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Sample records for advanced gc-ms technology

  1. A new type of GC-MS with advanced capabilities

    Science.gov (United States)

    Fialkov, Alexander B.; Steiner, Urs; Jones, Larry; Amirav, Aviv

    2006-03-01

    We have combined the benefits of supersonic molecular beam interface and its related fly-through electron ionization (EI) ion source with the advanced features of the Varian 1200L gas chromatography-mass spectrometry (GC-MS) and mass spectrometry-mass spectrometry (MS-MS), resulting in a new and powerful GC-MS platform with record setting performance. Electron ionization of vibrationally cold molecules in the supersonic molecular beams (SMB) (cold EI) provided mass spectra with enhanced molecular ion, yet with good library search results and superior identification probabilities. We found that high GC column flow rates lower the elution temperature for any given compounds. This allows much larger molecules to elute at the maximum temperature of standard columns. We analyzed a mixture of heavy linear chain hydrocarbons all the way to C84H170 with a molecular weight of 1179.3 amu, using a 4 m 0.25 mm i.d. column and 32 ml/min He flow rate. Furthermore, we obtained a dominant molecular ion to all these compounds. The lower elution temperatures also greatly enhance the ability to analyze very thermally labile compounds such as carbamate pesticides. The experimental 1200 system is capable of triple quadrupole based MS-MS. We found that MS-MS on the molecular ion is much more effective than on fragment ions, and thus, the enhancement of the molecular ion directly improves the MS-MS sensitivity. Fast GC-MS analysis was also explored, based on very high column flow rate for fast splitless injections without affecting the sensitivity, and on the high system selectivity due to the combination of enhanced molecular ion and MS-MS. We demonstrate a few seconds long GC-MS-MS analysis of diazinon, spiked at 10 ng/g in a mixed fruit and vegetable extract. The feature of enhanced molecular ion provides significant enhancement in the detection sensitivity via SIM and RSIM on the molecular ion. While octafluoronaphthalene (OFN) detection limit of below 1 fg in SIM mode is shown, the

  2. Py-GC/MS, GC/MS and FTIR investigations on Late Roman-Egyptian adhesives from opus sectile: new insights into ancient recipes and technologies.

    Science.gov (United States)

    Ribechini, Erika; Orsini, Sibilla; Silvano, Flora; Colombini, Maria Perla

    2009-04-06

    An analytical protocol based on optical microscopy, Fourier transforms infrared spectroscopy (FTIR), analytical pyrolysis in the presence of hexamethyldisilazane followed by gas chromatographic/mass spectrometric analysis (Py-GC/MS) and gas chromatography/mass spectrometry after alkaline hydrolysis, solvent extraction and trimethylsilylation (GC/MS) was used in the chemical characterisation of the original adhesives used to fix monochrome and mosaic glass and stone plaques coming from the Late Roman archaeological site of Antinoopolis (Egypt). FTIR analysis demonstrated the presence of calcite fragments, and Py-GC/MS and GC/MS analyses provided detailed molecular compositions, highlighting the presence of a wide range of compound classes including diterpenoid acids, tricyclic abietanes with a high degree of aromatisation, mid- and long-chain monocarboxylic fatty acids, mono- and di-hydroxy acids, alpha,omega-dicaboxylic fatty acids, n-alkanols, and n-alkanes. Characteristic biomarkers and their distribution patterns indicated the presence of pine pitch in all the adhesives, which in some cases was admixed with beeswax and brassicaceae seed oil. The results provided new insights into the complex recipes used by artisans in ancient Egypt in the production of adhesives and in the sophisticated manufacture of opus sectile decorations.

  3. MOMA GC-MS coupling

    Science.gov (United States)

    Buch, A.; Pinnick, V. T.; Grand, N.; Szopa, C.; Danell, R.; Lustrement, B.; Freissinet, C.; van Amerom, F. H.; Raulin, F.; Glavin, D. P.; Stalport, F.; Coll, P. J.; Arevalo, R. D.; Brinckerhoff, W. B.; Goesmann, F.; Mahaffy, P. R.

    2013-12-01

    The joint ESA-Roscosmos Exo-Mars-2018 rover mission seeks the signs of past or present life on Mars. The Mars Organic Molecule Analyzer (MOMA) aboard the ExoMars rover will be a key analytical tool in providing chemical (molecular) information from the solid samples, with particular focus on the characterization of organic content. Central to MOMA instrumentation is a gas chromatograph-mass spectrometer (GC-MS) which provides the unique ability to characterize a broad range of compounds allowing chemical analyses of volatile and non-volatile species. The Gas chromatograph and the oven have been built at LATMOS/LISA (France) and at MPS (Germany) respectively whereas the mass spectrometer has been built at the NASA Goddard Space Flight Center (USA). Both instruments have been tested separately first and have been coupled in order to test the efficiency of the future MOMA GC-MS instrument. The main objective of the second step has been to test the quantitative response of both instruments while they are coupled and to characterize the combined instrument detection limit for several compounds. A final experiment has been done in order to test the feasibility of the separation and detection of a mixture contained in a soil sample introduced in the MOMA oven.

  4. GC/MS DETERMINATION OF BIOACTIVE COMPONENTS OF PLEUROTUS OSTREATUS

    Directory of Open Access Journals (Sweden)

    V.Priya

    2012-03-01

    Full Text Available In this study, the bioactive components of Pleurotus ostreatus have been evaluated using GC/MS. The chemical compositions of the hydroalcholic extract of Pleurotus ostreatus were investigated using Perkin-Elmer Chromatography–Mass Spectrometry, while the mass spectra of the compounds found in the extract was matched with the National Institute of Standards and Technology (NIST library. GC/MS analysis of hydroalcholic extract of Pleurotus ostreatus revealed the existence of Cholestane-3,7,1,25-tetrol tetraacetate,(3a,5a,7a,12 a-55.20, 9,12-Octadecadienoic acid,methyl ester(E,E-18.55,14,17- Octadecadienoic acid,methyl ester(E,E-5.59,Pentadecanoic acid, ethyl ester-3.84.. The results of this study offer a platform for using Pleurotus ostreatus as herbal alternative for the current synthetic antimicrobial agents.

  5. A comparison of direct infusion MS and GC-MS for metabolic footprinting of yeast mutants

    DEFF Research Database (Denmark)

    Mass, S.; Villas-Bôas, Silas Granato; Hansen, Michael Adsetts Edberg;

    2007-01-01

    Recent technical advances in mass spectrometry (MS) have propelled this technology to the forefront of methods employed in metabolome analysis. Here, we compare two distinct analytical approaches based on MS for their potential in revealing specific metabolic footprints of yeast single-deletion m......Recent technical advances in mass spectrometry (MS) have propelled this technology to the forefront of methods employed in metabolome analysis. Here, we compare two distinct analytical approaches based on MS for their potential in revealing specific metabolic footprints of yeast single......-deletion mutants. Filtered fermentation broth samples were analyzed by GC-MS and direct infusion ESI-MS. The potential of both methods in producing specific and, therefore, discriminant metabolite profiles was evaluated using samples from several yeast deletion mutants grown in batch-culture conditions....... Thus, the GC-MS method is good for classification of mutants with altered nitrogen regulation as it primarily measures amino acids, whereas this method cannot classify mutants involved in regulation of phospholipids metabolism as well as the direct infusion MS (DI-MS) method. From the analysis, we find...

  6. Study on Catalytic Pyrolysis of DiatomChaetoceros sp. by Py-GC/MS Technology%Py-GC/MS技术用于Chaetoceros sp.硅藻的催化热解研究

    Institute of Scientific and Technical Information of China (English)

    张晓红; 苏秋成; 林福华; 陈晓丽; 付娟

    2015-01-01

    The catalytic pyrolysis characteristics of diatom Chaetoceros sp. powders were investigated by pyrolysis–gas chromatography/mass spectrometry (Py-GC/MS) technology. Using HZSM-5 as catalyst, the effect of Si/Al ratio in HZSM-5, catalyst consumption, pyrolysis heating rate and pyrolysisreaction time on pyrolysis products of diatom Chaetoceros sp. were studied. The results show that the pyrolysis products of diatomChaetoceros sp. without catalysts are mainly fatty acids with the contents of 50.05%, and the contents of benzenes are only 0.87%. When catalysts were added, the contents of fatty acids are decreased and aromatic compounds are significantly increased. Pyrolysis results suggest that, desired products of 57.76% benzenes and 2.63% fatty acids could be obtained on the conditions of Si/Al ratio of 38, diatom:HZSM-5 at a 1:9 mass ratio, heating rate 10 000oC/s and reaction time of 10 s, which indicates that the reaction of deoxygenation and aromatization significantly happen with HZSM-5(38)'s addition. Thus, HZSM-5(38) is favorable for Diatom Chaetoceros sp. to produce high quality bio-oil products by catalytic pyrolysis.%采用热裂解?气质联用(Py-GC/MS)技术研究Chaetoceros sp.硅藻粉末的催化热解特性.以HZSM-5为催化剂,考察了不同Si/Al比的HZSM-5催化剂对硅藻热解产物的影响,并考察了催化剂的使用量、热解升温速率、热解反应时间对产物的影响.结果表明:未加催化剂时,硅藻热解产物以脂肪酸为主,含量为 50.05%,苯系物含量仅为0.87%;加入HZSM-5催化剂后,硅藻热解产物中脂肪酸含量减少,芳香类化合物显著增加.热解实验结果发现,Si/Al比为38、硅藻和HZSM-5比例为1:9、热解速率10 000℃/s、热解时间为10 s时,能得到较理想的热解产品,其中苯系物产率可达 57.76%,脂肪酸含量为 2.63%.这说明 HZSM-5(38)具有较好的脱氧和芳构化功能,有利于硅藻催化热解生成高品质的生物油产品.

  7. Recently developed GC/MS and LC/MS methods for determining NSAIDs in water samples.

    Science.gov (United States)

    Farré, M; Petrovic, M; Barceló, D

    2007-02-01

    Pharmaceuticals have become major targets in environmental chemistry due to their presence in aquatic environments (following incomplete removal in wastewater treatment or point-source contaminations), threat to drinking water sources and concern about their possible effects to wildlife and humans. Recently several methods have been developed for the determination of drugs and their metabolites in the lower nanogram per litre range, most of them using solid-phase extraction (SPE) or solid-phase microextraction (SPME), derivatisation and finally gas chromatography mass spectrometry (GC-MS), gas chromatography tandem mass spectrometry (GC-MS/MS) and liquid chromatography electrospray tandem mass spectrometry (LC-ES/MS/MS). Due to the elevated polarity of non-steroidal anti-inflamatory drugs (NSAIDs), analytical techniques based on either liquid chromatography coupled to mass spectrometry (LC-MS) and gas chromatography coupled to mass spectrometry (GC-MS) after a previous derivatisation step are essential. The most advanced aspects of current GC-MS, GC-MS/MS and LC-MS/MS methodologies for NSAID analysis are presented.

  8. Molecular analysis of intact preen waxes of Calidris Canutus (Aves: Scolopacidae) by GC/MS and GC/MS/MS

    NARCIS (Netherlands)

    Sinninghe Damsté, J.S.; Dekker, M.H.A.; Piersma, T.

    2000-01-01

    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 additi

  9. Determination of Paraffin in Bean Thread Noodles by Employing GC/MS and GC/FID Technology%GC-MS、GC-FID测定粉丝中的石蜡含量

    Institute of Scientific and Technical Information of China (English)

    舒平; 杨卫花; 甘献明

    2010-01-01

    利用GC-MS,GC-FID技术,对粉丝样品中的石蜡检测进行了方法建立及实际样品测试.分析结果表明,该方法对粉丝中百蜡检测的相对标准偏差为2.3%~4.7%,样品的回收率为96%~103%.方法简便、准确、可靠、前处理简单.

  10. Analysis of eicosanoids by LC-MS/MS and GC-MS/MS: a historical retrospect and a discussion.

    Science.gov (United States)

    Tsikas, Dimitrios; Zoerner, Alexander A

    2014-08-01

    Eicosanoids are a large family that derives from arachidonic acid, i.e., eicosatetraenoic acid. Prominent members include prostaglandins, thromboxane and leukotrienes. They are biologically highly active lipid mediators and play multiple physiological roles. GC-MS/MS has played a pivotal role in the identification and quantification of eicosanoids in biological samples. This technology generated a solid knowledge of their analytical chemistry, biochemistry, physiology and pharmacology. Since about a decade, GC-MS and GC-MS/MS are increasingly displaced by the seemingly more simple, rapid and powerful LC-MS/MS in the area of instrumental analysis of physiological substances, drugs and their metabolites. In this article, we review and discuss LC-MS/MS methods published over the last decade from the perspective of the GC-MS/MS user. Our analysis revealed that the shift from the adult GC-MS/MS to the youthful emerging LC-MS/MS technology in eicosanoid analysis is associated with several important challenges. Known pitfalls and problematic issues discovered by eicosanoid pioneers by using GC-MS/MS are often ignored by LC-MS/MS users. Established reference values and intervals provided by GC-MS-based methods are not considered properly in developing and validating LC-MS/MS methods. Virtually, there is a belief in the unlimited capability of the LC-MS/MS technique in eicosanoid analysis, a thought that simulates analytical certainty. LC-MS/MS users should profit from the plethora of solid knowledge acquired from the use of GC-MS/MS in eicosanoid analysis in basic and clinical research.

  11. Use of Gas Chromatography-Mass Spectrometry (GC-MS) in Nonscience Major Course Laboratory Experiments

    Science.gov (United States)

    Kostecka, Keith S.; Lerman, Zafra M.; Angelos, Sanford A.

    1996-06-01

    Gas chromatography-mass spectrometry (GC-MS) has been utilized with nonscience majors in the courses: "Modern Methods in Science: Discovering Molecular Secrets"; "The Extraordinary Chemistry of Ordinary Things"; "From Ozone to Oil Spills: Chemistry, the Environment and You"; and "Crime Lab Chemistry: Solving Crime through Analytical Chemistry". Our efforts have centered on introducing prospective science communicators (film, video, radio, television, and journalism majors) to science relative to their majors and personal interests. Quality lecture-discussion topics, "mystery"-based laboratory activities have assisted in introducing and/or explaining specific areas of chemistry that attempt to reduce fear of subject matter. Students have also used GC-MS, as a form of alternative assessment, in course projects that have been based on their majors, personal interests, and cultural backgrounds. Students have also conducted advanced independent work in different areas of chemistry, including the analysis of nail polishes and lacquers and eleven aromatic compounds present in three different brands of gasoline.

  12. Gas Chromatography-mass Spectrometry (GC-MS analysis of alkaloids isolated from Epipremnum aureum (Linden and Andre Bunting

    Directory of Open Access Journals (Sweden)

    Anju Meshram

    2015-02-01

    Full Text Available Recent advances in the use of GC coupled to MS have allowed a chemically guided isolation of uncommon and bioactive alkaloids. The present study was aimed to focus on the extraction and screening of alkaloids from Epipremnum aureum (Linden and Andre Bunting. It has been observed that the plant is very rich in alkaloids and the modified method employed for the extraction of alkaloid is efficient and selective, where the interference of other secondary metabolites is negligible. The identification of each compound was made through gas chromatography-mass spectrometry (GC-MS. A total of twenty six structurally different alkaloids were identified for the first time from this plant. E. aureum is highly rich in alkaloids and twenty six different alkaloids were characterized. The present study may help in the field of natural products’ chemistry and pharmaceuticals as well as drug discovery science and technology.

  13. Clandestine laboratory scene investigation and processing using portable GC/MS

    Science.gov (United States)

    Matejczyk, Raymond J.

    1997-02-01

    This presentation describes the use of portable gas chromatography/mass spectrometry for on-scene investigation and processing of clandestine laboratories. Clandestine laboratory investigations present special problems to forensic investigators. These crime scenes contain many chemical hazards that must be detected, identified and collected as evidence. Gas chromatography/mass spectrometry performed on-scene with a rugged, portable unit is capable of analyzing a variety of matrices for drugs and chemicals used in the manufacture of illicit drugs, such as methamphetamine. Technologies used to detect various materials at a scene have particular applications but do not address the wide range of samples, chemicals, matrices and mixtures that exist in clan labs. Typical analyses performed by GC/MS are for the purpose of positively establishing the identity of starting materials, chemicals and end-product collected from clandestine laboratories. Concerns for the public and investigator safety and the environment are also important factors for rapid on-scene data generation. Here is described the implementation of a portable multiple-inlet GC/MS system designed for rapid deployment to a scene to perform forensic investigations of clandestine drug manufacturing laboratories. GC/MS has long been held as the 'gold standard' in performing forensic chemical analyses. With the capability of GC/MS to separate and produce a 'chemical fingerprint' of compounds, it is utilized as an essential technique for detecting and positively identifying chemical evidence. Rapid and conclusive on-scene analysis of evidence will assist the forensic investigators in collecting only pertinent evidence thereby reducing the amount of evidence to be transported, reducing chain of custody concerns, reducing costs and hazards, maintaining sample integrity and speeding the completion of the investigative process.

  14. GC-MS and FT-IR analysis of a coastal medicinal plant-Hyptis suaveolens (L. Poit

    Directory of Open Access Journals (Sweden)

    Joselin Joseph

    2016-05-01

    Full Text Available Objective: To investigate the bioactive components of a coastal medicinal plant, Hyptis suaveolens (L. Poit. (H. suaveolens leaves using fourier transform-infrared spectroscopy and gas chromatography-mass spectrometer (GC-MS. Methods: The chemical compositions of the ethanol extract of whole plant of H. suaveolens was investigated using PerkinElmer GC-MS, while the mass spectra of the compounds found in the extract was matched with the National Institute of Standard and Technology library. Results: The results of fourier transform-infrared spectroscopy analysis confirmed the presence of secondary alcohols, phenols, alkanes, alkynes, aromatics, nitro compounds and aliphatic compounds. GC-MS analysis of the ethanolic extract revealed the existence of 30 phytochemical compounds. 5,5-Dimethylimidazolidin-2,4-diamine (20.35% was found to be the major compound. Conclusions: The results of this study offer a platform to use H. suaveolens leaves as herbal alternative for various diseases.

  15. GC-MS and FT-IR analysis of a coastal medicinal plant-Hyptis suaveolens (L.) Poit

    Institute of Scientific and Technical Information of China (English)

    Joselin Joseph; Solomon Jeeva

    2016-01-01

    Objective:To investigate the bioactive components of a coastal medicinal plant,Hyptis suaveolens (L.) Poit. (H. suaveolens) leaves using fourier transform-infrared spectroscopy and gas chromatography-mass spectrometer (GC-MS). Methods: The chemical compositions of the ethanol extract of whole plant ofH. suaveolens was investigated using PerkinElmerGC-MS, while the mass spectra of the compounds found in the extract was matched with the National Institute of Standard and Technology library. Results: The results of fourier transform-infrared spectroscopy analysis confirmed the presence of secondary alcohols, phenols, alkanes, alkynes, aromatics, nitro compounds and aliphatic compounds.GC-MS analysis of the ethanolic extract revealed the existence of 30 phytochemical compounds. 5,5-Dimethylimidazolidin-2,4-diamine (20.35%) was found to be the major compound. Conclusions: The results of this study offer a platform to useH. suaveolens leaves as herbal alternative for various diseases.

  16. Phytochemical studies on Allamanda cathartica L. using GC-MS

    Institute of Scientific and Technical Information of China (English)

    Prabhadevi V; Sahaya Sathish S; Johnson M; Venkatramani B; Janakiraman N

    2012-01-01

    Objective: To explore the phytochemical constituents present in Allamanda cathartica (A. cathartica) L. using GC-MS. Methods: 20 g of the powdered leaf and stem sample of A. cathartica was equilibrated with 200 d/m of A. cathartica ethanol for 24 h, separately. The volume of the supernatant was later reduced by heating to 2 d/m. The concentrated ethanolic extracts were further subjected to GC-MS analysis. Results: The GC-MS analyses determined the presence of 28 different phytochemical compounds in the ethanolic leaf extract of A. cathartica. The major phytoconstituents were 9,12,15-octadecatrienoic acid (Z,Z,Z)- (16.39%), n-hexadecanoic acid (14.08%), 3-O-methyl-d-glucose (11.03%) and 9,12,15-octadecatrienoic acid ethyl ester (Z,Z,Z)-(10.58%). The ethanolic stem extract of A. cathartica showed the presence of 26 different bioactive compounds. The major ones are 3-O-methyl-d-glucose (29.86%), 2-furancarboxaldehyde 5-(hydroxymethyl)- (14.87%), n-hexadecanoic acid (9.13%) and 9,12,15-octadecatrienoic acid (Z,Z,Z)- (7.34%). Conclusions: This study helps to predict the formula and structure of biomolecules which can be used as drugs and further investigation may lead to the development of drug formulation.

  17. Detection of the Spermicide Nonoxynol-9 Via GC-MS

    Science.gov (United States)

    Musah, Rabi A.; Vuong, Angela L.; Henck, Colin; Shepard, Jason R. E.

    2012-05-01

    The spermicide nonoxynol-9 is actually a complex mixture of dozens of closely related amphiphilic compounds, and the chemical properties of this assortment significantly hamper its characterization by GC-MS. The inability to perform routine GC-MS testing on nonoxynol-9 has limited its evidentiary value in forensic casework, which relies heavily on this technique for analysis. A disturbing trend in sexual assault is the use of condoms by assailants, to avoid leaving behind DNA evidence that can connect a perpetrator to a victim. This observation necessitates the development of alternative methods for the analysis of trace evidence that can show causal links between a victim and a suspect. Detection of lubricants associated with sexual assault is one such way to establish this connection. The development of GC-MS methods that permit facile detection of both nonoxynol-9 alone and nonoxynol-9 extracted from other complex matrices that have potential as trace evidence in sexual assault is reported. A detection limit of 2.14 μg of nonoxynol-9 is demonstrated, and a detailed mass spectral profile that elaborates on what is known of its structure is provided.

  18. LC/MS and SFC/MS: will they replace GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Warner, M.

    1987-07-01

    Will LC/MS and SFC/MS eventually replace GC/MS as the method of choice for organic trace analysis. This question was addressed at a symposium organized by Richard Browner of the Georgia Institute of Technology at this year's Pittsburgh Conference in Atlantic City, NJ. The symposium, one of the best-attended technical sessions at this year's meeting, featured presentations by Browner, Ron Hites of Indiana University, Jack Henion of Cornell University, Dick Smith of Battelle's Pacific Northwest Laboratory, and Marvin Vestal of The University of Houston.

  19. GC-MS study of Nigella sativa (seeds fatty oil

    Directory of Open Access Journals (Sweden)

    Mehta, B. K.

    2002-06-01

    Full Text Available The GC-MS study of N. sativa (seeds fatty oil revealed the presence of 26 compounds which were identified as methyl hept-6-enoate,1-phenylhepta-2,4-dione, pentadecane, hexadec-1-ene, 1-phenyldecan-2-one, octadec-1-ene, octadecane, methyl pentadecanoate, bis(3-chlorophenyl ketone, diethyl phthalate, ethyl octadec-7-enoate, methyl octadecanoate, tricos-9-ene, octadeca-9,12-dienoic acid, hexadecanoic acid, methyl hexadecanoate, methyl octadec-15-enoate, henicosan-10-one, 2-methyl octadecanoic acid, docos-1-ene, ethyl octadecanoate, methyl octadecanoate, pentacos-5-ene,12-methyltricosane, dibutyl phthalate and 2-methyltetracosane.El estudio por GC-MS del aceite de la semilla de Nigella sativa reveló la presencia de 26 compuestos los cuales fueron identificados como: hept-6-enoato de metilo, 1-fenilhepta-2,4-diona, pentadecano, hexadec-1-eno, 1-fenildecan-2-ona, octadec-1-eno, octadecano, pentadecanoato de metilo, bis(3-clorofenil cetona, ftalato de dietilo, octadec-7-enoato de etilo, octadecanoato de metilo, tricos-9-eno, ácido octadeca-9,12-dienoico, ácido hexadecanoico, hexadecanoato de metilo, octadec-15-enoato de metilo, henicosan-10-ona, ácido 2-metil octadecanoico, docos-1-eno, octadecanoato de etilo, octadecanoato de metilo, pentacos-5-eno, 12-metiltricosano, ftalato de dibutilo y 2-metiltetracosano.

  20. Determination of aromatic compounds in eluates of pyrolysis solid residues using HS-GC-MS and DLLME-GC-MS.

    Science.gov (United States)

    Bernardo, Maria S; Gonçalves, M; Lapa, N; Barbosa, R; Mendes, B; Pinto, F; Gulyurtlu, Ibrahim

    2009-11-15

    A method for the determination of 15 aromatic hydrocarbons in eluates from solid residues produced during the co-pyrolysis of plastics and pine biomass was developed. In a first step, several sampling techniques (headspace solid phase microextraction (HS-SPME), static headspace sampling (HS), and dispersive liquid-liquid microextraction (DLLME) were compared in order to evaluate their sensitivity towards these analytes. HS-SPME and HS sampling had the better performance, but DLLME was itself as a technique able to extract volatiles with a significant enrichment factor. HS sampling coupled with GC-MS was chosen for method validation for the analytes tested. Calibration curves were constructed for each analyte with correlation coefficients higher than 0.999. The limits of detection were in the range of 0.66-37.85 ng/L. The precision of the HS method was evaluated and good repeatability was achieved with relative standard deviations of 4.8-13.2%. The recoveries of the analytes were evaluated by analysing fortified real eluate samples and were in the range of 60.6-113.9%. The validated method was applied in real eluate samples. Benzene, toluene, ethylbenzene and xylenes (BTEX) were the compounds in higher concentrations. The DLLME technique coupled with GC-MS was used to investigate the presence of less volatile contaminants in eluate samples. This analysis revealed the presence of significant amounts of alkyl phenols and other aromatic compounds with appreciable water solubility.

  1. GC/MS Analysis of the Aromatic Composition of Gasoline

    Science.gov (United States)

    Kostecka, Keith S.; Rabah, Ashraf; Palmer, Charles F., Jr.

    1995-09-01

    The gas chromatography/mass spectrometry (GC/MS) analysis of three brands of regular unleaded gasoline was conducted as part of the independent project of an undergraduate journalism major. In his work, samples of each gasoline were diluted down to part per million (ppm) levels with dichloromethane and then one microliter injections were made onto a Hewlett-Packard GC (5890 Series II unit). Mass spectra were also obtained on each sample through use of a 5971A mass selective detector (MSD). Subsequent characterization was consequently effected through utilization of the standard mass spectra available in a 49,000 compound National Bureau of Standards reference library. Comparison of the obtained and standard spectra revealed that the same aromatic hydrocarbons (including, in part: benzene, the xylenes, naphthalene, and methylated naphthalenes) were present in all three samples. Percentage values for these and other aromatic hydrocarbons were then generated and tabulated.

  2. Derivatization of carbohydrates for GC and GC-MS analyses.

    Science.gov (United States)

    Ruiz-Matute, A I; Hernández-Hernández, O; Rodríguez-Sánchez, S; Sanz, M L; Martínez-Castro, I

    2011-05-15

    GC and GC-MS are excellent techniques for the analysis of carbohydrates; nevertheless the preparation of adequate derivatives is necessary. The different functional groups that can be found and the diversity of samples require specific methods. This review aims to collect the most important methodologies currently used, either published as new procedures or as new applications, for the analysis of carbohydrates. A high diversity of compounds with diverse functionalities has been selected: neutral carbohydrates (saccharides and polyalcohols), sugar acids, amino and iminosugars, polysaccharides, glycosides, glycoconjugates, anhydrosugars, difructose anhydrides and products resulting of Maillard reaction (osuloses, Amadori compounds). Chiral analysis has also been considered, describing the use of diastereomers and derivatives to be eluted on chiral stationary phases.

  3. Determination of drugs in hair using GC/MS/MS.

    Science.gov (United States)

    Uhl, M

    1997-01-17

    An important task for the forensic toxicologist and expert witness is the detection of the noxa in biological matrices. Because of this, the identification and quantification of residues of illegal drugs in human hair is still of growing interest. Utilizing the advantages of GC/MS/MS testing human hair is performed for most common drugs of abuse like heroin and other opioides, cocaine, cannabis and amphetamine derivatives. Analyzing hair specimens for substances that present a toxicological risk is another challenge. Several quality control parameters must be observed to avoid false positive or false negative results and to gain additional information. Blank sample, blank hair as well as the combined wash extracts are tested for the presence of the relevant compounds within every series. Careful evaluation of the findings can provide an approximate measure of the intensity of drug use in the majority of cases.

  4. Mechanism of Xylan Pyrolysis by Py-GC/MS

    Institute of Scientific and Technical Information of China (English)

    WANG Shu-rong; LIANG Tao; RU Bin; GUO Xiu-juan

    2013-01-01

    In order to investigate the decomposition behavior of hemicellulose,xylan was chosen as the representative of hemicellulose to study the fast pyrolysis on the combination system of analytical pyrolyzer and gas chromatograph coupled with mass spectrometer(Py-GC/MS).The main condensable products of xylan pyrolysis consisted of acids,aldehydes,and ketones; while gas products contained CO2,CO,CH4 and H2.Acetic acid and furfural were the most abundant products with the highest contents of 20.11% and 20.24% respectively.While furfural and acetic acid were formed competitively with residence time and temperature increases,the distribution of xylan pyrolysis products did not vary with the residence time and temperature,while the total content of several kinds of products changed a lot.According to the analysis of experimental data,a reaction pathway of xylan decomposition was deduced so as to illustrate the formation mechanism of main products.

  5. Characterizing Vaccinium berry Standard Reference Materials by GC-MS using NIST spectral libraries.

    Science.gov (United States)

    Lowenthal, Mark S; Andriamaharavo, Nirina R; Stein, Stephen E; Phinney, Karen W

    2013-05-01

    A gas chromatography-mass spectrometry (GC-MS)-based method was developed for qualitative characterization of metabolites found in Vaccinium fruit (berry) dietary supplement Standard Reference Materials (SRMs). Definitive identifications are provided for 98 unique metabolites determined among six Vaccinium-related SRMs. Metabolites were enriched using an organic liquid/liquid extraction, and derivatized prior to GC-MS analysis. Electron ionization (EI) fragmentation spectra were searched against EI spectra of authentic standards compiled in the National Institute of Standards and Technology's mass spectral libraries, as well as spectra selected from the literature. Metabolite identifications were further validated using a retention index match along with prior probabilities and were compared with results obtained in a previous effort using collision-induced dissociation (CID) MS/MS datasets from liquid chromatography coupled to mass spectrometry experiments. This manuscript describes a nontargeted metabolite profile of Vaccinium materials, compares results among related materials and from orthogonal experimental platforms, and discusses the feasibility and development of using mass spectral library matching for nontargeted metabolite identification.

  6. GC/MS analysis of piperidinocyclohexanecarbonitrile (PCC) smoking products

    Energy Technology Data Exchange (ETDEWEB)

    Lue, L.P.; Scimeca, J.A.; Thomas, B.F.; Martin, B.R.

    1986-03-05

    Piperidinocyclohexanecarbonitrile (PCC), an intermediate in phencyclidine (PCP) synthesis, is a major contaminant of illicit PCP. Due to the frequent abuse of PCP by smoking, this study was conducted to determine the PCC pyrolysis products delivered in smoke. Marihuana placebo cigarettes were impregnated with /sup 3/H-piperidino-/sup 14/C-cyano-PCC (synthesized in the lab and recrystallized twice, m.p. 67/sup 0/C) and burned under conditions which simulated smoking. Mainstream smoke was passed through glass wool filters and H/sub 2/SO/sub 4/ and NaOH traps. Tritium and /sup 14/C were recovered as 83%, and 56%, respectively, of the starting material. Seventy-six percent of the recovered tritium was found in the glass wool trap followed by 13, 7 and 4% in the acid trap, base trap and in the ash/unburned butt, respectively. Seventy-three percent of the recovered /sup 14/C was found in the glass wool filter and 16 and 8% were found in the acid and base traps, respectively. GC/MS analysis revealed the presence of 1-piperidinocyclohexene (30%), PCC (24%), piperidine (7%), and 1-acetyl-piperidine (5%).

  7. GC/MS ANALYSIS OF RHEUM RIBES RHIZOMES

    Directory of Open Access Journals (Sweden)

    DR. RAGHAD DH ABDUL JALILL

    2015-03-01

    Full Text Available Objectives: Rheum ribes is a species of perennial and stout herbs that are distributed in southwest of Asia. Crude extracts of their rhizomes have different medicinal activities. Their pharmacological activity may due to their chemical compositions. Methods: This study was carrying out to determine the qualitative and quantitative analysis of chemical components of Rheum ribes rhizomes using two methods by GC-MS. The level of some elements and total protein was also determined. Result: The results of phytochemical screening showed the presence of sugar, flavonoids, glycosides and alkaloids. Nine compounds were identified using methods (1 while there were six different compounds when method (2 was used. Atomic Absorption Spectrometry determined the levels of Cu, Cd, Mn, K, Fe, Co and Ti. Nitrogen was determined by Macro Kjeldahl method. The amounts of them were (2.584, 3.513, 35.03, 0.0388, 126.85, 1, 0.02 and 0.59 percentage respectively. There were not neither phosphors nor Zinc in rhizomes of this plant. The level of total proteins were 3.688 %. Conclusion: The rhizomes R. ribes contain sixteen different components with different levels of more than eight elements.

  8. DETERMINATION OF PHTHALATES FROM BOTTLED WATER BY GC-MS

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    IRINA DUMITRAȘCU

    2012-03-01

    Full Text Available Determination of phthalates from bottled water by GC-MS. Phthalates are ubiquitous pollutants in the environment, due to their widespread use in the last years. These compounds are used principally as plasticizers, to impact flexibility, workability and durability to polymers but they can also be found in products such as paints, adhesives, inks and cosmetics. Phthalates are not chemically bounded to polymers; hence they are easily released and migrate into foods, beverages and drinking water from the packaging or bottling materials or manufacturing processes. This process accelerates as plastic products age and break down. With respect to their endocrine disrupting potential, phthalates such as benzyl butyl phthalate (BBP, di-butyl phthalate (DBP and di-isobutyl phthalate (DIBP have been found to elicit estrogenic responses in in vitro assays. It is possible that phthalates are a contributory factor to endocrine-mediated adverse effects observed in wildlife and humans over the past few decades. In this experiment we have analyzed the phthalates from different bottled waters purchased from the market. Determination by gas chromatography in combination with mass spectrometry detector (GC–MS in electronic ionization mode (EI with selected-ion monitoring (SIM acquisition method (GC–MS (EI–SIM has been carried out. Methods have been developed for both qualitative and quantitative analysis of phthalates. The base peak (m/z = 149 of all the phthalates was selected for the screening studies. The characteristic ions of each compound were chosen for quantitative studies.

  9. PBX 9501 Outgas Analysis by SPME/GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Chambers, D.M.

    2000-12-11

    The authors used equilibrium headspace gas chromatography/mass spectrometry (GC/MS) to monitor volatile and semivolate species that are expected to migrate through PBX 9501 under environmentally relevant conditions. In this work they screened 11 samples taken from deployed parts. Although a number of chemical permeates were identified, the antioxidant signature provided the most information with regard to decomposition aging. Specifically, they were able to monitor butylated hydroxytoluene (BHT) and other antioxidants, which are apparently added to either the Estane adipate or MDI precursor by the manufacturer. They found that in those parts where diphenylamine (DPA) was used as a stabilizer, BHT response was significantly lower than in those formulations stabilized with Irganox 1010 (Irganox). These results imply that DPA is less efficient as a radical scavenger than Irganox. This lower efficiency might be related to the lack of oxygen in the weapon environment, which is initially < 0.1%. With regard to DPA, it has been reported that radical scavenging activity is proportional to the oxygen pressure. At this time they are uncertain whether the low DPA efficiency is mainly attributed to the oxygen level or if there is another rate limiting step that would lead to the preferential consumption of BHT.

  10. Untargeted Metabolomic Analysis of Capsicum spp. by GC-MS.

    Science.gov (United States)

    Aranha, Bianca Camargo; Hoffmann, Jessica Fernanda; Barbieri, Rosa Lia; Rombaldi, Cesar Valmor; Chaves, Fábio Clasen

    2017-09-01

    In order to conserve the biodiversity of Capsicum species and find genotypes with potential to be utilised commercially, Embrapa Clima Temperado maintains an active germplasm collection (AGC) that requires characterisation, enabling genotype selection and support for breeding programmes. The objective of this study was to characterise pepper accessions from the Embrapa Clima Temperado AGC and differentiate species based on their metabolic profile using an untargeted metabolomics approach. Cold (-20°C) methanol extraction residue of freeze-dried fruit samples was partitioned into water/methanol (A) and chloroform (B) fractions. The polar fraction (A) was derivatised and both fractions (A and B) were analysed by gas chromatography coupled to mass spectrometry (GC-MS). Data from each fraction was analysed using a multivariate principal component analysis (PCA) with XCMS software. Amino acids, sugars, organic acids, capsaicinoids, and hydrocarbons were identified. Outlying accessions including P116 (C. chinense), P46, and P76 (C. annuum) were observed in a PCA plot mainly due to their high sucrose and fructose contents. PCA also indicated a separation of P221 (C. annuum) and P200 (C. chinense), because of their high dihydrocapsaicin content. Although the metabolic profiling did not allow for grouping by species, it permitted the simultaneous identification and quantification of several compounds complementing and expanding the metabolic database of the studied Capsicum spp. in the AGC. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  11. Analysis of Phenolic and Cyclic Compounds in Plants Using Derivatization Techniques in Combination with GC-MS-Based Metabolite Profiling

    Directory of Open Access Journals (Sweden)

    Jens Rohloff

    2015-02-01

    Full Text Available Metabolite profiling has been established as a modern technology platform for the description of complex chemical matrices and compound identification in biological samples. Gas chromatography coupled with mass spectrometry (GC-MS in particular is a fast and accurate method widely applied in diagnostics, functional genomics and for screening purposes. Following solvent extraction and derivatization, hundreds of metabolites from different chemical groups can be characterized in one analytical run. Besides sugars, acids, and polyols, diverse phenolic and other cyclic metabolites can be efficiently detected by metabolite profiling. The review describes own results from plant research to exemplify the applicability of GC-MS profiling and concurrent detection and identification of phenolics and other cyclic structures.

  12. Diethylstilbestrol in fish tissue determined through subcritical fluid extraction and with GC-MS

    Science.gov (United States)

    Qiao, Qinghui; Shi, Nianrong; Feng, Xiaomei; Lu, Jie; Han, Yuqian; Xue, Changhu

    2016-06-01

    As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol (DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane (R134a) extraction in combination with gas chromatography-mass spectrometry (GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C18 and NH2 solid phase extraction (SPE). Finally, the analyte was derived by heptafluorobutyric anhydride (HFBA), followed by GC-MS analysis. Response surface methodology (RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26°C; amount of co-solvent volume, 4.7 mL. Under this condition, at a spiked level of 1, 5, 10 μg kg-1, the mean recovery of DES was more than 90% with relative standard deviations (RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.

  13. DETERMINATION OF 16 LARGEST PEAKS IN COMMERCIAL TECHNICAL TOXAPHENE BY GC/MS

    Science.gov (United States)

    Under typical temperature and high vacuum associated with GC/MS technique, Toxaphene decomposes and produces countless fragments which are impractical to quantify. A GC/MS method has been developed using the lowest possible temperature to resolve more peaks and lower the interfer...

  14. Phytochemical screening and GC-MS determination of bioactive constituents from methanol leaf extract of Senna occidentalis

    Directory of Open Access Journals (Sweden)

    Aisha Mohammad Ibrahim

    2015-12-01

    Full Text Available Objective: To identify the active ingredients presented in methanol extract of Senna occidentalis (S. occidentalis. Methods: Dried powdered leaves of S. occidentalis were extracted with methanol by Soxhlet extraction and the extract was subjected to preliminary phytochemical screening by using standard procedure and methods. Gas chromatography-mass spectrometer (GC-MS analysis was performed by comprising a GC-MS (model: QP2010 Plus Shimadzu, Japan comprising an AOC-20i auto-sampler and gas-chromatograph interfaced to a mass spectrometer. Results: The phytochemical study revealed the presence of tannins, alkaloids, glycoside, flavonoids, steroids, saponins, anthraquinones and phlobatannins while cardiac glycoside was not detected. GC-MS chromatogram showed nine peaks. A total of 31 compounds were identified when the mass spectra of the constituents was compared with the National Institute Standard and Technology library. The first compounds identified with less retention time (15.929 s were n-hexadecanoic acid, octadecanoic acid and pentadecanoic acid while decanoic acid, decyl ester, ether, octadecyl vinyl, oleic acid, hexyl ester, stearic acid, octadecyl ester and decyl fluoride took the longest retention time (20.600 s for identification. Conclusions: The presence of these compounds in the plant extract may at least be responsible for one of the pharmacological properties of S. occidentalis and thus could be of considerable interest to the development of new drugs.

  15. Phytochemical screening and GC-MS determination of bioactive constituents from methanol leaf extract ofSenna occidentalis

    Institute of Scientific and Technical Information of China (English)

    Aisha Mohammad Ibrahim; Bashir Lawal; Ndababru Amos Tsado; Abubakar Awwal Yusuf; Adisa Mohammed Jimoh

    2015-01-01

    Objective:To identify the active ingredients presented in methanol extract ofSenna occidentalis(S. occidentalis). Methods: Dried powdered leaves ofS. occidentalis were extracted with methanol by Soxhlet extraction and the extract was subjected to preliminary phytochemical screening by using standard procedure and methods. Gas chromatography-mass spectrometer (GC-MS) analysis was performed by comprising aGC-MS (model: QP2010 Plus Shimadzu, Japan) comprising an AOC-20i auto-sampler and gas-chromatograph interfaced to a mass spectrometer. Results: The phytochemical study revealed the presence of tannins, alkaloids, glycoside, flavonoids, steroids, saponins, anthraquinones and phlobatannins while cardiac glycoside was not detected.GC-MS chromatogram showed nine peaks. A total of 31 compounds were identified when the mass spectra of the constituents was compared with the National Institute Standard and Technology library. The first compounds identified with less retention time (15.929 s) were n-hexadecanoic acid, octadecanoic acid and pentadecanoic acid while decanoic acid, decyl ester, ether, octadecyl vinyl, oleic acid, hexyl ester, stearic acid, octadecyl ester and decyl fluoride took the longest retention time (20.600 s) for identification. Conclusions:The presence of these compounds in the plant extract may at least be responsible for one of the pharmacological properties ofS. occidentalis and thus could be of considerable interest to the development of new drugs.

  16. Ecological observations and GC-MS analysis of methanolic extract of Sacoglossan Elysia bangtawaensis (Swennen)

    Digital Repository Service at National Institute of Oceanography (India)

    Shenai-Tirodkar, P.S.; Desai, N.M.; Jagtap, T.G.

    respective peak areas to TIC areas from the GC-MS. Significant variations of ecological parameters were investigated by correlation matrix. Difference were considered statistically significant when p<0.05. RESULTS In postmonsoon (November, 2007-January, 2008...

  17. A bioequivalency study of two trifluoperazine tablet formulations using RIA and GC-MS.

    Science.gov (United States)

    Midha, K K; Hawes, E M; Korchinski, E D; Hubbard, J W; McKay, G; Cooper, J K; Roscoe, R M

    1984-01-01

    Two sensitive analytical procedures, a radioimmunoassay (RIA) and a mass fragmentographic (GC-MS) method, were used to quantitate plasma trifluoperazine concentrations over 24 h in five healthy male volunteers following single 5 mg doses of two trifluoperazine tablet formulations (A and B) in a two-way cross-over design. Bioavailability in terms of area under the plasma concentration versus time curve to 24h or extrapolated to infinity, maximum plasma concentration and time to maximum plasma concentration using either RIA or GC-MS was not statistically significantly different from one formulation to the other. Also, there were no statistically significant differences between GC-MS and RIA values for AUC24(0) and Cmax for each of the two formulations examined. However, the mean AUC24(0) RIA/GC-MS ratios for formulations A and B were 3.1 and 3.4, respectively, while the mean Cmax RIA/GC-MS ratios were 1.7 and 2.1, respectively. These differences in AUC and Cmax are probably mainly due to the relative non-specificity of the RIA antiserum. Thus, where GC-MS is preferred for pharmacokinetic studies, both analytical procedures can be used for comparative single-dose bioequivalence studies of trifluoperazine. However, both the methods should be tested in patients in order to establish the suitability of one procedure over the other for the study of plasma level versus clinical response correlations.

  18. Molecular structure of kerogens from source rocks of the Tarim Basin: A study by Py-GC-MS and methylation-Py-GC-MS

    Institute of Scientific and Technical Information of China (English)

    JIA; Wanglu; PENG; Ping'an

    2005-01-01

    Flash pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) and in situ methylation-pyrolysis-gas chromatography-mass spectrometry (methylation-Py-GC-MS) have been employed for a study of molecular structure of kerogens from source rocks of the Tarim Basin. The main products from Py-GC-MS of the Ordovician and Triassic kerogens from the Tarim Basin are n-alkanes and n-alk-1-enes which decrease in relative abundance with increased carbon number. The major products from methylation-Py-GC-MS are normal saturated fatty acid methyl esters which show maxima at C16 and C18. These aliphatic compounds are mainly from lipids of planktonic algae. Moreover, there are more abundant long-chain fatty acids (C20-C26) and normal n-alkanes and n-alk-1-enes (C15-C25) in pyrolysates of Triassic kerogens than that of Ordovician kerogens, reflecting the discrepancies in sources of the Triassic kerogens and the Ordovician kerogens. Besides these aliphatic compounds, methoxyl benzoic acid methyl esters were detected only in products from methylation-Py-GC-MS of late Ordovician kerogen TAC1-1, which possibly was the first molecular evidence for the appearance of moss or other terrestrial plants in the Tarim Basin. In addition, the relative intensity of 17β(H)-trisnorhopane17 β(H),21 α(H)-30-normoretane and 17 β(H)-moretane is lower, but 17α(H)-trisnorhopane and17 α(H)-30-norhopane is higher in the pyrolysates of the Ordovician kerogens in comparison with the pyrolysates of the Triassic kerogens. Moreover, Pr-1-ene has been detected in pyrolysates of Triassic kerogens. These differences in pyrolysates consist with maturity of kerogens. In conclusion, combination of methylation-Py-GC-MS and Py-GC-MS are useful tools to investigate the molecular structure of geomacromolecules and can be subject to type the organic matter, compare the maturity of kerogens and carry out the oil-source correlation.

  19. GC/MS based identification of skunk spray maliciously deployed as "biological weapon" to harm civilians.

    Science.gov (United States)

    Wennig, Robert; Schneider, Serge; Meys, François

    2010-05-15

    Our laboratory has been asked to elucidate the origin of a strong "toxic smell" present in a prominent politician's office, private house and motorcar. This stinky and pungent atmosphere has caused serious nausea and vomiting to several individuals. Urine samples were collected from the persons presenting symptoms of nausea for toxicological analysis. Drops, paper and cotton swabs of an oily liquid found at the implicated places were submitted by police to our laboratory for investigation. Methanol extracts of the drops were acetylated for gas chromatography/mass spectrometry (GC/MS) analysis in the electron impact mode; the cotton and paper swabs were analysed using headspace-gas chromatography/mass spectrometry (HS-GC/MS). The GC/MS analysis of the acetylated methanol extracts revealed that the major peaks of the chromatogram could be attributed to 2-methylquinoline, to 2-quinolinemethanethiol, to S-2-quinolinemethyl thioacetate, to 2-phenylethanethiol, to bis(E)-2-butenyl disulphide and to bis(3-methylbutyl) disulphide. Several volatile sulphur-containing compounds have been identified with the HS-GC/MS system. Detailed examination of the spectra as well as GC/MS analysis of commercially available skunk secret allowed us to relate the identified compounds to those present in the defence spray of skunks. No health sequels were observed for any of the persons implicated in this case.

  20. Urinary metabolomics of pregnant women at term: a combined GC/MS and NMR approach.

    Science.gov (United States)

    Caboni, Pierluigi; Meloni, Alessandra; Lussu, Milena; Carta, Emanuela; Barberini, Luigi; Noto, Antonio; Deiana, Sara Francesca; Mereu, Rossella; Ragusa, Antonio; Paoletti, Anna Maria; Melis, Gian Benedetto; Fanos, Vassilios; Atzori, Luigi

    2014-10-01

    Physiological changes leading to parturition are not completely understood while clinical diagnosis of labour is still retrospective. Gas chromatography mass spectrometry (GC/MS) and nuclear magnetic resonance spectroscopy (NMR) represent two of the main analytical platforms used in clinical metabolomics. Metabolomics might help us to improve our knowledge about the biochemical mechanisms underlying labour. Urine samples (n = 59), collected from pregnant women at term of gestation before and/or after the onset of labour, were analysed by GC/MS and NMR techniques in order to identify the metabolic profile. Both GC/MS and NMR data matrices containing the identified metabolites were analysed by multivariate statistical techniques in order to characterise the discriminant variables between labour (L) and not labour (NL) status. 18 potential metabolites (11 with (1)H-NMR, eight with GC-MS: glycine was relevant in both) were found discriminant in urine of women during labour. Taken together, the identified metabolites produced a composite biomarker pattern, a sort of barcode, capable of differentiating between labour and not labour conditions. Major discriminant metabolites for NMR and GC/MS analysis were: alanine, glycine, acetone, 3-hydroxybutiyric acid, 2,3,4-trihydroxybutyric acid and succinic acid, giving a urine metabolite signature on the late phase of labour. The metabolomics analysis evidenced clusters of metabolites involved in labour condition able to discriminate between urine samples collected before the onset and during labour, potentially offering the promise of a robust screening test.

  1. THE IDENTIFICATION OF THE BINDING MEDIA IN THE TANG DYNASTY CHINESE WALL PAINTINGS BY USING Py-GC/MS AND GC/MS TECHNIQUES

    Directory of Open Access Journals (Sweden)

    Hong GUO

    2011-06-01

    Full Text Available The archaeological discoveries of Tang tomb murals in Xi’an, China brought to light unprecedented data for the study of the art of the Tang Dynasty (618-907 AD. The spectacular murals with their particular contents provided first-hand material for the study of Chinese history and the techniques of wall paintings during the Tang Dynasty. In order to gain a better understanding of the materials used and to preserve those paintings, pyrolysis-gas chromatography-mass spectrometry (Py-GC/MS and gas chromatography-mass spectrometry (GC/MS were applied for the characterization of the binding media in the paintings. The combination of these analytical techniques is an ideal methodology to identify binding media in unknown samples.

  2. GC-MS and GC-MS/MS in PCI mode determination of mescaline in peyote tea and in biological matrices.

    Science.gov (United States)

    Gambelunghe, Cristiana; Marsili, Remo; Aroni, Kyriaki; Bacci, Mauro; Rossi, Riccardo

    2013-01-01

    Peyote, a cactus containing the hallucinogen mescaline, is used to induce altered states of consciousness in religious ceremonies or for recreational purpose. This study reports a case of an underage boy suspected of mescaline abuse. For this purpose, we analyzed a dark green liquid sample found in the bedroom of the boy whose urine and hair samples were collected shortly after the drink was found. A method by gas chromatography-mass spectrometry tandem mass spectrometry (GC-MS/MS) in positive chemical ionization mode was developed and validated in terms of linearity, specificity, accuracy, and sensitivity for mescaline determination at the low concentrations present in hair. GC-MS analysis of the liquid identified mescaline, while urine was negative; GC-MS/MS segmental hair analysis identified mescaline in the proximal segment (root to 2 cm), while the distal segments were negative. Although peyote was uncommonly encountered, its use was confirmed by segmental hair analysis that can provide long-term information about drugs use.

  3. Analytical Approaches Based on Gas Chromatography Mass Spectrometry (GC/MS) to Study Organic Materials in Artworks and Archaeological Objects.

    Science.gov (United States)

    Bonaduce, Ilaria; Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla

    2016-02-01

    Gas chromatography/mass spectrometry (GC/MS), after appropriate wet chemical sample pre-treatments or pyrolysis, is one of the most commonly adopted analytical techniques in the study of organic materials from cultural heritage objects. Organic materials in archaeological contexts, in classical art objects, or in modern and contemporary works of art may be the same or belong to the same classes, but can also vary considerably, often presenting different ageing pathways and chemical environments. This paper provides an overview of the literature published in the last 10 years on the research based on the use of GC/MS for the analysis of organic materials in artworks and archaeological objects. The latest progresses in advancing analytical approaches, characterising materials and understanding their degradation, and developing methods for monitoring their stability are discussed. Case studies from the literature are presented to examine how the choice of the working conditions and the analytical approaches is driven by the analytical and technical question to be answered, as well as the nature of the object from which the samples are collected.

  4. Metabolomics and Trace Element Analysis of Camel Tear by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Raish, Mohammad; Yaqoob, Syed Hilal; Khan, Altaf; Shakeel, Faiyaz

    2017-06-01

    Camel tear metabolomics and elemental analysis are useful in getting the information regarding the components responsible for maintaining the protective system that allows living in the desert and dry regions. The aim of this study was to correlate that the camel tears can be used as artificial tears for the evaluation of dryness in the eye. Eye biomarkers of camel tears were analyzed by gas chromatography-mass spectroscopy (GC-MS) and inductively coupled plasma mass spectroscopy (ICP-MS). The major compounds detected in camel tears by GC-MS were alanine, valine, leucine, norvaline, glycine, cadaverine, urea, ribitol, sugars, and higher fatty acids like octadecanoic acid and hexadecanoic acid. GC-MS analysis of camel tears also finds several products of metabolites and its associated metabolic participants. ICP-MS analysis showed the presence of different concentration of elemental composition in the camel tears.

  5. GC-MS determination of isoflavonoids in seven red Cuban propolis samples.

    Science.gov (United States)

    Campo Fernández, Mercedes; Cuesta-Rubio, Osmany; Rosado Perez, Arístides; Montes De Oca Porto, Rodny; Márquez Hernández, Ingrid; Piccinelli, Anna Lisa; Rastrelli, Luca

    2008-11-12

    In the present study, the phenolic composition analysis of seven red varieties of propolis, collected in different regions of Cuba, was evaluated by gas chromatography/mass spectrometry (GC-MS). Seventeen compounds were identified in all samples by the interpretation of their mass spectra. This appears to be the first report on the GC-MS analysis of isoflavonoids in the propolis. The results confirmed the presence of the main isoflavonoids isolated previously and suggested the general structure for the other five isoflavonoids. Vestitol, 7-O-methylvestitol, and medicarpin were present in high amounts in all propolis samples analyzed. This result indicates that propolis samples rich in isoflavonoids are not exclusively found in Pinar del Rio province and proves that GC-MS technique is a useful and alternative tool for the chemical analysis of tropical red propolis.

  6. 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.

  7. Active and realistic passive marijuana exposure tested by three immunoassays and GC/MS in urine

    Energy Technology Data Exchange (ETDEWEB)

    Mule, S.J.; Lomax, P.; Gross, S.J.

    1988-05-01

    Human urine samples obtained before and after active and passive exposure to marijuana were analyzed by immune kits (Roche, Amersham, and Syva) and gas chromatography/mass spectrometry (GC/MS). Seven of eight subjects were positive for the entire five-day test period with one immune kit. The latter correlated with GC/MS in 98% of the samples. Passive inhalation experiments under conditions likely to reflect realistic exposure resulted consistently in less than 10 ng/mL of cannabinoids. The 10-100-ng/mL cannabinoid concentration range essential for detection of occasional and moderate marijuana users is thus unaffected by realistic passive inhalation.

  8. Catalytic pyrolysis of Laminaria japonica over nanoporous catalysts using Py-GC/MS

    Directory of Open Access Journals (Sweden)

    Jeon Jong-Ki

    2011-01-01

    Full Text Available Abstract The catalytic pyrolysis of Laminaria japonica was carried out over a hierarchical meso-MFI zeolite (Meso-MFI and nanoporous Al-MCM-48 using pyrolysis gas chromatography/mass spectrometry (Py-GC/MS. The effect of the catalyst type on the product distribution and chemical composition of the bio-oil was examined using Py-GC/MS. The Meso-MFI exhibited a higher activity in deoxygenation and aromatization during the catalytic pyrolysis of L. japonica. Meanwhile, the catalytic activity of Al-MCM-48 was lower than that of Meso-MFI due to its weak acidity.

  9. An appraisal on the degradation of paracetamol by TiO2/UV system in aqueous medium: product identification by gas chromatography-mass spectrometry (GC-MS)

    OpenAIRE

    Dalmázio,Ilza; Alves,Tânia M. A.; Augusti,Rodinei

    2008-01-01

    The advanced oxidation of paracetamol (1) promoted by TiO2/UV system in aqueous medium was investigated. Continuous monitoring by several techniques, such as UV-Vis spectroscopy, HPLC (high performance liquid chromatography), TOC (total organic carbon), and ESI-MS (electrospray ionization mass spectrometry), revealed that whereas the removal of paracetamol was highly efficient under these conditions, its mineralization was not likewise accomplished. GC-MS (gas chromatography-mass spectrometry...

  10. ACR-700 advanced technologies

    Energy Technology Data Exchange (ETDEWEB)

    Tapping, R.L.; Turner, C.W. [Atomic Energy of Canada Limited, Chalk River, Ontario (Canada); Yu, S.K.W. [Atomic Energy of Canada Limited, Mississauga, Ontario (Canada); Olmstead, R.; Speranzini, R.A. [Atomic Energy of Canada Limited, Chalk River, Ontario (Canada)

    2004-12-01

    A successful advanced reactor plant will have optimized economics including reduced operating and maintenance costs, improved performance, and enhanced safety. Incorporating improvements based on advanced technologies ensures cost, safety and operational competitiveness of the ACR-700. These advanced technologies include modern configuration management; construction technologies; operational technology for the control centre and information systems for plant monitoring and analysis. This paper summarizes the advanced technologies used to achieve construction and operational improvements to enhance plant economic competitiveness, advances in the operational technology used for reactor control, and presents the development of the Smart CANDU suite of tools and its application to existing operating reactors and to the ACR-700. (author)

  11. GC-MS analysis of bioactive compounds in the methanol extract of Clerodendrum viscosum leaves

    Directory of Open Access Journals (Sweden)

    Pritipadma Panda

    2015-01-01

    Full Text Available Background: Clerodendrum viscosum is commonly found in India and Bangladesh. Previously, various parts of this plant were reported for treatment of different types of diseases and there was no report on GC-Ms analysis. Objective: To analyze and characterize the phytochemical compounds of methanol extract of Clerodendrum viscosum using GC-MS. Materials and Methods: The preliminary phytochemical screening of methanol extract was carried out according to standard procedures described in WHO guidelines. Various bioactive compounds of the extract were determined by GC-MS technique. Results: The presence of steroids, triterpenoids, alkaloids, saponins, flavonoids, tannins and carbohydrate was found on phytochemical screening of methanol extract of the leaves. The GC-MS analysis showed 16 peaks of different phytoconstituents namely acetamide,N,N-carbonylbis-, 4-Pyranone,2,3-dihydro-, alpha-D-Galactofuranoside, methyl 2,3,5,6-tetra-O-methyl-, Glycerin, Xylitol, N,N-Dimethylglycine, 4H-Pyran-4-one,2,3-dihydro-3, 5-dihydroxy-6-methyl-, Benzofuran,2,3-dihydro-, 5-Hydroxymethylfurfural, 2(1HPyrimidinone,1-methyl-, 2,4-Dihydroxy-5,6-dimethylpyrimidine, 3-Deoxy-d-mannoic lactone, 1,3-Methylene-d-arabitol, Orcinol, n-Hexadecanoic acid and Phenol,4,4′-(1-methyl ethylidene bis etc. Conclusion: The bioactive compounds present in the methanol extract of Clerodendrum viscosum suggest the application of this extract for the treatment of various diseases by the aborigine tribes.

  12. [Study on supercritical CO2 extraction of xiaoyaosan and its GC-MS fingerprint].

    Science.gov (United States)

    Zuo, Ya-Mei; Tian, Jun-Sheng; Guo, Xiao-Qing; Zhou, Yu-Zhi; Gao, Xiao-Xia; Qin, Xue-Mei

    2014-02-01

    To determine the optimum conditions of supercritical CO2 extraction of Xiaoyaosan, and establish its fingerprint by gas chromatography-mass spectrometry (GC-MS), the yield of extract were investigated, an orthogonal test was used to quantify the effects of extraction temperature, pressure, CO2 flow rate and time, and fingerprint analysis of different batches of extracts were by GC-MS. The optimal extraction conditions were determined as follows: extraction pressure 20 MPa, extraction temperature 50 degrees C, CO2 flow rate 25 kg x h(-1), extraction time 3 h, and average yield 2.2%. The GC-MS fingerprint was established and 27 common peaks were found, whose contents add up to 81.89% of the total peak area. Among them, 21 compounds were identified, accounting for 53.20% of the total extract. The extraction process is reasonable and favorable for industrial production. The GC-MS method is accurate, reliable, reproducible, and can be used for quality control of supercritical CO2 extract from Xiaoyaosan.

  13. Identification and Determination of Nicorandil and its Degradation Products by HPLC and GC/MS

    Institute of Scientific and Technical Information of China (English)

    Zhong Zhou CHENG; Ze Hui JIA; Yan CHEN; Li Ying CHEN; Hua LI

    2006-01-01

    A rapid and sensitive HPLC-DAD method is developed for simultaneous determination of nicorandil and its degradation products, N-(2-hydroxyethyl) nicotinamide, nitrate ion and nicotinic acid, using nicotinamide (NT) as internal standard, at wavelength 204 nm. Nicotinic acid is identified by HPLC and GC/MS. The method can also be applied to study kinetic of degradation processes of nicorandil in storage.

  14. Identification and quantification of isoquinoline alkaloids in the genus Sarcocapnos by GC-MS.

    Science.gov (United States)

    Suau, R; Cabezudo, B; Valpuesta, M; Posadas, N; Diaz, A; Torres, G

    2005-01-01

    Six cularine alkaloids, cularicine, O-methylcularicine, celtisine, cularidine, cularine and celtine, three isocularine alkaloids, sarcophylline, sarcocapnine and sarcocapnidine, and five non-cularine alkaloids, glaucine, protopine, ribasine, dihydrosanguinarine and chelidonine, were identified and quantified by GC-MS in nine taxa of the genus Sarcocapnos (Fumariaceae). The chemotaxonomic significance of the results is discussed.

  15. GC-MS Analysis of [gamma]-Hydroxybutyric Acid Analogs: A Forensic Chemistry Experiment

    Science.gov (United States)

    Henck, Colin; Nally, Luke

    2007-01-01

    An upper-division forensic chemistry experiment is described. It involves using glycolic acid and sodium glycolate as analogs of [gamma]-hydroxybutyric acid and its sodium salt. The experiment shows the use of silylation in GC-MS analysis and gives students the opportunity to work with a commonly used silylating reagent,…

  16. Determination of Cinnamaldehyde in Cinnamon by SPME-GC-MS: An Instrumental Analysis Experiment

    Science.gov (United States)

    Wang, Yimin; Ocariz, Jessica; Hammersand, Jennifer; MacDonald, Evan; Bartczak, Ashley; Kero, Frank; Young, Vaneica Y.; Williams, Kathryn R.

    2008-01-01

    Students analyze "trans"-cinnamaldehyde in commercial cinnamon using solid-phase microextraction and GC-MS with ethyl benzoate as the internal standard. Aside from the instrumentation, the experiment utilizes readily available low hazard materials and can be completed within one four-hour laboratory period. (Contains 2 figures.)

  17. Selecting parameters for the environmental interpretation of peat molecular chemistry - A pyrolysis-GC-MS study

    NARCIS (Netherlands)

    Schellekens, J.F.P.; Buurman, P.; Pontevedra Pombal, X.

    2009-01-01

    A number of samples from a deep peat bog in Tierra del Fuego were analyzed using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) in order to extract parameters that might be used to interpret the peat chemistry in terms of vegetation change, anaerobic and aerobic decomposition, and fire in

  18. Comparison of GC-MS and FTIR methods for quantifying naphthenic acids in water samples.

    Science.gov (United States)

    Scott, Angela C; Young, Rozlyn F; Fedorak, Phillip M

    2008-11-01

    The extraction of bitumen from the oil sands in Canada releases toxic naphthenic acids into the process-affected waters. The development of an ideal analytical method for quantifying naphthenic acids (general formula C(n)H(2n+Z)O(2)) has been impeded by the complexity of these mixtures and the challenges of differentiating naphthenic acids from other naturally-occurring organic acids. The oil sands industry standard FTIR method was compared with a newly-developed GC-MS method. Naphthenic acids concentrations were measured in extracts of surface and ground waters from locations within the vicinity of and away from the oil sands deposits and in extracts of process-affected waters. In all but one case, FTIR measurements of naphthenic acids concentrations were greater than those determined by GC-MS. The detection limit of the GC-MS method was 0.01 mg L(-1) compared to 1 mg L(-1) for the FTIR method. The results indicated that the GC-MS method is more selective for naphthenic acids, and that the FTIR method overestimates their concentrations.

  19. Rapid Py-GC/MS assessment of the structural alterations of lignins in genetically modified plants

    NARCIS (Netherlands)

    Rencoret, Jorge; Del Río, José Carlos; Nierop, Klaas G J|info:eu-repo/dai/nl/182329895; Gutiérrez, Ana; Ralph, John

    Genetic modifications for perturbing the lignin pathway in three different species of angiosperm plants, including non-woody (Arabidopsis and alfalfa) and woody (poplar) plants, were readily evaluated by analytical pyrolysis coupled to gas chromatography-mass spectrometry (Py-GC/MS). Pyrolysis

  20. GC-MS Quantitation and Identification of Bisphenol-A Isolated from Water

    Science.gov (United States)

    Mead, Ralph N.; Seaton, Pamela J.

    2011-01-01

    Isolation and identification of organic compounds is a necessary skill chemistry students must be able to do with proficiency. In this upper-level undergraduate laboratory, students isolate bisphenol-A (BPA; 4-4'-isopropylidenediphenol) from water using solid-phase extraction (SPE) followed by derivatization with analysis by GC-MS. The students…

  1. GC-MS Analysis of [gamma]-Hydroxybutyric Acid Analogs: A Forensic Chemistry Experiment

    Science.gov (United States)

    Henck, Colin; Nally, Luke

    2007-01-01

    An upper-division forensic chemistry experiment is described. It involves using glycolic acid and sodium glycolate as analogs of [gamma]-hydroxybutyric acid and its sodium salt. The experiment shows the use of silylation in GC-MS analysis and gives students the opportunity to work with a commonly used silylating reagent,…

  2. Fast, high temperature and thermolabile GC--MS in supersonic molecular beams

    Science.gov (United States)

    Dagan, Shai; Amirav, Aviv

    1994-05-01

    This work describes and evaluates the coupling of a fast gas chromatograph (GC) based on a short column and high carrier gas flow rate to a supersonic molecular beam mass spectrometer (MS). A 50 cm long megabore column serves for fast GC separation and connects the injector to the supersonic nozzle source. Sampling is achieved with a conventional syringe based splitless sample injection. The injector contains no septum and is open to the atmosphere. The linear velocity of the carrier gas is controlled by a by-pass (make-up) gas flow introduced after the column and prior to the supersonic nozzle. The supersonic expansion serves as a jet separator and the skimmed supersonic molecular beam (SMB) is highly enriched with the heavier organic molecules. The supersonic molecular beam constituents are ionized either by electron impact (EI) or hyperthermal surface ionization (HSI) and mass analyzed. A 1 s fast GC--MS of four aromatic molecules in methanol is demonstrated and some fundamental aspects of fast GC--MS with time limit constraints are outlined. The flow control (programming) of the speed of analysis is shown and the analysis of thermolabile and relatively non-volatile molecules is demonstrated and discussed. The tail-free, fast GC--MS of several mixtures is shown and peak tailing of caffeine is compared with that of conventional GC--MS. The improvement of the peak shapes with the SMB--MS is analyzed with the respect to the elimination of thermal vacuum chamber background. The extrapolated minimum detected amount was about 400 ag of anthracence-d10, with an elution time which was shorter than 2s. Repetitive injections could be performed within less than 10 s. The fast GC--MS in SMB seems to be ideal for fast target compound analysis even in real world, complex mixtures. The few seconds GC--MS separation and quantification of lead (as tetraethyllead) in gasoline, caffeine in coffee, and codeine in a drug is demonstrated. Controlled HSI selectivity is demonstrated in

  3. 尿中MDMA和MDA的三氟乙酰化-GC/MS/MS分析法%Determination of MDA and MDMA by TFA Derivatization-GC/MS/MS

    Institute of Scientific and Technical Information of China (English)

    于晓娟; 李国平

    2009-01-01

    建立了尿中MDMA和MDA的、用环己烷提取的、三氟乙酸酐衍生化的、GC/MS/MS检测的分析方法.方法操作简便快速,检测MDMA最灵敏的检出限为4ng/mL,检测MDA最灵敏的检出限为2.0ng/mI.方法的回收率为73%-94%,具有较好的线性关系.

  4. Technical Note: Fast two-dimensional GC-MS with thermal extraction for anhydro-sugars in fine aerosols

    Science.gov (United States)

    A fast two-dimensional gas chromatography (GC-MS) method that uses heart-cutting and thermal extraction (TE) and requires no chemical derivatization is developed for the determination of anhydro-sugars in fine aerosols. Evaluation of the TE-GC-GC-MS method shows high average rela...

  5. Semi-automated non-target processing in GC × GC-MS metabolomics analysis: Applicability for biomedical studies

    NARCIS (Netherlands)

    Koek, M.M.; Kloet, F.M. van der; Kleemann, R.; Kooistra, T.; Verheij, E.R.; Hankemeier, T.

    2011-01-01

    Due to the complexity of typical metabolomics samples and the many steps required to obtain quantitative data in GC × GC-MS consisting of deconvolution, peak picking, peak merging, and integration, the unbiased non-target quantification of GC × GC-MS data still poses a major challenge in metabolomic

  6. GC/MS technique and AMDIS software application in identification of hydrophobic compounds of grasshoppers' abdominal secretion (Chorthippus spp.).

    Science.gov (United States)

    Buszewska-Forajta, Magdalena; Bujak, Renata; Yumba-Mpanga, Arlette; Siluk, Danuta; Kaliszan, Roman

    2015-01-01

    The automated mass spectral deconvolution and identification system (AMDIS) is a modern analytical tool, mostly used as a data processing method in environmental studies. The most attractive feature of that software is a fast, automatic data processing, which includes removal of interferences from the overlapping peaks and purification of the obtained mass spectra. The identification of analytes is based on their retention time and retention index and on comparison of the spectra obtained in GC/MS analysis with the spectra from the library of the National Institute of Standards and Technology (NIST). The main aim of the study reported was to elaborate and test a new data processing method with the use of AMDIS software for identification of lipidomic compounds present in the grasshopper's abdominal secretion. For the first time to the best of our knowledge, we have demonstrated the usage of AMDIS in a lipidomic study concerning a complex insect matrix. The samples processed with AMDIS software were analyzed with the use of GC/MS in order to determine the main fatty components of grasshoppers' abdominal secretion. The purification, concentration and fractionation of compounds present in a complex insect matrix were investigated with the use of liquid-liquid extraction as a pretreatment procedure. Moreover, a double-step derivatization process was carried out in order to obtain more volatile and stable derivatives of polar, non-volatile components of insects' secretion. This process, necessary for GC/MS analysis, was performed with the use of methoxyamine hydrochloride dissolved in pyridine and a mixture of bis-N-O-trimethylsilyl trifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). As a result, we obtained a fast, automatic method based on the use of AMDIS software, which enabled identification of 28 analytes, mainly fatty compounds. Moreover, 10 compounds out of 28 were determined to appear with 100% frequency in the tested samples, namely: seven fatty acids

  7. A Simple Method for Measuring Carbon-13 Fatty Acid Enrichment in the Major Lipid Classes of Microalgae Using GC-MS

    Directory of Open Access Journals (Sweden)

    Sheik Nadeem Elahee Doomun

    2016-11-01

    Full Text Available A simple method for tracing carbon fixation and lipid synthesis in microalgae was developed using a combination of solid-phase extraction (SPE and negative ion chemical ionisation gas chromatography mass spectrometry (NCI-GC-MS. NCI-GC-MS is an extremely sensitive technique that can produce an unfragmented molecular ion making this technique particularly useful for stable isotope enrichment studies. Derivatisation of fatty acids using pentafluorobenzyl bromide (PFBBr allows the coupling of the high separation efficiency of GC and the measurement of unfragmented molecular ions for each of the fatty acids by single quadrupole MS. The key is that isotope spectra can be measured without interference from co-eluting fatty acids or other molecules. Pre-fractionation of lipid extracts by SPE allows the measurement of 13C isotope incorporation into the three main lipid classes (phospholipids, glycolipids, neutral lipids in microalgae thus allowing the study of complex lipid biochemistry using relatively straightforward analytical technology. The high selectivity of GC is necessary as it allows the collection of mass spectra for individual fatty acids, including cis/trans isomers, of the PFB-derivatised fatty acids. The combination of solid-phase extraction and GC-MS enables the accurate determination of 13C incorporation into each lipid pool. Three solvent extraction protocols that are commonly used in lipidomics were also evaluated and are described here with regard to extraction efficiencies for lipid analysis in microalgae.

  8. Microwave-assisted Extraction and GC-MS Analysis of Zanthoxylum Oil from Zanthoxylum bungeanum

    Directory of Open Access Journals (Sweden)

    Xiaoguang Wang

    2015-03-01

    Full Text Available The conditions for microwave-assisted extracting oil from Zanthoxylum bungeanum seeds were studied and its chemical composition was analyzed by GC-MS. The effects of extract medium, microwave power, time and ratio of liquid to solid on extraction yield of Zanthoxylum bungeanum oil were investigated, using an orthogonal array design. The experimental results showed that using petroleum ether as extract medium, microwave power 350 w, solid-to-solvent ratio 1:5 (g/mL, 60 sec, can obtained 7.85% of Zanthoxylum bungeanum oil. Thirty-three substances in Zanthoxylum bungeanum oil were authenticated by GC-MS, of which 33 were identified for the first time and its chemical composition was analyzed. Accounting for 97.82% of the total volatile compounds.

  9. Analysis of Valproic Acid, Salicylic Acid and Ibuprofen in Whole Blood by GC-MS.

    Science.gov (United States)

    Stephenson, Jon B; Flater, Melanie L; Bain, Lisa T

    2016-10-01

    The Georgia Bureau of Investigation utilized a silylation method of analysis for low molecular weight carboxylic acids in the past. Due to the negative impact such derivatizations can have on gas chromatography-mass spectrometry (GC-MS) systems an alternative means of analysis was investigated. The described method is a whole blood solid phase extraction of valproic acid, salicylic acid and ibuprofen utilizing butylation for sensitivity and improved chromatography by GC-MS. The method produced a limit of detection and limit of quantitation at 1 mg/L for valproic acid, 2 mg/L for salicylic acid and 0.25 mg/L for ibuprofen. The variability based upon the middle of the calibration curve estimated to be 7% for valproic acid, 8% for salicylic acid and 11% for ibuprofen established upon a 95% confidence interval, with the highest percent coefficient of variation being 5.3% for ibuprofen.

  10. Preliminary phytochemical screening, Antibacterial potential and GC-MS analysis of two medicinal plant extracts.

    Science.gov (United States)

    Vijayaram, Seerangaraj; Kannan, Suruli; Saravanan, Konda Mani; Vasantharaj, Seerangaraj; Sathiyavimal, Selvam; P, Palanisamy Senthilkumar

    2016-05-01

    The presence study was aimed to catalyze the primary metabolites and their confirmation by using GC-MS analysis and antibacterial potential of leaf extract of two important medicinal plant viz., Eucalyptus and Azadirachta indica. The antibacterial potential of the methanol leaf extract of the studied species was tested against Escherichia coli, Pseudomonas aeruginosa, Klebsiellap neumoniae, Streptococcus pyogens, Staphylococcus aureus using by agar well diffusion method. The higher zone of inhibition (16mm) was observed against the bacterium Pseudomonas aeruginosa at 100μl concentration of methanol leaf extract. Preliminary phytochemical analysis of studied species shows that presence of phytochemical compounds like steroids, phenolic compounds and flavonoids. GC-MS analysis confirms the occurrence of 20 different compounds in the methanol leaf extract of the both studied species.

  11. GC-MS and spectrophotometric analysis of biodegradation of new disazo dye by Trametes versicolor.

    Science.gov (United States)

    Akdogan, H Ardag; Demircali, A; Aydemir, C; Pazarlioglu, N; Karci, F

    2011-01-01

    In this study; sub-tropical white rot fungi, Trametes versicolor was investigated for its ability to degrade 4-(3'-methyl-4'-(4"-nitrophenyl)azo- 1'H-pyrazol-5'-ylazo)-3-methyl- H-pyrazol-5-on in the mediums containing glucose and different concentrations of degrade dye in batch systems. This dye was synthetized at Pamukkale Universtiy of Organic Chemistry research laboratory. Samples were collected on 10 days, and was detected by Shimadzu UV-1600A spectrophotometry. Decolorization study showed that this disazo dye was removed by more than 70% in 10 days. Laccase enzyme activity was detected in samples and then last sample was analyzed by GC-MS. Metabolites weren't showed in GC-MS result. It was concluded that T. versicolor could achieve the biodegradation of this new disazo dye.

  12. Phytochemical investigation GC-MS analysis and in vitro antimicrobial activity of Coleus forskohlii

    Directory of Open Access Journals (Sweden)

    Krishnamoorthy Rajkumar

    2015-12-01

    Full Text Available The aim of this study was to investigate the phytochemical constituents, gas chromatography-mass spectrometry (GC-MS analysis and antimicrobial activity of Coleus forskohlii. The different solvents such as ethanol, chloroform, acetone and aqueous extracts were identified pharmacologically as important bioactive compounds and their antimicrobial properties were studied. In the phytochemical investigation almost all the ethanol extract of leaf, stem and root having secondary metabolites like alkaloids, flavonoids, tannins, saponins, terpenoids, and steroids. The active constituents of the ethanol extract of C. forskohlii root was studied by GC-MS analysis. According to the antimicrobial results ethanol extract of C. froshkolii root showed highest antibacterial activity compared with stem and leaf. The highest antimicrobial activity was observed against Klebsiella pneumonia (19 mm and Candida albicans (16 mm in ethanol extract of root. Among the above extracts of leaf, stem and root, ethanol extract of root having antimicrobial activities due to the presence of phytoconstituents.

  13. First detection of an NSAID, flunixin, in sheep's wool using GC-MS.

    Science.gov (United States)

    Richards, Ngaio; Hall, Sarah; Scott, Karen; Harrison, Nancy

    2011-05-01

    Exposure to the nonsteroidal anti-inflammatory drug (NSAID) diclofenac resulted in the near extinction of three species of Gyps vultures on the Indian subcontinent. Other NSAIDs present in the environment, including flunixin, may pose a similar risk. In the course of a study to determine the feasibility of detecting NSAIDs in keratinous matrices (i.e., hair, nails and feathers) using GC-MS, wool opportunistically collected from a sheep treated with flunixin was analysed for residues. Flunixin was detected qualitatively in external wool wash and extract samples. While residues of veterinary agents and pesticides have previously been found in sheep's wool, our preliminary investigation provides the first instance of an NSAID being detected in this matrix. Here we provide the sample preparation methods and GC-MS parameters used to enable further refinement as part of ongoing conservation and consumer quality control measures.

  14. Identification of the main phenolic compounds in wood of Ceratonia siliqua by GC-MS.

    Science.gov (United States)

    Balaban, Mualla

    2004-01-01

    The tannin composition of wood of Ceratonia siliqua (carob) was studied using GC-MS and classical chemical assays. Aqueous methanolic extracts of carob heartwood and sapwood were fractionated using organic solvents of increasing polarity, and GC-MS analyses were performed before and after hydrolysis. Prior to hydrolysis, gallic acid, catechin and its derivatives, methyl inositol and chalcone were determined as the major compounds found in the free form. Aqueous fractions of both wood types were hydrolysed with hydrochloric acid in methanol and extracted with organic solvents and water. These fractions were rich in methyl inositol, gallic acid, glucose and other monosaccharides. The results show that carob wood contains predominantly gallotannins and proanthocyanidins. The technique employed is shown to be a valuable tool and an alternative method to HPLC determination of hydrolysable tannin composition.

  15. [Determination of diphenyl and o-phenylphenol in agricultural products by GC/MS].

    Science.gov (United States)

    Takahashi, Kunihiko; Horie, Masakazu; Hirose, Yoshihumi

    2008-01-01

    A simple determination method of diphenyl (DP) and o-phenylphenol (OPP) in agricultural products by GC/MS was examined. DP and OPP were extracted with ethyl acetate in the presence of anh. sodium sulfate. After addition of n-butanol, the extract solution was concentrated. Clean-up was achieved by shaking with graphitized bulk carbon (Supelclean ENVI-Carb). Addition of polyethylene glycol sharpened the OPP peak on GC/MS analysis. The recoveries from 9 kinds of agricultural products spiked at 0.01 and 0.5 microg/g each were mostly in the range of 70 to 120%, except for 50% recovery of OPP from barley spiked at 0.01 microg/g. The quantification limits (S/N > or =10) of DP and OPP were 0.0013 and 0.005 microg/g (0.0025 and 0.01 microg/g in barley and soybean), respectively.

  16. Methanol ice VUV photoprocessing: GC-MS analysis of volatile organic compounds

    Science.gov (United States)

    Abou Mrad, Ninette; Duvernay, Fabrice; Chiavassa, Thierry; Danger, Grégoire

    2016-05-01

    Next to water, methanol is one of the most abundant molecules in astrophysical ices. A new experimental approach is presented here for the direct monitoring via gas chromatography coupled to mass spectrometry (GC-MS) of a sublimating photoprocessed pure methanol ice. Unprecedentedly, in a same analysis, compelling evidences for the formation of 33 volatile organic compounds are provided. The latter are C1-C6 products including alcohols, aldehydes, ketones, esters, ethers and carboxylic acids. Few C3 and all C4 detected compounds have been identified for the first time. Tentative detections of few C5 and C6 compounds are also presented. GC-MS allows for the first time the direct quantification of C2-C4 photoproducts and shows that their abundances decrease with the increase of their carbon chain length. These qualitative and quantitative measurements provide important complementary results to previous experiments, and present interesting similarities with observations of sources rich in methanol.

  17. Preliminary Phytochemical Screening and GC- MS Profiling of Ethanolic Flower Extract of Calotropis gigantea Linn. (Apocyanaceae

    Directory of Open Access Journals (Sweden)

    R. Dhivya

    2013-09-01

    Full Text Available Calotropis gigantea Linn is popularly known as the swallow-wort or milkweed and is used as one of the most important drug in Traditional System of Medicine to treat various ailments. The aim of this study is to screen the phytochemicals present in the ethanolic flower extract of Calotropis gigantea and further analysis of the components present in it by GC-MS analysis. Ten grams of flower power was sequentially extracted by ethanol. The results showed the presence of phytochemical compounds of alkaloids, tannins, phenol, flavanoids, sterols, antraquinones, proteins and quinones in the flower extract. The GC-MS analysis of the ethanolic extract revealed the presence of 14 major compounds. This study forms a basis for the biological characterization and importance of the compounds identified and creates a platform to screen many bioactive components to treat many diseases.

  18. GC-MS analysis of off-odor volatiles from irradiated pork

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The main compounds of off-odor volatiles from irradiated refrigerated vacuum-packaged pork were analyzed by gas chromatograph/mass spectrometer (GC-MS). The analytical results showed that the main compounds of off-odor volatiles were dimethyl disulfide, dimethyl sulfide, dimethyl trisulfide, S-methyl thioacetate, and methanethiol. It was proved that the off-odor volatile came from irradiated S-containing amino acid and thiamin.

  19. Outdoor and indoor benzene evaluation by GC-FID and GC-MS/MS

    OpenAIRE

    José A. Sousa; Domingues, Valentina F.; Rosas, Mónica S.; Ribeiro, Susana; Alvim-Ferraz, Maria da Conceição M.

    2011-01-01

    The evaluation of benzene in different environments such as indoor (with and without tobacco smoke), a city area, countryside, gas stations and near exhaust pipes from cars running on different types of fuels was performed. The samples were analyzed using gas chromatography (GC) with flame ionization detection (FID) and tandem mass spectrometric detection (MS/MS) (to confirm the identification of benzene in the air samples). Operating conditions for the GC-MS analysis were optimized ...

  20. Identification and determination of (+)-sesamin in Semen Cuscutae by capillary GC and GC-MS

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    (+)-Sesamin was found in Semen Cuscutae for the first time. A rapid and simple approach for the analysis of (+)-sesamin in different sources of Semen Cuscutae is proposed, which used GC-FID for the determination of (+)-sesamin and GC-MS for its identification. The result suggested that this approach could be used to identify Semen Cuscutae from various sources based on the different content of (+)-sesamin in them.

  1. GC-MS Characterisation of Sapogenins from Sisal Waste and a Method to Isolate Pure Hecogenin

    Directory of Open Access Journals (Sweden)

    Jener David G. Santos

    2014-01-01

    Full Text Available Five steroidal sapogenins (tigogenin, neotigogenina, hecogenin, gloriogenin, and dehydrohecogenin were characterised by gas chromatography coupled with mass spectrometry (GC-MS from a hydrolysed extract of sisal waste. In addition, pure hecogenin, an important raw material for the pharmaceutical industry, was obtained from this waste by selective liquid-liquid extraction of saponins with only hecogenin as aglycone, followed by acid hydrolysis. The yield of pure hecogenin was 460 mg.Kg-1 of sisal waste.

  2. Phytochemical Analysis and GC-MS profiling in the leaves of Sauropus Androgynus (l) MERR

    OpenAIRE

    Senthamarai Selvi. V; Anusha Basker

    2012-01-01

    In the present the phytochemical analysis of Sauropus androgynus was carried out. Phytochemical analysis of the leaves of this plant is reported for the first time. The leaves indicated the presence of proteins, resins, steroids, tannins, glycosides, reducing sugar, carbohydrates, saponins, sterols, terpenoids, acidic compounds, cardiac glycosides, catechol, phenols, alkaloids, flavonoids. In the GC-MS analysis the Sauropus androgynus extract result shows the presence of bioactive compounds w...

  3. In vitro characterization of borneol metabolites by GC-MS upon incubation with rat liver microsomes.

    Science.gov (United States)

    Zhang, Rong; Liu, Chang-hui; Huang, Tian-lai; Wang, Ning-sheng; Mi, Sui-qing

    2008-01-01

    The metabolism of borneol is studied by the analysis of incubations of in vitro-prepared rat liver microsomes. A sensitive gas chromatography (GC)-mass spectrometry (MS) method is developed for the identification of borneol and its metabolites. Four novel metabolites, which have not previously been reported, are isolated and confirmed by comparison of the GC-MS method. The biotransformation pathway of borneol in rat liver microsomes is proposed based on the in vitro results.

  4. THE STUDY OF PHTHALATES MIGRATION IN WINE PRODUCTS BY GC-MS METHOD

    Directory of Open Access Journals (Sweden)

    Gh. Duca

    2012-12-01

    Full Text Available A number of studies have shown phthalates’ potential impact on human health due to their carcinogenic and endocrinedisrupting effects. More than 2000 analyses for determination of phthalates’ rests in alcoholic beverages were done in the laboratory of National Center for Quality Testing of the Alcoholic Beverages (Republic of Moldova using modern method of analysis like GC-MS. This article is an extended abstract of a communication presented at the Conference Ecological Chemistry 2012

  5. GC-MS ANALYSIS OF THE FATTY ACID METHYL ESTER IN JAPANESE QUAIL FAT

    Directory of Open Access Journals (Sweden)

    Ion Dragalin

    2015-12-01

    Full Text Available The accumulated as production waste fat from Faraon quail breeds has been investigated for the first time by using GC-MS technique, preventively converting it via methanolysis to fatty acid methyl esters. The test results, regarding the content of unsaturated fatty acids having a favorable to human body cis-configuration (77.8%, confirm their nutritional value and the possibility of using this fat in cosmetic, pharmaceutical and food industries.

  6. Efficiency of GC-MS method in detection of beeswax adulterated with paraffin

    OpenAIRE

    Waś Ewa; Szczęsna Teresa; Rybak-Chmielewska Helena

    2016-01-01

    The efficiency of the gas chromatography - mass detector (GC-MS) technique for the detection of beeswax adulterated with paraffin, was evaluated. For this purpose, beeswax samples with paraffin additions (3, 5, 10, 30, 50%) were analysed. Since not enough is known about paraffin compositions, and since it is difficult to detect paraffin in beeswax, the aim of our research was also to compare the hydrocarbon composition of different types of paraffin. The analysis showed that the types of para...

  7. Preliminary Phytochemical Screening and GC- MS Profiling of Ethanolic Flower Extract of Calotropis gigantea Linn. (Apocyanaceae)

    OpenAIRE

    R.Dhivya; K. Manimegalai

    2013-01-01

    Calotropis gigantea Linn is popularly known as the swallow-wort or milkweed and is used as one of the most important drug in Traditional System of Medicine to treat various ailments. The aim of this study is to screen the phytochemicals present in the ethanolic flower extract of Calotropis gigantea and further analysis of the components present in it by GC-MS analysis. Ten grams of flower power was sequentially extracted by ethanol. The results showed the presence of phytochemical compounds ...

  8. Simultaneous analysis of synthetic cannabinoids in the materials seized during drug trafficking using GC-MS.

    Science.gov (United States)

    Choi, Hyeyoung; Heo, Sewoong; Choe, Sanggil; Yang, Wonkyung; Park, Yuran; Kim, Eunmi; Chung, Heesun; Lee, Jaesin

    2013-05-01

    A rapid and simple gas chromatography-mass spectrometry (GC-MS) method was developed and validated to identify and quantify synthetic cannabinoids in the materials seized during drug trafficking. Accuracy and reproducibility of the method were improved by using deuterated JWH-018 and JWH-073 as internal standards. Validation results of the GC-MS method showed that it was suitable for simultaneous qualitative and quantitative analyses of synthetic cannabinoids, and we analyzed synthetic cannabinoids in seized materials using the validated GC-MS method. As a result of the analysis, ten species of synthetic cannabinoids were identified in dried leaves (n = 40), bulk powders (n = 6), and tablets (n = 14) seized in Korea during 2009-2012, as a single ingredient or as a mixture with other active co-ingredients. JWH-018 and JWH-073 were the most frequently identified compounds in the seized materials. Synthetic cannabinoids in the dried leaves showed broad concentration ranges, which may cause unexpected toxicity to abusers. The bulk powders were considered as raw materials used to prepare legal highs, and they contained single ingredient of JWH-073, JWH-019, or JWH-250 with the purity over 70 %. In contrast, JWH-018 and JWH-073 contents in the tablets were 7.1-13.8 and 3.0-10.2 mg/g, respectively. Relatively low contents in the tablets suggest that the synthetic cannabinoids may have been added to the tablets as supplements to other active co-ingredients.

  9. GC-MS analysis of allergens in plant oils meant to cosmetics

    Directory of Open Access Journals (Sweden)

    Kaloustian Jacques

    2007-03-01

    Full Text Available Cutaneous allergy occurs mainly as a result of the use of domestic products and cosmetics. Some fragrances, present in these products, may contain compounds that are responsible for allergy (allergens. The European Council offered a Directive limiting the level of 26 allergens found in cosmetics. GC-MS technique was used to determine the retention times of 25 allergens, determine detection and quantification limits and make calibration with standard solution of each allergen in concentrations ranging from 10 to 200 mgL–1 (21 allergens and 50 to 200 mgL–1 (4 allergens. Quantification was performed by the use of 2 internal standards (tetradecane and hexadecane. Seven oils issued from plants were studied by GC-MS. For all of them, the concentration of potential allergens was lower than their minimum detectable level. The alcoholic solution of extracts issued from different samples of oil did not demonstrate the presence of any quantifiable allergen, even when was concentrated 25 times. GC-MS could be a useful technique in the identification and, if necessary, quantification of allergen in ingredients meant to cosmetics.

  10. Comparison of Two Species of Notopterygium by GC-MS and HPLC

    Directory of Open Access Journals (Sweden)

    Yaping Wang

    2015-03-01

    Full Text Available Notopterygii Rhizoma et Radix (Qianghuo, including Notopterygium incisum Ting ex H. T. Chang (NI and Notopterygium franchetii H. de Boiss (NF, is an important traditional Chinese medicine. Of these two plants, NI, is more commonly used and has a much higher price in the marketplace. To compare these two plants, a combination of gas chromatography-mass spectrometry (GC-MS and high performance liquid chromatography (HPLC was carried out, thus obtaining an overall characterization for both volatile and none-volatile compounds. Combined with hierarchical cluster analysis (HCA and principal component analysis, GC-MS was successfully applied to distinguish NF and NI. The chemical constitutes of volatile oil in NI and NF were firstly compared in detail, and 1R-alpha-pinene, beta-pinene and 4-isopropyl-1-methyl-1,4-cyclohexadiene had great contribution to the discrimination. Fingerprints of 14 batches of Qinghuo samples were also established based on HPLC, and an obvious difference was found between the two species. The chromatographic fingerprints were further analyzed by similarity analysis and HCA. The present study is the first reported evaluation of two origins of Notopterygii Rhizoma et Radix by GC-MS and HPLC, which will facilitate quality control and its clinical application.

  11. Identification of volatile degradants in formulations containing sesame oil using SPME/GC/MS.

    Science.gov (United States)

    Chen, Wencan; Zhou, Pengzu; Wong-Moon, Kirby C; Cauchon, Nina S

    2007-06-28

    Solid-phase microextraction (SPME), in combination with gas chromatography/mass spectrometry (GC/MS), was used to identify an unknown degradant observed during stability studies of a pharmaceutical formulation containing sesame oil. SPME is a solvent-less, rapid, sensitive, and inexpensive extraction method that minimizes sample preparation. SPME combined with GC is a widely used technique in certain fields, such as food, environmental analysis, forensics, and consumer products, but has only rarely been used for the analysis of pharmaceutical formulations. Hexanal, octanal, 2-octenal, 2-decenal, 2-undecenal, and 2,4-decadienal can be detected and identified by GC/MS, but they cannot be detected by LC/MS due to their volatility and low ionization efficiency under atmospheric pressure ionization conditions. Combining the MS data from the GC/MS with LC/DAD data resulted in the identification of the unknown degradant in the formulation as 2,4-decadienal. The presence of this and other aldehydes was attributed to the oxidative degradation of the unsaturated fatty-acid component in vegetable oils.

  12. Automated dynamic headspace/GC-MS analyses affect the repeatability of volatiles in irradiated Turkey.

    Science.gov (United States)

    Nam, Ki-Chang; Cordray, Joseph; Ahn, Dong U

    2004-03-24

    Although a dynamic headspace/gas chromatography-mass spectrometry (DH/GC-MS) method is an effective tool for determining volatiles of irradiated turkey meat, the profile of volatiles may be changeable depending upon the availability of oxygen in the sample vial and sample holding time before purge. The objective of this study was to evaluate the effects of helium flushing and sample holding time before purge on the volatiles profiles of irradiated raw and cooked turkey breast meat. Vacuum-packaged turkey breasts were irradiated at 2.5 kGy, and the volatiles of irradiated raw and cooked samples were analyzed using a DH/GC-MS with different holding times up to 280 min. The amounts of dimethyl disulfide and dimethyl trisulfide decreased as sample holding time in an autosampler (4 degrees C) before purge increased, whereas those of aldehdyes increased as holding time increased due to lipid oxidation. Helium flush of sample vials before sample loading on an autosampler retarded lipid oxidation and minimized the changes of sulfur volatiles in raw meat but was not enough to prevent oxidative changes in cooked meat. Although DH/GC-MS is a convenient method for automatic analysis of volatiles in meat samples, the number of samples that can be loaded in an autosampler at a time should be limited within the range that can permit reasonable repeatabilities for target volatile compounds.

  13. Performance characteristics of cryofocusing GC/MS system at BWXT Pantex Plant.

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Jason R.; Banet, Judith F.; Ithaca, Jerry (BWXT Pantex Plant, Amarillo, TX); Thornberg, Steven Michael; Woods, Lorelei (BWXT Pantex Plant, Amarillo, TX)

    2006-07-01

    Ensuring the reliability of all components within a weapon system becomes increasingly important as the stockpile ages. One of the most noteworthy surveillance techniques designed to circumvent (or take place alongside) traditional D&I operations is to collect a sample of gas from within the internal atmosphere of a particular region in a weapon. While a wealth of information about the weapon may be encoded within the composition of its gas sample, our access to that information is only as good as the method used to analyze the sample. It has been shown that cryofocusing-GC/MS offers advantages in terms of sensitivity, ease of sample collection, and robustness of the equipment/hardware used. Attention is therefore focused on qualifying a cryo-GC/MS system for routine stockpile surveillance operations at Pantex. A series of tests were performed on this instrument to characterize the linearity and repeatability of its response using two different standard gas mixes (ozone precursor and TO-14) at various concentrations. This paper outlines the methods used and the results of these tests in order to establish a baseline by which to compare future cryo-GC/MS analyses. A summary of the results is shown.

  14. First detection of an NSAID, flunixin, in sheep's wool using GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Richards, Ngaio, E-mail: ngaio.richards@anglia.ac.uk [Life Sciences, Anglia Ruskin University, East Road, Cambridge, CB1 1PT (United Kingdom); Hall, Sarah [Life Sciences, Anglia Ruskin University, East Road, Cambridge, CB1 1PT (United Kingdom); Scott, Karen [Forensic Medicine and Science, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Harrison, Nancy [Life Sciences, Anglia Ruskin University, East Road, Cambridge, CB1 1PT (United Kingdom)

    2011-05-15

    Exposure to the nonsteroidal anti-inflammatory drug (NSAID) diclofenac resulted in the near extinction of three species of Gyps vultures on the Indian subcontinent. Other NSAIDs present in the environment, including flunixin, may pose a similar risk. In the course of a study to determine the feasibility of detecting NSAIDs in keratinous matrices (i.e., hair, nails and feathers) using GC-MS, wool opportunistically collected from a sheep treated with flunixin was analysed for residues. Flunixin was detected qualitatively in external wool wash and extract samples. While residues of veterinary agents and pesticides have previously been found in sheep's wool, our preliminary investigation provides the first instance of an NSAID being detected in this matrix. Here we provide the sample preparation methods and GC-MS parameters used to enable further refinement as part of ongoing conservation and consumer quality control measures. - Highlights: > In this study we qualitatively detected the NSAID flunixin in sheep's wool using GC-MS. > Potential applications of this technique to the conservation of avian scavengers are outlined. > The quantitative and confirmatory steps required to fully validate the method are also provided. - This is the first time that an NSAID has been investigated or detected in sheep's wool. As such, it details a novel exposure pathway for scavenging species in the environment and offers a potential tool for future monitoring effort in vulture conservation.

  15. Multiresidue pesticide analysis of ginseng powders using acetonitrile- or acetone-based extraction, solid-phase extraction cleanup, and gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS).

    Science.gov (United States)

    Wong, Jon W; Zhang, Kai; Tech, Katherine; Hayward, Douglas G; Krynitsky, Alexander J; Cassias, Irene; Schenck, Frank J; Banerjee, Kaushik; Dasgupta, Soma; Brown, Don

    2010-05-26

    A multiresidue method for the analysis of 168 pesticides in dried powdered ginseng has been developed using acetonitrile or acetone mixture (acetone/cyclohexane/ethyl acetate, 2:1:1 v/v/v) extraction, solid-phase extraction (SPE) cleanup with octyl-bonded silica (C(8)), graphitized carbon black/primary-secondary amine (GCB/PSA) sorbents and toluene, and capillary gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS). The geometric mean limits of quantitation (LOQs) were 53 and 6 microg/kg for the acetonitrile extraction and 48 and 7 microg/kg for the acetone-based extraction for GC-MS/SIM and GC-MS/MS, respectively. Mean percent recoveries and standard deviations from the ginseng fortified at 25, 100, and 500 microg/kg using GC-MS/SIM were 87 +/- 10, 88 +/- 8, and 86 +/- 10% from acetonitrile extracts and 88 +/- 13, 88 +/- 12, and 88 +/- 14% from acetone mixture extracts, respectively. The mean percent recoveries from the ginseng at the 25, 100, and 500 microg/kg levels using GC-MS/MS were 83 +/- 19, 90 +/- 13, and 89 +/- 11% from acetonitrile extracts and 98 +/- 20, 91 +/- 13, and 88 +/- 14% from acetone extracts, respectively. Twelve dried ginseng products were found to contain one or more of the following pesticides and their metabolites: BHCs (benzene hexachlorides, alpha-, beta-, gamma-, and delta-), chlorothalonil, chlorpyrifos, DDT (dichlorodiphenyl trichloroethane), dacthal, diazinon, iprodione, quintozene, and procymidone ranging from 4000 microg/kg. No significant differences were found between the two extraction solvents, and GC-MS/MS was found to be more specific and sensitive than GC-MS/SIM. The procedures described were shown to be effective in screening, identifying, confirming, and quantitating pesticides in commercial ginseng products.

  16. Advanced Surface Technology

    DEFF Research Database (Denmark)

    Møller, Per; Nielsen, Lars Pleht

    This new significant book on advanced modern surface technology in all its variations, is aimed at both teaching at engineering schools and practical application in industry. The work covers all the significant aspects of modern surface technology and also describes how new advanced techniques make......, nitriding, carbonitriding, and many other lesser-known thermochemical processes used for solving technological problems. The book is richly illustrated with pictures and figures showing how the technology creates new innovative solutions for industry and how surfaces are becoming integral to the function...

  17. Sustainable advanced construction technologies

    CSIR Research Space (South Africa)

    Kuchena, JC

    2009-11-01

    Full Text Available Advanced Construction Technologies (ACTs) are set to become the sustainable mainstay of the construction industry due to the demand for innovative housing solutions. Like most emerging economies, South Africa from a historical perspective and global...

  18. Advanced GPS Technologies (AGT)

    Science.gov (United States)

    2015-05-01

    V Air Force Research Laboratory ••• Advanced GPS Technologies (AGT) Integrity *Service *Excellence 1 May 2015 Kevin Slimak Program Manager...2015 2. REPORT TYPE 3. DATES COVERED 00-00-2015 to 00-00-2015 4. TITLE AND SUBTITLE Advanced GPS Technologies (AGT) 5a. CONTRACT NUMBER 5b...DISTRIBUTION/AVAILABILITY STATEMENT Approved for public release; distribution unlimited 13. SUPPLEMENTARY NOTES Presented at the GPS Partnership

  19. The role of GC-MS/MS with triple quadrupole in pesticide residue analysis in food and the environment

    OpenAIRE

    Hernández Hernández, Félix; Cervera Vidal, María Inés; Portolés Nicolau, Tania; Beltrán Arandes, Joaquim; Pitarch Arquimbau, María Elena

    2013-01-01

    Gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) using a triple quadrupole (QqQ) analyzer has in the last few years become a powerful technique for the determination of pesticide residues due to its robustness, and excellent sensitivity and selectivity. This review gives an overview of currently published applications of GC-MS/MS with a QqQ analyzer for pesticide residue analysis of different food and environmental sample matrices. This technique allows the reliable quantific...

  20. Use of On-Site GC/MS Analysis to Distinguish between Vapor Intrusion and Indoor Sources of VOC

    Science.gov (United States)

    2013-12-01

    ER-201119) Use of On-Site GC/MS Analysis to Distinguish between Vapor Intrusion and Indoor Sources of VOC December 2013 This document...SUBTITLE Use of On-Site GC/MS Analysis to Distinguish between Vapor Intrusion and Indoor Sources of VOC 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c...ANALYSIS TO EVALUATE VAPOR INTRUSION ........................ 21 6.3.1 Site-by-Site Analysis of Results: Building VI Classifications ................. 21

  1. Development of a fast GC/MS-system for airborne measurements of Volatile Organic Compounds

    Science.gov (United States)

    Wenk, Ann-Kathrin; Wegener, Robert; Hofzumahaus, Andreas; Wahner, Andreas

    2010-05-01

    Volatile Organic Compounds (VOC) determine the radical chemistry of the atmosphere. They can serve both as sources, or sinks for radicals. Mass spectrometry linked to gas chromatography (GC/MS) is a widespread technique in environmental analysis since it can be used to separate and analyze any compound which can be evaporated and pass the analytical column with very high precision and a good sensitivity. The use of special chromatographic phases and long capillary columns enables the quantification of a wide range of compounds with little interference from other sample constituents. An in situ GC/MS consists in principle of three compartments, 1) a preconcentration unit where the sample is extracted from the air, focussed onto a small volume and volatilized, 2) a chromatographic system where the analytes are separated on the analytical column and 3) a mass spectrometer where the compounds are ionized and detected. VOC have to be preconcentrated due to their low concentration level and in order to get enough sensitivity for analysis. The aim of this project was to develop an in situ GC/MS system to analyze volatile Nonmethane Hydrocarbons (NMHC) and Oxygenated Volatile Organic Compounds (OVOC) for the High Altitude and LOng Range Research Aircraft (HALO). In contrast to other analytical instruments a GC/MS works discontinuously. The preconcentration unit is either heated up when the compounds are volatilized or cooled down when substances are adsorbed. The same is true for the GC oven. It is heated up when the compounds are separated or it is cooled down to be ready for the next injection. On a system with a single GC oven, these processes will inevitably lengthen the whole analytical procedure. To speed up the analytical process the GC/MS system described here was equipped with two GC ovens and two adsorption units. While the components are adsorbed in one adsorption unit, in the other unit the components are desorbed and transferred to the GC unit. The second GC

  2. Analysis Natural Volatile Constituents of Nothapodytes Pittosporoides with SPME-GC-MS%SPME-GC-MS 分析马比木中挥发性成分

    Institute of Scientific and Technical Information of China (English)

    杨艳; 柳小兰; 王道平; 李齐激; 杨小生; 高渐飞; 张凡; 曹佩雪; 张明; 周美

    2016-01-01

    Nothapodytes pittosporoides containing camptothe-cin and its methyl derivatives which are im-portant anti-cancer active ingredients was extensively attracted as an alternative to camptotheca acuminate.Nat-ural volatile constituents of Nothapodytes pittosporoides were extracted by using solid-phase microextraction (SPME)and separated and analysed by gas chromatography-mass spectrometry (GC-MS).The relative content of natural volatile constituents for Nothapodytes pittospo-roides was calculated to take area normalization meth-od of chromatographic peak.Through computer retrieval,80 natural volatile constituents of Nothapodytes pit-tosporoides were identified.The main ingredients were 2-methyl Butanal (4.85 1%),2-Methyl-2-butenal (3. 088%),Hexanal (5.780%),2-Furancarboxaldehyde (40.413%),(E)-2-Hexenal (6.099%),3-Hexen-1-ol (2. 739%),(Z)-Hexenol(3.260%),1-Hexanol(1 1.5 14%)and so on.%马比木(Nothapodytes pittosporoides )含有重要的抗癌活性成分喜树碱及其甲基衍生物.利用固相微萃取技术(SPME)提取马比木中的挥发性成分,采用气相色谱-质谱联用(GC-MS)技术对其化学成分进行分离分析,并用色谱峰面积归一化法测定各成分的相对含量.通过计算机检索,鉴定出80个挥发性化学成分,其中主要成分为2-甲基丁醛(4.851%)、2-甲基-2-丁烯醛(3.088%)、己醛(5.780%)、2-呋喃甲醛(40.413%)、(E)-2-己烯醛(6.099%)、3-己烯-1-醇(2.739%)、(Z)-己烯醇(3.260%)、正己醇(11.514%)等.

  3. Technological advances transforming rheumatology

    Science.gov (United States)

    Robinson, William H.; Mao, Rong

    2016-01-01

    Technological advances over the past decade have revolutionized many areas of rheumatology, ranging from diagnosis, prognosis and therapeutic development to the mechanistic understanding of rheumatic diseases. This overview highlights key technological innovations and discusses the major impact that these developments are having on research and clinical practice. PMID:26439404

  4. Advanced Cell Technology, Inc.

    Science.gov (United States)

    Caldwell, William M

    2007-03-01

    Advanced Cell Technology, Inc. (OTCBB: ACTC) is a biotechnology company applying novel human embryonic stem cell technologies in the emerging field of regenerative medicine. We believe that regenerative medicine has the potential to revolutionize the field by enabling scientists to produce human cells of any kind for use in a wide array of therapies.

  5. Advanced Mirror Technology Development

    Science.gov (United States)

    Stahl, H. Philip

    2017-01-01

    The Advanced Mirror Technology Development (AMTD) project matures critical technologies required to enable ultra-stable 4-m-or-larger monolithic or segmented ultraviolet, optical, and infrared (UVOIR) space telescope primary-mirror assemblies for general astrophysics and ultra-high-contrast observations of exoplanets.

  6. A simplified method for the analysis of urinary cotinine by GC-MS

    Directory of Open Access Journals (Sweden)

    Luiz Carlos da Cunha

    2013-04-01

    Full Text Available Cotinine is the major metabolite of nicotine and, being very stable and having a long biological half-life, it can be used as a biomarker for tobacco exposure. The aim of this study was to develop an analytical GC-MS technique to measure levels of cotinine in the urine of active and passive smokers and to compare the results with reference values. The extraction of cotinine to generate the calibration curve was performed by mixing urine (250 µL with 50 µL of a cotinine standard, 50 µL of an internal standard of deuterated cotinine (15 µg∙mL-1 and 50 µL of 10% NH4 OH solution. Next, 2 mL of a mixture of MTBE:dichloromethane:ethyl acetate (30:30:40 by volume was added and the whole was vortexed, then centrifuged at 3000 rpm. Finally, 1.6 mL of the organic layer was evaporated under a stream of dry air at 50 °C. The resulting extract was dissolved in methanol and injected into the GC-MS system. The LOQ and LOD for cotinine were 100 and 20 ng∙mL-1, respectively. The curve was linear over the whole tested range of 100 - 5000 ng∙mL-1 and the method achieved 50% recovery. The intra and inter-day precisions were 1.62 – 7.28% and 0.86 – 2.68%, respectively. Accuracy was determined at three concentrations (low, medium and high, with six replicates (95.24 – 97.67%. The validation of this cotinine assay by GC-MS showed that it exhibited satisfactory limits and the assay could be performed with a one-step liquid-liquid extraction. The technique presented here can thus be used for the quantitation of cotinine levels in the urine of passive and active smokers.

  7. Rapid analysis for 567 pesticides and endocrine disrupters by GC/MS using deconvolution reporting software

    Energy Technology Data Exchange (ETDEWEB)

    Wylie, P.; Szelewski, M.; Meng, Chin-Kai [Agilent Technologies, Wilmington, DE (United States)

    2004-09-15

    More than 700 pesticides are approved for use around the world, many of which are suspected endocrine disrupters. Other pesticides, though no longer used, persist in the environment where they bioaccumulate in the flora and fauna. Analytical methods target only a subset of the possible compounds. The analysis of food and environmental samples for pesticides is usually complicated by the presence of co-extracted natural products. Food or tissue extracts can be exceedingly complex matrices that require several stages of sample cleanup prior to analysis. Even then, it can be difficult to detect trace levels of contaminants in the presence of the remaining matrix. For efficiency, multi-residue methods (MRMs) must be used to analyze for most pesticides. Traditionally, these methods have relied upon gas chromatography (GC) with a constellation of element-selective detectors to locate pesticides in the midst of a variable matrix. GC with mass spectral detection (GC/MS) has been widely used for confirmation of hits. Liquid chromatography (LC) has been used for those compounds that are not amenable to GC. Today, more and more pesticide laboratories are relying upon LC with mass spectral detection (LC/MS) and GC/MS as their primary analytical tools. Still, most MRMs are target compound methods that look for a small subset of the possible pesticides. Any compound not on the target list is likely to be missed by these methods. Using the techniques of retention time locking (RTL) and RTL database searching together with spectral deconvolution, a method has been developed to screen for 567 pesticides and suspected endocrine disrupters in a single GC/MS analysis. Spectral deconvolution helps to identify pesticides even when they co-elute with matrix compounds while RTL helps to eliminate false positives and gives greater confidence in the results.

  8. Identification of natural indigo in historical textiles by GC-MS.

    Science.gov (United States)

    Degani, Laura; Riedo, Chiara; Chiantore, Oscar

    2015-02-01

    The possibility of successfully applying a common GC-MS procedure for identification in one step of all types of dyes from plants of unknown origin and from historical objects is particularly attractive due to the high separation efficiency of the capillary columns, the MS detection sensitivity and the reproducibility of results. In this work, GC-MS analysis, previously and successfully used for the characterization of anthraquinones, flavonoids and tannins from plant extracts and historical samples, has been tested on indigoid dyestuffs. An analytical procedure based on the silylating agent N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) was applied to pure molecules of indigotin and indirubin and to plant extracts of Indigofera tinctoria L. and Isatis tinctoria L. Preliminary tests have been done to establish the chromatographic conditions and the derivatization amounts most suitable for the simultaneous detection of indigoid molecules and of the other natural compounds, such as fatty acids, carboxylic acids and sugars, contained within the plant extracts. In order to assess the capacity and the sensitivity of the analytical procedure in typical archaeometric applications, wool samples dyed in the laboratory with indigo were analysed by mimicking the sample amounts typically available with historical objects. The electron ionization (EI) spectra of the main silylated derivatives of indigoid molecules obtained in this way constitute the necessary data set for the characterization of natural extracts and historical works of art. Subsequently, the procedure has been applied to historical samples for the detection of indigo and of other dyestuffs eventually contained in samples. Additional information, useful for restoration and preservation of works of art, could be also obtained on the nature of stains and smudges present on the sampled textile material. The GC-MS method turns out to be an efficient and fast analytical tool

  9. Correlation of thermal analysis and pyrolysis coupled to GC-MS in the characterization of tacrolimus.

    Science.gov (United States)

    Böer, Tania Maria; Procópio, José Valdilânio Virgulino; Nascimento, Ticiano Gomes do; Macêdo, Rui Oliveira

    2013-01-25

    In recent years, thermal analysis has assumed major role in the pharmaceutical industry because it can be used to evaluate the stability both in the control of raw materials and the finished product, having employment potential in the development and characterization of new products and assessment processes. Tacrolimus (TCR) is a macrolide lactone with potent immunosuppressive activity. The purpose of this study was to characterize tacrolimus raw material using Thermal analysis and Pyrolysis coupled to Gas chromatography-Mass spectrometry (Pyr-GC-MS). It was analyzed four samples of tacrolimus named TCR A, B, C and D. Thermal analysis experiments was performed in Shimadzu equipment, under nitrogen and synthetic air atmosphere in different heating rate. Pyrolysis analysis was conducted in isothermal conditions of 300°C and 400°C coupled to GC-MS, in which the mass spectrometer was operated in scan mode to detect ions in the range of mass of m/z 25-900. The thermal studies by DSC, DTA and DSC-Photovisual showed desolvation process for all tacrolimus raw materials and TG-dynamical demonstrated two pseudo-polymorphic forms (monohydrate and sesquihydrate) of tacrolimus. It was observed good correlation between the stoichiometric mass losses of the TG-dynamical and identification of product ion in Pyr-GC/MS technique. It was possible to correlate the five pyrolytic product ions with the Ozawa kinetic analysis from the thermal decomposition of TG-dynamical. The thermal studies (DSC, DSC-Photovisual, DTA and TG-dynamical) were applied in the thermal characterization of the raw materials of tacrolimus which showed pseudo-polymorphic forms, which must be monitored by pharmaceutical industry, avoiding future problems in pharmaceutical process, chemical stability and bioavailability of the tacrolimus product.

  10. A potential tool for diagnosis of male infertility: Plasma metabolomics based on GC-MS.

    Science.gov (United States)

    Zhou, Xinyi; Wang, Yang; Yun, Yonghuan; Xia, Zian; Lu, Hongmei; Luo, Jiekun; Liang, Yizeng

    2016-01-15

    Male infertility has become an important public health problem worldwide. Nowadays the diagnosis of male infertility frequently depends on the results of semen quality or requires more invasive surgical intervention. Therefore, it is necessary to develop a novel approach for early diagnosis of male infertility. According to the presence or absence of normal sexual function, the male infertility is classified into two phenotypes, erectile dysfunction (ED) and semen abnormalities (SA). The aim of this study was to investigate the GC-MS plasma profiles of infertile male having erectile dysfunction (ED) and having semen abnormalities (SA) and discover the potential biomarkers. The plasma samples from healthy controls (HC) (n=61) and infertility patients with ED (n=26) or with SA (n=44) were analyzed by gas chromatography-mass spectrometry (GC-MS) for discrimination and screening potential biomarkers. The partial least squares-discriminant analysis (PLS-DA) was performed on GC-MS dataset. The results showed that HC could be discriminated from infertile cases having SA (AUC=86.96%, sensitivity=78.69%, specificity=84.09%, accuracy=80.95%) and infertile cases having ED (AUC=94.33%, sensitivity=80.33%, specificity=100%, accuracy=87.36%). Some potential biomarkers were successfully discovered by two commonly used variable selection methods, variable importance on projection (VIP) and original coefficients of PLS-DA (β). 1,5-Anhydro-sorbitol and α-hydroxyisovaleric acid were identified as the potential biomarkers for distinguishing HC from the male infertility patients. Meanwhile, lactate, glutamate and cholesterol were the found to be the important variables to distinguish between patients with erectile dysfunction from those with semen abnormalities. The plasma metabolomics may be developed as a novel approach for fast, noninvasive, and acceptable diagnosis and characterization of male infertility.

  11. GC-MS investigation of Amaryllidaceae alkaloids in Galanthus xvalentinei nothosubsp. subplicatus.

    Science.gov (United States)

    Sarikaya, Buket Bozkurt; Berkov, Strahil; Bastida, Jaume; Kaya, Gulen Irem; Onur, Mustafa Ali; Somer, Nehir Unver

    2013-03-01

    A GC-MS analysis of alkaloids in the aerial parts and bulbs of Galanthus xvalentinei nothosubsp. subplicatus was performed for the first time. Totally, twenty-six alkaloids were identified, of which tazettine and galanthindole were the major ones. Acetylcholinesterase inhibitory activity of the alkaloidal extracts was determined using modified in vitro Ellman's method. Significant anticholinesterase activity was observed in the tested samples (bulbs: IC50 = 21.3 microg/mL, aerial parts: IC50 = 16.3 microg/mL).

  12. GC-MS investigation and acetylcholinesterase inhibitory activity of Galanthus rizehensis.

    Science.gov (United States)

    Sarikaya, Buket Bozkurt; Somer, Nehir Unver; Kaya, Gulen Irem; Onur, Mustafa Ali; Bastida, Jaume; Berkov, Strahil

    2013-01-01

    GC-MS (gas chromatography-mass spectrometry) analyses of alkaloids in the aerial parts and bulbs of Galanthus rizehensis Stern (Amaryllidaceae), collected during two different vegetation periods, was performed. Twenty three alkaloids were identified in four different alkaloid extracts. Acetylcholinesterase (AChE) inhibitory activities of the alkaloid extracts were tested. Both the highest alkaloid diversity and the most potent inhibitory activity (IC50 12.94 microg/ml) were obtained in extracts from the bulbs of G. rizehensis collected during the fruiting period.

  13. [Analysis of essential oil extracted from Lactuca sativa seeds growing in Xinjiang by GC-MS].

    Science.gov (United States)

    Xu, Fang; Wang, Qiang; Haji, Akber Aisa

    2011-12-01

    To analyze the components of essential oil from Lactuca sativa seeds growing in Xinjiang. The components of essential oil from Lactuca sativa seeds were analyzed by gas chromatography-mass spectrometry (GC-MS). 62 components were identified from 71 separated peaks,amounting to total mass fraction 95.07%. The dominant compounds were n-Hexanol (36.31%), n-Hexanal (13.71%), trans-2-Octen-l-ol (8.09%) and 2-n-Pentylfuran (4.41%). The research provides a theoretical basis for the exploitation and use of Lactuca sativa seeds resource.

  14. MDMA毒品简介及GC/MS分析%Determination of MDMA by GC/MS

    Institute of Scientific and Technical Information of China (English)

    张春水; 郑珲; 徐鹏

    2004-01-01

    对一例MDMA毒品案件进行技术检测,采用气质联用技术(GC/MS)准确分析了MDMA片剂中物质成分,检出了MDMA、胡椒素甲醛及咖啡因等成分,并建立了该类毒品检验的快速分析方法,为打击毒品犯罪提供了技术保障.

  15. GC/MS Analysis of Organic Compounds in Hot Water-Extractable Fraction from Shenfu Coal

    Institute of Scientific and Technical Information of China (English)

    LI Bao-min; YUAN Cheng; ZONG Zhi-min; CAO Jing-pei; LIU Guang-feng; WEI Xian-yong

    2007-01-01

    Shenfu Coal was extracted with hot pure water and slurry was isolated. The concentrated benzene-soluble fraction (CBSF) was analyzed with GC/MS and four types of organic compounds (OCs) were detected: HACOCs, DTEs, DMDT and LCAs. The amount of benzyl benzoate which is the most abundant OC was calculated by an internal standard method with an indicated amount of BP. The broken hydrogen bonds and ether bonds were responsible for the extraction of OCs from the coal .DTEs, DMDT and LCAs are essentially insoluble in water, whereas they are soluble, probably owing to intermolecular interaction of OCs with HACOCs.

  16. Analysis of Turkish lignite tar by coupled LC/GC, GC/MS, and capillary SFC

    Energy Technology Data Exchange (ETDEWEB)

    Davies, I.L.; Raynor, M.W.; Urwin, D.J.; Bartle, K.D.; Tolay, M.; Ekinci, E.; Schwartz, H.E.

    1988-11-01

    This work describes the analysis of a pyrolysis product of a lignite sample obtained from the Turkish Goynuk reserve. The aliphatic, aromatic and polar compounds present in the tar are separated and identified by various chromatographic techniques: capillary gas chromatography/mass spectrometry (GC/MS), on-line high performance microbore liquid chromatography/capillary gas chromatography (LC/GC) and capillary supercritical fluid chromatography (SFC). The suitability of each technique for this particular application is discussed, and semi-quantitative results are presented for the major components detected. 35 refs., 6 figs., 3 tabs.

  17. Determination of the Juglone Content of Juglans regia Leaves by GC/MS.

    Science.gov (United States)

    Matławska, Irena; Bylka, Wiesława; Widy-Tyszkiewicz, Ewa; Stanisz, Beata

    2015-07-01

    The constituents of walnut (Juglans regia L.) leaves are represented by tannins, phenolics, and naphthoquinones, the characteristic compound being juglone. The content of juglone in the methanolic extract of the leaves determined by the GC/MS method was 9.9 ± 0.2 mg/100 g; small amounts (1.3 ± 0.02 mg/100 g) were recorded in the infusion, whereas in the decoction it was not detected. As some studies indicate toxicity of juglone, only decoctions should be recommended for therapeutic use.

  18. [Volatile Oil Analysis of Piper hongkongense form Different Hatbitats by GC-MS].

    Science.gov (United States)

    Cai, Yi; Xie, Feng-feng; Yan, Ping-hua; Gan, Ri-cheng; Zhu, Hua

    2015-02-01

    To analyze the volatile oil in Piper hongkongense from five different habitats. The volatile oil was analyzed by GC-MS. The volatile components oil of each sample varied significantly. Caryophyllene, α-caryophyllene and nerolidol 2 were common constituents of five samples. The volatile oil and chemical constituent contents of fresh sample were higher than that of the old sample. The volatile oil and chemical constituent contents of Piper hongkongense from different habitats have sig- nificant differences, which are affected by habitats, harvest season, storage time and so on.

  19. Analysis of flavor-related compounds from tabacco using SPME-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Park, G.B.; Lee, S.G. [Korea Research Institute of Chemical Technology, Taejeon (Korea)

    2001-04-01

    The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry (GC-MS). Flavor-related compounds were estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin More than one of the flavor-related compounds were detected in the range of 0.001-1.3 {mu}g/g from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%. (author). 19 refs., 4 tabs., 2 figs.

  20. Quantitative analysis of IBP-C/sub 20/ fraction of oil by GC/MS coupling

    Energy Technology Data Exchange (ETDEWEB)

    Castex, H.; Boulet, R.; Juguin, J.; Lepinasse, A. (Institut Francais du Petrole 92 - Rueil-Malmaison (France))

    A quantitative analysis method has been developed by coupling GC/MS with a packed column. It operates at medium resolution, sorting out the exact masses of saturated, aromatic and sulfur-containing hydrocarbons. Based on the obtaining of an average spectrum of well-defined carbon fractions, this method uses coefficient matrices available in the literature and plots a detailed hydrocarbon distribution for which the applications described are interesting. The method fulfills several aims. It makes a distillation and separation by liquid chromatography unnecessary. It can be used with very small quantities of product, with a reduced operating cost.

  1. GC-MS studies of the chemical composition of two inedible mushrooms of the genus Agaricus

    Directory of Open Access Journals (Sweden)

    Gjosheva Melania

    2007-12-01

    Full Text Available Abstract Background Mushrooms in the genus Agaricus have worldwide distribution and include the economically important species A. bisporus. Some Agaricus species are inedible, including A. placomyces and A. pseudopratensis, which are similar in appearance to certain edible species, yet are known to possess unpleasant odours and induce gastrointestinal problems if consumed. We have studied the chemical composition of these mushrooms using GC-MS. Results Our GC-MS studies on the volatile fractions and butanol extracts resulted in the identification of 44 and 34 compounds for A. placomyces and A. pseudopratensis, respectively, including fatty acids and their esters, amino acids, and sugar alcohols. The most abundant constituent in the volatiles and butanol were phenol and urea respectively. We also identified the presence of ergosterol and two Δ7-sterols. In addition, 5α,8α-Epidioxi-24(ξ-methylcholesta-6,22-diene-3β-ol was isolated for the first time from both mushrooms. Our study is therefore the first report on the chemical composition of these two species. Conclusion The results obtained contribute to the knowledge of the chemical composition of mushrooms belonging to the Agaricus genus, and provide some explanation for the reported mild toxicity of A. placomyces and A. pseudopratensis, a phenonomenon that can be explained by a high phenol content, similar to that found in other Xanthodermatei species.

  2. [Screening and identification of stimulant and psychedelic drugs as acetyl-derivatives by GC-MS].

    Science.gov (United States)

    Szkutová, M; Balíková, M

    2006-10-01

    With the increasing number of abused stimulant and psychedelic drugs, along with so called "dance drugs" and "new synthetic drugs" available on the Czech illegal market, there is a need to update methods in toxicological laboratories and therefore it is necessary to develop and optimalize screening and identification procedures for new toxic substances appearing in the laboratory practice. It is well known that relatively popular commercial screening immunoassays have some limits: for instance restricted amount of detectable substances, specificity and sensitivity of detection. Therefore, it is mandatory to combine or complete them with more specific methods based on a different principle. In this paper we have focused on collecting useful analytical data to introduce or complete the system of detection and identification of unknown drugs and their metabolites which can appear in biological samples by using gas chromatography-mass spectrometry (GC-MS) after preparation of relevant acetylated derivatives. The collection of experimental data involves retention indexes and mass spectra of acetylated phenylalkylamines, tryptamines and piperazines and some of their metabolites. These data are fundamental for laboratory diagnostics of drugs of abuse or intoxication and they can be useful for practical application in a number of toxicological laboratories. The mean limit of detection 0.1 ng analyte injected to GC-MS is low enough to allow the method to be successfully applied to real toxicological samples.

  3. Detection and quantification of gas-phase oxidized mercury compounds by GC/MS

    Science.gov (United States)

    Jones, Colleen P.; Lyman, Seth N.; Jaffe, Daniel A.; Allen, Tanner; O'Neil, Trevor L.

    2016-05-01

    Most mercury pollution is emitted to the atmosphere, and the location and bioavailability of deposited mercury largely depends on poorly understood atmospheric chemical reactions that convert elemental mercury into oxidized mercury compounds. Current measurement methods do not speciate oxidized mercury, leading to uncertainty about which mercury compounds exist in the atmosphere and how oxidized mercury is formed. We have developed a gas chromatography/mass spectrometry (GC-MS)-based system for identification and quantification of atmospheric oxidized mercury compounds. The system consists of an ambient air collection device, a thermal desorption module, a cryofocusing system, a gas chromatograph, and an ultra-sensitive mass spectrometer. It was able to separate and identify mercury halides with detection limits low enough for ambient air collection (90 pg), but an improved ambient air collection device is needed. The GC/MS system was unable to quantify HgO or Hg(NO3)2, and data collected cast doubt upon the existence of HgO in the gas phase.

  4. TD-GC-MS Investigation of the VOCs Released from Blood Plasma of Dogs with Cancer

    Directory of Open Access Journals (Sweden)

    Seung-Woo Lee

    2013-01-01

    Full Text Available An analytical TD-GC-MS method was developed and used for the assessment of volatile organic compounds (VOCs released from the blood plasma of dogs with/without cancer. VOCs released from 40 samples of diseased blood and 10 control samples were compared in order to examine the difference between both sample groups that were showing qualitatively similar results independent from the disease’s presence. However, mild disturbances in the spectra of dogs with cancer in comparison with the control group were observed, and six peaks (tentatively identified by comparison with mass spectral library as hexanal, octanal, toluene, 2-butanone, 1-octen-3-ol and pyrrole revealed statistically significant differences between both sample groups, thereby suggesting that these compounds are potential biomarkers that can be used for cancer diagnosis based on the blood plasma TD-GC-MS analysis. Statistical comparison with the application of principal component analysis (PCA provided accurate discrimination between the cancer and control groups, thus demonstrating stronger biochemical perturbations in blood plasma when cancer is present.

  5. Determination of tramadol by dispersive liquid-liquid microextraction combined with GC-MS.

    Science.gov (United States)

    Habibollahi, Saeed; Tavakkoli, Nahid; Nasirian, Vahid; Khani, Hossein

    2015-01-01

    Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) has been developed for preconcentration and determination of tramadol, ((±)-cis-2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol-HCl), in aqueous and biological samples (urine, blood). DLLME is a simple, rapid and efficient method for determination of drugs in aqueous samples. Efficient factors on the DLLME process has defined and optimized for extraction of tramadol including type of extraction and disperser solvents and their volumes, pH of donor phase, time of extraction and ionic strength of donor phase. Based on the results of this study, under optimal conditions and by using 2-nitro phenol as internal standard, tramadol was determined by GC-MS, and the figures of merit of this work were evaluated. The enrichment factor, relative recovery and limit of detection were obtained 420, 99.2% and 0.08 µg L(-1), respectively. The linear range was between 0.26 and 220.00 µg L(-1) (R(2) = 0.9970). The relative standard deviation for 50.00 µg L(-1) of tramadol in aqueous samples by using 2-nitro phenol as IS was 3.6% (n = 7). Finally, the performance of DLLME was evaluated for analysis of tramadol in urine and blood.

  6. GC/MS Analysis of Fractional Extraction of Fusain from Tongting Bituminous Coal in CS2

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Fusain from Tongting (Huaibei, Anhui Province) bituminous (FTTB) coal was fractionally extracted using Soxhlet extractor with CS2. Then the extracts were analyzed with GC/MS. Comparison of experimental data between FTTB coal and clarain from Tongting bituminous (CTTB) coal was carried out. The results show that the kinds of small molecule components detected by GC/MS of FTTB are less than those of CTTB. Long-chain alkanes exist mostly in the extracts of fusain. Macromolecular networks are predominant in the FTTB coal mainly composed of inertinite in the coal petrography. The size of micropores in the FTTB coal is relatively small, and the development of micropores is relatively low. Thus the content of aromatic compounds with affinity for micropores is relative low in FTTB, while the content of long-chain alkanes with affinity for macromolecule networks is relatively high. Sub-components in exinite determine the distribution of long-chain alkanes extracted in the last stage. Odd-numbered carbon distribution appears when resin is most in exinite, while high carbon alkane distribution appears when exinite is dominant in cutinite. Small aromatic molecules are firstly packed in micropores, and exist in a free state after micropores are saturated.

  7. Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Medeiros Vinci, Raquel [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Canfyn, Michael [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); De Meulenaer, Bruno [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); Van Loco, Joris, E-mail: Joris.VanLoco@iph.fgov.BE [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium)

    2010-07-05

    Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 {mu}g L{sup -1}).

  8. Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS.

    Science.gov (United States)

    Vinci, Raquel Medeiros; Canfyn, Michael; De Meulenaer, Bruno; de Schaetzen, Thibault; Van Overmeire, Ilse; De Beer, Jacques; Van Loco, Joris

    2010-07-01

    Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 microg L(-1)).

  9. GC-MS analysis of fluoxetine and its active metabolite norfluoxetine in human urine

    Directory of Open Access Journals (Sweden)

    Münevver Açıkkol

    2010-05-01

    Full Text Available A gas chromatographic-mass spectrometric (GC-MS method was developed for detection of fluoxetine and its active metabolite norfluoxetine in urine. Liquid and solid phase extraction were applied to urine samples using maprotiline as an internal standard (IS. The GC-MS analysis were carried out using HP-5MS capillary column. The linearity ranges of the method were 5-75 ng mL-1 for fluoxetine and 6-125 ng mL-1 for norfluoxetine by solid phase extraction (SPE, and 10-80 ng mL-1 for fluoxetine and also norfluoxetine by liquid- liquid extraction (LLE. Also the range of detection limits were between 1-10 ng mL-1, the range of quantification limits were between 5-10 ng mL-1 for fluoxetine and norfluoxetine by both SPE and LLE. The range of recoveries were between 87 -109 % by both SPE and LLE for analytes. The developed method allowed clinical and toxicological analysis of fluoxetine and norfluoxetine in urine samples.

  10. Identification of additives in poly(vinylacetate) artist's paints using PY-GC-MS.

    Science.gov (United States)

    Silva, Miguel F; Doménech-Carbó, Maria Teresa; Fuster-López, Laura; Mecklenburg, Marion F; Martin-Rey, Susana

    2010-05-01

    Commercial poly(vinyl acetate) (PVAc) paint formulations for artists include a number of compounds in addition to the PVAc polymer and pigments to improve the physical and chemical properties of the resulting product. Among the most common additives are surfactants, coalescing agents, defoamers, freeze-thaw agents and thickeners. These products significantly influence the behaviour of the dried film. Nevertheless, they are usually difficult to detect with conventional analytical methods given their low concentration. In order to identify these additives, present in the dried film as minor components, an analytical method based on in situ thermally assisted pyrolysis-silylation gas chromatography-mass spectrometry (GC-MS) using hexamethyldisilazane as a derivatisation reagent is proposed. This method improves the conventional GC-MS analysis performed by direct pyrolysis and enables the simultaneous identification of the PVAc binding medium and the additives included by the manufacturer in the commercial paint. Five different commercial PVAc paints have been analysed, namely, armour green, burnt umber, oriental red, raw umber and white from Flashe. Internal plasticiser VeoVa consisting of C(10) fatty acids with highly branched chains has been recognised from the MS spectra. On the other hand, the differences found in the additive content of the studied paints, in particular the poly(ethylene glycol)-type surfactant, are in good agreement with their mechanical properties.

  11. Identification of odorous compounds in reclaimed water using FPA combined with sensory GC-MS

    Institute of Scientific and Technical Information of China (English)

    Zhiming Yan; Yu Zhang; Jianwei Yu; Hongying Yuan; Min Yang

    2011-01-01

    Odorous compounds in the influent of a reclaimed water treatment plant (RWTP),consisting of coagulation,sedimentation,continuous micro-filtration (CMF),and chlorination in succession,in a north China city,were identified by combining flavor profile analysis (FPA) with sensory gas chromatograph-mass spectrometry (GC-MS).The sewery/swampy/septic odor with an odor intensity of 6.4 was found to be the major odor group in the RWTP influent,and the existence of well-known odorant including dimethyl disulfide,dimethyl trisulfide,indole and skatole were confirmed using GC-MS.The result of a spiking test showed that the intensity (3.6) of the sewery/swampy/septic odor caused by these four chemicals contributed to over 50% of the odor intensity of the influent.The FPA intensity for sewery/swampy/septic odor in the RWTP effluent was 3.8,showing that the treatment process was not efficient for the removal of odorants,particularly indole and skatole.

  12. SPME GC/MS determination of organochlorine pesticides in water samples

    Directory of Open Access Journals (Sweden)

    Yerbolat Sailaukhanuly

    2013-05-01

    Full Text Available Headspace solid phase microextraction (HS-SPME in combination with gas chromatography and mass-spectrometry (GC/MS was studied for analysis of water samples. The organochlorine pesticides (OCPs, p,p'-DDT, p,p'-DDD, and p,p'-DDE were collected and analyzed by GC/MS. To select of effective fiber coatings four types of SPME fibers were examined and compared. The parameters effecting the efficiency of HS-SPME such as extraction and pre-incubation time and extraction temperature, effect of solvent nature, ionic strength were studied to obtain optimal parameters. The method was developed using spiked water samples in a concentration range  10 - 500 ng/L. The calibration curve was linear over the studied concentration range with r≥0.9925. The detection limits varied from 1.57 to 2.08 ng/L. An authentic water samples from contaminated lake with OCPs were analyzed by developed method.

  13. Analysis of organic micropollutants in drinking water using SPME and GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Guidotti, M.; Ravaioli, G. [Presidio Multizonale di Prevenzione, Rieti (Italy). Settore Ambiente

    1999-12-01

    In this work the purpose was to develop accurate and reproducible methods for the qualitative and quantitative analysis of pesticides/herbicides, phthalates, chlorinated solvents, trihalomethanes, polycyclic aromatic hydrocarbons (PAHs) and chlorophenols in drinking waters, using solid-phase micro extraction and GC-MS techniques. The SPME developed by J. Pawliszyn and co-workers, consists of an fused silica fibre, coated with an appropriate absorbent phase, hosted inside the needle of a holder that looks like a GC-syringe; the needle pierces the septum of a sealed vial and the fibre is lowered, by depressing the plunger of the holder, into the liquid (or in the headspace, if that is the case) that contains the analytes of interest. After a set period of time, necessary to reach the partitioning equilibrium, the fibre is retracted inside the needle, the needle is inserted into the GC injector port and the fibre pushed in the heated injector. Here the compounds of interest (that have adsorbed onto the fibre) are thermally desorbed and analysed by GC-MS. After three minutes the fibre is extracted and is ready for a new analysis. The SPME technique has already found many applications in food and environmental analysis. Many of the analytes investigated in this research are listed Italian legislation as possible pollutants of drinking waters and their presence and concentrations require monitoring. The list of compounds included in this work is reported in Table 1.

  14. ANALISIS KOMPONEN KIMIA EKSTRAK METANOL FRAKSI PETROLEUM ETER DAUN EUPATORIUM ODORATUM DENGAN GC-MS

    Directory of Open Access Journals (Sweden)

    Purwati

    2008-05-01

    Full Text Available The purpose of this investigation was to analize the organic compounds of Eupatorium odoratum leaf and identification of the compounds using Gas Chromatography Mass Spectrometry (GC-MS. The sample was soaked in metanol. The extract of metanol was partitioned using petroleum ether. The extracts obtained were analyzed and identified by GC-MS. The results showed that in the extract of petroleum ether contained the organic compounds: germacrene, isocaryophyllene, 2,6,6,9-tetramethyl-1,4,8-cycloundecatriene, 1-methyl-5-methylene-8-(1-methylethyl-1,7-cyclodecadiene, 1,2,4a,5,8,8a-hexahydro-4,7-dimethyl-1-(1-methylethyl naphthalene, 1,12- dodecanediol, octahydro-1-(2-octyldecyl pentalene, 3,7,11,15-tetramethyl-2-hexadecen-1-ol, methyl (12-acetyloxy-9-octadecanoic, bis (2-ethylhexyl phthalat, farnesol, 4,22-cholestadien-3-one and 1,2,3,5,6,7,8,8a-octahydro-1,4-dimethyl-7-(1-methylethenyl azulene. In the extract of ethyl acetate contained the organic compounds: methyl heptadecanoic, hexadecanoic acid, methyl 13-octadecenoic, 14,16-octadecadienal and octadecanoic acid.

  15. Potential Health Benefits and Metabolomics of Camel Milk by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Raish, Mohammad; Ahmad, Ajaz; Shakeel, Faiyaz

    2017-02-01

    None of the research reports reveals the metabolomics and elemental studies on camel milk. Recent studies showed that camel milk possesses anticancer and anti-inflammatory activity. Metabolomics and elemental studies were carried out in camel milk which showed us the pathways and composition that are responsible for the key biological role of camel milk. Camel milk was dissolved in methanol and chloroform fraction and then vortexed and centrifuged. Both the fractions were derivatized by N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) and TMCS after nitrogen purging and analyzed by GC-MS. Camel milk was also analyzed by ICP-MS after microwave digestion. We found that higher alkanes and fatty acids are present in the chloroform fraction and amino acids, sugars and fatty acid derivatives are present in aqueous fractions. All the heavy metals like As, Pb, Cd, Co, Cu, and Ni were in the safe limits in terms of maximum daily intake of these elements. Na, K, Mg, and Ca were also present in the safe limits in terms of maximum daily intake of these elements. These results suggested that the camel milk drinking is safe and there is no health hazard. The present data of GC-MS and ICP-MS correlate the activities related to camel milk.

  16. Distinguishing Foeniculum vulgare fruit from two adulterants by combination of microscopy and GC-MS analysis.

    Science.gov (United States)

    Ma, Xiao-Dong; Mao, Wen-Wen; Zhou, Ping; Li, Ping; Li, Hui-Jun

    2015-07-01

    Foeniculum vulgare fruit (FVF) is a widely used traditional medicine. However, two adulterants, namely Anethum graveolens fruit (AGF) and Cuminum cyminum fruit (CCF), have been found in use as FVF in China owing to similar appearance and odor. For the purpose of accurate differentiation of the three herbal medicines, extensive anatomical examination and chemical profiling were conducted. Using light microscopy and fluorescence microscopy, the macroscopic and microscopic features of the three species were compared. It was found that some microscopic characteristics, including transverse shape of mericarp, presence or absence of reticulate cells and non-glandular hairs, as well as fluorescence of endocarp, were of diagnostic significance. Moreover, essential oils were qualitatively and semi-quantitatively analyzed using GC-MS. The analytical results indicated significant chemical variations in different species: in FVF, trans-anethole (83.20%) was the predominant volatile compound followed by estragole (5.03%) and limonene (3.45%), while in AGF, the first, second and third compounds with highest content were carvone (42.58%), apiol (20.76%) and limonene (20.32%), and in CCF were cuminlaldehyde (36.00%), 2-caren-10-al (23.25%) and γ-terpinene (9.65%), respectively. In conclusion, the proposed light microscopy coupled with fluorescence microscopy and/or GC-MS analysis allowed successful distinguishing FVF from AGF and CCF.

  17. Determination of phthalates in polymer materials - comparison of GC/MS and GC/ECD methods

    Directory of Open Access Journals (Sweden)

    Katarzyna Jaworek

    2013-01-01

    Full Text Available The paper presents two methods for determination of phthalates in polymer materials. The methods compared were gas chromatography combined with the mass spectrometry (GC/MS and gas chromatography with electron capture detector (GC/ECD. The GC/ECD technique was chosen for this comparison, because the ECD detector was one of few capable of detecting phthalates. In both cases the same procedure of sample preparation with ultrasonic extraction was applied. Overall recoveries were 76-100 % with relative of standard deviation (R.S.D. values in the range 0.6-19 %. The values of limit of detection (LOD for GC/MS method ranged from 3.46 µg mL- 1 to 10.10 µg mL- 1, depending on the determined phthalate, while in case of the GC/ECD method they were in the range from 2.97 µg mL- 1 to 4.29 µg mL- 1. The methods were applied for determination of: dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl phthalate, diisononyl phthalate, diisoocyl phthalate in polymer material. The seventeen kinds of samples were analyzed. Most of the materials selected for the analyses were made from polyethylene (PE, polyvinyl chloride (PVC and polystyrene (PS.

  18. Analysis of acrylamide by LC-MS/MS and GC-MS in processed Japanese foods.

    Science.gov (United States)

    Ono, H; Chuda, Y; Ohnishi-Kameyama, M; Yada, H; Ishizaka, M; Kobayashi, H; Yoshida, M

    2003-03-01

    Acrylamide concentrations in processed foods (63 samples covering 31 product types) from Japan were analysed by LC-MS/MS and GC-MS methods. The limit of detection and limit of quantification of acrylamide were 0.2 ng x ml(-1) (6 fmol) and 0.8 ng x ml(-1) (22 fmol), respectively, by LC-MS/MS, and those of 2,3-dibromopropionamide derived from acrylamide were 12 ng x ml(-1) (52 fmol) and 40 ng x ml(-1) (170 fmol), respectively, by GC-MS. Repeatability given as RSD was 1000 microg x kg(-1). The concentrations in non-whole potato-based snacks, rice crackers processed by grilling or frying, and candied sweet potatoes were lower compared with those in the potato crisps and the whole potato-based fried snacks. One of the whole potato-based fried snacks, however, showed low acrylamide concentration (instant precooked noodles and won-tons were <100 microg x kg(-1) with only one exception. Roasted barley grains for 'Mugi-cha' tea contained 200-600 microg x kg(-1) acrylamide.

  19. Efficiency of GC-MS method in detection of beeswax adulterated with paraffin

    Directory of Open Access Journals (Sweden)

    Waś Ewa

    2016-06-01

    Full Text Available The efficiency of the gas chromatography - mass detector (GC-MS technique for the detection of beeswax adulterated with paraffin, was evaluated. For this purpose, beeswax samples with paraffin additions (3, 5, 10, 30, 50% were analysed. Since not enough is known about paraffin compositions, and since it is difficult to detect paraffin in beeswax, the aim of our research was also to compare the hydrocarbon composition of different types of paraffin. The analysis showed that the types of paraffin available on the market, differ qualitatively and quantitatively as far as their hydrocarbon compositions are concerned. In all kinds of paraffin, we found homologous series of n-alkanes that were much longer than those in beeswax. In beeswax, the amount of added paraffin that is possible to detect, differs and depends on the kind of paraffin used for adulteration. In this study, the minimum estimated percent that was detected using the GC-MS technique, was 3%. The adulteration is indicated by the presence of hydrocarbons containing over 35 carbon atoms in the molecule, and by the higher contents of n-alkanes (C20H42 - C35H72, in comparison to the concentration of these compounds determined in pure beeswax. We also presented the results of the quality control of commercial beeswax. Based on our results, it can be stated that beeswax adulteration is currently a problem.

  20. Advanced manufacturing: Technology diffusion

    Energy Technology Data Exchange (ETDEWEB)

    Tesar, A.

    1995-12-01

    In this paper we examine how manufacturing technology diffuses rom the developers of technology across national borders to those who do not have the capability or resources to develop advanced technology on their own. None of the wide variety of technology diffusion mechanisms discussed in this paper are new, yet the opportunities to apply these mechanisms are growing. A dramatic increase in technology diffusion occurred over the last decade. The two major trends which probably drive this increase are a worldwide inclination towards ``freer`` markets and diminishing isolation. Technology is most rapidly diffusing from the US In fact, the US is supplying technology for the rest of the world. The value of the technology supplied by the US more than doubled from 1985 to 1992 (see the Introduction for details). History shows us that technology diffusion is inevitable. It is the rates at which technologies diffuse to other countries which can vary considerably. Manufacturers in these countries are increasingly able to absorb technology. Their manufacturing efficiency is expected to progress as technology becomes increasingly available and utilized.

  1. Comparative GC/MS and LC/MS detection of hexabromocyclododecane (HBCD) in soil and water samples

    Energy Technology Data Exchange (ETDEWEB)

    Petersen, M.; Hamm, S. [Eurofins, Hamburg (Germany)]|[Gesellschaft fuer Arbeitswissenschaft e.V. (GfA), Dortmund (Germany); Schaefer, A. [Eurofins Analytik GmbH, Wiertz - Eggert - Joerissen, Hamburg (Germany); Esser, U. [GfA Constult GmbH, Muenster (Germany)

    2004-09-15

    Hexabromocyclododecane (HBCD) is a crucial additive flame retardant (FR) for FR Polystyrene insulation foams (both expandable (EPS) as well as extrudable polystyrene (XPS)), polystyrene masterbatches and textile FR coatings. The total consumption of HBCD within the European Union (EU) is estimated to be about 10,000 tons out of 16,700 worldwide per year. The technical HBCD product usually is a mixture of the three diastereoisomers {alpha}-, {beta}- and {gamma}-HBCD with the {gamma}- isomer as main component. Compared to other flame retardants only few data on HBCD levels in the environment have been published. Within this study a series of soil and water samples from HBCD processing plants was analysed by GC/MS (LRMS-EI). Besides GC/MS, also liquid chromatography coupled to mass spectrometry (LC/MS) is often used for HBCD detection in environmental samples. Whilst GC/MS only provides information about the total of the three HBCD isomers, LC/MS is able to selectively monitor and quantify the three components. On the other hand GC/MS usually has the advantage of a higher sensitivity. In order to verify the GC/MS results and to check the comparability to LC/MS analytical data, five soil and five water samples showing a wide range of HBCD concentrations were analysed by using both techniques. The comparative analyses by means of LC/MS confirmed the HBCD identification and quantification of the GC/MS. The differences between the total HBCD results of the GC/MS and the LC/MS analyses were less than 24%. The {gamma}- isomer proved to be the main HBCD diastereoisomer in the soil and water samples tested.

  2. Thermal Hazard Evaluation of Cumene Hydroperoxide-Metal Ion Mixture Using DSC, TAM III, and GC/MS

    Directory of Open Access Journals (Sweden)

    Mei-Li You

    2016-04-01

    Full Text Available Cumene hydroperoxide (CHP is widely used in chemical processes, mainly as an initiator for the polymerization of acrylonitrile–butadiene–styrene. It is a typical organic peroxide and an explosive substance. It is susceptible to thermal decomposition and is readily affected by contamination; moreover, it has high thermal sensitivity. The reactor tank, transit storage vessel, and pipeline used for manufacturing and transporting this substance are made of metal. Metal containers used in chemical processes can be damaged through aging, wear, erosion, and corrosion; furthermore, the containers might release metal ions. In a metal pipeline, CHP may cause incompatibility reactions because of catalyzed exothermic reactions. This paper discusses and elucidates the potential thermal hazard of a mixture of CHP and an incompatible material’s metal ions. Differential scanning calorimetry (DSC and thermal activity monitor III (TAM III were employed to preliminarily explore and narrate the thermal hazard at the constant temperature environment. The substance was diluted and analyzed by using a gas chromatography spectrometer (GC and gas chromatography/mass spectrometer (GC/MS to determine the effect of thermal cracking and metal ions of CHP. The thermokinetic parameter values obtained from the experiments are discussed; the results can be used for designing an inherently safer process. As a result, the paper finds that the most hazards are in the reaction of CHP with Fe2+. When the metal release is exothermic in advance, the system temperature increases, even leading to uncontrollable levels, and the process may slip out of control.

  3. Thermal Hazard Evaluation of Cumene Hydroperoxide-Metal Ion Mixture Using DSC, TAM III, and GC/MS.

    Science.gov (United States)

    You, Mei-Li

    2016-04-28

    Cumene hydroperoxide (CHP) is widely used in chemical processes, mainly as an initiator for the polymerization of acrylonitrile-butadiene-styrene. It is a typical organic peroxide and an explosive substance. It is susceptible to thermal decomposition and is readily affected by contamination; moreover, it has high thermal sensitivity. The reactor tank, transit storage vessel, and pipeline used for manufacturing and transporting this substance are made of metal. Metal containers used in chemical processes can be damaged through aging, wear, erosion, and corrosion; furthermore, the containers might release metal ions. In a metal pipeline, CHP may cause incompatibility reactions because of catalyzed exothermic reactions. This paper discusses and elucidates the potential thermal hazard of a mixture of CHP and an incompatible material's metal ions. Differential scanning calorimetry (DSC) and thermal activity monitor III (TAM III) were employed to preliminarily explore and narrate the thermal hazard at the constant temperature environment. The substance was diluted and analyzed by using a gas chromatography spectrometer (GC) and gas chromatography/mass spectrometer (GC/MS) to determine the effect of thermal cracking and metal ions of CHP. The thermokinetic parameter values obtained from the experiments are discussed; the results can be used for designing an inherently safer process. As a result, the paper finds that the most hazards are in the reaction of CHP with Fe(2+). When the metal release is exothermic in advance, the system temperature increases, even leading to uncontrollable levels, and the process may slip out of control.

  4. Results of the First Mars Organic Molecule Analyzer (MOMA) GC-MS Coupling

    Science.gov (United States)

    Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Danell, Ryan; Grand, Noel; Van Amerom, Friso; Glavin, Daniel; Freissinet, Caroline; Humeau, Olivier; Coll, Patrice; Arevalo, Ricardo; Stalport, Fabien; Brinckerhoff, William; Steininger, Harald; Goesmann, Fred; Mahaffy, Paul; Raulin, Francois

    2014-11-01

    The Mars Organic Molecule Analyzer (MOMA) aboard the ExoMars rover will be a key analytical tool in providing chemical (molecular) information from the solid samples collected by the rover, with a particular focus on the char-acterization of the organic content. The core of the MOMA instrument is a gas chromatograph coupled with a mass spectrometer (GC-MS) which provides the unique capability to characterize a broad range of compounds, including both of volatile and non-volatile species. Samples will be crushed and deposited into sample cups seated in a rotating carousel. Soil samples will be analyzed either by UV laser desorption / ionization (LDI) or pyrolysis gas chromatography ion trap mass spectrometry (pyr-GC-ITMS).The French GC brassboard was coupled to the US ion trap mass spectrometer brassboard in a flight-like con-figuration for several coupling campains. The MOMA GC setup is based on the SAM heritage design with a He reservoir and 4 separate analytical modules including traps, columns and Thermal Conductivity Detectors. Solid samples are sealed and heated in this setup using a manual tapping station, designed and built at MPS in Germany, for GC-MS analysis. The gaseous species eluting from the GC are then ionized by an electron impact ionization source in the MS chamber and analyzed by the linear ion trap mass spectrometer. Volatile and non-volatile compounds were injected in the MOMA instrumental suite. Both of these compounds classes were detected by the TCD and by the MS. MS signal (total ion current) and single mass spectra by comparison with the NIST library, gave us an unambiguous confirmation of these identifications. The mass spectra arise from an average of 10 mass spectra averaged around a given time point in the total ion chromatogram.Based on commercial instrument, the MOMA requirement for sensitivity in the GC-MS mode for organic molecules is 1 pmol. In this test, sensitivity was determined for the GC TCD and MS response to a dilution

  5. Comparison of purge and trap GC/MS and purgeable organic chloride analysis for monitoring volatile chlorinated hydrocarbons

    Science.gov (United States)

    Barber, Larry B.; Thurman, E. Michael; Takahashi, Yoshi; Noriega, Mary C.

    1992-01-01

    A combined field and laboratory study was conducted to compare purge and trap gas chromatography/mass spectrometry (PT-GC/MS) and purgeable organic chloride (POCl) analysis for measuring volatile chlorinated hydrocarbons (VCH) in ground water. Distilled-water spike and recovery experiments using 10 VCH indicate that at concentrations greater than 1 ??g/l recovery is more than 80 percent for both methods with relative standard deviations of about 10 percent. Ground-water samples were collected from a site on Cape Cod, Massachusetts, where a shallow unconfined aquifer has been contaminated by VCH, and were analyzed by both methods. Results for PT-GC/MS and POCl analysis of the ground-water samples were not significantly different (alpha = 0.05, paired t-test analysis) and indicated little bias between the two methods. Similar conclusions about concentrations and distributions of VCH in the ground-water contamination plume were drawn from the two data sets. However, only PT-GC/MS analysis identified the individual compounds present and determined their concentrations, which was necessary for toxicological and biogeochemical evaluation of the contaminated ground water. POCl analysis was a complimentary method for use with PT-GC/MS analysis for identifying samples with VCH concentrations below the detection limit or with high VCH concentrations that require dilution. Use of POCl as a complimentary monitoring method for PT-GC/MS can result in more efficient use of analytical resources.

  6. Metabolomic and elemental analysis of camel and bovine urine by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Alhaider, Abdul Qader; Raish, Mohammad; Shakeel, Faiyaz

    2017-01-01

    Recent studies from the author's laboratory indicated that camel urine possesses antiplatelet activity and anti-cancer activity which is not present in bovine urine. The objective of this study is to compare the volatile and elemental components of bovine and camel urine using GC-MS and ICP-MS analysis. We are interested to know the component that performs these biological activities. The freeze dried urine was dissolved in dichloromethane and then derivatization process followed by using BSTFA for GC-MS analysis. Thirty different compounds were analyzed by the derivatization process in full scan mode. For ICP-MS analysis twenty eight important elements were analyzed in both bovine and camel urine. The results of GC-MS and ICP-MS analysis showed marked difference in the urinary metabolites. GC-MS evaluation of camel urine finds a lot of products of metabolism like benzene propanoic acid derivatives, fatty acid derivatives, amino acid derivatives, sugars, prostaglandins and canavanine. Several research reports reveal the metabolomics studies on camel urine but none of them completely reported the pharmacology related metabolomics. The present data of GC-MS suggest and support the previous studies and activities related to camel urine.

  7. GC-MS法检测球花石斛花中挥发性成分%Determination of volatile components From flower of Dendrobium thyrsiflorum by GC-MS

    Institute of Scientific and Technical Information of China (English)

    崔娟; 刘圣; 胡江苗

    2013-01-01

    Objective To study the chemical constituents of volatile oil from flower of Dendrobium thyrsiflorum by GC-MS technology. Methods The chemical compositions of volatile oil of the plant were obtained by water reflux method and then analyzed by GC-MS e-quipped. Results About twenty-two compounds were identified with the computer standard spectra as linoleic acid( 51. 82% ),linolenic acid( 10.056% ),palmitic acid( 9. 282% ),stearic acid ( 4. 579% ),8-hydroxy-4,7-dimethyl coumarin( 4. 727% )6,7-dimethoxy cou-marin( 3. 083% ),tricosane( 4. 490% )etc. Conclusions This paper reports,for the first time,the composition of volatile oils of flowers Dendrobium thyrsiflorum by GC-MS.%目的 研究球花石斛花中挥发性的化学成分.方法 采用水回流法从球花石斛花中提取挥发性成分,并用气相色谱-质谱(GC-MS)联用技术,对球花石斛花中的挥发性成分进行了测定.结果 共鉴定出22种化学成分,其中含量较高的主要有亚油酸(51.82%)、亚麻酸(10.056%)、棕榈酸(9.282%)、硬脂酸(4.579%)、8-羟基-4,7-二甲基香豆素(4.727%)、6,7-二甲氧基香豆素(3.083%)、二十三烷(4.490%)等.结论 该文首次采用气相色谱-质谱(GC-MS)联用技术对球花石斛花挥发性成分进行提取研究.

  8. [Naphtha analysis of different processed products of Rhizoma Curcumae from Guangxi by GC-MS].

    Science.gov (United States)

    Pan, Ying; Qin, Bao; Jiang, Hai-Yan; Bao, Chuan-Hong

    2009-03-01

    To approach the naphtha analysis of different processed products of Rhizoma Curcumae from Guangxi. The naphtha was extracted by steam distillation. The relative content of every compound was determined with area normalization method and the structures were elucidated by GC-MS technique. 33 kinds of chemical compositions were identified in the naphtha of the six samples,the main contents were Cyclohexane, 1-ethenyl-1-methyl-2,4-bis (1-methylethenyl)-, 5-Benzofuranacetic acid, 6-ethenyl-4,5,6,7-terahydro-3, 6-dimethyl-alpha. -methylene-,methyl ester, and so on. Six samples of Rhizoma Curcumae are significantly different in quality,and the naphtha's content of the sample processing with vinegar is the highest.

  9. Characterization of volatiles from cultured dairy spreads during storage by dynamic headspace GC/MS

    DEFF Research Database (Denmark)

    Lund, Pia; Hølmer, Gunhild Kofoed

    2001-01-01

    The effect of storage time and storage temperature on the formation of volatile compounds in dairy spreads was investigated. Dairy spreads were stored for 10 weeks at -18, 5 and 20 degreesC, respectively, and analyzed after 0, 38, 54 and 67 days of storage. By means of a dynamic headspace GC....../MS method using Tenax traps the dairy spreads were analyzed for volatile aromatic compounds. 61 components were identified and their relative content was followed during the storage period. Among these were four alcohols, 17 aldehydes, four esters, ten alkanes, 11 ketones and six lactones. A general...... increase in the concentration of most of the volatile compounds during storage was found. The content of volatile compounds in dairy spreads stored at -18 OC was nearly constant or showed a rather low increase in the content during the storage period. Storage at higher temperatures (5 and 20 degrees...

  10. Chemical Analysis of Essential oil of "Artemisia haussknechtii Boiss" by GC and GC/ MS

    Directory of Open Access Journals (Sweden)

    A. Nassir- Ahraadi . A. Rustaiyan

    1994-08-01

    Full Text Available The composition of the essential oil from the leaves and flowers of "Artemisia haussknechtii Boiss growing wild in the north-west of Iran, was investigated by GC and GC/MS."nThe main components of the volatile oil were 1,8 - cineol (16.5%, camphor (14.1%. artemisia ketone (10.5%, fragranol (9.0%, Yomogi alcohol (7.5% and B- pinene (5.4%. The total contribution of these compounds to the oil amounted to 63.0%."nMonoterpens and sesquiterpenes represent 90.08% and 1.52% of the oil respectively. Of the twenty oxygen-containing monoterpenes which made up a fairly large fraction of the terpenoid composition, the predominant components were 1,8 - cineole and camphor.

  11. Profiling the anaerobic response of C. elegans using GC-MS.

    Directory of Open Access Journals (Sweden)

    Jeffrey A Butler

    Full Text Available The nematode Caenorhabditis elegans is a model organism that has seen extensive use over the last four decades in multiple areas of investigation. In this study we explore the response of the nematode Caenorhabditis elegans to acute anoxia using gas-chromatography mass-spectrometry (GC-MS. We focus on the readily-accessible worm exometabolome to show that C. elegans are mixed acid fermenters that utilize several metabolic pathways in unconventional ways to remove reducing equivalents - including partial reversal of branched-chain amino acid catabolism and a potentially novel use of the glyoxylate pathway. In doing so, we provide detailed methods for the collection and analysis of excreted metabolites that, with minimal adjustment, should be applicable to many other species. We also describe a procedure for collecting highly volatile compounds from C. elegans. We are distributing our mass spectral library in an effort to facilitate wider use of metabolomics.

  12. Qualitative and quantitative studies of chemical composition of sandarac resin by GC-MS.

    Science.gov (United States)

    Kononenko, I; de Viguerie, L; Rochut, S; Walter, Ph

    2017-01-01

    The chemical composition of sandarac resin was investigated qualitatively and quantitatively by gas chromatography-mass spectrometry (GC-MS). Six compounds with labdane and pimarane skeletons were identified in the resin. The obtained mass spectra were interpreted and the mass spectrometric behaviour of these diterpenoids under EI conditions was described. Quantitative analysis by the method of internal standard revealed that identified diterpenoids represent only 10-30% of the analysed sample. The sandarac resin from different suppliers was analysed (from Kremer, Okhra, Color Rare, La Marchande de Couleurs, L'Atelier Montessori, Hevea). The analysis of different lumps of resins showed that the chemical composition differs from one lump to another, varying mainly in the relative distributions of the components.

  13. A GC-MS-based metabolomics study on the tubers of commercial potato cultivars upon storage.

    Science.gov (United States)

    Uri, Csilla; Juhász, Zsófia; Polgár, Zsolt; Bánfalvi, Zsófia

    2014-09-15

    Using gas chromatography-mass spectrometry (GC-MS) as a system for the detection of amino acids, organic acids, sugars, sugar alcohols, and fatty acids, we characterised six commercial potato cultivars (Hópehely, Katica, Lorett, Somogyi kifli, Vénusz Gold, and White Lady) with different pedigrees, starch contents, cooking types, and dormancy periods, in five developmental stages from harvest to sprouting. The tubers were stored at 20-22°C in the dark. The metabolite data were subjected to principal component analysis. No correlation between metabolite contents of freshly harvested tubers and starch content or cooking type of the cultivars was detected. The storage decreased the fructose and sucrose and increased the proline concentrations of tubers. Irrespective of the length of dormancy a substantial difference in metabolite composition at each time point upon storage was detected in each cultivar except Somogyi kifli, the only cultivar amongst those tested with a pure Solanum tuberosum origin and A cooking type.

  14. Choosing between GC FTIR and GC MS spectra for an efficient intelligent identification of illicit amphetamines

    Science.gov (United States)

    Gosav, S.; Dinica, R.; Praisler, M.

    2008-09-01

    In this paper we are presenting a comparative analysis between several expert systems built for the identification of illicit amphetamines based on their GC-FTIR and GC-MS spectra. The systems were built using Artificial Neural Networks (ANNs), and are dedicated to the recognition of amphetamines. Structure-activity relationships are incorporated into the knowledge base, allowing the systems to identify the amphetamines according to their toxicological activity (stimulant or hallucinogenic). The results show that GC-FTIR data are much more relevant for the efficiency of the expert systems, probably due to the fact that these spectra constitute a "fingerprint" of the molecular structures. We are also presenting a spectroscopic analysis in order to evaluate the relevance of each type of input variable (absorption and abundance) on which the recognition of an unknown sample is based.

  15. Study of the red lacquer from a pair of Namban stirrups by Py-GC/MS

    Directory of Open Access Journals (Sweden)

    José Carlos Frade

    2009-01-01

    Full Text Available Oriental lacquer is a material of vegetal origin that is used in the Asian countries as a coating for the most varied kinds of religious and civil use objects. With the Portuguese arrival to the East, the Europeans started to develop a taste for the exotic and exquisite Art of Lacquer. From the 16th century onwards a lacquerware market developed with numerous lacquered objects being brought to Europe. In this work, the red lacquer from a pair of Namban stirrups was studied by Py-GC/MS (pyrolysis-gas chromatography/mass spectrometry. The results were compared with lacquer references, and the lacquer type was identified. Based on the results, the stirrups' lacquering technique and the performance of Py-CG/MS in the identification of oriental lacquers are also discussed.

  16. GC-MS ANALYSIS OF STICKY CONTAMINANTS IN A DEINKING PULPING LINE

    Directory of Open Access Journals (Sweden)

    Yang Gao,

    2012-04-01

    Full Text Available Pulps were sampled from three major points of a deinking pulping line and classified as fibers fraction, fines fraction, and aqueous phase, respectively, then extracted with tetrahydrofuran (THF or methyl tert-butyl ether (MTBE. Sticky contaminants in the extractives were examined by GC-MS analysis. The results showed that the contaminants can be grouped as adhesive substances, wood extractives, lignin-derivatives, and other organic acids, of which the adhesive substances were accounted as the major component. Contents of sticky components in each group and their removal were further evaluated according to the related unit operation. Adhesives remaining in fibers and fines fractions were removed by the post-flotation. Wood extractives and degraded residual lignins were also released to some extent from pulp fibers during heat-dispersing, and then removed during the post-flotation.

  17. GC-MS ANALYSIS OF SOME BIOACTIVE CONSTITUENTS OF THE LEAVES OF DESMODIUM GYRANS DC.

    Directory of Open Access Journals (Sweden)

    S.Gopalakrishnan

    2012-08-01

    Full Text Available Desmodium gyrans DC is one of the medicinally valuable plants belonging to the family Fabaceae, commonly known as “Thozhukanni” in Tamil and ‘ Namaskari’ in Sanskrit. Traditionally leaves are used as antidote, cardiac-tonic and for wound healing. In the present study the ethanolic extract of Desmodium gyrans has been subjected to GC-MS analysis. Eighteen chemical constituents have been identified, The major chemical constituents are: 4,5-Dihydro-2-amino-4-(2,4-dichlorophenyl-7-methyl-5-oxo- pyrano[3,2-c]pyran-3-carbonitrile (59.07%, Pentaborane (13.86%, Pentanedinitrile (6.63% and 3-Chloro-1-butyne, (4.82%.

  18. Analysis of bioactive Amaryllidaceae alkaloid profiles in Lycoris species by GC-MS.

    Science.gov (United States)

    Guo, Ying; Pigni, Natalia B; Zheng, Yuhong; de Andrade, Jean Paulo; Torras-Claveria, Laura; Borges, Warley de Souza; Viladomat, Frances; Codina, Carles; Bastida, Jaume

    2014-08-01

    The genus Lycoris, a group of Amaryllidaceae plants distributed in temperate regions of Eastern Asia, is already known for containing representative alkaloids typical of this botanical family with a wide range of biological activities (for example, lycorine and galanthamine). In the present work, the alkaloid profiles of nine species, L. albiflora, L. aurea, L. chinensis, L. haywardii, L. incarnata, L. longituba, L. radiata, L. sprengeri, and L. squamigera, and one variety (L. radiata var. pumila) have been evaluated by GC-MS. Structures belonging to the lycorine-, homolycorine-, haemanthamine-, narciclasine-, tazettine-, montanine- and galanthamine-series were identified and quantified, with galanthamine- and lycorine-type alkaloids predominating and usually showing a high relative abundance in comparison with other alkaloids of the extracts. Interestingly, L. longituba revealed itself to be a potential commercial source of bioactive alkaloids. In general terms, our results are consistent with the alkaloid profiles reported in the literature for previously studied species.

  19. Analysis on fat-soluble components of sinapis semina from different habitats by GC-MS

    Institute of Scientific and Technical Information of China (English)

    Cheng Peng; Tao Zhang; Gang Zhao; Sicen Wang

    2013-01-01

    A simple and rapid gas chromatography/mass spectrometry (GC/MS) analysis method was developed for the determination of fat-soluble parts of sinapis semina. Four major compounds were chosen as marker compounds to evaluate the method. Various extraction techniques were evaluated and the greatest efficiency was observed with sonication extraction using diethyl ether. The method was valuated as follows:acceptable apparatus suitability was obtained by testing the resolutions, tailing factors and theoretical plate number of the marker compounds; the precision and reproducibility, expressed as relative standard deviation (RSD), fell within the prescribed limits. Eight samples of sinapis semina collected from markets in Xi’an were monitored by using the method. The fingerprints of those samples were analyzed by hierarchical cluster analysis (HCA) similarity analysis. The result indicated that the combination of fingerprint and HCA could be used to analyze sinapis semina from different habitats.

  20. Determination of toxaphene residues in fish foodstuff by GC-MS.

    Science.gov (United States)

    Barbini, D Attard; Stefanelli, P; Girolimetti, S; Di Muccio, A; Dommarco, R

    2007-08-01

    A method for the determination of toxaphene residues in fish and fish-based baby foods has been developed. The cleanup of the fatty matrices was performed using an acid treatment on an Extrelut-NT3 and ENVI-Florisil SPE cartridges system, using light petroleum as eluent. Instrumental analysis was carried out by gaschromatography with mass spectrometry detector (GC/MS) in SIM mode. Recoveries from spiked samples were tested at 0.005 and 0.01 mg/kg per single congener and were in the range 82-104% while relative standard deviations (RSDs) were in the range 3.7-10.9%. Nineteen samples of both frozen fish food and fish-based baby foods representative of the Italian market were collected from local dealers and analysed.

  1. A robust GC-MS method for the quantitation of fatty acids in biological systems.

    Science.gov (United States)

    Jayasinghe, Nirupama Samanmalie; Dias, Daniel Anthony

    2013-01-01

    Fatty acids (FAs) are involved in a wide range of functions in biological systems. It is important to measure the exact amount of fatty acids in biological matrices in order to determine the level of fatty acids and understand the role they play. The ability to quantify fatty acids in various systems, especially plant species and microbes has recently paved the way to the mass production of pharmaceuticals and energy substitutes including biodiesel. This chapter describes an efficient method to quantify the total fatty acids (TFAs) in biological systems using gas chromatography-mass spectrometry (GC-MS) and a commercially available standard mix of fatty acid methyl esters (FAMEs) using a step-by-step methodology to setup a quantitation method using the Agilent Chemstation software.

  2. Pyrolysis Process in Aramid Fibers Investigated by Py-GC/MS & TGA-DTA/MS

    Institute of Scientific and Technical Information of China (English)

    WANG Xin-wei; HU Zu-ming; LIU Zhao-feng

    2007-01-01

    Poly(m-phenylene isophthalamine) (PMIA) and Poly( p-phenylene terphthalamine) (PPTA) are among the most important high-temperature resistant aramid fibers. The pyrolysis behaviors of these two fibers under inert gases were studied using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and thermogravimetric analysis coupled with mass spectrometry ( TGA-DTA/MS ). The pyrolysis processes of PMIA and PPTA are distinguishing, and the stepwise pyrolysates reflect these differences. A mechanism system of pyrolysis is suggested, which involving hydrolysis and homolysis. At low pyrolysis temperatures, hydrolysis is a primary reaction, and it is very noticeable in the first-step pyrolysis region of PMIA. Elevating pyrolysis temperature, homolysis is enhanced and keep a large advantage in the high temperature range. On the other hand, at higher temperatures, carbonization appens and the homolysis and carbonization of PPTA are emphasized more than of PMIA.

  3. Analysis of Amaryllidaceae alkaloids from Zephyranthes grandiflora by GC/MS and their cholinesterase activity

    Directory of Open Access Journals (Sweden)

    Lucie Cahlíková

    2011-08-01

    Full Text Available Amaryllidaceae are known as ornamental plants, furthermore some species of this family contain galanthamine, an acetylcholinesterase inhibitor approved for the treatment of Alzheimer's disease, and other alkaloids with interesting pharmacological activity. The chemical composition of alkaloids from Zephyranthes grandiflora Lindl. was analyzed by GC/MS. Seven known compounds, belonging to five structural types of Amaryllidaceae alkaloids, were identified. The alkaloid extract from the bulbs showed promising cholinesterase inhibitory activities against human blood acetylcholinesterase (HuAChE; IC50 39.2±3.0 µg/mL and human plasma butyrylcholinesterase (HuBuChE; IC50 356±9.3 µg/mL.

  4. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS

    DEFF Research Database (Denmark)

    Hansen, Anne-Mette Sølvbjerg; Frandsen, Henrik Lauritz; Fromberg, Arvid

    2015-01-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers the naturalness of a raspberry...... flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. 27 food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry...... jam, dried raspberries and sodas declared to contain natural aroma all contained almost only R-(E)-α-ionone supporting the content of natural raspberry aroma. Six out of eight sweets tested did not indicate a content of natural aroma on the labelling which was in agreement with the almost equal...

  5. A validated GC/MS method for the determination of amisulpride in whole blood.

    Science.gov (United States)

    Papoutsis, Ioannis; Rizopoulou, Anna; Nikolaou, Panagiota; Pistos, Constantinos; Spiliopoulou, Chara; Athanaselis, Sotiris

    2014-02-01

    A sensitive GC/MS method for the determination of amisulpride in whole blood was developed, optimized and validated. Sample preparation included solid-phase extraction using HF Bond Elut C18 cartridges and further derivatization with heptafluorobutyric anhydride (HFBA). The limits of detection and quantification were 3.00 and 10.0 μg/L, respectively. The calibration curves were linear up to 1000 μg/L (R(2)≥0.991). Absolute recovery ranged from 94.2 to 101%. Accuracy was found to be between -8.7 and 1.9% and imprecision was less than 10.0%. The developed method covers the generally accepted therapeutic range but it can also cover levels above them. This makes our method suitable for the determination of amisulpride not only for clinical purposes on psychiatric patients, but also during the investigation of forensic cases where amisulpride is involved.

  6. Analysis of organic contaminants from silicon wafer and disk surfaces by thermal desorption-GC-MS

    Science.gov (United States)

    Camenzind, Mark J.; Ahmed, Latif; Kumar, Anurag

    1999-03-01

    Organic contaminants can affect semiconductor wafer processing including gate oxide integrity, polysilicon growth, deep ultraviolet photoresist line-width, and cleaning & etching steps. Organophosphates are known to counter dope silicon wafers. Organic contaminants in disk drives can cause failures due to stiction or buildup on the heads. Therefore, it is important to identify organic contaminants adsorbed on wafer or disk surfaces and find their sources so they can be either completely eliminated or at least controlled. Dynamic headspace TD-GC-MS (Thermal Desorption-Gas Chromatography-Mass Spectrometry) methods are very sensitive and can be used to identify organic contaminants on disks and wafers, in air, or outgassing from running drives or their individual components.

  7. Differentiation of Toxic Molds via Headspace SPME-GC/MS and Canine Detection

    Directory of Open Access Journals (Sweden)

    Kenneth G. Furton

    2007-08-01

    Full Text Available Indoor mold growth has recently become a concern in the legal world in regards to insurance litigation. Hazardous mold exposure to humans has been linked to many acute and chronic adverse health effects including death. As it grows, mold produces several types of primary and secondary metabolites, including microbial volatile organic compounds (MVOCs. Microbial volatile organic compound emission may be used as a preliminary indication of a mold infestation that is invisible to the unaided eye. The objective of the study is to identify the unique odor signatures of three species of molds, Aspergillus versicolor, Penicillium chrysogenum, and Stachybotrys chartarum by SPME-GC/MS analysis. Determining the compounds that are emitted by the selected species has made it possible to conduct validation studies of canine detection of these mold species through a series of field tests.

  8. [Study on the chemical compositions of VOCs emitted by cooking oils based on GC-MS].

    Science.gov (United States)

    He, Wan-Qing; Nie, Lei; Tian, Gang; Li, Jing; Shao, Xia; Wang, Min-Yan

    2013-12-01

    Volatile organic compounds (VOCs) are key precursors of ozone and secondary organic aerosols in air, and the differences in the compositions of VOCs lead to their different contribution to atmospheric reaction. Cooking oil fume is one of the important sources of atmospheric VOCs, and its chemical compositions are distinct under different conditions of oil types, food types, cooking methods and heating temperatures etc. In this study, the production of cooking oil fume was simulated by heating typical pure vegetable oils (peanut oil, sunflower oil, soybean oil, olive oil and blend oil) at different temperatures in beakers to investigate the chemical compositions of VOCs. The emitted VOCs were sampled with a Tenax adsorption tube and analyzed using GC-MS after thermal desorption. According to spectral library search and map analysis, using area normalized semi-quantitative method, preliminary qualitative and quantitative tests were conducted for the specific components of VOCs under different conditions.

  9. Identification and measurement of pesticide contaminants in food products by electron impact GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Tusa, Florina; Moldovan, Zaharie [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Vlassa, Mircea, E-mail: zaharie.moldovan@itim-cj.r [Faculty of Chemistry and Chemical Engineering, Babes Bolyai University, 11 Arany Janos, 400028 Cluj-Napoca (Romania)

    2009-08-01

    The paper concern is determination of eight pesticides in food products samples. The target compounds are: Lindane, Heptachlor, Aldrin, o,p-DDE, Dieldrin, Endrin, p,p'-DDT, and Methoxychlor. The compounds quantities were performed from chromatographic area obtained in full scan GC/MS mode after baseline separation and by comparation with surrogate internal standard area (Diphenylamine). The samples were concentrated by extraction with organic solvents (acetone) by Solid-Liquid Extraction (SLE) procedures the recovery factors being better than 80% except for Heptachlors. The coefficient of correlation of detector response function was better than 0.913 and LOQ under 0.015 {mu}g/g. The method enables to determine pesticides at low {mu}g/g in food supplements.

  10. Fully Automated Trimethylsilyl (TMS Derivatisation Protocol for Metabolite Profiling by GC-MS

    Directory of Open Access Journals (Sweden)

    Erica Zarate

    2016-12-01

    Full Text Available Gas Chromatography-Mass Spectrometry (GC-MS has long been used for metabolite profiling of a wide range of biological samples. Many derivatisation protocols are already available and among these, trimethylsilyl (TMS derivatisation is one of the most widely used in metabolomics. However, most TMS methods rely on off-line derivatisation prior to GC-MS analysis. In the case of manual off-line TMS derivatisation, the derivative created is unstable, so reduction in recoveries occurs over time. Thus, derivatisation is carried out in small batches. Here, we present a fully automated TMS derivatisation protocol using robotic autosamplers and we also evaluate a commercial software, Maestro available from Gerstel GmbH. Because of automation, there was no waiting time of derivatised samples on the autosamplers, thus reducing degradation of unstable metabolites. Moreover, this method allowed us to overlap samples and improved throughputs. We compared data obtained from both manual and automated TMS methods performed on three different matrices, including standard mix, wine, and plasma samples. The automated TMS method showed better reproducibility and higher peak intensity for most of the identified metabolites than the manual derivatisation method. We also validated the automated method using 114 quality control plasma samples. Additionally, we showed that this online method was highly reproducible for most of the metabolites detected and identified (RSD < 20 and specifically achieved excellent results for sugars, sugar alcohols, and some organic acids. To the very best of our knowledge, this is the first time that the automated TMS method has been applied to analyse a large number of complex plasma samples. Furthermore, we found that this method was highly applicable for routine metabolite profiling (both targeted and untargeted in any metabolomics laboratory.

  11. Outdoor and indoor benzene evaluation by GC-FID and GC-MS/MS.

    Science.gov (United States)

    Sousa, José A; Domingues, Valentina F; Rosas, Mónica S; Ribeiro, Susana O; Alvim-Ferraz, Conceiçao M; Delerue-Matos, Cristina F

    2011-01-01

    The evaluation of benzene in different environments such as indoor (with and without tobacco smoke), a city area, countryside, gas stations and near exhaust pipes from cars running on different types of fuels was performed. The samples were analyzed using gas chromatography (GC) with flame ionization detection (FID) and tandem mass spectrometric detection (MS/MS) (to confirm the identification of benzene in the air samples). Operating conditions for the GC-MS analysis were optimized as well as the sampling and sample preparation. The results obtained in this work indicate that i) the type of fuel directly influences the benzene concentration in the air. Gasoline with additives provided the highest amount of benzene followed by unleaded gasoline and diesel; ii) the benzene concentration in the gas station was always higher than the advisable limit established by law (5 μg m⁻³) and during the unloading of gasoline the achieved concentration was 8371 μg m⁻³; iii) the data from the countryside (Taliscas) and the urban city (Matosinhos) were below 5 μg m⁻³ except 5 days after a fire on a petroleum refinery plant located near the city; iv) it was proven that in coffee shops where smoking is allowed the benzene concentration is higher (6 μg m⁻³) than in coffee shops where this is forbidden (4 μg m⁻³). This method may also be helpful for environmental analytical chemists who use GC-MS/MS for the confirmation or/and quantification of benzene.

  12. Rapid GC-MS confirmation of amphetamines in urine by extractive acylation.

    Science.gov (United States)

    Marais, Adriaan A S; Laurens, Johannes B

    2009-01-10

    Amphetamine and related derivatives are widely abused central- and psychostimulants. Detection of certain derivatives, such as methcathinone, by commonly available immunoassay screening techniques is insufficient. Multi-analyte confirmations for amphetamine type stimulants are therefore required, but traditional gas chromatography-mass spectrometry methods necessitate lengthy analytical procedures with prolonged sample turn-around times. A validated rapid GC-MS assay for urinary confirmation of amphetamine, methamphetamine, methcathinone, ephedrine, norephedrine, methylenedioxyamphetamine, methylenedioxymethamphetamine, methylenedioxyethylamphetamine and N-methyl-1-(3,4 methylenedioxyphenyl)-2-butanamine is reported. The method entailed in situ derivatization of urine specimens by extractive acylation with pentafluoropropionic anhydride, followed by rapid chromatography on a microbore capillary column. Analytes were separated in less than 3 min and quantified simultaneously by selected-ion monitoring using stable isotope substituted internal standards. The total instrument cycle-time was 6 min per sample. The limits of detection were between 1.5 ng/mL and 6.25 ng/mL for the various analytes. Intermediate precision and accuracy were in the range of 6.3-13.8% and 90.5-107.3% for the respective analytes at the lower limit of quantitation, and between 5.8-12.6% and 95.4-103.1% for the high control. Long-term storage of methcathinone positive specimens at -20 degrees C proved insufficient stability of this analyte. The proposed assay is precise and accurate for confirmation of amphetamine and derivatives in urine. The complementary approach of extractive-derivatization and fast GC-MS analysis is especially applicable in routine clinical settings where reduced sample turn-around times are required. Further investigation of cathinone as a possible metabolite of methcathinone is warranted, based on results from analyzed authentic urine samples.

  13. GC-MS analysis of clove (Syzygium aromaticum) bud essential oil from Java and Manado

    Science.gov (United States)

    Amelia, B.; Saepudin, E.; Cahyana, A. H.; Rahayu, D. U.; Sulistyoningrum, A. S.; Haib, J.

    2017-07-01

    The largest clove production contributors in Indonesia are mostly coming from Java and Manado. Different flavor among clove origins is caused by chemical constituents in clove oil. Unfortunately, scientific research and publications about flavor in clove from Indonesia's origin are still limited. The objective of this research is to determine significant differences of constituents in terms of flavor in clove oil originated from Java and Manado. The essential oils were isolated from cut clove bud samples by steam distillation method. The chemical constituents of clove bud oil were analyzed by using gas chromatography-mass spectrometry (GC-MS). Constituents were then identified by comparing the results of the chromatogram and reference retention time using Wiley mass spectra library (Wiley W9N11). Thirty-six and thirty-four chemical constituents were identified based on GC-MS from clove oil collected from Java and Manado, respectively. Major classes of compounds are sesquiterpenes, phenyl propanoid, oxygenated sesquiterpenes, and esters. Different compositions in major constituents were found between both origins. Clove Java contained eugenol (55.60 %), eugenyl acetate (20.54 %), caryophyllene (14.84 %), and α-humulene (2.75 %). While, in clove Manado, the composition were eugenol (74.64 %), caryophyllene (12.79 %), eugenyl acetate (8.70 %), and α-humulene (1.53 %). Moreover, minor constituents β-elemene (0.04 %), α-cadinene (0.05 %) and ledol (0.06 %) were existed only in clove Java, while clove Manado had some unique minor constituents which were not found in clove Java, i.e. β-gurjunene (0.04 %), γ-cadinene %), and humulene oxide (0.05 %). In conclusion, both clove oils from Java and Manado contained same major chemical constituents but different in their composition. In addition, some minor constituents existed only in specific origin.

  14. Pyrolysis characteristic of tobacco stem studied by Py-GC/MS, TG-FTIR, and TG-MS

    Directory of Open Access Journals (Sweden)

    Bei Liu

    2013-02-01

    Full Text Available Pyrolysis characteristics and mechanism of tobacco stem were studied by pyrolysis coupled with gas chromatography/mass spectrometry (Py-GC/MS, thermogravimetric analyzer coupled with Fourier transform infrared spectrometry, and mass spectrometry (TG-FTIR and TG-MS techniques. The composition of evolved volatiles from fast pyrolysis of tobacco stem was determined by Py-GC/MS analysis, and the evolution patterns of the major products were investigated by TG-FTIR and TG-MS. Py-GC/MS data indicated that furfural and phenol were the major products in low temperature pyrolysis, and these were generated from depolymerization of cellulose. Indene and naphthalene were the major products in high temperature pyrolysis. TG-FTIR and TG-MS results showed that CO, CO2, phenols, aldehydes, and ketones were released between 167ºC and 500ºC; at temperatures >500ºC, CO and CO2 were the main gaseous products.

  15. Advanced Situation Awareness Technologies Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Advanced Situation Awareness Technologies (ASAT) will facilitate exploration of the moon surface, and other planetary bodies. ASAT will create an Advanced Situation...

  16. The analysis of aroma components in marjoram oil by GC/MS%GC/MS 法分析甘牛至油中香味成分

    Institute of Scientific and Technical Information of China (English)

    李源栋; 刘秀明; 冒德寿; 夏建军; 者为; 段焰青

    2016-01-01

    The aroma components of marjoram oil were analyzed by GC /MS,and the peak area normaliza-tion method was used to calculate the relative content of each component.With the mass spectrometry li-brary search,58 compounds which account for 95.61% in the aroma components of marjoram oil,were identified by using reference literature,retention index.The cis(trans)-isomers isomers were confirmed by using retention index,and the accuracy of compound qualitative analysis in natural flavor was im-proved.The aroma of the key aroma compositions of the marjoram oil (linalool,alpha -terpineol,1,8 -cineole,linalyl acetate,alpha pinene,beta -pinene,myrcene,camphene,beta -caryophyllene, sabinene,camphor,borneol,et al)was determined,and the results provided the technical support for the development and application of marjoram oil.%利用 GC /MS 对甘牛至油中香味成分进行了分析,并用峰面积归一化法计算各成分相对含量,通过质谱库检索,保留指数比对,分析并确定了58个化合物,占甘牛至油香味成分95.61%,采用保留指数来鉴别同系物及同分异构体,提高了对甘牛至油中成分定性的准确性。通过香气分析,确定了甘牛至油中关键致香成分分别为芳樟醇、α-松油醇、1,8-桉叶素、乙酸芳樟酯、α-蒎烯、β-蒎烯、月桂烯、莰烯、β-石竹烯、桧烯、樟脑、龙脑等,为甘牛至油产品开发和应用提供了理论依据。

  17. Using Py-GC/MS to detect and measure silicone defoamers in pulp fibres and mill deposits

    CSIR Research Space (South Africa)

    Sithole, Bruce

    2013-09-01

    Full Text Available cause pitch deposition in pulp and paper making operations. Please cite this article in press as: B. Sithole, C. Watanabe, Using Py-GC/MS to detect and measure silicone defoamers in pulp fibres and mill deposits, J. Anal. Appl. Pyrol. (2012), http... cite this article in press as: B. Sithole, C. Watanabe, Using Py-GC/MS to detect and measure silicone defoamers in pulp fibres and mill deposits, J. Anal. Appl. Pyrol. (2012), http://dx.doi.org/10.1016/j.jaap.2012.08.013 ARTICLE IN PRESSG ModelJAAP 2804...

  18. GC/MS analytical procedure for the characterization of glycerolipids, natural waxes, terpenoid resins, proteinaceous and polysaccharide materials in the same paint microsample avoiding interferences from inorganic media.

    Science.gov (United States)

    Lluveras, Anna; Bonaduce, Ilaria; Andreotti, Alessia; Colombini, Maria Perla

    2010-01-01

    An innovative GC/MS procedure for the characterization of organic materials in samples from works of art was developed. It is based on a multistep chemical pretreatment of the samples based on the ammonia extraction of proteins and polysaccharide materials, in order to separate them from lipid and resinous materials. The extraction is then followed by the separation and purification of proteinaceous and polysaccharide materials before hydrolysis, based on the use of monolithic sorbent tip technology with a C4 stationary phase. Lipids and resins are saponified/salified separately. Three fractions are generated and analyzed separately by GC/MS, thus enabling a quantitative analysis to be performed on aldoses and uronic acids, amino acids, mono- and dicarboxylic aliphatic acids, to determine polysaccharide, proteinaceous, and glycerolipid materials and molecular pattern recognition for the natural resin and wax components. With this analytical procedure, for the first time, glycerolipids, natural waxes, and proteinaceous, resinous, and polysaccharide materials can be simultaneously characterized in the same microsample from painted works of art. This new analytical approach prevents any analytical difficulties arising when the sample is divided into several different aliquots to be chemically processed separately, in order to characterize the various classes of organic materials. The procedure was successfully applied to samples from paintings from the Bamiyan Buddhas and a panel painting from the 15th century, highlighting the occurrence of glycerolipids, animal and plant resins, proteinaceous and polysaccharide materials.

  19. Advanced Situation Awareness Technologies Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Advanced Situation Awareness Technologies (ASAT) will facilitate exploration of the moon surface, and other planetary bodies. This powerful technology will also find...

  20. Technologic advances in endodontics.

    Science.gov (United States)

    Mortman, Rory E

    2011-07-01

    This article addresses technologic advances in endodontics pertaining to new and emerging technology. Cone-beam computed tomography and optical occurrence tomography are 2 new imaging technologies that can assist the practitioner in the diagnosis of pulpal disease. The self-adjusting file and the Apexum device can be used for instrumentation and bulk debridement of an apical lesion, respectively. Neodymium:yttrium-aluminum-garnet laser, erbium:chromium:yttrium-scandium-gallium-garnet laser, EndoActivator, EndoVac, and light-activated disinfection may assist the practitioner in cleaning the root canal system. Computed tomography-guided surgery shows promise in making endodontic surgery easier, as does mineral trioxide aggregate cement for regenerative endodontic procedures.

  1. Characterization and Determination of 2-(2-Phenylethylchromones in Agarwood by GC-MS

    Directory of Open Access Journals (Sweden)

    Hao-Fu Dai

    2013-10-01

    Full Text Available Agarwood is the fragrant resinous heartwood obtained from certain trees in the genus Aquilaria belonging to the family Thymelaeaceae. 2-(2-Phenylethylchromones and characteristic sesquiterpenes are the main classes of aromatic compounds isolated from agarwood. Although there are many sesquiterpenes, relatively few 2-(2-phenylethylchromones have been determined in agarwood by GC-MS. After analysis of the MS spectra of eighteen 2-(2-phenylethylchromone derivatives isolated from agarwood and identified by NMR spectroscopy, together with the reported MS data and characteristic of structures of 2-(2-phenylethylchromones, the MS characterization, fragmentation patterns and characteristic fragment peaks for the compounds were deduced and a table summarizing MS characterization of 2-(2-phenylethylchromones in agarwood is presented. All the 2-(2-phenylethylchromones previously reported in agarwood are substituted by methoxy or/and hydroxy groups, except for one compound. Due to the fact they all possess the same basic skeleton (molecular weight: 250 and similar substituent groups (methoxy or hydroxy groups, a formula (30m + 16n = MW − 250 is provided to calculate the number of methoxy (m or hydroxy (n groups according to molecular ion peak or molecular weight (MW. We deduced that the characteristic fragmentation behaviors of the 2-(2-phenylethylchromones are the cleavages of the CH2-CH2 bond between chromone moiety and phenyl moiety. Thus, characteristic fragment ions, such as m/z 91 [C7H7], 107 [C7H6+OH], 121 [C7H6+OCH3], 137 [C7H5+OH+OCH3] are formed by different substituted benzyl moieties, while characteristic fragment ions such as m/z 160 [C10H8O2], 176 [C10H7O2+OH], 190 [C10H7O2+OCH3], 220 [C10H6O2+OCH3×2] are formed by different substituted chromone moieties. Furthermore, rules regarding to the relationship between the positions of hydroxy or methoxy groups and the relative abundances of benzyl and chromone fragment ions have been deduced

  2. Characterization and determination of 2-(2-phenylethyl)chromones in agarwood by GC-MS.

    Science.gov (United States)

    Mei, Wen-Li; Yang, De-Lan; Wang, Hao; Yang, Jin-Ling; Zeng, Yan-Bo; Guo, Zhi-Kai; Dong, Wen-Hua; Li, Wei; Dai, Hao-Fu

    2013-10-08

    Agarwood is the fragrant resinous heartwood obtained from certain trees in the genus Aquilaria belonging to the family Thymelaeaceae. 2-(2-Phenylethyl)chromones and characteristic sesquiterpenes are the main classes of aromatic compounds isolated from agarwood. Although there are many sesquiterpenes, relatively few 2-(2-phenylethyl)chromones have been determined in agarwood by GC-MS. After analysis of the MS spectra of eighteen 2-(2-phenylethyl)chromone derivatives isolated from agarwood and identified by NMR spectroscopy, together with the reported MS data and characteristic of structures of 2-(2-phenylethyl)chromones, the MS characterization, fragmentation patterns and characteristic fragment peaks for the compounds were deduced and a table summarizing MS characterization of 2-(2-phenylethyl)chromones in agarwood is presented. All the 2-(2-phenylethyl)chromones previously reported in agarwood are substituted by methoxy or/and hydroxy groups, except for one compound. Due to the fact they all possess the same basic skeleton (molecular weight: 250) and similar substituent groups (methoxy or hydroxy groups), a formula (30m + 16n = MW - 250) is provided to calculate the number of methoxy (m) or hydroxy (n) groups according to molecular ion peak or molecular weight (MW). We deduced that the characteristic fragmentation behaviors of the 2-(2-phenylethyl)chromones are the cleavages of the CH₂-CH₂ bond between chromone moiety and phenyl moiety. Thus, characteristic fragment ions, such as m/z 91 [C₇H₇], 107 [C₇H₆+OH], 121 [C₇H₆+OCH₃], 137 [C₇H5+OH+OCH₃] are formed by different substituted benzyl moieties, while characteristic fragment ions such as m/z 160 [C₁₀H₈O₂], 176 [C₁₀H₇O₂+OH], 190 [C₁₀H₇O₂+OCH₃], 220 [C₁₀H₆O₂+OCH₃×2] are formed by different substituted chromone moieties. Furthermore, rules regarding to the relationship between the positions of hydroxy or methoxy groups and the relative abundances of benzyl

  3. Steroids excreted in urine by neonates with 21-hydroxylase deficiency: characterization, using GC-MS and GC-MS/MS, of the D-ring and side chain structure of pregnanes and pregnenes.

    Science.gov (United States)

    Christakoudi, Sofia; Cowan, David A; Taylor, Norman F

    2010-01-01

    Steroid metabolites in urine from neonates with 21-hydroxylase deficiency are predominantly polyhydroxylated 17-hydroxyprogesterone and androgen metabolites, and most have incompletely defined structure. This study forms part of a comprehensive project to characterize and identify these in order to enhance diagnosis and to further elucidate neonatal types of steroid metabolism. Steroids were analyzed, after extraction and enzymatic conjugate hydrolysis, as methyloxime-trimethylsilyl ether derivatives on gas-chromatographs coupled to quadrupole and ion-trap mass-spectrometers. GC-MS and GC-MS/MS spectra, obtained with constant excitation conditions, were used together to determine the structure of the D-ring and the side chain of 20-oxo and 20-hydroxy pregnane(ene)s without oxo groups on the A-, B-, and C-ring. All possible combinations of D-ring and side chain configuration were considered. Most fragmentations could be interpreted as partial or complete D-ring cleavages with loss of the side chain, aided by comparison with spectra of deuterated derivatives and of borohydride reduced metabolites. Possible rearrangement ions are also discussed. More than 140 endogenous metabolites were characterized. GC-MS/MS was especially beneficial for characterization of compounds with 16,17-dihydroxy-20-oxo structure, interpreted as markers of intra-uterine enzyme induction. It also assisted the differentiation of 16-hydroxy-20-oxo metabolites, present in urine of non-affected neonates, from the diagnostic 17-hydroxy-20-oxosteroids and enabled the detection of 15,17-dihydroxy-20-oxo compounds in low concentrations. The presence of 17,21-dihydroxylated pregnane(ene)s despite the deficit in CYP21A2 is discussed. We conclude that GC-MS combined with GC-MS/MS allows reliable identification of the structure of the D-ring and side chain of pregnane(ene)s without prior isolation, even when in low concentrations in urine.

  4. Comparison of Michigan and Dutch podzolized soils: Organic matter characterization by micromorphology and pyrolysis-GC/MS

    NARCIS (Netherlands)

    Buurman, P.; Jongmans, A.G.; Nierop, K.G.J.

    2008-01-01

    Soil organic matter in a chronosequence of Michigan soils (Spodic Udipsamments and precursors) was studied in thin section and by pyrolysis-gas chromatography/mass spectrometry (GC/MS). The Michigan soils were compared with a well-drained Dutch Typic Haplorthod that was studied with the same methods

  5. Determination of Glyphosate Levels in Breast Milk Samples from Germany by LC-MS/MS and GC-MS/MS

    NARCIS (Netherlands)

    Steinborn, Angelika; Alder, Lutz; Michalski, Britta; Zomer, Paul; Bendig, Paul; Martinez, Sandra Aleson; Mol, Hans G.J.; Class, Thomas J.; Costa Pinheiro, Nathalie

    2016-01-01

    This study describes the validation and application of two independent analytical methods for the determination of glyphosate in breast milk. They are based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively. For L

  6. Headspace GC-MS Analysis of Halogenated Volatile Organic Compounds in Aqueous Samples: An Experiment for General Chemistry Laboratory

    Science.gov (United States)

    Keller, John W.; Fabbri, Cindy E.

    2012-01-01

    Analysis of halogenated volatile organic compounds (HVOCs) by GC-MS demonstrates the use of instrumentation in the environmental analysis of pollutant molecules and enhances student understanding of stable isotopes in nature. In this experiment, students separated and identified several HVOCs that have been implicated as industrial groundwater…

  7. Soil organic matter chemistry changes upon secondary succession in Imperata Grasslands , Indonesia: A pyrolysis - GC/MS study

    NARCIS (Netherlands)

    Yassir, I.; Buurman, P.

    2012-01-01

    The chemical composition of soil organic matter (SOM) following secondary succession in Imperata grassland was investigated by Pyrolysis-Gas Chromatography/Mass Spectrometry (GC/MS). We studied 46 samples from different stages of succession using plots that last burned 3 and 9 years previously,

  8. [Multiresidue method for determination of pesticides in fruits and vegetables by GC/MS (SCAN) and LC/MS (SIM)].

    Science.gov (United States)

    Kakimoto, Yoshihisa; Naetoko, Yoshitaka; Iwasaki, Yoshinari; Nakamura, Shigeru; Tatsuguchi, Hisako

    2005-08-01

    A rapid multiresidue method has been developed for determination of many pesticides in fruits and vegetables using GC/MS and LC/MS. The method of analysis was the same as that reported by Kakimoto et al. in 2003 except for the use of LC/MS. Good recoveries in the range of 70-120% were obtained for 70 (32 by GC/MS, 38 by LC/MS) of 113 pesticides spiked at 0.1 microg/g into fruits and vegetables. For screening purposes, the method could be appiled to 82 pesticides. Considering the report by Kakimoto et al. in 2004, 177 pesticides were suitable for screening by this method. The limits of detection were 0.001-0.015 microg/g (by GC/MS) and < 0.001-0.010 microg/g (by LC/MS). The calibration curves were linear for most pesticides, with correlation coefficients of 0.976-1.000 (by GC/MS) and 0.968-1.000 (by LC/MS). The values obtained for fruits and vegetables naturally contaminated with pesticides by this method were nearly equal to those by the official method.

  9. Got a Match? Ion Extraction GC-MS Characterization of Accelerants Adsorbed in Charcoal Using Negative Pressure Dynamic Headspace Concentration

    Science.gov (United States)

    Anzivino, Barbara; Tilley, Leon J.; Ingalls, Laura R.; Hall, Adam B.; Drugan, John E.

    2009-01-01

    An undergraduate organic chemistry experiment demonstrating real-life application of GC-MS to arson accelerant identification is described. Students are given the task of comparing a sample recovered from a "crime scene" to that from a "suspect's clothing". Accelerants subjected to different conditions are recovered using a quick and simple…

  10. Investigation into some aspects of EMIT d.a.u., TLC, and GC-MS urinalysis of bromazepam.

    Science.gov (United States)

    El-Haj, B M; Al-Amri, A M; Hassan, M H; Bin-Khadem, R K

    2001-01-01

    Among the different 1,4-benzodiazepine urinary metabolites, those of bromazepam possess distinctive chemical features that may be used in their selective isolation and detection. The detection of bromazepam metabolites in urine was carried out using EMIT d.a.u., thin-layer chromatography (TLC), and gas chromatography-mass spectrometry (GC-MS). The positive EMIT d.a.u. benzodiazepine assay for bromazepam was found to be due to the 3-hydroxybromazepam (3HOB) metabolite. The detection by TLC and GC-MS was carried out after enzyme or acid hydrolysis of the glucuronide conjugates. Both the 2-amino-3-hydroxy5-bromobenzoylpyridine (AHBBP) metabolite and the acid hydrolysis product of 3-HOB, 2-amino-5-bromobenzoylpyridine (ABBP), were selectively detected by TLC. The bromazepam metabolites in urine could be both isolated and detected selectively by GC-MS in the presence of the metabolites of other 1,4-benzodiazepines that were sometimes used in combination with bromazepam. Both 3-HOB and AHBBP were detected by GC-MS only after trimethylsilyl (TMS) derivatization and not as the free compounds or the acetyl derivatives. Only ABBP was detected in three forms: ABBP, the TMS derivative, and the acetyl derivative. Evidence has been obtained from the enzyme hydrolysis and the TLC studies for the formation of the glucuronide conjugate of AHBBP at the 3-OH group rather than at the 2-NH2 group. All the results have been validated using reference 3-HOB and AHBBP.

  11. Bromination of Aromatic Compounds by Residual Bromide in Sodium Chloride Matrix Modifier Salt During Heated Headspace GC/MS Analysis

    Science.gov (United States)

    Analytical artifacts attributed to the bromination of toluene, xylenes, and trimethylbenzenes were found during the heated headspace gas chromatography/mass spectrometry (GC/MS) analysis of aqueous samples. The aqueous samples were produced from Fenton-like chemical oxidation rea...

  12. [Analysis of headspace constituents of Gardenia flower by GC/MS with solid-phase microextraction and dynamic headspace sampling].

    Science.gov (United States)

    Liu, B Z; Gao, Y

    2000-09-01

    The headspace constituents of fresh Gardenia flower were investigated by GC/MS. The headspace volatiles were sampled by solid-phase microextraction (SPME) and dynamic headspace sampling (DHS). SPME sampling was conducted with 100 microns PDMS fiber at 28 degrees C for 60 min. In DHS sampling, purified nitrogen was used as purging gas with a flow rate at 80 mL/min for 120 min. Tenax GR(20 mesh-40 mesh) was used as adsorbent and the volatiles were eluted by ether, and concentrated to 0.5 mL for GC/MS analysis. A Supelco-wax capillary column (30 m x 0.25 mm i.d. x 0.25 micron df) was employed in GC/MS analysis. Initial oven temperature was kept at 45 degrees C for 2 min, then raised to 250 degrees C at 4 degrees C/min, and kept at 250 degrees C for 10 min. According to SPME-GC/MS analysis, the main compounds in headspace of fresh Gardenia flower included farnesene(64.86%), cis-ocimene(29.33%), linalool(2.74%), cis-3-hexenyl tiglate(1.34%), methyl benzoate(0.25%). Results obtained from SPME and DHS sampling were also compared. In this study, SPME afforded a simpler and more sensitive sampling method, and much more accurate information about headspace volatiles of Gardenia flower.

  13. Determination of Glyphosate Levels in Breast Milk Samples from Germany by LC-MS/MS and GC-MS/MS

    NARCIS (Netherlands)

    Steinborn, Angelika; Alder, Lutz; Michalski, Britta; Zomer, Paul; Bendig, Paul; Martinez, Sandra Aleson; Mol, Hans G.J.; Class, Thomas J.; Costa Pinheiro, Nathalie

    2016-01-01

    This study describes the validation and application of two independent analytical methods for the determination of glyphosate in breast milk. They are based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively. For L

  14. Metabolic profiling for studying chemotype variations in Withania somnifera (L.) Dunal fruits using GC-MS and NMR spectroscopy.

    Science.gov (United States)

    Bhatia, Anil; Bharti, Santosh K; Tewari, Shri K; Sidhu, Om P; Roy, Raja

    2013-09-01

    Withania somnifera (L.) Dunal (Solanaceae), commonly known as Ashwagandha, is one of the most valued Indian medicinal plant with several pharmaceutical and nutraceutical applications. Metabolic profiling was performed by GC-MS and NMR spectroscopy on the fruits obtained from four chemotypes of W. somnifera. A combination of (1)H NMR spectroscopy and GC-MS identified 82 chemically diverse metabolites consisting of organic acids, fatty acids, aliphatic and aromatic amino acids, polyols, sugars, sterols, tocopherols, phenolic acids and withanamides in the fruits of W. somnifera. The range of metabolites identified by GC-MS and NMR of W. somnifera fruits showed various known and unknown metabolites. The primary and secondary metabolites observed in this study represent MVA, DOXP, shikimic acid and phenylpropanoid biosynthetic metabolic pathways. Squalene and tocopherol have been rated as the most potent naturally occurring compounds with antioxidant properties. These compounds have been identified by us for the first time in the fruits of W. somnifera. Multivariate principal component analysis (PCA) on GC-MS and NMR data revealed clear distinctions in the primary and secondary metabolites among the chemotypes. The variation in the metabolite concentration among different chemotypes of the fruits of W. somnifera suggest that specific chemovars can be used to obtain substantial amounts of bioactive ingredients for use as potential pharmacological and nutraceuticals agents.

  15. Buildings for advanced technology

    CERN Document Server

    Teague, E; Murday, James

    2015-01-01

    This book deals with the design and construction of buildings for nanoscale science and engineering research. The information provided in this book is useful for designing and constructing buildings for such advanced technologies as nanotechnology, nanoelectronics and biotechnology. The book outlines the technology challenges unique to each of the building environmental challenges outlined below and provides best practices and examples of engineering approaches to address them: • Establishing and maintaining critical environments: temperature, humidity, and pressure • Structural vibration isolation • Airborne vibration isolation (acoustic noise) • Isolation of mechanical equipment-generated vibration/acoustic noise • Cost-effective power conditioning • Grounding facilities for low electrical interference • Electromagnetic interference (EMI)/Radio frequency interference (RFI) isolation • Airborne particulate contamination • Airborne organic and chemical contamination • Environment, safety a...

  16. Advanced finite element technologies

    CERN Document Server

    Wriggers, Peter

    2016-01-01

    The book presents an overview of the state of research of advanced finite element technologies. Besides the mathematical analysis, the finite element development and their engineering applications are shown to the reader. The authors give a survey of the methods and technologies concerning efficiency, robustness and performance aspects. The book covers the topics of mathematical foundations for variational approaches and the mathematical understanding of the analytical requirements of modern finite element methods. Special attention is paid to finite deformations, adaptive strategies, incompressible, isotropic or anisotropic material behavior and the mathematical and numerical treatment of the well-known locking phenomenon. Beyond that new results for the introduced approaches are presented especially for challenging nonlinear problems.

  17. State Technologies Advancement Collaborative

    Energy Technology Data Exchange (ETDEWEB)

    David S. Terry

    2012-01-30

    The U. S. Department of Energy (DOE), National Association of State Energy Officials (NASEO), and Association of State Energy Research and Technology Transfer Institutions (ASERTTI) signed an intergovernmental agreement on November 14, 2002, that allowed states and territories and the Federal Government to better collaborate on energy research, development, demonstration and deployment (RDD&D) projects. The agreement established the State Technologies Advancement Collaborative (STAC) which allowed the states and DOE to move RDD&D forward using an innovative competitive project selection and funding process. A cooperative agreement between DOE and NASEO served as the contracting instrument for this innovative federal-state partnership obligating funds from DOE's Office of Energy Efficiency and Renewable Energy and Office of Fossil Energy to plan, fund, and implement RDD&D projects that were consistent with the common priorities of the states and DOE. DOE's Golden Field Office provided Federal oversight and guidance for the STAC cooperative agreement. The STAC program was built on the foundation of prior Federal-State efforts to collaborate on and engage in joint planning for RDD&D. Although STAC builds on existing, successful programs, it is important to note that it was not intended to replace other successful joint DOE/State initiatives such as the State Energy Program or EERE Special Projects. Overall the STAC process was used to fund, through three competitive solicitations, 35 successful multi-state research, development, deployment, and demonstration projects with an overall average non-federal cost share of 43%. Twenty-two states were awarded at least one prime contract, and organizations in all 50 states and some territories were involved as subcontractors in at least one STAC project. Projects were funded in seven program areas: (1) Building Technologies, (2) Industrial Technologies, (3) Transportation Technologies, (4) Distributed Energy

  18. Mathematical Model Developed for Environmental Samples: Prediction of GC/MS Dioxin TEQ from XDS-CALUX Bioassay Data

    Science.gov (United States)

    Brown, David J.; Orelien, Jean; Gordon, John D.; Chu, Andrew C.; Chu, Michael D.; Nakamura, Masafumi; Handa, Hiroshi; Kayama, Fujio; Denison, Michael S.; Clark, George C.

    2010-01-01

    Remediation of hazardous waste sites requires efficient and cost-effective methods to assess the extent of contamination by toxic substances including dioxin-like chemicals. Traditionally, dioxin-like contamination has been assessed by gas chromatography/high-resolution mass spectrometry (GC/MS) analysis for specific polychlorinated dibenzo-p-dioxins, dibenzofurans, and biphenyl congeners. Toxic equivalency factors for these congeners are then used to estimate the overall dioxin toxic equivalency (TEQ) of complex mixtures found in samples. The XDS-CALUX bioassay estimates contamination by dioxin-like chemicals in a sample extract by measuring expression of a sensitive reporter gene in genetically engineered cells. The output of the XDS-CALUX assay is a CALUX-TEQ value, calibrated based on TCDD standards. Soil samples taken from a variety of hazardous waste sites were measured using the XDS-CALUX bioassay and GC/MS. TEQ and CALUX-TEQ from these methods were compared, and a mathematical model was developed describing the relationship between these two data sets: log(TEQ) = 0.654 × log(CALUX-TEQ) + 0.058-(log(CALUX-TEQ))2. Applying this equation to these samples showed that predicted and GC/MS measured TEQ values strongly correlate (R2 = 0.876) and that TEQ values predicted from CALUX-TEQ were on average nearly identical to the GC/MS-TEQ. The ability of XDS-CALUX bioassay data to predict GC/MS-derived TEQ data should make this procedure useful in risk assessment and management decisions. PMID:17626436

  19. Serum and urine concentrations of flunitrazepam and metabolites, after a single oral dose, by immunoassay and GC-MS.

    Science.gov (United States)

    Snyder, H; Schwenzer, K S; Pearlman, R; McNally, A J; Tsilimidos, M; Salamone, S J; Brenneisen, R; ElSohly, M A; Feng, S

    2001-01-01

    A clinical study was conducted to assess the ability of commercially available immunoassays to detect flunitrazepam (FNP) in plasma and urine samples and to compare the results with those obtained by gas chromatography-mass spectrometry (GC-MS). The clinical study consisted of four individuals (two male and two female) who had taken a single 2-mg dose of FNP. Serum was collected over a 48-h period and urine was collected over a 72-h period. The serum and urine samples were analyzed by the COBAS INTEGRA Serum Benzodiazepines assay (SBENZ), the TDx serum and urine Benzodiazepines assay, and GC-MS. The GC-MS procedure was developed for analysis of FNP and metabolites in plasma and urine using an acid hydrolysis step resulting in the formation of specific benzophenones corresponding to FNP and its metabolites. The relative sensitivities of the assays for the detection of FNP and metabolites in serum and urine were GC-MS > SBENZ > TDx. The immunoassay results for serum samples showed peak concentrations of FNP metabolites at 8 h after FNP ingestion for three individuals and at about 1 h for the fourth individual. The GC-MS, SBENZ, and TDx urine immunoassays detected drug above the stated limit of detection (LOD) in 44, 41, and 35 serial FNP urine samples, respectively. FNP metabolites were detected in urine samples with all three assays for up to 72 h after a 2-mg dose. The improved detection rate with the SBENZ assay as compared to the TDx assay is likely explained by its higher cross-reactivity with the major metabolite, 7-amino-flunitrazepam (7-amino-FNP), and its lower LOD.

  20. Advanced Crystal Growth Technology

    Energy Technology Data Exchange (ETDEWEB)

    Land, T A; Hawley-Fedder, R A

    2005-03-01

    Although the fundamental mechanism of crystal growth has received and continues to receive deserved attention as a research activity, similar research efforts addressing the need for advanced materials and processing technology required to grow future high quality crystals has been sorely lacking. The purpose of this research effort is to develop advanced rapid growth processing technologies and materials suitable for providing the quality of products needed for advanced laser and photonics applications. In particular we are interested in developing a methodology for growing high quality KDP crystals based on an understanding of the fundamental mechanisms affecting growth. One problem in particular is the issue of control of impurities during the growth process. Many unwanted impurities are derived from the growth system containers and can adversely affect the optical quality and aspect ratio (shape) of the crystals. Previous studies have shown that even trace concentrations ({approx}10{sup -9} M) of impurities affect growth and even 'insignificant' species can have a large impact. It is also known that impurities affect the two growth faces of KDP very differently. Traces of trivalent metal impurities such as Fe{sup 3+}, Cr{sup 3+}, and Al{sup 3+} in solution are known to inhibit growth of the prismatic {l_brace}100{r_brace} faces of KDP while having little effect on the growth of the pyramidal {l_brace}101{r_brace} faces. This differentiation opens the possibility of intentionally adding select ions to control the aspect ratio of the crystal to obtain a more advantageous shape. This document summarizes our research efforts to improve KDP crystal growth. The first step was to control unwanted impurity addition from the growth vessel by developing an FEP liner to act as a barrier to the glass container. The other focus to develop an understanding of select impurities on growth rates in order to be able to use them to control the habit or shape of the

  1. Fast Pyrolysis of Four Lignins from Different Isolation Processes Using Py-GC/MS

    Directory of Open Access Journals (Sweden)

    Xiaona Lin

    2015-06-01

    Full Text Available Pyrolysis is a promising approach that is being investigated to convert lignin into higher value products including biofuels and phenolic chemicals. In this study, fast pyrolysis of four types of lignin, including milled Amur linden wood lignin (MWL, enzymatic hydrolysis corn stover lignin (EHL, wheat straw alkali lignin (AL and wheat straw sulfonate lignin (SL, were performed using pyrolysis gas-chromatography/mass spectrometry (Py-GC/MS. Thermogravimetric analysis (TGA showed that the four lignins exhibited widely different thermolysis behaviors. The four lignins had similar functional groups according to the FTIR analysis. Syringyl, guaiacyl and p-hydroxyphenylpropane structural units were broken down during pyrolysis. Fast pyrolysis product distributions from the four lignins depended strongly on the lignin origin and isolation process. Phenols were the most abundant pyrolysis products from MWL, EHL and AL. However, SL produced a large number of furan compounds and sulfur compounds originating from kraft pulping. The effects of pyrolysis temperature and time on the product distributions from corn stover EHL were also studied. At 350 °C, EHL pyrolysis mainly produced acids and alcohols, while phenols became the main products at higher temperature. No obvious influence of pyrolysis time was observed on EHL pyrolysis product distributions.

  2. [GC-MS analysis of essential oil from Curcuma aromatica rhizome of different growth periods].

    Science.gov (United States)

    Feng, Jie; Xu, Ming-ming; Huang, Xiu-lan; Liu, Hua-gang; Lai, Mao-xiang; Wei, Meng-han

    2013-12-01

    To analyze the essential oil from the rhizome of Curcuma aromatica of different growth periods, and to provide the scientific reference for reasonable cultivation and quality control of this plant. The essential oil was extracted by hydrodistillation and analyzed with GC-MS. The relative contents were determined with area normalization method. The main volatile constituents in the rhizome of Curcuma aromatica were basically the same. Among these volatile constituents, curdione was the major. The relative content of curdione was 16.35% in the rhizome of wild plant in Hengxian county, and 15.81% in the rhizome of one-year-old plant in Mingyang farm, Nanning city. The relative content of eucalyptol in the 2-year-old cultivated rhizome in Hengxian county was 15.40%, and 14.59% in the rhizome of wild plant in Hengxian county. beta-Elemene, beta-caryophyllene,eugenol and germacrone were also the main constituents in the rhizome essential oil. Volatile constituents in the rhizome of Curcuma aromatica are similar to each other,but the relative content of each component is different. This result can provide the scientific foundation for the cultivation of Curcuma aromatica.

  3. In Vitro Antimicrobial, Antioxidant, Cytotoxicity and GC-MS Analysis of Mazus goodenifolius

    Directory of Open Access Journals (Sweden)

    Muhammad Riaz

    2012-12-01

    Full Text Available The antimicrobial, antioxidant and cytotoxic properties of Mazus goodenifolius (Hornem. Pennell essential oil, methanol extract and some solvent-extracted subfractions of the latter were appraised. A qualitative, quantitative analysis of the classes of phytochemicals in the various fractions and GC-MS analysis of the essential oil was carried out. The activity of the plant extract and various subfractions against selected bacterial (Pasturella multocida, Escherichia coli, Bacillus subtilis and Staphylococcus aureus and fungal strains (Aspergillus niger, Aspergillus flavus, Alternaria alternata and Rhizopus solani was evaluated. The antioxidant activity was assayed using the DPPH radical scavenging and % inhibition of linoleic acid peroxidation tests. In the DPPH radical scavenging test the IC50 values ranged from 7.21 to 91.79 µg/mL, and in the latter the range of % peroxidation inhibition was 35.42–93.48%. Protective effects of the absolute methanol extract, which had the highest content of phenolics and flavonoids, against H2O2 induced oxidative damage in plasmid pBR322 DNA was also evaluated, and it was found to offer some protection at the highest tested dose (1,000 µg/mL. Finally the cytotoxicity of the plant extract, fractions and essential oil was analyzed by examining haemolytic activity against human blood erythrocytes (RBCs, whereby the % lysis of RBCs was found to be in the range of 1.65 to 4.01%.

  4. GC-MS Analysis of Insecticidal Essential Oil of Flowering Aerial Parts of Saussurea Nivea Turcz

    Directory of Open Access Journals (Sweden)

    Zhi Long Liu

    2012-08-01

    Full Text Available Background:Several species from Saussurea have been used in the traditional medicine, such as S. lappa, S. involucrate, and S. obvallata. There is no report on medicinal use of S. nivea. The aim of this research was to determine chemical composition and insecticidal activity of the essential oil of S. nivea Turcz (Asteraceae aerial parts against maize weevils (Sitophilus zeamais Motschulsky for the first time.Results:Essential oil of S. nivea flowering aerial parts was obtained by hydrodistillation and analyzed by gas chromatography--mass spectrometry (GC-MS. A total of 43 components of the essential oil of S. nivea were identified. The principal compounds in the essential oil were (+-limonene (15.46%, caryophyllene oxide (7.62%, linalool (7.20%, alpha-pinene (6.43%, beta-pinene (5.66% and spathulenol (5.02% followed by beta-eudesmoll (4.64% and eudesma-4,11-dien-2-ol (3.76%. The essential oil of S. nivea exhibited strong contact toxicity against S. zeamais with an LD50 value of 10.56 mug/adult. The essential oil also possessed fumigant toxicity against S. zeamais with an LC50 value of 8.89 mg/L.Conclusion: The study indicates that the essential oil of S. nivea flowering aerial parts has a potential for development into a natural insecticide/fumigant for control of insects in stored grains.

  5. Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

    Directory of Open Access Journals (Sweden)

    Lidong Cao

    2013-01-01

    Full Text Available The toxic inert ingredients in pesticide formulations are strictly regulated in many countries. In this paper, a simple and efficient headspace-gas chromatography-mass spectrometry (HSGC-MS method using fluorobenzene as an internal standard (IS for rapid simultaneous determination of benzene and toluene in pesticide emulsifiable concentrate (EC was established. The headspace and GC-MS conditions were investigated and developed. A nonpolar fused silica Rtx-5 capillary column (30 m×0.20 mm i.d. and 0.25 μm film thickness with temperature programming was used. Under optimized headspace conditions, equilibration temperature of 120°C, equilibration time of 5 min, and sample size of 50 μL, the regression of the peak area ratios of benzene and toluene to IS on the concentrations of analytes fitted a linear relationship well at the concentration levels ranging from 3.2 g/L to 16.0 g/L. Standard additions of benzene and toluene to blank different matrix solutions 1ead to recoveries of 100.1%–109.5% with a relative standard deviation (RSD of 0.3%–8.1%. The method presented here stands out as simple and easily applicable, which provides a way for the determination of toxic volatile adjuvant in liquid pesticide formulations.

  6. Hyphenated GC-FTIR and GC-MS techniques applied in the analysis of bioactive compounds

    Science.gov (United States)

    Gosav, Steluta; Paduraru, Nicoleta; Praisler, Mirela

    2014-08-01

    The drugs of abuse, which affect human nature and cause numerous crimes, have become a serious problem throughout the world. There are hundreds of amphetamine analogues on the black market. They consist of various alterations of the basic amphetamine molecular structure, which are yet not yet included in the lists of forbidden compounds although they retain or slightly modify the hallucinogenic effects of their parent compound. It is their important variety that makes their identification quite a challenge. A number of analytical procedures for the identification of amphetamines and their analogues have recently been reported. We are presenting the profile of the main hallucinogenic amphetamines obtained with the hyphenated techniques that are recommended for the identification of illicit amphetamines, i. e. gas chromatography combined with mass spectrometry (GC-MS) and gas chromatography coupled with Fourier transform infrared spectrometry (GC-FTIR). The infrared spectra of the analyzed hallucinogenic amphetamines present some absorption bands (1490 cm-1, 1440 cm-1, 1245 cm-1, 1050 cm-1 and 940 cm-1) that are very stable as position and shape, while their intensity depends of the side-chain substitution. The specific ionic fragment of the studied hallucinogenic compounds is the 3,4-methylenedioxybenzyl cation (m/e = 135) which has a small relative abundance (lesser than 20%). The complementarity of the above mentioned techniques for the identification of hallucinogenic compounds is discussed.

  7. GC-MS Analysis on Volatile Oil from Branches of Picrasma quassioides

    Institute of Scientific and Technical Information of China (English)

    HUANG Lin-fang; WANG Zeng-hui; CHEN Shi-lin

    2013-01-01

    Objective To analyze the volatile oil from the branches of Picrasma quassioides.Methods Volatile oil was extracted from the branches of P quassioides by steam distillation.GC-MS method was used to analyze the components.Results A total of 49 compounds were isolated,and 46 compounds were successfully identified,which represented over 98% of the total oil composition.The major components of the volatile oil in the branches of P.quassioides included caryophyllene (12.83%),12-oxabicyclo[9.1.0]dodeca-3,7-diene,1,5,5,8-tetramethyl-[1R-(1R*,3E,7E,11-R*)] (12.29%),1-hexanol (9.96%),naphthalene,1,2,3,5,6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methyletheyl)-[1S-(1a,7a,8aa)] (7.32%),aromadendrene oxide-(2) (6.69%),and α-caryophyllene (3.88%).Conclusion The major components in volatile oil are terpenoids,hydroxy compounds,and other acyclic alkane compounds.

  8. GC-MS Analysis on Volatile Oil from Branches of Picrasma quassioides

    Institute of Scientific and Technical Information of China (English)

    HUANG; Lin-fang; WANG; Zeng-hui; CHEN; Shi-lin

    2013-01-01

    Objective To analyze the volatile oil from the branches of Picrasma quassioides. Methods Volatile oil was extracted from the branches of P. quassioides by steam distillation. GC-MS method was used to analyze the components. Results A total of 49 compounds were isolated, and 46 compounds were successfully identified, which represented over 98% of the total oil composition. The major components of the volatile oil in the branches of P. quassioides included caryophyllene (12.83%), 12-oxabicyclo[9.1.0]dodeca-3,7-diene,1,5,5,8-tetramethyl-[1R-(1R*,3E,7E,11-R*)] (12.29%), 1-hexanol (9.96%), naphthalene, 1,2,3,5,6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methyletheyl)-[1S-(1a,7a,8aa)] (7.32%), aromadendrene oxide-(2) (6.69%), and α-caryophyllene (3.88%). Conclusion The major components in volatile oil are terpenoids, hydroxy compounds, and other acyclic alkane compounds.

  9. GC-MS analysis of polybrominated diphenyl ethers in Lake Erie

    Science.gov (United States)

    Vagula, Mary C.; Vartak, Marissa; Tallmadge, Weslene

    2012-06-01

    Lake Erie is one of the five great lakes of North America. It is the shallowest, the warmest, and the most biologically productive of the Great Lakes producing more fish than all of the other four lakes combined. It is also a source of drinking water for 11 million people and a recreational asset. On the flipside, it is also very vulnerable and troubled with environmental challenges because it has the smallest water volume, but the greatest pressures from the human settlement. One of the many issues faced by the Lake is pollution. It receives larger loads of many pollutants than any other Great Lake. Even with the best pollution controls many pesticides and organohalogens continue to enter the lake. Polybrominated diphenyl ethers (PBDEs) are a class of flame-retardants that have been used in a variety of consumer products since the 1970s. They are added to many commercial and household products such as computers, foam mattresses, carpets, etc. Being largely non-polar and chemically stable, these chemicals are extremely lipophilic and resist degradation in the environment, thus giving them a high affinity for their bioaccumulation. Due to these properties PBDEs have become ubiquitous environmental contaminants. These compounds are reported to be endocrine disruptors and could cause oxidative damage. This report presents the sample preparation protocol, the GC-MS analysis of PBDEs in Lake Erie sediment samples.

  10. The GC/MS Analysis of Volatile Components Extracted by Different Methods from Exocarpium Citri Grandis

    Directory of Open Access Journals (Sweden)

    Zhisheng Xie

    2013-01-01

    Full Text Available Volatile components from Exocarpium Citri Grandis (ECG were, respectively, extracted by three methods, that is, steam distillation (SD, headspace solid-phase microextraction (HS-SPME, and solvent extraction (SE. A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD, 56 (HS-SPME, and 48 (SE compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81% were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E-, and trans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level.

  11. Hydrogen Isotope Measurements of Organic Acids and Alcohols by Pyrolysis-GC-MS-TC-IRMS

    Science.gov (United States)

    Socki, Richard A.; Fu, Qi; Niles, Paul B.

    2011-01-01

    One possible process responsible for methane generation on Mars is abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions. Measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane by tracing the geochemical pathway during formation. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible hydrogen isotope measurements. Reported here are results of experiments to characterize the hydrogen isotope composition of low molecular weight organic acids and alcohols. The presence of these organic compounds has been suggested by others as intermeadiary products made during mineral surface catalyzed reactions. This work compliments our previous study characterizing the carbon isotope composition of similar low molecular weight intermediary organic compounds (Socki, et al, American Geophysical Union Fall meeting, Abstr. #V51B-2189, Dec., 2010). Our hydrogen isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-High Temperature Conversion-Isotope Ratio Mass Spectrometry (Py-GC-MS-TC-IRMS). Our technique is unique in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II? quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of separated organic compounds, therefore both chemical and isotopic measurements can be carried out simultaneously on the same sample.

  12. Determination of Menthol in Plasma and Urine by Gas Chromatography/Mass Spectrometry (GC/MS).

    Science.gov (United States)

    Peat, Judy; Frazee, Clint; Kearns, Gregory; Garg, Uttam

    2016-01-01

    Menthol, a monoterpene, is a principal component of peppermint oil and is used extensively in consumer products as a flavoring aid. It is also commonly used medicinally as a topical skin coolant; to treat inflammation of the mucous membranes, digestive problems, and irritable bowel syndrome (IBS); and in preventing spasms during endoscopy and for its spasmolytic effect on the smooth muscle of the gastrointestinal tract. Menthol has a half life of 3-6 h and is rapidly metabolized to menthol glucuronide which is detectable in urine and serum following menthol use. We describe a method for the determination of total menthol in human plasma and urine using liquid/liquid extraction, gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode and menthol-d4 as the internal standard. Controls are prepared with menthol glucuronide and all samples undergo enzymatic hydrolysis for the quantification of total menthol. The method has a linear range of 5-1000 ng/mL, and coefficient of variation <10%.

  13. HPTLC and GC/MS Study of Amaryllidaceae Alkaloids of Two Narcissus Species.

    Science.gov (United States)

    Shawky, Eman; Abou-Donia, Amina H; Darwish, Fikria A; Toaima, Soad M; Takla, Sarah S; Pigni, Natalia B; Bastida, Jaume

    2015-08-01

    In this article, we report on the alkaloid profile and dynamic of alkaloid content and diversity in two Narcissus plants at different stages of development. The alkaloid profile of the two Narcissus species was investigated by GC/MS and HPTLC. Fifty eight Amaryllidaceae alkaloids were detected, and 25 of them were identified in the different organs of N. tazetta and N. papyraceus. The alkaloid 3-O-methyl-9-O-demethylmaritidine is tentatively identified here for the first time from the Amaryllidaceae family, and four alkaloids (tazettamide, sternbergine, 1-O-acetyllycorine, 2,11-didehydro-2-dehydroxylycorine) are tentatively identified for the first time in the genus Narcissus. The different organs of the two species analyzed showed remarkable differences in their alkaloid pattern, type of biosynthesis, main alkaloid and number of alkaloids. Lycorine-type alkaloids dominated the alkaloid, metabolism in N. papyraceus, while alkaloids of narciclasine-, galanthamine- and homolycorine-types were found only in the species N. tazetta L.

  14. Characterization of Fatty Acids in Crenarchaeota by GC-MS and NMR.

    Science.gov (United States)

    Hamerly, Timothy; Tripet, Brian; Wurch, Louie; Hettich, Robert L; Podar, Mircea; Bothner, Brian; Copié, Valérie

    2015-01-01

    Lipids composed of condensed isoprenyl units connected to glycerol backbones by ether linkages are a distinguishing feature of Archaea. Data suggesting that fatty acids with linear hydrocarbon chains are present in some Archaea have been available for decades. However, lack of genomic and biochemical evidence for the metabolic machinery required to synthesize and degrade fatty acids has left the field unclear on this potentially significant biochemical aspect. Because lipids are energy currency and cell signaling molecules, their presence in Archaea is significant for understanding archaeal biology. A recent large-scale bioinformatics analysis reignited the debate as to the importance of fatty acids in Archaea by presenting genetic evidence for the presence of enzymes required for anabolic and catabolic fatty acid metabolism across the archaeal domain. Here, we present direct biochemical evidence from gas chromatography-mass spectrometry (GC-MS) and nuclear magnetic resonance (NMR) spectroscopy for the presence of fatty acids in two members of the Crenarchaeota, Sulfolobus solfataricus and Ignicoccus hospitalis. This is the first report providing biochemical data for the existence of fatty acids in these Crenarchaeota, opening new discussions on energy balance and the potential for the discovery of new thermostable enzymes for industry.

  15. GC-MS metabolomics analysis of mesenchymal stem cells treated with copper oxide nanoparticles.

    Science.gov (United States)

    Murgia, Antonio; Mancuso, Luisa; Manis, Cristina; Caboni, Pierluigi; Cao, Giacomo

    2016-10-01

    Human exposure to copper oxide (CuO) nanoparticles (NPs) is rapidly increasing and for this reason reliable toxicity test systems are urgently needed. Recently, the acute cytotoxicity of CuO NPs using the new toxicity test based on human bone marrow mesenchymal stem cells (hBMMSCs) has been evaluated. It was shown that CuO NPs are much more toxic when compared to CuO microparticles (MPs). Several studies associate CuO toxicity to a possible alteration of reactive oxygen species (ROS) system. Unluckily, the mechanism that causes the toxicity is still not clear. In this work, the polar metabolite pool of treated cells, at the corresponding IC50 value, for CuO micro and NPs has been studied by gas chromatography coupled to mass spectrometry (GC-MS) and multivariate statistical data analysis. By the same means, differences due to different treatments, on samples, were investigated. Results of discriminant analysis were considered with the aim of finding the relevant metabolites unique for each class. Serine, glyceric acid, and succinic acid were upregulated on samples treated with CuO microparticles, while glutamine was the only discriminant metabolite for the class of samples treated with nanoparticles.

  16. "Detection of Morphine in Opioid Abusers Hair by GC/MS "

    Directory of Open Access Journals (Sweden)

    Khosrou Abdi

    2004-07-01

    Full Text Available Thirty hair samples were collected from the male opioid abusers in which the presence of morphine in their urine samples was confirmed by Thin Layer Chromatography (TLC analyses. The hair samples were washed, cut into small pieces and extracted in a mixture of methanol-triflouroacetic acid (9:1. The methanolic phase was evaporated to dryness under nitrogen stream and derivitized by addition of N-methyl-N-trimethylsilyl triflouroacetamide (MSTFA and 1% trimethyl iodosilane (TMIS with sonication. One micro liter of each derivitized sample was injected into a Gas Chromatograph-Mass Spectrometer (GC/MS system consisting of a capillary column and finnigan MS with selective ion monitoring (SIM mode. The selected mass for ions codeine and morphine were 370 and 429, respectively. The limit of detection (LOD was set at 0.03ng/mg of the hair. By using the above procedure, morphine was detectable in all of the examined samples and this method is capable to detec low levels of morphine in hair for a long period of time following the last intake of the drug

  17. A novel GC-MS method in urinary estrogen analysis from postmenopausal women with osteoporosis.

    Science.gov (United States)

    Moon, Ju-Yeon; Kim, Kwang Joon; Moon, Myeong Hee; Chung, Bong Chul; Choi, Man Ho

    2011-08-01

    Estrogen metabolites play important roles in the development of female-related disorders and homeostasis of the bone. To improve detectability, a validated gas chromatography-mass spectrometry (GC-MS) method was conducted with two-phase extractive ethoxycarbonlyation (EOC) and subsequent pentafluoropropionyl (PFP) derivatization was introduced. The resulting samples were separated through a high-temperature MXT-1 column within an 8 min run and were detected in the selected ion monitoring (SIM) mode. The optimized analytical conditions led to good separation with a symmetric peak shape for 19 estrogens as their EOC-PFP derivatives. The limit of quantification (LOQ) was from 0.02 to ∼0.1 ng/ml for most estrogens analyzed, except for 2-hydroxyestriol (0.5 ng/ml). The devised method was found to be linear (r² > 0.995) in the range from the LOQ to 40 ng/ml, whereas the precision (% CV) and accuracy (% bias) ranged from 1.4 to 10.5% and from 91.4 to 108.5%, respectively. The good sensitivity and selectivity of this method even allowed quantification of the estrogen metabolites in urine samples obtained from the postmenopausal female patients with osteoporosis. The present technique can be useful for clinical diagnosis as well as to better understand the pathogenesis of estrogen-related disorders in low-level quantification.

  18. A rapid and sensitive technique for assessing exposure to VX via GC-MS-MS analysis.

    Science.gov (United States)

    McGuire, Jeffrey M; Byers, Christopher E; Hulet, Stanley W; Jakubowski, Edward M; Thomson, Sandra A

    2008-01-01

    A rapid and sensitive method for the determination of the chemical warfare agent VX in plasma taken from Göttingen minipigs has been developed using isotope-dilution gas chromatography-tandem mass spectrometry (GC-MS-MS). Chromatographic separation was achieved on a 5% diphenyl/95% dimethyl polysiloxane capillary column with a total run time of about 11 min. The analyte was detected using ammonia chemical ionization in the multiple reaction monitoring mode, following a simple extraction with 10% 2-propanol in hexane. A good linear relationship was obtained in the quantitative concentration range of 10 ng/mL to 1000 ng/mL (r(2) = 0.9998) with an average slope of 1.275 +/- 0.037 (n = 7), and an absolute detection limit of 0.4 pg on column. The average recovery for VX was 95% in saline in the concentration range of 50-100 ng/mL. The method was successfully applied to the analysis of VX in minipig plasma in a preliminary toxicokinetic study.

  19. Exposure assessment approach through mycotoxin/creatinine ratio evaluation in urine by GC-MS/MS.

    Science.gov (United States)

    Rodríguez-Carrasco, Yelko; Moltó, Juan Carlos; Mañes, Jordi; Berrada, Houda

    2014-10-01

    In this pilot survey human urine samples were analyzed for presence of 15 mycotoxins and some of their metabolites using a novel urinary multi-mycotoxin GC-MS/MS method following salting-out liquid-liquid extraction. Fifty-four urine samples from children and adults residents in Valencia were analyzed for presence of urinary mycotoxin and expressed in gram of creatinine. Three out of 15 mycotoxins were detected namely, HT-2 toxin, nivalenol and deoxynivalenol (DON). 37 samples showed quantifiable values of mycotoxins. Co-occurrence of these contaminants was also observed in 20.4% of assayed samples. DON was the most frequently detected mycotoxin (68.5%) with mean levels of 23.3 μg/g creatinine (range: 2.8-69.1 μg/g creatinine). The levels of urinary DON were used to carry out an exposure assessment approach. 8.1% of total subjects were estimated to exceed the DON provisional maximum tolerable daily intake (PMTDI) (1 μg/kg b.w.). Two out of 9 exposed children exceeded the DON PMTDI thus, making them the most exposed based on the urinary results.

  20. Study on the Aromatic Components of Green Plum Wine by HS-SPME-GC-MS

    Institute of Scientific and Technical Information of China (English)

    Yingying MA; Hechuan WU; Qingbin LIU; Lingyun WANG; Xiao DOU; Lin YANG; Jiangang YANG

    2016-01-01

    In order to better blend green plum wine and study aromatic components of green plum wine,a qualitative analysis on aromatic components of soaked base liquor,green plum soaked wine,green plum juice,and fermented wine of green plum juice by Head Space Solid-phase Microextraction( HS-SPME) and Gas Chromatograph Mass Spectrometer( GC-MS) was studied in this paper. Experiment results indicated that14,32,17,and 46 kinds of aromatic components were identified respectively from four samples. Different aromatic components determined the special flavor and taste of green plum wine. Unique aromatic components generated in soaking process include benzaldehyde,1-butanol,2-methyl-,S-(-),benzoic acid ethyl ester,and 5-( hydroxymethyl). Special aromatic components in green plum juice were furfural,phenylethyl alcohol,and benzyl alcohol. The aromatic components in fermented wine of green plum juice mainly included phenylethyl alcohol( 6. 941%,relative content of peak area,same below),1-butanol,3-methyl-( 6. 940%),octanoic acid,ethyl ester( 3. 734%),decanoic acid,ethyl ester( 2. 590%),hexanoic acid,ethyl ester( 2. 479%),ethyl 9-decenoate( 2. 080%),and 5-hydroxymethyl( 1. 756%). This study was expected to provide scientific basis and data reference for quality improvement of green plum wine.

  1. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS.

    Science.gov (United States)

    Hansen, Anne-Mette S; Frandsen, Henrik L; Fromberg, Arvid

    2016-05-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers, the naturalness of a raspberry flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. Twenty-seven food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry jam, dried raspberries, and sodas declared to contain natural aroma all contained almost only R-(E)-α-ionone supporting the content of natural raspberry aroma. Six out of eight sweets tested did not indicate a content of natural aroma on the labeling which was in agreement with the almost equal distribution of the R and S isomer. Two products were labeled to contain natural raspberry flavors but were found to contain almost equal amounts of both enantiomers indicating a presence of synthetic raspberry flavors only. Additionally, two products that were labeled to contain both raspberry juice and flavor showed equal amounts of both enantiomers, indicating the presence of synthetic flavor.

  2. Analysis on Volatile Constituents in Leaves and Fruits of Ficus carica by GC-MS

    Institute of Scientific and Technical Information of China (English)

    LI Jun; TIAN Yu-zeng; SUN Bao-ya; YANG Dan; CHEN Ji-ping; MEN Qi-ming

    2012-01-01

    Objective To identify and analyze the volatile constituents in the leaves and fruits ofFicus carica.Methods Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) were used.Results The major components detected in volatile oil of the leaves were psoralen (10.12%),β-damascenone (10.17%),benzyl alcohol (4.56%),behenic acid (4.79%),and bergapten (1.99%),etc.The major components detected in volatile oil of the fruits were furfural (10.55%),5-methyl-2-furaldehyde (10.1%),and benzeneacetaldehyde (6.59%),etc.Conclusion A total of 121 volatile constituents are identified in the leaves and 108 in the fruits ofF.carica,among which 103 constituents are identified for the first time in the leaves and 100 in the fruits.Eighteen volatile constituents are identified in both leaves and fruits.

  3. GC-MS analysis of insecticidal essential oil of flowering aerial parts of Saussurea nivea Turcz

    Directory of Open Access Journals (Sweden)

    Chu Sha

    2012-08-01

    Full Text Available Abstract Background Several species from Saussurea have been used in the traditional medicine, such as S. lappa, S. involucrate, and S. obvallata. There is no report on medicinal use of S. nivea. The aim of this research was to determine chemical composition and insecticidal activity of the essential oil of S. nivea Turcz (Asteraceae aerial parts against maize weevils (Sitophilus zeamais Motschulsky for the first time. Results Essential oil of S. nivea flowering aerial parts was obtained by hydrodistillation and analyzed by gas chromatography–mass spectrometry (GC-MS. A total of 43 components of the essential oil of S. nivea were identified. The principal compounds in the essential oil were (+-limonene (15.46%, caryophyllene oxide (7.62%, linalool (7.20%, α-pinene (6.43%, β-pinene (5.66% and spathulenol (5.02% followed by β-eudesmoll (4.64% and eudesma-4,11-dien-2-ol (3.76%. The essential oil of S. nivea exhibited strong contact toxicity against S. zeamais with an LD50 value of 10.56 μg/adult. The essential oil also possessed fumigant toxicity against S. zeamais with an LC50 value of 8.89 mg/L. Conclusion The study indicates that the essential oil of S. nivea flowering aerial parts has a potential for development into a natural insecticide/fumigant for control of insects in stored grains.

  4. GC-MS Analysis of Insecticidal Essential Oil of Aerial Parts of Echinops latifolius Tausch

    Directory of Open Access Journals (Sweden)

    Xin Chao Liu

    2013-01-01

    Full Text Available The roots of Echinops latifolius Tausch (Asteraceae have been used in the traditional medicine. However, no report on chemical composition and insecticidal activities of the essential oil of this plant exists. The aim of this research was to determine chemical composition and insecticidal activities of the essential oil of E. latifolius aerial parts against maize weevils (Sitophilus zeamais Motschulsky for the first time. Essential oil of E. latifolius aerial parts at flowering stage was obtained by hydrodistillation and analyzed by gas chromatography-mass spectrometry (GC-MS. A total of 35 components of the essential oil of E. latifolius aerial parts were identified. The major compounds in the essential oil were 1,8-cineole (19.63%, (Z-β-ocimene (18.44%, and β-pinene (15.56% followed by β-myrcene (4.75% and carvone (4.39%. The essential oil of E. latifolius possessed contact toxicity against S. zeamais with an LD50 value of 36.40 µg/adult. The essential oil also exhibited fumigant toxicity against S. zeamais with an LC50 value of 9.98 mg/L. The study indicates that the essential oil of E. latifolius aerial parts has a potential for development into a natural insecticide/fumigant for control of insects in stored grains.

  5. HS-GC-MS method for the analysis of fragrance allergens in complex cosmetic matrices.

    Science.gov (United States)

    Desmedt, B; Canfyn, M; Pype, M; Baudewyns, S; Hanot, V; Courselle, P; De Beer, J O; Rogiers, V; De Paepe, K; Deconinck, E

    2015-01-01

    Potential allergenic fragrances are part of the Cosmetic Regulation with labelling and concentration restrictions. This means that they have to be declared on the ingredients list, when their concentration exceeds the labelling limit of 10 ppm or 100 ppm for leave-on or rinse-off cosmetics, respectively. Labelling is important regarding consumer safety. In this way, sensitised people towards fragrances might select their products based on the ingredients list to prevent elicitation of an allergic reaction. It is therefore important to quantify potential allergenic ingredients in cosmetic products. An easy to perform liquid extraction was developed, combined with a new headspace GC-MS method. The latter was capable of analysing 24 volatile allergenic fragrances in complex cosmetic formulations, such as hydrophilic (O/W) and lipophilic (W/O) creams, lotions and gels. This method was successfully validated using the total error approach. The trueness deviations for all components were smaller than 8%, and the expectation tolerance limits did not exceed the acceptance limits of ± 20% at the labelling limit. The current methodology was used to analyse 18 cosmetic samples that were already identified as being illegal on the EU market for containing forbidden skin whitening substances. Our results showed that these cosmetic products also contained undeclared fragrances above the limit value for labelling, which imposes an additional health risk for the consumer. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Phytochemical Analysis of Leaf Extract of Abutilon hirtum (Lam. Sweet by GC-MS Method

    Directory of Open Access Journals (Sweden)

    Vivekraj P.

    2015-08-01

    Full Text Available Abutilon hirtum (Lam. Sweet (Malvaceae commonly known as Vadathuthi. It is used as one of the most important drugs in traditional system of medicine to treat various ailments. The plant is used for to its various properties as demulcent, diuretics, anti-diabetics, anthelmintic, laxative, wound healing properties, antibacterial and antifungal properties. The present study revealed the presence of phytochemicals like Diethyl Phthalate (19.171%,Benzaldehyde 4-propyl (5.219%,Methoxyacetic acid 3-tridecyl ester (5.196%,Sulfurous acid dodecyl 2-propyl ester (0.455%,Sulfurous acid, butyl dodecyl ester (0.442%etc., from the chloroform extracts of leaves in A. hirtum. In the present study an attempt was made to investigate the phytochemical present in the extracts in the preliminary level by using Gas Chromatography coupled with Mass Spectrometry (GC-MS. The study will provide information for the correct identification of the crude drug. This will be further considered for pharmacological activities and isolation of individual components would however, help to find new drugs.The results are reported for the first time in A. hirtum.

  7. GC-MS analysis and ecotoxicological risk assessment of triclosan, carbamazepine and parabens in Indian rivers.

    Science.gov (United States)

    Ramaswamy, Babu Rajendran; Shanmugam, Govindaraj; Velu, Geetha; Rengarajan, Bhuvaneshwari; Larsson, D G Joakim

    2011-02-28

    Pharmaceutical and personal care products are used extensively worldwide and their residues are frequently reported in aquatic environments. In this study, antiepileptic, antimicrobial and preservative compounds were analyzed in surface water and sediment from the Kaveri, Vellar and Tamiraparani rivers, and in the Pichavaram mangrove in India by gas chromatography-mass spectrometry (GC-MS). The mean concentration of carbamazepine recorded in the Kaveri River water (28.3 ng/L) was higher than in the other rivers and the mangrove. Because carbamazepine is used only in human drugs, this may reflect the relative contributions of human excretions/sewage in these rivers. The mean triclosan level in the Tamiraparani River (944 ng/L) was an order of magnitude greater than in the other water systems, and the concentrations at two of the sites reported here (3800-5160 ng/L) are, to our best knowledge, among the highest detected in surface waters. Sediment levels were, however, comparable with other sites. We conclude that industrial releases are likely major contributors of triclosan into this river system. Among parabens, ethyl paraben was predominantly observed. Hazard Quotients suggest greater environmental risks for triclosan than for carbamazepine and parabens. This is the first study on antiepileptic, antimicrobial and preservatives in rivers and mangroves from India.

  8. Study of flavour compounds from orange juices by HS-SPME and GC-MS

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Covaciu, F.; Feher, I.; Magdas, A.; David, L.; Moldovan, Z.

    2013-11-01

    The flavour of the orange juices, which gives the taste and odour of the product, is an important criterion about the products quality for consumers. A fresh single strength and two commercial orange juices (obtained from concentrate) flavour profile were studied using a selective and sensitive gas chromatography - mass spectrometry (GC-MS) analytical system, after a solvent free, single step preconcentration and extraction technique, the headspace solid phase microextraction (HP-SPME). In the studied orange juices 55 flavour compounds were detected and classified as belonging to the esters, alcohols, ketones, monoterpenes and sesquiterpenes chemical families. The fresh single strength orange juice was characterized by high amount of esters, monoterpenes and sesquiterpenes. Limonene and valencene were the most abundant flavours in this fresh natural orange juice. Alcohols and ketones were found in higher concentration in the commercial orange juices made from concentrate, than in the single strength products. Nevertheless, in commercial juices the most abundant flavour was limonene and α-terpineol. The results highlight clear differences between fresh singles strength orange juice and juice from concentrate. The orange juices reconstructed from concentrate, made in Romania, present low quantity of flavour compounds, suggesting the absence or a low rearomatization process, but extraneous components were not detected.

  9. Analysis of octylphenol, nonylphenol, di-octylphthalate in sewage sludge by GC/MS-SIM

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J.H. [Jeonju University, Cheonju (Korea)

    1999-06-01

    Sewage sludge samples were extracted with dichlomethane by Soxhlet extraction. The extracts were analysed for the endocrine disrupting compounds (EDC), octylphenol(OP), nonylphenol (NP) and bis (2-ethylhexyl)phthalate(DOP) using GC/MS-SIM. In industrial sewage sludge (sample Z-I) the concentration of NP and DOP were respectively 1168 {mu}g/g and 1172{mu}g/g whereas in domestic sludge (sample Z-2) the concentration were respectively 10.8 {mu}g/g and 80 {mu}g/g. OP was not detected in Z-2, but detected a small amount in Z-2 of the samples. Environmental EDC have been shown to affect the fertility of range of living organisms, including humans, and the high levels of NP and DOP in industrial sewage sludge could have serious implications for the reproductive health of humans particularly if the compounds entered the human food chain through water or the ingestion of vegetables or animal products. 17 refs., 6 figs., 3 tabs.

  10. Rapid discrimination and feature extraction of three Chamaecyparis species by static-HS/GC-MS.

    Science.gov (United States)

    Chen, Ying-Ju; Lin, Chun-Ya; Cheng, Sen-Sung; Chang, Shang-Tzen

    2015-01-28

    This study aimed to develop a rapid and accurate analytical method for discriminating three Chamaecyparis species (C. formosensis, C. obtusa, and C. obtusa var. formosana) that could not be easily distinguished by volatile compounds. A total of 23 leaf samples from three species were analyzed by static-headspace (static-HS) coupled with gas chromatography-mass spectrometry (GC-MS). The static-HS procedure, whose experimental parameters were properly optimized, yielded a high Pearson correlation-based similarity between essential oil and VOC composition (r = 0.555-0.999). Thirty-six major constituents were identified; along with the results of cluster analysis (CA), a large variation in contents among the three different species was observed. Principal component analysis (PCA) methods illustrated graphically the relationships between characteristic components and tree species. It was clearly demonstrated that the static-HS-based procedure enhanced greatly the speed of precise analysis of chemical fingerprint in small sample amounts, thus providing a fast and reliable tool for the prediction of constituent characteristics in essential oil, and also offering good opportunities for studying the role of these feature compounds in chemotaxonomy or ecophysiology.

  11. Simultaneous GC-MS determination of seven phthalates in total and migrated portions of paper cups.

    Science.gov (United States)

    Park, Yu Na; Choi, Min Sun; Rehman, Shaheed Ur; Gye, Myung Chan; Yoo, Hye Hyun

    2016-05-01

    Phthalate acid esters are widely used as plasticizers to impart plastic flexibility in various industrial applications. In this study, the content of seven phthalates, dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), di-(2-ethylhexyl) adipate (DEHA), di-2-ethylhexyl phthalate (DEHP), di-n-octyl phthalate (DNOP), di-isononyl phthalate (DINP), and di-isodecyl phthalate (DIDP) were determined in paper cups using gas chromatography-mass spectrometry (GC-MS). In addition, the potential migration of these seven phthalates from paper cups into various food stimulants under different conditions was evaluated. The levels of DBP, DEHA, DEHP, and DNOP were in the ranges of 0.07-3.14, 0.16-42.69, 0.45-58.56, and 0.3-2.4 mg/kg, respectively. Meanwhile, BBP, DINP, and DIDP were not detected in most of the tested samples. In the migration test, DEHA was released to 50 % ethanol and n-heptane in a time-dependent manner and the maximum migration levels were 65.62 ± 3.61 and 95.56 ± 19.76 μg/L, respectively. The release of other phthalates was very low or negligible. These results demonstrated that paper cups are not a significant source of phthalate exposure; however, DEHA could be released from paper cups into alcoholic beverages or oily liquid beverages in the human diet.

  12. Determination of Alprazolam in Rabbit Plasma by GC-MS Method

    Directory of Open Access Journals (Sweden)

    Bilal Yilmaz

    2010-02-01

    Full Text Available This paper describes a gas chromatography-mass spectrometry (GC-MS method for determination of alprazolam in rabbit plasma. Alprazolam and internal standard (IS medazepam were extracted from plasma by using liquid-liquid extraction method. The samples were separated by GC on a DB-5MS analytical column and determined by a quadrupole mass spectrometer detector operated under selected ion monitoring mode (SIM. Excellent linearity was found between 50 and 1000 ng/mL r=0.998 for plasma samples. Intra-day and inter-day precisions expressed as the relative standard deviation (RSD for the method were 1.07-2.69% and 2.42-3.98%, respectively. The mean recovery of alprazolam samples was 98.82%. The limits of detection and uantification of alprazolam were 15 and 50 ng/mL, respectively. Also, the method was successfully applied to three New Zealand white abbits which had been given an oral tablet of 1.0 mg alprazolam.

  13. Homogenity of oil and sugar components of flour amaranth investigated by GC-MS

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    Psodorov Đorđe B.

    2015-01-01

    Full Text Available Gas chromatography with mass spectrometry (GC-MS was used for performing a qualitative analysis of liposoluble and hydrosoluble flour extracts of three genotypes of Amaranthus sp. All three samples were first defatted with hexane. Hexane extracts were used for the analysis of fatty acids of lipid components. TMSH (Trimethylsulfonium hydroxide, 0.2M in methanol was used as the transesterification reagent. With transesterification reaction, fatty acids were esterified from acilglycerol to methyl-esters. Defatted flour samples were dried in the air and then extracted with ethanol. Ethanol extracts were used for the analysis of soluble carbohydrates. TMSI (trimethylsilylimidazole was used as a reagent for the derivatization of carbohydrates into trimethylsilylethers. The results show that the dominant methyl-esters of fatty acids are very similar in all the three samples. Such a similarity was not detected in the analysis of soluble sugars. The following test cluster analysis was used for the comparison of liposoluble and hydrosoluble flour extracts of three genotypes of Amaranthus sp.

  14. TLC and GC-MS Analyses of Essential Oil Isolated from Macedonian Foeniculi fructus

    Directory of Open Access Journals (Sweden)

    Menče Najdoska

    2011-05-01

    Full Text Available The essential oil of Foeniculi fructus, the ripe fruit from the plant Foeniculum vulgare Mill. ssp. vulgare var. dulce Batt. and Trab. (sweet fennel, македонски анасон was isolated and the main components were identified and quantified using thin-layer chromatography (TLC and gas chromatography and mass spectrometry (GC-MS. The Aetherloeum Foeniculi had pale yellow color and characteristic pleasant odor and was obtained in 3.2% yield (by weight from the plant fruits. The main components of the oil were: trans-anethole, 1, (70%, p-anisaldehyde, 2, (19% estragole, 3, (6% and anisacetone, 4, (2%. The identity of the components was determined by matching the mass spectra to the library spectra. The identity of the main component, trans-anethole, was confirmed directly by isolation using column chromatography and indirectly by potassium permanganate oxidation of the essential oil. The oxidation product from this reaction, pmethoxybenzoic acid, 16, was isolated and characterized. The potential products of autooxidation of trans-anethole (epoxy anethole, anethole glycol and 16 were not detected in the freshly obtained essential oils.

  15. Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS

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    Zhen Ding

    2014-01-01

    Full Text Available The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME coupled to chromatography-mass spectrometry (GC-MS, including geosmin (GSM and 2-methylisoborneol (2-MIB, as well as dimethyl trisulfide (DMTS, β-cyclocitral, and β-ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA, the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5. The limits of detection (LOD are all below 1.3 ng L−1, and the relative standard deviation (%RSD is between 4.4% and 9.9% (n = 7 and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters.

  16. GC-MS Analysis and Preliminary Antimicrobial Activity of Albizia adianthifolia (Schumach and Pterocarpus angolensis (DC

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    Mustapha N. Abubakar

    2016-01-01

    Full Text Available The non-polar components of two leguminoceae species Albizia adianthifolia (Schumach, and Pterocarpus angolensis (DC were investigated. GC-MS analysis of the crude n-hexane and chloroform extracts together with several chromatographic separation techniques led to the identification and characterization (using NMR of sixteen known compounds from the heartwood and stem bark of Albizia adianthifolia and Pterocarpus angolensis respectively. These constituents include, n-hexadecanoic acid (palmitic acid 1, oleic acid 2, chondrillasterol 3, stigmasterol 4, 24S 5α-stigmast-7-en-3β-ol 5, 9,12-octadecadienoic acid (Z,Z-, methyl ester 6, trans-13-octadecanoic acid, methyl ester 7, tetradecanoic acid 8, hexadecanoic acid, methyl ester 9, octadecanoic acid 10, tetratriacontane 11, 7-dehydrodiosgenin 12, lupeol 13, stigmasta-3,5-diene-7-one 14, friedelan-3-one (friedelin 15, and 1-octacosanol 16. Using agar over lay method, the preliminary antimicrobial assay for the extracts was carried out against bacterial (E. coli, P. aeruginosa, B. subtilis, S. aueus and a fungus/yeast (C. albicans strains. The n-hexane and chloroform extracts of A. adianthifolia showed the best activity against E. coli with minimum inhibition quantity (MIQ of 1 µg each while the remaining exhibited moderate-to-weak activity against the test microorganisms.

  17. Bioactive Compound Evaluation of Ethanol Extract from Geodorum densiflorum (Lam. Schltr. by GC-MS analysis

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    Keerthiga Manohar

    2015-06-01

    Full Text Available The phytochemical constituents are responsible for medicinal value of the plant species. The present investigation was carried out to analyze the bioactive components from the whole plant of Geodorum densiflorum (Lam. Schltr using GC-MS technique. The chemical compositions of the ethanolic extract of G. densiflorum were investigated using Perkin - Elmer Gas Chromatography – Mass Spectrometry and about twenty one bioactive phytochemical compounds were identified. The prevailing compounds where Hexadecanoic acid, Ethyl ester (38.884 %, Ionone (7.125 %, 3-Deoxy-d-mannoic lactone (7.4441 %, 2,3-Butanediol (4.725 % and 2-Piperidinone, N-[4-bromo-n-butyl]- (4.004 %, (E-9-Octadeconoic acid ethyl ester (3.891 %, 1H-Pyrrole-2-Carbonitrile (3.778 %, Pyridinium, 1-amino-, chloride (3.305 %, 4H- Pyran-4-one, 3,5-dihydroxy-2-methyl- (3.274 and having various biological activities. This was the first report on the identification of bioactive compounds from ethanol extract of G. densiflorum.

  18. Characterization of Fatty Acids in Crenarchaeota by GC-MS and NMR

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    Timothy Hamerly

    2015-01-01

    Full Text Available Lipids composed of condensed isoprenyl units connected to glycerol backbones by ether linkages are a distinguishing feature of Archaea. Data suggesting that fatty acids with linear hydrocarbon chains are present in some Archaea have been available for decades. However, lack of genomic and biochemical evidence for the metabolic machinery required to synthesize and degrade fatty acids has left the field unclear on this potentially significant biochemical aspect. Because lipids are energy currency and cell signaling molecules, their presence in Archaea is significant for understanding archaeal biology. A recent large-scale bioinformatics analysis reignited the debate as to the importance of fatty acids in Archaea by presenting genetic evidence for the presence of enzymes required for anabolic and catabolic fatty acid metabolism across the archaeal domain. Here, we present direct biochemical evidence from gas chromatography-mass spectrometry (GC-MS and nuclear magnetic resonance (NMR spectroscopy for the presence of fatty acids in two members of the Crenarchaeota, Sulfolobus solfataricus and Ignicoccus hospitalis. This is the first report providing biochemical data for the existence of fatty acids in these Crenarchaeota, opening new discussions on energy balance and the potential for the discovery of new thermostable enzymes for industry.

  19. Determination of Polycyclic Aromatic Hydrocarbons in Industrial Harbor Sediments by GC-MS

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    Chiu-Wen Chen

    2012-06-01

    Full Text Available Analysis of the 16 polycyclic aromatic hydrocarbons (PAHs of the US Environmental Protection Agency priority pollutant list was carried out in sediment samples of an industrial port in the southern Kaohsiung Harbor of Taiwan which is supposed to be extensively polluted by industrial wastewater discharges. The determination and quantification of PAHs in sediment samples were performed using gas chromatography coupled to mass spectrometry (GC-MS with the aid of deuterated PAH internal standards and surrogate standards. The total concentrations of the 16 PAHs varied from 4,425 to 51,261 ng/g dw, with a mean concentration of 13,196 ng/g dw. The PAHs concentration is relatively high in the river mouth region, and gradually diminishes toward the harbor region. Diagnostic ratios showed that the possible source of PAHs in the industrial port area could be coal combustion. As compared with the US Sediment Quality Guidelines (SQGs, the various observed levels of PAHs exceeded the effects range median (ERM, and could thus cause acute biological damages. The results can be used for regular monitoring, and future pollution prevention and management should target the various industries in this region for reducing pollution.

  20. Analysis of PVC plasticizers in medical devices and infused solutions by GC-MS.

    Science.gov (United States)

    Bourdeaux, Daniel; Yessaad, Mouloud; Chennell, Philip; Larbre, Virginie; Eljezi, Teuta; Bernard, Lise; Sautou, Valerie

    2016-01-25

    In 2008, di-(2-ethylhexyl) phthalate (DEHP), was categorized as CMR 1B under the CLP regulations and its use in PVC medical devices (MD) was called into question by the European authorities. This resulted in the commercialization of PVC MDs plasticized with the DEHP alternative plasticizers tri-octyl trimellitate (TOTM), di-(2-ethylhexyl) terephthalate (DEHT), di-isononyl cyclohexane-1,2-dicarboxylate (DINCH), di-isononyl phthalate (DINP), di-(2-ethylhexy) adipate (DEHA), and Acetyl tri-n-butyl citrate (ATBC). The data available on the migration of these plasticizers from the MDs are too limited to ensure their safe use. We therefore developed a versatile GC-MS method to identify and quantify both these newly used plasticizers and DEHP in MDs and to assess their migration abilities in simulant solution. The use of cubic calibration curves and the optimization of the analytical method by an experimental plan allowed us to lower the limit of plasticizer quantification. It also allowed wide calibration curves to be established that were adapted to this quantification in MDs during migration tests, irrespective of the amount present, and while maintaining good precision and accuracy. We then tested the developed method on 32 PVC MDs used in our hospital and evaluated the plasticizer release from a PVC MD into a simulant solution during a 24h migration test. The results showed a predominance of TOTM in PVC MDs accompanied by DEHP (plasticizers and a non-linear kinetic release.

  1. GC-MS Analysis and Preliminary Antimicrobial Activity of Albizia adianthifolia (Schumach) and Pterocarpus angolensis (DC).

    Science.gov (United States)

    Abubakar, Mustapha N; Majinda, Runner R T

    2016-01-28

    The non-polar components of two leguminoceae species Albizia adianthifolia (Schumach), and Pterocarpus angolensis (DC) were investigated. GC-MS analysis of the crude n-hexane and chloroform extracts together with several chromatographic separation techniques led to the identification and characterization (using NMR) of sixteen known compounds from the heartwood and stem bark of Albizia adianthifolia and Pterocarpus angolensis respectively. These constituents include, n-hexadecanoic acid (palmitic acid) 1, oleic acid 2, chondrillasterol 3, stigmasterol 4, 24S 5α-stigmast-7-en-3β-ol 5, 9,12-octadecadienoic acid (Z,Z)-, methyl ester 6, trans-13-octadecanoic acid, methyl ester 7, tetradecanoic acid 8, hexadecanoic acid, methyl ester 9, octadecanoic acid 10, tetratriacontane 11, 7-dehydrodiosgenin 12, lupeol 13, stigmasta-3,5-diene-7-one 14, friedelan-3-one (friedelin) 15, and 1-octacosanol 16. Using agar over lay method, the preliminary antimicrobial assay for the extracts was carried out against bacterial (E. coli, P. aeruginosa, B. subtilis, S. aueus) and a fungus/yeast (C. albicans) strains. The n-hexane and chloroform extracts of A. adianthifolia showed the best activity against E. coli with minimum inhibition quantity (MIQ) of 1 µg each while the remaining exhibited moderate-to-weak activity against the test microorganisms.

  2. Bacteria-based polythene degradation products: GC-MS analysis and toxicity testing.

    Science.gov (United States)

    Shahnawaz, Mohd; Sangale, Manisha K; Ade, Avinash B

    2016-06-01

    Polythene degradation leads to the production of various by-products depending upon the type of degradation process. The polythene degradation products (PEDP) in the culture supernatant of the two bacteria (Lysinibacillus fusiformis strain VASB14/WL and Bacillus cereus strain VASB1/TS) were analyzed with GC-MS technique. The major by-products in the PEDP in the culture supernatant of L. fusiformis strain VASB14/WL (1,2,3,4 tetra methyl benzene) and B. cereus strain VASB1/TS (1,2,3 trimethyl benzene, 1 ethyl 3,5-dimethyl benzene, 1,4 di methyl 2 ethyl benzene, and dibutyl phthalate) dissolved in diethyl ether were recorded. To assess the environmental applicability of polythene degradation using L. fusiformis strain VASB14/WL and B. cereus strain VASB1/TS at in vitro level. The effect of PEDP produced after 2 months of regular shaking at room temperature on both plants and animal system was studied. No significant decrease in the percent seed germination was recorded with the PEDP of both the bacteria. PEDP produced by L. fusiformis strain VASB14/WL did not report any significant change in germination index (GI) at 10 and 25 %, but least GI (39.66 ± 13.94) was documented at 50 % concentration of PEDP. Highest elongation inhibition rate (53.83 ± 15.71) of Sorghum was also recorded with L. fusiformis and at the same concentration.

  3. Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS-MS.

    Science.gov (United States)

    Páleníková, Agneša; Martínez-Domínguez, Gerardo; Arrebola, Francisco Javier; Romero-González, Roberto; Hrouzková, Svetlana; Frenich, Antonia Garrido

    2015-04-15

    An analytical method based on a modified QuEChERS extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was evaluated for the determination of 177 pesticides in soya-based nutraceutical products. The QuEChERS method was optimised and different extraction solvents and clean-up approaches were tested, obtaining the most efficient conditions with a mixture of sorbents (PSA, C18, GBC and Zr-Sep(+)). Recoveries were evaluated at 10, 50 and 100 μg/kg and ranged between 70% and 120%. Precision was expressed as relative standard deviation (RSD), and it was evaluated for more than 160 pesticides as intra and inter-day precision, with values always below 20% and 25%, respectively. Limits of detection (LODs) ranged from 0.1 to 10 μg/kg, whereas limits of quantification (LOQs) from 0.5 to 20 μg/kg. The applicability of the method was proved by analysing soya-based nutraceuticals. Two pesticides were found in these samples, malathion and pyriproxyfen, at 11.1 and 1.5 μg/kg respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. Quality evaluation of Terpinen-4-ol type Australian Tea Tree oils and commercial products: An integrated approach using conventional and chiral GC/MS combined with chemometrics

    Science.gov (United States)

    Conventional GC/MS, chiral GC/MS and chemometric techniques were used to evaluate a large set of tea tree oils (TTO) and commercial products purported to contain tea tree oils. Fifty-seven known provenance pure Australian tea tree oils and forty-seven commercial TTO products were investigated. Twent...

  5. GC-MS metabolomic differentiation of selected citrus varieties with different sensitivity to citrus huanglongbing.

    Science.gov (United States)

    Cevallos-Cevallos, Juan M; Futch, David B; Shilts, Turksen; Folimonova, Svetlana Y; Reyes-De-Corcuera, José I

    2012-04-01

    Huanglongbing (HLB) is the most destructive disease of citrus worldwide. The rapid identification of tolerant varieties is considered a critical step towards controlling HLB. GC-MS metabolite profiles were used to differentiate HLB-tolerant citrus varieties 'Poncirus trifoliata' (TR) and 'Carrizo citrange' (CAR) from HLB-sensitive varieties 'Madam Vinous sweet orange' (MV) and 'Duncan' grapefruit (DG). PCR analyses revealed that MV was the most sensitive variety followed by DG and the tolerant varieties CAR and TR. Metabolomic multivariate analysis allowed classification of the cultivars in apparent agreement with PCR results. Higher levels of the amino acids l-proline, l-serine, and l-aspartic acid, as well as the organic acids butanedioic and tetradecanoic acid, and accumulation of galactose in healthy plants were characteristic of the most sensitive variety MV when compared to all other varieties. Only galactose was significantly higher in DG when compared to the tolerant varieties TR and CAR. The tolerant varieties showed higher levels of l-glycine and mannose when compared to sensitive varieties MV and DG. Profiling of the sensitive varieties MV and DG over a 20-week period after inoculation of those with the HLB-containing material revealed strong responses of metabolites to HLB infection that differed from the response of the tolerant varieties. Significant changes of l-threonine level in the leaves from old mature flushes and l-serine, l-threonine, scyllo-inositol, hexadecanoic acid, and mannose in the leaves from young developing flushes were observed in MV. Significant changes in myo-inositol in old flushes and l-proline, indole, and xylose in new flushes were observed in DG. Copyright © 2012 Elsevier Masson SAS. All rights reserved.

  6. Determination of Beeswax Hydrocarbons by Gas Chromatography with a Mass Detector (GC -MS Technique

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    Waś Ewa

    2014-06-01

    Full Text Available Here we describe a method of hydrocarbon (alkanes, alkenes, dienes identification and quantitative determination of linear saturated hydrocarbons (n-alkanes in beeswax using gas chromatography with a mass detector technique (GC -MS . Beeswax hydrocarbons were isolated using a solid-phase extraction (SPE technique with neutral aluminum oxide (Alumina - N, 1000 mg, 6 mL, then were separated on a non-polar gas chromatography column ZB-5HT INFERNO (20 m×0.18 mm×0.18 μm. Qquantitative analysis of n-alkanes was conducted by the method of internal standard with squalane used as the internal standard. The basic parameters of validation (linearity and working range, limit of determination, repeatability and reproducibility, recovery were determined. For all of the identified compounds, satisfactory (≥0.997 coefficients of correlation in the working ranges of the method (from 0.005 to 5.0 g/100 g were obtained. The elaborated method was characterized by satisfactory repeatability and within-laboratory reproducibility. The average coefficients of variation for the total n-alkanes did not exceed 2% under conditions of repeatability or 4% under conditions of reproducibility. The recovery for individual n-alkanes was above 94%; for their total content, it was 100.5%. In beeswax originating from Apis mellifera, n-alkanes containing from 20 to 35 carbon atoms in their molecules were determined. The total content of these alkanes was between 9.08 g and 10.86 g/100 g (on average, 9.81 g/100 g. Additionally, apart from the saturated hydrocarbons, unsaturated hydrocarbons and dienes were identified.

  7. Characterization of Source Signatures of Fine Roadway Particles by Pyrolysis-GC-MS

    Science.gov (United States)

    van Bergen, S. K.; Holmén, B. A.

    2001-12-01

    Fine particulate matter, defined as particles with an aerodynamic diameter less than 2.5 μ m (PM2.5), is of growing concern due to its detrimental effects on human health and the environment. Roadway traffic generates a significant fraction of PM2.5 in urban areas. Since exposure to fine particles derived from mobile sources commonly occurs, understanding the physicochemical processes that contribute to the generation, transport and atmospheric reactivity of roadway PM is important. Factors that influence the properties of roadway PM include: the mass, number and size distribution of the particles as well as their chemical composition. These factors are partially determined by the sources of the roadway particles. The focus of this effort is to identify unique organic chemical profiles of known roadway sources of PM using a new rapid characterization technique. A pyrolysis GC-MS analytical method is being developed to uniquely characterize the sources of roadway PM2.5 such as brake dust, tire wear, and direct emissions from diesel and gasoline engines. The source profiles will be used in conjunction with measurements of the composition of ambient roadway PM to determine the importance of the various roadway sources. The advantages of this technique over conventional solvent extractions include: smaller (mg) sample mass requirements, short extraction times and minimal sample handing. Preliminary two-step pyrolysis results will be presented for PM samples from individual sources and an ambient roadway. Specific analytical issues that will be discussed include: modifications of commercial pyrolysis hardware to improve reproducibility; desorption versus pyrolysis; developing appropriate pyrolysis programs for heterogenous sample materials; and method detection limits.

  8. Application of GC-FID and GC-MS for assessing PAHs in suspended dust.

    Science.gov (United States)

    Weglarz, A; Skrok, R

    2000-07-01

    The social concern about polycyclic aromatic hydrocarbons (PAHs) is due to the awareness that several of them are carcinogens and are present in polluted air. Several epidemiological investigations have tried to assess the influence of air pollution on the incidence in the population (1). Some authors have suggest that 1-10% of the incidence of lung cancer is caused by air pollution (2, 3). Several sources, e.g. traffic, oil heating, wood stoves, industry may contribute PAHs to the air pollution. Therefore continuous air pollution control applying selective and precise analytical procedures is needed. The submitted work presents results of examination of sixteen polycyclic aromatic hydrocarbons [naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, chrysene, benzo(a)anthracene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, indeno(1,2,3-cd)pyrene, dibenzo(a, h)anthracene, benzo(ghi)perylene] settled on particles of 10 microns fractions of ashes, emitted from industrial and communication sources. Samples of suspended dust were collected at twelve measuring points, from May to June 1998, in 24-hour cycles, in accordance with US EPA methodology. PAHs were extracted from suspended dust in a Soxhlet apparatus and then exposed to extraction in a liquid-solid system (solid extraction-SPE) to eliminate redundant pollution, which may interfere with compounds by determined analysis. Samples were then analyzed using by capillary gas chromatographs "Varian" model 3400 with FID and MS detectors. Results of analysis make it possible to determine the influence of industry and traffic on atmospheric pollution, to compare results of two analytical methods (GC-FID and GC-MS).

  9. Hypoglycemic Potential of Aqueous Extract of Moringa oleifera Leaf and In Vivo GC-MS Metabolomics

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    Washim Khan

    2017-09-01

    Full Text Available Moringa oleifera Lam. (family; Moringaceae, commonly known as drumstick, have been used for centuries as a part of the Ayurvedic system for several diseases without having any scientific data. Demineralized water was used to prepare aqueous extract by maceration for 24 h and complete metabolic profiling was performed using GC-MS and HPLC. Hypoglycemic properties of extract have been tested on carbohydrate digesting enzyme activity, yeast cell uptake, muscle glucose uptake, and intestinal glucose absorption. Type 2 diabetes was induced by feeding high-fat diet (HFD for 8 weeks and a single injection of streptozotocin (STZ, 45 mg/kg body weight, intraperitoneally was used for the induction of type 1 diabetes. Aqueous extract of M. oleifera leaf was given orally at a dose of 100 mg/kg to STZ-induced rats and 200 mg/kg in HFD mice for 3 weeks after diabetes induction. Aqueous extract remarkably inhibited the activity of α-amylase and α-glucosidase and it displayed improved antioxidant capacity, glucose tolerance and rate of glucose uptake in yeast cell. In STZ-induced diabetic rats, it produces a maximum fall up to 47.86% in acute effect whereas, in chronic effect, it was 44.5% as compared to control. The fasting blood glucose, lipid profile, liver marker enzyme level were significantly (p < 0.05 restored in both HFD and STZ experimental model. Multivariate principal component analysis on polar and lipophilic metabolites revealed clear distinctions in the metabolite pattern in extract and in blood after its oral administration. Thus, the aqueous extract can be used as phytopharmaceuticals for the management of diabetes by using as adjuvants or alone.

  10. Steroids excreted in urine by neonates with 21-hydroxylase deficiency. 2. Characterization, using GC-MS and GC-MS/MS, of pregnanes and pregnenes with an oxo- group on the A- or B-ring.

    Science.gov (United States)

    Christakoudi, Sofia; Cowan, David A; Taylor, Norman F

    2012-04-01

    Urine from neonates with 21-hydroxylase deficiency contains a large range of metabolites of 17-hydroxyprogesterone, 21-deoxycortisol and androgens but few have been previously described. We present the second part of a comprehensive project to characterize and identify these in order to enhance diagnosis and to further elucidate neonatal steroid metabolism. Steroids were analyzed, after extraction and enzymatic conjugate hydrolysis, as methyloxime-trimethylsilyl ether derivatives on gas-chromatographs coupled to quadrupole and ion-trap mass-spectrometers. GC-MS and GC-MS/MS spectra were used together to determine the structure of the A- and B-rings containing an oxo group. Fragmentations indicating presence of 3-, 6-, and 7-oxo groups and also 1β-, 2α-, 4β-, and 6β-hydroxyls are presented and discussed for the first time. Interpretation was aided by comparison with spectra of available relevant standards, of oxidation products of standards and urinary metabolites and of deuterated derivatives. Endogenous 1-enes and 2(3)-ene artifacts of non-hydrolyzed 3α-sulfates are also reported. D-ring and side chain structure was determined according to our previously published criteria. Likely metabolic relationships were also explored. We conclude that GC-MS combined with GC-MS/MS allows identification of the A- and B-ring structure of pregnane and pregnenes in the presence of an oxo group on one of these rings. Major oxygenations are 1β, 15β, 16α and 21-hydroxy and 6- and 7-oxo groups. Minor positions of hydroxylation are those at 2α, 4β and 6β. Three major metabolic streams exist in affected neonates in addition to the classical 3α-hydroxy-5β-pregnane pathway, i.e. these of the 3-oxo-4-enes as well as 3α- and 3β-hydroxy-5α-anes.

  11. Advanced Adaptive Optics Technology Development

    Energy Technology Data Exchange (ETDEWEB)

    Olivier, S

    2001-09-18

    The NSF Center for Adaptive Optics (CfAO) is supporting research on advanced adaptive optics technologies. CfAO research activities include development and characterization of micro-electro-mechanical systems (MEMS) deformable mirror (DM) technology, as well as development and characterization of high-resolution adaptive optics systems using liquid crystal (LC) spatial light modulator (SLM) technology. This paper presents an overview of the CfAO advanced adaptive optics technology development activities including current status and future plans.

  12. The analysis of linear and monomethylalkanes in exhaled breath samples by GC×GC-FID and GC-MS/MS.

    Science.gov (United States)

    Hengerics Szabó, Alexandra; Podolec, Peter; Ferenczy, Viktória; Kubinec, Róbert; Blaško, Jaroslav; Soják, Ladislav; Górová, Renáta; Addová, Gabriela; Ostrovský, Ivan; Višňovský, Jozef; Bierhanzl, Václav; Čabala, Radomír; Amann, Anton

    2015-01-26

    A new arrangement of the INCAT (inside needle capillary adsorption trap) device with Carbopack X and Carboxen 1000 as sorbent materials was applied for sampling, preconcentration and injection of C6C19n-alkanes and their monomethyl analogs in exhaled breath samples. For the analysis both GC-MS/MS and GC×GC-FID techniques were used. Identification of the analytes was based on standards, measured retention indices and selective SRM transitions of the individual isomers. The GC-MS/MS detection limits were in the range from 2.1 pg for n-tetradecane to 86 pg for 5-methyloctadecane. The GC×GC-FID detection limits ranged from 19 pg for n-dodecane to 110 pg for 3-methyloctane.

  13. THE SULFONATION STUDY OF REACTION MECHANISM ON PAPAVERINE ALKALOID BY GC-MS AND FT-IR

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    I Made Sudarma

    2010-06-01

    Full Text Available The aim of this research was to prove theoretical mechanism reaction on the sulfonation of papaverine alkaloid and the result could be used as a reference on the transformation of these alkaloid to the other derivatives. Theoriticaly sulfonation of papaverine (1 by HO-SO2Cl could produced papaverine sulfonyl chloride (1a. The formation of this product was analyzed by analytical thin layer chromatography GC-MS, and FT-IR. These analysis showed the formation of product (1a more favorable than the other. Tlc showed product (1a less polar than papaverine, and supported by GC-MS and infrared which showed molecular ion at m/z 412 due to the presence of -SO2Cl and vibration at 1153,4 dan 1265,2 Cm-1 due to absorption of sulfonyl group.   Keywords: reaction mechanism, sulfonation, papaverine alkaloid.

  14. GC/GC-MS analysis, isolation and identification of bioactive essential oil components from the Bhutanese medicinal plant, Pleurospermum amabile.

    Science.gov (United States)

    Wangchuk, Phurpa; Keller, Paul A; Pyne, Stephen G; Taweechotipatr, Malai; Kamchonwongpaisan, Sumalee

    2013-09-01

    We have hydrodistilled the essential oil (EO) from the aerial parts of the Bhutanese medicinal plant, Pleurospermum amabile using a Clevenger apparatus and evaluated this EO by GC/GC-MS and NMR analysis followed by testing for bioactivity. The GC-MS analysis identified 52 compounds with (E)-isomyristicin as a major component (32.2%). Repeated purification yielded four compounds; (E)-isomyristicin (1), (E)-isoapiol (2), methyl eugenol (3) and (E)-isoelemicin (4). Compound 2 and the mother EO showed the best antiplasmodial activity against the Plasmodium falciparum strains, TM4/8.2 (chloroquine and antifolate sensitive) and K1CB1 (multidrug resistant). They exhibited mild antibacterial activity against Bacillus subtilis. None of the test samples showed cytotoxicity.

  15. Enantioselective GC-MS analysis of volatile components from rosemary (Rosmarinus officinalis L.) essential oils and hydrosols.

    Science.gov (United States)

    Tomi, Kenichi; Kitao, Makiko; Konishi, Norihiro; Murakami, Hiroshi; Matsumura, Yasuki; Hayashi, Takahiro

    2016-05-01

    Essential oils and hydrosols were extracted from rosemary harvested in different seasons, and the chemical compositions of volatile components in the two fractions were analyzed by gas chromatography-mass spectrometry (GC-MS). Enantiomers of some volatile components were also analyzed by enantioselective GC-MS. Classification of aroma components based on chemical groups revealed that essential oils contained high levels of monoterpene hydrocarbons but hydrosols did not. Furthermore, the enantiomeric ratios within some volatile components were different from each other; for example, only the (S)-form was observed for limonene and the (R)-form was dominant for verbenone. These indicate the importance of determining the enantiomer composition of volatile components for investigating the physiological and psychological effects on humans. Overall, enantiomeric ratios were determined by volatile components, with no difference between essential oils and hydrosols or between seasons.

  16. Quantitative determination of volatile organic compounds (VOC) in milk by multiple dynamic headspace extraction and GC-MS.

    Science.gov (United States)

    Ciccioli, Paolo; Brancaleoni, Enzo; Frattoni, Massimiliano; Fedele, Vincenzo; Claps, Salvatore; Signorelli, Federica

    2004-01-01

    A method for the accurate determination of volatile organic compounds (VOC) in milk samples has been developed and tested. It combines multiple dynamic headspace extraction with GC-MS. Absolute amounts of VOC in the liquid phase are obtained by determining the first order kinetic dependence of the stepwise extraction of the analytes and internal standards from the liquid matrix. Compounds released from milk were collected on a train of traps filled with different solid sorbents to cover all components having a number of carbon atoms ranging from 4 to 15. They were analysed by GC-MS after thermal desorption of VOC from the collecting traps. Quantification of VOC in milk was performed using deuterated compounds as internal standards. The method was used to follow seasonal variations of monoterpenes in goat milk and to detect the impact of air pollution on the quality of milk.

  17. Analysis of the essential oils of Coriandrum sativum Using GC-MS coupled with chemometric resolution methods.

    Science.gov (United States)

    Zhou, Zhi-Feng; Chen, Ling-Yun; Shen, Mei; Ma, An-De; Yang, Xue-Mei; Zou, Fei

    2011-01-01

    The essential oils extracted from Coriandrum sativum L. were analyzed by GC-MS coupled with chemometric resolution methods. Through the chemometric resolution methods, peak clusters were uniquely resolved into the pure chromatographic profiles and mass spectra of each component. Qualitative analysis was performed by comparing the pure mass spectra with those in the NIST 05 mass spectral library. Quantitative analysis was performed using the total volume integration method. A total of 118 constituents were detected, of which 104 were identified, accounting for 97.27% of the total content. The results indicate that GC-MS combined with chemometric resolution methods can greatly enhance the capability of separation and the reliability of qualitative and quantitative results. The combined method is an economical and accurate approach for the rapid analysis of the complex essential oil samples in Coriandrum sativum L.

  18. Advanced stitching technology

    Science.gov (United States)

    Scardino, Frank L.

    1992-01-01

    In the design of textile composites, the selection of materials and constructional techniques must be matched with product performance, productivity, and cost requirements. Constructional techniques vary. A classification of various textile composite systems is given. In general, the chopped fiber system is not suitable for structural composite applications because of fiber discontinuity, uncontrolled fiber orientation and a lack of fiber integration or entanglement. Linear filament yarn systems are acceptable for structural components which are exposed to simple tension in their applications. To qualify for more general use as structural components, filament yarn systems must be multi-directionally positioned. With the most sophisticated filament winding and laying techniques, however, the Type 2 systems have limited potential for general load-bearing applications because of a lack of filament integration or entanglement, which means vulnerability to splitting and delamination among filament layers. The laminar systems (Type 3) represented by a variety of simple fabrics (woven, knitted, braided and nonwoven) are especially suitable for load-bearing panels in flat form and for beams in a roled up to wound form. The totally integrated, advanced fabric system (Type 4) are thought to be the most reliable for general load-bearing applications because of fiber continuity and because of controlled multiaxial fiber orientation and entanglement. Consequently, the risk of splitting and delamination is minimized and practically omitted. Type 4 systems can be woven, knitted, braided or stitched through with very special equipment. Multiaxial fabric technologies are discussed.

  19. Determination of acrylamide in Thai-conventional snacks from Nong Mon market, Chonburi using GC-MS technique.

    Science.gov (United States)

    Komthong, P; Suriyaphan, O; Charoenpanich, J

    2012-01-01

    Acrylamide in Thai-conventional snacks was analysed by GC/MS with a linear response ranged of 5-50 µg and r² > 0.99. The limit of detection (s/n = 3) and limit of quantification (s/n = 10) were 4 and 15 µg kg⁻¹, respectively, and RSD snacks possessed low concentrations (habits by 400 tourists indicate a daily intake of acrylamide <150 ng, well below a toxic dose.

  20. Pyrolysis-GC-MS analysis of the formation and degradation stages of charred residues from lignocellulosic biomass

    OpenAIRE

    González-Vila, Francisco Javier; Tinoco, Pilar; Almendros Martín, Gonzalo; Martín Martínez, Francisco

    2001-01-01

    The structural transformations undergone by lignocellulosic biomass (freeze-dried rye grass, Lolium rigidum) subjected to progressive isothermal heating (burning at 350°C under oxidizing conditions for 30, 45, 60, 75, and 90 s) have been monitored by Curie-point pyrolysis-gas chromatographymass spectrometry (Py-GC-MS). The pyrograms suggest that even charred residues after severe heating (carbon loss ca. 50%) still contain substantial concentrations of some resistant plant structural componen...

  1. The MetabolomeExpress Project: enabling web-based processing, analysis and transparent dissemination of GC/MS metabolomics datasets

    Directory of Open Access Journals (Sweden)

    Carroll Adam J

    2010-07-01

    Full Text Available Abstract Background Standardization of analytical approaches and reporting methods via community-wide collaboration can work synergistically with web-tool development to result in rapid community-driven expansion of online data repositories suitable for data mining and meta-analysis. In metabolomics, the inter-laboratory reproducibility of gas-chromatography/mass-spectrometry (GC/MS makes it an obvious target for such development. While a number of web-tools offer access to datasets and/or tools for raw data processing and statistical analysis, none of these systems are currently set up to act as a public repository by easily accepting, processing and presenting publicly submitted GC/MS metabolomics datasets for public re-analysis. Description Here, we present MetabolomeExpress, a new File Transfer Protocol (FTP server and web-tool for the online storage, processing, visualisation and statistical re-analysis of publicly submitted GC/MS metabolomics datasets. Users may search a quality-controlled database of metabolite response statistics from publicly submitted datasets by a number of parameters (eg. metabolite, species, organ/biofluid etc.. Users may also perform meta-analysis comparisons of multiple independent experiments or re-analyse public primary datasets via user-friendly tools for t-test, principal components analysis, hierarchical cluster analysis and correlation analysis. They may interact with chromatograms, mass spectra and peak detection results via an integrated raw data viewer. Researchers who register for a free account may upload (via FTP their own data to the server for online processing via a novel raw data processing pipeline. Conclusions MetabolomeExpress https://www.metabolome-express.org provides a new opportunity for the general metabolomics community to transparently present online the raw and processed GC/MS data underlying their metabolomics publications. Transparent sharing of these data will allow researchers to

  2. Determination of volatile aroma compounds of Ganoderma lucidum by gas chromatography mass spectrometry (HS-GC/MS).

    Science.gov (United States)

    Taşkın, Hatıra; Kafkas, Ebru; Çakıroğlu, Özgün; Büyükalaca, Saadet

    2013-01-01

    This study was conducted at Horticulture Department of Cukurova University, Adana, Turkey during 2010-2011. Fresh sample of Ganoderma lucidum collected from Mersin province of Turkey was used as material. Volatile aroma compounds were performed by Headspace Gas Chromatography (HS-GC/MS). Alcohols, aldehydes, acids, phenol, L-Alanine, d-Alanine, 3Methyl, 2-Butanamine, 2-Propanamine were determined. 1-Octen-3-ol (Alcohol) and 3-methyl butanal (Aldehyde) were identified as major aroma compounds.

  3. Biodiesel production from microalgal isolates of southern Pakistan and quantification of FAMEs by GC-MS/MS analysis

    Directory of Open Access Journals (Sweden)

    Musharraf Syed

    2012-12-01

    Full Text Available Abstract Background Microalgae have attracted major interest as a sustainable source for biodiesel production on commercial scale. This paper describes the screening of six microalgal species, Scenedesmus quadricauda, Scenedesmus acuminatus, Nannochloropsis sp., Anabaena sp., Chlorella sp. and Oscillatoria sp., isolated from fresh and marine water resources of southern Pakistan for biodiesel production and the GC-MS/MS analysis of their fatty acid methyl esters (FAMEs. Results Growth rate, biomass productivity and oil content of each algal species have been investigated under autotrophic condition. Biodiesel was produced from algal oil by acid catalyzed transesterification reaction and resulting fatty acid methyl esters (FAMEs content was analyzed by GC/MS. Fatty acid profiling of the biodiesel, obtained from various microalgal oils showed high content of C-16:0, C-18:0, cis-Δ9C-18:1, cis-Δ11C-18:1 (except Scenedesmus quadricauda and 10-hydroxyoctadecanoic (except Scenedesmus acuminatus. Absolute amount of C-14:0, C-16:0 and C-18:0 by a validated GC-MS/MS method were found to be 1.5-1.7, 15.0-42.5 and 4.2-18.4 mg/g, respectively, in biodiesel obtained from various microalgal oils. Biodiesel was also characterized in terms of cetane number, kinematic viscosity, density and higher heating value and compared with the standard values. Conclusion Six microalgae of local origin were screened for biodiesel production. A method for absolute quantification of three important saturated fatty acid methyl esters (C-14, C-16 and C-18 by gas chromatography-tandem mass spectrometry (GC-MS/MS, using multiple reactions monitoring (MRM mode, was employed for the identification and quantification of biodiesels obtained from various microalgal oils. The results suggested that locally found microalgae can be sustainably harvested for the production of biodiesel. This offers the tremendous economic opportunity for an energy-deficient nation.

  4. Effect of Genetics, Environment, and Phenotype on the Metabolome of Maize Hybrids Using GC/MS and LC/MS.

    Science.gov (United States)

    Tang, Weijuan; Hazebroek, Jan; Zhong, Cathy; Harp, Teresa; Vlahakis, Chris; Baumhover, Brian; Asiago, Vincent

    2017-06-28

    We evaluated the variability of metabolites in various maize hybrids due to the effect of environment, genotype, phenotype as well as the interaction of the first two factors. We analyzed 480 forage and the same number of grain samples from 21 genetically diverse non-GM Pioneer brand maize hybrids, including some with drought tolerance and viral resistance phenotypes, grown at eight North American locations. As complementary platforms, both GC/MS and LC/MS were utilized to detect a wide diversity of metabolites. GC/MS revealed 166 and 137 metabolites in forage and grain samples, respectively, while LC/MS captured 1341 and 635 metabolites in forage and grain samples, respectively. Univariate and multivariate analyses were utilized to investigate the response of the maize metabolome to the environment, genotype, phenotype, and their interaction. Based on combined percentages from GC/MS and LC/MS datasets, the environment affected 36% to 84% of forage metabolites, while less than 7% were affected by genotype. The environment affected 12% to 90% of grain metabolites, whereas less than 27% were affected by genotype. Less than 10% and 11% of the metabolites were affected by phenotype in forage and grain, respectively. Unsupervised PCA and HCA analyses revealed similar trends, i.e., environmental effect was much stronger than genotype or phenotype effects. On the basis of comparisons of disease tolerant and disease susceptible hybrids, neither forage nor grain samples originating from different locations showed obvious phenotype effects. Our findings demonstrate that the combination of GC/MS and LC/MS based metabolite profiling followed by broad statistical analysis is an effective approach to identify the relative impact of environmental, genetic and phenotypic effects on the forage and grain composition of maize hybrids.

  5. GC-MS in the analysis of organic compounds in meteorites. [Gas Chromatography-Mass Spectroscopy approaches

    Science.gov (United States)

    Lawless, J. G.; Romiez, M. P.

    1974-01-01

    The application of an analytical approach combining gas chromatography with mass spectrometry (GC-MS) has shown that the amino acid composition of meteorite extracts is quite complex. A computer was used in the evaluation of the data obtained in the investigations. The computer programs developed have been concerned solely with the mass spectra of amino acids. Specialized programs have been written to determine the number of carbon atoms in an amino acid which is a member of any of three subclasses.

  6. Application of Gas Chromatography with the Mass Detector (GC-MS) Technique for Detection of Beeswax Adulteration with Paraffin

    OpenAIRE

    Waś Ewa; Szczęsna Teresa; Rybak-Chmielewska Helena

    2015-01-01

    To detect beeswax adulteration with hydrocarbons of alien origin (e.g. paraffin), gas chromatography with mass detector (GC-MS) technique was used. The method has been verified here on beeswax samples with different addition (3, 5, 10, 30, and 50%) of paraffin and validated under the conditions of repeatability and within - laboratory reproducibility. The addition of paraffin to beeswax can already be detected on the basis of an analysis of the chromatograms. The intensity of individual alkan...

  7. Electronic nose and GC-MS analysis of volatile compounds in Tuber magnatum Pico: evaluation of different storage conditions.

    Science.gov (United States)

    Pennazza, G; Fanali, C; Santonico, M; Dugo, L; Cucchiarini, L; Dachà, M; D'Amico, A; Costa, R; Dugo, P; Mondello, L

    2013-01-15

    The characteristic aromatic composition of white truffles (Tuber magnatum Pico) determines its culinary and commercial value. However modifications of truffle organoleptic proprieties occur during preservation. A study of headspace of white truffles by using Electronic nose (E-nose), gas chromatography-mass spectrometry (GC-MS) and sensory analyses was performed. Truffles were stored at different conditions for 7 days: +4 and +8°C wrapped in blotting paper or covered by rice or none of the above. Headspace E-nose measurements and sensory analyses were performed each day. Statistical multivariate analysis of the data showed the capability of E-nose to predict sensorial analysis scores and to monitor aroma profile changes during storage. Truffle's volatile molecules were also extracted by headspace solid phase microextraction technique and separated and identified by GC-MS. Partial Components Analysis of data was performed. E-nose and GC-MS results were in agreement and showed that truffle storage in paper at +8°C seemed to be the best storage condition.

  8. High Throughput Analytical Techniques for the Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea by GC/MS, GC/MS/MS, and LC/MS/MS: Collaborative Study, First Action 2014.09.

    Science.gov (United States)

    Pang, Guo-Fang; Fan, Chun-Lin; Cao, Yan-Zhong; Yan, Fang; Li, Yan; Kang, Jian; Chen, Hui; Chang, Qiao-Ying

    2015-01-01

    Thirty laboratories from fom North and South America, Europe, and Asia participated in this AOAC collaborative study (15 from China; five from Germany; two each from Italy and the United States; and one each from the Republic of Korea, Canada, Spain, Japan, Belgium, and India). Participants represented government regulatory, commercial testing, university, research institute, and private laboratories. The single-laboratory validated (SLV) tea method was evaluated in the collaborative study to determine the recovery and reproducibility of the method under multilaboratory conditions. Since there were no restrictions regarding the type of analytical instrumentation to use for the analyses, laboratories used a combination of equipment that included GC/MS, GC/MS/MS, and LC/MS/MS instruments from 22 different manufacturers, 21 brands of GC and LC columns, 13 different GC temperature programming profiles, 11 LC gradient elution programs, and six different vendor manufactured SPE cartridges. Even though all the analytical performance parameters for all the 653 compounds had been determined in the SLV study, guidance was obtained from an expert review panel of the AOAC Method-Centric Committee on Pesticide Residues to conduct the multilaboratory collaborative study based on 20 selected compounds that can be analyzed by GC/MS and 20 compounds that can be analyzed by LC/MS/MS. Altogether, 560 samples covering the 40 selected pesticides were analyzed in the study. These samples included green tea and oolong tea samples fortified typically at the European Union maximum residue limit for regulatory guidance and compliance, aged tea samples incurred with 20 pesticides, and green tea and oolong tea samples incurred with five pesticides. The analysis of the 560 samples generated a total of 82 459 test results by the 30 participating laboratories. One laboratory failed to meet the proficiency requirements in the precollaborative study. Therefore, its data submitted for the

  9. Marketing technologically advanced products

    NARCIS (Netherlands)

    Bender, Horst

    1989-01-01

    This paper calls for a merger of technology and marketing under a customer value perspective; for an enhancement of the traditional technological innovation orientation of the technology-based firm with a market thrust. It establishes technology-based products as product-service offerings that are d

  10. Comparative analysis of EPA and DHA in fish oil nutritional capsules by GC-MS.

    Science.gov (United States)

    Yi, Tao; Li, Shuk-Man; Fan, Jia-Yi; Fan, Lan-Lan; Zhang, Zhi-Feng; Luo, Pei; Zhang, Xiao-Jun; Wang, Jian-Gang; Zhu, Lin; Zhao, Zhong-Zhen; Chen, Hu-Biao

    2014-12-13

    Fish oil is a popular nutritional product consumed in Hong Kong. Eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are the two main bioactive components responsible for the health benefits of fish oil. Market survey in Hong Kong demonstrated that various fish oil capsules with different origins and prices are sold simultaneously. However, these capsules are labelled with same ingredient levels, namely EPA 180 mg/g and DHA 120 mg/g. This situation makes the consumers very confused. To evaluate the quality of various fish oil capsules, a comparative analysis of the contents of EPA and DHA in fish oil is crucial. A gas chromatography-mass spectrometry (GC-MS) method was developed for identification and determination of EPA and DHA in fish oil capsules. A comprehensive validation of the developed method was conducted. Ten batches of fish oil capsules samples purchased from drugstores of Hong Kong were analyzed by using the developed method. The present method presented good sensitivity, precision and accuracy. The limits of detection (LOD) for EPA and DHA were 0.08 ng and 0.21 ng, respectively. The relative standard deviation (RSD) values of EPA and DHA for repeatability tests were both less than 1.05%; and the recovery for accuracy test of EPA and DHA were 100.50% and 103.83%, respectively. In ten fish oil samples, the contents of EPA ranged from 39.52 mg/g to 509.16 mg/g, and the contents of DHA ranged from 35.14 mg/g to 645.70 mg/g. The present method is suitable for the quantitative analysis of EPA and DHA in fish oil capsules. There is a significant variation in the contents of the quantified components in fish oil samples, and there is not a linear relationship between price and contents of EPA and DHA. Strict supervision of the labelling of the fish oil capsules is urgently needed.

  11. Organization of GC/MS and LC/MS metabolomics data into chemical libraries

    Directory of Open Access Journals (Sweden)

    DeHaven Corey D

    2010-10-01

    Full Text Available Abstract Background Metabolomics experiments involve generating and comparing small molecule (metabolite profiles from complex mixture samples to identify those metabolites that are modulated in altered states (e.g., disease, drug treatment, toxin exposure. One non-targeted metabolomics approach attempts to identify and interrogate all small molecules in a sample using GC or LC separation followed by MS or MSn detection. Analysis of the resulting large, multifaceted data sets to rapidly and accurately identify the metabolites is a challenging task that relies on the availability of chemical libraries of metabolite spectral signatures. A method for analyzing spectrometry data to identify and Quantify Individual Components in a Sample, (QUICS, enables generation of chemical library entries from known standards and, importantly, from unknown metabolites present in experimental samples but without a corresponding library entry. This method accounts for all ions in a sample spectrum, performs library matches, and allows review of the data to quality check library entries. The QUICS method identifies ions related to any given metabolite by correlating ion data across the complete set of experimental samples, thus revealing subtle spectral trends that may not be evident when viewing individual samples and are likely to be indicative of the presence of one or more otherwise obscured metabolites. Results LC-MS/MS or GC-MS data from 33 liver samples were analyzed simultaneously which exploited the inherent biological diversity of the samples and the largely non-covariant chemical nature of the metabolites when viewed over multiple samples. Ions were partitioned by both retention time (RT and covariance which grouped ions from a single common underlying metabolite. This approach benefitted from using mass, time and intensity data in aggregate over the entire sample set to reject outliers and noise thereby producing higher quality chemical identities. The

  12. Tire traces - discrimination and classification of pyrolysis-GC/MS profiles.

    Science.gov (United States)

    Gueissaz, Line; Massonnet, Geneviève

    2013-07-10

    Tire traces can be observed on several crime scenes as vehicles are often used by criminals. The tread abrasion on the road, while braking or skidding, leads to the production of small rubber particles which can be collected for comparison purposes. This research focused on the statistical comparison of Py-GC/MS profiles of tire traces and tire treads. The optimisation of the analytical method was carried out using experimental designs. The aim was to determine the best pyrolysis parameters regarding the repeatability of the results. Thus, the pyrolysis factor effect could also be calculated. The pyrolysis temperature was found to be five time more important than time. Finally, a pyrolysis at 650°C during 15s was selected. Ten tires of different manufacturers and models were used for this study. Several samples were collected on each tire, and several replicates were carried out to study the variability within each tire (intravariability). More than eighty compounds were integrated for each analysis and the variability study showed that more than 75% presented a relative standard deviation (RSD) below 5% for the ten tires, thus supporting a low intravariability. The variability between the ten tires (intervariability) presented higher values and the ten most variant compounds had a RSD value above 13%, supporting their high potential of discrimination between the tires tested. Principal Component Analysis (PCA) was able to fully discriminate the ten tires with the help of the first three principal components. The ten tires were finally used to perform braking tests on a racetrack with a vehicle equipped with an anti-lock braking system. The resulting tire traces were adequately collected using sheets of white gelatine. As for tires, the intravariability for the traces was found to be lower than the intervariability. Clustering methods were carried out and the Ward's method based on the squared Euclidean distance was able to correctly group all of the tire traces

  13. Unique ion filter: a data reduction tool for GC/MS data preprocessing prior to chemometric analysis.

    Science.gov (United States)

    Adutwum, L A; Harynuk, J J

    2014-08-01

    Using raw GC/MS data as the X-block for chemometric modeling has the potential to provide better classification models for complex samples when compared to using the total ion current (TIC), extracted ion chromatograms/profiles (EIC/EIP), or integrated peak tables. However, the abundance of raw GC/MS data necessitates some form of data reduction/feature selection to remove the variables containing primarily noise from the data set. Several algorithms for feature selection exist; however, due to the extreme number of variables (10(6)-10(8) variables per chromatogram), the feature selection time can be prolonged and computationally expensive. Herein, we present a new prefilter for automated data reduction of GC/MS data prior to feature selection. This tool, termed unique ion filter (UIF), is a module that can be added after chromatographic alignment and prior to any subsequent feature selection algorithm. The UIF objectively reduces the number of irrelevant or redundant variables in raw GC/MS data, while preserving potentially relevant analytical information. In the m/z dimension, data are reduced from a full spectrum to a handful of unique ions for each chromatographic peak. In the time dimension, data are reduced to only a handful of scans around each peak apex. UIF was applied to a data set of GC/MS data for a variety of gasoline samples to be classified using partial least-squares discriminant analysis (PLS-DA) according to octane rating. It was also applied to a series of chromatograms from casework fire debris analysis to be classified on the basis of whether or not signatures of gasoline were detected. By reducing the overall population of candidate variables subjected to subsequent variable selection, the UIF reduced the total feature selection time for which a perfect classification of all validation data was achieved from 373 to 9 min (98% reduction in computing time). Additionally, the significant reduction in included variables resulted in a concomitant

  14. Flunitrazepam excretion patterns using the Abuscreen OnTrak and OnLine immunoassays: comparison with GC-MS.

    Science.gov (United States)

    Salamone, S J; Honasoge, S; Brenner, C; McNally, A J; Passarelli, J; Goc-Szkutnicka, K; Brenneisen, R; elSohly, M A; Feng, S

    1997-09-01

    A study was conducted to compare the performance of the OnLine and OnTrak immunoassays for benzodiazepines with gas chromatographic-mass spectrometric (GC-MS) analysis in detecting flunitrazepam (FNP) and its metabolites in human urine. Urine was collected over a 72-h period from six individuals (four male and two female) who had taken a single oral dose of either 1 or 4 mg of FNP. The OnTrak assay was run at a 100-ng/mL cutoff of nordiazepam (NDP), and the OnLine assay was run with a standard curve from zero to 200 ng/mL of NDP with and without beta-glucuronidase treatment. Each sample was analyzed by GC-MS using FNP, 7-amino-FNP, 3-hydroxy-FNP, desmethyl-FNP, 7-amino-3-hydroxy-FNP, and desmethyl-3-hydroxy-FNP as standards with beta-glucuronidase treatment. The specimens from the 1-mg dose did not yield a positive result by immunoassay over the 72-h collection period. Specimens from the 4-mg dose did yield positive results in both immunoassays. The time of the first positive result ranged from 4 to 12 h, and the time to the last positive result ranged from 18 to 60 h. Treatment of the samples with beta-glucuronidase increased the OnLine values between 20 and 60%, but it did not appreciably increase the detection time. GC-MS analysis showed no detectable levels of FNP, 3-hydroxy-FNP, desmethyl-FNP, 7-amino-3-hydroxy-FNP, and desmethyl-3-hydroxy-FNP. However, all samples collected past time zero showed detectable levels of 7-amino-FNP (> 2 ng/mL) with peak concentrations at 12-36 h. The peak levels of 7-amino-FNP by GC-MS paralleled the peak levels of the immunoassay response. The amount of 7-amino-FNP metabolite quantitated by GC-MS, however, accounted for only 15-20% of the total immunoassay crossreactive FNP metabolites.

  15. Advances in FIV vaccine technology

    OpenAIRE

    Uhl, Elizabeth W.; Martin, Marcus; Coleman, James K.; Yamamoto, Janet K.

    2008-01-01

    Advances in vaccine technology are occurring in the molecular techniques used to develop vaccines and in the assessment of vaccine efficacy, allowing more complete characterization of vaccine-induced immunity correlating to protection. FIV vaccine development has closely mirrored and occasionally surpassed the development of HIV-1 vaccine, leading to first licensed technology. This review will discuss technological advances in vaccine designs, challenge infection assessment, and characterizat...

  16. A post-modification approach to independent component analysis for resolution of overlapping GC/MS signals: from independent components to chemical components

    Institute of Scientific and Technical Information of China (English)

    WANG Wei; CAI WenSheng; SHAO XueGuang

    2007-01-01

    Independent component analysis (ICA) has demonstrated its power to extract mass spectra from overlapping GC/MS signal. However, there is still a problem that mass spectra with negative peaks at some m/z will be obtained in the resolved results when there are overlapping peaks in the mass spectra of a mixture. Based on a detail theoretical analysis of the preconditions for ICA and the non-negative property of GC/MS signals, a post-modification based on chemical knowledge (PMBK) strategy is proposed to solve this problem. By both simulated and experimental GC/MS signals, it was proved that the PMBK strategy can improve the resolution effectively.

  17. Advancement in Engineering Technology

    DEFF Research Database (Denmark)

    Kalia, Kartik; Rehman, M. Atiqur; Hussain, Dil muhammed Akbar

    2016-01-01

    In this paper we will be discussing about the impact of technology on our daily lives. How everybody is dependent upon technology in one or other way. Methods/Statistical Analysis: Technology has played a significant role in the evolution of the society. Science has produced many new ideas...... but to harvest those ideas, technology is a must. With the huge requirement of engineering equipment's, the industry needs specialists who can manage and operate these technologies. Detailed information about the merits and demerits of technology is also mentioned in this paper. Findings: Technology has affected...... the environment on a great scale; in some cases, technology is even replacing human being or use of manpower. So proper counter measures have been mentioned, which can be used to control and limit harmful effect....

  18. Advancement in Engineering Technology

    DEFF Research Database (Denmark)

    Kalia, Kartik; Rehman, M. Atiqur; Hussain, Dil muhammed Akbar

    2016-01-01

    In this paper we will be discussing about the impact of technology on our daily lives. How everybody is dependent upon technology in one or other way. Methods/Statistical Analysis: Technology has played a significant role in the evolution of the society. Science has produced many new ideas...... but to harvest those ideas, technology is a must. With the huge requirement of engineering equipment's, the industry needs specialists who can manage and operate these technologies. Detailed information about the merits and demerits of technology is also mentioned in this paper. Findings: Technology has affected...... the environment on a great scale; in some cases, technology is even replacing human being or use of manpower. So proper counter measures have been mentioned, which can be used to control and limit harmful effect....

  19. GC-MS and NMR analysis of the bioactive compounds from the crude extracts ofWaltheria indica and the histopathological changes induced in albino rats challenged withNaja nigricollis venom

    Institute of Scientific and Technical Information of China (English)

    Philip Ilani; Nicholas Ajodo; Folashade Adewusi; Samirat Yakubu; Victor Yakubu Cosmos; Ache Eunice; Atonila Kayode Ezekiel; Oshiedu Sarah; Emmanuel Amlabu

    2016-01-01

    Objective:To develop a characteristic fingerprint of the different chemical compounds of plant by gas chromatography-mass spectrometer (GC-MS) and nuclear magnetic resonance (NMR) analysis and assess the effect of the crude extract on histological changes induced inNaja nigricollis(N. nigricollis)envenomed albino rats. Methods: The coarsely powderedWaltheria indica (W. indica) whole plant material was extracted using 70% methanol.GC-MS analysis was carried out using a ShimadzuGC-MS QP 2010 plus system of gas chromatography interfaced to a mass spectrometer. The identification of components was based on National Institute of Standard and Technology-08 and Willey-8 libraries. Hydrogen-NMR spectra of the extracts was performed using Bruker Biospin Avance 400-MHzNMR spectrophotometer with a 5 mm broad inverse probe head, equipped with shielded z-gradient accessories andC-13 NMR hetero-nuclear single quantum correction was carried out using the Brucker’s standard pulse library. The efficacy of the crude extract ofW. indica whole plant was tested and the lesions induced in the liver, brain and kidney of albino rats challenged withN. nigricollis were analyzed by light microscopy. Results:The identification of the bioactive compounds fromW. indica byGC-MS analysis revealed 41 peaks. A total of 38 compounds were identified with majority having important pharmacological activities that included anti-microbial, anti-cancer, anti-oxidant anti-inflammatory, anti-allergenic, anti-ageing, anti-arthritic, larvicidal, anti-convulsant and herbicidal activities.C-13 and hydrogen-NMR analysis ofW. indica elucidated key bioactive compounds in the whole plant that were consistent with the classes of bioactive compounds detected byGC-MS analysis. The efficacy of the crude extract ofW. indica whole plant in ameliorating histopathological lesions induced in the liver, brain and kidney of albino rats challenged withN. nigricollis venom revealed the abrogation of tissue degeneration when

  20. GC-MS and NMR analysis of the bioactive compounds from the crude extracts of Waltheria indica and the histopathological changes induced in albino rats challenged with Naja nigricollis venom

    Directory of Open Access Journals (Sweden)

    Philip Ilani

    2016-05-01

    Full Text Available Objective: To develop a characteristic fingerprint of the different chemical compounds of plant by gas chromatography-mass spectrometer (GC-MS and nuclear magnetic resonance (NMR analysis and assess the effect of the crude extract on histological changes induced in Naja nigricollis (N. nigricollis envenomed albino rats. Methods: The coarsely powdered Waltheria indica (W. indica whole plant material was extracted using 70% methanol. GC-MS analysis was carried out using a Shimadzu GC-MS QP 2010 plus system of gas chromatography interfaced to a mass spectrometer. The identification of components was based on National Institute of Standard and Technology-08 and Willey-8 libraries. Hydrogen-NMR spectra of the extracts was performed using Bruker Biospin Avance 400-MHz NMR spectrophotometer with a 5 mm broad inverse probe head, equipped with shielded z-gradient accessories and C-13 NMR hetero-nuclear single quantum correction was carried out using the Brucker’s standard pulse library. The efficacy of the crude extract of W. indica whole plant was tested and the lesions induced in the liver, brain and kidney of albino rats challenged with N. nigricollis were analyzed by light microscopy. Results: The identification of the bioactive compounds from W. indica by GC-MS analysis revealed 41 peaks. A total of 38 compounds were identified with majority having important pharmacological activities that included anti-microbial, anti-cancer, anti-oxidant antiinflammatory, anti-allergenic, anti-ageing, anti-arthritic, larvicidal, anti-convulsant and herbicidal activities. C-13 and hydrogen-NMR analysis of W. indica elucidated key bioactive compounds in the whole plant that were consistent with the classes of bioactive compounds detected by GC-MS analysis. The efficacy of the crude extract of W. indica whole plant in ameliorating histopathological lesions induced in the liver, brain and kidney of albino rats challenged with N. nigricollis venom revealed the

  1. Advanced Materials Technology

    Science.gov (United States)

    Blankenship, C. P. (Compiler); Teichman, L. A. (Compiler)

    1982-01-01

    Composites, polymer science, metallic materials (aluminum, titanium, and superalloys), materials processing technology, materials durability in the aerospace environment, ceramics, fatigue and fracture mechanics, tribology, and nondestructive evaluation (NDE) are discussed. Research and development activities are introduced to the nonaerospace industry. In order to provide a convenient means to help transfer aerospace technology to the commercial mainstream in a systematic manner.

  2. GC-MS analysis, preliminary phytochemical screening, physicochemical analysis and anti-diabetic activity of ethanol extract of Jasminum cuspidatum leaves

    National Research Council Canada - National Science Library

    Singumsetty Vinay; Shaik Karimulla; Devarajan Saravanan

    2014-01-01

    The purpose of the present study was investigating the GC-MS analysis, preliminary phytochemical screening, physicochemical analysis and anti-diabetic activity of ethanol extract of the leaves of Jasminum cuspidatum...

  3. EPA Method 525.3 - Determination of Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

    Science.gov (United States)

    Method 525.3 is an analytical method that uses solid phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) for the identification and quantitation of 125 selected semi-volatile organic chemicals in drinking water.

  4. Advances in Gyroscope Technologies

    CERN Document Server

    Armenise, Mario N; Dell'Olio, Francesco; Passaro, Vittorio MN

    2011-01-01

    This monograph collects and critically reviews the main results obtained by the scientific community in gyroscope technologies research field. It describes architectures, design techniques and fabrication technology of angular rate sensors proposed in literature. MEMS, MOEMS, optical and mechanical technologies are discussed together with achievable performance. The book also considers future research trends aimed to cover special applications. The book is intended for researchers and Ph.D. students interested in modelling, design and fabrication of gyros. The book may be a useful education su

  5. Advances in production technology

    CERN Document Server

    2015-01-01

    This edited volume contains the selected papers presented at the scientific board meeting of the German Cluster of Excellence on “Integrative Production Technology for High-Wage Countries”,  held in November 2014. The topical structure of the book is clustered in six sessions: Integrative Production Technology, Individualised Production, Virtual Production Systems, Integrated Technologies, Self-Optimising Production Systems and Human Factors in Production Technology. The Aachen perspective on a holistic theory of production is complemented by conference papers from external leading researchers in the fields of production, materials science and bordering disciplines. The target audience primarily comprises research experts and practitioners in the field but the book may also be beneficial for graduate students.

  6. Assessing Advanced Technology in CENATE

    Energy Technology Data Exchange (ETDEWEB)

    Tallent, Nathan R.; Barker, Kevin J.; Gioiosa, Roberto; Marquez, Andres; Kestor, Gokcen; Song, Shuaiwen; Tumeo, Antonino; Kerbyson, Darren J.; Hoisie, Adolfy

    2016-08-08

    PNNL's Center for Advanced Technology Evaluation (CENATE) is a new U.S. Department of Energy center whose mission is to assess and facilitate access to emerging computing technology. CENATE is assessing a range of advanced technologies, from evolutionary to disruptive. Technologies of interest include the processor socket (homogeneous and accelerated systems), memories (dynamic, static, memory cubes), motherboards, networks (network interface cards and switches), and input/output and storage devices. CENATE is developing a multi-perspective evaluation process based on integrating advanced system instrumentation, performance measurements, and modeling and simulation. We show evaluations of two emerging network technologies: silicon photonics interconnects and the Data Vortex network. CENATE's evaluation also addresses the question of which machine is best for a given workload under certain constraints. We show a performance-power tradeoff analysis of a well-known machine learning application on two systems.

  7. Identification and quantification of 14 phthalates and 5 non-phthalate plasticizers in PVC medical devices by GC-MS.

    Science.gov (United States)

    Gimeno, Pascal; Thomas, Sébastien; Bousquet, Claudine; Maggio, Annie-Françoise; Civade, Corinne; Brenier, Charlotte; Bonnet, Pierre-Antoine

    2014-02-15

    A GC/MS method was developed for the identification and quantification of 14 phthalates: 8 phthalates classified H360 (DBP, DEHP, BBP, DMEP, DnPP, DiPP, DPP and DiBP), 3 phthalates proposed to be forbidden in medical devices (DnOP, DiNP and DiDP) and 3 other phthalates none regulated (DMP, DCHP and DEP) which may interfere with hormone function. In order to identify and quantify other plasticizers that are commonly used in PVC medical devices such as DEHP substitute, 5 non-phthalate plasticizers (ATBC, DEHA, DEHT, TOTM, and DINCH) were included in this study. Analyses are carried out on a GC/MS system with electron impact ionization mode (EI). The separation of plasticizers is obtained on a cross-linked 5%-phenyl/95%-dimethylpolysiloxane capillary column 30m×0.25mm (i.d.)×0.25μm film thickness using a gradient temperature. Compounds quantification is performed by external calibration using an internal standard. Validation elements on standard solutions were determined using the ISO 12787 standard approach. Plasticizers are extracted from PVC medical devices using THF for dissolving the PVC part of the sample followed by precipitation of the PVC by addition of ethanol. The supernatant is injected into a GC/MS system after dilution in ethanol. Different validation elements, including extraction recoveries for all compounds or for DEHP a cross-validation of the extraction process using the European pharmacopoeia monograph 3.1.14 as reference method, are discussed. Results obtained on 61 medical devices in PVC and 12 raw materials used as plasticizers are given. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Analysis of tomato matrix effect in pesticide residue quantification through QuEChERS and single quadrupole GC/MS

    Directory of Open Access Journals (Sweden)

    Ana M Domínguez

    2014-04-01

    Full Text Available The detection of pesticide in tomato (Solanum lycopersicum L. matrix using Gas Chromatography hyphenated to Mass Spectrometry detector (GC/MS can affect the sensitivity of the analysis by enhancement or suppression of their chromatography response, the percentages of recoveries and leading to errors in the quantification of the pesticides. In this study, the matrix effect was investigated using nine pesticides, and "Quick, Easy, Cheap, Effective, Rugged and Safe" (QuEChERS-GC/MS analytical technique was validated for pesticides multiresidue analysis. The matrix effect was determined using not statistical and statistical procedures including ANOVA, with similar results. Strong negative matrix effect was found for the pesticides trifluralin, 4,4'-DDT, and permethrin, resulting in the increment of the chromatogram background and a decrease in their detection responses. Contrary, an enhancement induced by the matrix presence was obtained for carbaryl and azinphos methyl, showing a positive medium matrix effect. While, dimethoate, simazine, 4,4'-DDE, and iprodione did not exhibit matrix effect. The detection limits (LOD obtained, varied from 0.003 to 0.1 mg kg-1. Reproducibility was less than 20% for each pesticide. Recoveries were found to be between 71% and 121%, except for dimethoate, carbaryl, and azinphos methyl which reached values lower than 70%. Recoveries relative standard deviations were less than 22%. QuEChERS-GC/MS technique was used for evaluation of fresh commercial tomatoes samples, detecting carbaryl in all of them, but in concentration levels lower than the maximum residue limits according to regulations of Codex.

  9. Determining plasma morphine levels using GC-MS after solid phase extraction to monitor drug levels in the postoperative period

    Directory of Open Access Journals (Sweden)

    Veronica Santos

    2008-01-01

    Full Text Available OBJECTIVE: To implement a selective and sensitive analytical method to quantify morphine in small volumes of plasma by gas-liquid chromatography-mass spectrometry (GC-MS, aimed at post-operatively monitoring the drug. METHOD: A gas-liquid chromatographic method with mass detection has been developed to determine morphine concentration in plasma after solid phase extraction. Morphine-d3 was used as an internal standard. Only 0.5 mL of plasma is required for the drug solid-phase extraction in the Bond Elut-Certify®, followed by the quantification of morphine derivative by GC-MS using a linear temperature program, a capillary fused silica column, and helium as the carrier and make-up gas. The method was applied to determine morphine content in plasma samples of four patients during the postoperative period of cardiac surgery. Patient-controlled analgesia with morphine was performed by a venous catheter, and a series of venous blood samples were collected. After the oro-After the orotracheal extubation, morphine plasma levels were monitored for up to 36 hours. RESULTS: The run time was 16 minutes because morphine and the internal standard were eluted after 8.8 minutes. The GC-MS method had 0.5 -1000 ng/mL linearity range (r²=0.9995, 0.1 ng/mL limit of detection, intraday and interday precision equivalent to 1.9% and 6.8%, and 0.1% and 0.8% systematic error (intraday and interday, respectively. The analytical method showed optimal absolute (98% and relative (100.7% recoveries. Morphine dose requirements and plasma levels are discussed. CONCLUSION: The analytical gas-liquid chromatography-mass spectrometry method is selective and adequate for morphine measurements in plasma for applications in clinical studies.

  10. Pyrolysis-GC/MS of charred purified condensed tannin: towards identification of tannin-derived black carbon in environmental samples

    Science.gov (United States)

    Kaal, Joeri; Nierop, Klaas G. J.; Kraal, Peter; Preston, Caroline M.

    2010-05-01

    Tannins account for a significant proportion of plant biomass and are therefore a possible source of Black C in the charred remains from wildfires. Nonetheless, in contrast with other major biocomponents such as lignin and cellulose, the thermal degradation of tannins has not been investigated in laboratory charring experiments. We used pyrolysis-GC/MS to investigate the effects of furnace charring (30 min at fixed temperatures up to 600 °C under limited oxygen supply) on the degradation of pure condensed tannin (CT) isolated from Corsican pine (Pinus nigra) needles. The experiments showed a rapid loss (at 300 °C and higher) of the pyrogallol moieties of the B-ring of prodelphinidin-type CT, due to dehydroxylation. The relative abundance of catechols (from procyanidin-type CT) decreased at 350 °C and higher temperatures. This led to the formation of phenols that were strongly enriched between 300 and 400 °C. At higher temperatures, further dehydroxylation caused a decline in contributions of phenols producing a series of monocyclic aromatics ((alkyl)benzenes) and condensation of aromatics produced polycyclic aromatic hydrocarbons (PAHs), i.e. the typical pyrolysis fingerprint of strongly charred biomass. We conclude that (i) the thermal degradation of CT can be successfully monitored by pyrolysis-GC/MS, (ii) thermal degradation of CT is characterized by dehydroxylation of phenolic groups and condensation of aromatics that increase with temperature and (iii) CT-derived Black C may be recognized by catechol enrichments at low temperatures and possibly (relative) abundance of phenol and biphenyl at higher levels of thermal breakdown. Applying the same method to natural charcoal from gorse bushfires indicated that pyrolysis-GC/MS fingerprinting may allow for tannin identification in environmental Black C samples.

  11. ISOLASI DAN AKTIVITAS LARVACIDA MINYAK ATSIRI AKAR (Curcuma mangga, Val. TERHADAP LARVA Aedes Aegypti DAN PROFIL GC-MS NYA

    Directory of Open Access Journals (Sweden)

    Lolita Lolita

    2012-11-01

    Full Text Available Curcuma mangga, Val. has been recognized as a traditional drug since a long time ago. The active ingrediences of this plant especially the volatile oil contains monoterpenes and sesquiterpenes. This research was aimed to study about the larvacide’s activity of the volatile oil Curcuma mangga, Val. rhizome and also to analyze its chemical compounds using the GC-MS. The volatile oil was isolated from Curcuma mangga, Val. with steam and water distillation. The test method for larvicide was done by dissolving the substances into water and added by Tween 20 10% v/v to the the volatile oil. The concentration of the volatile oil of Curcuma mangga, Val. rhizome were 100 ppm, 150 ppm, 200 ppm, 250 ppm, 300 ppm, and 350 ppm. The concentration of positive control “abate” were 0,01 ppm; 0,025 ppm; 0,05 ppm; 0,1 ppm; 0,5 ppm while as the negative control was Tween 20 solution. The perception time of larvae’s mortality was 24 hours. The chemical compound of Curcuma mangga, Val. can be analysed by the GC-MS. Data of larvae’s mortality were used to estimate the values of LC50 with the probit analyzis method. This study showed that the volatile oil of Curcuma mangga, Val. have clear-brass colour, bitter taste, typically aromatic like mango, rendement equal to (1,23 ± 0,029% v/b and refractive index 1,4881. The value of LC50 for the volatile oil of Curcuma mangga, Val. rhizome is (216,17 ±12,51 ppm while abate equal to (0,072 ± 0,024 ppm. This finding indicates that abate were more potent to larvae of Aedes aegypti. The GC-MS showes 30 peaks chromatogram and six peaks which indicates the possibility of alpha-pinene, camphene, beta-pinene, beta-myrcene, eukalyptole, ar-turmerone presence.

  12. Determining plasma morphine levels using GC-MS after solid phase extraction to monitor drug levels in the postoperative period.

    Science.gov (United States)

    Santos, Veronica; López, Karin Jannet Vera; Santos, Luciana Moraes; Yonamine, Mauricio; Carmona, Maria José Carvalho; Santos, Silvia Regina Cavani Jorge

    2008-06-01

    To implement a selective and sensitive analytical method to quantify morphine in small volumes of plasma by gas-liquid chromatography-mass spectrometry (GC-MS), aimed at post-operatively monitoring the drug. A gas-liquid chromatographic method with mass detection has been developed to determine morphine concentration in plasma after solid phase extraction. Morphine-d3 was used as an internal standard. Only 0.5 mL of plasma is required for the drug solid-phase extraction in the Bond Elut-Certify, followed by the quantification of morphine derivative by GC-MS using a linear temperature program, a capillary fused silica column, and helium as the carrier and make-up gas. The method was applied to determine morphine content in plasma samples of four patients during the postoperative period of cardiac surgery. Patient-controlled analgesia with morphine was performed by a venous catheter, and a series of venous blood samples were collected. After the oro-After the orotracheal extubation, morphine plasma levels were monitored for up to 36 hours. The run time was 16 minutes because morphine and the internal standard were eluted after 8.8 minutes. The GC-MS method had 0.5 -1000 ng/mL linearity range (r(2)=0.9995), 0.1 ng/mL limit of detection, intraday and interday precision equivalent to 1.9% and 6.8%, and 0.1% and 0.8% systematic error (intraday and interday, respectively). The analytical method showed optimal absolute (98%) and relative (100.7%) recoveries. Morphine dose requirements and plasma levels are discussed. The analytical gas-liquid chromatography-mass spectrometry method is selective and adequate for morphine measurements in plasma for applications in clinical studies.

  13. Relating Pyrolysis GC-MS to Traditional Soil Organic Matter Characterization: a Comparative Study Across a Landscape.

    Science.gov (United States)

    Kelleher, J. A.; Carrasco, J. J.; Neff, J. C.

    2004-12-01

    Ecosystem scale soil organic matter studies commonly involve measurements such as physical or chemical separations to bulk soil elemental estimates, however, these measurements provide limited information about SOM structure and how it varies across landscapes. To bridge the gap between molecular-scale and pool-based understanding of SOM dynamics, we compared soil density fractionation and chemical digestion techniques to more detailed pyrolysis GC-MS measurements. Composite soil samples from 0-10 cm were collected from four sites with observably different soil characteristics along the Front Range in Colorado: aspen grove, spruce-fir forest, and alpine dry and wet meadows. Samples were separated into heavy, light, and water fractions (slow, intermediate, and fast SOM turnover pools, respectively) using a 1.8 g/mL density fractionation. Non-polar extractives, polar extractives, cellulose, and lignin abundances were determined using a standard method for organic matter digestion. Significant differences were absent between sites for all density derived components as well as the non-polar and polar extractives. The spruce-fir SOM, however, showed higher % lignin and lower % cellulose compared to all other sites. We measured lignin, polysaccharide, and long-chain aliphatic derivatives using pyrolysis GC-MS and then compared relative abundances using principal component analysis. Spruce-fir SOM was distinguished by the high relative abundance of lignin derivatives that parallels observed higher % lignin by digestion. The dry and wet meadow SOM was distinguished by the relative abundance of long-chain aliphatic compounds. While the density and chemical fractionations were unable to fully distinguish these soils apart, pyrolysis GC-MS provided more detailed information about the chemical composition of SOM across different ecosystems.

  14. GC-MS analysis, Antibacterial, Antioxidant and Anticancer activity of essential oil of Pinus roxburghii from Kashmir, India

    Directory of Open Access Journals (Sweden)

    Wajaht A. Shah

    2014-05-01

    Full Text Available This work was carried out to evaluate chemical composition, antibacterial, antioxidant and anticancer activity of Pinus roxburghii essential oil. The oil was extracted by hydro-distillation which was analysed through GC-MS. The antibacterial activity was evaluated by agar well diffusion method and antioxidant activity was evaluated through DPPH assay while as anticancer activity was evaluated through MTT method. Alpha-pinene and beta-pinene were the major constituents present in the oil. This oil showed significant antibacterial and anticancer activity. 

  15. Relationships between algal coals and resistant cell wall biopolymers of extant algae as revealed by Py-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Derenne, S.; Largeau, C.; Casadevall, E.; Tegelaar, E.; De Leeuw, J.W.

    1988-12-01

    The resistant biopolymers (PRB A, PRB B and PRB L), isolated from the walls of three different races of the extant alga Botryococcus braunii and two algal coals (Torbanite, Kukersite) were examined using Py-GC and Py-GC-MS. These pyrolytic methods appear as particularly efficient tools in comparative studies of such materials. The structure of PRB L was thus shown to be different from those of PRB A, PRB B and Torbanite while the spectroscopic features (FT IR, solid state /sup 13/C NMR) of all these products are similar. It also appeared that Kukersite does not consist of selectively preserved PRB L. 34 refs., 2 figs., 1 tab.

  16. Investigation of Hopanoid Biomarkers in Lake Sediments by GC-MS and RP-HPLC-APCI-MS

    Directory of Open Access Journals (Sweden)

    Gamze Kavran Belin

    2009-01-01

    Full Text Available Hopanoids are mainly derived from bacteriohopanpolyols that occur especially in bacteria, show the importance of bacterial lipid contributions in geological materials. In this work, GC-MS and RP-HPLC-APCI-MS analyses of hopanoid biomarkers in oxic and anoxic sediment samples from Lake Cadagno (Swiss Alps and Lake Voua de la Motte (Haute Savoie, France are presented and discussed. Samples were ultrasonically extracted, fractionated by flush chromatography on silica gel and derivatised before the analyses. Periodic acid/ sodium borohydride cleavage was used to identify highly functionalised hopanoids

  17. Shenzhen Institute of Advanced Technology

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    @@ The CAS Shenzhen Institute of Advanced Technology (SIAT) is jointly founded by CAS and the government of Shenzhen, China's first special economic region. It is the first R&D entity in China specializing in modernized manufacturing and independent innovation with integrated technologies as its disciplinary orientation.

  18. 血清中16种有机磷农药GC/MS/MS检测方法的研究%Determination of 16 kinds of organophosphorus pesticides in serum by using GC/MS/MS

    Institute of Scientific and Technical Information of China (English)

    周志荣; 付慧; 罗添; 林少彬

    2012-01-01

    Objective To establish a method of determining the presence and concentration of 16 kinds of organophosphorus pesticides in serum by GC/MS/MS. Method The parent ions of each pesticide was detected by running GC/MS in a full scan mode, and the peak areas and the ratio of signal to noise of each product ion were compared by setting different CID voltages. The CID voltage for each parent ion was optimized and determined. Serum samples were solid-phase extracted by Oasis HLB and eluted with ethyl ether after being concentrated and made to constant volume with ethyl ether, and then were tested by GC/MS/MS. Results The correlation coefficient for each compound in the range of 0 - 1000ng/ml was greater than 0. 990. Recoveries of standard addition were 75% - 129% ,RSD < 10% . The intra-day and inter-day RSD was less than 15% (n =6). The limits of quantification were less than 2ng/ml except for dichlorovos (55ng/ml). Conclusion GC/MS/MS assay is sensitive and accurate for the determination of pesticides in serum.%目的 应用GC/MS/MS建立测定血清中敌敌畏、氧化乐果等16种有机磷农药的分析方法.方法 首先做GC/MS全扫描分析,确定16种化合物的母离子,然后比较不同碰撞诱导裂解(CID)电压时二级质谱中特征离子的峰面积大小以及信噪比,对CID电压进行优化,从而确定各化合物的色谱质谱条件.样品用Oasis HLB小柱进行固相萃取后,用乙酸乙酯洗脱,浓缩后再用乙酸乙酯定容后上机测定.结果 在0~1000ng/ml范围内,16种化合物的线性相关系数均大于0.995,加标回收率在75%~129%之间,RSD <10%;日内和日间相对标准偏差小于15%(n=6).除敌敌畏的检测限为55ng/ml外,其余待测物均检出限均小于2ng/ml.结论 该方法灵敏度高、准确性好,适合于血清中有机磷农药的分析测定.

  19. Advanced composites technology

    Energy Technology Data Exchange (ETDEWEB)

    DeTeresa, S J; Groves, S E; Sanchez, R J

    1998-10-01

    The development of fiber composite components in next-generation munitions, such as sabots for kinetic energy penetrators and lightweight cases for advanced artillery projectiles, relies on design trade-off studies using validated computer code simulations. We are developing capabilities to determine the failure of advanced fiber composites under multiaxial stresses to critically evaluate three-dimensional failure models and develop new ones if necessary. The effects of superimposed hydrostatic pressure on failure of composites are being investigated using a high-pressure testing system that incorporates several unique features. Several improvements were made to the system this year, and we report on the first tests of both isotropic and fiber composite materials. The preliminary results indicate that pressure has little effect on longitudinal compression strength of unidirectional composites, but issues with obtaining reliable failures in these materials still remain to be resolved. The transverse compression strength was found to be significantly enhanced by pressure, and the trends observed for this property and the longitudinal strength are in agreement with recent models for failure of fiber composites.

  20. PyMS: a Python toolkit for processing of gas chromatography-mass spectrometry (GC-MS data. Application and comparative study of selected tools

    Directory of Open Access Journals (Sweden)

    O'Callaghan Sean

    2012-05-01

    Full Text Available Abstract Background Gas chromatography–mass spectrometry (GC-MS is a technique frequently used in targeted and non-targeted measurements of metabolites. Most existing software tools for processing of raw instrument GC-MS data tightly integrate data processing methods with graphical user interface facilitating interactive data processing. While interactive processing remains critically important in GC-MS applications, high-throughput studies increasingly dictate the need for command line tools, suitable for scripting of high-throughput, customized processing pipelines. Results PyMS comprises a library of functions for processing of instrument GC-MS data developed in Python. PyMS currently provides a complete set of GC-MS processing functions, including reading of standard data formats (ANDI- MS/NetCDF and JCAMP-DX, noise smoothing, baseline correction, peak detection, peak deconvolution, peak integration, and peak alignment by dynamic programming. A novel common ion single quantitation algorithm allows automated, accurate quantitation of GC-MS electron impact (EI fragmentation spectra when a large number of experiments are being analyzed. PyMS implements parallel processing for by-row and by-column data processing tasks based on Message Passing Interface (MPI, allowing processing to scale on multiple CPUs in distributed computing environments. A set of specifically designed experiments was performed in-house and used to comparatively evaluate the performance of PyMS and three widely used software packages for GC-MS data processing (AMDIS, AnalyzerPro, and XCMS. Conclusions PyMS is a novel software package for the processing of raw GC-MS data, particularly suitable for scripting of customized processing pipelines and for data processing in batch mode. PyMS provides limited graphical capabilities and can be used both for routine data processing and interactive/exploratory data analysis. In real-life GC-MS data processing scenarios PyMS performs

  1. Odor-active compounds in cooked rice cultivars from Camargue (France) analyzed by GC-O and GC-MS.

    Science.gov (United States)

    Maraval, Isabelle; Mestres, Christian; Pernin, Karine; Ribeyre, Fabienne; Boulanger, Renaud; Guichard, Elisabeth; Gunata, Ziya

    2008-07-09

    Volatile compounds of cooked rice from scented (Aychade, Fidji) and nonscented (Ruille) cultivars grown in the Camargue area in France were compared to that of a marketed Asian scented one (Thai) by gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). GC-O analyses of the organic extracts resulted in the perception of 40 odorous compounds. Only two compounds, oct-1-en-3-one and 2-acetyl-1-pyrroline, were almost always perceived. Hierarchical cluster analysis showed that most of the difference between rice odors was linked to quantitative differences with only 11 compounds being specific to some of the rice. Sixty compounds were identified and quantified by GC-MS, including a few new odor-active components. Principal component analysis enabled us to differentiate scented cultivars from a nonscented one, and scented rice cultivars from Camargue from a Thai sample. Calculated odor-active values evidenced that the Thai sample odor differed from that of scented Camargue cultivars because of the degradation of lipids and of cinnamic acid compounds.

  2. GC-MS Based Plasma Metabolomics for Identification of Candidate Biomarkers for Hepatocellular Carcinoma in Egyptian Cohort.

    Directory of Open Access Journals (Sweden)

    Mohammad R Nezami Ranjbar

    Full Text Available This study evaluates changes in metabolite levels in hepatocellular carcinoma (HCC cases vs. patients with liver cirrhosis by analysis of human blood plasma using gas chromatography coupled with mass spectrometry (GC-MS. Untargeted metabolomic analysis of plasma samples from participants recruited in Egypt was performed using two GC-MS platforms: a GC coupled to single quadruple mass spectrometer (GC-qMS and a GC coupled to a time-of-flight mass spectrometer (GC-TOFMS. Analytes that showed statistically significant changes in ion intensities were selected using ANOVA models. These analytes and other candidates selected from related studies were further evaluated by targeted analysis in plasma samples from the same participants as in the untargeted metabolomic analysis. The targeted analysis was performed using the GC-qMS in selected ion monitoring (SIM mode. The method confirmed significant changes in the levels of glutamic acid, citric acid, lactic acid, valine, isoleucine, leucine, alpha tocopherol, cholesterol, and sorbose in HCC cases vs. patients with liver cirrhosis. Specifically, our findings indicate up-regulation of metabolites involved in branched-chain amino acid (BCAA metabolism. Although BCAAs are increasingly used as a treatment for cancer cachexia, others have shown that BCAA supplementation caused significant enhancement of tumor growth via activation of mTOR/AKT pathway, which is consistent with our results that BCAAs are up-regulated in HCC.

  3. Determination of Urinary PAH Metabolites Using DLLME Hyphenated to Injector Port Silylation and GC-MS-MS.

    Science.gov (United States)

    Gupta, Manoj Kumar; Jain, Rajeev; Singh, Pratibha; Ch, Ratnasekhar; Mudiam, Mohana Krishna Reddy

    2015-06-01

    Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous environmental pollutants and well-known carcinogens. Hydroxy derivatives of PAH are considered as biomarkers of PAH exposure, and there is a need to measure these metabolites at low concentrations. So, a precise and eco-friendly analytical method has been developed for rapid determination of PAH metabolites. For the first time, a new analytical method based on coupling of dispersive liquid-liquid microextraction (DLLME) with auto-injector port silylation (auto-IPS) followed by gas chromatography-tandem mass spectrometry (GC-MS-MS) analysis is reported for the analysis of seven urinary PAH metabolites. Factors affecting DLLME and IPS, such as type and volume of extraction and disperser solvent, pH, ionic strength, injector port temperature, volume of N,O-bis(trimethylsilyl)trifluoroacetamide and type of solvent were investigated. Under optimized conditions, the limit of detection and limit of quantification were found to be in the range of 1-9 and 3-29 ng/mL, respectively. Satisfactory recoveries of metabolites in urine samples in the range of 87-95% were found. The developed method has been successfully applied for the determination of PAH metabolites in urine samples of exposed workers. DLLME-auto-IPS-GC-MS-MS method is time, labor, solvent and reagent saving, which can be routinely used for the analysis of urinary PAH metabolites.

  4. Quality changes during storage of cooked and sliced meat products measured with PTR-MS and HS-GC-MS.

    Science.gov (United States)

    Holm, E S; Adamsen, A P S; Feilberg, A; Schäfer, A; Løkke, M M; Petersen, M A

    2013-10-01

    The changes in the VOC composition of industrially produced saveloy were measured with Proton-Transfer-Reaction Mass-Spectrometry (PTR-MS) and HeadSpace Gas chromatography-mass spectrometry (HS-GC-MS) during a six weeks storage period. A decrease in the volatile organic compounds contributing to the fresh aroma of saveloy was the main change observed with both PTR-MS and HS-GC-MS. Samples of four other types of cooked and sliced meat product were measured with PTR-MS in the middle and at the end of the four week shelf-life period. These measurements showed an increase in m/z 69, 71, 87 and 89 for the pork loin and in m/z 61 for the herbal saveloy samples. These ions were assigned to the microbial spoilage markers: acetic acid, 2- and 3-methylbutanol, 2- and 3-methylbutanal, diacetyl and acetoin. Overall, this study shows that PTR-MS has potential for quality control of cooked and sliced meat products. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Dynamic liquid phase nanoextraction coupled to GC/MS for rapid analysis of methoxyacetophenone and anisaldehyde isomers in urine.

    Science.gov (United States)

    Wu, Hui-Fen; Yen, Jyh-Hao

    2008-07-01

    This study introduces a novel extraction technique in the nanoscale and challenges the limits of solvent extraction in the GC/MS using electronic ionization (EI) method for quantitative determination of six methoxyacetophenone (MAP) and anisaldehye (AAH) isomers in one drop of water and urine. This technique is termed as dynamic liquid phase nanoextraction (DLPNE). The optimum parameters for the DLPNE technique were: selection of solvent, toluene; sampling volume, 0.44 microL; dwell time, 2 s; number of sampling, 15; extraction time, 1.5 min; volume of extraction solvent, 60 nL; and no salt addition. The LODs for this technique were 5-20 ng/mL. The RSDs were in the range of 9.7-12.6% (n = 6). The linear dynamic range of the calibration curve of DLPNE is from 0.02 to 0.5 microg/mL with correlation coefficient (r(2)) >0.9705. The advantages of the DLPNE technique are rapidity, ease of operation, simple device, and extremely little solvent and sample consumption. This technique was also compared with the static liquid phase nanoextraction (SLPNE) while the SLPNE failed to detect any signal for the six isomers. We believe that this technique can be very useful for the detection of volatile organic compounds in environmental science from microscale of water or it can be applied to clinical or pharmaceutical application such as diagnosis of microamount of urine or blood samples by GC/MS.

  6. Volatile profile analysis and quality prediction of Longjing tea (Camellia sinensis) by HS-SPME/GC-MS

    Institute of Scientific and Technical Information of China (English)

    Jie LIN; Yi DAI; Ya-nan GUO; Hai-rong XU; Xiao-chang WANG

    2012-01-01

    This study aimed to analyze the volatile chemical profile of Longjing tea,and further develop a prediction model for aroma quality of Longjing tea based on potent odorants.A total of 21 Longjing samples were analyzed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS).Pearson's linear correlation analysis and partial least square (PLS) regression were applied to investigate the relationship between sensory aroma scores and the volatile compounds.Results showed that 60 volatile compounds could be commonly detected in this famous green tea.Terpenes and esters were two major groups characterized,representing 33.89% and 15.53% of the total peak area respectively.Ten compounds were determined to contribute significantly to the perceived aroma quality of Longjing tea,especially linalool (0.701),nonanal (0.738),(Z)-3-hexenyl hexanoate (-0.785),and β-ionone (-0.763).On the basis of these 10 compounds,a model (correlation coefficient of 89.4% and cross-validated correlation coefficient of 80.4%) was constructed to predict the aroma quality of Longjing tea.Summarily,this study has provided a novel option for quality prediction of green tea based on HS-SPME/GC-MS technique.

  7. Analysis of volatile components in herbal pair Semen Persicae-Flos Carthami by GC-MS and chemometric resolution.

    Science.gov (United States)

    Fu, Jiangang; Li, Xiaoru; Lu, Hongmei; Liang, Yizeng

    2012-11-01

    Analysis of volatile components in herbal pair (HP) Semen Persicae-Flos Carthami (SP-FC) was performed by GC-MS coupled with chemometric resolution method (CRM). Furthermore, temperature-programmed retention indices were used together with mass spectra for identification of the volatile components. With the help of CRM, the two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound. By use of these methods upon two-dimensional data, 26, 49, and 59 volatile chemical components in essential oils of single herb Semen Persicae, Flos Carthami, and HP SP-FC were determined qualitatively and quantitatively, accounting for 78.42, 81.08, and 82.48% total contents of essential oil of single herb Semen Persicae, Flos Carthami, and HP SP-FC, respectively. It is shown that the accuracy of qualitative and quantitative analysis can be enhanced greatly by means of CRM. It is further demonstrated that the numbers of volatile chemical components of HP SP-FC are almost the addition of those of two single herbs, but the main volatile chemical components of the former are completely different from those of single herb Semen Persicae or Flos Carthami because of chemical reactions and physical changes occurring in the process of decocting two single herbs. This means that chemical components especially pharmacologically active compounds in the recipe might be different from those of single herbs.

  8. Characterization of Brazilian green propolis throughout the seasons by headspace GC/MS and ESI-MS.

    Science.gov (United States)

    Nunes, Cleiton A; Guerreiro, Mário C

    2012-01-30

    A screening of the chemical composition of eight commercial classes of raw Brazilian green propolis throughout the seasons was carried out. A multivariate exploratory analysis of chemical composition obtained by gas chromatography associated with mass spectrometry with headspace extraction (HS-GC/MS), and by mass spectrometry with electrospray ionization (ESI-MS) was carried out using principal component analysis (PCA). Differences in the volatile and polyphenolic profiles of propolis samples were verified during the seasons. Within each season, the high quality commercial classes of propolis presented similar characteristics, while the low quality classes presented distinct compositions. In spring and summer, propolis of the trimming class, commonly considered of low quality by beekeepers, presented a composition similar to the superior quality propolis. Seasonality influences the chemical composition of the commercial classes of raw Brazilian green propolis. Headspace-GC/MS and ESI-MS assisted by PCA are effective to characterize volatile and non-volatile compounds of the propolis samples, and to correlate it to the seasons. Copyright © 2011 Society of Chemical Industry.

  9. Composition of Sulla (Hedysarum coronarium L. Honey Solvent Extractives Determined by GC/MS: Norisoprenoids and Other Volatile Organic Compounds

    Directory of Open Access Journals (Sweden)

    Dragan Bubalo

    2010-09-01

    Full Text Available Samples of unifloral sulla (Hedysarum coronarum L. honey from Sardinia (Italy were analysed. To investigate the chemical composition of the honey volatiles two solvent systems were used for ultrasonic solvent extraction (USE: 1 a 1:2 (v/v pentane and diethyl ether mixture and 2 dichloromethane. All the extracts were analysed by GC and GC/MS. These procedures have permitted the identification of 56 compounds that include norisoprenoids, benzene derivatives, aliphatic compounds and Maillard reaction products. Norisoprenoids were the major compounds in both extracts, dominated by vomifoliol (5.3-11.2%; 9.6-14.0% followed by minor percentages of other norisoprenoids such as α-isophorone, 4-ketoisophorone, 3-oxo-α-ionol or 3-oxo-α-ionone. Other abundant single compounds in the extracts were 3-hydroxy-4-phenylbutan-2-one (0.8-5.4%; 0.6-5.7% and methyl syringate (3.0-5.7%; 2.2-4.1%. The composition of the volatiles and semi-volatiles in the obtained extracts suggests that sulla honey is quite distinctive relative to the other honeys that have been chemically studied by GC/MS, but no specific markers of the honey botanical origin were found.

  10. [Headspace GC/MS analysis of residual vinyl chloride and vinylidene chloride in polyvinyl chloride and polyvinylidene chloride products].

    Science.gov (United States)

    Ohno, Hiroyuki; Mutsuga, Motoh; Kawamura, Yoko; Suzuki, Masako; Aoyama, Taiki

    2005-02-01

    A headspace GC/MS analysis method for the simultaneous determination of residual vinyl chloride (VC) and vinylidene chloride (VDC) in polyvinyl chloride (PVC) and polyvinylidene chloride (PVDC) products was developed. A test sample was swelled overnight with N,N-dimethylacetamide in a sealed vial. The vial was incubated for 1 hour at 90 degrees C, then the headspace gas was analyzed by GC/MS using a PLOT capillary column. The recoveries from spiked PVC and PVDC samples were 90.0-112.3% for VC and 85.2-108.3% for VDC. The determination limits were 0.01 microg/g for VC and 0.06/microg/g for VDC, respectively. By this method, VC was detected in two PVC water supply pipes at the levels of 0.61 and 0.01 microg/g. On the other hand, VC and VDC were not detected in any of the food container-packages or toys tested.

  11. A fast and reliable method for GHB quantitation in whole blood by GC-MS/MS (TQD) for forensic purposes.

    Science.gov (United States)

    Castro, André L; Tarelho, Sónia; Dias, Mário; Reis, Flávio; Teixeira, Helena M

    2016-02-01

    Gamma-hydroxybutyric acid (GHB) is an endogenous compound with a story of clinical use since the 1960s. However, due to its secondary effects, it has become a controlled substance, entering the illicit market. A fully validated, sensitive and reproducible method for the quantification of GHB by methanolic precipitation and GC-MS/MS (TQD) in whole blood is presented. Using 100μL of whole blood, obtained results included a LOD and LLOQ of 0.1mg/L and a recovery of 86% in a working range between 0.1 and 100mg/L. This method is sensitive and specific to detect the presence of GHB in small amounts of whole blood (both ante-mortem or post-mortem), and is, to the authors' knowledge, the first GC-MS-MS TQD method that uses different precursor ions and product ions for the identification of GHB and GHB-D6 (internal standard). Hence, this method may be especially useful for the study of endogenous values in this biological sample.

  12. Alkaloid metabolite profiles by GC/MS and acetylcholinesterase inhibitory activities with binding-mode predictions of five Amaryllidaceae plants.

    Science.gov (United States)

    Cortes, Natalie; Alvarez, Rafael; Osorio, Edison H; Alzate, Fernando; Berkov, Strahil; Osorio, Edison

    2015-01-01

    Acetylcholinesterase (AChE) enzymatic inhibition is an important target for the management of Alzheimer disease (AD) and AChE inhibitors are the mainstay drugs for its treatment. In order to discover new sources of potent AChE inhibitors, a combined strategy is presented based on AChE-inhibitory activity and chemical profiles by GC/MS, together with in silico studies. The combined strategy was applied on alkaloid extracts of five Amaryllidaceae species that grow in Colombia. Fifty-seven alkaloids were detected using GC/MS, and 21 of them were identified by comparing their mass-spectral fragmentation patterns with standard reference spectra in commercial and private library databases. The alkaloid extracts of Zephyranthes carinata exhibited a high level of inhibitory activity (IC50 = 5.97 ± 0.24 μg/mL). Molecular modeling, which was performed using the structures of some of the alkaloids present in this extract and the three-dimensional crystal structures of AChE derived from Torpedo californica, disclosed their binding configuration in the active site of this AChE. The results suggested that the alkaloids 3-epimacronine and lycoramine might be of interest for AChE inhibition. Although the galanthamine group is known for its potential utility in treating AD, the tazettine-type alkaloids should be evaluated to find more selective compounds of potential benefit for AD.

  13. Analgesic, Anti-Inflammatory, and GC-MS Studies on Castanospermum australe A. Cunn. & C. Fraser ex Hook.

    Directory of Open Access Journals (Sweden)

    Thankarajan Sajeesh

    2014-01-01

    Full Text Available The present study was aimed to evaluate the analgesic and anti-inflammatory properties of Castanospermum australe and to profile phytochemicals by GC-MS. The ethanolic extracts were prepared by successive solvent extraction using Soxhlet apparatus. The analgesic activity was analyzed by hot plate method and acetic acid-induced writhing test whereas anti-inflammatory study was done by carrageenan induced paw oedema model. The acute toxicity study revealed that ethanol extracts of leaf and bark of C. australe were safe even at a higher dose of 2000 mg/kg whereas ethanol extract of seed was toxic at the same dose. In both hot plate method (5.85 s and acetic acid-induced writhing test (57%, the leaf ethanol extract exhibited significant analgesic activity (P<0.001 at a dose of 400 mg/kg. The anti-inflammatory activity of leaf extract was exhibited by the reduction in paw linear diameter by 64.76% at 400 mg/kg in carrageenan induced paw oedema. The GC-MS analysis of the ethanol extract of leaf revealed sixteen major compounds of which 1,7-dimethyl-4,10-dioxa-1,7-diazacyclododecane, (+-N-methylephedrine, and permethylspermine were found to be pharmaceutically and the most important. These findings justify that C. australe can be a valuable natural analgesic and anti-inflammatory source which seemed to provide potential phytotherapeutics against various ailments.

  14. Rapid determination of parabens in personal care products by stable isotope GC-MS/MS with dynamic selected reaction monitoring.

    Science.gov (United States)

    Wang, Perry G; Zhou, Wanlong

    2013-06-01

    In this study, a rapid and sensitive analytical method for the determination of methyl-, ethyl-, propyl-, and butyl esters of para-hydroxy benzoic acid (parabens) in personal care products was developed and fully validated. Test portions were extracted with methanol followed by vortexing, sonication, centrifugation, and filtration without derivatization. The four parabens were quantified by GC-MS/MS in the electron ionization mode. Four corresponding isotopically labeled parabens were selected as internal standards, which were added at the beginning of the sample preparation and used to correct for recovery and matrix effects. Sensitivity, extraction efficiency, and recovery of the respective analytes were evaluated. The coefficients of determination (r(2)) were all greater than 0.995 for the four parabens investigated. The recoveries ranged from 97 to 107% at three spiked levels and a one-time (single) extraction efficiency greater than 97% was obtained. This method has been applied to screen 26 personal care products. This is the first time that a unique GC-MS/MS method with dynamic selected reaction monitoring and confirmation of analytes has been used to determine these parabens in cosmetic personal care products.

  15. Solid phase micro-extraction GC-MS analysis of natural volatile components in melon and rice.

    Science.gov (United States)

    Verhoeven, Harrie A; Jonker, Harry; De Vos, Ric C H; Hall, Robert D

    2012-01-01

    The natural fragrance compounds produced by plants play key roles in the long-term fitness and survival of these plants as well as being of direct/indirect benefit to man. Almost all plant fragrances, either pleasant or unpleasant, comprise many different compounds, from different chemical classes and can indeed be highly complex in composition involving several hundred types of volatile molecule. Analyzing these mixtures and identifying their main (bio)active components is of importance in both fundamental and applied science. Gas Chromatography-Mass Spectrometry (GC-MS) plays a central role here. GC-MS has regularly been used for fragrance analysis and different extraction/adsorption and detection protocols have been designed specifically for plant materials. In this chapter, two methods are presented for two highly contrasting plant organs-a melon fruit and rice grains. Metabolomics analyses of these important food crops are already helping us understand better which components are most important in determining the flavour of these important food crops and how we might go about producing new "designer" crops which are even tastier than the existing ones.

  16. Composition of sulla (Hedysarum coronarium L.) honey solvent extractives determined by GC/MS: norisoprenoids and other volatile organic compounds.

    Science.gov (United States)

    Jerković, Igor; Tuberoso, Carlo I G; Tuberso, Carlo I G; Gugić, Mirko; Bubalo, Dragan

    2010-09-09

    Samples of unifloral sulla (Hedysarum coronarum L.) honey from Sardinia (Italy) were analysed. To investigate the chemical composition of the honey volatiles two solvent systems were used for ultrasonic solvent extraction (USE): 1) a 1:2 (v/v) pentane and diethyl ether mixture and 2) dichloromethane. All the extracts were analysed by GC and GC/MS. These procedures have permitted the identification of 56 compounds that include norisoprenoids, benzene derivatives, aliphatic compounds and Maillard reaction products. Norisoprenoids were the major compounds in both extracts, dominated by vomifoliol (5.3-11.2%; 9.6-14.0%) followed by minor percentages of other norisoprenoids such as α-isophorone, 4-ketoisophorone, 3-oxo-α-ionol or 3-oxo-α-ionone. Other abundant single compounds in the extracts were 3-hydroxy-4-phenylbutan-2-one (0.8-5.4%; 0.6-5.7%) and methyl syringate (3.0-5.7%; 2.2-4.1%). The composition of the volatiles and semi-volatiles in the obtained extracts suggests that sulla honey is quite distinctive relative to the other honeys that have been chemically studied by GC/MS, but no specific markers of the honey botanical origin were found.

  17. Determination of Glyphosate Levels in Breast Milk Samples from Germany by LC-MS/MS and GC-MS/MS.

    Science.gov (United States)

    Steinborn, Angelika; Alder, Lutz; Michalski, Britta; Zomer, Paul; Bendig, Paul; Martinez, Sandra Aleson; Mol, Hans G J; Class, Thomas J; Pinheiro, Nathalie Costa

    2016-02-17

    This study describes the validation and application of two independent analytical methods for the determination of glyphosate in breast milk. They are based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively. For LC-MS/MS, sample preparation involved an ultrafiltration followed by chromatography on an anion exchange column. The analysis by GC-MS/MS involved an extraction step, cleanup on a cation exchange column, and derivatization with heptafluorobutanol and trifluoroacetic acid anhydride. Both methods were newly developed for breast milk and are able to quantify glyphosate residues at concentrations as low as 1 ng/mL. The methods were applied to quantify glyphosate levels in 114 breast milk samples, which had been collected from August to September of 2015 in Germany. The mothers participated at their own request and thus do not form a representative sample. In none of the investigated samples were glyphosate residues above the limit of detection found.

  18. Simultaneous Determination of Furan and Vinyl Acetate in Vapor Phase of Mainstream Cigarette Smoke by GC-MS

    Directory of Open Access Journals (Sweden)

    AIFEI XU

    Full Text Available ABSTRACT A simple and sensitive method for simultaneous determination of furan and vinyl acetate (VA in vapor phase of mainstream cigarette smoke with cold trap and gas chromatography-mass spectrometry (GC-MS was developed. A Cambridge filter pad (CFP was placed in front of the impingers of smoking machine to remove the particle phase from cigarette smoke. Furan and VA in vapor phase of mainstream cigarette smoke were collected in two impingers connected in series by filled with methanol at -78°C. The solutions were added with deuterium-labeled furan-d4 and VA-d6 as internal standards and analyzed by GC-MS. The results showed that the calibration curves for furan and VA were linear (r2 > 0.9995 over the studied concentration range. The intra- and inter-day precision values for furan and VA were <7.07% and <9.62%, respectively. The extraction recoveries of furan and VA were in the range of 94.5-97.7% and 92.3-94.9%, respectively. Moreover, the limits of detection for furan and VA were 0.028 µg mL-1 and 1.3 ng mL-1, respectively. The validated method has been successfully applied to determine the emissions of furan and VA in the vapor phase of mainstream cigarette smoke under International Organization for Standardization (ISO and Canadian Intense (CI smoking regimen.

  19. Identification of volatile components in Chinese Sinkiang fermented camel milk using SAFE, SDE, and HS-SPME-GC/MS.

    Science.gov (United States)

    Ning, Li; Fu-Ping, Zheng; Hai-Tao, Chen; Si-Yuan, Liu; Chen, Gu; Zhen-Yang, Song; Bao-Guo, Sun

    2011-12-01

    The volatile components of Chinese Sinkiang fermented camel milk were isolated by solvent assisted flavour evaporation (SAFE), simultaneous distillation extraction (SDE, dichloromethane and diethyl ether as solvent, respectively) and headspace solid-phase microextraction (HS-SPME, CAR/PDMS, PDMS/DVB and DVB/CAR/PDMS fibre extraction, respectively) and analysed by GC/MS. A total of 133 volatile components were identified under 6 different conditions, including 30 esters, 20 acids, 18 saturated alcohols, 15 unsaturated aliphatic alcohols, 8 saturated ketones, 9 saturated aldehydes, 8 unsaturated aliphatic aldehydes, 6 furans, 5 sulphur-containing compounds, 5 ethers, 5 lactones, 3 other compounds, and 1 unsaturated aliphatic ketone. Three pretreatment methods were compared, assisted by principal component analysis (PCA). The results indicated that the volatile components obtained using different methods varied greatly both in categories and in content, and therefore, a multi-pretreatment method should be adopted together with GC/MS. A total of 71 aroma-active compounds were detected by gas chromatography-olfactometry (GC-O), among which 66 aroma-active compounds were found by SDE (60, dichloromethane as solvent; 24, diethyl ether as solvent), 26 by SAFE.

  20. Identification of volatile compounds in codfish ( Gadus) by a combination of two extraction Methods coupled with GC-MS analysis

    Science.gov (United States)

    Chang, Yufei; Hou, Hu; Li, Bafang

    2016-06-01

    Codfish is a kind of abyssal fish species with a great value in food industry. However, the flavor of codfish, especially the unpleasant odor, has caused serious problems in its processing. To accurately identify the volatile compounds in codfish, a combination of solid phase micro-extraction (SPME) method and simultaneous distillation extraction (SDE) method was used to extract the volatiles. Gas chromatography-mass spectrometry (GC-MS) along with Kovats indices (KI) and authentic standard compounds were used to identify the volatiles. The results showed that a total of 86 volatile compounds were identified in codfish, of them 24 were extracted by SDE, 69 compounds by SPME, and 10 compounds by both SDE and SPME. Seventy volatile compounds were found to have specific odors, of them 7 typical compounds contributed significantly to the flavor of codfish. Alcohols ( i.e., (E)-2-penten-1-ol and 2-octanol), esters ( i.e., ethyl butyrate and methyl geranate), aldehydes ( i.e., 2-dodecenal and pentadecanal) contributed the most to fresh flavor while nitrogen compounds, sulphur compounds, furans, as well as some ketones ( i.e., 2-hydroxy-3-pentanone) brought unpleasant odor, such as fishy and earthy odor. It was indicated that the combination of multiple extraction methods and GC-MS analysis can enhance the accuracy of identification, and provide a reference for the further study on flavor of aquatic products.

  1. Measurement of Hydroxyl-Radical Formation in the Rat Striatum by In Vivo Microdialysis and GC-MS.

    Science.gov (United States)

    Nguyen, V; Bonds, D V; Prokai, L

    2008-10-01

    A GC-MS method was developed for measuring hydroxyl-radical capture products of salicylic acid, a common trapping agent for this reactive oxygen species, in samples obtained by in vivo cerebral microdialysis experiments. The assay employed liquid-liquid extraction followed by derivatization of 2,3- and 2,5-dihydroxybenzoic acid, along with 3,5-dihydroxybenzoic acid added as an internal standard. Due to their simple electron ionization mass spectra featuring [M - 57](+) ions through the loss of tertiary alkyl group from the corresponding molecular ions, tert-butyldimethylsilyl (TBDMS) derivatives afforded straightforward method development based on selected-ion monitoring. In addition, tandem mass spectrometry probing collision-induced dissociation of [M - 57](+) ions obtained from the isomeric tert-butyldimethylsilyl derivatives revealed characteristic differences in the resultant product-ion spectra. Our work has demonstrated the applicability of GC-MS for the assay of microdialysates for 2,3- and 2,5-dihydroxybenzoic acid by confirming that local administration of the excitotoxic glutamate into the rat striatum significantly increased in vivo hydroxyl-radical production in this brain region and that subsequent systemic administration of α-phenyl-tert-butylnitrone reversed glutamate-induced oxidative stress.

  2. Determination of homovanillic acid and vanillylmandelic acid in neuroblastoma screening by stable isotope dilution GC-MS.

    Science.gov (United States)

    Fauler, G; Leis, H J; Huber, E; Schellauf, C; Kerbl, R; Urban, C; Gleispach, H

    1997-05-01

    A method for the quantitative determination of homovanillic acid (HVA) and vanillylmandelic acid (VMA), two metabolites of catecholamines, is presented. The assay is based on gas chromatography/electron impact mass spectrometry. The preparation of 13C-labeled VMA from [13C6]vanillin is described. Together with purchased deuterated HVA the 13C-labeled VMA is used as an internal standard in stable isotope dilution GC/MS. The method involves elution from soaked filter-papers, determination of creatinine content, extraction of HVA and VMA from eluted and urinary samples and derivatization to the di-and tri(trimethylsilyl) derivatives, respectively. The detection limits were found to be 4.0 pg for HVA and 0.8 pg for VMA. The method was applied to the routine determination of urinary HVA and VMA in a range from 5 to 100 ng HVA and VMA per microgram creatinine. The lower limits of pathological concentrations are set at 35 ng micrograms-1 creatinine for HVA and to 20 ng micrograms-1 creatinine for VMA, which are in close correlation with the values from other methods, but with the main advantage of reducing the amount of questionable or elevated results from 6.7% (high-performance liquid chromatography (HPLC) alone) to 0.9% (HPLC and GC/MS).

  3. Application of Gas Chromatography with the Mass Detector (GC-MS Technique for Detection of Beeswax Adulteration with Paraffin

    Directory of Open Access Journals (Sweden)

    Waś Ewa

    2015-06-01

    Full Text Available To detect beeswax adulteration with hydrocarbons of alien origin (e.g. paraffin, gas chromatography with mass detector (GC-MS technique was used. The method has been verified here on beeswax samples with different addition (3, 5, 10, 30, and 50% of paraffin and validated under the conditions of repeatability and within - laboratory reproducibility. The addition of paraffin to beeswax can already be detected on the basis of an analysis of the chromatograms. The intensity of individual alkane peaks increased with the increase of the amount of paraffin added to the beeswax. This increase was the mostly visible for the alkanes with even numbers of carbon atoms in the molecule: C24H50, C26H54, C28H58, C30H62, C32H66, and C34H70. These observations have also been proven by quantitative analysis performed using the internal standard method. Adding paraffin to beeswax resulted in an increase in the total contents of n-alkanes as well as individual alkanes, and in particular, of the even-numbered alkanes. The addition of paraffin to beeswax also resulted in the appearance of alkanes containing over 35 carbon atoms in the molecule, which were not detected in beeswax. The method for determination of beeswax hydrocarbons with the GC-MS technique is characterised by satisfactory repeatability and within-laboratory reproducibility. This method can be used for the detection of beeswax adulteration with hydrocarbons of alien origin (e.g. paraffin.

  4. Advanced Metasearch Engine Technology

    CERN Document Server

    Meng, Weiyi

    2010-01-01

    Among the search tools currently on the Web, search engines are the most well known thanks to the popularity of major search engines such as Google and Yahoo!. While extremely successful, these major search engines do have serious limitations. This book introduces large-scale metasearch engine technology, which has the potential to overcome the limitations of the major search engines. Essentially, a metasearch engine is a search system that supports unified access to multiple existing search engines by passing the queries it receives to its component search engines and aggregating the returned

  5. Advances in water resources technology

    Science.gov (United States)

    The presentation of technological advances in the field of water resources will be the focus of Advances in Water Resources Technology, a conference to be held in Athens, Greece, March 20-23, 1991. Organized by the European Committee for Water Resources Management, in cooperation with the National Technical University of Athens, the conference will feature state-of-the art papers, contributed original research papers, and poster papers. Session subjects will include surface water, groundwater, water resources conservation, water quality and reuse, computer modeling and simulation, real-time control of water resources systems, and institutions and methods for technology.The official language of the conference will be English. Special meetings and discussions will be held for investigating methods of effective technology transfer among European countries. For this purpose, a wide representation of research institutions, universities and companies involved in water resources technology will be attempted.

  6. [Technological advances in neurorehabilitation].

    Science.gov (United States)

    Gutiérrez-Martínez, Josefina; Núñez-Gaona, Marco Antonio; Carrillo-Mora, Paul

    2014-07-01

    Neurological rehabilitation arose as formal method in the 60's, for the therapeutic treatment of patients with stroke or spinal cord injury, which develop severe sequelae that affect their motor and sensory abilities. Although the Central Nervous System has plasticity mechanisms for spontaneous recovery, a high percentage of patients should receive specialized therapies to regain motor function, such as Constraint Induced Movement Therapy or Upright physical Therapy. The neurorehabilitation has undergone drastic changes over the last two decades due to the incorporation of computer and robotic electronic devices, designed to produce positive changes in cortical excitability of the cerebral hemisphere damaged and so to improve neuroplasticity. Among equipment, we can mention those for electrotherapy devices, apparatus for transcranial magnetic stimulation, the robotic lower limb orthoses, robot for upper limb training, systems for functional electrical stimulation, neuroprosthesis and brain computer interfaces. These devices have caused controversy because of its application and benefits reported in the literature. The aim of Neurorehabilitation technologies is to take advantage of the functional neuromuscular structures preserved, and they compensate or re-learn the functions that previously made the damaged areas. The purpose of this article is to mention some clinical applications and benefits that these technologies offer to patients with neuronal injury.

  7. A new aerosol collector for quasi on-line analysis of particulate organic matter: the Aerosol Collection Module (ACM) and first applications with a GC/MS-FID

    Science.gov (United States)

    Hohaus, T.; Trimborn, D.; Kiendler-Scharr, A.; Gensch, I.; Laumer, W.; Kammer, B.; Andres, S.; Boudries, H.; Smith, K. A.; Worsnop, D. R.; Jayne, J. T.

    2010-10-01

    In many environments organic matter significantly contributes to the composition of atmospheric aerosol particles influencing its properties. Detailed chemical characterization of ambient aerosols is critical in order to understand the formation process, composition, and properties of aerosols and facilitates source identification and relative contributions from different types of sources to ambient aerosols in the atmosphere. However, current analytical methods are far from full speciation of organic aerosols and often require sampling times of up to one week. Offline methods are also subjected to artifacts during aerosol collection and storage. In the present work a new technique for quasi on-line compound specific measurements of organic aerosol particles was developed. The Aerosol Collection Module (ACM) focuses particles into a beam which is directed to a cooled sampling surface. The sampling takes place in a high vacuum environment where the gas phase from the sample volume is removed. After collection is completed volatile and semi-volatile compounds are evaporated from the collection surface through heating and transferred to a detector. For laboratory characterization the ACM was interfaced with a Gas Chromatograph Mass Spectrometer, Flame Ionization Detector system (GC/MS-FID), abbreviated as ACM GC-MS. The particle collection efficiency, gas phase transfer efficiency, and linearity of the ACM GC-MS were determined using laboratory generated octadecane aerosols. The ACM GC-MS is linear over the investigated mass range of 10 to 100 ng and a recovery rate of 100% was found for octadecane particles. The ACM GC-MS was applied to investigate secondary organic aerosol (SOA) formed from β-pinene oxidation. Nopinone, myrtanal, myrtenol, 1-hydroxynopinone, 3-oxonopinone, 3,7-dihydroxynopinone, and bicyclo[3,1,1]hept-3-ene-2-one were found as products in the SOA. The ACM GC-MS results are compared to quartz filter samples taken in parallel to the ACM GC-MS

  8. GC-MS Analysis on Aroma Components in Three Basils%3个不同罗勒种叶中香气成分的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    黄碧兰; 张玄兵; 王健

    2013-01-01

    The aroma components of three basils (Ocimum basilicum, Ocimum tashiroi Hayata, Ocimum gratissimum)were analyzed by GC/MS technology. The results showed that there were differences in both aroma kinds and relative contents among the three basils. There were 37 kinds of aroma components in Ocimum basilicum, and the relative content was 91.15%. 21 kinds of aroma components in Ocimum tashiroi Hayata and the relative content was 95.08%. 29 kinds of aroma components in Ocimum gratissimum and the relative content was 89.49%. The major compounds of aroma were alcohol and hydrocarbons, their total relative contents were 84.39%、 78.61% and 77.88% in the three cultivars respectively. The three basils shared one major aroma component, Bicycloheptane, 6, 6-dimethyl-2-methylene-, (1S)of. Eucalyptol, Benzene, 1-methoxy-4-(1-propenyl)-and Cyclofenchene were the proper major aroma components of Ocimum basilicum, Ocimum tashiroi Hayata and Ocimum gratissimum, respectively.%利用 GC/MS 技术分析罗勒(Ocimum basilicum L.)、台湾罗勒(Ocimum tashiroi Hayata)和丁香罗勒(Ocimum gratissimum)成龄叶的香气成分。结果表明:3个罗勒品种的叶片中香气成分的种类和含量存在明显差异:罗勒中检出37种香气物质,占其总挥发性物质的91.15%;台湾罗勒中检出21种香气物质,占95.08%;丁香罗勒中有29种,占89.49%。其中,烃类和醇类2类化合物在3种罗勒叶片中分别占挥发物总量的84.39%、78.61%和77.88%。β-蒎烯是3种罗勒共有的主要香气成分,桉树脑、茴香脑和环葑烯则分别是罗勒、台湾罗勒和丁香罗勒的主要香气成分。

  9. Study on the flavor components in milk using SPME/GC-MS%SPME/GC-MS分析比较热处理乳中的挥发性化合物

    Institute of Scientific and Technical Information of China (English)

    陈伟; 闫宁环; 邬子燕; 李洪亮; 于景华; 母智深

    2013-01-01

    TO analyze the main qualitative of volatile components in UTH and pasteurization milk using SPME-GC-MS method. The results showed that the samples can be enrichmented effectively by SPME technology, 74 kinds of flavor components were detected in UHT milk and 57 kinds of flavor compounds were detected in pasteurization milk by GC -MS separation and detection, but some of the flavor components in these two kinds of milk were different, the characteristic flavor components in UHT milk were mainly ketones, acids and hydrocarbon substances, the characteristic flavor components in pasteurized milk were mainly hydrocarbons, acids and alcohols, which belong to the unique flavor of pasteurized milk.%采用固相微萃取-气相色谱-质谱法(SPME-GC-MS)对UHT灭菌乳和巴氏杀菌乳中的主要挥发性成分进行定性分析.结果表明,采用固相微萃取技术能够有效达到富集样品中风味成分的目的,通过GC-MS分离与检测,UHT牛奶共检出74种风味物质,UHT灭菌乳和巴氏杀菌乳存在57种共同风味成分,但二者在某些风味物质的组成及质量分数方面也存在差异,UHT灭菌乳的特征性风味物质为酮类、酸类及烃类物质,巴氏杀菌乳的特征性风味物质为烃类、酸类和醇类物质.

  10. Advanced Technology for Engineering Education

    Science.gov (United States)

    Noor, Ahmed K. (Compiler); Malone, John B. (Compiler)

    1998-01-01

    This document contains the proceedings of the Workshop on Advanced Technology for Engineering Education, held at the Peninsula Graduate Engineering Center, Hampton, Virginia, February 24-25, 1998. The workshop was jointly sponsored by the University of Virginia's Center for Advanced Computational Technology and NASA. Workshop attendees came from NASA, other government agencies, industry and universities. The objectives of the workshop were to assess the status of advanced technologies for engineering education and to explore the possibility of forming a consortium of interested individuals/universities for curriculum reform and development using advanced technologies. The presentations covered novel delivery systems and several implementations of new technologies for engineering education. Certain materials and products are identified in this publication in order to specify adequately the materials and products that were investigated in the research effort. In no case does such identification imply recommendation or endorsement of products by NASA, nor does it imply that the materials and products are the only ones or the best ones available for this purpose. In many cases equivalent materials and products are available and would probably produce equivalent results.

  11. Energy Storage (II): Developing Advanced Technologies

    Science.gov (United States)

    Robinson, Arthur L

    1974-01-01

    Energy storage, considered by some scientists to be the best technological and economic advancement after advanced nuclear power, still rates only modest funding for research concerning the development of advanced technologies. (PEB)

  12. Chemical Costituents in Volatile Oil from Ganteling Capsule with GC-MS Analysis%感特灵胶囊中挥发油化学成分的 GC-MS 分析

    Institute of Scientific and Technical Information of China (English)

    刘海宇; 林美妤; 张庆贺; 刘传贵; 李平亚

    2012-01-01

    Objective; To enrich the study of chemical composition and provide a theoretical basis for quality control, GC-MS was used to analyze the volatile oil components in Ganteling capsule. Method; The volatile oil components were extracted and isolated with steam distillation method according to ChP (2010). The chemical compositions were separated by GC capillary column chromatography, and the relative contents of constituents were determined by area normalization method, Result; Twenty seven compounds were detected and 24 compounds of them were identified by contrast with the mass standard map. And the compounds that the relative contents were more than 5% were palmitic acid ( 31.82%), falcarinol ( 16.89%), 1-naphthalenepropanol, a-ethenyldecahydro-a, 5, 5, 8a-tetramethyl-2-methylene-, [15, [la (R * ) , 4a/3, 8aa

  13. GC-MS analysis of essential oil from Peristrophe japonica%GC-MS 分析九头狮子草挥发油的化学成分

    Institute of Scientific and Technical Information of China (English)

    2014-01-01

    采用水蒸气蒸馏法提取九头狮子草挥发油,利用 GC-MS 联用技术,结合化学计量方法对其化学成分进行定性和定量分析,用面积归一法测定各组分的相对质量分数.结果表明:九头狮子草中挥发油主要由植酮(19.82%)、丁香油酚甲醚(3.96%)、β-石竹烯(3.75%)、肉豆蔻醚(3.08%)、3-甲基-2-(3,7,11-三甲基十二烷基)呋喃(3.64%)、2-戊基呋喃(2.73%)和氧化石竹烯(2.69%)等51种成分组成,占总量的98.82%.%The essential oils of Peristrophe japonica obtained by hydrodistillation from dried aerial parts of P .japon-ica ,were analyzed by gas chromatography-mass spectrometry(GC-MS).About 51 volatile components,consisting of 2-pentadecanone,6,10,14-trimethyl-(19.82%),eugenol methyl ether(3.96%),β-caryophyllene(3.75%),myristicin (3.08%),3-methyl-2-(3,7,11-trimethyldodecyl)furan(3.64%),furan,2-pentyl (2.73%)and caryophyllene oxide (2.69%),were identified on the basis of their mass spectral characteristics,comprising 98.82% of the total oil.

  14. Characterization and pyrolysis of Chlorella vulgaris and Arthrospira platensis: potential of bio-oil and chemical production by Py-GC/MS analysis.

    Science.gov (United States)

    Almeida, Hanna N; Calixto, Guilherme Q; Chagas, Bruna M E; Melo, Dulce M A; Resende, Fabio M; Melo, Marcus A F; Braga, Renata Martins

    2017-06-01

    Biofuels have been seen as potential sources to meet future energy demand as a renewable and sustainable energy source. Despite the fact that the production technology of first-generation biofuels is consolidated, these biofuels are produced from foods crops such as grains, sugar cane, and vegetable oils competing with food for crop use and agricultural land. In recent years, it was found that microalgae have the potential to provide a viable alternative to fossil fuels as source of biofuels without compromising food supplies or arable land. On this scenario, this paper aims to demonstrate the energetic potential to produce bio-oil and chemicals from microalgae Chlorella vulgaris and Arthrospira platensis. The potential of these biomasses was evaluated in terms of physical-chemical characterization, thermogravimetric analysis, and analytical pyrolysis interfaced with gas chromatograph (Py-GC/MS). The results show that C. vulgaris and A. platensis are biomasses with a high heating value (24.60 and 22.43 MJ/kg) and low ash content, showing a high percentage of volatile matter (72.49 and 79.42%). These characteristics confirm their energetic potential for conversion process through pyrolysis, whereby some important aromatic compounds such as toluene, styrene, and phenol were identified as pyrolysis products, which could turn these microalgae a potential for biofuels and bioproduct production through the pyrolysis.

  15. Advanced Communications Technology Satellite (ACTS)

    Science.gov (United States)

    Gedney, Richard T.; Schertler, Ronald J.

    1989-01-01

    The NASA Advanced Communications Technology Satellite (ACTS) was conceived to help maintain U.S. leadership in the world's communications-satellite market. This experimental satellite is expected to be launched by NASA in 1992 and to furnish the technology necessary for establishing very small aperture terminal digital networks which provide on-demand full-mesh connectivity, and 1.544-MBPS services with only a single hop. Utilizing on-board switching and processing, each individual voice or data circuit can be separately routed to any location in the network. This paper provides an overview of the ACTS and discusses the value of the technology for future communications systems.

  16. Handbook of advanced lighting technology

    CERN Document Server

    Sun, Ching-Cherng; Zissis, Georges; Ma, Ruiqing

    2017-01-01

    The Handbook of Advanced Lighting Technology is a major reference work on the subject of light source science and technology, with particular focus on solid-state light sources – LEDs and OLEDs – and the development of 'smart' or 'intelligent' lighting systems; and the integration of advanced light sources, sensors, and adaptive control architectures to provide tailored illumination which is 'fit to purpose.' The concept of smart lighting goes hand-in-hand with the development of solid-state light sources, which offer levels of control not previously available with conventional lighting systems. This has impact not only at the scale of the individual user, but also at an environmental and wider economic level. These advances have enabled and motivated significant research activity on the human factors of lighting, particularly related to the impact of lighting on healthcare and education, and the Handbook provides detailed reviews of work in these areas. The potential applications for smart lighting span ...

  17. Classification of vegetable oils according to their botanical origin using n-alkane profiles established by GC-MS.

    Science.gov (United States)

    Troya, F; Lerma-García, M J; Herrero-Martínez, J M; Simó-Alfonso, E F

    2015-01-15

    n-Alkane profiles established by gas chromatography-mass spectrometry (GC-MS) were used to classify vegetable oils according to their botanical origin. The n-alkanes present in corn, grapeseed, hazelnut, olive, peanut and sunflower oils were isolated by means of alkaline hydrolysis followed by silica gel column chromatography of the unsaponifiable fractions. The n-alkane fraction was constituted mainly of n-alkanes in the range C8-C35, although only those most abundant (15 n-alkanes, from 21 to 35 carbon No.) were used as original variables to construct linear discriminant analysis (LDA) models. Ratios of the peak areas selected by pairs were used as predictors. All the oils were correctly classified according to their botanical origin, with assignment probabilities higher than 95%, using an LDA model.

  18. Determination of acrylamide in coffee and coffee products by GC-MS using an improved SPE clean-up.

    Science.gov (United States)

    Soares, C; Cunha, S; Fernandes, J

    2006-12-01

    An improved gas chromatography-mass spectrometry (GC-MS) method to determine acrylamide (AA) in coffee and coffee products was developed. The method was based on two main purification steps: the first with ethanol and Carrez solutions in order to precipitate polysaccharides and proteins, respectively; and the second with a layered solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. The method is applicable to a wide range of coffee products. Twenty-six samples of different coffee products were analysed. The levels of AA were in the range 11.4-36.2 microg l-1 for 'espresso coffee' and 200.8-229.4 microg l-1 for coffee blends with cereals. The results indicate that the presence of cereals significantly increased the levels of AA.

  19. Identification of the Bacterial Cellular Lipid Fraction by Using Fast GC × GC-MS and Innovative MS Libraries

    Science.gov (United States)

    Mondello, Luigi; Tranchida, Peter Quinto; Purcaro, Giorgia; Fanali, Chiara; Dugo, Paola; La Camera, Erminia; Bisignano, Carlo

    The bacteria fatty acid (FA) profile has been extensively studied for taxonomic classification purposes, since bacteria, in general, contain particular and rare fatty acids, compared to animal and plant tissues. In the last few years, the concern about pathogenic microorganisms used as bioterrorist agents has increased; therefore, rapid methods for the characterization of bacteria are necessary. In the present research, a half-an-hour procedure, to analyze bacteria, was developed: a 2-min one-step sample preparation step, was followed by a relatively fast comprehensive 2D GC-MS separation (25 min). Furthermore, dedicated mass spectrometry libraries were constructed for bacteria and FA identification. Finally, data-processing was carried out with the support of novel comprehensive 2D GC software.

  20. GC-MS analysis of the chemical constituents of the essential oil from the leaves of yacon (Smallanthus sonchifolia)

    Institute of Scientific and Technical Information of China (English)

    Jingwei LI; Jian LIU; Hai LAN; Mingmin ZHENG; Tingzhao RONG

    2009-01-01

    The essential oil from the leaves of yacon grown in China was isolated by hydrodistillation and distillation-extraction. Chemical constituents of the essen-tial oil were separated and identified by means of gas chromatography/mass spectrometry (GC/MS) for the first time, and the relative content of each constituent was determined by area normalization. Twenty-one chemical constituents were identified, and their amounts accounted for 96.2% of the total composition. The main components of the essential oil were β-phellandrene (26.3%), β-cubebene (17.7%), β-caryophyllene (14.0%) and β-bourbonene (10.2%). Therefore, in the volatile oil from the leaves of yacon, sesquiterpenes are major compounds, accounting for 52.2%.

  1. Determination of 2,8-dichlorodibenzo-p-dioxin in toothpaste and mouthwash consumer products using GC-MS.

    Science.gov (United States)

    Wu, Jianlin; Hu, Chuanqin; Li, Charlie; Cai, Zongwei; Hu, Di

    2015-12-01

    A gas chromatography-mass spectrometry (GC-MS) method was developed for the identification and quantification of 2,8-dichlorodibenzo-p-dioxin (2,8-DCDD) in toothpaste and mouthwash consumer products. Liquid-liquid extraction and solid-phase extraction were used in the sample preparation. The limit of detection was 0.96 ng/g in toothpaste and 0.83 ng/g in mouthwash. The accuracy represented by relative errors was less than 12.5%. The intra-day and inter-day precision, which are represented by the relative standard deviation values, were within 11.2 and 10.6%, respectively. The method was successfully applied to analyze 2,8-DCDD in toothpaste and mouthwash products, as well as that from the photo-degradation of triclosan spiked in both sample matrix.

  2. Simultaneous determination of borneol and its metabolite in rat plasma by GC-MS and its application to pharmacokinetic study

    Institute of Scientific and Technical Information of China (English)

    Xiu-Man Sun; Qiong-Feng Liao; Yu-Ting Zhou; Xue-Jiao Deng; Zhi-Yong Xie

    2014-01-01

    A gas chromatography mass spectrometry (GC-MS) method has been developed and fully validated for the simultaneous determination of natural borneol (NB) and its metabolite, camphor, in rat plasma. Following a single liquid-liquid extraction, the analytes were separated using an HP-5MS capillary column (0.25 mm ? 30 m ? 0.25μm) and analyzed by MS in the selected ion monitoring mode. Selected ion monitor (m/z) of borneol, camphor and internal standard was 95, 95 and 128, respectively. Linearity, accuracy, precision and extraction recovery of the analytes were all satisfactory. The method was successfully applied to pharmacokinetic studies of NB after oral administration to Wistar rats.

  3. COMPARATIVE ACCOUNT ON GC-MS ANALYSIS OF MENTHA ARVENSIS L. CORN MINT FROM THREE DIFFERENT LOCATIONS OF NORTH INDIA

    Directory of Open Access Journals (Sweden)

    SHARMA VIVEK1*, SHARMA NISHA1, SINGH HARBANS 1, SRIVASTAVA K. DEVENDRA1, PATHANIA VIJAYLATA2, SINGH BIKRAM2, GUPTA C. RAGHBIR1

    2009-12-01

    Full Text Available The essential oil analysis of Mentha arvensis L. (Corn Mint has been done for the first time from three locations of NorthIndia. The extraction yields for the essential oils of three locations of M. arvensis were: 0.38% for sample M-1 collectedfrom Fatehpur (415m, 0.31% for sample M-2 from Dhameta (435m and 0.36% for sample MP from Patiala (250m. Theoils were analyzed by GC-MS, the components of oil were identified by comparing their retention indices and mass spectrafragmentation patterns with those stored on the MS-computer library and also from the published literatures. The majorconstituents reported from essential oils of M. arvensis were: L-Menthone, Menthol, Isomenthone, Eucalyptol, Piperitoneoxide, Carvone, dl-Limonene, trans-Dihydrocarvone, Germacrene-D, etc. from all three samples collected from Punjab andHimachal Pradesh of Northern India.

  4. ESI(+-MS and GC-MS Study of the Hydrolysis of N-Azobenzyl Derivatives of Chitosan

    Directory of Open Access Journals (Sweden)

    Fernanda S. Pereira

    2014-10-01

    Full Text Available New N-p-chloro-, N-p-bromo-, and N-p-nitrophenylazobenzylchitosan derivatives, as well as the corresponding azophenyl and azophenyl-p-sulfonic acids, were synthesized by coupling N-benzylvchitosan with aryl diazonium salts. The synthesized molecules were analyzed by UV-Vis, FT-IR, 1H-NMR and 15N-NMR spectroscopy. The capacity of copper chelation by these materials was studied by AAS. Chitosan and the derivatives were subjected to hydrolysis and the products were analyzed by ESI(+-MS and GC-MS, confirming the formation of N-benzyl chitosan. Furthermore, the MS results indicate that a nucleophilic aromatic substitution (SnAr reaction occurs under hydrolysis conditions, yielding chloroaniline from N-p-bromo-, and N-p-nitrophenylazo-benzylchitosan as well as bromoaniline from N-p-chloro-, and N-p-nitrophenylazobenzyl-chitosan.

  5. A GC-MS Based Metabonomics Study of Rheumatoid Arthritis and the Interventional Effects of the Simiaowan in Rats

    Directory of Open Access Journals (Sweden)

    Yuming Wang

    2015-12-01

    Full Text Available Simiaowan (SMW is a famous Chinese prescription widely used in clinical treatment of rheumatoid arthritis (RA. The aim of the present study is to determine novel biomarkers to increase the current understanding of RA mechanisms, as well as the underlying therapeutic mechanism of SMW, in RA-model rats. Plasma extracts from control, RA model, and SMW-treated rats were analyzed by gas chromatography coupled with mass spectrometry (GC-MS. An orthogonal partial least-square discriminant analysis (OPLS-DA model was created to detect metabolites that were expressed in significantly different amounts between the RA model and the control rats and investigate the therapeutic effect of SMW. Metabonomics may prove to be a valuable tool for determining the efficacy of complex traditional prescriptions.

  6. Variation in Fatty Acids Composition Including Trans Fat in Different Brands of Potato Chips by GC-MS

    Directory of Open Access Journals (Sweden)

    Aftab A. Kandhro

    2010-06-01

    Full Text Available Twelve different brands of potato chips were analyzed for their fatty acid compositions with eminence on trans fatty acid (TFA using GC-MS. Results of the present study showed that the dominant fatty acids were saturated fatty acids. Among the saturated fatty acids, palmitic acid (23.91–42.64 % was found in greater amount in all analyzed chips samples. The amount of TFA’s determined was ranged between (4.91–14.13 %. Although there was significant variation in the fatty acid profile of all analyzed chips samples but high amount of palmitic acid and trans fat was commonly observed. The results of present study clearly indicated fat used in the manufacturing of chips was partially hydrogenated and palm oil had major contribution. The high level of trans as well as saturated fat is startling issue for the health of consumers.

  7. PIXE and GC-MS investigation for the determination of the chemical composition of Syrian Cuminum cyminum L.

    Science.gov (United States)

    Rihawy, M S; Bakraji, E H; Odeh, A

    2014-04-01

    The chemical composition and concentration of Syrian cumin (Cuminum cyminum L.) were investigated. The particle-induced X-ray emission (PIXE) analytical technique was used to analyze a wide range of elements from Mg to Sr. The advantages and disadvantages of the PIXE technique in plant material elemental analysis are discussed. A high level of iron was detected in the cumin samples, clarifying the possible contribution of cumin to maintaining the immune system. The contribution of the elements in cumin seeds to the dietary recommended intakes (DRI) of elements was evaluated. Additionally, GC-MS measurements were performed to determine the chemical composition of cumin essential oil. Twenty-one components were identified, and cuminaldehyde, γ-terpinene, o-cymene, limonene and β-pinene were determined to be the major constituents. A correlation between the chemical composition of cumin seeds and their use as a traditional remedy is proposed.

  8. Qualitative analysis of the smoke-stream of different kinds of incense by SPME/GC-MS.

    Science.gov (United States)

    Lombardozzi, Antonietta; Strano, Morela; Cortese, Manuela; Ricciutelli, Massimo; Vittori, Sauro; Maggi, Filippo

    2010-08-01

    Seventeen different kinds of incenses were analyzed for the volatile components emitted during burning using a HS-SPME method coupled with GC-MS, in order to check their conformity to IFRA (International Fragrance Association) guidelines and 67/548/CEE Directive rules. A total of 51 volatiles were identified in the smoke of the incenses. They were represented mainly by aromatic compounds (17) and oxygenated monoterpenes (10), with esters (5) and aldehydes (4) being the most widespread volatiles in the former, and alcohols (4) and esters (4) in the latter. The aromatic ester benzyl benzoate and the oxygenated sesquiterpene patchouli alcohol were the most frequent volatile compounds, occurring in the smokes emitted from 10 and 8 kinds of incenses, respectively.

  9. An automated Pearson's correlation change classification (APC3) approach for GC/MS metabonomic data using total ion chromatograms (TICs).

    Science.gov (United States)

    Prakash, Bhaskaran David; Esuvaranathan, Kesavan; Ho, Paul C; Pasikanti, Kishore Kumar; Chan, Eric Chun Yong; Yap, Chun Wei

    2013-05-21

    A fully automated and computationally efficient Pearson's correlation change classification (APC3) approach is proposed and shown to have overall comparable performance with both an average accuracy and an average AUC of 0.89 ± 0.08 but is 3.9 to 7 times faster, easier to use and have low outlier susceptibility in contrast to other dimensional reduction and classification combinations using only the total ion chromatogram (TIC) intensities of GC/MS data. The use of only the TIC permits the possible application of APC3 to other metabonomic data such as LC/MS TICs or NMR spectra. A RapidMiner implementation is available for download at http://padel.nus.edu.sg/software/padelapc3.

  10. Analysis of essential oils from Scutellaria orientalis ssp. alpina and S. utriculata by GC and GC-MS.

    Science.gov (United States)

    Formisano, Carmen; Rigano, Daniela; Senatore, Felice; Piozzi, Franco; Arnold, Nelly Apostolides

    2011-09-01

    The chemical composition of the essential oils obtained from aerial parts of Scutellaria orientalis L. ssp. alpina (Boiss.) O. Schwarz and S. utriculata Labill. growing wild in Lebanon, were analyzed by GC and GC-MS. In S. orientalis ssp. alpina, strongly characterized by sesquiterpenes (41.2%) and particularly sesquiterpene hydrocarbons (31.7%), hexahydrofarnesylacetone (11.7%) was recognized as the main constituent, together with hexadecanoic acid (7.6%), caryophyllene (7.4%), caryophyllene oxide (6.8%), 4-vinylguaiacol (5.4%) and germacrene D (5.4%). S. utriculata oil was instead constituted above all by monoterpenes (42.2%), particularly oxygen containing monoterpenes (39.9%), and in this oil the main compounds were linalool (20.1%), 4-vinyl guaiacol (15.5%), alpha-terpineol (8.9%), (E)-nerolidol (8.9%) and geraniol (8.2%).

  11. [Determination of five pyrethroid pesticides residues in Anoectochilus roxburghii by cloud point extraction-back extraction and GC-MS].

    Science.gov (United States)

    Liu, Hong-Bo; Zhao, Xiao-Fang; Shi, Gui-Ying; Shao, Qing-Song; Li, Mine-Van

    2014-08-01

    A method for residual determination of 5 pyrethroid pesticides in Anoectochilus roxburghii by cloud point extraction-back extraction-GC-MS was established. PEG 6000 was used as extraction agent and isooctane was used for back-extractant. The con- tent was calculated by external standard method. The linear range was from 15 to 2 000 μg x kg(-1) with the good correlation coefficients (0.955-0.999). The recoveries at spiked concentrations of 50-500 μg x kg(-1) ranged from 85.12% to 101.6%. The limit of detection and quantification of 5 pyrethroid pesticides were in the range of 0.63-3.10 μg x kg(-1) and 2.10-10.31 μg x kg(-1), respectively. The proposed method can be applied to the determination of pyrethroid pesticides residues in A. roxburghii.

  12. Formation of the aroma of a raw goat milk cheese during maturation analysed by SPME-GC-MS.

    Science.gov (United States)

    Delgado, Francisco José; González-Crespo, José; Cava, Ramón; Ramírez, Rosario

    2011-12-01

    The volatile profile of the Spanish goat raw milk cheese of the protected designation of origin (PDO) "Queso Ibores" was studied at four stages of maturation (day 1, 30, 60, and 90) by the method of solid-phase micro-extraction-gas chromatography-mass spectrometry (SPME-GC-MS) to determinate the characteristic volatile compounds of this cheese and to know the changes in the volatile profile of this cheese during maturation. According to the PDO, Ibores cheese aroma varies between sweet and mild and it has a strong taste, slightly tart. A total of 64 compounds were detected: 14 acids, 18 alcohols, 13 esters, 6 ketones and 13 compounds which could not be classified in these groups. Carboxylic acids were the most abundant volatile compounds in the headspace of Ibores cheese. Content of volatile compounds was significantly modified (Pdecalactone. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Comparative determination of methyl mercury in whole blood samples using GC-ICP-MS and GC-MS techniques.

    Science.gov (United States)

    Hippler, J; Hoppe, H W; Mosel, F; Rettenmeier, A W; Hirner, A V

    2009-08-15

    Two methods for the determination of methyl mercury (MeHg) in whole blood samples based on different mass spectrometric detection techniques are compared. The methods were employed in two studies in which the internal exposure of a group of mercury-exposed workers to total mercury and MeHg was investigated. Blood samples of these workers were analysed for MeHg independently from each other in two laboratories using similar extraction procedures but different detection techniques, viz. coupled GC-EI-MS/ICP-MS and GC-MS using D(3)-MeHg as internal standard. MeHg was detected in all blood samples in concentrations ranging from 0.3 to 9.0 microg/L. Though different detection techniques were employed, the results obtained by the two laboratories were in relatively good agreement.

  14. GC-MS evaluation of Cymbopogon citratus (DC) Stapf oil obtained using modified hydrodistillation and microwave extraction methods.

    Science.gov (United States)

    Ajayi, E O; Sadimenko, A P; Afolayan, A J

    2016-10-15

    Bioactive compounds of Cymbopogon citratus essential oil, using different media have been tentatively identified with the aid of gas chromatography-mass spectrometry (GC-MS). Hydrodistillation was complemented using weakly acidic and alkaline media for the oil extraction. Solvent-free microwave extraction (SFME) was also used. Analyses of the oils revealed the presence of 7, 16, 22, and 15 compounds in the water-distilled (WD), microwave-distilled (MD), acid-distilled (AD), and base-distilled (BD), essential oils, respectively. Total yield of the volatile fractions was 0.73%, 0.64%, 0.70%, and 0.45%, respectively. Citral was found to be the major component, the base extraction having the highest content. This was followed by 2-isopropenyl-5-methylhex-4-enal, p-cymene, and 2-thujene. The antimicrobial, antibacterial, and antioxidant activities and assessment of medicinal/nutritional uses of the essential oils are subjects of future studies.

  15. Characterization of Volatile Components from Hüller Bitterer Hop Variety Using In-Tube Extraction GC-MS Analysis

    Directory of Open Access Journals (Sweden)

    Liana Claudia Salanță

    2015-05-01

    Full Text Available The composition of hop oil contributes to the aroma of beer and the essential oil profile of hop samples contains valuable information for brewers. The aim of this study was to characterize the Hüller Bitterer hop variety, during the development of hop cones, by analysis the composition of volatile oil using in-tube extraction gas chromatography–mass spectrometry (ITEX-GC–MS. The obtained results show that the ITEX-GC/MS method is suitable for the determination of volatile compounds from hop samples. A number of 60 compounds were separated and 50 of them were identified. The most important volatile compounds found in Hüller Bitterer hop variety belonging to the monoterpenes and sesquiterpenes classes are represented by: β-myrcene, β-caryophyllene and α-humulene. 

  16. Aroma compound analysis of Eruca sativa (Brassicaceae) SPME headspace leaf samples using GC, GC-MS, and olfactometry.

    Science.gov (United States)

    Jirovetz, Leopold; Smith, David; Buchbauer, Gerhard

    2002-07-31

    The aroma compounds of rocket salad (Eruca sativa) SPME headspace samples of fresh leaves were analyzed using GC, GC-MS, and olfactometry. More than 50 constituents of the Eruca headspace could be identified to be essential volatiles, responsible for the characteristic intense green; herbal; nutty and almond-like; Brassicaceae-like (direction of cabbage, broccoli, and mustard); and horseradish-like aroma of these salad leaves. As aroma impact compounds, especially isothiocyanates, and derivatives of butane, hexane, octane, and nonane were identified. 4-Methylthiobutyl isothiocyanate (14.2%), cis-3-hexen-1-ol (11.0%), cis-3-hexenyl butanoate (10.8%), 5-methylthiopentyl isothiocyanate (9.3%), cis-3-hexenyl 2-methylbutanoate (5.4%), and 5-methylthiopentanenitrile (5.0%) were found in concentrations higher than 5.0% (calculated as % peak area of GC analysis using a nonpolar column).

  17. GC/MS analyses of fractionated extraction of Shenfu coal with CS2, n-hexane, benzene

    Institute of Scientific and Technical Information of China (English)

    WANG Xiao-hua; WEI Xian-yong

    2008-01-01

    Shenfu coal was extracted with CS2,n-hexane,benzene sequentially.The extracts were analyzed with GC/MS.It is presented that group seperation of soluble organic compounds in the coal can be achieved by fractionated extraction using different solvents.Main components in CS2 soluble fraction from Shenfu coal are alkyl-substituted arenes.Aliphatic hydrocarbons are overwhelmingly predominant in n-hexane-soluble fraction.Dito tricyclic aramatic hydrocarbons are identified in benzene-soluble fraction.The molecular structures detection of 2,4,6-trichlorobenzenamine and 3,3',4,4',5,5'-hexachloro-1,1'-biphenyl and 2-chiorocyclohexanol firstly provide information for existence form of chlorine in coal.

  18. GC/MS analyses of fractionated extraction of Shenfu coal with CS2, n-hexane, benzene

    Institute of Scientific and Technical Information of China (English)

    WANG Xiao-hua; WEI Xian-yong

    2008-01-01

    Shenfu coal was extracted with CS2, n-hexane, benzene sequentially. The ex-tracts were analyzed with GC/MS. It is presented that group seperation of soluble organic compounds in the coal can be achieved by fractionated extraction using different solvents. Main components in CS2 soluble fraction from Shenfu coal are alkyl-substituted arenes. Aliphatic hydrocarbons are overwhelmingly predominant in n-hexane-soluble fraction. Di-to tricyclic aramatic hydrocarbons are identified in benzene-soluble fraction. The molecular structures detection of 2, 4, 6-trichlorobenzenamine and 3, 3', 4, 4', 5, 5'-hexachloro-1, 1'-biphenyl and 2-chlorocyclohexanol firstly provide information for existence form of chlorine in coal.

  19. Comparison of Three Methods for Extraction of Volatile Lipid Oxidation Products from Food Matrices for GC-MS Analysis

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Yesiltas, B.; Berner, Lis

    GC based methods are often used for determination of volatile oxidation products such as pentanal and hexanal. Different extraction methods for extracting volatiles before GC analysis can be used, e.g static headspace, dynamic headspace and solid phase microextraction (SPME). Traditionally, dynamic...... headspace extraction has been performed manually. Recently, automated dynamic headspace methods have become available. This presentation will summarize the principles of the different extraction methods. Moreover, results from fish oil, oil-in-water emulsion and milk obtained with SPME, manual dynamic...... headspace or automated dynamic headspace (TDU/DHS) extraction followed by GC-MS analysis will be compared. In all cases, concentrations of volatiles were quantified by calibration curves by addition of selected standards to oil, emulsion or milk. The results show that the linearity of calibration curves...

  20. [Study on rapid analysis method of pesticide contamination in processed foods by GC-MS and GC-FPD].

    Science.gov (United States)

    Kobayashi, Maki; Otsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Kamijo, Kyoko; Iwakoshi, Keiko; Sato, Chizuko; Nagayama, Toshihiro; Takano, Ichiro

    2011-01-01

    A simple and rapid method using GC-MS and GC-FPD for the determination of pesticide contamination in processed food has been developed. Pesticides were extracted from a sample with ethyl acetate in the presence of anhydrous sodium sulfate, then cleaned up with a combination of mini-columns, such as macroporous diatomaceous earth, C18, GCB (graphite carbon black) and PSA. Recovery tests of 57 pesticides (known to be toxic or harmful) from ten kinds of processed foods (butter, cheese, corned beef, dried shrimp, frozen Chinese dumplings, grilled eels, instant noodles, kimchi, retort-packed curry and wine) were performed, and the recovery rates were mostly between 70% and 120%. This method can be used to judge whether or not processed foods are contaminated with pesticides at potentially harmful levels.

  1. Measurements of Volatile Organic Compounds by GC-MS in Rural Alabama during the 2013 SOAS Campaign

    Science.gov (United States)

    Koss, A.; Olson, K. F.; De Gouw, J. A.; Goldstein, A. H.

    2013-12-01

    Volatile organic compounds (VOCs) are a large class of chemicals that are emitted into the atmosphere by both human and natural biological activity. VOCs are comprised of both precursor compounds that drive oxidation chemistry and oxidation products. Extensive measurements of VOCs can help determine the relationships between precursor and secondary compounds, and the relative effects of anthropogenic and biogenic emissions on climate and air quality. The Southeastern US is a region of particular research interest, as it is strongly affected by both anthropogenic and biogenic VOCs. As part of the 2013 Southern Oxidant and Aerosol intensive study (SOAS), an in-situ gas-chromatograph mass spectrometer (GC-MS) was deployed at a forested site in rural Alabama. This site was dominated by biogenic emissions, but was also subject to anthropogenic influence. The GC-MS measured a large number of primary and secondary anthropogenic and biogenic VOCs in the C2 to C11 range, with a time resolution of 30 minutes. Measured compounds of particular interest include isoprene, speciated monoterpenes, methylvinylketone (MVK), methacrolein, C2 to C11 alkanes, lightweight unsaturated hydrocarbons including ethene, propene, and acetylene, C6 to C9 aromatics, C1 to C7 oxygenated VOCS (alcohols, ketones, aldehydes), halogenated VOCs, acetonitrile, and several sulfur-containing compounds. A summary of these measurements will be presented. This summary will include characterization of various anthropogenic and biogenic sources sampled at the site, relationships of the most important VOCs to basic meteorological conditions, and diurnal profiles that illustrate shifts in photochemistry and emissions. These GCMS measurements will provide key information for constraints in models and to aid in the interpretation of data from other instruments.

  2. Decomposition kinetic and mechanism of syndiotactic polystyrene nanocomposites with MWCNTs and nanodiamonds studied by TGA and Py-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Chrissafis, Konstantinos; Pavlidou, Eleni [Solid State Physics Section, Physics Department, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki, Macedonia (Greece); Vouvoudi, Evangelia [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki, Macedonia (Greece); Bikiaris, Dimitrios, E-mail: dbic@chem.auth.gr [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24 Thessaloniki, Macedonia (Greece)

    2014-05-01

    Graphical abstract: - Highlights: • Syndiotactic polystyrene nanocomposites containing MWCNTs and nanodiamonds were prepared for first time. • Addition of nanofillers causes a substantial improvement of sPS thermal stability. • From EGA and Py-GC/MS, it was found that sPS decomposes through a radical process. • The decomposition mechanism of sPS was not affected by the addition of nanoparticles. - Abstract: In the present work, syndiotactic polystyrene (sPS) based nanocomposites containing 3 wt% of multi-walled carbon nanotubes (MWCNTs) and nanodiamonds (NDs) were prepared using the melt-mixing technique. Transmission electron microscopy (TEM) micrographs verified a good dispersion of the nanoparticles in the polymeric matrix, which resulted in a slight improvement of the mechanical properties of the nanocomposites. The addition of MWCNTs promotes the formation of β-type crystals while in sPS and sPS/NDs α-type crystals are mainly formed. From the thermogravimetric analysis experiments a substantial enhancement of sPS thermal stability was found, caused by the addition of nanofillers, especially from NDs. The temperature corresponding to a mass loss of 0.5% was found 295 °C for sPS, 352.4 °C for sPS-MWCNTs and 370.7 °C for sPS-NDs nanocomposites. The analytical method of Py-GC/MS was also used for further characterization of the samples. The main chain fragments collected from sPS pyrolysis were styrene monomers, dimers and trimers, while the three pyrolization temperatures applied (390, 420 and 500 °C) indicated some variations in intensity of decomposition fragments. The decomposition temperature as well as the nanoparticle addition (NDs or MWCNTs) affected the intensity of the recorded fragments but did not induce a change on the decomposition mechanism of sPS.

  3. Profiles of urine samples taken from Ecstasy users at Rave parties: analysis by immunoassays, HPLC, and GC-MS.

    Science.gov (United States)

    Zhao, H; Brenneisen, R; Scholer, A; McNally, A J; ElSohly, M A; Murphy, T P; Salamone, S J

    2001-01-01

    The abuse of the designer amphetamines such as 3,4-methylenedioxymethamphetamine (MDMA, Ecstasy) is increasing throughout the world. They have become popular drugs, especially at all-night techno dance parties (Raves), and their detection is becoming an important issue. Presently, there are no MDMA- or MDA-specific immunoassays on the market, and detection of the designer amphetamines is dependent upon the use of commercially available amphetamine assays. The success of this approach has been difficult to assess because of the general unavailability of significant numbers of samples from known drug users. The objectives of the present study are to characterize the drug content of urine samples from admitted Ecstasy users by chromatographic methods and to assess the ability of the available amphetamine/methamphetamine immunoassays to detect methylenedioxyamphetamines. We found that, when analyzed by high-performance liquid chromatography with diode-array detection (HPLC-DAD), 64% of 70 urine samples (by gas chromatography-mass spectrometry [GC-MS]: 88% of 64 urine samples) obtained from Rave attendees contained MDMA and/or 3,4-methylenedioxyamphetamine (MDA) alone or in combination with amphetamine, methamphetamine, or other designer amphetamines such as 3,4-methylenedioxyethylamphetamine (MDEA). This suggests that the majority of the Ravers are multidrug users. At the manufacturer's suggested cutoffs, the Abbott TDx Amphetamine/Methamphetamine II and the new Roche HS Amphetamine/MDMA assays demonstrated greater detection sensitivity for MDMA than the other amphetamine immunoassays tested (Abuscreen OnLine Hitachi AMPS, Abuscreen OnLine Integra AMPS, Abuscreen OnLine Integra AMPSX, CEDIA AMPS, and EMIT II AMPS). There is 100% agreement between each of the two immunoassays with the reference chromatographic methods, HPLC-DAD and GC-MS, for the detection of methylenedioxyamphetamines.

  4. Identification of polymer types and additives in marine microplastic particles using pyrolysis-GC/MS and scanning electron microscopy.

    Science.gov (United States)

    Fries, Elke; Dekiff, Jens H; Willmeyer, Jana; Nuelle, Marie-Theres; Ebert, Martin; Remy, Dominique

    2013-10-01

    Any assessment of plastic contamination in the marine environment requires knowledge of the polymer type and the additive content of microplastics. Sequential pyrolysis-gas chromatography coupled to mass spectrometry (Pyr-GC/MS) was applied to simultaneously identify polymer types of microplastic particles and associated organic plastic additives (OPAs). In addition, a scanning electron microscope equipped with an energy-dispersive X-ray microanalyser was used to identify the inorganic plastic additives (IPAs) contained in these particles. A total of ten particles, which were optically identified as potentially being plastics, were extracted from two sediment samples collected from Norderney, a North Sea island, by density separation in sodium chloride. The weights of these blue, white and transparent fragments varied between 10 and 350 μg. Polymer types were identified by comparing the resulting pyrograms with those obtained from the pyrolysis of selected standard polymers. The particles consisted of polyethylene (PE), polypropylene, polystyrene, polyamide, chlorinated PE and chlorosulfonated PE. The polymers contained diethylhexyl phthalate, dibutyl phthalate, diethyl phthalate, diisobutyl phthalate, dimethyl phthalate, benzaldehyde and 2,4-di-tert-butylphenol. Sequential Py-GC/MS was found to be an appropriate tool for identifying marine microplastics for polymer types and OPAs. The IPAs identified were titanium dioxide nanoparticles (TiO2-NPs), barium, sulphur and zinc. When polymer-TiO2 composites are degraded in the marine environment, TiO2-NPs are probably released. Thus, marine microplastics may act as a TiO2-NP source, which has not yet been considered.

  5. Development and application of GC-MS method for monitoring of long-term exposure to the pesticide cypermethrin.

    Science.gov (United States)

    Kavvalakis, Matthaios P; Tzatzarakis, Manolis N; Alegakis, Athanasios K; Vynias, Dionysios; Tsakalof, Andreas K; Tsatsakis, Aristidis M

    2014-06-01

    Cypermethrin (CPMN) is a synthetic pyrethroid used as an insecticide in large-scale commercial agricultural applications as well as for domestic purposes. In the present study a gas chromatography-mass spectrometry (GC-MS) based method was developed and validated for the quantitation of CPMN metabolites, 3-phenoxybenzoic acid (3-PBA) and cis- and trans- 3-(2,2-dichlorovinyl)-2,2-dimethyl-1-cyclopropane (cis- and trans- Cl2 CA). The developed method was applied for the monitoring of CPMN metabolites in hair of laboratory animals (rabbits) intentionally exposed per os to CPMN at 40 (low dose) and 80 (high dose) mg/kg weight/day for 16 weeks. The analytical method comprises three main steps: isolation of analytes from hair, analytes derivatization, and subsequent instrumental analysis by GC-MS. The limits of detection ensured by the method are 4.0, 3.9 and 1.0 pg/mg hair for cis-Cl2 CA, trans-Cl2 CA and 3-PBA, respectively. The instrument responce is linear (r(2)  > 0.99) in the investigated concentrations range from 25 to 1000 pg/mg. With and between-run precision as well as accuracy were estimated and found satisfactory. Analytes were efficiently isolated by solid-liquid extraction from hair with recoveries greater than 84.8% for cis-Cl2 CA, 87.2% for trans-Cl2 CA and 96.4% for 3-PBA. Rabbit's hair showed increasing levels for all metabolites (metabolites accumulation in a time and dose dependent manner) over time and in a dose-dependent manner. The developed experimental procedure could be used for biomonitoring of population exposure to CPMN.

  6. Trace Analysis of Mutagenic Heterocyclic Aromatic Amines in Cigarette Smoke Condensate and its Base Fractions via Silylation-GC-MS

    Directory of Open Access Journals (Sweden)

    Liu S

    2014-12-01

    Full Text Available Among the more than 5000 chemicals reported in cigarette smoke condensate (CSC, heterocyclic aromatic amines (HAAs are considered to be a contributor to observed biological activity. HAAs are non-volatile and are reported at ppb levels in CSC. A new method for HAA analysis at the trace level is reported here. N, O-Bis(trimethylsilyl trifluoroacetamide (BSTFA containing 1% trimethylchlorosilane was employed to derivatize amino groups by heating the reagent containing a sample of CSC at 80 °C for 30 min followed by analysis employing gas chromatography-mass spectroscopy (GC-MS in the selected-ion-monitoring (SIM mode. This derivatization method afforded symmetrical peak shapes on a ZB-50 stationary phase and achieved instrumental limits of quantification (LOQ at 10:1 S/N from -1 ng/mL for AαC to120 ng/mL for Glu-P-1. The chemical identity of each derivative was confirmed by comparison of retention time and mass spectra of standards. The latter were characterized by the following ions: M·+ or [M-1]+, [M-15]+, and m/z 73 (i.e., trimethylsilyl. CSC and its base sub-fractions were studied using the GC-MS method. Ten HAAs were screened and five were quantified in cigarette smoke condensate, while 2-5 HAAs were quantified in each of three base sub-fractions. Values obtained with the new procedure agree well with values reported in the literature and with results obtained from a commercial laboratory via a different analytical method. The potential contribution of each HAA to the overall mutagenic activity observed for CSC and its base fractions is discussed. When considered together, HAAs account for only a small portion (-7.8% of the observed mutagenicity of the CSC.

  7. Quantification of pesticides in food crops using QuEChERS approaches and GC-MS/MS.

    Science.gov (United States)

    Cho, Jimi; Lee, Jonghwa; Lim, Chai-Uk; Ahn, Jongsung

    2016-12-01

    The analysis of pesticides in food products requires accurate measurements for which standardised protocols have been developed. This paper reports the validation of QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods applied to three different food samples (brown rice, red pepper and mandarin orange) analysed using gas chromatography-tandem mass spectrometry (GC-MS/MS). The validation of the analytical methods used to measure 113 pesticides, including various insecticides, fungicides and herbicides, was conducted in three food matrices and at three spiking levels by three different laboratories. The set of validated results was interpreted, statistically analysed and visualised using principal component analysis (PCA). Notably, the matrix effects in GC-MS analysis for most of the tested pesticides from different matrices were lowered to practical values (less than 30%) appropriate for routine analysis. This allowed for the quantification of pesticides in the samples using standard and analyte protectants (APs) in the reagent method blank as a screening measure, providing an alternative to matrix-matched calibration. Alternatively, the use of only one standardised calibration (grape matrix) in combination with APs also allowed for the qualitative and semi-quantitative analysis of pesticides in different matrices. The inclusion of APs reduced the differences in the matrix-induced enhancement effects of various samples. The use of an internal standard (IS) to correct the matrix effects was also noted. The normalisation of the analyte peak with triphenyl phosphate (TPP) as an IS resulted in a slight improvement of validation values such as precision and linearity in only one laboratory, but it lowered the value of matrix effects in all three laboratories.

  8. Determining the degradation efficiency and mechanisms of ethyl violet using HPLC-PDA-ESI-MS and GC-MS

    Directory of Open Access Journals (Sweden)

    Chung Wen-Hsin

    2012-06-01

    Full Text Available Abstract Background The discharge of wastewater that contains high concentrations of reactive dyes is a well-known problem associated with dyestuff activities. In recent years, semiconductor photocatalysis has become more and more attractive and important since it has a great potential to contribute to such environmental problems. One of the most important aspects of environmental photocatalysis is in the selection of semiconductor materials like ZnO and TiO2, which are close to being two of the ideal photocatalysts in several respects. For example, they are relatively inexpensive, and they provide photo-generated holes with high oxidizing power due to their wide band gap energy. In this work, nanostructural ZnO film on the Zn foil of the Alkaline-Manganese Dioxide-Zinc Cell was fabricated to degrade EV dye. The major innovation of this paper is to obtain the degradation mechanism of ethyl violet dyes resulting from the HPLC-PDA-ESI-MS analyses. Results The fabrication of ZnO nanostructures on zinc foils with a simple solution-based corrosion strategy and the synthesis, characterization, application, and implication of Zn would be reported in this study. Other objectives of this research are to identify the reaction intermediates and to understand the detailed degradation mechanism of EV dye, as model compound of triphenylmethane dye, with active Zn metal, by HPLC-ESI-MS and GC-MS. Conclusions ZnO nanostructure/Zn-foils had an excellent potential for future applications on the photocatalytic degradation of the organic dye in the environmental remediation. The intermediates of the degradation process were separated and characterized by the HPLC-PDA-ESI-MS and GC-MS, and twenty-six intermediates were characterized in this study. Based on the variation of the amount of intermediates, possible degradation pathways for the decolorization of dyes are also proposed and discussed.

  9. An approach to determination of phenolic compounds in seawater using SPME-GC-MS based on SWCNTs coating

    Science.gov (United States)

    Zhu, Jia; Wang, Ying; Zeng, Lin

    2016-08-01

    Phenolic compounds have become one kind of the important pollutants of the marine environment. Single-walled Carbon nanotubes, as one-dimensional nano materials, have light weight and perfect hexagonal structure of connections, with many unusual mechanical, chemical and electrical properties. In recent years, with the research of carbon nanotubes and other nano materials, the application prospect is also constantly discussed. In this paper, homemade single-walled carbon nanotubes (SWCNTs) coating was used for establishing an analytical approach to the determination of five kinds of phenolic compounds in seawater using SPME-GC-MS. Optimal conditions: After saturation was conducted with NaCl, and pH was adjusted to 2.0 with H2SO4, the extract was immersed in a water bath at 40°C for GC-MS determination through 40-min agitating extraction at 500 rmin-1 and 3-min desorption at 280°C. The liniearities ranged between 0.01-100 μg L-1, and the determination limits ranged between 1.5-10 ng L-1. The relative standard deviation (RSD, n = 5) was less than 6.5%. For the phenolic compounds obtained from the spiked recovery test for actual seawater samples, the rates of recovery were 87.5%-101.7%, and the RSDs were less than 8.8%, which met the requirements of determination. Due to its simplicity, high efficiency and low consumption, this approach is suitable for the analysis of trace amounts of phenolic compounds in marine waters.

  10. Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases

    Directory of Open Access Journals (Sweden)

    Lluveras-Tenorio Anna

    2012-10-01

    Full Text Available Abstract Background Saccharide materials have been used for centuries as binding media, to paint, write and illuminate manuscripts and to apply metallic leaf decorations. Although the technical literature often reports on the use of plant gums as binders, actually several other saccharide materials can be encountered in paint samples, not only as major binders, but also as additives. In the literature, there are a variety of analytical procedures that utilize GC-MS to characterize saccharide materials in paint samples, however the chromatographic profiles are often extremely different and it is impossible to compare them and reliably identify the paint binder. Results This paper presents a comparison between two different analytical procedures based on GC-MS for the analysis of saccharide materials in works-of-art. The research presented here evaluates the influence of the analytical procedure used, and how it impacts the sugar profiles obtained from the analysis of paint samples that contain saccharide materials. The procedures have been developed, optimised and systematically used to characterise plant gums at the Getty Conservation Institute in Los Angeles, USA (GCI and the Department of Chemistry and Industrial Chemistry of the University of Pisa, Italy (DCCI. The main steps of the analytical procedures and their optimisation are discussed. Conclusions The results presented highlight that the two methods give comparable sugar profiles, whether the samples analysed are simple raw materials, pigmented and unpigmented paint replicas, or paint samples collected from hundreds of centuries old polychrome art objects. A common database of sugar profiles of reference materials commonly found in paint samples was thus compiled. The database presents data also from those materials that only contain a minor saccharide fraction. This database highlights how many sources of saccharides can be found in a paint sample, representing an important step

  11. Quantitative analysis of the endogenous GHB level in the hair of the Chinese population using GC/MS/MS.

    Science.gov (United States)

    Shi, Yan; Cui, Xiaopei; Shen, Min; Xiang, Ping

    2016-04-01

    Endogenous production complicates interpretation when gamma-hydroxybutyrate (GHB) is measured in hair for forensic purposes. A method capable of quantifying the endogenous concentration of GHB in human head hair was developed and validated using GC/MS/MS. Hair was digested under alkaline conditions (1 mol/L NaOH, 90 °C 10 min), and GHB-d6 was used as an internal standard. Before derivatization with BSTFA and ethyl acetate, a liquid-liquid extraction with ethyl acetate under acidic conditions was performed. GHB-TMS derivatives were detected using GC/MS/MS in the multiple-reaction monitoring mode. This method exhibited good linearity (y = 0.018x + 0.038, R(2) = 0.9998), and the limit of detection was 0.02 ng/mg. The extraction recoveries were more than 60%, and the inter-day and intra-day relative standard deviations (RSD) were less than 15%. This method has been applied for the analysis of the endogenous GHB in hair samples from 66 drug-free Chinese donors. The mean measured concentration for 0-3 cm hair was 1.93 ± 1.40 ng/mg (n = 66), and extreme values were in the range of 0.28-4.91 ng/mg. The mean male endogenous GHB level was 2.95 ng/mg (0.92-4.91 ng/mg, n = 35), while the mean female level was 0.77 ng/mg (0.28-1.95 ng/mg, n = 31). This method was applied to a forensic case for the determination of GHB in hair samples but it is hard to make a reasonable "cut off" in hair. The solution is to use each subject as his own control.

  12. A post-modification approach to independent compo-nent analysis for resolution of overlapping GC/MS signals:from independent components to chemical components

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Independent component analysis (ICA) has demonstrated its power to extract mass spectra from over-lapping GC/MS signal. However, there is still a problem that mass spectra with negative peaks at some m/z will be obtained in the resolved results when there are overlapping peaks in the mass spectra of a mixture. Based on a detail theoretical analysis of the preconditions for ICA and the non-negative property of GC/MS signals, a post-modification based on chemical knowledge (PMBK) strategy is pro-posed to solve this problem. By both simulated and experimental GC/MS signals, it was proved that the PMBK strategy can improve the resolution effectively.

  13. Identification of ten new designer drugs by GC-MS, UPLC-QTOF-MS, and NMR as part of a police investigation of a Danish internet company

    DEFF Research Database (Denmark)

    Reitzel, Lotte A; Dalsgaard, Petur Weihe; Müller, Irene B;

    2012-01-01

    The ability of forensic laboratories to detect and identify unknown compounds is highly important since new, non-controlled designer drugs are appearing on the market with increasing frequency. In this study, the combined use of gas chromatography-mass spectrometry (GC-MS) and ultra performance...... liquid chromatography-quadrupole time of flight-mass spectrometry (UPLC-QTOF-MS) was used for screening of new unknowns. In one large seizure from a Danish Internet company, ten different drugs were identified. Several of the compounds were seized for the first time in Denmark. The GC-MS and UPLC...

  14. Development of a new porous gold SPME fiber for selective and efficient extraction of dodecanethiol followed by GC-MS analysis.

    Science.gov (United States)

    Hafez, Aly M; Wenclawiak, Bernd W

    2013-02-01

    The efficiency of a porous gold fiber used for solid-phase microextraction (PG-SPME) was investigated for the extraction of dodecanethiol out of ethanolic solution. A commercially available standard SPME (polydimethylsiloxane, carboxen, divinylbenzene-PDMS-Carb-DVB) was used as a reference to compare the extraction efficiency and selectivity of dodecanethiol with the PG-SPME fiber. The porous gold SPME fiber allowed the analysis of self-assembled monolayers on gold by gas chromatography-mass spectrometry (GC-MS). The PG-SPME fiber showed a five times higher peak area for dodecanethiol in GC-MS compared to the standard PDMS-Carb-DVB fiber.

  15. Advanced technologies, systems, and applications

    CERN Document Server

    Avdaković, Samir

    2017-01-01

    This volume spans a wide range of technical disciplines and technologies, including complex systems, biomedical engineering, electrical engineering, energy, telecommunications, mechanical engineering, civil engineering, and computer science. The papers included in this volume were presented at the International Symposium on Innovative and Interdisciplinary Applications of Advanced Technologies (IAT), held in Neum, Bosnia and Herzegovina on June 26 and 27, 2016. This highly interdisciplinary volume is devoted to various aspects and types of systems. Systems thinking is crucial for successfully building and understanding man-made, natural, and social systems. .

  16. Advanced Communications Technology Satellite (ACTS)

    Science.gov (United States)

    Olmstead, Dean A.; Schertler, Ronald J.

    The benefits that will be offered by the NASA-sponsored communication spacecraft ACTS which is scheduled for launch in 1992 are described together with examples of demonstrations on proposed data, video, and voice applications supported by the advanced ACTS technologies. Compared to existing satellite service, the ACTS will provide lower cost, better service, greater convenience, and improved service reliability of telecommunications to customers around the world. In addition, the pioneering ACTS technology will provide many capabilities qualitatively different from those of current satellite systems, such as on-demand assignment, frequency reuse, and the flexible targeting of spot beams directly to the very-small-aperture terminals at customer premises.

  17. Advanced tufted carpet patterning technology

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    After a review of the tufting industry's development, and a brief introduction to available systems for producing patterned tufted carpets, the principle of ICN (Individually Controlled Needle) and the related advanced tufting technology Colortec are presented. Finally, Colortec machine, Axminster weaving machine, and Wilton loom are compared. It is believed that the Cobble Colortec machine is a significant jump forward in the tufted carpets industry as it now allows access to all major carpet markets in a competitive fashion.

  18. Large floating structures technological advances

    CERN Document Server

    Wang, BT

    2015-01-01

    This book surveys key projects that have seen the construction of large floating structures or have attained detailed conceptual designs. This compilation of key floating structures in a single volume captures the innovative features that mark the technological advances made in this field of engineering, and will provide a useful reference for ideas, analysis, design, and construction of these unique and emerging urban projects to offshore and marine engineers, urban planners, architects and students.

  19. GT Advanced Technologies Inc. Bankruptcy

    OpenAIRE

    Souply-Pierard, Fernand

    2014-01-01

    GT Advanced Technologies (GTAT), une société américaine de haute technologie produisant du saphir synthétique (fournisseur d’Apple), a fait faillite ce lundi 6 octobre 2014 et s’est placée sous la protection du chapitre 11 de la loi américaine sur la faillite. Cette faillite était-elle prévisible ?

  20. Protocols for the measurement of the F2-isoprostane, 15(S)-8-iso-prostaglandin F2α, in biological samples by GC-MS or GC-MS/MS coupled with immunoaffinity column chromatography.

    Science.gov (United States)

    Tsikas, Dimitrios; Suchy, Maria-Theresia

    2016-04-15

    Arachidonic acid, the origin of the eicosanoids family, occurs in biological samples as free acid and as ester in lipids. Free arachidonic acid is oxidized to numerous metabolites by means of enzymes including cyclooxygenase (COX). Arachidonic acid esterified to lipids is attacked by reactive oxygen species (ROS) to generate numerous oxidized arachidonic acid derivatives. Generally, it is assumed that ROS-derived arachidonic acid derivatives are distinct from those generated by enzymes such as COX. Therefore, ROS-generated eicosanoids are considered specific biomarkers of oxidative stress. However, there are serious doubts concerning a strict distinction between the enzyme-derived eicosanoids and the ROS-derived iso-eicosanoids. Prominent examples are prostaglandin F2α (PGF2α) and 15(S)-8-iso-prostaglandin F2α (15(S)-8-iso-PGF2α) which have been originally considered to exclusively derive from COX and ROS, respectively. There is convincing evidence that both COX and ROS can oxidize arachidonic acid to PGF2α and 15(S)-8-iso-PGF2α. Thus, many results previously reported for 15(S)-8-iso-PGF2α as exclusive ROS-dependent reaction product, and consequently as a specific biomarker of oxidative stress, require a careful re-examination which should also consider the analytical methods used to measure 15(S)-8-iso-PGF2α. This prominent but certainly not the only example underlines more than ever the importance of the analytical chemistry in basic and clinical research areas of oxidative stress. In the present work, we report analytical protocols for the reliable quantitative determination of 15(S)-8-iso-PGF2α in human biological samples including plasma and urine by mass spectrometry coupled to gas chromatography (GC-MS, GC-MS/MS) after specific isolation of endogenous 15(S)-8-iso-PGF2α and the externally added internal standard [3,3',4,4'-(2)H4]-15(S)-8-iso-PGF2α by immunoaffinity column chromatography (IAC). 15(S)-8-iso-PGF2α esterified to plasma lipids is

  1. Center for Advanced Separation Technology

    Energy Technology Data Exchange (ETDEWEB)

    Honaker, Rick

    2013-09-30

    The U.S. is the largest producer of mining products in the world. In 2011, U.S. mining operations contributed a total of $232 billion to the nation’s GDP plus $138 billion in labor income. Of this the coal mining industry contributed a total of $97.5 billion to GDP plus $53 billion in labor income. Despite these contributions, the industry has not been well supported with research and development funds as compared to mining industries in other countries. To overcome this problem, the Center for Advanced Separation Technologies (CAST) was established to develop technologies that can be used by the U.S. mining industry to create new products, reduce production costs, and meet environmental regulations. Originally set up by Virginia Tech and West Virginia University, CAST is now a five-university consortium – Virginia Tech, West Virginia University, University of Kentucky, University of Utah and Montana Tech, - that is supported through U.S. DOE Cooperative Agreement No. DE-FE0000699, Center for Advanced Separation Technology. Much of the research to be conducted with Cooperative Agreement funds will be longer term, high-risk, basic research and will be carried out in two broad areas: Advanced Pre-Combustion Clean Coal Technologies and Gas-Gas Separations. Distribution of funds is handled via competitive solicitation of research proposals through Site Coordinators at the five member universities. These were reviewed and the selected proposals were forwarded these to the DOE/NETL Project Officer for final review and approval. The successful projects are listed below by category, along with abstracts from their final reports.

  2. Advanced USC technology in Japan

    Energy Technology Data Exchange (ETDEWEB)

    Fukuda, Masafumi [National Institute for Materials Science, Tsukuba, Ibaraki (Japan). High Temperature Materials Center

    2010-07-01

    The 600deg-C class Ultra Super-Critical(USC) steam condition technology was mainly developed through projects led by J-Power in the '80s and 90s'. In 2001, the project was successfully finished with newly developed 9-12% chromium steels. These materials were selected for the major parts of the USC power plants in Japan and almost half of the coal power plants have the USC steam condition today. However, aged plants, which were built in the '70s and early '80s will reach the point where they will need to be rebuilt or refurbished in the near future. The steam temperatures of the older plants are 538 deg-C or 566deg-C. We did a case study, retrofitting these plants with the USC and an advanced USC technology that takes a 700deg-C class steam temperature to increase thermal efficiency and to reduce CO{sub 2} emissions. The study showed that the advanced USC Technology(A-USC) is suitable for the retrofitting of aged plants and can reduce CO{sub 2} emissions by about 15%. The Japanese government launched the ''Cool Earth-Innovative Energy Technology Program'' in 2008 March to promote international cooperation and actively contribute to substantial global greenhouse gas emissions reductions. 21 technologies that will contribute to substantial reductions in CO{sub 2} emissions by efficiency improvement and low carbonization were selected. The A-USC that aims at 46% (net, HHV) thermal efficiency of coal power generation is included in the technologies. We started a large-scale development project of the A-USC technology in 2008 August. 700deg-C class boiler, turbine and valve technologies, which include high temperature material technology, will be developed. Some candidate materials for boilers are being tested. Turbine rotor and casing materials are being developed and tested, as well. Two years from the beginning of the project, we have obtained some useful test results regarding the candidate materials. (orig.)

  3. GC-MS Anzlysis of Ether Extrzct from Fritillaria wabuensis znd Its Antioxidznt Activity%瓦布贝母乙醚提取物 GC-MS 分析及其抗氧化活性评价

    Institute of Scientific and Technical Information of China (English)

    潘峰; 张敏敏; 董品利; 吴卫

    2015-01-01

    Abstrzct:[Objective]The aim of the study was to study the chemical composition of the ether ex-tract from Fritillaria wabuensis and its antioxidant activity.[Method]GC-MS was used to detect the ether extract from the dry and fresh samples of F .wabuensis by soxhlet extraction method (SEM)and ultrasonication extraction (UE),respectively.The relative contents of chemical com-position from F .wabuensis were determinated by area normalization.The antioxidant capacity was evaluated by DPPH and ABTS+ radical scavenging assay.[Results]There was higher extraction efficiency by UE than SEM.69 and 58 kinds of components from the fresh samples by SEM and UE were determined but 73 and 57 kinds of components from dry samples by SEM and UE were determined, respectively. Moreover, the percentages of those components were 62.16%, 53.70%,65.18% and 58.76% in the total number of components as well as 80.01%,68.91%, 68.62% and 74.89% in the total content,respectively.The main components were n-hexadecano-ic acid,linoleic acid ethyl ester,(Z,Z)-9,12-octadecadienoic acid and 1,2-benzenedicarboxylic acid,mono (2-ethylhexyl)ester in all samples.The ether extracts from fresh and dry samples by SEM and UE all showed antioxidant activity (IC50 values were 30.66,29.77,15.99 and 21.11 mg/mL with DPPH;35.72,21.08,23.40 and 15.45 mg/mL with ABTS+ ,respectively).[Con-clusion]The different extract methods and treatments had a relatively little effect on the main components.However,there was obvious difference in the low content ingredients in different samples.Furthermore,the ether extracts from F .wabuensis had certain antioxidant activity.GC-MS is a simple,sensitive and rapid method for determination of the chemical composition.It is helpful for our understanding of F .wabuensis .%【目的】分析瓦布贝母鳞茎乙醚提取物中化学成分及其抗氧化活性。【方法】瓦布贝母鳞茎干、鲜样分别采用索氏提取法和超声提取法以乙醚为

  4. Carbon Isotope Characterization of Organic Intermediaries in Hydrothermal Hydrocarbon Synthesis by Pyrolysis-GC-MS-C-IRMS

    Science.gov (United States)

    Socki, Richard A.; Fu, Qi; Niles, Paul B.

    2010-01-01

    We report results of experiments designed to characterize the carbon isotope composition of intermediate organic compounds produced as a result of mineral surface catalyzed reactions. The impetus for this work stems from recently reported detection of methane in the Martian atmosphere coupled with evidence showing extensive water-rock interaction during Martian history. Abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions may be one possible process responsible for methane generation on Mars, and measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible isotope measurements. Our isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-Combustion-Isotope Ratio Mass Specrometry (Py-GC-MS-C-IRMS). Others have conducted similar pyrolysis-IRMS experiments on low molecular weight organic acids (Dias, et al, Organic Geochemistry, 33 [2002]). Our technique differs in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of the organic compounds. A sample of carboxylic acid (mixture of C1 through C6) was pyrolyzed at 100 XC and passed through the GC-MS-C-IRMS (combusted at 940 XC). In order to test the reliability of our technique we compared the _13C composition of different molecular weight organic acids (from C1 through C6) extracted individually by the traditional sealed-tube cupric oxide combustion (940 XC) method with the _13C produced by our pyrolysis technique. Our data indicate that an average 4.3. +/-0.5. (V

  5. GC/MS analysis of triclosan and its degradation by-products in wastewater and sludge samples from different treatments.

    Science.gov (United States)

    Tohidi, Fatemeh; Cai, Zongwei

    2015-08-01

    A gas chromatography/mass spectrometry (GC/MS)-based method was developed for simultaneous determination of triclosan (TCS) and its degradation products including 2,4-dichlorophenol (2,4-DCP), 2,8-dichlorodibenzo-p-dioxin (2,8-DCDD), and methyl triclosan (MTCS) in wastewater and sludge samples. The method provides satisfactory detection limit, accuracy, precision and recovery especially for samples with complicated matrix such as sewage sludge. Liquid-liquid extraction and accelerated solvent extraction (ASE) methods were applied for the extraction, and column chromatography was employed for the sample cleanup. Analysis was performed by GC/MS in the selected ion monitoring (SIM) mode. The method was successfully applied to wastewater and sludge samples from three different municipal wastewater treatment plants (WWTPs). Satisfactory mean recoveries were obtained as 91(±4)-106(±7)%, 82(±3)-87(±4)%, 86(±6)-87(±8)%, and 88(±4)-105(±3)% in wastewater and 88(±5)-96(±8)%, 84(±2)-87(±3)%, 84(±7)-89(±4)%, and 88(±3)-97(±5)% in sludge samples for TCS, 2,4-DCP, 2,8-DCDD, and MTCS, respectively. TCS degradation products were detected based on the type of the wastewater and sludge treatment. 2,8-DCDD was detected in the plant utilizing UV disinfection at the mean level of 20.3(±4.8) ng/L. 2,4-DCP was identified in chemically enhanced primary treatment (CEPT) applying chlorine disinfection at the mean level of 16.8(±4.5) ng/L). Besides, methyl triclosan (MTCS) was detected in the wastewater collected after biological treatment (10.7 ± 3.3 ng/L) as well as in sludge samples that have undergone aerobic digestion at the mean level of 129.3(±17.2) ng/g dry weight (dw).

  6. Characterization of Essential Oil Composition in Different Basil Species and Pot Cultures by a GC-MS Method

    Directory of Open Access Journals (Sweden)

    Andrea Muráriková

    2017-07-01

    Full Text Available Basil (Ocimum L. species are used as medicinal plants due to their essential oils exhibiting specific biological activity. The present work demonstrated that both the variety and season/conditions of cultivation had a significant effect on (i the produced amount (extraction yield, (ii qualitative, as well as (iii quantitative profile of basil essential oil. Among studied basil varieties, a new variety, ‘Mánes’, was characterized for the first time. Based on our quantitative evaluation of GC-MS profiles, the following chemotypes and average concentrations of a main component were detected in the studied basil varieties: ‘Ohře’, ‘Lettuce Leaf’, ‘Purple Opaal’, ‘Dark Green’ (linalool, 5.99, 2.49, 2.34, 2.01 mg/mL, respectively, and ‘Mammolo Genovese’, ‘Mánes’, ‘Red Rubin’ (eucalyptol, 1.34, 0.96, 0.76 mg/mL, respectively. At the same time, when considering other compounds identified in GC-MS profiles, all the studied varieties, except from ‘Lettuce Leaf’, were methyl eugenol-rich with a strong dependence of the eugenol:methyl eugenol ratio on the seasonal changes (mainly solar irradiation, but also temperature and relative humidity. More complex and/or variable (depending on the season and cultivation chemotypes were observed with ‘Lettuce Leaf’ (plus estragole, 2.27 mg/mL, ‘Dark Green’ (plus eucalyptol, 1.36 mg/mL, ‘Mammolo Genovese’ (plus eugenol, 1.19 mg/mL, ‘Red Rubin’ (plus linalool and eugenol, 0.46 and 0.56 mg/mL, respectively, and ‘Mánes’ (plus linalool and eugenol, 0.58 and 0.40 mg/mL, respectively. When considering superior extraction yield (ca. 17 mL·kg−1, i.e., two to five times higher than other examined varieties and consistent amounts (yields of essential oil when comparing inter-seasonal or inter-year data (RSD and inter-year difference in mean yield values ˂2.5%, this new basil variety is very promising for use in the pharmaceutical, food, and cosmetic industries.

  7. GC-MS detection of chiral markers in cocoa beans of different quality and geographic origin.

    Science.gov (United States)

    Caligiani, Augusta; Cirlini, Martina; Palla, Gerardo; Ravaglia, Roberta; Arlorio, Marco

    2007-05-05

    Fermented cocoa beans (Theobroma cacao L., Sterculiaceae) from different countries of origin (Ecuador, Ghana, Trinidad) and cocoa beans roasted under defined conditions (industrial roasting; 150-220 degrees C for 20 min, dry roasting in conventional oven) were analyzed for their contents of certain chiral hydroxy acids, catechins, and amino acids. Cocoa beans are fermented, dried, and industrially transformed by roasting for the production of chocolate, cocoa powders, and other cocoa-related products. Fermentation and roasting conditions influence the contents of chiral compounds such as hydroxy acids, amino acids, and polyphenols, depending on technological procedures as well as some technical parameters. The aim of this work was to check if the content and nature of the named chiral compounds present both in fermented and roasted cocoa beans could be related to the traditional parameters used to classify the variety of seeds and the degree of fermentation. The extent of racemization of amino acids in fermented cocoa beans was low while it slowly increased during roasting, depending on the temperature applied. L-lactic acid was always higher than the D-form while citric acid was generally the most abundant hydroxy acid detected in beans. A correlation was found between polyphenol content and degree of fermentation, while epimerization of (-)-epicatechin to (+)-catechin was observed during roasting. On the whole, results showed that several chiral compounds could be considered as good quality markers for cocoa seeds and cocoa-related products of different quality and geographic origin.

  8. Precautions for in-injection port thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) as applied to aerosol filter samples

    Science.gov (United States)

    Ho, Steven Sai Hang; Chow, Judith C.; Watson, John G.; Ting Ng, Louisa Pan; Kwok, Yuk; Ho, K. F.; Cao, Junji

    2011-03-01

    In-injection port thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) allows for analysis for >130 non-polar organic compounds on small quartz-fiber filter samples without extraction chemicals. TD-GC/MS has been applied to samples from long-term U.S. networks since it is cost effective and less labor intensive. However, analysis of large numbers of samples results in sensitivity reductions over time. Instrument sensitivity and reproducibility were examined after 100, 200, and 500 sample analyses. Analyses of standards between batches of heavily loaded samples from China and Japan showed signal decreases of 28-78% for major organic classes. In the GC injection port, residues can accumulate on the gold-plated seal resulting in analyte adsorption as well as elevating signal background. Decreases in signal response were 28-43% for n-alkanes, 33-45% for hopanes and steranes, 28-56% for PAHs, and 38-78% for phthalates when the gold-plated seal was not replaced after 500 TD-GC/MS sample analyses. Limits of detection (LODs) also increased by 14-76% for the targeted non-polar organic compounds. Residues trapped in the capillary column head can cause peak broadening and overlap. The GC/MS system, including the injection port and gold seal, the column head (where the eluted sample is pre-concentrated), and the ion source should be cleaned after every batch of 50-100 samples.

  9. Prediction of Klason lignin and lignin thermal degradation products by Py-GC/MS in a collection of Lolium and Festuca grasses

    Energy Technology Data Exchange (ETDEWEB)

    Fahmi, R.; Bridgwater, A.V. [Bio-Energy Research Group, Chemical Engineering and Applied Chemistry, Aston University, Birmingham B4 7ET (United Kingdom); Thain, S.C.; Donnison, I.S.; Morris, P.M. [Institute of Grassland and Environmental Research, Plas Gogerddan, Aberystwyth SY23 3EB (United Kingdom); Yates, N. [Rothamsted Research, Harpenden, Hertfordshire AL5 2JQ (United Kingdom)

    2007-08-15

    A rapid method for the analysis of biomass feedstocks was established to identify the quality of the pyrolysis products likely to impact on bio-oil production. A total of 15 Lolium and Festuca grasses known to exhibit a range of Klason lignin contents were analysed by pyroprobe-GC/MS (Py-GC/MS) to determine the composition of the thermal degradation products of lignin. The identification of key marker compounds which are the derivatives of the three major lignin subunits (G, H, and S) allowed pyroprobe-GC/MS to be statistically correlated to the Klason lignin content of the biomass using the partial least-square method to produce a calibration model. Data from this multivariate modelling procedure was then applied to identify likely 'key marker' ions representative of the lignin subunits from the mass spectral data. The combined total abundance of the identified key markers for the lignin subunits exhibited a linear relationship with the Klason lignin content. In addition the effect of alkali metal concentration on optimum pyrolysis characteristics was also examined. Washing of the grass samples removed approximately 70% of the metals and changed the characteristics of the thermal degradation process and products. Overall the data indicate that both the organic and inorganic specification of the biofuel impacts on the pyrolysis process and that pyroprobe-GC/MS is a suitable analytical technique to asses lignin composition. (author)

  10. A detailed pyrolysis-GC/MS analysis of a black carbon-rich acidic colluvial soil (Atlantic ranker) from NW Spain

    NARCIS (Netherlands)

    Kaal, J.; Martinez-Cortizas, A.; Nierop, K.G.J.; Buurman, P.

    2008-01-01

    Despite the potentially large contribution of black carbon (BC) to the recalcitrant soil organic matter pool, the molecular-level composition of aged BC has hardly been investigated. Pyrolysis-GC/MS, which provides structural information on complex mixtures of organic matter, was applied to the NaOH

  11. A gas chromatography-mass spectrometry (GC-MS) method for the detection and quantitation of monofluoroacetate in plants toxic to livestock

    Science.gov (United States)

    Monofluoroacetate (MFA) is a potent toxin that occurs in over 50 plant species in Africa, Australia, and South America and is responsible for significant livestock deaths in these regions. A gas chromatography–mass spectrometry (GC-MS) method for the analysis of MFA in plants based on the derivatiza...

  12. Use of a Deuterated Internal Standard with Pyrolysis-GC/MS Dimeric Marker Analysis to Quantify Tire Tread Particles in the Environment

    Directory of Open Access Journals (Sweden)

    Julie M. Panko

    2012-11-01

    Full Text Available Pyrolysis(pyr-GC/MS analysis of characteristic thermal decomposition fragments has been previously used for qualitative fingerprinting of organic sources in environmental samples. A quantitative pyr-GC/MS method based on characteristic tire polymer pyrolysis products was developed for tread particle quantification in environmental matrices including soil, sediment, and air. The feasibility of quantitative pyr-GC/MS analysis of tread was confirmed in a method evaluation study using artificial soil spiked with known amounts of cryogenically generated tread. Tread concentration determined by blinded analyses was highly correlated (r2 ³ 0.88 with the known tread spike concentration. Two critical refinements to the initial pyrolysis protocol were identified including use of an internal standard and quantification by the dimeric markers vinylcyclohexene and dipentene, which have good specificity for rubber polymer with no other appreciable environmental sources. A novel use of deuterated internal standards of similar polymeric structure was developed to correct the variable analyte recovery caused by sample size, matrix effects, and ion source variability. The resultant quantitative pyr-GC/MS protocol is reliable and transferable between laboratories.

  13. Use of a Deuterated Internal Standard with Pyrolysis-GC/MS Dimeric Marker Analysis to Quantify Tire Tread Particles in the Environment

    Science.gov (United States)

    Unice, Kenneth M.; Kreider, Marisa L.; Panko, Julie M.

    2012-01-01

    Pyrolysis(pyr)-GC/MS analysis of characteristic thermal decomposition fragments has been previously used for qualitative fingerprinting of organic sources in environmental samples. A quantitative pyr-GC/MS method based on characteristic tire polymer pyrolysis products was developed for tread particle quantification in environmental matrices including soil, sediment, and air. The feasibility of quantitative pyr-GC/MS analysis of tread was confirmed in a method evaluation study using artificial soil spiked with known amounts of cryogenically generated tread. Tread concentration determined by blinded analyses was highly correlated (r2 ≥ 0.88) with the known tread spike concentration. Two critical refinements to the initial pyrolysis protocol were identified including use of an internal standard and quantification by the dimeric markers vinylcyclohexene and dipentene, which have good specificity for rubber polymer with no other appreciable environmental sources. A novel use of deuterated internal standards of similar polymeric structure was developed to correct the variable analyte recovery caused by sample size, matrix effects, and ion source variability. The resultant quantitative pyr-GC/MS protocol is reliable and transferable between laboratories. PMID:23202830

  14. Evaluating pyrolysis-GC/MS and 13C CPMAS NMR in conjunction with a molecular mixing model of the Penido Vello peat deposit, NW Spain

    NARCIS (Netherlands)

    Kaal, J.; Baldock, J.A.; Buurman, P.; Nierop, K.G.J.; Pontevedra-Pombal, X.; Martínez-Cortizas, A.

    2007-01-01

    We performed solid state 13C cross-polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR) spectroscopy and pyrolysis¿gas chromatography/mass spectrometry (Py¿GC/MS) on the Penido Vello peat deposit located in Galicia, NW Spain. Often regarded as complementary techniques, solid st

  15. Dehydration of Methylcyclohexanol Isomers in the Undergraduate Organic Laboratory and Product Analysis by Gas Chromatography-Mass Spectroscopy (GC-MS)

    Science.gov (United States)

    Clennan, Malgorzata M.; Clennan, Edward L.

    2011-01-01

    Dehydrations of "cis"- and "trans"-2-methylcyclohexanol mixtures were carried out with 60% sulfuric acid at 78-80 [degrees]C as a function of time and the products were identified by gas chromatography-mass spectroscopy (GC-MS) analysis. The compounds identified in the reaction mixtures include alkenes, 1-, 3-, and 4-methylcyclohexenes and…

  16. Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

    Science.gov (United States)

    Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

    2012-01-01

    The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

  17. 24-HOUR DIFFUSIVE SAMPLING OF 1,3-BUTADIENE IN AIR ONTO CARBONPAK X SOLID ADSORBENT WITH THEMAL DESORPTION/GC/MS ANALYSIS - FEASIBILITY STUDIES

    Science.gov (United States)

    Diffusive sampling of 1,3-butadiene for 24 hours onto the graphitic adsorbent Carbopack X contained in a stainless steel tube badge (6.3 mm OD, 5 mm ID, and 90 mm in length) with analysis by thermal desorption/GC/MS has been evaluated in controlled tests. A test matrix of 42 tr...

  18. Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

    Science.gov (United States)

    Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

    2012-01-01

    The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

  19. Degradation of biogenetic amines by gamma radiation process and identification by GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Cardozo, Monique; Souza, Stefania P. de; Lima, Keila dos S.C.; Lima, Antonio L. dos S., E-mail: santoslima@ime.eb.br [Departamento de Quimica - IME, Instituto Militar de Engenharia, RJ (Brazil)

    2011-07-01

    Biogenic amines are low molecular weight organic bases with aliphatic (putrescine, cadaverine, spermine, spermidine), aromatic (tyramine, phenylethylamine) or heterocyclic (histamine, tryptamine) structures that can be found in several foods, in which they are mainly produced by microbial decarboxylation of amino acids. The reasons to control amines in food are their potential toxicity and their use like food quality markers. The consumption of food containing large amounts of biogenic amines can result in allergic reactions, characterized by difficulty in breathing, rash, vomiting, and hypertension. Biogenic amines are also known as possible precursors of carcinogens, such as N-nitrosamines. Traditionally, biogenic amine formation in food has been prevented, primarily by limiting microbial growth. However, control measures to reduce their levels once formed need to be also considered. The biogenic amines are frequently found in high concentrations and not reduced by high-temperature treatment, which makes difficult to use conventional methods of food preservation for this purpose. Food irradiation has been used in many countries for inhibition of sprouting, destruction of food borne insects, extension of shelf life or improvement of the technological of food. Irradiation is also known as a good method for inactivating pathogens and reducing microorganisms in food materials. Furthermore, besides the sanitary purpose, irradiation technology in new trials can be applied to induce radiolysis of toxic contaminants in food products reducing their content. This study has the objective to evaluate the effect of different gamma irradiation doses (1, 3 and 5kGy) in methanol solutions of three different biogenic amines: tryptamine, tyramine and b-phenylethylamine. The solutions were prepared using standard biogenic amines purchased from Sigma-Aldrich Brazil and methanol HPLC grade with a concentration of 100 {mu}g/mL. They were irradiated in Centro Tecnologico do Exercito

  20. A new aerosol collector for quasi on-line analysis of particulate organic matter: the Aerosol Collection Module (ACM and first applications with a GC/MS-FID

    Directory of Open Access Journals (Sweden)

    T. Hohaus

    2010-10-01

    Full Text Available In many environments organic matter significantly contributes to the composition of atmospheric aerosol particles influencing its properties. Detailed chemical characterization of ambient aerosols is critical in order to understand the formation process, composition, and properties of aerosols and facilitates source identification and relative contributions from different types of sources to ambient aerosols in the atmosphere. However, current analytical methods are far from full speciation of organic aerosols and often require sampling times of up to one week. Offline methods are also subjected to artifacts during aerosol collection and storage.

    In the present work a new technique for quasi on-line compound specific measurements of organic aerosol particles was developed. The Aerosol Collection Module (ACM focuses particles into a beam which is directed to a cooled sampling surface. The sampling takes place in a high vacuum environment where the gas phase from the sample volume is removed. After collection is completed volatile and semi-volatile compounds are evaporated from the collection surface through heating and transferred to a detector.

    For laboratory characterization the ACM was interfaced with a Gas Chromatograph Mass Spectrometer, Flame Ionization Detector system (GC/MS-FID, abbreviated as ACM GC-MS. The particle collection efficiency, gas phase transfer efficiency, and linearity of the ACM GC-MS were determined using laboratory generated octadecane aerosols. The ACM GC-MS is linear over the investigated mass range of 10 to 100 ng and a recovery rate of 100% was found for octadecane particles.

    The ACM GC-MS was applied to investigate secondary organic aerosol (SOA formed from β-pinene oxidation. Nopinone, myrtanal, myrtenol, 1-hydroxynopinone, 3-oxonopinone, 3,7-dihydroxynopinone, and bicyclo[3,1,1]hept-3-ene-2-one were found as products in the SOA. The ACM GC-MS results are compared to quartz filter

  1. Advanced Artificial Intelligence Technology Testbed

    Science.gov (United States)

    Anken, Craig S.

    1993-01-01

    The Advanced Artificial Intelligence Technology Testbed (AAITT) is a laboratory testbed for the design, analysis, integration, evaluation, and exercising of large-scale, complex, software systems, composed of both knowledge-based and conventional components. The AAITT assists its users in the following ways: configuring various problem-solving application suites; observing and measuring the behavior of these applications and the interactions between their constituent modules; gathering and analyzing statistics about the occurrence of key events; and flexibly and quickly altering the interaction of modules within the applications for further study.

  2. Uncertainty Evaluation of Determination of Chloral in Water with GC/MS%GC/MS测定水中三氯乙醛的不确定度评定

    Institute of Scientific and Technical Information of China (English)

    杭培红; 徐巍

    2012-01-01

    系统介绍了吹扫捕集气相色谱/质谱法测定水中三氯乙醛不确定度评定过程,对吹扫捕集气相色谱/质谱法测定水中三氯乙醛的测定过程进行分析,通过数学模型分析并计算测试过程中的不确定度分量,最后计算出相对合成标准不确定度和相对扩展不确定度。结果表明,吹扫捕集气相色谱/质谱法测定水中三氯乙醛的不确定度主要有四个来源:标准样品浓度及稀释过程,标准曲线及回归偏差,样品取样量,仪器稳定性。%The uncertainty of determining chloral in water was evaluated by purge and trap-gas chromatography-mass spectrometry(purge trap-GC-MS).The determination process of chloral in water was analyzed by purge trap-GC-MS.The uncertainty factors in analyzing process were determined and calculated by mathematic model,and the relative synthesis standard uncertainty and the relative expansion standard uncertainty were calculated out.The four main sources were the uncertainty of standard samples and by dilution process,the uncertainty of linear and regression variance,the uncertainty brought in the sampling process,and the uncertainty resulted from the instrument stability of purge trap-GC-MS.Four main sources of the uncertainty of determining chloral in water by purge trap-GC-MS was determined.The uncertainty evaluation process of determining chloral in water by purge trap-GC-MS was introduced systematically.

  3. Advanced Mirror & Modelling Technology Development

    Science.gov (United States)

    Effinger, Michael; Stahl, H. Philip; Abplanalp, Laura; Maffett, Steven; Egerman, Robert; Eng, Ron; Arnold, William; Mosier, Gary; Blaurock, Carl

    2014-01-01

    The 2020 Decadal technology survey is starting in 2018. Technology on the shelf at that time will help guide selection to future low risk and low cost missions. The Advanced Mirror Technology Development (AMTD) team has identified development priorities based on science goals and engineering requirements for Ultraviolet Optical near-Infrared (UVOIR) missions in order to contribute to the selection process. One key development identified was lightweight mirror fabrication and testing. A monolithic, stacked, deep core mirror was fused and replicated twice to achieve the desired radius of curvature. It was subsequently successfully polished and tested. A recently awarded second phase to the AMTD project will develop larger mirrors to demonstrate the lateral scaling of the deep core mirror technology. Another key development was rapid modeling for the mirror. One model focused on generating optical and structural model results in minutes instead of months. Many variables could be accounted for regarding the core, face plate and back structure details. A portion of a spacecraft model was also developed. The spacecraft model incorporated direct integration to transform optical path difference to Point Spread Function (PSF) and between PSF to modulation transfer function. The second phase to the project will take the results of the rapid mirror modeler and integrate them into the rapid spacecraft modeler.

  4. Validation and application of a GC-MS method for the determination of haloacetic acids in drinking water

    Directory of Open Access Journals (Sweden)

    Chiavelli Lucas U.R.

    2016-01-01

    Full Text Available Usually, water treatment plants employ chlorine or sodium hypochlorite during the disinfection process, ensuring that there are not any pathogenic microorganisms in water. However, chlorine might react with natural organic matter and lead to formation of potentially carcinogenic by-products regarding human health, such as haloacetic acids (HAAs. Several countries regulate the levels of these acids in drinking water. Therefore, their concentrations must be monitored with the greatest accuracy as possible. In order to achieve this goal, a method through gas chromatography coupled with mass spectrometry (GC-MS was validated and applied to the determination of HAAs in samples of water destined to the public water service provision from the city of Maringá, Paraná State, Brazil. Measurements between two periods have close recovery values, indicating that the method has good accuracy during the same day. The limits of detection (LOD and quantification (LOQ were satisfactory, with LOD 0.42 μg L-1 and LOQ 1.40 μg L-1 for dichloro-acetic acid (DCAA analysis. Recovery values obtained for the nine haloace-tics acids (HAA9 corresponded to 69.9-107.3 % for samples. The repeatability performed for two periods presented close relative standard deviation (RSD values, indicating that the method has good accuracy during the same day.

  5. Metabolic profiling of root exudates from two ecotypes of Sedum alfredii treated with Pb based on GC-MS

    Science.gov (United States)

    Luo, Qing; Wang, Shiyu; Sun, Li-Na; Wang, Hui

    2017-01-01

    Phytoremediation is an effective method to remediate Pb-contaminated soils and root exudates play an important role in this process. Based on gas chromatography-mass spectrometry (GC-MS) and metabolomics method, this study focuses on the comparative metabolic profiling analysis of root exudates from the Pb-accumulating and non-accumulating ecotypes of Sedum alfredii treated with 0 and 50 μmol/L Pb. The results obtained show that plant type and Pb stress can significantly change the concentrations and species of root exudates, and fifteen compounds were identified and assumed to be potential biomarkers. Leaching experiments showed that l-alanine, l-proline and oxalic acid have a good effect to activate Pb in soil, glyceric acid and 2-hydroxyacetic acid have a general effect to activate Pb in soil. 4-Methylphenol and 2-methoxyphenol might be able to activate Pb in soil, glycerol and diethyleneglycol might be able to stabilize Pb in soil, but these activation effect and stabilization effect were all not obvious.

  6. Metabolic heterogeneity in polycystic ovary syndrome is determined by obesity: plasma metabolomic approach using GC-MS.

    Science.gov (United States)

    Escobar-Morreale, Héctor F; Samino, Sara; Insenser, María; Vinaixa, María; Luque-Ramírez, Manuel; Lasunción, Miguel A; Correig, Xavier

    2012-06-01

    Abdominal adiposity and obesity influence the association of polycystic ovary syndrome (PCOS) with insulin resistance and diabetes. We aimed to characterize the intermediate metabolism phenotypes associated with PCOS and obesity. We applied a nontargeted GC-MS metabolomic approach to plasma samples from 36 patients with PCOS and 39 control women without androgen excess, matched for age, body mass index, and frequency of obesity. Patients with PCOS were hyperinsulinemic and insulin resistant compared with the controls. The increase in plasma long-chain fatty acids, such as linoleic and oleic acid, and glycerol in the obese patients with PCOS suggests increased lipolysis, possibly secondary to impaired insulin action at adipose tissue. Conversely, nonobese patients with PCOS showed a metabolic profile consisting of suppression of lipolysis and increased glucose utilization (increased lactic acid concentrations) in peripheral tissues, and PCOS patients as a whole showed decreased 2-ketoisocaproic and alanine concentrations, suggesting utilization of branched-chain amino acids for protein synthesis and not for gluconeogenesis. These metabolic processes required effective insulin signaling; therefore, insulin resistance was not universal in all tissues of these women, and different mechanisms possibly contributed to their hyperinsulinemia. PCOS was also associated with decreased α-tocopherol and cholesterol concentrations irrespective of obesity. Substantial metabolic heterogeneity, strongly influenced by obesity, underlies PCOS. The possibility that hyperinsulinemia may occur in the absence of universal insulin resistance in nonobese women with PCOS should be considered when designing diagnostic and therapeutic strategies for the management of this prevalent disorder.

  7. A validated GC-MS method for the determination and quantification of residual solvents in counterfeit tablets and capsules.

    Science.gov (United States)

    Deconinck, E; Canfyn, M; Sacré, P-Y; Baudewyns, S; Courselle, P; De Beer, J O

    2012-11-01

    A fast headspace GC-MS method was developed and validated for the detection and quantification of residual solvents of all three ICH-classes in counterfeit tablets and capsules. The method was validated for 10 solvents, selected based on an initial screening of counterfeit medicinal products. The considered solvents were ethanol, 2-propanol, acetone, ethylacetate, chloroform, carbon tetrachloride, benzene, toluene, dichloromethane and ethylbenzene. The proposed method uses a Phenomenex 624 capillary column (60 m × 0.32 mm; 1.8 μm film thickness) (Phenomenex, Torrance, USA) with an oven temperature program from 60 °C (held for 5 min) to 270 °C at 25 °C/min. 270 °C is held for 10 min. The total run time is 23.4 min. The obtained method was fully validated by applying the "total error" profile. Calibration lines for all components were linear within the studied ranges. The relative bias and the relative standard deviations for all components were smaller than 5%, the β-expectation tolerance limits did not exceed the acceptance limits of ±10% and the relative expanded uncertainties were acceptable for all of the considered components. A method was obtained for the screening and quantification of residual solvents in counterfeit tablets and capsules, which will allow a fast screening of these products for the presence of residual solvents. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Determination of plasticisers and BPA in Sicilian and Calabrian nectar honeys by selected ion monitoring GC/MS.

    Science.gov (United States)

    Lo Turco, Vincenzo; Di Bella, Giuseppa; Potortì, Angela Giorgia; Tropea, Alessia; Casale, Ermina Katia; Fede, Maria Rita; Dugo, Giacomo

    2016-11-01

    Twenty-six plasticisers and bisphenol A (BPA) in 39 Sicilian and Calabrian nectar honeys of different botanical south Italian origin were determined by GC-MS. Di-(2-ethylhexyl)phthalate was the most abundant plasticiser in all samples, reaching up 202.7 ± 153.1 µg kg(-1), followed by di-butylphthalate with a concentration of 40.3 ± 9.3 µg kg(-1), whereas the concentration of the other phthalates varied from not detectable to 68.2 µg kg(-1). Trace levels of adipate, sebacate and BPA were not detected in any samples. Among the different floral origin honeys, di-ethylphthalate levels were above the limit of quantification (LOQ) in orange blossom, wildflower and chestnut honey samples. Among the honeys of different geographical origin, di-methylphthalate, di-butylphthalate and di-(2-ethylhexyl)phthalate concentrations were similar. Calabrian honeys showed levels of di-ethylphthalate always lower than the LOQ, moreover di-(2-methylpropyl)phthalate levels were lower than the Sicilian ones. On the contrary, in Sicilian honeys di-(2-methylpropyl)phthalate levels were higher and di-ethylphthalate was present in 37% of samples.

  9. GC-MS Metabolomics Identifies Metabolite Alterations That Precede Subclinical Mastitis in the Blood of Transition Dairy Cows.

    Science.gov (United States)

    Dervishi, Elda; Zhang, Guanshi; Dunn, Suzanna M; Mandal, Rupasri; Wishart, David S; Ametaj, Burim N

    2017-02-03

    The objectives of this study were to determine alterations in the serum metabolites related to amino acid (AA), carbohydrate, and lipid metabolism in transition dairy cows before diagnosis of subclinical mastitis (SCM), during, and after diagnosis of disease. A subclinical mastitis case was determined as a cow having somatic cell count (SCC) > 200 000/mL of milk for two or more consecutive reports. Blood samples were collected from 100 Holstein dairy cows at five time points at -8 and -4 weeks before parturition, at the week of SCM diagnosis, and +4 and +8 weeks after parturition. Twenty healthy control cows (CON) and six cows that were diagnosed with SCM were selected for serum analysis with GC-MS. At -8 weeks a total of 13 metabolites were significantly altered in SCM cows. In addition, at the week of SCM diagnosis 17 metabolites were altered in these cows. Four weeks after parturition 10 metabolites were altered in SCM cows and at +8 weeks 11 metabolites were found to be different between the two groups. Valine (Val), serine (Ser), tyrosine (Tyr), and phenylalanine (Phe) had very good predictive abilities for SCM and could be used at -8 weeks and -4 weeks before calving. Combination of Val, isoleucine (Ile), Ser, and proline (Pro) can be used as diagnostic biomarkers of SCM during early stages of lactation at +4 to +8 weeks after parturition. In conclusion, SCM is preceded and followed by alteration in AA metabolism.

  10. Formulation of sage essential oil (Salvia officinalis, L.) monoterpenes into chitosan hydrogels and permeation study with GC-MS analysis.

    Science.gov (United States)

    Kodadová, Alexandra; Vitková, Zuzana; Herdová, Petra; Ťažký, Anton; Oremusová, Jarmila; Grančai, Daniel; Mikuš, Peter

    2015-01-01

    This study deals with the formulation of natural drugs into hydrogels. For the first time, compounds from the sage essential oil were formulated into chitosan hydrogels. A sample preparation procedure for hydrophobic volatile analytes present in a hydrophilic water matrix along with an analytical method based on the gas chromatography coupled with the mass spectrometry (GC-MS) was developed and applied for the evaluation of the identity and quantity of essential oil components in the hydrogels and saline samples. The experimental results revealed that the chitosan hydrogels are suitable for the formulation of sage essential oil. The monoterpene release can be effectively controlled by both chitosan and caffeine concentration in the hydrogels. Permeation experiment, based on a hydrogel with the optimized composition [3.5% (w/w) sage essential oil, 2.0% (w/w) caffeine, 2.5% (w/w) chitosan and 0.1% (w/w) Tween-80] in donor compartment, saline solution in acceptor compartment, and semi-permeable cellophane membrane, demonstrated the useful permeation selectivity. Here, (according to lipophilicity) an enhanced permeation of the bicyclic monoterpenes with antiflogistic and antiseptic properties (eucalyptol, camphor and borneol) and, at the same time, suppressed permeation of toxic thujone (not exceeding its permitted applicable concentration) was observed. These properties highlight the pharmaceutical importance of the developed chitosan hydrogel formulating sage essential oil in the dermal applications.

  11. GC-MS quantitative analysis of black market pharmaceutical products containing anabolic androgenic steroids seized by the Brazilian Federal Police.

    Science.gov (United States)

    Neves, Diana Brito da Justa; Caldas, Eloisa Dutra

    2017-06-01

    The use of counterfeit or substandard medicines can have an important health impact, resulting in therapeutic failure, be toxic or even cause death. Anabolic steroids are a frequent target for counterfeiters worldwide, being the second most frequent counterfeited class in Brazil. The aims of this work were to optimize and validate a GC-MS method for the quantitative determination of anabolic steroids in tablet, aqueous suspension and oil solution forms, and to analyze pharmaceutical products sent to Brazilian Federal Police (BFP) for forensic analysis. Sample preparation included extraction with methanol in ultrasonic bath followed by centrifugation. The method was successfully validated and 345 samples of pharmaceutical products were analyzed (328 medicines and 17 dietary supplements). About 42% of the medicines were counterfeits, 28.7% of tablets, 12.0% of suspensions and 65.2% of oil solutions; 11% were considered substandards. Five dietary supplements contained undeclared anabolic steroids, including two containing methandrostenolone at 5.4 and 5.8mg/capsule, equivalent to levels found in medicines. The proposed method is suitable for implementation in routine analysis for identification of counterfeits and substandard products. The analytical results show the need to raise awareness of consumers over the risks from the consumption of anabolic steroids from the clandestine market and for more incisive actions from government agencies aiming at decreasing the availability of these products. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. In vitro anti-oxidative activities and GC-MS analysis of various solvent extracts of Cassia singueana parts.

    Science.gov (United States)

    Ibrahim, Mohammed Auwal; Koorbanally, Neil Anthony; Islam, Md Shahidul

    2013-01-01

    The present study was conducted to investigate the anti-oxidative activities of different solvent extracts of Cassia singueana parts. Our results indicate that all the extracts have reducing power (Fe3+ --> Fe2+) and DPPH radical scavenging abilities. However, the ethyl acetate extract of the stem bark has the highest total reducing power whilst the ethanol extract of the stem bark has more potent free radical scavenging activity than all the other extracts. The ethyl acetate extract of the stem bark exhibited more powerful hydroxyl radical scavenging activity than other extracts whilst the aqueous extract of the leaves displayed more potent nitric oxide inhibition activity than other extracts. The GC-MS analysis of the ethyl acetate extract of the stem bark and the ethanol extract of the root and leaves indicated that several aromatic compounds, including phenolics, fatty acids, amino acids and triterpenoids were present in these extracts. Data from this study suggest that the parts of C. singueana possessed anti-oxidative activities and can be used as a potential alternative medicine for oxidative stress related non-communicable chronic diseases. Further experimental and clinical studies in this regard are warranted.

  13. An Optimized Method of Metabolite Extraction from Formalin-Fixed Paraffin-Embedded Tissue for GC/MS Analysis.

    Science.gov (United States)

    Wojakowska, Anna; Marczak, Łukasz; Jelonek, Karol; Polanski, Krzysztof; Widlak, Piotr; Pietrowska, Monika

    2015-01-01

    Formalin-fixed paraffin-embedded (FFPE) tissue specimens constitute a highly valuable source of clinical material for retrospective molecular studies. However, metabolomic assessment of such archival material remains still in its infancy. Hence, there is an urgent need for efficient methods enabling extraction and profiling of metabolites present in FFPE tissue specimens. Here we demonstrate the methodology for isolation of primary metabolites from archival tissues; either fresh-frozen, formalin-fixed or formalin-fixed and paraffin-embedded specimens of mouse kidney were analysed and compared in this work. We used gas chromatography followed by mass spectrometry (GC/MS approach) to identify about 80 metabolites (including amino acids, saccharides, carboxylic acids, fatty acids) present in such archive material. Importantly, about 75% of identified compounds were detected in all three types of specimens. Moreover, we observed that fixation with formalin itself (and their duration) did not affect markedly the presence of particular metabolites in tissue-extracted material, yet fixation for 24h could be recommended as a practical standard. Paraffin embedding influenced efficiency of extraction, which resulted in reduced quantities of several compounds. Nevertheless, we proved applicability of FFPE specimens for non-targeted GS/MS-based profiling of tissue metabolome, which is of great importance for feasibility of metabolomics studies using retrospective clinical material.

  14. Urinary (1)H-NMR and GC-MS metabolomics predicts early and late onset neonatal sepsis.

    Science.gov (United States)

    Fanos, Vassilios; Caboni, Pierluigi; Corsello, Giovanni; Stronati, Mauro; Gazzolo, Diego; Noto, Antonio; Lussu, Milena; Dessì, Angelica; Giuffrè, Mario; Lacerenza, Serafina; Serraino, Francesca; Garofoli, Francesca; Serpero, Laura Domenica; Liori, Barbara; Carboni, Roberta; Atzori, Luigi

    2014-03-01

    The purpose of this article is to study one of the most significant causes of neonatal morbidity and mortality: neonatal sepsis. This pathology is due to a bacterial or fungal infection acquired during the perinatal period. Neonatal sepsis has been categorized into two groups: early onset if it occurs within 3-6 days and late onset after 4-7 days. Due to the not-specific clinical signs, along with the inaccuracy of available biomarkers, the diagnosis is still a major challenge. In this regard, the use of a combined approach based on both nuclear magnetic resonance ((1)H-NMR) and gas-chromatography-mass spectrometry (GC-MS) techniques, coupled with a multivariate statistical analysis, may help to uncover features of the disease that are still hidden. The objective of our study was to evaluate the capability of the metabolomics approach to identify a potential metabolic profile related to the neonatal septic condition. The study population included 25 neonates (15 males and 10 females): 9 (6 males and 3 females) patients had a diagnosis of sepsis and 16 were healthy controls (9 males and 7 females). This study showed a unique metabolic profile of the patients affected by sepsis compared to non-affected ones with a statistically significant difference between the two groups (p = 0.05). Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  15. Pyrolysis-GC-MS analysis of the formation and degradation stages of charred residues from lignocellulosic biomass.

    Science.gov (United States)

    González-Vila, F J; Tinoco, P; Almendros, G; Martin, F

    2001-03-01

    The structural transformations undergone by lignocellulosic biomass (freeze-dried rye grass, Lolium rigidum) subjected to progressive isothermal heating (burning at 350 degrees C under oxidizing conditions for 30, 45, 60, 75, and 90 s) have been monitored by Curie-point pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS). The pyrograms suggest that even charred residues after severe heating (carbon loss ca. 50%) still contain substantial concentrations of some resistant plant structural components. Several trends were observed when monitoring the relative concentrations of the different groups of pyrolysis compounds released during successive charring stages: (i) the tetrapyrrole moiety of chlorophylls is rapidly destroyed as indicated by the decreasing yields of pyrroles and pyrrolines, whereas the phytol backbone is comparatively more resistant, leading to phytadienes after dehydration and reduction; (ii) the increasing yields of imidazoles from progressively heated samples (maximum at 45 s stage) suggest accumulation of newly formed nitrogen-containing compounds that may survive natural fires; (iii) the lignin backbone shows a relative resistance, the yields of aromatic products pointing to progressive demethoxylation; and, (iv) a selective accumulation of recalcitrant alkyl material occurred, which is interpreted as the result of thermal condensation of hydrocarbons and fatty acids into macromolecular materials in the charred residue. In terms of the intensity of the isothermal heating, the yields of the different classes of alkyl compounds follow the order phytadienes < fatty acids < alkanes < wax esters < sterols.

  16. Determination of atractylon in rat plasma by a GC-MS method and its application to a pharmacokinetic study

    Institute of Scientific and Technical Information of China (English)

    Han Yan; Yuanyuan Sun; Yuying Ma; Bin Ji; Xiaohong Hou; Zhiguo Yu; Yunli Zhao

    2015-01-01

    A sensitive and selective method based on gas chromatography hyphenated to mass spectrometry (GC-MS) was developed and validated for the determination of atractylon in rat plasma. Plasma samples were processed by liquid-liquid extraction with ethyl acetate-n-hexane (1:1, v/v) using acetophenone as an internal standard (IS). Analytes were determined in selective ion monitoring (SIM) mode using target ions at m/z 108.1 for atractylon and m/z 105.1 for acetophenone. The calibration curve was linear over the concentration range of 10-1000 ng/mL with lower limit of quantification of 10 ng/mL. The intra- and inter-day precision variations were not more than 10.4% and 9.6%, respectively, whilst accuracy values ranged from -6.5% to 4.9%. Extraction recovery of the assay was satisfactory. This method was suc-cessfully applied to quantification and pharmacokinetic study of atractylon in rat plasma after in-tragastric administration of Atractylodis extract.

  17. Studies on thermal decomposition mechanism of CL-20 by pyrolysis gas chromatography-mass spectrometry (Py-GC/MS)

    Energy Technology Data Exchange (ETDEWEB)

    Naik, N.H.; Gore, G.M. [High Energy Materials Research Laboratory, Sutarwadi, Pune 411021 (India); Gandhe, B.R. [Directorate of Armament, DRDO Bhavan, New Delhi 110011 (India); Sikder, A.K. [High Energy Materials Research Laboratory, Sutarwadi, Pune 411021 (India)], E-mail: ak_sikder@yahoo.com

    2008-11-30

    The thermal decomposition study of CL-20 (hexanitrohexaazaisowurtzitane) using pyrolysis GC/MS was carried out mainly by electron impact (EI) mode. Chemical ionization (CI) mode was used for further confirmation of identified species. Mass spectrum of CL-20 decomposition products predominantly revealed fragments with m/z 81 and 96 corresponding to C{sub 4}H{sub 5}N{sub 2}{sup +} and C{sub 4}H{sub 4}N{sub 2}O{sup +} ions, respectively. The total ion chromatogram (TIC) of CL-20 pyrolysis shows peak within first 2 min due to the presence of low molecular weight gases. Peaks corresponding to several other products were also observed including the atmospheric gases. Cyanogen formation (C{sub 2}N{sub 2}, m/z 52) observed to be enriched at the scan number 300-500. The low molecular mass range decomposition products formed by cleavage of C-N ring structure were found in majority. Additional structural information was sought by employing chemical ionization mode. The data generated during this study was instrumented in determining decomposition pathways of CL-20.

  18. Detection and quantification of traces of bisphenol A and bisphenol S in paper samples using analytical pyrolysis-GC/MS.

    Science.gov (United States)

    Becerra, Valentina; Odermatt, Jürgen

    2012-05-01

    In this paper a simplified method based on analytical pyrolysis gas chromatography mass spectrometry (Py-GC/MS) for the detection and quantification of bisphenol A and bisphenol S in paper samples is presented. The method enables a direct analysis of the samples without tedious sample preparation. As the analytes are thermally desorbed, a solvent extraction is not needed. The method is applicable to small samples of ~120 μg. The limits of detection are below 1 mg kg(-1) for bisphenol A and for bisphenol S. The limits of quantification are about 1.3 mg kg(-1). Several validation characteristics of the method developed like standard error of calibration, limit of determination, linearity, and accuracy are given. To prove the accuracy of the method, interferences and matrix dependencies were also investigated. The influence of the pyrolysis crucibles, a special effect of analytical pyrolysis, was additionally investigated. It was found that the impact of the crucibles on the results is significant and one cause for matrix effects.

  19. Effect of extraction time on antioxidants and bioactive volatile components of green tea (Camellia sinensis, using GC/MS

    Directory of Open Access Journals (Sweden)

    Mudasir Ahmad

    2015-12-01

    Full Text Available Two green tea types, leaf grade and sanding, were extracted at different time intervals: 20, 40, and 120 min at a constant temperature of 50°C. The extracts were analyzed by GC/MS technique. The major compounds identified were myristic acid, palmitic acid, stearic acid, oleic acid, 1H-purine-2,6-dione, caffeine, linoleic acid, diethyl ester, and 1H-purine-6-amine. Stearic acid, palmitic acid, linoleic acid, and myristic acid were more abundantly present in the leaf-grade variety than sanding. However, some levels of acetic acid, cyclobutanol, hexadecanoic acid, octadecanoic acid, 9-octadecenoic acid, and caffeine were also found in both the tea types. Most of the volatile compounds were detected between 20–40-min time of extraction. The 40-min time of extraction also showed the maximum content of polyphenols and antioxidants in both the tea types. Thus, 40 min was suggested as the most suitable time for maximum extraction of bioactive volatiles, antioxidants, and polyphenols from green tea.

  20. Determination of tetrachloroethylene and other volatile halogenated organic compounds in oil wastes by headspace SPME GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Fabbri, D.; Bezzi, R.; Torri, C.; Galletti, P.; Tagliavini, E. [Bologna Univ., Ravenna (Italy). Lab. of Chemistry, C.I.R.S.A

    2007-09-15

    Oil wastes and slops are complex mixtures of hydrocarbons, which may contain a variety of contaminants including tetrachloroethylene (perchloroethylene, PCE) and other volatile halogenated organic compounds (VHOCs). The analytical determination of PCE at trace levels in petroleum-derived matrices is difficult to carry out in the presence of large amounts of hydrocarbon matrix components. In the following study, we demonstrate that headspace solid-phase microextraction (HS-SPME) combined with GC-MS analysis can be applied for the rapid measurement of PCE concentration in oil samples. The HS-SPME method was developed using liquid paraffin as matrix matching reference material for external and internal calibration and optimisation of experimental parameters. The limit of quantitation was 0.05 mg kg{sup -1}, and linearity was established up to 25 mg kg{sup -1}. The HS-SPME method was extended to several VHOCs, including trichloroethylene (TCE) in different matrices and was applied to the quantitative analysis of PCE and TCE in real samples.

  1. An integrated approach utilising chemometrics and GC/MS for classification of chamomile flowers, essential oils and commercial products.

    Science.gov (United States)

    Wang, Mei; Avula, Bharathi; Wang, Yan-Hong; Zhao, Jianping; Avonto, Cristina; Parcher, Jon F; Raman, Vijayasankar; Zweigenbaum, Jerry A; Wylie, Philip L; Khan, Ikhlas A

    2014-01-01

    As part of an ongoing research program on authentication, safety and biological evaluation of phytochemicals and dietary supplements, an in-depth chemical investigation of different types of chamomile was performed. A collection of chamomile samples including authenticated plants, commercial products and essential oils was analysed by GC/MS. Twenty-seven authenticated plant samples representing three types of chamomile, viz. German chamomile, Roman chamomile and Juhua were analysed. This set of data was employed to construct a sample class prediction (SCP) model based on stepwise reduction of data dimensionality followed by principle component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). The model was cross-validated with samples including authenticated plants and commercial products. The model demonstrated 100.0% accuracy for both recognition and prediction abilities. In addition, 35 commercial products and 11 essential oils purported to contain chamomile were subsequently predicted by the validated PLS-DA model. Furthermore, tentative identification of the marker compounds correlated with different types of chamomile was explored. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Classification of Coffee Beans by GC-C-IRMS, GC-MS, and 1H-NMR

    Directory of Open Access Journals (Sweden)

    Victoria Andrea Arana

    2016-01-01

    Full Text Available In a previous work using 1H-NMR we reported encouraging steps towards the construction of a robust expert system for the discrimination of coffees from Colombia versus nearby countries (Brazil and Peru, to assist the recent protected geographical indication granted to Colombian coffee in 2007. This system relies on fingerprints acquired on a 400 MHz magnet and is thus well suited for small scale random screening of samples obtained at resellers or coffee shops. However, this approach cannot easily be implemented at harbour’s installations, due to the elevated operational costs of cryogenic magnets. This limitation implies shipping the samples to the NMR laboratory, making the overall approach slower and thereby more expensive and less attractive for large scale screening at harbours. In this work, we report on our attempt to obtain comparable classification results using alternative techniques that have been reported promising as an alternative to NMR: GC-MS and GC-C-IRMS. Although statistically significant information could be obtained by all three methods, the results show that the quality of the classifiers depends mainly on the number of variables included in the analysis; hence NMR provides an advantage since more molecules are detected to obtain a model with better predictions.

  3. Urinary metabolomics (GC-MS) reveals that low and high birth weight infants share elevated inositol concentrations at birth.

    Science.gov (United States)

    Barberini, Luigi; Noto, Antonio; Fattuoni, Claudia; Grapov, Dmitry; Casanova, Andrea; Fenu, Gianni; Gaviano, Mauro; Carboni, Roberta; Ottonello, Giovanni; Crisafulli, Maurizio; Fanos, Vassilios; Dessì, Angelica

    2014-10-01

    Metabolomics is a new "omics" platform aimed at high-throughput identification, quantification and characterization of small-molecule metabolites. The metabolomics approach has been successfully applied to the classification different physiological states and identification of perturbed biochemical pathways. The purpose of the current investigation is the application of metabolomics to explore biological mechanisms which may lead to the onset of metabolic syndrome in adulthood. We evaluated differences in metabolites in the urine collected within 12 h from 23 infants with IUGR (IntraUterine Growth Restriction), or LGA (Large for Gestational Age), compared to control infants (10 patients defined AGA: Appropriate for Gestational Age). Urinary metabolites were quantified by GC-MS and used to highlight similarities between the two metabolic diseases and identify metabolic markers for their predisposition. Quantified metabolites were analyzed using a multivariate statistics coupled with receiver operator characteristic curve (ROC) analysis of identified biomarkers. Urinary myo-inositol was the most important discriminant between LGA + IUGR and control infants, and displayed an area under the ROC curve = 1. We postulate that the increase in plasma and consequently urinary inositol may constitute a marker of altered glucose metabolism during fetal development in both IUGR and LGA newborns.

  4. Phytohormone profiling of the sweet orange (Citrus sinensis (L.) Osbeck) leaves and roots using GC-MS-based method.

    Science.gov (United States)

    Nehela, Yasser; Hijaz, Faraj; Elzaawely, Abdelnaser A; El-Zahaby, Hassan M; Killiny, Nabil

    2016-07-20

    Phytohormones mainly affect plant development and trigger varied responses to biotic and abiotic stresses. The sensitivity of methods used to profile phytohormones is a vital factor that affects the results. We used an improved GC-MS-based method in the selective ion-monitoring (SIM) mode to study the phytohormone profiling in citrus tissues. One extraction solvent mixture and two derivatization reagents were used, methyl chloroformate (MCF) and N-Methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA). The method showed a low limit of detection and low limit of quantification with high extraction recovery percentage and reproducibility. Overall, we detected 13 phytohormones belonging to six different groups. Auxins, SAs, tJA, and ABA were detected after derivatization with MCF while cytokinins and GAs were detected after derivatization with MSTFA. Cytokinins, SAs, and gibberellins were found in all tissues while auxins and tJA were observed only in the leaves. ABA was found in leaves and roots, but not in root tips. The method we used is efficient, precise, and appropriate to study citrus phytohormonal profiles to understand their crosstalk and responses to environmental and biological stresses.

  5. Discrimination and characterization of breath from smokers and non-smokers via electronic nose and GC/MS analysis.

    Science.gov (United States)

    Witt, Katharina; Reulecke, Sina; Voss, Andreas

    2011-01-01

    The objective of this study was to prove the general applicability of an electronic nose for analyzing exhaled breath considering the dependency on smoking. At first, odor compounds from spices (n=6) were detected via the electronic nose and further characterized and classified with gas chromatography/ mass spectrometry to demonstrate the principle ability of the electronic nose. Then, the exhaled breath from smokers and non-smokers were analyzed to prove the influence of smoking on breath analyses with the electronic nose. The exhaled breath was sampled from 11 smokers and 11 non-smokers in a special sampling bag with the mounted sensor chip of the electronic nose. Additionally, solid phase micro-extraction (SPME) technique was established for detection of the specific chemical compounds with gas chromatography and mass spectrometry (GC/MS). For analyses of the sensor signals the principle component analysis (PCA) was applied and the groups were differentiated by linear discriminant function analysis. In accordance to the discrimination between the different spices and between smokers and non-smokers the PCA analysis leads to an optimum accuracy of 100%. The results of this study show that an electronic nose has the ability to detect different changes of odor components and provides separation of smoking side effects in smelling different diseases.

  6. Quantitative analysis by GC-MS/MS of 18 aroma compounds related to oxidative off-flavor in wines.

    Science.gov (United States)

    Mayr, Christine M; Capone, Dimitra L; Pardon, Kevin H; Black, Cory A; Pomeroy, Damian; Francis, I Leigh

    2015-04-08

    A quantitation method for 18 aroma compounds reported to contribute to "oxidative" flavor in wines was developed. The method allows quantitation of the (E)-2-alkenals ((E)-2-hexenal, (E)-2-heptenal, (E)-2-octenal, and (E)-2-nonenal), various Strecker aldehydes (methional, 2-phenylacetaldehyde, 3-methylbutanal, and 2-methylpropanal), aldehydes (furfural, 5-methylfurfural, hexanal, and benzaldehyde), furans (sotolon, furaneol, and homofuraneol), as well as alcohols (methionol, eugenol, and maltol) in the same analysis. The aldehydes were determined after derivatization directly in the wine with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride; the formed oximes along with the underivatized aroma compounds were isolated by solid-phase extraction and analyzed by means of GC-MS/MS. The method was used to investigate the effect of different closures (synthetic closures, natural corks, and screw cap) on the formation of oxidation-related compounds in 14 year old white wine. Results showed a significant increase in the concentration of some of the monitored compounds in the wine, particularly methional, 2-phenylacetaldehyde, and 3-methylbutanal.

  7. Catalytic fast co-pyrolysis of biomass and food waste to produce aromatics: Analytical Py-GC/MS study.

    Science.gov (United States)

    Zhang, Bo; Zhong, Zhaoping; Min, Min; Ding, Kuan; Xie, Qinglong; Ruan, Roger

    2015-01-01

    In this study, catalytic fast co-pyrolysis (co-CFP) of corn stalk and food waste (FW) was carried out to produce aromatics using quantitative pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), and ZSM-5 zeolite in the hydrogen form was employed as the catalyst. Co-CFP temperature and a parameter called hydrogen to carbon effective ratio (H/C(eff) ratio) were examined for their effects on the relative content of aromatics. Experimental results showed that co-CFP temperature of 600 °C was optimal for the formation of aromatics and other organic pyrolysis products. Besides, H/C(eff) ratio had an important influence on product distribution. The yield of total organic pyrolysis products and relative content of aromatics increased non-linearly with increasing H/C(eff) ratio. There was an apparent synergistic effect between corn stalk and FW during co-CFP process, which promoted the production of aromatics significantly. Co-CFP of biomass and FW was an effective method to produce aromatics and other petrochemicals.

  8. Optimization of espresso machine parameters through the analysis of coffee odorants by HS-SPME-GC/MS.

    Science.gov (United States)

    Caprioli, Giovanni; Cortese, Manuela; Cristalli, Gloria; Maggi, Filippo; Odello, Luigi; Ricciutelli, Massimo; Sagratini, Gianni; Sirocchi, Veronica; Tomassoni, Giacomo; Vittori, Sauro

    2012-12-01

    The aroma profile and the final quality of espresso coffee (EC) are influenced by such technical conditions as the EC machine extraction temperature and the pressure used. The effect of these two parameters on EC quality were studied in combination by headspace solid phase micro extraction-gas chromatography-mass spectrometry (SPME-GC-MS) and sensory profile. Moreover, 10 key odorants at the best EC machine settings were examined to compare the two coffee cultivars (Arabica and Robusta) and two EC machines [Aurelia Competizione (A) and Leva Arduino (B)]. The data obtained provides important information about espresso making technique, suggesting that the usual espresso machine temperature and pressure settings (i.e. 92°C and 9bar) are very close to those needed to obtain the best quality espresso. This confirms the traditional wisdom of coffee making, which judges 25ml, the typical volume of a certified Italian EC, to be ideal for very strong aroma intensity. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. Radiolytic degradation of methoxychlor in methanol and monitoring of radiolytic products by HPLC and GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Butt, S.B. [Central Analytical Facility Div., Pakistan Inst. of Nuclear Science and Technology, P.O. Nilore, Islamabad (Pakistan); Riaz, M. [Chemistry Div., Pakistan Inst. of Nuclear Science and Technology, P.O. Nilore, Islamabad (Pakistan)

    2010-07-01

    Degradation of priority organic pollutant methoxychlor in methanol solution by gamma irradiation under varied experimental conditions has been optimized. The solution of methoxychlor was air saturated before irradiation. The extent of radiolytic degradation efficiency was monitored by reversed phase HPLC-UV; two major and two minor degradation products were detected. For 5 kGy gamma radiation dose at a rate of 200 kGy h{sup -1} {>=} 95% methoxychlor was degraded. The degradation was also monitored by GC-ECD and the degradation products were identified using GC-MS after comparing their mass spectra with the NIST 98m mass spectral library. It is proposed that major degradation occurs through dechlorination, dehydrochlorination, by the detachment of methoxyphenyl from methoxychlor and by interaction of other radicals generated by the methanol radiolysis. The probable reaction schemes for the formation of products have been proposed. Most of the generated products were methoxy substituted, probably due to the availability of the methoxy radical from methanol radiolysis. The identified radiolytic products of methoxychlor and the removal efficiency have been compared with those of UV photolysis. It is observed that although the source of degradation is somewhat different, the end products or radical generated species are of similar nature. (orig.)

  10. Gamma radiolytic eradication of methoxychlor in aqueous media. The degradation pathways using HPLC and SPME-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Butt, S.B.; Zafar, A. [PINSTECH, Nilore, Islamabad (Pakistan). Central Analytical Facility Div.; Riaz, M. [PINSTECH, Nilore, Islamabad (Pakistan). Chemistry Div.

    2013-08-01

    The gamma radiation-induced degradation of environmental pollutant methoxychlor in water was investigated. A {sup 60}Co gamma radiation source with a dose rate of 372 Gy h{sup -1} was used for gamma irradiation of 1 mg L{sup -1} and 10 mg L{sup -1} methoxychlor in water with a varied absorbed dose of 1-5 kGy. A single step clean up and pre-concentration procedure based on solid phase micro-extraction was optimized. The extent of radiolytic degradation was monitored by reversed phase HPLC-UV and GC-ECD. The trace and ultra trace level degradation products were identified using GC-MS-SPME by comparing their mass spectra with the NIST 98 m mass spectral library. Most of the generated products for 4 kGy dose are substituted chlorophenols. The reaction pathways of these substituted chlorophenols and benzophenone formation are also proposed. However, generated chlorophenols disappeared along with methoxychlor for an absorbed dose of 5 kGy. The attained degradation of methoxychlor is {proportional_to} 95% that reflects the potential use of ionization radiation for wastewater treatment. (orig.)

  11. GC-MS Analysis and anti-microbial activity of Psidium Guajava (leaves grown in Malva region of India

    Directory of Open Access Journals (Sweden)

    Kapoor Nisha

    2011-12-01

    Full Text Available The essential oil of the leaves of Psidium guajava grown at Ujjain M.P. (India was isolated and analyzed by gas chromatography coupled with mass spectrometry (GC-MS. The components of the essential oil were identified by comparing their retention indices and mass spectra fragmentation patterns with those stored on the MScomputer library and also from the published literatures. The present study describes the phytochemical profile and anti-microbial activity of essential oil of P. guajava. Furthermore, anti-microbial activity of oil was evaluated using agar well diffusion method. The anti-microbial test results showed that the oil had a potential anti-microbial activity against all twelve Gram+ve and Gram-ve bacterial strains such as: Staphylococcus aureus, Streptoccocus faecalis, Bacillus subtillis, Lactobacillus spp., Enterococcus aerogenes, Acinetobacter spp.(Gram Positive and Escherichia coli, Proteus vulgari, Enterobacter aerogenes , Salmonella typhimurium, Pseudomonas aeruginoso, Klebsiella pneumoniae (Gram Nagative . Essential oil showed maximum zone of inhibition and minimal inhibition concentration against Bacillus subtillus and Escherichia coli bacterial strains. These results permitted the conclusion to be made that, it is the first report of the GCMS analysis and anti-microbial activity on a P. guajava., a naturally growing species from Malva Region of India.

  12. Comparison of Volatile Components between Raw and Vinegar Baked Radix Bupleuri by GC-MS Based Metabolic Fingerprinting Approach

    Directory of Open Access Journals (Sweden)

    Jie Xing

    2015-01-01

    Full Text Available Radix Bupleuri (RB, also named Chaihu in Chinese, is a commonly used herbal drug in traditional Chinese medicine (TCM, and the processing of RB with vinegar to prepare vinegar-baked Radix Bupleuri (VBRB has a long history in the clinic of TCM. In the present study, GC-MS coupled with multivariate data analysis was applied to compare the volatile components between crude and two vinegar processed RBs. After vinegar baking, the oil yields were decreased significantly, and the chemical compositions were also changed greatly. The chemical changes included the disappearance or appearance, as well as the content increase or decrease of some volatile compounds. The oil yields of two different VBRBs showed no significant difference but differed markedly in their chemical compositions, suggesting that the type of vinegar exerted great impacts on the vinegar-baking process. Thus, the effect of different vinegars on processing should be further investigated to ensure the therapeutic effect and safety of VBRB in clinic.

  13. Extraction and analysis of fungal spore biomarkers in atmospheric bioaerosol by HPLC-MS-MS and GC-MS.

    Science.gov (United States)

    Buiarelli, Francesca; Canepari, Silvia; Di Filippo, Patrizia; Perrino, Cinzia; Pomata, Donatella; Riccardi, Carmela; Speziale, Roberto

    2013-02-15

    Airborne microorganisms, as bacteria and fungi, are ubiquitous components of the atmospheric aerosol particles. In this paper, we report a method for the simultaneous extraction, purification, separation, identification and quantification of ergosterol, mannitol and arabitol as biomarkers of fungal spores in bioaerosol particles. After sampling by a low volume sampler, filters were spiked with mannitol-(13)C and dehydrocholesterol as internal standards. Samples were then extracted by accelerated solvent extraction using pure ethanol. The extract was then passed through an amino cartridge and divided in two parts: the apolar fraction, released from the cartridge, was subjected to liquid liquid extraction (by n-hexane), while polar compounds, retained by the cartridge, were eluted by a mixture of methanol-water. The two fractions were joined and analyzed by HPLC equipped with two different columns in series, and coupled to a triple-quadrupole mass spectrometer with Atmospheric Pressure Chemical Ionization source. In addition, the same fractions were analyzed, after derivatization, by GC-MS. The results obtained by the two techniques were finally compared, showing good agreement between them. Last, the contents of the three biomarkers have been estimated in three atmospheric samples collected in a suburban/rural site and, using literature conversion factors, correlated to fungal biomass.

  14. Exploring the Role of Different Neonatal Nutrition Regimens during the First Week of Life by Urinary GC-MS Metabolomics

    Directory of Open Access Journals (Sweden)

    Angelica Dessì

    2016-02-01

    Full Text Available In this study, a gas-chromatography mass spectrometry (GC-MS metabolomics study was applied to examine urine metabolite profiles of different classes of neonates under different nutrition regimens. The study population included 35 neonates, exclusively either breastfed or formula milk fed, in a seven-day timeframe. Urine samples were collected from intrauterine growth restriction (IUGR, large for gestational age (LGA, and appropriate gestational age (AGA neonates. At birth, IUGR and LGA neonates showed similarities in their urine metabolite profiles that differed from AGA. When neonates started milk feeding, their metabolite excretion profile was strongly characterized by the different diet regimens. After three days of formula milk nutrition, urine had higher levels of glucose, galactose, glycine and myo-inositol, while up-regulated aconitic acid, aminomalonic acid and adipic acid were found in breast milk fed neonates. At seven days, neonates fed with formula milk shared higher levels of pseudouridine with IUGR and LGA at birth. Breastfed neonates shared up-regulated pyroglutamic acid, citric acid, and homoserine, with AGA at birth. The role of most important metabolites is herein discussed.

  15. A GC-MS method for the detection and quantitation of ten major drugs of abuse in human hair samples.

    Science.gov (United States)

    Orfanidis, A; Mastrogianni, O; Koukou, A; Psarros, G; Gika, H; Theodoridis, G; Raikos, N

    2017-03-15

    A sensitive analytical method has been developed in order to identify and quantify major drugs of abuse (DOA), namely morphine, codeine, 6-monoacetylmorphine, cocaine, ecgonine methyl ester, benzoylecgonine, amphetamine, methamphetamine, methylenedioxymethamphetamine and methylenedioxyamphetamine in human hair. Samples of hair were extracted with methanol under ultrasonication at 50°C after a three step rinsing process to remove external contamination and dirt hair. Derivatization with BSTFA was selected in order to increase detection sensitivity of GC/MS analysis. Optimization of derivatization parameters was based on experiments for the selection of derivatization time, temperature and volume of derivatising agent. Validation of the method included evaluation of linearity which ranged from 2 to 350ng/mg of hair mean concentration for all DOA, evaluation of sensitivity, accuracy, precision and repeatability. Limits of detection ranged from 0.05 to 0.46ng/mg of hair. The developed method was applied for the analysis of hair samples obtained from three human subjects and were found positive in cocaine, and opiates. Published by Elsevier B.V.

  16. Identification of sink spots in two thermal desorption GC/MS systems for the analysis of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Li, Yingjie; Zhu, Jiping

    2017-04-08

    Thermal desorption (TD) GC/MS has been used for the analysis of polycyclic aromatic hydrocarbons (PAHs) and other semi-volatile organic compounds. However, thermal desorption recovery of PAHs have not been well studied and the cause of PAH residues in a TD system has not been clearly understood. Our results showed that low volatility of PAHs can lead to their incomplete recovery in a TD system: for the PAHs with low vapour pressures, up to 10% and 3% could be lost in a two-stage (TS) TD system and a short-path (SP) TD system, respectively. Within the TSTD system, the majority of residues were found in the 4-port valve and in the spot where internal trap and the 4-port valve connects. Within the SPTD system, residues were largely confined to the tube needle connecting the sample tube and GC injection port as well as inside the injection port. Since the volatility of PAHs can represent the range typical of semi-volatile organic compounds (SVOCs), our results have a wide implication for the thermal desorption of SVOCs in general. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  17. Determination of Ethyl Carbamate in Chinese Yellow Rice Wine by Diatomaceous Earth Extraction and GC/MS Method.

    Science.gov (United States)

    Wu, Pinggu; Zhang, Liqun; Shen, Xianghong; Wang, Liyuan; Zou, Yan; Zhang, Jing; Tan, Ying; Tang, Jun; Ma, Bingjie; Pan, Xiaodong; Jiang, Wei

    2015-01-01

    A sensitive and rapid analytical method based on alkaline diatomaceous earth extraction followed by GC/MS was developed for the quantitative determination of the toxic contaminant ethyl carbamate (EC) in yellow rice wines. The optimal extraction conditions were investigated. With the application of diatomaceous earth extraction, the damage of organic acids to the capillary column was greatly reduced. By using d5-EC as an internal standard for quantitative analysis of EC, the linearity of the calibration curves was good between 10 and 1000 ng/mL. The LOD and LOQ were 1.7 and 5.0 μg/kg, respectively. The spiked level of EC was 5.0-300 μg/kg, and the average recovery of the spikes was between 78.4 and 98.2%, with an RSD between 4.3 and 8.3%. Upon validation by five laboratories when spiked with 50, 100, and 300 μg/kg, the average respective recoveries were 102.9, 102.2, and 98.7% with a RSD between 0.7 and 8.1%. The validation results demonstrated that the method is fast, simple, selective, and suitable for the determination of EC in yellow rice wines.

  18. Chronological study of diazinon in putrefied viscera of rats using GC/MS, GC/EC and TLC.

    Science.gov (United States)

    Elsirafy, A A; Ghanem, A A; Eid, A E; Eldakroory, S A

    2000-03-27

    A qualitative and qualitative weekly study of diazinon in experimental rats after a lethal dose is described. GC/MS and TLC were used for qualitative, and GC/EC for quantitative analysis. The replicate content of diazinon in stomach and intestine (S/I) revealed a high rate of decrease during the first month. The liver (L) content fluctuates through a general trend of decrease. Immediate post-mortem content of 34.5 mg in summer and 94 in winter was found in S/L samples, while it was 0.79 and 0.63 respectively for L-samples. The respective remaining amount after 2 months was 1. 16, 4.40 (S/I), 0.61 and 0.66 mg (L). A round figure of 4% remains in S/L samples. The chronological plots indicate the possibility of detection at longer periods. Interpretation of data is outlined regarding relative contents of organs and the factors affecting persistence of diazinon in putrefied viscera.

  19. Study on the source of polycyclic aromatic hydrocarbons (PAHs) during coal pyrolysis by PY-GC-MS.

    Science.gov (United States)

    Dong, Jie; Li, Fan; Xie, Kechang

    2012-12-01

    Hazardous organic pollutants such as polycyclic aromatic hydrocarbons (PAHs) generated during the course of coal pyrolysis are highly mutagenic and carcinogenic. The relation between the amount of PAHs from the raw coal and that generated from coal pyrolysis were studied. Firstly, three Chinese coals from Huolinhe, Ximeng and Fenxi were respectively extracted by dichloromethane, and then, online pyrolysis analysis of the raw coals, their extraction residues and extracts were carried out respectively by PY (Pyro-probe CDS 5250)-GC-MS. The experimental results showed that the PAHs generated from the Huolinhe, Ximeng and Fenxi coals in the course of their pyrolysis was 523, 327 and 1707 μg/g, respectively, which were much higher than the free PAHs extracted from their corresponding raw coals. The PAHs in the raw coals were dominated by 4,5-ring PAHs, while those generated from the coal pyrolysis were dominated by lower-ring (2,3-rings) PAHs. A lot of important information about the generation of PAHs from residue pyrolysis was also included in the paper which indicated that the PAHs were mainly from complex chemical reactions of the coal pyrolysis, and PAHs were more likely to be generated from the residue pyrolysis due to the increased pores that appeared on the coal surface during the course of extraction operation. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Multianalytical Method Validation for Qualitative and Quantitative Analysis of Solvents of Abuse in Oral Fluid by HS-GC/MS

    Directory of Open Access Journals (Sweden)

    Bruna Claudia Coppe

    2016-01-01

    Full Text Available The use of oral fluid as a biological matrix to monitor the use of drugs of abuse is a global trend because it presents several advantages and good correlation to the blood level. Thus, the present work aimed to develop and validate an analytical method for quantification and detection of solvents used as inhalants of abuse in oral fluid (OF, using Quantisal™ as collector device by headspace and gas chromatography coupled with a mass detector (HS-GC/MS. Chromatographic separation was performed with a ZB-BAC1 column and the total time of analysis was 11.8 min. The method showed good linearity (correlation coefficient higher than 0.99 for all solvents. The limits of detection ranged from 0.05 to 5 mg/L, while the lower limits of quantification ranged from 2.5 to 12.5 mg/L. Accuracy, precision, matrix effect, and residual effect presented satisfactory results, meeting the criteria accepted for the validation of bioanalytical methods. The method showed good selectivity considering that, for solvents coeluting at the same retention time, resolution was performed by the mass detector. The method developed proved to be adequate when applied in OF samples from users of drugs and may be used to monitor the abuse of inhalants in routine forensic analyses.

  1. HS-SPME-GC-MS ANALYSIS OF VOLATILE AND SEMI-VOLATILE COMPOUNDS FROM DRIED LEAVES OF Mikania glomerata Sprengel

    Directory of Open Access Journals (Sweden)

    Esmeraldo A. Cappelaro

    2015-03-01

    Full Text Available This paper reports on the identification of volatile and semi-volatile compounds and a comparison of the chromatographic profiles obtained by Headspace Solid-Phase Microextraction/Gas Chromatography with Mass Spectrometry detection (HS-SPME-GC-MS of dried leaves of Mikania glomerata Sprengel (Asteraceae, also known as 'guaco.' Three different types of commercial SPME fibers were tested: polydimethylsiloxane (PDMS, polydimethylsiloxane/divinylbenzene (PDMS/DVB and polyacrylate (PA. Fifty-nine compounds were fully identified by HS-SPME-HRGC-MS, including coumarin, a marker for the quality control of guaco-based phytomedicines; most of the other identified compounds were mono- and sesquiterpenes. PA fibers performed better in the analysis of coumarin, while PDMS-DVB proved to be the best choice for a general and non-selective analysis of volatile and semi-volatile guaco-based compounds. The SPME method is faster and requires a smaller sample than conventional hydrodistillation of essential oils, providing a general overview of the volatile and semi-volatile compounds of M. glomerata.

  2. GC-MS Profiling of Triterpenoid Saponins from 28 Quinoa Varieties (Chenopodium quinoa Willd.) Grown in Washington State.

    Science.gov (United States)

    Medina-Meza, Ilce G; Aluwi, Nicole A; Saunders, Steven R; Ganjyal, Girish M

    2016-11-16

    Quinoa (Chenopodium quinoa Willd) contains 2 to 5% saponins in the form of oleanane-type triterpenoid glycosides or sapogenins found in the external layers of the seeds. These saponins confer an undesirable bitter flavor. This study maps the content and profile of glycoside-free sapogenins from 22 quinoa varieties and 6 original breeding lines grown in North America under similar agronomical conditions. Saponins were recovered using a novel extraction protocol and quantified by GC-MS. Oleanolic acid (OA), hederagenin (HD), serjanic acid (SA), and phytolaccagenic acid (PA) were identified by their mass spectra. Total saponin content ranged from 3.81 to 27.1 mg/g among the varieties studied. The most predominant sapogenin was phytolaccagenic acid with 16.72 mg/g followed by hederagenin at 4.22 mg/g representing the ∼70% and 30% of the total sapogenin content. Phytolaccagenic acid and the total sapogenin content had a positive correlation of r(2) = 0.88 (p quinoa in food products. The multivariate analysis showed no correlations between origin of seeds and saponin profile and/or content.

  3. Analyzing the flavor compounds in Chinese traditional fermented shrimp pastes by HS-SPME-GC/MS and electronic nose

    Science.gov (United States)

    Fan, Yan; Yin, Li'ang; Xue, Yong; Li, Zhaojie; Hou, Hu; Xue, Changhu

    2017-04-01

    Shrimp paste is a type of condiments with high nutritional value. However, the flavors of shrimp paste, particularly the non-uniformity flavors, have limited its application in food processing. In order to identify the characteristic flavor compounds in Chinese traditional shrimp pastes, five kinds of typical commercial products were evaluated in this study. The differences in the volatile composition of the five products were investigated. Solid phase micro-extraction method was employed to extract the volatile compounds. GC-MS and electronic nose were applied to identify the compounds, and the data were analyzed using principal component analysis (PCA). A total of 62 volatile compounds were identified, including 8 alcohols, 7 aldehydes, 3 ketones, 7 ethers, 7 acids, 3 esters, 6 hydrocarbons, 12 pyrazines, 2 phenols, and 7 other compounds. The typical volatile compounds contributing to the flavor of shrimp paste were found as follows: dimethyl disulfide, dimethyl tetrasulfide, dimethyl trisulfide, 2, 3, 5-trimethyl-6-ethyl pyrazine, ethyl-2, 5-dimethyl-pyrazine, phenol and indole. Propanoic acid, butanoic acid, furans, and 2-hydroxy-3-pentanone caused unpleasant odors, such as pungent and rancid odors. Principal component analysis showed that the content of volatile compounds varied depending on the processing conditions and shrimp species. These results indicated that the combinations of multiple analysis and identification methods could make up the limitations of a single method, enhance the accuracy of identification, and provide useful information for sensory research and product development.

  4. Assessment of gamma radiolytic degradation in waste lubricating oil by GC/MS and UV/VIS

    Science.gov (United States)

    Scapin, Marcos A.; Duarte, Celina L.; Bustillos, José Oscar W. V.; Sato, Ivone M.

    2009-07-01

    The hydrocarbons degradation by gamma irradiation of the waste automotive lubricating oil at different absorbed doses has was investigated. The waste automotive oil in a Brazilian oil recycling company was collected. This sample was fractioned and 50% and 70% (v/v) Milli-Q water were added. Each sample was irradiated with 100, 200 and 500 kGy doses using a gamma source Co-60—GAMMACELL type, with 5×10 3 Ci total activity. Gas chromatography-mass spectrometry (GC/MS) was used to identify degraded organic compounds. The mass spectra were analyzed using the mass spectral library from NIST, installed in the spectrometer. The sample irradiated at 500 kGy dose with 70% (v/v) Milli-Q water addition formed eight degradation products, namely diethanolmethylamine (C 5H 13NO), diethyldiethylene glycol (C 8H 18O 3), 1-octyn-3-ol, 4-ethyl (C 10H 18O) and 1.4-pentanediamine, N1, N1-diethyl (C 9H 22N 2). The color changing of the waste lubricating oil, for different absorbed doses, was determined by UV/VIS spectrophotometer. The related sample showed the lowest absorbance value evidencing the formation of 2-ethoxyethyl ether (C 8H 18O 3) compound.

  5. Distinct urine metabolome after Asian ginseng and American ginseng intervention based on GC-MS metabolomics approach

    Science.gov (United States)

    Yang, Liu; Yu, Qing-Tao; Ge, Ya-Zhong; Zhang, Wen-Song; Fan, Yong; Ma, Chung-Wah; Liu, Qun; Qi, Lian-Wen

    2016-01-01

    Ginseng occupies a prominent position in the list of best-selling natural products worldwide. Asian ginseng (Panax ginseng) and American ginseng (Panax quinquefolius) show different properties and medicinal applications in pharmacology, even though the main active constituents of them are both thought to be ginsenosides. Metabolomics is a promising method to profile entire endogenous metabolites and monitor their fluctuations related to exogenous stimulus. Herein, an untargeted metabolomics approach was applied to study the overall urine metabolic differences between Asian ginseng and American ginseng in mice. Metabolomics analyses were performed using gas chromatography-mass spectrometry (GC-MS) together with multivariate statistical data analysis. A total of 21 metabolites related to D-glutamine and D-glutamate metabolism, glutathione metabolism, TCA cycle and glyoxylate and dicarboxylate metabolism, differed significantly under the Asian ginseng treatment; 34 metabolites mainly associated with glyoxylate and dicarboxylate metabolism, TCA cycle and taurine and hypotaurine metabolism, were significantly altered after American ginseng treatment. Urinary metabolomics reveal that Asian ginseng and American ginseng can benefit organism physiological and biological functions via regulating multiple metabolic pathways. The important pathways identified from Asian ginseng and American ginseng can also help to explore new therapeutic effects or action targets so as to broad application of these two ginsengs. PMID:27991533

  6. Model studies on the oxygen-induced formation of benzaldehyde from phenylacetaldehyde using pyrolysis GC-MS and FTIR.

    Science.gov (United States)

    Chu, Fong Lam; Yaylayan, Varoujan A

    2008-11-26

    Benzaldehyde, a potent aroma chemical of bitter almond, can also be formed thermally from phenylalanine and may contribute to the formation of off-aroma. To identify the precursors involved in its generation during Maillard reaction, various model systems containing phenylalanine, phenylpyruvic acid, phenethylamine, or phenylacetaldehyde were studied in the presence and absence of moisture using oxidative and nonoxidative Py-GC-MS. Analysis of the data indicated that phenylacetaldehyde, the Strecker aldehyde of phenylalanine, is the most effective precursor and that both air and water significantly enhanced the rate of benzaldehyde formation from phenylacetaldehyde. Phenylpyruvic acid was the most efficient precursor under nonoxidative conditions. Phenethylamine, on the other hand, needed the presence of a carbonyl compound to generate benzaldehyde only under oxidative conditions. On the basis of the results obtained, a free radical initiated oxidative cleavage of the carbon-carbon double bond of the enolized phenylacetaldehyde was proposed as a possible major mechanism for benzaldehyde formation, and supporting evidence was provided through monitoring of the evolution of the benzaldehyde band from heated phenylacetaldehyde in the presence and absence of 1,1'-azobis(cyclohexanecarbonitrile) on the ATR crystal of an FTIR spectrophotometer. In the presence of the free radical initiator, the enol band of the phenylacetaldehyde centered at 1684 cm(-1) formed and increased over time, and after 18 min of heating time the benzaldehyde band centered at 1697 cm(-1) formed and increased at the expense of the enol band of phenylacetaldehyde, indicating a precursor product relationship.

  7. Catalytic Upgrading of Biomass Fast Pyrolysis Vapors with Nano Metal Oxides: An Analytical Py-GC/MS Study

    Directory of Open Access Journals (Sweden)

    Qiang Lu

    2010-11-01

    Full Text Available Fast pyrolysis of poplar wood followed with catalytic cracking of the pyrolysis vapors was performed using analytical pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS. The catalysts applied in this study were nano MgO, CaO, TiO2, Fe2O3, NiO and ZnO. These catalysts displayed different catalytic capabilities towards the pyrolytic products. The catalysis by CaO significantly reduced the levels of phenols and anhydrosugars, and eliminated the acids, while it increased the formation of cyclopentanones, hydrocarbons and several light compounds. ZnO was a mild catalyst, as it only slightly altered the pyrolytic products. The other four catalysts all decreased the linear aldehydes dramatically, while the increased the ketones and cyclopentanones. They also reduced the anhydrosugars, except for NiO. Moreover, the catalysis by Fe2O3 resulted in the formation of various hydrocarbons. However, none of these catalysts except CaO were able to greatly reduce the acids.

  8. Advanced Modular Inverter Technology Development

    Energy Technology Data Exchange (ETDEWEB)

    Adam Szczepanek

    2006-02-04

    Electric and hybrid-electric vehicle systems require an inverter to convert the direct current (DC) output of the energy generation/storage system (engine, fuel cells, or batteries) to the alternating current (AC) that vehicle propulsion motors use. Vehicle support systems, such as lights and air conditioning, also use the inverter AC output. Distributed energy systems require an inverter to provide the high quality AC output that energy system customers demand. Today's inverters are expensive due to the cost of the power electronics components, and system designers must also tailor the inverter for individual applications. Thus, the benefits of mass production are not available, resulting in high initial procurement costs as well as high inverter maintenance and repair costs. Electricore, Inc. (www.electricore.org) a public good 501 (c) (3) not-for-profit advanced technology development consortium assembled a highly qualified team consisting of AeroVironment Inc. (www.aerovironment.com) and Delphi Automotive Systems LLC (Delphi), (www.delphi.com), as equal tiered technical leads, to develop an advanced, modular construction, inverter packaging technology that will offer a 30% cost reduction over conventional designs adding to the development of energy conversion technologies for crosscutting applications in the building, industry, transportation, and utility sectors. The proposed inverter allows for a reduction of weight and size of power electronics in the above-mentioned sectors and is scalable over the range of 15 to 500kW. The main objective of this program was to optimize existing AeroVironment inverter technology to improve power density, reliability and producibility as well as develop new topology to reduce line filter size. The newly developed inverter design will be used in automotive and distribution generation applications. In the first part of this program the high-density power stages were redesigned, optimized and fabricated. One of the main

  9. Gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) in toxicological analysis. Studies on the detection of clobenzorex and its metabolites within a systematic toxicological analysis procedure by GC-MS and by immunoassay and studies on the detection of alpha- and beta-amanitin in urine by atmospheric pressure ionization electrospray LC-MS.

    Science.gov (United States)

    Maurer, H H; Kraemer, T; Ledvinka, O; Schmitt, C J; Weber, A A

    1997-02-07

    GC-MS is the method of choice for toxicological analysis of toxicants volatile in GC while non-volatile and/or thermally labile toxicants need LC-MS for their determination. Studies are presented on the toxicological detection of the amphetamine-like anorectic clobenzorex in urine by GC-MS after acid hydrolysis, extraction and acetylation and by fluorescence polarization immunoassay (FPIA, TDx (meth)amphetamine II). After ingestion of 60 mg of clobenzorex, the parent compound and/or its metabolites could be detected by GC-MS for up to 84 h or by FPIA for up to 60 h. Since clobenzorex shows no cross-reactivity with the used immunoassay, the N-dealkylated metabolite amphetamine is responsible for the positive TDx results. The intake of clobenzorex instead of amphetamine can be differentiated by GC-MS detection of hydroxyclobenzorex which is detectable for at least as long as amphetamine. In addition, the described GC-MS procedure allows the simultaneous detection of most of the toxicologically relevant drugs. Furthermore, studies are described on the atmospheric pressure ionization electrospray LC-MS detection of alpha- and beta-amanitin, toxic peptides of amanita mushrooms, in urine after solid-phase extraction on RP-18 columns. Using the single ion monitoring mode with the ions m/z 919 and 920 the amanitins could be detected down to 10 ng/ml of urine which allows us to diagnose intoxications with amanita mushrooms.

  10. Isotope internal standard method analysis of N-nitrosodimethylamine in meat products by GC-MS/MS%GC-MS/MS同位素内标法测定肉制品中N-二甲基亚硝胺

    Institute of Scientific and Technical Information of China (English)

    周佳; 孙嘉茵; 李宇茜; 唐维英; 徐小平

    2016-01-01

    采用同位素内标定量,建立一种快速、准确测定各种肉制品N-二甲基亚硝胺的GC-MS/MS法。样品中加入D6-N-二甲基亚硝胺内标,经水蒸气蒸馏、二氯甲烷提取、分离、浓缩,用多反应监测模式(MRM)进样分析。色谱柱为HP-Innowax毛细管柱(30 m×0.32 mm,0.25μm),氦气为载气,氮气为碰撞气,流量为1.4 mL/min。结果表明:该方法检测范围在10~300 ng/mL内,线性关系良好y=77.16x-500.16(r2=0.9996),精密度RSD为2.36%;回收率为82.9%~99.5%,检出限0.2μg/kg。对4种不同来源的肉制品共40批次进行检测,检出13批次,但均未超过限量(3μg/kg)。该方法灵敏、简便、准确、重复性好,可作为肉制品中N-二甲基亚硝胺检测的好方法。%A rapid and accurate method to determinate N-nitrosodimethylamine with Isotope internal standard in meat products by GC-MS/MS was established in this paper. Meat and its products, were assayed by used in the mode of multiple reaction monitoring (MRM) after water add Isotope internal standard D6-NDMA, vapor distillation, dichloromethane extraction, separation and concentration. The method was used HP capillary column (30 m ×0.32 mm,0.25μm) as the analytical column, helium as the carrier gas, nitrogen as the collision gas, and 1.4 mL/min as the flow rate. Results showed that the method had wide linear range (up to 10 to 300 ng/mL) high line correlation (y=77.16x-500.16,r2=0.999 6)), high RSD (less than 2.36%). The recovery of the method was 82.9%-99.5%, and the detection limit was 0.2 μg/kg. 40 batches of 4 kinds of different sources of meat products for inspection and 13 batches of positive, but all does not exceed limited (3 μg/kg). The results were accurate, reliable, good repeatability and high sensitivity. This method can meet the requirement for the determination of N-nitrosodimethylamine residues in meat and meat product.

  11. Composition analysis of fatty acids from four edible oils by GC-MS%GC-MS 法分析四种食用植物油脂中脂肪酸成分

    Institute of Scientific and Technical Information of China (English)

    李莎; 王维香

    2015-01-01

    The fatty acid compositions of olive oil,linseed oil,sesame oil and rapesee d oil were analyzed by GC/MS after esterification through potassium hydroxide. It showed that the content of polyunsaturated fatty acids in olive oil and linseed oil were high,77.16% and 82.25%,respectively. The content of oleic acid in olive oil was 62.95%,the content of linolenic acid was 0.87%. The content of linolenic acid in linseed oil was 62.34%,the content of oleic acid was 8.03%. The content of essential fatty acids in rapeseed oil was lower. Sesame oil might be adultered.%以不同来源的橄榄油、胡麻油、芝麻油和菜籽油为材料,通过碱法甲酯化,利用 GC–MS 法对四种植物油脂脂肪酸组成进行分析。结果表明,四种植物油脂中,橄榄油和胡麻油的不饱和脂肪酸含量高,分别为77.16%和82.25%;橄榄油中油酸含量(62.95%)高,亚麻酸含量(0.87%)低;胡麻油中亚麻酸含量(62.34%)高,油酸含量(8.03%)低;菜籽油的必需脂肪酸含量低,而芝麻油可能掺伪。

  12. Advanced analytical method of nereistoxin using mixed-mode cationic exchange solid-phase extraction and GC/MS.

    Science.gov (United States)

    Park, Yujin; Choe, Sanggil; Lee, Heesang; Jo, Jiyeong; Park, Yonghoon; Kim, Eunmi; Pyo, Jaesung; Jung, Jee H

    2015-07-01

    Nereistoxin(NTX) was originated from a marine annelid worm Lumbriconereis heteropoda and its analogue pesticides including cartap, bensultap, thiocyclam and thiobensultap have been commonly used in agriculture, because of their low toxicity and high insecticidal activity. However, NTX has been reported about its inhibitory neuro toxicity in human and animal body, by blocking nicotinic acetylcholine receptor and it cause significant neuromuscular toxicity, resulting in respiratory failure. We developed a new method to determine NTX in biological fluid. The method involves mixed-mode cationic exchange based solid phase extraction and gas chromatography/mass spectrometry for final identification and quantitative analysis. The limit of detection and recovery were substantially better than those of other methods using liquid-liquid extraction or headspace solid phase microextraction. The good recoveries (97±14%) in blood samples were obtained and calibration curves over the range 0.05-20 mg/L have R2 values greater than 0.99. The developed method was applied to a fatal case of cartap intoxication of 74 years old woman who ingested cartap hydrochloride for suicide. Cartap and NTX were detected from postmortem specimens and the cause of the death was ruled to be nereistoxin intoxication. The concentrations of NTX were 2.58 mg/L, 3.36 mg/L and 1479.7 mg/L in heart, femoral blood and stomach liquid content, respectively. The heart blood/femoral blood ratio of NTX was 0.76.

  13. Advanced Hybrid Computer Systems. Software Technology.

    Science.gov (United States)

    This software technology final report evaluates advances made in Advanced Hybrid Computer System software technology . The report describes what...automatic patching software is available as well as which analog/hybrid programming languages would be most feasible for the Advanced Hybrid Computer...compiler software . The problem of how software would interface with the hybrid system is also presented.

  14. Advances in medical diagnostic technology

    CERN Document Server

    Lai, Khin Wee; Mohamad Salim, Maheza Irna; Ong, Sang-Bing; Utama, Nugraha Priya; Myint, Yin Mon; Mohd Noor, Norliza; Supriyanto, Eko

    2014-01-01

    This book provides the most recent findings and knowledge in advanced diagnostics technology, covering a wide spectrum including brain activity analysis, breast and lung cancer detection, echocardiography, computer aided skeletal assessment to mitochondrial biology imaging at the cellular level. The authors explored magneto acoustic approaches and tissue elasticity imaging for the purpose of breast cancer detection. Perspectives in fetal echocardiography from an image processing angle are included. Diagnostic imaging in the field of mitochondrial diseases as well as the use of Computer-Aided System (CAD) are also discussed in the book. This book will be useful for students, lecturers or professional researchers in the field of biomedical sciences and image processing.

  15. MOF-5 metal-organic framework as sorbent for in-field sampling and preconcentration in combination with thermal desorption GC/MS for determination of atmospheric formaldehyde.

    Science.gov (United States)

    Gu, Zhi-Yuan; Wang, Gen; Yan, Xiu-Ping

    2010-02-15

    Metal-organic frameworks (MOFs) are one kind of highly porous crystalline materials, which are constructed by metal-containing inorganic nodes and organic linkers. With large surface area and high thermal stability, MOFs have great potential as sorbents for the preconcentration of trace analytes. However, such application of MOFs to the analysis of real samples has not been reported before. Here we report the utilization of MOF-5 as sorbent for in-field sampling and preconcentration of atmospheric formaldehyde before thermal desorption (TD) GC/MS (TD-GC/MS) determination without the need for any chemical derivatization. MOF-5 gave a 53 and 73 times better concentration effect than Tenax TA (organic polymers) and Carbograph 1TD (graphitized carbon black), respectively, for TD-GC/MS determination of formaldehyde. MOF-5 showed good performance for in-field sampling and preconcentration of formaldehyde from air samples with a relative humidity less than 45%. The collected formaldehyde on MOF-5 sorbent was stable for at least 72 h at room temperature before TD-GC/MS analysis. One tube packed with 300 mg of MOF-5 lasted 200 cycles of adsorption/TD without significant loss of collection efficiency. The breakthrough volume of such a tube was 1.2 L of 28.35 mg m(-3) formaldehyde at a sampling flow rate of 100 mL min(-1). The use of MOF-5 for in-field sampling and preconcentration in combination with TD-GC/MS for the determination of formaldehyde offered a linear range covering 3 orders of magnitude, and a detection limit of 0.6 microg m(-3). The precision for six replicate cycles of in-field sampling and preconcentration for TD-GC/MS determination using one 300 mg MOF-5 packed tube ranged from 2.8% to 5.3%. The tube-to-tube reproducibility of three MOF-5 tubes prepared in parallel was 7.7%. The developed method was applied to analysis of local indoor and outdoor air samples for formaldehyde and validated by the standard method TO-11A of the United States Environmental

  16. GC-MS method for determining faecal sterols as biomarkers of human and pastoral animal presence in freshwater sediments.

    Science.gov (United States)

    Battistel, Dario; Piazza, Rossano; Argiriadis, Elena; Marchiori, Enrico; Radaelli, Marta; Barbante, Carlo

    2015-11-01

    In order to determine sterols and stanols in freshwater sediments to reconstruct the past presence of humans and pastoral animals, we developed an analytical method based on pressurised liquid extraction (PLE), clean-up performed using solid phase extraction (SPE) and sterol determination using gas chromatography-mass spectrometry (GC-MS) analysis. PLE extraction conditions were optimised using dichloromethane (DCM) and DCM/methanol mixtures. Clean-up was performed with 2 g silica SPE cartridges, and the concentrated extracts were eluted with 70 mL DCM. Extraction yield was evaluated using an in-house reference material spiked with (13)C-labelled cholesterol and aged for 10 days. In comparison with pre-extraction, where the sediment is extracted and then spiked with a known analyte concentration, this approach preserves the original composition of the sediment. DCM and DCM/methanol mixtures resulted in high extraction yields ranging from 86 to 92 % with good reproducibility (relative standard deviation (RSD) 5-8 %). PLE extraction yields obtained with DCM as the extracting solvent were about 1.5 times higher than extractions using an ultrasonic bath. The solvent extraction mixture and matrix composition strongly affected the solvent extraction composition where higher overall recoveries (70-80 %) for each compound were obtained with DCM. The extraction mixture and matrix composition also affected the analyte concentrations, resulting in a method precision ranging from 1 to 18 %. Diatomaceous earth spiked with 10 to 100 ng of sterols, and environmental samples fortified with suitable amounts of sterols provided apparent recovery values ranging from 90 to 110 %. We applied the method to environmental samples both close to and upstream from sewage discharge zones, resulting in substantially higher faecal sterol (FeSt) concentrations near the sewage. In addition, we also applied the method to a 37-cm freshwater sediment core in order to evaluate its applicability for

  17. GC/MS evaluation of thyme (Thymus vulgaris L.) oil composition and variations during the vegetative cycle.

    Science.gov (United States)

    Hudaib, Mohammad; Speroni, Ester; Di Pietra, Anna Maria; Cavrini, Vanni

    2002-07-20

    Capillary GC/MS analysis based on polar and non-polar columns has been applied to evaluation of the volatile oils hydrodistilled from thyme (Thymus vulgaris L.) plants. The adopted methodology has been used to monitor seasonal variations in the composition of the oil obtained from thyme herbs harvested at different periods during the plant vegetative and life cycles. Oils from thyme plants of young (2 years) and old (5 years) cultivations have been evaluated from four and two collections, respectively, effected throughout May/December growth period. Generally, the oil was found to be rich in the active monoterpene phenols (thymol and carvacrol) and their corresponding monoterpene hydrocarbon (HC) precursors (p-cymene and gamma-terpinene), which collectively showed synchronized patterns of variation during the different collection periods and in different seasons. The oil from old plant collected in May/June period (0.15% v/w) was characterized by significantly lower levels of monoterpene HCs (mainly gamma-terpinene) and the highest levels of the oxygenated monoterpenes (linalool and borneol), monoterpene phenols (mainly thymol) and their derivatives (mainly carvacrol methyl ether), sesquiterpenes (mainly beta-caryophyllene) and their oxygenated derivatives (e.g. caryophyllene oxide) in comparison with all other samples. A characteristic presence of camphor and thymodihydroquinone was also observed in the old plant oils. On the other hand, the young plant, collected in June/July just before the end of the vegetative cycle, provided the best oil yield (1.2%) with also the highest % content of the monoterpene phenols (thymol: 51.2% and carvacrol: 4%). This latter growth period can represent the best harvest time of young thyme plants in order to obtain an essential oil with better quality and quantity.

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

    Directory of Open Access Journals (Sweden)

    Azadeh Emami

    2014-12-01

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

  19. Aroma Volatile Compound Analysis of SPME Headspace and Extract Samples from Crabapple (Malus sp.) Fruit Using GC-MS

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Volatile compounds from the ripened crabapple fruit of six varieties (Red Splendor, Strawberry Parfait, Pink Spire, Radiant, Sparkler, and Flame) were analyzed by the use of the SPME/GC/MS method. The changes in the volatiles between the ripened and upon full maturity fruit states were studied in Red Splendor and Strawberry Parfait. An effort was made to summarize an effective method for searching and identifying new idioplasms containing a particular fruit aroma within Malus. A total of 37 compounds were identified from the sample. The main aroma volatiles of the six varieties of fruit were comprised of 2-hexenal, 3-hexenal, hexanal, 2,4-hexadienal, benzaldehyde, diethyl phthalate. The main volatile compound of the crabapple fruit was 2-hexenal, but the relative content percentages were different (45.37, 21.98, 33.56, 32.21, 38.60, and 45.88%). The aroma components accumulated differently as the fruits ripened. The relative content of aldehydes and esters decreased as alcohols increased after the Red Splendor and Strawberry Parfait fruit ripened. For Red Splendor, the main volatile was still 2-hexenal, but the relative content decreased to 42.89%, and the relative content of alcohols increased by 13.86% as aldehydes and esters declined by 12.16 and 7.18%, respectively. For Strawberry Parfait, the main volatile was changed to cyclohexanol, and the relative content increased to 46.43%, while the relative content of alcohols increased by 49.03% as aldehydes and esters declined by 23.74 and 9.34%, respectively.

  20. Detection and identification of plasma progesterone metabolites in the female Florida manatee (Trichechus manatus latirostris) using GC/MS/MS.

    Science.gov (United States)

    Tripp, K M; Dubois, M; Delahaut, P; Verstegen, J P

    2009-08-01

    Florida manatees (Trichechus manatus latirostris) have relatively low peripheral concentrations of progesterone (P4). The objective of this study was to determine if these relatively low P4 concentrations are associated with a high ratio of progestin metabolites and to document metabolite concentrations from individual blood samples obtained from manatees during diestrus or pregnancy. Metabolites known to exist in elephants-terrestrial manatee relatives-were targeted. These included 5alpha-reduced progestins (5alpha-pregnane-3,20-dione [5alpha-DHP] and 3alpha-hydroxy-5alpha-pregnan-20-one [5alpha-P3-OH]) and 17alpha-hydroxyprogesterone (17alpha-OHP), which occurs in Asian elephants. An additional, inactive metabolite, 20alpha-hydroxyprogesterone (20alpha-OHP), indicative of P4 overproduction, was also targeted. Progesterone itself was the predominant progestin detected in pregnant and nonpregnant manatee plasma (n = 10) using gas chromatography-mass spectrometry with tandem quadrupole detectors (GC/MS/MS). Progesterone concentrations in pregnant females varied from early (moderate to high) through mid and late (low) pregnancy. Progesterone concentrations ranged from low to high in nonpregnant, nonlactating females. The most commonly detected metabolite was 5alpha-P3-OH (n = 7), which occurred in pregnant (lower limit of detection [LLOD] to high) and nonpregnant (trace to high) females. The 5alpha-DHP metabolite was also detected in pregnant (LLOD to moderate) and nonpregnant (low) females. The 17alpha-OHP metabolite was not detected in any tested female. The 20alpha-OHP metabolite was detected in one nonpregnant, nonlactating, captive female (LLOD). Metabolites were most prevalent during early pregnancy, concurrent with maximum P4 concentrations. Based on their concentrations in peripheral circulation, we inferred that these metabolites may have, opposite to elephants, a limited physiologic role during luteal, pregnant, and nonpregnant phases in the manatee.

  1. Comparison of Spot and Time Weighted Averaging (TWA Sampling with SPME-GC/MS Methods for Trihalomethane (THM Analysis

    Directory of Open Access Journals (Sweden)

    Don-Roger Parkinson

    2016-02-01

    Full Text Available Water samples were collected and analyzed for conductivity, pH, temperature and trihalomethanes (THMs during the fall of 2014 at two monitored municipal drinking water source ponds. Both spot (or grab and time weighted average (TWA sampling methods were assessed over the same two day sampling time period. For spot sampling, replicate samples were taken at each site and analyzed within 12 h of sampling by both Headspace (HS- and direct (DI- solid phase microextraction (SPME sampling/extraction methods followed by Gas Chromatography/Mass Spectrometry (GC/MS. For TWA, a two day passive on-site TWA sampling was carried out at the same sampling points in the ponds. All SPME sampling methods undertaken used a 65-µm PDMS/DVB SPME fiber, which was found optimal for THM sampling. Sampling conditions were optimized in the laboratory using calibration standards of chloroform, bromoform, bromodichloromethane, dibromochloromethane, 1,2-dibromoethane and 1,2-dichloroethane, prepared in aqueous solutions from analytical grade samples. Calibration curves for all methods with R2 values ranging from 0.985–0.998 (N = 5 over the quantitation linear range of 3–800 ppb were achieved. The different sampling methods were compared for quantification of the water samples, and results showed that DI- and TWA- sampling methods gave better data and analytical metrics. Addition of 10% wt./vol. of (NH42SO4 salt to the sampling vial was found to aid extraction of THMs by increasing GC peaks areas by about 10%, which resulted in lower detection limits for all techniques studied. However, for on-site TWA analysis of THMs in natural waters, the calibration standard(s ionic strength conditions, must be carefully matched to natural water conditions to properly quantitate THM concentrations. The data obtained from the TWA method may better reflect actual natural water conditions.

  2. LC-MS-MS and GC-MS analyses of biologically active extracts and fractions from Tunisian Juniperus phoenice leaves.

    Science.gov (United States)

    Keskes, Henda; Belhadj, Sahla; Jlail, Lobna; El Feki, Abdelfattah; Damak, Mohamed; Sayadi, Sami; Allouche, Noureddine

    2017-12-01

    Despite some studies related to Juniperus phoenicea L. (Cupressaceae), phytochemical and biological investigations of this plant remain unexplored. This work is the first report dealing with the identification and characterization of volatile components and flavonoids in hexane and methanol extracts from J. phoenicea leaves Materials and methods: Antioxidant activity of hexane, and methanol extracts from J. phoenicea leaves were determined by DPPH-radical scavenging assay. α-Amylase inhibitory activity was evaluated by enzyme inhibition using in vitro assay (each extract was dissolved in DMSO to give concentrations of 50, 100 and 200 mg/mL). The chemical composition of fractions (Fr1-Fr3) from methanol extract was determined by high-performance liquid chromatography coupled with mass spectroscopy (HPLC-MS) analysis. The hexane extract was analyzed by GC-MS technique which allowed the identification of 32 compounds. The main constituents were α-humulene (16.9%), pentadecane (10.2%) and α-cubebene (9.7%). Fraction Fr 2 exhibited a strong DPPH radical-scavenging activity (IC50 = 20.1 μg/mL) compared to that of BHT as well as the highest α-amylase inhibitory activity (IC50 = 28.4 μg/mL). Three flavonoids were identified in these fractions using HPLC-MS analysis: Quercetin 3-O-glucoside, isoscutellarein 7-O-pentoside and quercetin 3-O-pentoside. In addition, the more active fraction (Fr 2) was purified with semi-preparative HPLC affording one pure compound (amentoflavone) using (1)H NMR analysis. This compound exhibited powerful DPPH radical-scavenging (IC50 = 14.1 μg/mL) and α-amylase inhibition (IC50 = 20.4 μg/mL) effects. This study provides scientific support to some medicinal uses of J. phoenicea found in North Africa.

  3. Relative correlation of Jet-REMPI monitoring with adsorption tube sampling followed by TDS-CIS-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Zyaykina, N.; Buekens, A. [Vrije Univ., Brussels (Belgium); Desmet, K.; Sandra, P. [Ghent Univ. (Belgium)

    2004-09-15

    During earlier work rapid and highly sensitive Jet-REMPI (resonance-enhanced multiphoton ionization) mass spectrometry was applied for monitoring the effluent from thermal treatment of a filter dust during a de novo test under laboratory conditions. The sample, from ESP-Field 2 of an iron ore sintering plant, was already loaded with dioxins ({sigma}PCDD/F = 132 ng/g), their precursors (PCBz, PCPh) and other products of incomplete combustion. Heating filter dust in a temperature window 200-350 C under a flow of air results in further formation of these pollutants. As described elsewhere, on-line detection was mostly carried out using a non-selective ionization mode, to measure a wide range of compounds simultaneously. The changes of output suggest that the reaction products increase in chlorination level with time. Another explanation is that higherchlorinated compounds appear later as a consequence of lower volatility and stronger adsorption. However, due to mass spectrometric interferences, the basis of any interpretation was ambiguous. To resolve this uncertainty experiments were repeated, and the gas phase was sequentially sampled on a series of Tenax absorption tubes, which were then thermally desorbed and GC/MS-analysed. Since test conditions were comparable to those, when the effluent was monitored with Jet-REMPI, it is plausible that the gaseous products are similar in quality in both cases. In this paper the resulting peaks' identifications are combined with earlier Jet-REMPI data with the purpose of investigating: How well do Jet-REMPI profiles, measured in a non-selective mode, reflect target compounds such as low chlorinated PCDF, PCBzF, PCBz and PCPhenols/PCNaphthalenes? If these target compounds are ill-represented, which are the other compounds present that could be mistaken for target compounds.

  4. In-vitro Antioxidant Activity and GC/MS Studies on the Leaves of Mentha piperita (Lamiaceae from Morocco

    Directory of Open Access Journals (Sweden)

    Elhoussine derwich

    2011-04-01

    Full Text Available The present study was to evaluate the in vitro antioxidant activity and chemical composition of essential oil of Mentha piperita from Morocco. Mentha species from the Lamiaceae family are widely distributed in Morocco and commonly used as herbal tea, flavoring agent and medicinal plant. In this stud y, the essential oils of Mentha piperita collected in the region of Meknes (Morocco were obtained by hydro-distillation of the leaves and analysed by gas chromatography equipped with flame ionisation detector (GC-FID and gas chromatography coupled to mass spectrometry system (GC/MS for their chemical composition. The antioxidant activity of essential oils against DPPH radical was determined in vitro by treated with different concentrations of essential oil and vitamin C as standard antioxidant compound. The percentages of DPPH inhibition and IC50 were recorded. Thirty compounds were identified in leaves oil representing 58.61% of the total oil composition. The yield of essential oil of Mentha piperita was 1.02% and the major compound in the leaves was: Menthone (29.01% followed by menthol (5.58%, menthyl acetate (3.34%, menthofuran (3.01%, 1,8-cineole (2.40%, isomenthone (2.12%, limonene (2.10%, α-pinene (1.56%, germacrene-D (1.50%, β-pinene (1.25%, sabinene (1.13% and pulegone (1.12%. The radical scavenging activity (% inhibition of the essential oil from Mentha piperita was the highest (81.09± 1.21% at the concentration of 150µg/ml and the IC50 values of these plant extracts were 53.67µg/ml.

  5. GC-MS-based metabolomic study on the antidepressant-like effects of diterpene ginkgolides in mouse hippocampus.

    Science.gov (United States)

    Liang, Zihong; Bai, Shunjie; Shen, Peng; Hu, Qingchuan; Wang, Xingfa; Dong, Meixue; Wang, Wei; Li, Juan; Cheng, Ke; Zhang, Shuxiao; Zou, Dezhi; Han, Yu; Wang, Haiyang; Xie, Peng

    2016-11-01

    Ginkgo biloba extract (GBE), including EGb-761, have been suggested to have antidepressant activity based on previous behavioral and biochemical analyses. However, because GBE contain many constituents, the mechanisms underlying this suggested antidepressant activity are unclear. Here, we investigated the antidepressant-like effects of diterpene ginkgolides (DG), an important class of constituents in GBE, and studied their effects in the mouse hippocampus using a GC-MS-based metabolomics approach. Mice were randomly divided into five groups and injected daily until testing with 0.9% NaCl solution, one of three doses of DG (4.06, 12.18, and 36.54mg/kg), or venlafaxine. Sucrose preference (SPT) and tail suspension (TST) tests were then performed to evaluate depressive-like behaviors in mice. DG (12.18 and 36.54mg/kg) and venlafaxine (VLX) administration significantly increased hedonic behavior in mice in the SPT. DG (12.18mg/kg) treatment also shortened immobility time in the TST, suggestive of antidepressant-like effects. Significant differences in the metabolic profile in the DG (12.18mg/kg) compared with the control or VLX group indicative of an antidepressant-like effect were observed using multivariate analysis. Eighteen differential hippocampal metabolites were identified that discriminated the DG (12.18mg/kg) and control groups. These biochemical changes involved neurotransmitter metabolism, oxidative stress, glutathione metabolism, lipid metabolism, energy metabolism, and kynurenic acid, providing clues to the therapeutic mechanisms of DG. Thus, this study showed that DG has antidepressant-like activities in mice and shed light on the biological mechanisms underlying the effects of diterpene ginkgolides on behavior, providing an important drug candidate for the treatment of depression.

  6. Advanced Near Net Shape Technology

    Science.gov (United States)

    Vickers, John

    2015-01-01

    The objective of the Advanced Near Net Shape Technology (ANNST) project is to radically improve near net shape manufacturing methods from the current Technology/ Manufacturing Readiness Levels (TRL/MRL 3-4) to the point where they are viable candidates (TRL/ MRL-6) for shortening the time and cost for insertion of new aluminum alloys and revolutionary manufacturing methods into the development/improvement of space structures. Conventional cyrotank manufacturing processes require fabrication of multiple pieces welded together to form a complete tank. A variety of near net shape manufacturing processes has demonstrated excellent potential for enabling single-piece construction of components such as domes, barrels, and ring frames. Utilization of such processes can dramatically reduce the extent of welding and joining needed to construct cryogenic tanks and other aerospace structures. The specific focus of this project is to successfully mature the integrally stiffened cylinder (ISC) process in which a single-piece cylinder with integral stiffeners is formed in one spin/flow forming process. Structural launch vehicle components, like cryogenic fuel tanks (e.g., space shuttle external tank), are currently fabricated via multipiece assembly of parts produced through subtractive manufacturing techniques. Stiffened structural panels are heavily machined from thick plate, which results in excessive scrap rates. Multipiece construction requires welds to assemble the structure, which increases the risk for defects and catastrophic failures.

  7. ADVANCED RECIPROCATING COMPRESSION TECHNOLOGY (ARCT)

    Energy Technology Data Exchange (ETDEWEB)

    Danny M. Deffenbaugh; Klaus Brun; Ralph E. Harris; J. Pete Harrell; Robert J. Mckee; J. Jeffrey Moore; Steven J. Svedeman; Anthony J. Smalley; Eugene L. Broerman; Robert A Hart; Marybeth G. Nored; Ryan S. Gernentz; Shane P. Siebenaler

    2005-12-01

    The U.S. natural gas pipeline industry is facing the twin challenges of increased flexibility and capacity expansion. To meet these challenges, the industry requires improved choices in gas compression to address new construction and enhancement of the currently installed infrastructure. The current fleet of installed reciprocating compression is primarily slow-speed integral machines. Most new reciprocating compression is and will be large, high-speed separable units. The major challenges with the fleet of slow-speed integral machines are: limited flexibility and a large range in performance. In an attempt to increase flexibility, many operators are choosing to single-act cylinders, which are causing reduced reliability and integrity. While the best performing units in the fleet exhibit thermal efficiencies between 90% and 92%, the low performers are running down to 50% with the mean at about 80%. The major cause for this large disparity is due to installation losses in the pulsation control system. In the better performers, the losses are about evenly split between installation losses and valve losses. The major challenges for high-speed machines are: cylinder nozzle pulsations, mechanical vibrations due to cylinder stretch, short valve life, and low thermal performance. To shift nozzle pulsation to higher orders, nozzles are shortened, and to dampen the amplitudes, orifices are added. The shortened nozzles result in mechanical coupling with the cylinder, thereby, causing increased vibration due to the cylinder stretch mode. Valve life is even shorter than for slow speeds and can be on the order of a few months. The thermal efficiency is 10% to 15% lower than slow-speed equipment with the best performance in the 75% to 80% range. The goal of this advanced reciprocating compression program is to develop the technology for both high speed and low speed compression that will expand unit flexibility, increase thermal efficiency, and increase reliability and integrity

  8. Utilização do índice de retenção linear para caracterização de compostos voláteis em café solúvel utilizando GC-MS e coluna HP-Innowax Linear retention index for characterization of volatile compounds in soluble coffee using GC-MS and HP-Innowax column

    Directory of Open Access Journals (Sweden)

    Marcelo Caldeira Viegas

    2007-01-01

    Full Text Available Gas chromatography coupled with mass spectrometry (GC-MS is widely used for the characterization of volatile compounds. However, due to the complexity of the soluble coffee matrix, a complete identification of the components should not be based on mass spectra interpretation only. The linear index of retention (LRI is frequently used to give support to mass spectra. The aim of this work is to investigate the characterization of the volatile compounds in soluble coffee samples by GC-MS using LRI values found with a HP-INNOWAX column. The method used allows a significant increase of the reliability of identifying compounds.

  9. Advanced Training Technologies and Learning Environments

    Science.gov (United States)

    Noor, Ahmed K. (Compiler); Malone, John B. (Compiler)

    1999-01-01

    This document contains the proceedings of the Workshop on Advanced Training Technologies and Learning Environments held at NASA Langley Research Center, Hampton, Virginia, March 9-10, 1999. The workshop was jointly sponsored by the University of Virginia's Center for Advanced Computational Technology and NASA. Workshop attendees were from NASA, other government agencies, industry, and universities. The objective of the workshop was to assess the status and effectiveness of different advanced training technologies and learning environments.

  10. GC-MS analysis, preliminary phytochemical screening, physicochemical analysis and anti-diabetic activity of ethanol extract of Jasminum cuspidatum leaves

    Directory of Open Access Journals (Sweden)

    Singumsetty Vinay

    2014-12-01

    Full Text Available The purpose of the present study was investigating the GC-MS analysis, preliminary phytochemical screening, physicochemical analysis and anti-diabetic activity of ethanol extract of the leaves of Jasminum cuspidatum. The anti-diabetic activity was investigated in streptozotocin-induced diabetes rats with treatment of ethanol extract at the dose level of 200 and 400 mg/kg, which was compared with glibenclamide at a dose level of 4 mg/kg and the parameter measured being the blood glucose, total cholesterol, HDL, LDL, VLDL, triglycerides, and total protein. An oral glucose tolerance test (OGTT was also investigated in experimental rats. The GC-MS analysis revealed that the ethanol extract contained seven phytoconstituents. Preliminary phytochemical screening showed the presence of triterpenoids, flavonoids, glycosides and steroids. The result of in vivo anti-diabetic activity revealed that the ethanol extract of J. cuspidatum showed significant anti-diabetic activity.

  11. Use of an Acetyl Derivative to Improve GC-MS Determination of Norbuprenorphine in the Presence of High Concentrations of Buprenorphine in Urine.

    Science.gov (United States)

    Gervais, Joel R; Hobbs, Gregory A

    2016-04-01

    Certain patients being treated with Suboxone™ or Subutex™ can exhibit very high buprenorphine and low norbuprenorphine concentrations in urine. Very high buprenorphine can interfere with buprenorphine-D4 used as an internal standard, causing errors in norbuprenorphine determination by gas chromatography-mass spectrometry (GC-MS). We used a modified method of Wu et al. to introduce norbuprenorphine-D3 as a separate internal standard for norbuprenorphine. This allowed us to accurately measure norbuprenorphine in neat urine specimens when buprenorphine is present in extremely high concentrations. Laboratories measuring buprenorphine and metabolite by GC-MS may face this problem if their clientele includes patients being treated with other medications that interfere with the cytochrome p450 CYP 3A4-mediated conversion of buprenorphine to norbuprenorphine.

  12. An improved facile method for extraction and determination of steroidal saponins in Tribulus terrestris by focused microwave-assisted extraction coupled with GC-MS.

    Science.gov (United States)

    Li, Tianlin; Zhang, Zhuomin; Zhang, Lan; Huang, Xinjian; Lin, Junwei; Chen, Guonan

    2009-12-01

    An improved fast method for extraction of steroidal saponins in Tribulus terrestris based on the use of focus microwave-assisted extraction (FMAE) is proposed. Under optimized conditions, four steroidal saponins were extracted from Tribulus terrestris and identified by GC-MS, which are Tigogenin (TG), Gitogenin (GG), Hecogenin (HG) and Neohecogenin (NG). One of the most important steroidal saponins, namely TG was quantified finally. The recovery of TG was in the range of 86.7-91.9% with RSDTribulus terrestris from different areas of occurrence. The difference in chromatographic characteristics of steroidal saponins was proved to be related to the different areas of occurrence. The results showed that FMAE-GC-MS is a simple, rapid, solvent-saving method for the extraction and determination of steroidal saponins in Tribulus terrestris.

  13. Conversion of Natural Aldehydes from Eucalyptus citriodora, Cymbopogon citratus, and Lippia multiflora into Oximes: GC-MS and FT-IR Analysis †

    Directory of Open Access Journals (Sweden)

    Igor W. Ouédraogo

    2009-08-01

    Full Text Available Three carbonyl-containing extracts of essential oils from Eucalyptus citriodora (Myrtaceae, Cymbopogon citratus (Gramineae and Lippia multiflora (Verbenaceae were used for the preparation of oximes. The reaction mixtures were analyzed by GC-MS and different compounds were identified on the basis of their retention times and mass spectra. We observed quantitative conversion of aldehydes to their corresponding oximes with a purity of 95 to 99%. E and Z stereoisomers of the oximes were obtained and separated by GC-MS. During GC analysis, the high temperature in the injector was shown to cause partial dehydratation of oximes and the resulting nitriles were readily identified. Based on FT-IR spectroscopy, that revealed the high stability and low volatility of these compounds, the so-obtained oximes could be useful for future biological studies.

  14. Effects of water washing and torrefaction on the pyrolysis behavior and kinetics of rice husk through TGA and Py-GC/MS.

    Science.gov (United States)

    Zhang, Shuping; Dong, Qing; Zhang, Li; Xiong, Yuanquan

    2016-01-01

    The effects of water washing and torrefaction on the pyrolysis behavior and kinetics of rice husk were investigated through TGA and Py-GC/MS in this study. Two iso-conversional methods, i.e. Starink and FWO methods were applied for determination of the activation energy of original and pretreated rice husk samples at three different heating rates. It was found that activation energy of water washed rice husk was lower than that of original rice husk. Whereas, the activation energy increased with the increase of torrefaction temperature. The result of Py-GC/MS analysis indicated that both water washing and torrefaction pretreatments decreased the contents of acids, ketones, aldehydes and furans, while significantly increased the contents of sugars, especially levoglucosan. The relative content of released levoglucosan from pyrolysis of rice husk sample with combined water washing and 280°C torrefaction pretreatment is almost 9 times of that from original rice husk, which is about 3%.

  15. Determination of geosmin, 2-methylisoborneol, and a musty-earthy odor in wheat grain by SPME-GC-MS, profiling volatiles, and sensory analysis.

    Science.gov (United States)

    Jeleń, Henryk H; Majcher, Małgorzata; Zawirska-Wojtasiak, Renata; Wiewiórowska, Małgorzata; Wasowicz, Erwin

    2003-11-19

    Geosmin and 2-methylisoborneol-compounds responsible for the musty-earthy off-odor of wheat grain, were isolated by SPME and analyzed by GC-MS. Carboxen/PDMS/DVB fiber coating was selected because of its highest extraction efficiency. Concentrations of geosmin and 2-methylisoborneol as low as 0.001 microg/kg were detected in SIM mode using ion trap mass spectrometer. Apart from GC-MS determination of geosmin and 2-methylisoborneol, various methods for evaluating the musty-earthy off-odor caused by these compounds in wheat grain are presented. Sensory profile analysis differentiated wheat grain into sound and off-flavored, but the method was tedious. Similar groupings, however, were obtained using more rapid methods such as comparison of volatile profiles using SPME-fast GC with PCA projection of data and metal oxide (MOS) based electronic nose.

  16. HPLC-MS and GC-MS analyses combined with orthogonal partial least squares to identify cytotoxic constituents from turmeric (Curcuma longa L.).

    Science.gov (United States)

    Jiang, Jianlan; Zhang, Huan; Li, Zidan; Zhang, Xiaohang; Su, Xin; Li, Yan; Qiao, Bin; Yuan, Yingjin

    2013-08-01

    We investigated the fingerprints of 48 batches of turmeric total extracts (TTE) by HPLC-MS-MS and GC-MS analyses and 43 characteristic peaks (22 constituents from HPLC-MS-MS; 21 from GC-MS) were analyzed qualitatively and quantitatively. An MTT {3-(4,5-dimethylthiazol-2-yl)- 2,5-diphenyltetrazolium bromide} assay was implemented to measure the cytotoxicity of the TTE against HeLa cells. Then we utilized orthogonal partial least squares analysis, which correlated the chemical composition of the TTE to its cytotoxic activity, to identify potential cytotoxic constituents from turmeric. The result showed that 19 constituents contributed significantly to the cytotoxicity. The obtained result was verified by canonical correlation analysis. Comparison with previous reports also indicated some interaction between the curcuminoids and sesquiterpenoids in turmeric.

  17. GC/MS detection of central nervous tissue as specified BSE risk material in meat products and meat and bone meals: thermal stability of markers in comparison with immunochemistry and RT-PCR.

    Science.gov (United States)

    Lücker, Ernst; Biedermann, Wolfgang; Alter, Thomas; Hensel, Andreas

    2010-09-01

    Methods for the detection of central nervous tissue (CNT) are urgently needed in food control as a means for controlling strict adherence to both food labeling and banning of specified BSE risk material. Here, we report data on heat stability of the CNT markers neuron-specific enolase (NSE) in western blotting, glial fibrillary acidic protein (GFAP) in an enzyme linked immunoassay, mRNA(GFAP) in a real-time PCR assay, and several fatty acids (C22:6, C24:0-OH, C24:1ω9/ω7, C24:1ω9-OH/ω7-OH, and C24:0) in gas chromatography mass spectrometry (GC/MS). The sample matrix, a standard material of emulsion-type sausage with varied contents of CNT (brain), was heat-treated in three studies: (1) routine meat technological heat treatment with low (85 °C, 30 min), medium (115 °C, 30 min), and high (133 °C, 30 min, 3 bar) heating of 72 anonymous samples from a blind trial; (2) heat treatment under experimental conditions (100, 110, …, 200 °C, 45 min); and (3) fractionized heating of central nervous system (up to three times) under moderate routine technological conditions (85, 100, and 115 °C, 30 min). The markers of the immunochemical methods showed a low GFAP or very low NSE temperature stability at medium and high temperature conditions. The real-time PCR assay gave inconsistent, non-quantitative results, which indicated an uncontrollable matrix effect. The relevant GC/MS markers (C24:0-OH, C24:1ω9/ω7, and C24:1ω9-OH/ω7-OH) proved to be extremely stable. Neither meat and bone meal conditions (133 °C) nor experimental heating (up to and above 140 °C) showed any reduction of GC/MS CNT quantification. On the contrary, a slight but significant increase was noted over a certain temperature range (120-140 °C) for most fatty acids, possibly due to an improved extractability of the fatty acids. We conclude that a quantitative approach is highly unreliable when using immunochemical methods; moreover, these methods might be basically prone to false-negative results

  18. Qualitative and quantitative analysis on aroma characteristics of ginseng at different ages using E-nose and GC-MS combined with chemometrics.

    Science.gov (United States)

    Cui, Shaoqing; Wang, Jun; Yang, Liangcheng; Wu, Jianfeng; Wang, Xinlei

    2015-01-01

    Aroma profiles of ginseng samples at different ages were investigated using electronic nose (E-nose) and GC-MS techniques combined with chemometrics analysis. The bioactive ginsenoside and volatile oil content increased with age. E-nose performed well in the qualitative analyses. Both Principal Component Analysis (PCA) and Discriminant Functions Analysis (DFA) performed well when used to analyze ginseng samples, with the first two principal components (PCs) explaining 85.51% and the first two factors explaining 95.51% of the variations. Hierarchical Cluster Analysis (HCA) successfully clustered the different types of ginsengs into four groups. A total of 91 volatile constituents were identified. 50 of them were calculated and compared using GC-MS. The main fragrance ingredients were terpenes and alcohols, followed by aromatics and ester. The changes in terpenes, alcohols, aromatics, esters, and acids during the growth year once again confirmed the dominant role of terpenes. The Partial Least Squares (PLS) loading plot of gas sensors and aroma ingredients indicated that particular sensors were closely related to terpenes. The scores plot indicated that terpenes and its corresponding sensors contributed the most in grouping. As regards to quantitative analyze, 7 constituent of terpenes could be accurately explained and predicted by using gas sensors in PLS models. In predicting ginseng age using Back Propagation-Artificial Neural Networks (BP-ANN), E-nose data was found to predict more accurately than GC-MS data. E-nose measurement may be a potential method for determining ginseng age. The combination of GC-MS can help explain the hidden correlation between sensors and fragrance ingredients from two different viewpoints. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. The Development of a SPME-GC/MS Method for the Analysis of VOC Emissions from Historic Plastic and Rubber Materials

    OpenAIRE

    Curran, K.; Underhill, M.; Gibson, L. T.; Strlic, M.

    2015-01-01

    Analytical methods have been developed for the analysis of VOC emissions from historic plastic and rubber materials using SPME-GC/MS. Parameters such as analysis temperature, sampling time and choice of SPME fibre coating were investigated and sampling preparation strategies explored, including headspace sampling in vials and in gas sampling bags. The repeatability of the method was evaluated. It was found that a 7 d accumulation time at room temperature, followed by sampling using a DVB/CAR/...

  20. 巴豆种子油的GC-MS分析%Analysis of Oil from Seeds of Croton Tiglium By GC-MS

    Institute of Scientific and Technical Information of China (English)

    梁英; 潘英明

    2002-01-01

    巴豆种子经石油醚和无水乙醇提取得巴豆种子油,通过气相色谱-质谱联用仪(GC-MS)测定其中的化学成分,结果显示,巴豆种子油中含有26个组分,本文确定了其中22个组分的结构.

  1. Comparative Studies on the Characteristic Fatty Acid Profiles of Four Different Chinese Medicinal Sargassum Seaweeds by GC-MS and Chemometrics

    OpenAIRE

    Chen, Zhen; Xu, Yibing; Liu, Tao; Zhang, Lining; Hongbing LIU; Guan, Huashi

    2016-01-01

    Sargassum seaweeds produce abundant biomass in China and have long been used as herbal medicine and food. Their characteristic fatty acid (FA) profiles and related potential function in promoting cardiovascular health (CVH) have not been systematically investigated. In this study, FA profiles of four medicinal Sargassum were characterized using GC-MS. Principal component analysis was used to discriminate the four medicinal Sargassum, and orthogonal projection to latent structures discriminant...

  2. 气质联用仪在染整助剂检测中的应用%Application of GC-MS in Dyeing and Finishing Auxiliary Detection

    Institute of Scientific and Technical Information of China (English)

    黄旭; 张炜栋

    2010-01-01

    以匀染剂1227和有机硅柔软剂为实例,利用气相色谱-质谱联用仪(GC-MS)对其有效成分或杂质成分进行分析与确认.分析方法为常用染整助剂基本结构的确认和复配加工提供了有利的技术支撑.

  3. Determination of Wine Aroma Compounds by Head Space “In Tube Extraction” Technique and Gas Chromatography (HS-ITEX-GC/MS)

    OpenAIRE

    Luminiţa Vârva; Sonia Socaci; Anca Fărcaş; Liana Salanţă; Ana Viorica Pop Cuceu; Elena Mudura; Maria Tofană

    2015-01-01

    This study investigates the influence of vintage on the aroma compounds of white wine Episcopal from vineyard Ciumbrud, located in central Transylvania, by a non-destructive head space in tube extraction technique in tandem with GC-MS. The samples selected for analysis come from three consecutive years (2009, 2010 and 2011) from Episcopal assortment, a high quality wine obtained by blending three types of wine varieties: Sauvignon Blanc, Traminer and Pinot Gris. The results reflect the compos...

  4. GC/MS based analyses of individual organic constituents of chao phraya river water and estimated discharge rates into the upper gulf of Thailand

    Science.gov (United States)

    Ehrhardt, Manfred; Wattayakorn, Gullaya; Dawson, Rodger

    1990-05-01

    Detailed GC/MS based chemical analyses of organic concentrates from the Chao Phraya River obtained from a water sample collected in the Bangkok metropolitan area indicated that hydrocarbons of petroleum or combustion sources may be minor constituents of the dissolved lipophilic fraction relative to biogenic hydrocarbons and industrial chemicals. Using published data on river discharge and the concentrations measured in an integrated sample, tentative input rates into the Upper Gulf of Thailand for characterized chemicals are calculated.

  5. Investigation of the Material Basis Underlying the Correlation between Presbycusis and Kidney Deficiency in Traditional Chinese Medicine via GC/MS Metabolomics

    OpenAIRE

    2013-01-01

    Objective. To investigate the correlation between presbycusis and kidney deficiency as defined by traditional Chinese medicine (TCM) and its material basis from the perspective of metabolism. Methods. Pure-tone audiometry was used to test auditory function. A kidney deficiency symptom scoring table was used to measure the kidney deficiency accumulated scores of the research subjects. Gas chromatography/mass spectrometry (GC/MS) was used to measure the metabolites in the urine samples from 11 ...

  6. GC/MS ANALYSIS AND ANTIMICROBIAL ACTIVITY OF DIETHYL ETHER FRACTION OF METHANOLIC EXTRACT FROM THE STEM BARK OF ANNONA SENEGALENSIS PERS.

    Directory of Open Access Journals (Sweden)

    E. P. Awa*, S. Ibrahim and D. A. Ameh

    2012-11-01

    Full Text Available The Diethyl ether fraction of the Methanolic extract of Annona senegalensis (Pers stem bark was prepared in yield of (0.16%. Preparative Thin Layer Chromatography analysis of the fraction resulted in the identification of two spots with antimicrobial activity. Subsequent GC/MS analysis of these spots resulted in the identification of ten components (spot one and fourteen components (spot two. The fraction showed significant antimicrobial activity against clinical isolates of E. coli, S. enteriditis and S. dysenteriae.

  7. GC-MS Analysis of the liposoluble constituents from Arenaria kansuensis Maxim%藏药甘肃蚤缀脂溶性成分的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    雷宁; 马萍; 许本善; 吕亚丽; 杜树山; 张以善

    2014-01-01

    研究藏药甘肃蚤缀的脂溶性成分,进一步揭示该药材的化学成分,为这一传统藏药资源的开发利用提供实验依据。采用95%乙醇回流提取甘肃蚤缀全草,滤液浓缩后用石油醚萃取,得到脂溶性部位,通过气相色谱-质谱联用技术分析其化学成分,结合计算机检索技术及美国国家标准技术研究所( NIST)化合物谱库检索进行鉴定,采用面积归一化法确定其相对含量。从甘肃蚤缀石油醚部位共分离鉴定出25个化合物,相对含量占总含量的91.31%,包括脂肪类、甾体、三萜及芳香化合物等。%The first study was to explore the chemical compounds of the liposoluble parts from Arenaria kansuensis Maxim,and pro-vide the test basis for further rational expoitation and utilization of its medicinal resources. The air-dried whole plants of Arenaria kansuensis Maxim. were extracted with 95% ethano1. The extract was concentrated and extracted with petroleum ether to get the li-posoluble parts,and the chemical composition was identified and analyzed by GC-MS method. Combining with computer retrieval technology and search of national institute of standards and technology( NIST) compound spectral-library for identification,their rela-tive content was determined by the area normalization method. Totally 25 compounds were identified and their corresponding relative contents were evaluated by area normalization method. The content of all identified compounds is 91. 31%,of them,most are ali-phatic derivatives,steroids,triterpene and aromatic compounds.

  8. Extraction of essential oil from Ku-shui rose and component analysis by GC/MS%苦水玫瑰精油提取及其成分的GC/MS分析

    Institute of Scientific and Technical Information of China (English)

    周学森; 蒋玉梅; 毕阳; 李霁昕; 齐治国; 张顺花

    2009-01-01

    The production process of Ku-shui rose essential oil was optimized.Some main affecting factors were analyzed about yield of extraction.The results showed.the optimum extraction conditions of Ku-shui rose essential oil:the rose-water ratio was 1:4,the time of distillation was 3h,distillation rate:distillate materials was 10% of the volume of liquid per hour. Under the best conditions of the extracted, Ku- shui rose essential oil yield reached 3.982 x 10 -4.Ku-shui rose essential oil from the optimum technology was analyzed by GC/MS,the main ingredients for the fragrance was citronellol 54.58%, nerol 0.09%, geraniol 10.55%, linalool 2.90%.%对苦水玫瑰精油的生产工艺进行了优化研究,探讨了影响玫瑰精油得率的主要因素,结果显示:苦水玫瑰精油提取的最佳工艺务件为:料液比1:4、蒸馏时间3h、蒸馏速率每小时馏出液为原料液体体积的10%,在最佳的提取工艺条件下苦水玫瑰精油得率达到了3.982 × 10-4.最佳工艺所得苦水玫瑰精油气相-质谱(GC/MS)分析显示:主要香气成分含量为香茅醇54.58%、橙花醇0.09%、香叶醇10.55%、芳樟醇2.90%.

  9. Technological advances in avalanche survival.

    Science.gov (United States)

    Radwin, Martin I; Grissom, Colin K

    2002-01-01

    Over the last decade, a proliferation of interest has emerged in the area of avalanche survival, yielding both an improved understanding of the pathophysiology of death after avalanche burial and technological advances in the development of survival equipment. The dismal survival statistics born out of the modern era of winter recreation unmistakably reveal that elapsed time and depth of burial are the most critical variables of survival and the focus of newer survival devices on the market. Although blunt trauma may kill up to one third of avalanche victims, early asphyxiation is the predominant mechanism of death, and hypothermia is rare. A survival plateau or delay in asphyxiation may be seen in those buried in respiratory communication with an air pocket until a critical accumulation of CO2 or an ice lens develops. The newest survival devices available for adjunctive protection, along with a transceiver and shovel, are the artificial air pocket device (AvaLung), the avalanche air bag system (ABS), and the Avalanche Ball. The artificial air pocket prolongs adequate respiration during snow burial and may improve survival by delaying asphyxiation. The ABS, which forces the wearer to the surface of the avalanche debris by inverse segregation to help prevent burial, has been in use in Europe for the last 10 years with an impressive track record. Finally, the Avalanche Ball is a visual locator device in the form of a spring-loaded ball attached to a tether, which is released from a fanny pack by a rip cord. Despite the excitement surrounding these novel technologies, avalanche avoidance through knowledge and conservative judgment will always be the mainstay of avalanche survival, never to be replaced by any device.

  10. Chromatographic Characterization and GC-MS Evaluation of the Bioactive Constituents with Antimicrobial Potential from the Pigmented Ink of Loligo duvauceli.

    Science.gov (United States)

    Girija, Smiline; Duraipandiyan, Veeramuthu; Kuppusamy, Pandi Suba; Gajendran, Hariprasad; Rajagopal, Raghuraman

    2014-01-01

    Chromatographic characterization and the GC-MS evaluation of the black pigmented ink of Loligo duvauceli in the present study have yielded an array of bioactive compounds with potent antimicrobial property. Facing an alarm of antimicrobial resistance globally, a need for elucidating antimicrobial agents from natural sources will be the need for the hour. In this view, this study is aimed at characterizing the black pigmented ink of the Indian squid L. duvauceli. The squid ink was subjected to crude solvent extraction and was fractionated by silica gel column chromatography. TLC and HPTLC profiles were recorded. Antimicrobial bioassay of the squid ink fractions was done by agar well diffusion method. The antimicrobial fraction was then characterized using GC-MS analysis. The results showed that the n-hexane extract upon column fractionation yielded a total of 8 fractions with the mobile phase of Hex/EtOAc in different gradients. TLC and HPTLC profiles showed a single spot with a retention factor of 0.76. Fraction 1 showed significant antibacterial activity against Escherichia coli, Klebsiella pneumoniae, Staphylococcus aureus, and Lactobacillus acidophilus and a promising antifungal activity against Candida albicans. The antimicrobial fraction upon GC-MS analysis of bis(2-ethylhexyl) phthalate (BEHP) possesses the highest percentage of area normalisation (91%) with other few minor constituents. The study is concluded by stating that the antimicrobial efficacy of the squid ink might be due to the synergistic effects of the phthalate derivative and the other minor volatile compounds analysed in the squid ink.

  11. Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS

    Directory of Open Access Journals (Sweden)

    Jae Sung Pyo

    2016-01-01

    Full Text Available A gas chromatography-mass spectrometry (GC-MS method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ of propofol was 25 ng/mL. The validated method exhibited good linearity (R2=0.9989 with accuracy and precision −5.8%~11.7% and 3.7%~11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes.

  12. Comparison of fast gas chomatography-surface acoustic wave (FGC-SAW) detection and GC-MS for characterizing blueberry cultivars and maturity.

    Science.gov (United States)

    Du, Xiaofen; Olmstead, James; Rouseff, Russell

    2012-05-23

    A novel analytical method using fast gas chromatography-surface acoustic wave detection (FGC-SAW) was employed to rapidly characterize blueberry volatile profiles according to genotypes and fruit maturity. Fourteen FGC-SAW peaks were observed and 11 peaks were tentatively identified in the 15 s chromatogram. Peak identifications were confirmed by matching retention index values with similar values from GC-MS analyses of the same samples. Eighty peaks were observed in the 40 min GC-MS analysis of identical samples. Principal component analysis (PCA) score plots of FGC-SAW and GC-MS data both differentiated blueberries according to genotype, maturity stage, and harvest date even though FGC-SAW PCA's used far fewer peak area values. PCA plots clearly separated 'FL02-40', 'Snowchaser', 'Jewel', and 'Primadonna' blueberry cultivars into four quarters using two-dimensional PCA projections. FGC-SAW was also successful in differentiating three berry maturity stages in PCA score plots for both 'Jewel' and 'Primadonna' cultivars. FGC-SAW is an effective technique for rapid analysis of major blueberry volatiles, but could not determine many mid- and low-level volatiles as they were often coeluted with higher concentration volatiles.

  13. Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS.

    Science.gov (United States)

    Pyo, Jae Sung

    2016-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX) cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ) of propofol was 25 ng/mL. The validated method exhibited good linearity (R (2) = 0.9989) with accuracy and precision -5.8%~11.7% and 3.7%~11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes.

  14. FTIR and py-GC-MS spectra of true-fern and seed-fern sphenopterids (Sydney Coalfield, Nova Scotia, Canada, Pennsylvanian)

    Science.gov (United States)

    Zodrow, E.L.; Mastalerz, Maria

    2002-01-01

    Sphenopterid specimens from the Late Pennsylvanian of Sydney Coalfield, Canada, are investigated by FTIR and py-GC-MS techniques as part of an on-going research project into the biochemistry and chemotaxonomy of Pennsylvanian-age pteridophylls. Included in the investigation are samples of the true-fern species Oligocarpia brongniartii and Zeilleria delicatula that are preserved as naturally macerated cuticles (NMC), and the seed-fern Eusphenopteris neuropteroides that is also preserved as a compression/impression. FTIR spectra of NMC seed-fern E. neuropteroides, and fern sphenopterid O. brongniartii are very similar, except that the latter does not have aromatic bands in the 700-900 cm-1 out-of-plane region, py-GC-MS show more aromatic compounds for the seed fern than for the two true-fern sphenopterids. Another difference between seed-fern and true-fern sphenopterids is a lower ratio of CH2 to CH3 in chemically treated specimens (CTC) for the seed fern. These observations suggest slightly higher aromaticity for the seed ferns, perhaps related to some chemotaxonomic differences. Comparison of FTIR and py-GC-MS characteristics of sphenopterids and other plant groups shows that these two techniques have potential to identifying chemotaxonomic signals from Carboniferous pteridophylls in general, although more data are needed to confirm this. ?? 2002 Elsevier Science B.V. All rights reserved.

  15. GC-MS analysis of headspace and liquid extracts for metabolomic differentiation of citrus Huanglongbing and zinc deficiency in leaves of 'Valencia' sweet orange from commercial groves.

    Science.gov (United States)

    Cevallos-Cevallos, Juan Manuel; García-Torres, Rosalía; Etxeberria, Edgardo; Reyes-De-Corcuera, José Ignacio

    2011-01-01

    Citrus Huanglongbing (HLB) is considered the most destructive citrus disease worldwide. Symptoms-based detection of HLB is difficult due to similarities with zinc deficiency. To find metabolic differences between leaves from HLB-infected, zinc-deficient, and healthy 'Valencia' orange trees by using GC-MS based metabolomics. Analysis based on GC-MS methods for untargeted metabolite analysis of citrus leaves was developed and optimized. Sample extracts from healthy, zinc deficient, or HLB-infected sweet orange leaves were submitted to headspace solid phase micro-extraction (SPME) and derivatization treatments prior to GC-MS analysis. Principal components analysis achieved correct classification of all the derivatized liquid extracts. Analysis of variance revealed 6 possible biomarkers for HLB, of which 5 were identified as proline, β-elemene, (-)trans- caryophyllene, and α-humulene. Significant (P < 0.05) differences in oxo-butanedioic acid, arabitol, and neo-inositol were exclusively detected in samples from plants with zinc deficiency. Levels of isocaryophyllen, α-selinene, β-selinene, and fructose were significantly (P < 0.05) different in healthy leaves only. Results suggest the potential of using identified HLB biomarkers for rapid differentiation of HLB from zinc deficiency. Copyright © 2010 John Wiley & Sons, Ltd.

  16. Development and Validation of a GC-MS Method for the Detection and Quantification of Clotiapine in Blood and Urine Specimens and Application to a Postmortem Case

    Science.gov (United States)

    Mannocchi, Giulio; Pantano, Flaminia; Tittarelli, Roberta; Catanese, Miriam; Umani Ronchi, Federica; Busardò, Francesco Paolo

    2015-01-01

    Introduction. Clotiapine is an atypical antipsychotic of the dibenzothiazepine class introduced in a few European countries since 1970, efficient in treatment-resistant schizophrenic patients. There is little published data on the therapeutic and toxic concentrations of this drug. Aims. The aim of the present study is the development and validation of a method that allows the detection and quantification of clotiapine in blood and urine specimens by gas chromatography-mass spectrometry (GC-MS). Methods. Validation was performed working on spiked postmortem blood and urine samples. Samples were extracted with liquid-liquid extraction (LLE) technique at pH 8.5 with n-hexane/dichloromethane (85/15 v/v) and analysis was followed by GC-MS. Methadone-d9 was used as internal standard. Results. The limit of detection (LOD) was 1.2 and 1.3 ng/mL for urine and blood, respectively, while the lower limit of quantification (LLOQ) was 3.9 and 4.3 ng/mL, respectively. Linearity, precision, selectivity, accuracy, and recovery were also determined. The method was applied to a postmortem case. The blood and urine clotiapine concentrations were 1.32 and 0.49 μg/mL, respectively. Conclusions. A reliable GC-MS method for the detection and quantification of clotiapine in blood and urine samples has been developed and fully validated and then applied to a postmortem case. PMID:26236337

  17. Development and Validation of a GC-MS Method for the Detection and Quantification of Clotiapine in Blood and Urine Specimens and Application to a Postmortem Case

    Directory of Open Access Journals (Sweden)

    Giulio Mannocchi

    2015-01-01

    Full Text Available Introduction. Clotiapine is an atypical antipsychotic of the dibenzothiazepine class introduced in a few European countries since 1970, efficient in treatment-resistant schizophrenic patients. There is little published data on the therapeutic and toxic concentrations of this drug. Aims. The aim of the present study is the development and validation of a method that allows the detection and quantification of clotiapine in blood and urine specimens by gas chromatography-mass spectrometry (GC-MS. Methods. Validation was performed working on spiked postmortem blood and urine samples. Samples were extracted with liquid-liquid extraction (LLE technique at pH 8.5 with n-hexane/dichloromethane (85/15 v/v and analysis was followed by GC-MS. Methadone-d9 was used as internal standard. Results. The limit of detection (LOD was 1.2 and 1.3 ng/mL for urine and blood, respectively, while the lower limit of quantification (LLOQ was 3.9 and 4.3 ng/mL, respectively. Linearity, precision, selectivity, accuracy, and recovery were also determined. The method was applied to a postmortem case. The blood and urine clotiapine concentrations were 1.32 and 0.49 μg/mL, respectively. Conclusions. A reliable GC-MS method for the detection and quantification of clotiapine in blood and urine samples has been developed and fully validated and then applied to a postmortem case.

  18. Granger causality in integrated GC-MS and LC-MS metabolomics data reveals the interface of primary and secondary metabolism.

    Science.gov (United States)

    Doerfler, Hannes; Lyon, David; Nägele, Thomas; Sun, Xiaoliang; Fragner, Lena; Hadacek, Franz; Egelhofer, Volker; Weckwerth, Wolfram

    2013-06-01

    Metabolomics has emerged as a key technique of modern life sciences in recent years. Two major techniques for metabolomics in the last 10 years are gas chromatography coupled to mass spectrometry (GC-MS) and liquid chromatography coupled to mass spectrometry (LC-MS). Each platform has a specific performance detecting subsets of metabolites. GC-MS in combination with derivatisation has a preference for small polar metabolites covering primary metabolism. In contrast, reversed phase LC-MS covers large hydrophobic metabolites predominant in secondary metabolism. Here, we present an integrative metabolomics platform providing a mean to reveal the interaction of primary and secondary metabolism in plants and other organisms. The strategy combines GC-MS and LC-MS analysis of the same sample, a novel alignment tool MetMAX and a statistical toolbox COVAIN for data integration and linkage of Granger Causality with metabolic modelling. For metabolic modelling we have implemented the combined GC-LC-MS metabolomics data covariance matrix and a stoichiometric matrix of the underlying biochemical reaction network. The changes in biochemical regulation are expressed as differential Jacobian matrices. Applying the Granger causality, a subset of secondary metabolites was detected with significant correlations to primary metabolites such as sugars and amino acids. These metabolic subsets were compiled into a stoichiometric matrix N. Using N the inverse calculation of a differential Jacobian J from metabolomics data was possible. Key points of regulation at the interface of primary and secondary metabolism were identified.

  19. Quality evaluation of terpinen-4-ol-type Australian tea tree oils and commercial products: an integrated approach using conventional and chiral GC/MS combined with chemometrics.

    Science.gov (United States)

    Wang, Mei; Zhao, Jianping; Avula, Bharathi; Wang, Yan-Hong; Chittiboyina, Amar G; Parcher, Jon F; Khan, Ikhlas A

    2015-03-18

    GC/MS, chiral GC/MS, and chemometric techniques were used to evaluate a large set (n=104) of tea tree oils (TTO) and commercial products purported to contain TTO. Twenty terpenoids were determined in each sample and compared with the standards specified by ISO-4730-2004. Several of the oil samples that were ISO compliant when distilled did not meet the ISO standards in this study primarily due to the presence of excessive p-cymene and/or depletion of terpinenes. Forty-nine percent of the commercial products did not meet the ISO specifications. Four terpenes, viz., α-pinene, limonene, terpinen-4-ol, and α-terpineol, present in TTOs with the (+)-isomer predominant were measured by chiral GC/MS. The results clearly indicated that 28 commercial products contained excessive (+)-isomer or contained the (+)-isomer in concentrations below the norm. Of the 28 outliers, 7 met the ISO standards. There was a substantial subset of commercial products that met ISO standards but displayed unusual enantiomeric+/-ratios. A class predictive model based on the oils that met ISO standards was constructed. The outliers identified by the class predictive model coincided with the samples that displayed an abnormal chiral ratio. Thus, chiral and chemometric analyses could be used to confirm the identification of abnormal commercial products including those that met all of the ISO standards.

  20. Differentiation of manuka honey from kanuka honey and from jelly bush honey using HS-SPME-GC/MS and UHPLC-PDA-MS/MS.

    Science.gov (United States)

    Beitlich, Nicole; Koelling-Speer, Isabelle; Oelschlaegel, Stefanie; Speer, Karl

    2014-07-01

    In the present study, pollen-identical pure manuka and kanuka honeys and an Australian jelly bush honey were analyzed for the nonvolatiles by UHPLC-PDA-MS/MS and for the volatiles by HS-SPME-GC/MS. A chromatographic profile matchup by means of characteristic marker compounds achieved a clear discrimination between manuka, kanuka, and jelly bush honey. UHPLC-PDA profiles of manuka honey show leptosin, acetyl-2-hydroxy-4-(2-methoxyphenyl)-4-oxobutanate, 3-hydroxy-1-(2-methoxyphenyl)-penta-1,4-dione, kojic acid, 5-methyl-3-furancarboxylic acid, and two unknown compounds as prominent, kanuka honey was characterized by 4-methoxyphenyllactic acid, methyl syringate, p-anisic acid, and lumichrome. 2-Methylbenzofuran, 2'-hydroxyacetophenone, and 2'-methoxyacetophenone were markant volatiles for manuka honey, whereas kanuka honey was characterized by 2,6,6-trimethyl-2-cyclohexene-1,4-dione, phenethyl alcohol, p-anisaldehyde, and an unknown compound in HS-SPME-GC/MS. The jelly bush honey differed from the manuka honey by higher contents of 2-methoxybenzoic acid and an individual unknown substance in the PDA profile and by lower intensities of 2'-methoxyacetophenone, higher concentrations of cis-linalool oxide, and 3,4,5-trimethylphenol in the HS-SPME-GC/MS profile.