnop, Douglas R. [Aerodyne Research, Inc., Billerica, MA (United States); Goldstein, Allen H. [Univ. of California, Berkeley, CA (United States); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2012-01-30

    Understanding the composition of complex hydrocarbon mixtures is important for environmental studies in a variety of fields, but many prevalent compounds cannot be confidently identified using traditional gas chromatography/mass spectrometry (GC/MS) techniques. In this study, we use vacuum-ultraviolet (VUV) ionization to elucidate the structures of a traditionally “unresolved complex mixture” by separating components by GC retention time, tR, and mass-to-charge ratio, m/z, which are used to determine carbon number, NC, and the number of rings and double bonds, NDBE. Constitutional isomers are resolved on the basis of tR, enabling the most complete quantitative analysis to date of structural isomers in an environmentally relevant hydrocarbon mixture. Unknown compounds are classified in this work by carbon number, degree of saturation, presence of rings, and degree of branching, providing structural constraints. The capabilities of this analysis are explored using diesel fuel, in which constitutional isomer distribution patterns are shown to be reproducible between carbon numbers and follow predictable rules. Nearly half of the aliphatic hydrocarbon mass is shown to be branched, suggesting branching is more important in diesel fuel than previously shown. Lastly, the classification of unknown hydrocarbons and the resolution of constitutional isomers significantly improves resolution capabilities for any complex hydrocarbon mixture.

  20. Search for sub-eV mass solar axions by the CERN Axion Solar Telescope with 3He buffer gas.

    Science.gov (United States)

    Arik, M; Aune, S; Barth, K; Belov, A; Borghi, S; Bräuninger, H; Cantatore, G; Carmona, J M; Cetin, S A; Collar, J I; Dafni, T; Davenport, M; Eleftheriadis, C; Elias, N; Ezer, C; Fanourakis, G; Ferrer-Ribas, E; Friedrich, P; Galán, J; García, J A; Gardikiotis, A; Gazis, E N; Geralis, T; Giomataris, I; Gninenko, S; Gómez, H; Gruber, E; Guthörl, T; Hartmann, R; Haug, F; Hasinoff, M D; Hoffmann, D H H; Iguaz, F J; Irastorza, I G; Jacoby, J; Jakovčić, K; Karuza, M; Königsmann, K; Kotthaus, R; Krčmar, M; Kuster, M; Lakić, B; Laurent, J M; Liolios, A; Ljubičić, A; Lozza, V; Lutz, G; Luzón, G; Morales, J; Niinikoski, T; Nordt, A; Papaevangelou, T; Pivovaroff, M J; Raffelt, G; Rashba, T; Riege, H; Rodríguez, A; Rosu, M; Ruz, J; Savvidis, I; Silva, P S; Solanki, S K; Stewart, L; Tomás, A; Tsagri, M; van Bibber, K; Vafeiadis, T; Villar, J A; Vogel, J K; Yildiz, S C; Zioutas, K

    2011-12-23

    The CERN Axion Solar Telescope (CAST) has extended its search for solar axions by using (3)He as a buffer gas. At T=1.8 K this allows for larger pressure settings and hence sensitivity to higher axion masses than our previous measurements with (4)He. With about 1 h of data taking at each of 252 different pressure settings we have scanned the axion mass range 0.39 eV≲m(a)≲0.64 eV. From the absence of excess x rays when the magnet was pointing to the Sun we set a typical upper limit on the axion-photon coupling of g(aγ)≲2.3×10(-10) GeV(-1) at 95% C.L., the exact value depending on the pressure setting. Kim-Shifman-Vainshtein-Zakharov axions are excluded at the upper end of our mass range, the first time ever for any solar axion search. In the future we will extend our search to m(a)≲1.15 eV, comfortably overlapping with cosmological hot dark matter bounds.

  1. Determination of 4-Methylimidazole in Ammonia Caramel Using Gas Chromatography–Tandem Mass Spectrometry (GC-MS/MS

    Directory of Open Access Journals (Sweden)

    Martyna N. Wieczorek

    2018-01-01

    Full Text Available One of Maillard reaction products formed in the production of ammonia caramel is 4(5-methylimidazole (4-MeI classified as carcinogen. A method of 4-MeI determination based on ion-pair extraction and derivatisation with isobutyl chloroformate with subsequent gas chromatography-tandem mass spectrometry analysis was proposed. Tandem mass spectrometry was applied to reduce the influence of matrix and increase the selectivity and sensitivity of the method. Triple quadrupole GC-MS system was used for this study. The collision energies were optimized for MRM mode. The detection (LOD and quantification limits (LOQ of the elaborated method were 17 and 37.8 μg kg−1, respectively, repeatability was <15% RSD for analyzed caramel samples, and the recovery for 4-MeI was 101%. Comparison of MS/MS with SIM detection on the same instrument proved almost 30 times lower LODs achieved by tandem mass spectrometry compared to SIM. Described method can be routinely used for monitoring 4-MeI as a quality and safety marker in the production of ammonia caramel.

  2. Integration and Ruggedization of a Commercially Available Gas Chromatograph and Mass Spectrometer (GCMS) for the Resource Prospector Mission (RPM)

    Science.gov (United States)

    Loftin, Kathleen; Griffin, Timothy; Captain, Janine

    2013-01-01

    The Resource Prospector is a mission to prospect for lunar volatiles (primarily water) at one of the two lunar poles, as well as demonstrate In-Situ Resource Utilization (ISRU) on the Moon. The Resource Prospector consists of a lander, a rover, and a rover-borne scientific payload. The Regolith and Environment Science and Oxygen & Lunar Volatile Extraction (RESOLVE) payload, will be able to (1) locate near subsurface volatiles, (2) excavate and analyze samples of the volatile-bearing regolith, and (3) demonstrate the form, extractability and usefulness of the materials. The gas chromatograph mass spectrometer (GCMS) is the primary instrument in the RESOLVE instrumentation suite responsible for identification and quantification of the volatiles evolved from the lunar regolith. Specifically, this instrument must have: a low mass, a low power consumption, be able to perform fast analyses of samples ranging from less than one to greater than ninety nine percent water by mass, be autonomously controlled by the payload's software and avionics platform, and be able to operate in the harsh lunar environment. The RPM's short mission duration is the primary driver of the requirement for a very fast analysis time currently base lined at less than 2 minutes per sample. This presentation will discuss the requirements levied upon the GCMS design, lessons learned from a preliminary field demonstration deployment, the current design, and the path forward.

  3. Comprehensive two-dimensional gas chromatography in combination with rapid scanning quadrupole mass spectrometry in perfume analysis.

    Science.gov (United States)

    Mondello, Luigi; Casillia, Alessandro; Tranchida, Peter Quinto; Dugo, Giovanni; Dugo, Paola

    2005-03-04

    Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI).

  4. Analysis and quantitation of volatile organic compounds emitted from plastics used in museum construction by evolved gas analysis-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Samide, Michael J; Smith, Gregory D

    2015-12-24

    Construction materials used in museums for the display, storage, and transportation of artwork must be assessed for their tendency to emit harmful pollution that could potentially damage cultural treasures. Traditionally, a subjective metals corrosion test known as the Oddy test has been widely utilized in museums for this purpose. To augment the Oddy test, an instrumental sampling approach based on evolved gas analysis (EGA) coupled to gas chromatography (GC) with mass spectral (MS) detection has been implemented for the first time to qualitatively identify off-gassed pollutants under specific conditions. This approach is compared to other instrumental methods reported in the literature. This novel application of the EGA sampling technique yields several benefits over traditional testing, including rapidity, high sensitivity, and broad detectability of volatile organic compounds (VOCs). Furthermore, unlike other reported instrumental approaches, the EGA method was used to determine quantitatively the amount of VOCs emitted by acetate resins and polyurethane foams under specific conditions using both an external calibration method as well as surrogate response factors. EGA was successfully employed to rapidly characterize emissions from 12 types of common plastics. This analysis is advocated as a rapid pre-screening method to rule out poorly performing materials prior to investing time and energy in Oddy testing. The approach is also useful for rapid, routine testing of construction materials previously vetted by traditional testing, but which may experience detrimental formulation changes over time. As an example, a case study on batch re-orders of rigid expanded poly(vinyl chloride) board stock is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Online Simultaneous Hydrogen/Deuterium Exchange of Multitarget Gas-Phase Molecules by Electrospray Ionization Mass Spectrometry Coupled with Gas Chromatography.

    Science.gov (United States)

    Jeong, Eun Sook; Cha, Eunju; Cha, Sangwon; Kim, Sunghwan; Oh, Han Bin; Kwon, Oh-Seung; Lee, Jaeick

    2017-11-21

    In this study, a hydrogen/deuterium (H/D) exchange method using gas chromatography-electrospray ionization/mass spectrometry (GC-ESI/MS) was first investigated as a novel tool for online H/D exchange of multitarget analytes. The GC and ESI source were combined with a homemade heated column transfer line. GC-ESI/MS-based H/D exchange occurs in an atmospheric pressure ion source as a result of reacting the gas-phase analyte eluted from GC with charged droplets of deuterium oxide infused as the ESI spray solvent. The consumption of the deuterated solvent at a flow rate of 2 μL min -1 was more economical than that in online H/D exchange methods reported to date. In-ESI-source H/D exchange by GC-ESI/MS was applied to 11 stimulants with secondary amino or hydroxyl groups. After H/D exchange, the spectra of the stimulants showed unexchanged, partially exchanged, and fully exchanged ions showing various degrees of exchange. The relative abundances corrected for naturally occurring isotopes of the fully exchanged ions of stimulants, except for etamivan, were in the range 24.3-85.5%. Methylephedrine and cyclazodone showed low H/D exchange efficiency under acidic, neutral, and basic spray solvent conditions and nonexchange for etamivan with an acidic phenolic OH group. The in-ESI-source H/D exchange efficiency by GC-ESI/MS was sufficient to determine the number of hydrogen by elucidation of fragmentation from the spectrum. Therefore, this online H/D exchange technique using GC-ESI/MS has potential as an alternative method for simultaneous H/D exchange of multitarget analytes.

  6. 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.

  7. The Mars Organic Molecule Analyser : in situ analysis of organic compounds on Mars by Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Buch, Arnaud; Sternberg, Robert; Freissinet, Caroline; Pinnick, Veronika; Szopa, Cyril; Coll, Patrice; Geffroy-Rodier, Claude; Raulin, Francois; Goesmann, Fred

    The search for signs of past or present life is one of the primary goals of the future Mars exploratory missions. With this aim the Mars Organic Molecule Analyzer (MOMA) experiment of the ExoMars 2016-2018 next coming joint ESA/NASA mission is designed to perform the in situ analysis of exobiological organic molecules of exobiological interest in the Martian soil such as amino acids, carboxylic acids, nucleobases or polycyclic aromatic hydrocarbons (PAHs). With the aim to separate and detect organic compounds from Martian soil, US and European teams have respectively built an ion trap mass spectrometer and a gas chromatograph. The mass spectrometer prototype has been coupled with the gas chromatograph prototype which is able to work in standalone mode by using a TCD detector. A GC-MS compatible sample processing system (SPS) allowing the extraction and the chemical transformation of the organic compounds from the soil, within space compatible operating conditions, has also been devel-oped. The sample processing is performed in an oven, dedicated to the MOMA experiment containing the solid sample (50-100mg). The internal temperature of which can be ranged from 20 to 1000 C. The extraction step is achieved by using thermodesorption in the range of 100 to 300C for 5 to 20 min. Then, the chemical derivatization and/or thermochemolysis of the extracted compounds is performed directly on the soil with a mixture of MTBSTFA-DMF, TMAH or DMF-DMA solution when enantiomeric separation is required. By decreasing the polarity of the target molecules, this step allows their volatilization at a temperature below 250C without any chemical degradation. Once derivatized, the volatile target molecules are trapped in a cold and chemical trap and promptly desorbed into the gas chromatograph coupled with a mass spectrometer. Preliminary tests, performed on Martian analogue soils (Atacama), with the MOMA SPS-GC/MS experiment, allowed the detection of organic compounds such as amino and

  8. Characteristics of low-mass-velocity vertical gas-liquid two-phase flow

    International Nuclear Information System (INIS)

    Adachi, Hiromichi; Abe, Yutaka; Kimura, Ko-ji

    1995-01-01

    In the present paper, characteristics of low mass velocity two-phase flow was analyzed based on a concept that pressure energy of two-phase flow is converted into acceleration work, gravitational work and frictional work, and the pressure energy consumption rate should be minimum at the stable two-phase flow condition. Experimental data for vertical upward air-water two-phase flow at atmospheric pressure was used to verify this concept and the turbulent model used in this method is optimized with the data. (author)

  9. Analysis of cyanolipids from Sapindaceae seed oils by gas chromatography-EI-mass spectrometry.

    Science.gov (United States)

    Tava, Aldo; Avato, Pinarosa

    2014-04-01

    As a continuation of our investigation on unusual lipids, in the present work we describe a method based on GC-FID and GC-EI-MS to analyze the molecular composition of intact cyanolipids (CL) from selected Sapindaceae plants. We applied our method to the study of CL of type I (1-cyano-2-hydroxymethyl-prop-2-en-1-ol-diester) from Paullinia cupana var. sorbilis and Allophylus dregeanus and CL type III (1-cyano-2-hydroxymethyl-prop-1-en-3-ol-diester) from A. natalensis and Nephelium lappaceum. Our analytical approach allowed us to obtain useful mass spectra to identify individual isomeric molecular species composing the CL mixtures and resulted in the very sensitive detection and identification of minor CL. Defined CL mass spectra resulted in suitable detection of these phytochemicals in complex plant oil mixtures containing acylglycerols. To the best of our knowledge GC-EI-MS spectra of cyanolipids have never been reported before. Moreover, this study improved previous knowledge of the lipid chemistry of Sapindaceae plants.

  10. Planck Intermediate Results. XI: The gas content of dark matter halos: the Sunyaev-Zeldovich-stellar mass relation for locally brightest galaxies

    DEFF Research Database (Denmark)

    Planck Collaboration,; Ade, P. A. R.; Aghanim, N.

    2013-01-01

    gas, and that this gas must be less concentrated than the dark matter in such halos in order to remain consistent with X-ray observations. At the high-mass end, the measured SZ signal is 20% lower than found from observations of X-ray clusters, a difference consistent with Malmquist bias effects......We present the scaling relation between Sunyaev-Zeldovich (SZ) signal and stellar mass for almost 260,000 locally brightest galaxies (LBGs) selected from the Sloan Digital Sky Survey (SDSS). These are predominantly the central galaxies of their dark matter halos. We calibrate the stellar-to-halo...... indication of signal at even lower stellar mass. We derive the scaling relation between SZ signal and halo mass by assigning halo properties from our mock catalogues to the real LBGs and simulating the Planck observation process. This relation shows no evidence for deviation from a power law over a halo mass...

  11. Computational-fluid-dynamics (CFD) analysis of mixing and gas-liquid mass transfer in shake flasks.

    Science.gov (United States)

    Zhang, Hu; Williams-Dalson, Wellae; Keshavarz-Moore, Eli; Shamlou, Parviz Ayazi

    2005-02-01

    CFD (computational fluid dynamics) techniques were used to predict mixing and gas-liquid mass transfer in a 250 ml shake flask operating over a range of shaking frequencies between 100 and 300 rev./min, shaking diameters between 20 and 60 mm, and fill volumes between 25 and 100 ml. Interfacial area, a, volumetric mass-transfer coeffcient, kLa, and the power input per unit volume, epsilonv, of the liquid were predicted to be 300bioreactors used in the fermentation of bacterial and fungal micro-organisms (100bioreactors. Bacterial and fungal micro-organisms require dissolved oxygen concentrations typically in the range 50-250 mmol of O2 . h(-1) . litre(-1), corresponding to volumetric mass-transfer coefficients, kLa, in the range of 250-400 h(-1). Poor mixing and dissolved-oxygen limitation in shake flasks may limit their use in process design and media optimization in fermentation. In contrast, mammalian cells have relatively low demand for oxygen and consequently require a lower specific power input, this being typically between 1 and 10 W . m(-3), allowing efficient operation in shake flasks. Experimental data presented as part of the present study showed that mammalian cell growth in shake flasks was essentially independent of the specific power input, the maximum specific cell growth rate being 0.056 h(-1). The corresponding maximum oxygen-uptake rate was 0.74 mmol of O2 . h(-1) . litre(-1) for a viable cell count of 1.3 x 10(6) cells . ml(-1). These values are comparable with reported values for laboratory and pilotscale bioreactors. This analysis suggests that growth of mammalian cells in shake flasks (and hence in laboratory bioreactors) is not limited by the gas-liquid mass-transfer rate. In mammalian cell cultures, the requirement for good mixing is driven by other considerations, including the need for good cell suspension and reduction in heterogeneity, for example, in pH, temperature, nutrient concentration, osmolality and lactate/glucose ratio.

  12. Analysis of expiration gas in intensive care patients with SIRS/sepsis using proton-transfer-reaction-mass-spectrometry

    International Nuclear Information System (INIS)

    Bodrogi, F.B.M.

    2003-11-01

    In 1971, Pauling and co-workers were the first to detect volatile organic compounds (VOC) in human breath. Since then, a number of technical applications for breath gas analyses have been designed and processed, among them gas chromatography and proton transfer reaction-mass spectrometry (PTR-MS). Due to this technical progress it is meanwhile possible to correlate different kinds and stages of diseases with measurable changes in the patient's VOC profile. The aim of the present study was to investigate the composition of VOC in exhaled air of patients with sepsis via PTR-MS. To isolate distinct volatile organic compounds that may serve as clinical markers for the onset, the progress, as well as the outcome of the disease, the results obtained from septic patients were compared with two different control groups: 25 healthy, non-smoking volunteers enrolled in the day-case-surgery and 25 post-operative in-patients residing in post-anaesthetic care units (PACU). PTR-MS is capable to analyze VOC according to their molecular weight with a range between 21-230 Da. A total of 210 different masses has been detected in the present study. 54 masses were significantly different in exhaled air of septic patients as compared to healthy controls as well as post-operative patients. Among them, mass 69 representing isoprene might be of special interest for the diagnosis of sepsis. Although no exact biochemical properties of isoprene have been described to date, it is known that isoprene synthesis is increased in plants following exposure to oxidative stress. Chronic, systemic infectious diseases like sepsis are accompanied by the production of reactive oxygen species, indicating that isoprene might be increased in the course of sepsis, too. In the present study, isoprene values were markedly higher in septic patients as compared to PACU residents (3.3-fold increase in mean value) and to healthy volunteers (2.2-fold increase in mean value). In addition (and in contrast to other VOC

  13. Distinguishing chinese star anise from Japanese star anise using thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Howes, Melanie-Jayne R; Kite, Geoffrey C; Simmonds, Monique S J

    2009-07-08

    The volatile compounds from the pericarps of Illicium anisatum L., Illicium brevistylum A.C.Sm., Illicium griffithii Hook.f. & Thomson, Illicium henryi Diels, Illicium lanceolatum A.C.Sm., Illicium majus Hook.f. & Thomson, Illicium micranthum Dunn, and Illicium verum Hook.f. were examined by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The volatiles desorbed from the pericarps of I. verum (Chinese star anise), the species traded for culinary purposes, were generally characterized by a high proportion of (E)-anethole (57.6-77.1%) and the presence of foeniculin; the latter was otherwise only detected in the pericarps of I. lanceolatum. In the pericarps of all other species analyzed, the percentage composition of (E)-anethole was comparatively lower (Illicium and can assist with differentiating the fruits of I. verum from other species of Illicium, particularly the more toxic I. anisatum.

  14. Quantification of 31 volatile organic compounds in whole blood using solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Blount, Benjamin C; Kobelski, Robert J; McElprang, David O; Ashley, David L; Morrow, John C; Chambers, David M; Cardinali, Frederick L

    2006-03-07

    The prevalence of exposure to volatile organic compounds (VOCs) has raised concern about possible health effects resulting from chronic human exposure. To support studies exploring the relation between VOC exposure and health effects, we developed an automated analytical method using solid-phase microextraction (SPME), capillary gas chromatography (GC), and quadrupole mass spectrometry (MS). This method quantifies trace levels (low parts per trillion) of 14 halogenated alkanes, 5 halogenated alkenes, 10 aromatic compounds, and 2 other VOCs in human blood. Detection limits for the SPME-GC-MS method range from 0.005 to 0.12 microg/L, with linear calibration curves spanning three orders of magnitude. The improved throughput of this method will enable us to expand biomonitoring efforts to assess nonoccupational VOC exposure in large epidemiological studies.

  15. Identification of Flavor Components in Perfumes by Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Knupp, Gerd; Kusch, Peter; Neugebauer, Michael

    2002-01-01

    An experiment for identification of flavor components in Original Eau de Cologne by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) with electron impact ionization was developed. A new SPME fiber with a dual coating of divinylbenzene and Carboxen, each suspended in polydimethylsiloxane, was used. The compounds were identified by search of the NIST 98 MS Library or by comparison with pure standards. The experiment was developed for second-year chemistry students to learn the principles of analytical instrumentation (GC-MS) and sample preparation techniques (HS-SPME). The students are able to complete this experiment in a single four-hour laboratory session.

  16. Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

    2012-02-01

    The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

  17. Determination of polychlorinated biphenyls in water using dynamic hollow fiber liquid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Guanhua; Zhang, Lijun; Zhang, Zhanen

    2008-09-12

    The application of dynamic hollow fiber liquid-phase microextraction (dynamic HF-LPME) and gas chromatography-mass spectrometry (GC-MS) for the determination of trace amounts of polychlorinated biphenyls (PCBs) in water was investigated. The experimental parameters were optimized. Under the optimum conditions, the concentration enrichment factors for PCBs were from 718-fold to 840-fold. The calibration curves were linear over a range of 0.05-90 microg/L, with a correlation coefficient (r(2)) of 0.9957-0.9979. The relative standard deviation (RSD) ranged from 3.4% to 5.8% for intra-day variation and from 4.1% to 7.3% for inter-day variation. The limits of detection (LODs, S/N=3:1) were in the range of 13-41 ng/L. The recoveries for spiked water samples ranged from 85.9% to 92.0%.

  18. Development of argon cover gas analysis for fast reactors using atmospheric pressure ionization mass spectrometry with collision-induced dissociation

    International Nuclear Information System (INIS)

    Harano, Hideki; Ito, Chikara

    2003-03-01

    The isotopic measurement of krypton in argon is partially obstructed by the isobaric interference in the fast reactor cover gas analysis that is performed using atmospheric pressure ionization mass spectrometry. Collision-induced dissociation is applied to decompose cluster ions and suppress the interference. Cluster ions are accelerated by an electric field in a relatively high-pressure region and are dissociated through multiple collisions with neutral particles. This process is controlled by changing the accelerating voltage in the present study. It is shown that the isobaric interference due to argon dimer ions are suppressed by increasing the accelerating voltage. The isobaric interference could be reduced to 1/60,000 in the most effective condition. It is also found that collision-induced dissociation enhances the detection sensitivity and permits quantitative analysis with a sub-ppt level for the krypton nuclides that are not interfered. (author)

  19. Hydrocarbons identified in extracts from estuarine water accommodated no. 2 fuel oil by gas chromatography-mass spectrometry

    Science.gov (United States)

    Lewis, B. W.; Walker, A. L.; Bieri, R. H.

    1974-01-01

    Results are presented on a computerized gas chromatograph-mass spectrometer analysis of methylene chloride and n-heptane extracts of a No. 2 fuel oil accommodated estuarine water sample. The analytical method is briefly described, and the limitations on the identifications are categorized. Some attempt was made to determine major and trace constituents in the water accommodate. Altogether 66 hydrocarbon compounds were identified specifically, and 75 compounds were partially identified. Seven compounds could be recognized as major constituents of the water accommodated oil and ten were present only as traces. The aromatic compounds found were alkyl benzenes, naphthalene, tetralin, indane, biphenyl, fluorene, anthracene, and some of their alkyl substituted isomers in the range of carbon numbers C7 to C15. Four n-alkanes, C10 to C13, were found along with four other assorted hydrocarbons.

  20. Analysis of tetramethylene disulfotetramine in foods using solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    De Jager, Lowri S; Perfetti, Gracia A; Diachenko, Gregory W

    2008-05-23

    An automated solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method for the determination of tetramethylene disulfotetramine in foods was developed. A comparison of direct immersion (DI) and headspace (HS) extraction techniques using a 70microm carbowax/divinylbenzene (CW/DVB) fiber is presented. The optimized DI-SPME method provided an aqueous extraction limit of detection (LOD) of 9.0ng/g while the HS-SPME LOD was 2.7ng/g. In both SPME modes, recovery was highly matrix dependent and quantification requires standard addition calibrations. Analysis of foods using DI-SPME encountered many obstacles including fiber fouling, low recovery and poor reproducibility. HS-SPME was successfully applied to food analysis with minimal interferences. Standard addition calibration curves for foods gave high linearity (R2>0.98), reproducibility (RSD<12%) and sensitivity with LODs ranging from 0.9 to 4.3ng/g.

  1. The identification of synthetic organic pigments in modern paints and modern paintings using pyrolysis-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Russell, Joanna; Singer, Brian W; Perry, Justin J; Bacon, Anne

    2011-05-01

    A collection of more than 70 synthetic organic pigments were analysed using pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS). We report on the analysis of diketo-pyrrolo-pyrrole, isoindolinone and perylene pigments which are classes not previously reported as being analysed by this technique. We also report on a number of azo pigments (2-naphthol, naphthol AS, arylide, diarylide, benzimidazolone and disazo condensation pigments) and phthalocyanine pigments, the Py-GC-MS analysis of which has not been previously reported. The members of each class were found to fragment in a consistent way and the pyrolysis products are reported. The technique was successfully applied to the analysis of paints used by the artist Francis Bacon (1909-1992), to simultaneously identify synthetic organic pigments and synthetic binding media in two samples of paint taken from Bacon's studio and micro-samples taken from three of his paintings and one painting attributed to him.

  2. Fatty acid composition of wild mushroom species of order Agaricales--examination by gas chromatography-mass spectrometry and chemometrics.

    Science.gov (United States)

    Marekov, Ilko; Momchilova, Svetlana; Grung, Bjørn; Nikolova-Damyanova, Boryana

    2012-12-01

    Applying gas chromatography-mass spectrometry of 4,4-dimethyloxazoline fatty acid derivatives, the fatty acid composition of 15 mushroom species belonging to 9 genera and 5 families of order Agaricales growing in Bulgaria is determined. The structure of 31 fatty acids (not all present in each species) is unambiguously elucidated, with linoleic, oleic and palmitic acids being the main components (ranging between 70.9% (Marasmius oreades) and 91.2% (Endoptychum agaricoides)). A group of three hexadecenoic positionally isomeric fatty acids, 6-, 9- and 11-16:1, appeared to be characteristic components of the examined species. By applying chemometrics it was possible to show that the fatty acid composition closely reflects the classification of the species. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Headspace solid-phase microextraction-gas chromatography-mass spectrometry applied to quality control in multilayer-packaging manufacture.

    Science.gov (United States)

    Ezquerro, Oscar; Pons, Begoña; Tena, María Teresa

    2003-08-01

    A method based on headspace solid-phase microextraction-gas chromatography-mass spectrometry is proposed for the quality control of multilayer packaging and its manufacturing process. Volatile organic compounds (VOCs) are produced in the manufacturing process of the packaging. They can cause organoleptic problems or modify the properties of the packaging depending on the nature and the amount of the VOCs formed. The quantification using packaging samples with a known VOC concentration for the calibration is proposed in order to reduce the analysis time, and the method is validated using a statistical test. Finally, the method is applied to the determination of odour-responsible compounds in multilayer packaging samples obtained under different extrusion-coating conditions, i.e. type of extruder, type of polymer and extrusion speed.

  4. Rapid determination of quetiapine in blood by gas chromatography-mass spectrometry. Application to post-mortem cases.

    Science.gov (United States)

    López-Guarnido, Olga; Tabernero, María Jesús; Hernández, Antonio F; Rodrigo, Lourdes; Bermejo, Ana M

    2014-10-01

    A simple, fast and sensitive method for the determination of quetiapine in human blood has been developed and validated. The method involved a basic liquid-liquid extraction procedure and subsequent analysis by gas chromatography-mass spectrometry, previous derivatization with bis(trimethylsilyl)-trifluoro-acetamide and chorotrimethylsilane (99 : 1). The methods of validation included linearity with a correlation coefficient > 0.99 over the range 0.02-1 µg ml(-1), intra- and interday precision (always < 12%) and accuracy (mean relative error always < 12%) to meet the bioanalytical acceptance criteria. The limit of detection was 0.005 µg ml(-1). The procedure was further applied to post mortems from the Institute of Legal Medicine, University of Santiago de Compostela. Copyright © 2013 John Wiley & Sons, Ltd.

  5. Gas chromatography-mass spectrometric study of 19-oxygenation of the aromatase inhibitor 19-methylandrostenedione with human placental microsomes.

    Science.gov (United States)

    Numazawa, Mitsuteru; Nagaoka, Masao; Handa, Wakako; Yamada, Akane

    2006-06-01

    To gain insight into the catalytic function of aromatase, we studied 19-oxygenation of 19-methyl-substituted derivative of the natural substrate androstenedione (AD), compound 1, with human placental aromatase by use of gas chromatography-mass spectrometry (GC-MS). Incubation of the 19-methyl derivative 1 with human placental microsomes in the presence of NADPH under an aerobic condition did not yield a detectable amount of [19S]19-hydroxy product 2 or its [19R]-isomer 3 when the product was analyzed as the bis-methoxime-trimethylsilyl (TMS) derivative by GC-MS; moreover, the production of estrogen was not detected as the bis-TMS derivative of estradiol (detection limit: about 3 ng and 10 pg per injection for the 19-ol and estradiol, respectively). The results reveal that the 19-methyl steroid 1 does not serve as a substrate of aromatase, although it does serve as a powerful inhibitor of the enzyme.

  6. Technical note: Characterization of key volatile odorants in rabbit meat using gas chromatography mass spectrometry with simultaneous distillation extraction

    Directory of Open Access Journals (Sweden)

    Y.J. Xie

    2016-12-01

    Full Text Available This study explored the key volatile compounds in both male and female rabbit meat. Simultaneous distillation extraction with dichloromethane was adopted to extract the volatile compounds in Hyla rabbit meat. A total of 35 volatile compounds were identified by gas chromatography–mass spectrometry and quantified with 2, 4, 6-thimethylpyridine as internal standard. Seventeen volatile aldehydes, 4 alcohols, 2 ketones, 2 acids, 1 heterocyclic compound, 2 alkanes and 7 esters were detected. Hexanal, heptanal, octanal, nonanal, (E, E-2, 4-decadienal, 1-octen-3-ol and (Z-2-decenal were the key odorant compounds, with high relative odour activity value. Furthermore, the concentration of volatile compounds in male rabbit meat was higher than that in female rabbit meat.

  7. Analytical study of a gas of gluonic quasiparticles at high temperature: Effective mass, pressure, and trace anomaly

    International Nuclear Information System (INIS)

    Giacosa, Francesco

    2011-01-01

    The thermodynamical properties of a pure Yang-Mills theory SU(N) is described by a gas of gluonic quasiparticles with temperature-dependent mass m(T) and a bag function B(T). The analytic behavior of m(T) and the pressure p in the temperature range 2.5-5T c are derived and constraints on the parameters defining B(T) are discussed. The trace anomaly θ=ρ-3p is evaluated in the high T domain: it is dominated by a quadratic behavior θ=nKT 2 , where n=2(N 2 -1) is the number of degrees of freedom and K is an integration constant which does not depend on the bag function B(T). The quadratic rise of θ is in good agreement with recent lattice simulations.

  8. Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Sklerov, J H; Kalasinsky, K S; Ehorn, C A

    1999-10-01

    A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

  9. A simple alkali-metal and noble gas ion source for SIMS equipments with mass separation of the primary ions

    International Nuclear Information System (INIS)

    Duesterhoeft, H.; Pippig, R.

    1986-01-01

    An alkali-metal ion source working without a store of alkali-metals is described. The alkali-metal ions are produced by evaporation of alkali salts and ionization in a low-voltage arc discharge stabilized with a noble gas plasma or in the case of small alkali-metal ion currents on the base of the well known thermic ionization at a hot tungsten wire. The source is very simple in construction and produces a stable ion current of 0.3 μA for more than 100 h. It is possible to change the ion species in a short time. This source is applicable to all SIMS equipments using mass separation for primary ions. (author)

  10. Analysis of Volatile Components of Varietal English Wines Using Stir Bar Sorptive Extraction/Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Darren J. Caven-Quantrill

    2017-12-01

    Full Text Available Aroma is an important property of wine and it can be influenced significantly by enological practices. The aim of this work was, by use of stir bar sorptive extraction/gas chromatography-mass spectrometry (SBSE/GC-MS, to compare semi-quantitative concentrations of the volatile constituents of stainless steel tank-fermented/matured Huxelrebe, Ortega, Schönburger and Siegerrebe varietal wines from a commercial English vineyard, with corresponding wines produced by oak cask (‘barrel’ fermentation/maturation. Aroma profiles of tank and barrel wines were different, with more volatiles detected and net concentrations being higher in barrel wines. Long chain ethyl carboxylate esters were generally more abundant in barrel wines, whereas acetate esters were generally more prominent in tank wines. By conducting a short (~7 month maturation period in secondhand (third or fourth fill casks, it was possible to make wines with more complex aromas, but without obvious oak aroma.

  11. Screening for sarin in air and water by solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Schneider, J F; Boparai, A S; Reed, L L

    2001-10-01

    A method of screening air and water samples for the chemical-warfare agent Sarin is developed using solid-phase microextraction (SPME)-gas chromatography (GC)-mass spectrometry (MS). The SPME field kit sampler is ideal for collecting air and water samples in the field and transporting samples safely to the laboratory. The sampler also allows the sample to be introduced into the GC-MS system without further sample preparation. Results of the tests with Sarin using the SPME technique indicate that a sample collection time of 5 min is sufficient to detect 100 ng/L of Sarin in air. For water samples, Sarin is detected at a concentration of 12 microg/mL or higher. This method is ideal for screening samples for quick response situations.

  12. Quantifying the loss of methane through secondary gas mass transport (or 'slip') from a micro-porous membrane contactor applied to biogas upgrading.

    Science.gov (United States)

    McLeod, Andrew; Jefferson, Bruce; McAdam, Ewan J

    2013-07-01

    Secondary gas transport during the separation of a binary gas with a micro-porous hollow fibre membrane contactor (HMFC) has been studied for biogas upgrading. In this application, the loss or 'slip' of the secondary gas (methane) during separation is a known concern, specifically since methane possesses the intrinsic calorific value. Deionised (DI) water was initially used as the physical solvent. Under these conditions, carbon dioxide (CO2) and methane (CH4) absorption were dependent upon liquid velocity (V(L)). Whilst the highest CO2 flux was recorded at high V(L), selectivity towards CO2 declined due to low residence times and a diminished gas-side partial pressure, and resulted in slip of approximately 5.2% of the inlet methane. Sodium hydroxide was subsequently used as a comparative chemical absorption solvent. Under these conditions, CO2 mass transfer increased by increasing gas velocity (VG) which is attributed to the excess of reactive hydroxide ions present in the solvent, and the fast conversion of dissolved CO2 to carbonate species reinitiating the concentration gradient at the gas-liquid interface. At high gas velocities, CH4 slip was reduced to 0.1% under chemical conditions. Methane slip is therefore dependent upon whether the process is gas phase or liquid phase controlled, since methane mass transport can be adequately described by Henry's law within both physical and chemical solvents. The addition of an electrolyte was found to further retard CH4 absorption via the salting out effect. However, their applicability to physical solvents is limited since electrolytic concentration similarly impinges upon the solvents' capacity for CO2. This study illustrates the significance of secondary gas mass transport, and furthermore demonstrates that gas-phase controlled systems are recommended where greater selectivity is required. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Metrological control of the gas flow and analysis of mass conservation in Bolivia-Brasil gas pipeline; Controle metrologico da vazao de gas e analise da conservacao de massa no gasoduto Bolivia-Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Palhares, Julio Cesar [TBG - Transportadora Brasileira Gasoduto Bolivia-Brasil, S.A., Rio de Janeiro, RJ (Brazil); Orlando, Alcir de Faro; Frota, Mauricio Nogueira [Pontificia Univ. Catolica do Rio de Janeiro, RJ (Brazil). Curso de Pos-graduacao em Metrologia para Qualidade Industrial

    2005-07-01

    International gas pipelines reflect a integrated commerce and impose a metrological challenge for the custody transferences that indistinctly imply in significant economic impact. This work argues the complex analysis of the mass balance and expression of uncertainties of the Gasoduto Bolivia-Brasil (3.150 Km of length, 557 Km in Bolivian territory and 2.593 Km that cross Brazil of West for East), today carrying approximately 60% from its maximum capacity (30 million of cubic meters daily), operating for the Transportadora Brasileira Gasoduto Bolivia Brasil S.A., a enterprise controlled by PETROBRAS Gas S/A (GASPETRO). The TBG measuring methods always taking care of the necessities of the customers as well as being lined up with the changes of the natural gas market. In six years of existence, the TBG came along with the legislation created for regulating agency in formation and adjusted to the establishment of the contract inspector, important landmarks of the evolution of the market. This work presents the definitions that guide the metrological subjects of the TBG, making use of efficient tools in answers for each demand and searching to satisfy its proper necessities, the necessities of its customers and the new demands of the regulating agency. (author)

  14. Validated gas chromatographic-negative ion chemical ionization mass spectrometric method for delta(9)-tetrahydrocannabinol in sweat patches.

    Science.gov (United States)

    Saito, Takeshi; Wtsadik, Abraham; Scheidweiler, Karl B; Fortner, Neil; Takeichi, Sanae; Huestis, Marilyn A

    2004-11-01

    A sensitive gas chromatography-negative ion chemical ionization mass spectrometry (GC/MS-NICI) method was developed and validated for the measurement of Delta(9)-tetrahydrocannabinol (THC) in human sweat patches. THC-d(0) and THC-d(3) were added to worn blank sweat patches (PharmChek; PharmChem Incorporated) and extracted with 3 mL of methanol-0.2 mol/L sodium acetate buffer (pH 5.0, 3:1 by volume) on a reciprocating shaker at ambient temperature for 30 min. Extracted solution (2 mL) was diluted with 8 mL of 0.1 mol/L sodium acetate buffer (pH 4.5) and extracted by use of solid-phase extraction columns (CleanScreen; United Chemical Technologies). Dried extracts were derivatized with trifluoroacetic acid and analyzed with an Agilent 6890 gas chromatograph interfaced with an Agilent 5973 mass selective detector operated in NICI-selected ion-monitoring mode. The lower limits of detection and quantification for THC in human sweat were 0.2 and 0.4 ng/patch, respectively. The calibration curve was linear from 0.4 to 10 ng/patch (R(2) >0.995). Overall recovery of THC from blank worn patches to which 0.6, 4.0, and 8.0 ng of THC had been added was 44-46%. Assay imprecision, expressed as CV, was THC quantification. This GC/MS-NICI assay for THC in human sweat provides adequate sensitivity and performance characteristics for analyzing THC in sweat patches and meets the requirements of the proposed Substance Abuse and Mental Health Administration's guidelines for sweat testing.

  15. Gas chromatography/chemical ionization triple quadrupole mass spectrometry analysis of anabolic steroids: ionization and collision-induced dissociation behavior.

    Science.gov (United States)

    Polet, Michael; Van Gansbeke, Wim; Van Eenoo, Peter; Deventer, Koen

    2016-02-28

    The detection of new anabolic steroid metabolites and new designer steroids is a challenging task in doping analysis. Switching from electron ionization gas chromatography triple quadrupole mass spectrometry (GC/EI-MS/MS) to chemical ionization (CI) has proven to be an efficient way to increase the sensitivity of GC/MS/MS analyses and facilitate the detection of anabolic steroids. CI also extends the possibilities of GC/MS/MS analyses as the molecular ion is retained in its protonated form due to the softer ionization. In EI it can be difficult to find previously unknown but expected metabolites due to the low abundance or absence of the molecular ion and the extensive (and to a large extent unpredictable) fragmentation. The main aim of this work was to study the CI and collision-induced dissociation (CID) behavior of a large number of anabolic androgenic steroids (AAS) as their trimethylsilyl derivatives in order to determine correlations between structures and CID fragmentation. Clarification of these correlations is needed for the elucidation of structures of unknown steroids and new metabolites. The ionization and CID behavior of 65 AAS have been studied using GC/CI-MS/MS with ammonia as the reagent gas. Glucuronidated AAS reference standards were first hydrolyzed to obtain their free forms. Afterwards, all the standards were derivatized to their trimethylsilyl forms. Full scan and product ion scan analyses were used to examine the ionization and CID behavior. Full scan and product ion scan analyses revealed clear correlations between AAS structure and the obtained mass spectra. These correlations were confirmed by analysis of multiple hydroxylated, methylated, chlorinated and deuterated analogs. AAS have been divided into three groups according to their ionization behavior and into seven groups according to their CID behavior. Correlations between fragmentation and structure were revealed and fragmentation pathways were postulated. Copyright © 2016 John Wiley

  16. Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Daniele Z., E-mail: daniele.dzs@dpf.gov.br [Setor Tecnico-Cientifico, Superintendencia Regional do Departamento de Policia Federal no Rio Grande do Sul, 1365 Ipiranga Avenue, Azenha, Zip Code 90160-093 Porto Alegre, Rio Grande do Sul (Brazil); Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil); Pechansky, Flavio [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Duarte, Paulina C.A.V. [Secretaria Nacional de Politicas sobre Drogas (SENAD), Esplanada dos Ministerios, Block ' A' , 5th floor, Zip Code 70050-907 Brasilia, Distrito Federal (Brazil); De Boni, Raquel [Centro de Pesquisa em Alcool e Drogas (CPAD), Hospital de Clinicas de Porto Alegre, Universidade Federal do Rio Grande do Sul, 2350, Ramiro Barcelos Street, Zip Code 90035-903 Porto Alegre, Rio Grande do Sul (Brazil); Froehlich, Pedro E.; Limberger, Renata P. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, 2752 Ipiranga Avenue, Santana, Zip Code 90610-000 Porto Alegre, Rio Grande do Sul (Brazil)

    2011-06-24

    Graphical abstract: Highlights: > Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. > Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. > Linear range 2(4)-256 ng mL{sup -1}, detection limits 0.5-2 ng mL{sup -1}. > Accuracy 98-112%, precision <15% of RSD, recovery 77-112%. > Importance of residual evaluation in checking model goodness-of-fit. - Abstract: A method for the simultaneous identification and quantification of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), diethylpropion (DIE) and methylphenidate (MPH) in oral fluid collected with Quantisal{sup TM} device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL{sup -1} (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL{sup -1}. The detection limits were 0.5 ng mL{sup -1} (MET), 1 ng mL{sup -1} (MPH) and 2 ng mL{sup -1} (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal{sup TM} device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

  17. Determination of amphetamine-type stimulants in oral fluid by solid-phase microextraction and gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Souza, Daniele Z.; Boehl, Paula O.; Comiran, Eloisa; Mariotti, Kristiane C.; Pechansky, Flavio; Duarte, Paulina C.A.V.; De Boni, Raquel; Froehlich, Pedro E.; Limberger, Renata P.

    2011-01-01

    Graphical abstract: Highlights: → Propylchloroformate derivatization of amphetamine-type stimulants in oral fluid. → Direct immersion solid-phase microextraction/gas chromatography-mass spectrometry. → Linear range 2(4)-256 ng mL -1 , detection limits 0.5-2 ng mL -1 . → Accuracy 98-112%, precision TM device has been developed and validated. Thereunto, in-matrix propylchloroformate derivatization followed by direct immersion solid-phase microextraction and gas chromatography-mass spectrometry were employed. Deuterium labeled AMP was used as internal standard for all the stimulants and analysis was performed using the selected ion monitoring mode. The detector response was linear for the studied drugs in the concentration range of 2-256 ng mL -1 (neat oral fluid), except for FEN, whereas the linear range was 4-256 ng mL -1 . The detection limits were 0.5 ng mL -1 (MET), 1 ng mL -1 (MPH) and 2 ng mL -1 (DIE, AMP, FEN), respectively. Accuracy of quality control samples remained within 98.2-111.9% of the target concentrations, while precision has not exceeded 15% of the relative standard deviation. Recoveries with Quantisal TM device ranged from 77.2% to 112.1%. Also, the goodness-of-fit concerning the ordinary least squares model in the statistical inference of data has been tested through residual plotting and ANOVA. The validated method can be easily automated and then used for screening and confirmation of amphetamine-type stimulants in drivers' oral fluid.

  18. [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.

  19. New psychoactive substances as part of polydrug abuse within opioid maintenance treatment revealed by comprehensive high-resolution mass spectrometric urine drug screening.

    Science.gov (United States)

    Heikman, Pertti; Sundström, Mira; Pelander, Anna; Ojanperä, Ilkka

    2016-01-01

    At present, polydrug abuse comprises, besides traditional illicit drugs, new psychoactive substances (NPS) and non-prescribed psychotropic medicines (N-PPM). Polydrug abuse was comprehensively evaluated among opioid-dependent patients undergoing opioid maintenance treatment (OMT). Two hundred consecutively collected urine samples from 82 OMT patients (52 male) treated with methadone or buprenorphine-naloxone medication were studied using a liquid chromatography/time-of-flight mass spectrometry screening method. The method enables simultaneous detection of hundreds of abused substances covering the traditional drugs of abuse and many NPS as well as N-PPM. Ninety-two (45.8%) samples were positive for the abused substances. Benzodiazepines (29.0%), amphetamines (19.5%), cannabinoids (17.0%), NPS (13.0%), N-PPM (9.0%), and opioids (9.0%) were detected in different combinations. The simultaneous occurrence of up to three groups of abused substances was common (40.0%), and in one sample, all six groups were found. The stimulant NPS alpha-pyrrolidinovalerophenone was found in 10.0% and the sedative N-PPM pregabalin in 4.0% of the samples. The patients were seldom aware of what particular NPS they had abused. A widespread occurrence of abused substances beyond the ordinary was revealed. Identifying these patients is essential as polydrug abuse is a safety risk to the patient and may cause attrition from OMT. Copyright © 2016 John Wiley & Sons, Ltd.

  20. Recognition of chitin and proteins in invertebrate cuticles using analytical pyrolysis/gas chromatography and pyrolysis/gas chromatography/mass spectrometry.

    Science.gov (United States)

    Stankiewicz, B A; Van Bergen, P F; Duncan, I J; Carter, J F; Briggs, D E; Evershed, R P

    1996-01-01

    Flash pyrolysis/gas chromatography (py/GC) and py/GC/mass spectrometry (MS) have been utilized to characterize the cuticles of invertebrates chemically. Pyrolysis products have been identified and assigned to specific cuticular components. Acetylpyridones, acetamidofuran, 3-acetamido-5-methylfuran and 3-acetamido-(2 and 4)-pyrones are proposed as characteristic pyrolysis markers for chitin. Pyrolysis products displaying ions of m/z 70, 154, 168, 194 are thought to derive from diketopiperazine structures and provide potential markers for proteins and peptides in which proline, alanine, valine, arginine and glycine are the dominant amino acids. These products, constituting specific pyrolysis markers for invertebrate cuticles, may reflect the amino acid composition of their constituent structural proteins. The source of the various pyrolysis products of proteins has been verified by pyrolysis of reference proteins, peptides and amino acid mixtures. The presence of additional pyrolysis products related directly to histidine and catechol moieties is consistent with the chemical structure and composition proposed for arthropod cuticles based on recent work utilizing solid state 13C and 15N nuclear magnetic resonance. This study constitutes the first comprehensive chemical characterization of the pyrolysis products of invertebrate cuticles and provides the basis for future investigations requiring qualitative screening for cross-linked chitin and proteins in modern and fossil cuticles and in materials, e.g. geopolymers, that may be derived from them.