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Sample records for capillary gas chromatography

  1. Analysis of phenolic type antioxidants; Capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Chopra, S.K. (Indian Inst. of Petroleum, Dehradun (India)); Kapoor, V.B. (Indian Inst. of Petroleum, Dehradun (India)); Vishnoi, S.C. (Indian Inst. of Petroleum, Dehradun (India)); Bhagat, S.D. (Indian Inst. of Petroleum, Dehradun (India))

    1994-06-01

    A simple gas chromatographic (GC) procedure has been developed to estimate the individual alkylated phenols used as antioxidants to improve the shelf life of fuels and lubricants. Preparative gas chromatography was applied for separation and collection in sufficient quantity of the isomers of tertiary butyl, octyl and dodecyl phenols prepared by catalytic alkylation of phenol with isobutylene or its oligomers. The separated fractions were characterised by Infra-red spectrometry (IR) and paper chromatography. Out of several GC columns studies, a high resolution capillary column of 100% Methyl, Silicone gum (SE-30) as stationary phase gave best results. Data generated on various packed and capillary columns are in good agreement. (orig.)

  2. A novel ionic liquids grafted polysiloxane for capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    Qing Quan Wei; Mei Ling Qi; Ruo Nong Fu

    2009-01-01

    A new ionic liquids grafted polysiloxane used as stationary phase for capillary gas chromatography(CGC)is described.The stationary phase of 1-vinyl-3-hexylimidazolium hexafluorophosphate anchored to polysiloxane(PMHS-[VHIm][PF6])was synthesized,characterized and coated onto capillary columns by static coating.The results show that the present stationary phase exhibits a very good chromatographic resolution and selectivity for Grob test mixture and alcohols with baseline resolution and symmetry peaks.The present work suggests that novel stationary phase has a great potential for further development and application.

  3. Fundamentals of the Theory of Capillary Gas-Liquid-Solid Chromatography

    Science.gov (United States)

    Berezkin, Viktor G.; Zolotarev, P. P.

    1984-11-01

    It is shown that the known instances of the separation of volatile compounds actually refer to gas-liquid-solid chromatography and not gas-liquid chromatography, the walls of the capillary column fulfilling the function of the solid. The theories of the retention and spreading of the chromatographic bands in elution gas-liquid-solid chromatography are examined. The results of theoretical and experimental studies indicate the need to take into account the role of adsorption in capillary gas-liquid chromatography. The bibliography includes 140 references.

  4. Urinary catecholamine metabolites: Capillary gas chromatography method and experience with 12 cases of neuroblastoma

    OpenAIRE

    Grkovic, Sanja; Nikolic, Rajko; Dordevic, Maja; Stojanov, Ljubomir

    2005-01-01

    We propose a rapid, simple metodology for routine analysis of human urine to detect vanillylmandelic and homovanillic acid related to neuroblastoma. The assay were specific capillary gas chromatography with flame ionization detection. In this methodology an internal standard is used and the procedure involves ethyl ester formation without isolation of the compounds of interest. The run time is 36 minutes. We also report quantitative results for urinary vanillylmandelic and homovanillic acid i...

  5. Capillary gas-liquid chromatography separation of phenethylamines in amphetamine-positive urine samples.

    Science.gov (United States)

    DePace, A; Verebey, K; elSohly, M

    1990-11-01

    Good gas chromatography (GC) separation of molecules is essential for clean gas chromatography/mass spectrometry (GC/MS) confirmation of compounds. The trifluoro derivatives of ephedrine (E) and methamphetamine (MA) coelute on dimethyl silicone capillary columns, such as DB-1, which are most commonly used by chromatographers. Methods are described to separate E and MA to aid GC/MS confirmations of methamphetamine, ephedrine, or both E and MA together, whichever may be present in Enzyme Immunoassay (EIA)-analyzed amphetamine-positive urine samples. The use of the heptafluoro derivatives of E and MA on a DB-1 column, or the trifluoro derivatives of E and MA on a DB-17 column, is suggested for good gas chromatographic separation.

  6. Estimating Fatty Acid Composition of Infant Buccal Mucosal Cells by Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    CHEN Fei; ZHANG Wei-li; LI Fang; ZHU Xiao-dong; ZHU Jian-xing

    2008-01-01

    Long chain polyunsaturated fatty adds, i. e., docosahexaenoic acid (DHA or C22 : 6n -3), arachidonic acid (AA or C20 : 4n - 6) have been identified as essential fatty acids and play an important role in growth and development of infants. Mensurement of fatty acid composition is usually by collection of blood, but to obtain blood in infants is difficult. Nowadays, the fatty acid composition can be estimated by collecting buccal mucosal cells, which can avoid repeated blood sampling. The purpose of this paper is to compare the fatty acid composition of cheek calls with that of plasma and red blood cells (RBCs). In this study, twenty-seven infants were enrolled, and buccal mucosal cells and blood samples were obtained from these infants of the same time. Fatty acid composition of buccal mucesal cells, plasma and RBCs were measured by capillary gas chromatography. The results show that the contents of AA and DHA in the buccal mucosal cells are correlated well with that in the plasma [r=0.36 (P=0.042) and r=0.38 (P=0.033), respectively]. The ratio of AA to DHA is 1.32% in buccal mucosal cells, 1.60% in plasma and 1.55% in RBCs and there are no significant differences among groups (P = 0.134). It shows that the fatty acid composition in buccal mucosal cells can reflect the fat nutrition status in infants and can be detected by capillary gas chromatography. Estimating fatty acid composition of buccal mucosal cells in infants by capillary gas chromatography is feasible, and because of its noninvasiveness, it can be suitable for nutrition research in infants.

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

    Directory of Open Access Journals (Sweden)

    Enrico Di Donato

    2007-01-01

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

  8. Novel guanidinium-based ionic liquids as stationary phases for capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    Li Zhen Qiao; Kai Lu; Mei Ling Qi; Ruo Nong Fu

    2010-01-01

    The present study describes guanidinium-based ionic liquids(GBILs)as stationary phases for capillary gas chromatography(CGC)and to the best of our knowledge,no related reports are available up to now.In this study,a hexaalkylguanidinium ionic liquid(DOTMG-NTf2)was synthesized and coated statically onto capillary columns.Selectivity of the stationary phase was evaluated by separating Grob test mixture,test mixture,alcohols mixture,and fatty acid methyl esters mixture,and thermal stability was investigated as well.The present study demonstrates that GBILs as CGC stationary phases exhibit satisfactory selectivity and thermal stability and have a great potential as new candidates for CGC stationary phases.

  9. On-column micro gas chromatography detection with capillary-based optical ring resonators.

    Science.gov (United States)

    Shopova, Siyka I; White, Ian M; Sun, Yuze; Zhu, Hongying; Fan, Xudong; Frye-Mason, Greg; Thompson, Aaron; Ja, Shiou-jyh

    2008-03-15

    We developed a novel on-column micro gas chromatography (microGC) detector using capillary based optical ring resonators (CBORRs). The CBORR is a thin-walled fused silica capillary with an inner diameter ranging from a few tens to a few hundreds of micrometers. The interior surface of the CBORR is coated with a layer of stationary phase for gas separation. The circular cross section of the CBORR forms a ring resonator and supports whispering gallery modes (WGMs) that circulate along the ring resonator circumference hundreds of times. The evanescent field extends into the core and is sensitive to the refractive index change induced by the interaction between the gas sample and the stationary phase. The WGM can be excited and monitored at any location along the CBORR by placing a tapered optical fiber against the CBORR, thus enabling on-column real-time detection. Rapid separation of both polar and nonpolar samples was demonstrated with subsecond detection speed. Theoretical work was also established to explain the CBORR detection mechanism. While low-nanogram detection limits are observed in these preliminary tests, many methods for improvements are under investigation. The CBORR is directly compatible with traditional capillary GC columns without any dead volumes. Therefore, the CBORR-based muGC is a very promising technology platform for rapid, sensitive, and portable analytical devices.

  10. Rapid separation of beryllium and lanthanide derivatives by capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Harvey, Scott D.; Lucke, Richard B.; Douglas, Matt

    2012-09-04

    Previous studies describe derivatization of metal ions followed by analysis using gas chromatography, usually on packed columns. In many of these studies, stable and volatile derivatives were formed using fluorinated β-diketonate reagents. This paper extends previous work by investigating separations of the derivatives on small-diameter capillary gas chromatography columns and exploring on-fiber, solid-phase microextraction derivatization techniques for beryllium. The β-diketonate used for these studies was 1,1,1,2,2,6,6,7,7,7-decafluoro-3,5-heptanedione. Derivatization of lanthanides also required addition of a neutral donor, dibutyl sulfoxide, in addition to 1,1,1,2,2,6,6,7,7,7-decafluoro-3,5-heptanedione. Unoptimized separations on a 100-μm i.d. capillary column proved capable of rapid separations (within 15 min) of lanthanide derivatives that are adjacent to one another in the periodic table. Full-scan mass spectra were obtained from derivatives containing 5 ng of each lanthanide. Studies also developed a simple on-fiber solid-phase microextraction derivatization of beryllium. Beryllium could be analyzed in the presence of other alkali earth elements (Ba(II) and Sr(II)) without interference. Finally, extension of the general approach was demonstrated for several additional elements (i.e. Cu(II), Cr(III), and Ga(III)).

  11. Polymer-coated fibrous materials as the stationary phase in packed capillary gas chromatography.

    Science.gov (United States)

    Saito, Yoshihiro; Tahara, Ai; Imaizumi, Motohiro; Takeichi, Tsutomu; Wada, Hiroo; Jinno, Kiyokatsu

    2003-10-15

    Synthetic polymer filaments have been introduced as the support material in packed capillary gas chromatography (GC). The filaments of the heat-resistant polymers, Zylon, Kevlar, Nomex, and Technora, were longitudinally packed into a short fused-silica capillary, followed by the conventional coating process for open-tubular GC columns. The separation of several test mixtures such as n-alkylbenzenes and n-alkanes was carried out with these polymer-coated fiber-packed capillary columns. With the coating by various polymeric materials on the surface of these filaments, the retentivity was significantly improved over the parent fiber-packed column (without polymer coating) as well as a conventional open-tubular capillary of the same length. The results demonstrated a good combination of Zylon as the support and poly(dimethylsiloxane)-based materials as the coating liquid-phase for the successful GC separation of n-alkanes and polycyclic aromatic hydrocarbons (PAHs), while successful applications for other separations such as poly(ethylene glycol) coating for the separation of alcohols were also obtained. From the results it has been suggested that the selectivity of the fiber-packed column could be tuned by selecting different coating materials, indicating the promising possibility for a novel usage of fine fibrous polymers as the support material that can be combined with newly synthesized coating materials specially designed for particular separations. Taking advantage of good thermal stability of the fibers, the column temperature could be elevated to higher than 350 degrees C with the combination of a short metallic capillary.

  12. Rapid determination of cholesterol in milk and milk products by direct saponification and capillary gas chromatography.

    Science.gov (United States)

    Fletouris, D J; Botsoglou, N A; Psomas, I E; Mantis, A I

    1998-11-01

    A simple method is described for the determination of cholesterol in milk and milk products. Samples (0.2 g) are saponified in capped tubes with 0.5 M methanolic KOH solution by heating for 15 min at 80 degrees C. Water is added to the mixtures, and the unsaponifiable fractions are extracted with hexane to be further analyzed by capillary gas chromatography. Because of the rapid sample preparation and gas chromatographic procedures, a single sample can be analyzed in 30 min. Overall recovery was 98.6%, and the linearity was excellent for the fortification range examined. Precision data that were based on the variation within and between days suggested an overall relative standard deviation value of 1.4%. The method has been successfully applied to quantitate cholesterol in a variety of milk products.

  13. Determination of pyrethroid residues in tobacco and cigarette smoke by capillary gas chromatography.

    Science.gov (United States)

    Cai, Jibao; Liu, Baizhan; Zhu, Xiaolan; Su, Qingde

    2002-07-26

    The extraction of fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin from tobacco (Nicotina tobaccum) and cigarette smoke condensate with acetone, followed by partition of resulting acetone mixture with petroleum ether, was investigated and found suitable for capillary gas chromatography (GC) residue analysis. Florisil column clean-up was found to provide clean-up procedure for tobacco and cigarette smoke condensate permitting analysis to < or = 0.01 microgram.g-1 for most of the pyrethroids by GC with a 63Ni electron capture detector (GC-ECD). Quantitative determination was obtained by the method of external standards. Cigarettes made from flue-cured tobacco spiked with different amounts of pyrethroids were used and the pyrethroid levels in mainstream smoke were determined. For all the pyrethroid residues, 1.51-15.50% were transferred from tobacco into cigarette smoke.

  14. Octopamine Levels in Blattella Germanica L. Tissues by Capillary Gas Chromatography with Electron Capture Detection

    Directory of Open Access Journals (Sweden)

    Shuren Jiang

    2005-05-01

    Full Text Available Abstract: Distribution and levels of octopamine (OA, one of the biogenic amines in the invertebrate nervous system, may have significant effects on insect physiological processes including growth, feeding and reproduction. In this paper capillary gas chromatography with electron capture detection (GC-ECD and mass selective detection (GC-MS were used to determine the content of OA in Blattella germanica L. central nervous system (CNS, and that of OA in cockroach stressed by kinds of insecticides, known octopaminergic agonists and some essential oils. A derivatization method for organic extracts via reaction with pentafluoropropionic anhydride (PFPA was developed. The resulting OA derivatives were confirmed by GC-MS to be tris-pentafluoropropionyl-OA. The method was used to quantify the amount of OA in insect issues by capillary GC-ECD through an extraction-derivatization-liquid/liquid partition procedure. Average OA content in normal cockroaches was determined to be 68.49 ± 7.31 ng/g tissue (N=5 determinations. It was shown that insecticides including chlordimeform, methomyl, permethrin, chlorfluazuron, malathion, trichlorfon and some oxazolidine agonists, essential oils including eugenol, cinnamic alcohol, phenyl ethyl alcohol could led to significant increase of OA levels in the cockroach CNS comparing with which in insect treated by 1-butanone. Malathion, trichlorfon, chlorfluazuron and cinnamic alcohol were shown to be able to cause a 20- fold increase in OA levels.

  15. Sensitive determination of xylenes in whole blood by capillary gas chromatography with cryogenic trapping.

    Science.gov (United States)

    Hattori, H; Iwai, M; Kurono, S; Yamada, T; Watanabe-Suzuki, K; Ishii, A; Seno, H; Suzuki, O

    1998-11-06

    A new and sensitive method for measurement of o-, m- and p-xylenes in human whole blood by capillary gas chromatography (GC) with cryogenic trapping is presented. After heating 0.5 ml of whole blood and 0.5 ml of distilled water containing the xylenes and aniline (internal standard, I.S.) in a 4.0-ml vial at 100 degrees C for 30 min, 2 ml of the headspace vapor was drawn into a glass syringe. All vapor was introduced through the GC port into an AT-Wax middle-bore capillary column in the splitless mode at an oven temperature of 5 degrees C to trap the entire analytes, and the oven temperature was then programmed up to 180 degrees C. The present conditions gave sharp peaks for xylenes and aniline (I.S.), and low background noises for whole blood samples; the peaks of p- and m-xylenes showed about 90% separation with the AT-Wax column. As much as 41.0-46.3% of xylenes, which had been spiked to whole blood could be recovered. The calibration curves showed linearity in the range of 0.1-0.5 microg/0.5 ml of whole blood. The detection limit was estimated to be about 10 ng/0.5 ml. The coefficients of intra-day and inter-day variations for xylenes were not greater than 9.38%. The data for actual detection of xylenes in post-mortem blood of self-ignition suicide cases by the present method were also presented.

  16. [Determination of alkyl-phenols in textiles by in-tube capillary solid-phase extraction-gas chromatography].

    Science.gov (United States)

    Zhang, Luohong; Du, Ting; Zhong, Jiayu

    2015-10-01

    An in-tube capillary solid-phase extraction (SPE) -gas chromatography (GC) method was developed for confirmation and quantitative determination of octylphenol (OP) and nonylphenol (NP) in textiles. To make the in-tube capillary SPE column, the best SPE cartridge was chosen from four kinds of SPE cartridges. The adsorbent in the cartridge was used as the filling material to make the in-tube capillary SPE column. The nature, volume used, flow rate and adsorption capacity of the eluent were compared. Finally, the in-tube capillary solid-phase extraction was combined with gas chromatography to detect the alkyl phenols (APs). Abselut NEXUS extraction cartridge was chosen as the best solid phase extractant. The optimal in-tube capillary SPE extraction conditions were as follows: 1.2 μL methanol and 1.2 μL ultra-pure water for activating the extraction column, 1.2 μL methanol for eluting, 0.4 μL/min for solution loading. The method showed a good linear relationship in the low concentration range, and the enrichment ratios for the APs were about 100 times. The detection limits of octylphenol and nonylphenol were 3.7 μg/L and 4.5 μg/L, respectively. The recoveries of octylphenol were 85.6%-98.2%, and those of nonylphenol were 83.8%-95.7%. The experimental results demonstrated that the method is simple, rapid, and useful for detecting APs in textiles.

  17. Isotopic fractionation of fentanyl and its deuterated analogues by capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan)

    1997-12-01

    Isotopic fractionation of fentanyl (FT) and its deuterated analogues by gas chromatography using capillary columns (CBP1 and CBP5) has been investigated. Seven kinds of analogues were labeled with 5 to 19 deuterium atoms at the anilino, propionyl and/or phenylethyl group of FT. The retention times of deuterated FT in CBP1 and CBP5 columns are inversely proportional to the number of labeled deuterium atoms in the molecule. The difference in free enegy changes ({Delta}{Delta}G) had a linear relationship with the number of labeled deuterium atoms, except for labeling at anilino and phenylethyl group. The contribution of a deuterium atom to the {Delta}{Delta}G value was estimated to be 1.13 cal/mol in CBP1 and 1.40 cal/mol in CBP5, respectively. While, its contribution in the propiony group was 2.84 cal/mol in CBP1 and 2.48 cal/mol in CBP5, respectively. An important factor in separation by GC may differences in interactions between the stationary phase of the column with the three dimensional protrusive moiety in the molecule. (author)

  18. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.;

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  19. Application of capillary gas chromatography mass spectrometry/computer techniques to synoptic survey of organic material in bed sediment

    Science.gov (United States)

    Steinheimer, T.R.; Pereira, W.E.; Johnson, S.M.

    1981-01-01

    A bed sediment sample taken from an area impacted by heavy industrial activity was analyzed for organic compounds of environmental significance. Extraction was effected on a Soxhlet apparatus using a freeze-dried sample. The Soxhlet extract was fractionated by silica gel micro-column adsorption chromatography. Separation and identification of the organic compounds was accomplished by capillary gas chromatography/mass spectrometry techniques. More than 50 compounds were identified; these include saturated hydrocarbons, olefins, aromatic hydrocarbons, alkylated polycyclic aromatic hydrocarbons, and oxygenated compounds such as aldehydes and ketones. The role of bed sediments as a source or sink for organic pollutants is discussed. ?? 1981.

  20. Determination of homovanillic, isohomovanillic and vanillylmandelic acids in human urine by means of glass capillary gas-liquid chromatography with temperature-programmed electron-capture detection.

    Science.gov (United States)

    Chauhan, J; Darbre, A

    1980-10-10

    The determination of urinary homovanillic, isohomovanillic and vanillylmandelic acids as their trifluoroacetylhexafluoroisopropyl ester derivatives by glass capillary gas-liquid chromatography has been studied. It was shown that even with high column efficiencies a single peak-single compound relationship could not be assumed and for reliable quantitation it was necessary to check determinations with a second gas-liquid chromatography column.

  1. High-temperature separation with polymer-coated fiber in packed capillary gas chromatography.

    Science.gov (United States)

    Saito, Yoshihiro; Ogawa, Mitsuhiro; Imaizumi, Motohiro; Ban, Kazuhiro; Abe, Akira; Takeichi, Tsutomu; Wada, Hiroo; Jinno, Kiyokatsu

    2005-06-01

    High-temperature gas chromatographic separation of several synthetic polymer mixtures with Dexsil-coated fiber-packed columns was studied. A bundle of heat-resistant filaments, Zylon, was longitudinally packed into a short metal capillary, followed by the conventional coating process with Dexsil 300 material. Prior to the packing process the metal capillary was deactivated by the formation of a silica layer. The typical size of the resulting column was 0.3-mm i.d., 0.5-mm o.d., 1-m length, and packed with about 170 filaments of the Dexsil-coated Zylon. The column temperature could be elevated up to 450 degrees C owing to the good thermal stability of the fiber, Dexsil coating, and metal capillary; furthermore, this allowed the separation of low-volatile compounds to be studied.

  2. Enantiomeric separation of organophosphorus pesticides by high-performance liquid chromatography, gas chromatography and capillary electrophoresis and their applications to environmental fate and toxicity assays.

    Science.gov (United States)

    Li, Ling; Zhou, Shanshan; Jin, Lixia; Zhang, Cheng; Liu, Weiping

    2010-05-15

    In recent years, the continuous evolution of the field of stereochemistry has produced a heightened awareness of the applications of pure enantiomers of agrochemicals. This review describes reports of the enantiomeric separation of commercial organophosphorus pesticides (OPs) and the applications of these methods to research on the enantioselectivity of the toxicity and environmental fate of these compounds. Chiral OPs can be analysed by high-performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE). These different separation techniques for OP enantiomers are briefly discussed, and their applications are presented.

  3. Gas Chromatography

    Science.gov (United States)

    Qian, Michael C.

    Gas chromatography (GC) has many applications in the analysis of food products. GC has been used for the determination of fatty acids, triglycerides, cholesterol, gases, water, alcohols, pesticides, flavor compounds, and many more. While GC has been used for other food components such as sugars, oligosaccharides, amino acids, peptides, and vitamins, these substances are more suited to analysis by high performance liquid chromatography. GC is ideally suited to the analysis of volatile substances that are thermally stable. Substances such as pesticides and flavor compounds that meet these criteria can be isolated from a food and directly injected into the GC. For compounds that are thermally unstable, too low in volatility, or yield poor chromatographic separation due to polarity, a derivatization step must be done before GC analysis. The two parts of the experiment described here include the analysis of alcohols that requires no derivatization step, and the analysis of fatty acids which requires derivatization. The experiments specify the use of capillary columns, but the first experiment includes conditions for a packed column.

  4. Germania-based, sol-gel hybrid organic-inorganic coatings for capillary microextraction and gas chromatography.

    Science.gov (United States)

    Fang, Li; Kulkarni, Sameer; Alhooshani, Khalid; Malik, Abdul

    2007-12-15

    Germania-based, sol-gel hybrid organic-inorganic coatings were developed for capillary microextraction and gas chromatography (GC). Being an isostructural analogue of SiO2, GeO2 is compatible with the silica network. Because of this similarity, germania-based materials possess great potential for being used in the areas of chromatographic separation and sample preparation. These possibilities, however, remain practically unexplored. To our knowledge, this is the first instance that a germania-based hybrid sol-gel material is used as a sorbent in analytical sample preparation or chromatographic separation. Tetramethoxygermane was used as a precursor to create a sol-gel network via hydrolytic polycondensation reactions performed within a fused-silica capillary. The growing sol-gel germania network was simultaneously reacted with an organic ligand that contained sol-gel-active sites in its chemical structure. Three different sol-gel-active ligands were used: (a) hydroxy-terminated poly(dimethylsiloxane), (b) hydroxy-terminated poly(dimethyldiphenylsiloxane), and (c) 3-aminopropyltrimethoxysilane. Sol-gel germania-coated capillaries of desired polarity and extraction selectivity were prepared by using an appropriately selected sol-gel-active ligand in the sol solution. These capillaries were further used to extract trace concentrations of polycyclic aromatic hydrocarbons, aldehydes, ketones, alcohols, phenols, and free fatty acids from aqueous samples. The extracted solutes were further analyzed by GC-FID. The new germania-based coatings showed excellent stability under harsh operation conditions involving extreme pH values, high temperatures, and aggressive solvents. Our preliminary results also indicate that sol-gel hybrid germania coatings have the potential to offer great analytical performance as GC stationary phases.

  5. Measurements of association constants between enantiomers and chiral selectors by capillary gas chromatography. Theoretical and practical considerations.

    Science.gov (United States)

    Lebed, Pablo J; Keunchkarian, Sonia; Osorio Grisales, Jaiver; Castells, Cecilia B

    2014-01-10

    The association constants of several volatile enantiomers with octakis(3-O-butanoyl-2,6-di-O-pentyl)-γ-cyclodextrin at temperatures between 50 and 100 °C were measured by gas-liquid chromatography using capillary columns coated with different amounts of chiral selector dissolved in polysiloxane OV-1701 and prepared with a precisely determined phase ratio. Simple expressions were deduced to estimate the apparent distribution constants from accurate hold-up and retention times along with that known phase ratio at each temperature. The enantiomer-chiral selector association constants were then calculated from the linear regression of the apparent constants as a function of the chiral selector concentration. One aim of this study consisted in discussing all the experimental uncertainties inherent in the determination of enantiomer/selector association constants with chiral analytes, and how these fundamental measurements can be performed precisely without resorting to the use of reference solutes.

  6. Gas chromatography

    Science.gov (United States)

    Guiochon, Georges; Guillemin, Claude L.

    1990-11-01

    Gas chromatography is a powerful separation technique for gas and vapor mixtures. Combining separation and on-line detection permits accurate quantitative analysis of complex mixtures, including traces of compounds down to parts per trillions in some particular cases. The importance of gas chromatography in quality control and process control in the chemical and drug industry, in environmental pollution investigations and in clinical analysis is critical. The principles of the technique are discussed, the main components of a gas chromatograph are described and some idea of the importance of the applications is given.

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

    Science.gov (United States)

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

    2008-01-01

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

  8. Quantification of fentanyl in serum by isotope dilution analysis using capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan); Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

    1998-06-01

    The quantitative determination of fentanyl (FT) in serum was examined by isotope dilution analysis using a capillary gas chromatograph equipped with a surface ionization detector. The separation of FT and its deuterated analogue, FT-{sup 2}H{sub 19}, was achieved within 15 min a column temperature of 260degC by using a 25 m column. Measurement of the samples prepared by the addition of a known amount of FT in the range of 0.2 to 40 ng/ml with 20 ng/ml of FT-{sup 2}H{sub 19} to human control serum allowed observation of a linear relationship between the peak area ratio and the added amount ratio. The correlation coefficient obtained by regression analysis was 0.999. The advantage of the present isotope dilution method was demonstrated by comparison with other FT analogues which substituted a propionyl group with an acetyl group or a phenethyl group with a benzyl group as the internal standard. The present method was used to determine the serum level of FT in surgical patients after i.v. administration. No endogenous compounds and concomitant drugs interfered with the detection of FT or FT-{sup 2}H{sub 19}. This method was considered to be useful for the pharmacokinetic study of FT in patients. (author)

  9. Separation performance of cucurbit[8]uril and its coordination complex with cadmium (II) in capillary gas chromatography.

    Science.gov (United States)

    Sun, Tao; Ji, Ningning; Qi, Meiling; Tao, Zhu; Fu, Ruonong

    2014-05-23

    Here we report the investigation of using cucurbit[8]uril (CB8) and its coordination complex with cadmium (II) (CB8-Cd) as stationary phases for capillary gas chromatography (GC). The prepared capillary columns of CB8 and CB8-Cd stationary phases achieved column efficiency of 2200plates/m and 1508plates/m, respectively, and showed weak polarity based on the measured McReynolds constants. Their separation performance was investigated by GC separation of mixtures of different types while a commercial column was used for comparison. The CB8 stationary phase achieved high resolution for a wide range of analytes from nonpolar to polar while the CB8-Cd stationary phase exhibited good separation mainly for nonpolar to weak polar analytes. The CB stationary phases differ from the commercial one in terms of retention behaviors and resolving ability due to their different molecular interactions with analytes. Moreover, energy effect on the retention of analytes on CB8 and CB8-Cd stationary phases was examined, showing that retention on CB8 column was determined mainly by enthalpy change for polar analytes and by both enthalpy change and entropy change for weak polar analytes whereas retention on CB8-Cd column was mainly controlled by entropy change. This work demonstrates the great potential of CB8 and CB8-Cd stationary phases as a new type of GC stationary phases in GC analysis.

  10. High-throughput capillary gas chromatography for the determination of polychlorinated biphenyls and fatty acid methyl esters in food samples.

    Science.gov (United States)

    Sandra, Pat; David, Frank

    2002-01-01

    High-throughput capillary gas chromatography (CGC) methods, developed during the Belgian 1999 "dioxin" food crisis, for the determination of the contaminating polychlorinated biphenyls (PCBs) and the fatty acid composition of the lipids are described. For PCB analysis, the fat obtained by ultrasonic extraction is fractionated by matrix solid-phase dispersion, and the PCBs are analyzed by CGC-electron capture detection on a 10-mL x 100-microm-i.d. HP-5MS column. Analytical conditions for the high-speed column are deduced from analyses on conventional CGC columns using the method translation software. The concept of retention time locking is implemented to facilitate the elucidation of the PCB markers. The fatty acid methyl esters (FAMEs) are prepared by the sodium methylate procedure on part of the ultrasonic extract followed by analysis on 10-mL x 100-microm-i.d. HP-WAX or BPX-70 capillary columns. By optimizing both the sample preparation and CGC analysis, the throughput is more than fifty PCB and FAME samples per day with the same robustness as conventional methods.

  11. Phenyl Functionalized Sol-gel Silica Sorbent for Capillary Microextraction and Chromia-Based Sol-gel Ucon Stationary Phase for Capillary Gas Chromatography

    Science.gov (United States)

    McLean, Michael M.

    The first chapter of this thesis presents an introduction to sol-gel methodology whose usefulness as a synthetic route will be demonstrated with two applications in chromatography. The first application involves the fabrication of a capillary micro-extraction (CME) device by coating a phenyl functionalized extracting phase on the inner surface of a fused silica capillary for analyte pre-concentration. The device was coupled on-line to a RP-HPLC system and practicality was demonstrated using allergens as target analytes. The allergens chosen as model analytes are typically found in fragrance products and food. Most of the 26 fragrance allergens that are monitored by various government authorities have a phenyl organic moiety (a strong chromophore), thus making them appropriate probes for exploring the extraction efficiency of the coating using a UV detector. The CME device showed ppt level limit of detection which makes it suitable for trace analyses of allergens and similar compounds in a variety of matrices. The second application explores the feasibility of using sol-gel derived chromia-based stationary phase in gas chromatographic columns. The organic moiety of the stationary phase was derived from Ucon 75-H-90,000 while the inorganic backbone was prepared using chromium(III) dichloride hydroxide - methacrylic acid - aqua complex, 40% in isopropanol/acetone . Usefulness of prepared chromia-based GC stationary phase was examined for petrochemical application. Promising results were obtained using aliphatic-aromatics, polyaromatic hydrocarbons, BTEX test mixture, cycloalkanes, branched alkanes and akylbenzenes. The column was able to perform without degradation despite being rinsed multiples times sequentially with the following solvents: dichloromethane, methanol, water and finally methanol again. Maximum theoretical plate number calculated is around 2,400 plates/m. The plate number clearly needs improvement but is a promising result for the newly explored

  12. Ultra-sensitive method for determination of ethanol in whole blood by headspace capillary gas chromatography with cryogenic oven trapping.

    Science.gov (United States)

    Watanabe-Suzuki, K; Seno, H; Ishii, A; Kumazawa, T; Suzuki, O

    1999-04-30

    We have established an ultra-sensitive method for determination of ethanol in whole blood by headspace capillary gas chromatography (GC) with cryogenic oven trapping. After heating a blood sample containing ethanol and isobutyl alcohol (internal standard, IS) in a 7.0-ml vial at 55 degrees C for 15 min, 5 ml of the headspace vapor was drawn into a glass syringe and injected into a GC port. All vapor was introduced into an Rtx-BAC2 wide-bore capillary column in the splitless mode at -60 degrees C oven temperature to trap entire analytes, and then the oven temperature was programmed up to 240 degrees C for GC measurements with flame ionization detection. The present method gave sharp peaks of ethanol and IS, and low background noise for whole blood samples. The mean partition into the gaseous phase for ethanol and IS was 3.06+/-0.733 and 8.33+/-2.19%, respectively. The calibration curves showed linearity in the range 0.02-5.0 microg/ml whole blood. The detection limit was estimated to be 0.01 microg/ml. The coefficients of intra-day and inter-day variation for spiked ethanol were 8.72 and 9.47%, respectively. Because of the extremely high sensitivity, we could measure low levels of endogenous ethanol in whole blood of subjects without drinking. The concentration of endogenous ethanol measured for 10 subjects under uncontrolled conditions varied from 0 to 0.377 microg/ml (mean, 0.180 microg/ml). Data on the diurnal changes of endogenous ethanol in whole blood of five subjects under strict food control are also presented; they are in accordance with the idea that endogenous blood ethanol is of enteric bacterial origin.

  13. Analysis of volatile organic compounds in water by dynamic stripping, thermal desorption, cryofocusing, and capillary gas chromatography (journal version)

    Energy Technology Data Exchange (ETDEWEB)

    Vandegrift, S.A.

    1988-01-01

    A dynamic headspace procedure developed for the determination of volatile organic compounds (VOCs) in water is described. The VOCs are purged from a water sample with an inert gas, transferring them to a tube packed with Tenax adsorbent. The adsorbent tube, or trap, is thermally desorbed, the analytes cryofocused, and subsequently transferred to a capillary column gas chromatograph.

  14. Detection and identification of volatile substances by headspace capillary gas chromatography to aid the diagnosis of acute poisoning.

    Science.gov (United States)

    Streete, P J; Ruprah, M; Ramsey, J D; Flanagan, R J

    1992-07-01

    Headspace gas chromatography with split flame-ionization-electron-capture detection is a simple method of screening for a wide range of volatile substances in biological fluids. A 60 m x 0.53 mm i.d. thick-film (5 microns) fused-silica capillary coated with SPB-1 (Supelchem) with split flame-ionization-electron-capture detection provides a valuable alternative to packed columns in this work. Most commonly abused compounds, including many with very low boiling-points such as bromochlorodifluoromethane (BCF), butane, dimethyl ether, FC 11, FC 12, isobutane and propane, can be retained and differentiated at an initial column temperature of 40 degrees C followed by programming to 200 degrees C. The total analysis time is 26 min. Retention and detector response data were generated for 244 compounds. Good peak shapes are obtained for polar analytes such as ethanol and injections of up to 0.30 cm3 of headspace can be performed with no discernable loss of efficiency. The sensitivity is thus at least as good as that attainable with packed columns. Of the commonly encountered compounds, only isobutane-methanol and paraldehyde-toluene are at all difficult to differentiate. Quantitative measurements can be performed either isothermally or by using the temperature programme.

  15. Capillary Separation: Micellar Electrokinetic Chromatography

    Science.gov (United States)

    Terabe, Shigeru

    2009-07-01

    Micellar electrokinetic chromatography (MEKC), a separation mode of capillary electrophoresis (CE), has enabled the separation of electrically neutral analytes. MEKC can be performed by adding an ionic micelle to the running solution of CE without modifying the instrument. Its separation principle is based on the differential migration of the ionic micelles and the bulk running buffer under electrophoresis conditions and on the interaction between the analyte and the micelle. Hence, MEKC's separation principle is similar to that of chromatography. MEKC is a useful technique particularly for the separation of small molecules, both neutral and charged, and yields high-efficiency separation in a short time with minimum amounts of sample and reagents. To improve the concentration sensitivity of detection, several on-line sample preconcentration techniques such as sweeping have been developed.

  16. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chlorinated pesticides in aquatic tissue by capillary-column gas chromatography with electron-capture detection

    Science.gov (United States)

    Leiker, Thomas J.; Madsen, J.E.; Deacon, J.R.; Foreman, W.T.

    1995-01-01

    A method for the determination of chlorinated organic compounds in aquatic tissue by dual capillary-column gas chromatography with electron-capture detection is described. Whole-body-fish or corbicula tissue is homogenized, Soxhlet extracted, lipid removed by gel permeation chromatography, and fractionated using alumina/silica adsorption chromatography. The extracts are analyzed by dissimilar capillary-column gas chromatography with electron-capture detection. The method reporting limits are 5 micrograms per kilogram (μg/kg) for chlorinated compounds, 50 μg/kg for polychlorinated biphenyls, and 200 μg/kg for toxaphene.

  17. Analysis of neutral nitromusks in incenses by capillary electrophoresis in organic solvents and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gotti, Roberto; Fiori, Jessica; Mancini, Francesca; Cavrini, Vanni

    2005-09-01

    Nitromusks used as fragrances in a variety of personal-care products, cleansers, and domestic deodorants, including incense sticks, are neutral nitro aromatic compounds; some of these have been reported as photosensitizers. In this work, their analysis was performed by capillary electrophoresis (CE) in a methanol-based background electrolyte (BGE). In particular, a 10 mM solution of citric acid in methanol was used; under these conditions the strong suppression of the electroosmotic flow favored the use of negatively charged surfactants as additives for the anodic migration of the studied analytes. To this end, sodium taurodeoxycholate (TDC) was supplemented at high concentration (190 mM) to the organic background electrolyte (BGE), showing strong indication of the ability to give micelle-like aggregates. Since nitromusks are characterized by the presence of a nitroaromatic ring with low charge density, their association with TDC aggregates can be ascribed to donor-acceptor interactions. Separation of musk xylene, musk ketone, and the banned musk moskene and musk ambrette was obtained under full nonaqueous BGE; the addition of relatively small water percentages (15% v/v) was found to be useful in improving the separation of pairs of adjacent peaks. Under optimized conditions (190 mM sodium TDC in methanol-water, 85-15 v/v containing citric acid 10 mM) the system was applied to the analysis of nitromusks in incense sticks extracted with methanol. The results were compared with those obtained by the analysis of the same samples using gas chromatography with mass detector. The expected different selectivity of separation obtained using the two techniques can be useful in the unambiguous determination of the analytes; furthermore, a substantial accord of the preliminary quantitative results achieved with the two methods was assumed as the confirmation of the potential reliability of CE performed with high percentage of organic solvent.

  18. Gas-Filled Capillary Model

    Science.gov (United States)

    Steinhauer, L. C.; Kimura, W. D.

    2006-11-01

    We have developed a 1-D, quasi-steady-state numerical model for a gas-filled capillary discharge that is designed to aid in selecting the optimum capillary radius in order to guide a laser beam with the required intensity through the capillary. The model also includes the option for an external solenoid B-field around the capillary, which increases the depth of the parabolic density channel in the capillary, thereby allowing for propagation of smaller laser beam waists. The model has been used to select the parameters for gas-filled capillaries to be utilized during the Staged Electron Laser Acceleration — Laser Wakefield (STELLA-LW) experiment.

  19. Advances in Capillary Chromatography%毛细管色谱的进展

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Capillary columns are used in both capillary liquid chromatography and capillary electrochromatography. The design for capillary liquid chromatography is discussed in comparison with capillary gas chromatography. The difference of diffusion coefficient in gas and liquid phase is a key role. The study for obtaining a high performance capillary liquid chromatography is discussed. Capillary electrochromatography is recently interesting for its instinct ability to realize a high performance chromatography. Capillary electrochromatography with and without pressurized flow is reviewed briefly. Instrumentation for capillary electrochromatography with pressurized flow is discussed. The port of splitting, and gradient elution of both solution and potential are described. The new findings of both the variation of column resistance and capacity factor according to the value of applied electric voltage are also discussed.

  20. Cellular uptake and retention measurements of alkylphosphocholines in the SK-BR-3 breast cancer and Molt-4 leukemia cell line using capillary gas chromatography.

    Science.gov (United States)

    Brochez, V; Van Heuverswyn, D; Diniz, J A; De Potter, C R; Van den Eeckhout, E G

    1999-05-01

    The determination of cellular content of octadecylphosphocholine (D-19391) and hexadecylphosphocholine (HePC, D-18506), two anticancer agents of the alkylphosphocholine group, using capillary gas chromatography is described. The compounds' cytotoxicity was first determined by the MTT [3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyltetrazolium] assay, being indicative for the concentration used in the uptake and retention measurements. D-19391 was added to the SK-BR-3 breast cancer cell line and HePC to the Molt-4 leukemia cell line in concentrations of, respectively, 18.6 and 15.0 microM, during a 36-h incubation period at 37 degrees C, 5% CO2. HePC uptake in the leukemia cells was followed by a 24-h reversibility test in drug-free medium. Subsequently, sample clean-up was performed on a weak cation-exchange column. For the quantitative analysis, HePC was used as internal standard for the D-19391 measurements and vice versa. Derivatization of the samples with trimethylsilylbromide was followed by capillary gas chromatographic analysis. From these data we conclude that our uptake results are quite similar with those of a previous study of HePC cellular uptake in the more resistant Caco-2T colon cancer cell line. Without having investigated the mechanism that underlies the cellular uptake results obtained, our study points to no direct correlation between the compounds' cellular uptake and their cytotoxic effects.

  1. Validation of a method for the determination of sterols and triterpenes in the aerial part of Justicia anselliana (Nees) T. Anders by capillary gas chromatography.

    Science.gov (United States)

    Kpoviéssi, Dossou Sika Salomé; Gbaguidi, Fernand; Gbénou, Joachim; Accrombessi, Georges; Moudachirou, Mansourou; Rozet, Eric; Hubert, Philippe; Quetin-Leclercq, Joëlle

    2008-12-01

    An accurate and sensitive method, combining soxhlet extraction, solid phase-extraction and capillary gas chromatography is described for the quantitative determination of one triterpene (lupeol) and three sterols (stigmasterol, campesterol and beta-sitosterol) and the detection of another triterpene (alpha-amyrin) from the aerial part of Justicia anselliana. This is the first method allowing the quantification of sterols and triterpenes in this plant. It has been fully validated in order to be able to compare the sterol and triterpene composition of different samples of J. anselliana and therefore help to explain the allelopathic activity due to these compounds. This method showed that the aerial part of J. anselliana contained (292+/-2)mg/kg of lupeol, (206+/-1)mg/kg of stigmasterol, (266+/-2)mg/kg of campesterol and (184+/-9)mg/kg of beta-sitosterol.

  2. Speciation of mercury in human whole blood by capillary gas chromatography with a microwave-induced plasma emission detector system following complexometric extraction and butylation.

    Science.gov (United States)

    Bulska, E; Emteborg, H; Baxter, D C; Frech, W; Ellingsen, D; Thomassen, Y

    1992-03-01

    Methyl- and inorganic mercury were extracted from human whole blood samples, as their diethyldithiocarbamate complexes, into toluene and butylated by using a Grignard reagent. The mercury species were then separated by gas chromatography (on a 12 m non-polar DB-1 capillary column) and detected by a microwave-induced plasma atomic emission spectrometric (GC-MPD) system. The accuracy and precision of the proposed method were established by the analysis of Seronorm lyophilized human whole blood standards for methyl- and inorganic mercury. No statistical difference (t-test) between the sum of these two species determined by the GC-MPD based method and the recommended total mercury concentrations in the Seronorm samples was observed. Results for the determination of methyl- and inorganic mercury in 60 controls and 90 previously occupationally exposed (to inorganic mercury) workers are presented to illustrate the practical utility of the proposed method. No significantly elevated inorganic mercury concentrations between the two groups were evident.

  3. Quantitative extraction of methylgermanium species at trace levels and determination by on-column capillary gas chromatography with flame photometric detector

    Institute of Scientific and Technical Information of China (English)

    1998-01-01

    A solvent extraction procedure for the quantitativeextraction of trace levels of methylgermanium species as theirchloride complex has been developed and the extract was determinedby an on-column capillary gas chromatography with a lab-modifiedflame phorometric detector(FPD) using quartz surface-inducedgermanium emission after pentylation with Grignard reaction. Theextracted percentages for TMGe, DMGe and MMGe in a 100-ml 9mol/LHCl aqueous solution by a single extraction with 1 ml hexane are86.6%, 87.4% and 96.2%, respectively. The precision for overallprocedure range from 3.9% to 7.5%. The extraction was found to beindependent of the initial concentration of methylgermanium speciesin the aqueous phase, which typically varied from 0.1 to 10 μg. This method is suitable for most types of environmental samples and, are superior to all hydride generation coupled spectrometric andspectrophotometric methods in terms of selectivity and toleranceability to interference.

  4. Analysis of polycyclic aromatic hydrocarbons I. Determination by gas chromatography with glass and fused silica capillary columns; Analisis de Hidrocarburos aromaticos policiclicos. I. Determinacion por cromatografia de gases con columnas capilares de vidrio de silice fundida

    Energy Technology Data Exchange (ETDEWEB)

    Perez, M. M.; Gonzalez, D.

    1987-07-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column. The limitations and the advantages of the procedure are discussed in terms of separation efficiency, sensitivity and precision. (Author) 17 refs.

  5. Application of capillary gas chromatography to the study of hydrolysis of the nerve agent VX in rat plasma.

    Science.gov (United States)

    Bonierbale, E; Debordes, L; Coppet, L

    1997-01-24

    We present here a gas chromatography technique allowing the detection and quantification of VX [O-ethyl S-(2-diisopropylaminoethyl)methylphosphonothiolate] as well as its P-S bond hydrolysis product diisopropylaminoethanethiol directly from spiked rat plasma. This technique was applied to study VX hydrolysis in rat plasma. We observed that 53 +/- 4% of 374 microM VX disappeared from spiked plasma after 2 h. VX disappearance was mainly related to enzymatic cleavage of the P-S bond (Km = 2.5 mM and Vmax = 13.3 nmol min-1 ml-1 of rat plasma). The activity was totally inhibited by 1 mM Hg2+ and was also inhibited by metal chelators.

  6. Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan). Faculty of Pharmacy and Pharmaceutical Sciences; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

    1998-07-01

    Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT-{sup 2}H{sub 19}), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT-{sup 2}H{sub 10}). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

  7. Regolith and Environment Science and Oxygen and Lunar Volatile Extraction (RESOLVE): Lunar Advanced Volatile Analysis (LAVA) Capillary Fluid Dynamic Restriction Effects on Gas Chromatography

    Science.gov (United States)

    Gonzalez, Marianne; Quinn, Jacqueline; Captain, Janine; Santiago-Bond, Josephine; Starr, Stanley

    2015-01-01

    The Resource Prospector (RP) mission with the Regolith and Environment Science and Oxygen Lunar Volatile Extraction (RESOLVE) payload aims to show the presence of water in lunar regolith, and establish a proving ground for NASAs mission to Mars. One of the analysis is performed by the Lunar Advanced Volatiles Analysis (LAVA) subsystem, which consists of a fluid network that facilitates the transport of volatile samples to a gas chromatograph and mass spectrometer (GC-MS) instrument. The understanding of fluid dynamics directed from the GC to the MS is important due to the influence of flow rates and pressures that affect the accuracy of and prevent the damage to the overall GC-MS instrument. The micro-scale capillary fluid network within the GC alone has various lengths and inner-diameters; therefore, determination of pressure differentials and flow rates are difficult to model computationally, with additional complexity from the vacuum conditions in space and lack of a lunar atmosphere. A series of tests were performed on an experimental set-up of the system where the inner diameters of the GC transfer line connecting to the MS were varied. The effect on chromatography readings were also studied by applying these lines onto a GC instrument. It was found that a smaller inner diameter transfer line resulted in a lower flow rate, as well as a lower pressure differential across the thermal conductivity detector (TCD) unit of the GC and a negligible pressure drop across the mock-up capillary column. The chromatography was affected with longer retention times and broader peak integrations. It was concluded that a 0.050 mm inner diameter line still proved most suitable for the systems flow rate preferences. In addition, it was evident that this small transfer line portrayed some expense to GC signal characteristics and the wait time for steady-state operation.

  8. Rapid confirmation of enzyme multiplied immunoassay technique (EMIT) cocaine positive urine samples by capillary gas-liquid chromatography/nitrogen phosphorus detection (GLC/NPD).

    Science.gov (United States)

    Verebey, K; DePace, A

    1989-01-01

    A rapid gas-liquid chromatographic (GLC) method was developed for the confirmation of benzoylecgonine (BE) positive urine samples screened by the enzyme multiplied immunoassay technique (EMIT) assay. The procedure is performed by solvent extraction of BE from 0.1 or 0.2 mL of urine, followed by an aqueous wash of the solvent and evaporation. The dried residue was derivatized with 50 microL of pentafluoropropionic anhydride and 25 microL of pentafluoropropropanol at 90 degrees C for 15 min. The derivatizing reagents were evaporated to dryness, and the derivatized BE, and cocaine if present, were reconstituted and injected into the gas chromatograph. The column was a 15-m by 0.2-mm fused silica capillary column, coated with 0.25 micron of DB-1, terminating in a nitrogen phosphorus detector (NPD). Cocaine and the pentafluoro BE derivatives retention times were 3.2 and 2.6 min, respectively. Nalorphine was used as reference or internal standard with a retention time of 4.78 min. The complete procedure can be performed in approximately 1.5 h. The EMIT cutoff between positive and negative urine samples is 300 ng/mL of BE. The lower limit of sensitivity of this method is 25 ng of BE extracted from urine. Validation studies resulted in confirmation of 101 out of 121 EMIT cocaine positive urine samples that could not be confirmed by thin-layer chromatography (TLC). This represents 84% confirmation efficiency.

  9. Capillaries modified by noncovalent anionic polymer adsorption for capillary zone electrophoresis, micellar electrokinetic capillary chromatography and capillary electrophoresis mass spectrometry

    DEFF Research Database (Denmark)

    Bendahl, L; Hansen, S H; Gammelgaard, Bente

    2001-01-01

    A simple coating procedure for generation of a high and pH-independent electroosmotic flow in capillary zone electrophoresis (CZE) and micellar electrokinetic capillary chromatography (MEKC) is described. The bilayer coating was formed by noncovalent adsorption of the ionic polymers Polybrene...

  10. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of organochlorine pesticides and polychlorinated biphenyls in bottom sediment by dual capillary-column gas chromatography with electron-capture detection

    Science.gov (United States)

    Foreman, William T.; Connor, Brooke F.; Furlong, Edward T.; Vaught, Deborah G.; Merten, Leslie M.

    1995-01-01

    A method for the determination of 30 individual organochlorine pesticides, total toxaphene, and total polychlorinated biphenyls (PCBs) in bottom sediment is described. The method isolates the pesticides and PCBs by solvent extraction with dichlorobenzene, removes inorganic sulfur, large naturally occurring molecules, and other unwanted interferences by gel permeation chromatography, and further cleans up and class fractionates the extract using adsorption chromatography. The com- pounds then are instrumentally determined using dual capillary-column gas chromatography with electron-capture detection. Reporting limits range from 1 to 5 micrograms per kilogram for 30 individual pesticides, 50 micrograms per kilogram for total PCBs, and 200 micrograms per kilogram for total toxaphene. The method also is designed to allow the simultaneous isolation of 79 other semivolatile organic compounds from the sediment, which are separately quantified using gas chromatography with mass spectrometric detection. The method was developed in support of the U.S. Geological Survey's National Water-Quality Assessment program.

  11. Metabolic Profiling with Gas Chromatography-Mass Spectrometry and Capillary Electrophoresis-Mass Spectrometry Reveals the Carbon-Nitrogen Status of Tobacco Leaves Across Different Planting Areas.

    Science.gov (United States)

    Zhao, Jieyu; Zhao, Yanni; Hu, Chunxiu; Zhao, Chunxia; Zhang, Junjie; Li, Lili; Zeng, Jun; Peng, Xiaojun; Lu, Xin; Xu, Guowang

    2016-02-05

    The interaction between carbon (C) and nitrogen (N) metabolism can reflect plant growth status and environmental factors. Little is known regarding the connections between C-N metabolism and growing regions under field conditions. To comprehensively investigate the relationship in mature tobacco leaves, we established metabolomics approaches based on gas chromatography-mass spectrometry (GC-MS) and capillary electrophoresis-time-of-flight-mass spectrometry (CE-TOF-MS). Approximately 240 polar metabolites were determined. Multivariate statistical analysis revealed that the growing region greatly influenced the metabolic profiles of tobacco leaves. A metabolic correlation network and related pathway maps were used to reveal the global overview of the alteration of C-N metabolism across three typical regions. In Yunnan, sugars and tricarboxylic acid (TCA) cycle intermediates were closely correlated with amino acid pools. Henan tobacco leaves showed positive correlation between the pentose phosphate pathway (PPP) intermediates and C-rich secondary metabolism. In Guizhou, the proline and asparagine had significant links with TCA cycle intermediates and urea cycle, and antioxidant accumulation was observed in response to drought. These results demonstrate that combined analytical approaches have great potential to detect polar metabolites and provide information on C-N metabolism related to planting regional characteristics.

  12. Quantitation of l-alpha-acetylmethadol and its metabolites in human serum by capillary gas-liquid chromatography and nitrogen detection.

    Science.gov (United States)

    Verebey, K; DePace, A; Mulé, S J

    1985-10-11

    A procedure is described for the simultaneous measurement of l-alpha-acetylmethadol and its two pharmacologically active metabolites: noracetylmethadol and dinoracetylmethadol. In the method an intramolecular conversion reaction of the two metabolites to their amide configuration is utilized. The reaction is performed while the metabolites are still in the serum. Following solvent extraction the samples are analyzed by capillary gas-liquid chromatography coupled with nitrogen detection. Quantitation is achieved by internal standardization. The lower limit of sensitivity is 5 ng/ml in serum. Absolute sensitivity is 0.1 ng for all three compounds. The advantages over other procedures are: speed due to the single extraction step; increased recovery of noracetylmethadol and dinoracetylmethadol due to decreased polarity of the amides; greater stability of the metabolites in the amide configuration; better chromatographic quantitation and separation because detector response for the amides is greater than it is for the original configuration of the metabolites and the area of the chromatographic tracing is free of interfering substances.

  13. Determination of Wastewater Compounds in Whole Water by Continuous Liquid-Liquid Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.

    2006-01-01

    A method for the determination of 69 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals on aquatic organisms in wastewater. This method also is useful for evaluating the effects of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are indicators of wastewater or have endocrine-disrupting potential. These compounds include the alkylphenol ethoxylate nonionic surfactants, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Wastewater compounds in whole-water samples were extracted using continuous liquid-liquid extractors and methylene chloride solvent, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 0.5 microgram per liter averaged 72 percent ? 8 percent relative standard deviation. The concentration of 21 compounds is always reported as estimated because method recovery was less than 60 percent, variability was greater than 25 percent relative standard deviation, or standard reference compounds were prepared from technical mixtures. Initial method detection limits averaged 0.18 microgram per liter. Samples were preserved by adding 60 grams of sodium chloride and stored at 4 degrees Celsius. The laboratory established a sample holding-time limit prior to sample extraction of 14 days from the date of collection.

  14. Organotin speciation in environmental matrices by automated on-line hydride generation-programmed temperature vaporization-capillary gas chromatography-mass spectrometry detection.

    Science.gov (United States)

    Serra, H; Nogueira, J M F

    2005-11-11

    In the present contribution, a new automated on-line hydride generation methodology was developed for dibutyltin and tributyltin speciation at the trace level, using a programmable temperature-vaporizing inlet followed by capillary gas chromatography coupled to mass spectrometry in the selected ion-monitoring mode acquisition (PTV-GC/MS(SIM)). The methodology involves a sequence defined by two running methods, the first one configured for hydride generation with sodium tetrahydroborate as derivatising agent and the second configured for speciation purposes, using a conventional autosampler and data acquisition controlled by the instrument's software. From the method-development experiments, it had been established that injector configuration has a great effect on the speciation of the actual methodology, particularly, the initial inlet temperature (-20 degrees C; He: 150 ml/min), injection volume (2 microl) and solvent characteristics using the solvent venting mode. Under optimized conditions, a remarkable instrumental performance including very good precision (RSD CRM 462, Nr. 330 dibutyltin: 68+/-12 ng/g; tributyltin: 54+/-15 ng/g on dry mass basis), using liquid-liquid extraction (LLE) and solid-phase extraction (SPE) sample enrichment and multiple injections (2 x 5 microl) for sensitivity enhancement. The methodology evidenced high reproducibility, is easy to work-up, sensitive and showed to be a suitable alternative to replace the currently dedicated analytical systems for organotin speciation in environmental matrices at the trace level.

  15. 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.

  16. Determination of Labeled Fatty Acids Content in Milk Products, Infant Formula, and Adult/Pediatric Nutritional Formula by Capillary Gas Chromatography: Collaborative Study, Final Action 2012.13.

    Science.gov (United States)

    Golay, Pierre-Alain; Moulin, Julie

    2016-01-01

    A collaborative study was conducted on AOAC First Action Method 2012.13 "Determination of Labeled Fatty Acids Content in Milk Products and Infant Formula by Capillary Gas Chromatography," which is based on an initial International Organization for Standardization (ISO)-International Dairy Federation (IDF) New Work Item that has been moved forward to ISO 16958:2015|IDF 231:2015 in November 2015. It was decided to merge the two activities after the agreement signed between ISO and AOAC in June 2012 to develop common standards and to avoid duplicate work. The collaborative study was performed after having provided highly satisfactory single-laboratory validation results [Golay, P.A., & Dong, Y. (2015) J. AOAC Int. 98, 1679-1696] that exceeded the performance criteria defined in AOAC Standard Method Performance Requirement (SMPR(®)) 2012.011 (September 29, 2012) on 12 products selected by the AOAC Stakeholder Panel on Infant Formula (SPIFAN). After a qualification period of 1 month, 18 laboratories participated in the fatty acids analysis of 12 different samples in duplicate. Six samples were selected to meet AOAC SPIFAN requirements (i.e., infant formula and adult nutritionals in powder and liquid formats), and the other Six samples were selected to meet ISO-IDF requirements (i.e., dairy products such as milk powder, liquid milk, cream, butter, infant formula with milk, and cheese). The fatty acids were analyzed directly in all samples without preliminary fat extraction, except in one sample (cheese). Powdered samples were analyzed after dissolution (i.e., reconstitution) in water, whereas liquid samples (or extracted fat) were analyzed directly. After addition of the internal standards solution [C11:0 fatty acid methyl ester (FAME) and C13:0 triacylglycerols (TAG)] to the samples, fatty acids attached to lipids were transformed into FAMEs by direct transesterification using methanolic sodium methoxide. FAMEs were separated using highly polar capillary GLC and were

  17. Separation performance of cucurbit[7]uril in ionic liquid-based sol-gel coating as stationary phase for capillary gas chromatography.

    Science.gov (United States)

    Wang, Xiaogang; Qi, Meiling; Fu, Ruonong

    2014-12-05

    Here we report the separation performance of a new stationary phase of cucurbit[7]uril (CB7) incorporated into an ionic liquid-based sol-gel coating (CB7-SG) for capillary gas chromatography (GC). The CB7-SG stationary phase showed an average polarity of 455, suggesting its polar nature. Abraham system constants revealed that its major interactions with analytes include H-bond basicity (a), dipole-dipole (s) and dispersive (l) interactions. The CB7-SG stationary phase achieved baseline separation for a wide range of analytes with symmetrical peak shapes and showed advantages over the conventional polar stationary phase that failed to resolve some critical analytes. Also, it exhibited different retention behaviors from the conventional stationary phase in terms of retention times and elution order. Most interestingly, in contrast to the conventional polar phase, the CB7-SG stationary phase exhibited longer retentions for analytes of lower polarity but relatively comparable retentions for polar analytes such as alcohols and phenols. The high resolving ability and unique retention behaviors of the CB7-SG stationary phase may stem from the comprehensive interactions of the aforementioned interactions and shape selectivity. Moreover, the CB7-SG column showed good peak shapes for analytes prone to peak tailing, good thermal stability up to 280°C and separation repeatability with RSD values in the range of 0.01-0.11% for intra-day, 0.04-0.41% for inter-day and 2.5-6.0% for column-to-column, respectively. As demonstrated, the proposed coating method can simultaneously address the solubility problem with CBs for the intended purpose and achieve outstanding GC separation performance.

  18. Environmental screening of acidic compounds based on capillary zone electrophoresis/laser-induced fluorescence detection with identification by gas chromatography/mass spectrometry and gas chromatography/high-resolution mass spectrometry.

    Science.gov (United States)

    Brumley, W C; Grange, A H; Kelliher, V; Patterson, D B; Montcalm, A; Glassman, J; Farley, J W

    2000-01-01

    This paper describes the application of capillary zone electrophoresis/laser-induced fluorescence detection (CZE/LIF) to the discovery of acidic compounds in environmental matrixes or the screening of extracts for acidic components. Published studies indicate that coal-derived materials contain a significant fraction of acidic compounds relative to materials derived from petroleum and shales. Such compounds may be useful as marker compounds for site assessment and source apportionment issues, and their identification may be important in toxicological and other health issues. We used deep-UV light from the frequency-doubled Ar ion laser at 244 and 257 nm to study extracts of samples. The CZE/LIF technique possesses good sensitivity and therefore overcomes one of the limitations of CZE with UV detection. The present work depends on high pressure/temperature solvent extraction of polynuclear aromatic hydrocarbon (PNA)-contaminated soil, followed by separation using CZE. The anionic analytes were separated by using borate or phosphate buffer (pH 9.2-12.3) after a chemical class separation. Samples were also characterized by gas chromatography/mass spectrometry (GC/MS) using full scans at low resolution, and elemental compositions were determined unequivocally by GC/high-resolution MS (GC/HRMS) using mass peak profiling (MPP). The similarity of low-resolution electron ionization mass spectra for a standard, 1-hydroxypyrene, and for a series of compounds in a contaminated-soil extract suggested that several types of phenolic and hydroxy-PNAs were present, including hydroxylated derivatives of fluorenes, fluoranthenes, and pyrenes. GC/HRMS using MPP confirmed the elemental compositions of the hydroxyfluorenes and hydroxypyrenes (and presumably hydroxyfluoranthenes) as [C13H10O] and [C16H10O], respectively. A new version of the MPP software was written for the Finnigan-MAT 900S-Trap and was similar to that developed previously for the VG 250SE. Inclusion of a calibration

  19. Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

    2006-01-01

    A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

  20. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  1. Quantitative determination of N-[trans-2-(dimethylamino)-cyclopentyl]-N-(3',4'-dichlorophenyl)propan amide, its 2H5-labeled analogue and their N-dealkylated metabolites in dog serum by capillary gas chromatography-mass spectrometry.

    Science.gov (United States)

    Theis, D L; Halstead, G W; Capponi, V J; Roach, B L; Robins, R H

    1986-03-07

    This paper describes the development of a capillary gas chromatographic--mass spectrometric method for the determination of N-[trans-2-(dimethylamino)cyclopentyl]-N-(3',4'-dichlorophenyl)propan amide and its metabolites in serum. The method utilizes an automated sample preparation whereby drug, metabolites and internal standard are extracted from polar serum components by adsorption chromatography onto an XAD-type resin. The N-demethylated metabolites are derivatized by acetylation prior to chromatography. Detection is by mass spectrometry with chemical ionization. This method was utilized to determine levels of unlabeled and pentadeuterated drug and their respective metabolites in canine serum after oral co-administration. No significant kinetic isotope effects were observed for either absorption or metabolism.

  2. Determination of Organic Acids in Forest Litters by a Capillary Gas Chromatography%毛细管气相色谱法测定森林凋落物中的有机酸

    Institute of Scientific and Technical Information of China (English)

    宋金凤; 刘永; 崔晓阳

    2004-01-01

    Organic acids in forest litters play important role in forests and forest soils. Based on the fresh litter materials of Fraxinus mandshurica and Larix olgensis forest in northeast China, a capillary gas chromatography procedure was established to determine organic acids in forest litters. Organic acids in forest litter were lixiviated and derived into corresponding esters with 7:100 (v:v) H2SO4:CH3OH at 60℃, extracted in CHCl3 and analyzed by capillary gas chromatography (GC) system. It resulted that, the method reported in this paper to separate, identify and determine organic acids in forest litter by GC was reliable and easy to operate. The disposal of sample was convenient, and the esterification with CH3 OH occurred while extracting organic acids with the same reagent, so volatilization loss of low-molecular-weight organic acids and oxidation of unsaturated fatty acids were avoided in course of condensation and esterification at high temperature when the conventional method to determine organic acids was used. Good selectivity was obtained, low-molecular-weight organic acids and high fatty acids could be determined simultaneously and accurately. Recovery of thirteen organic acids detected by adding standard samples ranged from 84.66% to 97.45% with relative standard deviation from 1.53% to 8.54%, and lowest detection limit of different organic acids was in range of 0.39 to 6.46 ng. The method could be used to determine organic acids in forest litters with satisfactory results.

  3. Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    Science.gov (United States)

    Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

    1992-01-01

    A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

  4. High-throughput analysis of bergamot essential oil by fast solid-phase microextraction-capillary gas chromatography-flame ionization detection.

    Science.gov (United States)

    Tranchida, Peter Quinto; Presti, Maria Lo; Costa, Rosaria; Dugo, Paola; Dugo, Giovanni; Mondello, Luigi

    2006-01-20

    The advantages of using a narrow-bore column in headspace solid-phase microextraction-gas chromatographic (HS-SPME-GC) analysis are investigated. An automated rapid HS-SPME-GC method for the determination of volatile compounds in a complex sample (bergamot essential oil) was developed. A low-capacity (7 microm) SPME fibre was employed, enabling a short equilibration time (15 min). The absorbed volatile compounds were then separated in 12.5 min on a 10 m x 0.1 mm I.D. capillary. The fast GC method was characterized by relatively moderate GC parameters (head pressure: 173 kPa; temperature program rate: 12 degrees C/min). The employment of the low-capacity fibre also suited the reduced sample capacity of the capillary employed, hence column overloading was avoided. Analytical repeatibility was determined in terms of retention times (maximum RSD: 0.32%) and peak areas (maximum RSD: 9.80%). The results obtained were compared to those derived from a conventional HS-SPME-GC (a 30 microm SPME fibre and 0.25 mm I.D. capillary were used) application on the same sample. In this respect, a great reduction of analytical time was obtained both with regard to the conventional SPME equilibration and GC run times, which both required 50 min. Peak resolution was altogether comparable in both applications. Although a slight loss in terms of sensitivity was observed in the rapid approach (generally within the 25-50% range), this did not impair the detection of all peaks of interest. Finally, the selectivities of the 30 and 7 microm fibres were evaluated and, as expected, these were in good agreement.

  5. MEMS Liquid and Gas Chromatography for Miniaturized Planetary In Situ Instruments

    Science.gov (United States)

    Kidd, R. D.; Bae, B.; Willis, P. A.; Noell, A. C.; Scianmarello, N.; Tai, Y.-C.

    2016-10-01

    Micro-Electro-Mechanical Systems (MEMS) technology to reduce the size, mass and power of the three classical chromatographic technologies: gas chromatography (GC), capillary electrophoresis (CE) and high performance liquid chromatography (HPLC).

  6. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

    Science.gov (United States)

    Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

    1995-01-01

    A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time.

  7. Capillary gas-chromatographic determination of urinary homovanillic acid and vanillylmandelic acid.

    Science.gov (United States)

    Tuchman, M; Crippin, P J; Krivit, W

    1983-05-01

    This relatively simple, rapid method for quantification of homovanillic acid (HVA) and vanillylmandelic acid (VMA) involves solvent extraction and capillary gas chromatography. With use of this extraction method, the overall analytical recovery from an aqueous solution is 92.5% for HVA and 79.2% for VMA. 3,4-Dihydroxybenzoic acid is the internal standard. Minimal detectable quantities with this method are less than 1 mg/g of creatinine. Capillary gas chromatography produces a chromatogram that is superior to that of packed-column gas chromatography. We also report quantitative results for urinary HVA and VMA in neuroblastoma patients and in normal individuals, demonstrating the diagnostic value of this method.

  8. Evaluation of monoterpenic biogenic volatile organic compounds in ambient air around Eucalyptus globulus, Pinus halepensis and Cedrus atlantica trees growing in Algiers city area by chiral and achiral capillary gas chromatography

    Science.gov (United States)

    Yassaa, Noureddine; Youcef Meklati, Brahim; Cecinato, Angelo

    The monoterpenic biogenic volatile organic compounds (BVOCs) in ambient air around either Eucalyptus globulus, Cedrus atlantica and Pinus halepensis trees from El- Hamma Botanical Garden (Algiers) or from Pinus halepensis trees field located in Bab-Ezzouar (suburb of Algiers) was qualitatively and semi-quantitatively evaluated. The sampling was carried out in ambient air by adsorption through an activated charcoal cartridge followed by the carbon disulfide extraction. The solution was subjected to high-resolution gas chromatography (HRGC) analysis in programmed temperature. The identification of the components was established by the means of retention Kovàts indexes. The use of a β-cyclodextrin chiral capillary column allowed a good separation of monoterpenic enantiomers released in the atmosphere. The enantiomeric ratio provided a good insight into the enantiomeric compound preferentially emitted by plants.

  9. Principles of Micellar Electrokinetic Capillary Chromatography Applied in Pharmaceutical Analysis

    Directory of Open Access Journals (Sweden)

    Árpád Gyéresi

    2013-02-01

    Full Text Available Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve. Micellar electrokinetic capillary chromatography, a hybrid method that combines chromatographic and electrophoretic separation principles, extends the applicability of capillary electrophoretic methods to neutral analytes. In micellar electrokinetic capillary chromatography, surfactants are added to the buffer solution in concentration above their critical micellar concentrations, consequently micelles are formed; micelles that undergo electrophoretic migration like any other charged particle. The separation is based on the differential partitioning of an analyte between the two-phase system: the mobile aqueous phase and micellar pseudostationary phase. The present paper aims to summarize the basic aspects regarding separation principles and practical applications of micellar electrokinetic capillary chromatography, with particular attention to those relevant in pharmaceutical analysis.

  10. Principles of micellar electrokinetic capillary chromatography applied in pharmaceutical analysis.

    Science.gov (United States)

    Hancu, Gabriel; Simon, Brigitta; Rusu, Aura; Mircia, Eleonora; Gyéresi, Arpád

    2013-01-01

    Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve. Micellar electrokinetic capillary chromatography, a hybrid method that combines chromatographic and electrophoretic separation principles, extends the applicability of capillary electrophoretic methods to neutral analytes. In micellar electrokinetic capillary chromatography, surfactants are added to the buffer solution in concentration above their critical micellar concentrations, consequently micelles are formed; micelles that undergo electrophoretic migration like any other charged particle. The separation is based on the differential partitioning of an analyte between the two-phase system: the mobile aqueous phase and micellar pseudostationary phase. The present paper aims to summarize the basic aspects regarding separation principles and practical applications of micellar electrokinetic capillary chromatography, with particular attention to those relevant in pharmaceutical analysis.

  11. Capillary supercritical fluid chromatography-mass spectrometry (SFC-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Kalinoski, H.T.; Udseth, H.R.; Chess, E.K.; Smith, R.D.

    1986-10-01

    The physical and chemical characteristics of supercritical fluids have prompted the development of supercritical fluid chromatography (SFC) for the analysis of labile and less volatile compounds. High resolution chromatographic separations with efficiencies approaching those of gas chromatography and high speed analyses are possible in capillary SFC using pressure programming methods and narrow bore columns. Further refinement of the SFC-mass spectrometry interface (SFC-MS) provides the basis for extension to more polar fluid systems with greater solvating power and the selectivity and sensitivity of mass spectrometric detection. The use of polar modified fluids has been facilitated by advances in understanding of supercritical fluid phase behavior. Fluid mixtures have been prepared for analysis of more polar, higher molecular weight analytes, that allow mild chromatographic temperatures and allow full exploitation of selectivity offered through control of fluid pressure (i.e., density). Continuing development of the SFC-MS interface has led to designs which can be near routinely applied with fluids such as CO/sub 2/, and providing enhanced transport of truly nonvolatile compounds to the mass spectrometer ionization regions. These advances also include an SFC interface to a high resolution, dual electric magnetic sector instrument, allowing supercritical fluid solvents to be explited for on-line extraction-mass spectrometry for characterization of complex, often otherwise intractable, materials. 26 refs., 5 figs., 1 tab.

  12. [Recent advances in capillary scale ion chromatography technology].

    Science.gov (United States)

    Yang, Bingcheng; Diao, Xuefang

    2012-04-01

    Ion chromatography (IC) has been a well-established technique for the analysis of ionic samples. The aqueous solution used for IC eluent is well suited for bioanalysis in relative to common liquid chromatography. This is especially true for capillary ion chromatography (CIC) due to its advantage of small sample needed. CIC is generally divided into three categories including open tubular, packed and monolithic. In this review, the recent progress of CIC is summarized based on the development of several key components associated with packed column-based system. The development of open tubular ion chromatography is also reviewed.

  13. Speciation analysis of organomercurial compounds in Fish Tissue by capillary gas chromatography coupled to microwave-induced plasma atomic emission detection

    Directory of Open Access Journals (Sweden)

    Dorfe Díaz

    Full Text Available This paper describes a novel approach for analysis of mercury speciation in fish using gas chromatography coupled with microwave-induced plasma optical emission spectrometry (GC-MIP-OES in surfatron resonant cavity. Sample treatment was based on quantitative leaching of mercury species from fish tissue with ultrasound-assisted acid-toluene extraction. The extracted mercury species analyzed with GC-MIP-OES attained detection limits of 5 and 9 pg for methylmercury (MeHg and ethylmercury (EtHg, respectively. A complete chromatogram could be completed in 1.5 min. MeHg values obtained with GC-MIP-OES were matched with organic mercury values obtained with selective reduction cold vapour- atomic absorption spectrometry (CV-AAS.

  14. Enantiomeric separation of chiral polychlorinated biphenyls on B-cyclodextrin capillary columns by means of heart-cut multidimensional gas chromatography and comprehensive two-dimensional gas chromatography. Application to food samples

    NARCIS (Netherlands)

    Bordajandi, L.R.; Korytar, P.; Boer, de J.; Gonzalez, M.J.

    2005-01-01

    Three commercially available chiral capillary columns, Chirasil-Dex, BGB-176SE. and BGB-172, have been evaluated for the separation into enantiomers of the 19 chiral polychlorinated biphenyls (PCB) congeners stable at room temperature. The enantiomers of 15 chiral PCBs were, at least to some extent,

  15. 毛细管气相色谱测定染发剂中苯二胺%Determination of phenylenediamine in hair dyes by capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    薛金花; 梁超; 李程

    2011-01-01

    A capillary gas chromatographic method for simultaneous determination of p-phenylenediamine, m-phenylenediamine,o-phenylenediamine in hair dyes was established.The samples of hair dyes were accurately weighted,selected with the ethylacetate and extracted by the ultrasonic,the impurity was removed by centrifugal work.The extraction was separated by capillary column and detected by FID for qualitativing with retention time and peak area.The linear relation of these three kinds of phenylenedianmine isoma in the range of 0.01 ~ 10 g/L were positive,and the "r" was about 0.9995 ~0.9996.The spiked recovery rates of the o-phenylenediamine, p-phenylenediamine and m-phenylenediamine were 88.6% ~97.8% ,93.3% ~ 105.0% and 88.5% ~99.1%.respectively.RSDs were 1.94% ~2.05% (n=7) ,and the detection limits were 2,2.5,2 ng/mL, respectively.This method was simple and rapid, which can effectively extract and separate the phenylenediamine isomer in hair dyes with satisfactory results.%建立了毛细管气相色谱法测定染发剂中邻、间、对苯二胺含量的分析方法.样品用乙酸乙酯、超声波提取,离心除去杂质,然后采用毛细管分离,FID检测,保留时间定性,峰面积定量.苯二胺三种异构体在0.01..10 g/L浓度范围内线性关系良好,相关系数为0.999 5~0.9996;邻苯二胺、对苯二胺、间苯二胺加标回收率分别为88.6%~97.8%,93.3%~105.0%,88.5%~99.1%,相对标准偏差为1.94%~2.05%(n=7),检出限分别为2,2.5,2 ng/mL.该方法简单、快速应用于实际样品测定,结果满意.

  16. 福辛普利钠中溶剂残留量的顶空毛细管GC法测定%Determination of Residual Organic Solvents in Fosinopril Sodium by Headspace Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    韩茹; 贾幼智

    2012-01-01

    A headspace capillary gas chromatography method was established for the determination of nine residual organic solvents: methanol, acetone, acetonitrile, dichloromethane, ethyl acetate, trichloromethane, benzene, toluene and pyridine in fosinopril sodium. A HP-624(6% cyanopropylphenyl-94% dimethylpolysiloxane) capillary column was used with the application of FID detector. Their average recoveries were 100.7% , 101.7% , 102.2% , 101.6% , 99.5% , 100.7% , 101.5% , 101.8% and 102.1% , with RSDs less than 2.5%.%建立了顶空毛细管气相色谱法测定福辛普利钠中的甲醇、丙酮、乙腈、二氯甲烷、乙酸乙酯、三氯甲烷、苯、甲苯和吡啶.采用HP-624(6%氰丙基苯基-94%二甲基硅氧烷)毛细管气相色谱柱,FID检测器.9种溶剂的平均回收率分别为100.7%、101.7%、102.2%、101.6%、99.5%、100.7%、101.5%、101.8%和102.1%,RSD均小于2.5%.

  17. Fast ultrasound-assisted extraction followed by capillary gas chromatography combined with nitrogen-phosphorous selective detector for the trace determination of tebuconazole in garlic, soil and water samples.

    Science.gov (United States)

    Singh, Sunil Kumar; Padmaja, P; Pandey, S Y

    2014-06-01

    A fast and an efficient ultrasound-assisted extraction technique using a lower density extraction solvent than water was developed for the trace-level determination of tebuconazole in garlic, soil and water samples followed by capillary gas chromatography combined with nitrogen-phosphorous selective detector (GC-NPD). In this approach, ultrasound radiation was applied to accelerate the emulsification of the ethyl acetate in aqueous samples to enhance the extraction efficiency of tebuconazole without requiring extra partitioning or cleaning, and the use of capillary GC-NPD was a more sensitive detection technique for organonitrogen pesticides. The experimental results indicate an excellent linear relationship between peak area and concentration obtained in the range 1-50 μg/kg or μg/L. The limit of detection (S/N, 3 ± 0.5) and limit of quantification (S/N, 7.5 ± 2.5) were obtained in the range 0.2-3 and 1-10 μg/kg or μg/L. Good spiked recoveries were achieved from ranges 95.55-101.26%, 96.28-99.33% and 95.04-105.15% in garlic, Nanivaliyal soil and Par River water, respectively, at levels 5 and 20 μg/kg or μg/L, and the method precision (% RSD) was ≤5%. Our results demonstrate that the proposed technique is a viable alternative for the determination of tebuconazole in complex samples.

  18. Use of a fluorosurfactant in micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    de Ridder, R; Damin, F; Reijenga, J; Chiari, M

    2001-05-04

    A fluorosurfactant, the anionic N-ethyl-N-[(heptadecafluorooctyl)sulfonyl]glycine potassium salt, trade name FC-129 [CAS 2991-51-7] was investigated for possible application in micellar electrokinetic capillary chromatography (MEKC). The surfactant was characterized with conductometric titration and test sample mixtures were investigated in MEKC systems, and compared with sodium dodecylsulphate. An increased efficiency and interesting selectivity differences were observed.

  19. Determination of Menthol in Yangyin Qingfei Syrups from Different Manufacturers by Capillary Gas Chromatography%毛细管柱气相色谱法测定养阴清肺糖浆中薄荷脑的含量

    Institute of Scientific and Technical Information of China (English)

    姜姗; 冯丽君; 孙茂; 林宏英; 倪健

    2013-01-01

    目的:建立毛细管柱气相色谱法测定养阴清肺糖浆中薄荷脑含量的方法.方法:采用气相色谱法(GC).色谱条件:DM-WAX毛细管柱(30m×0.25 mm×0.25 μm);载气:氮气,流速2.0 ml·min-1;进样口温度130℃;FID温度250℃;柱温:程序升温.结果:薄荷脑与内标物萘分离效果理想,薄荷脑浓度在0.051 ~0.306 mg· ml-1范围内线性关系良好(r=0.999 7),加样回收率为100.18%(RSD=2.26%,n=6).测得的11个厂家养阴清肺糖浆中薄荷脑含量差异明显,同一厂家不同批次产品薄荷脑含量无明显差异.结论:本方法简单、准确、重复性好,可用于测定养阴清肺糖浆中薄荷脑的含量.%Objective:To establish a determination method for menthol in Yangyin Qingfei syrups by capillary gas chromatography.Method:The content of menthol was determined by gas chromatography (GC).The DB-WAX capillary column (30 m ×0.25 mm × 0.25 μm) was used with nitrogen as the carrier gas,the flow rate was 2.0 ml · min-1,the temperature was set at 130℃for sample injection and 250℃ for FID.The rising of the column temperature was programmed.Result:Menthol and naphthaline using as the internal standard exhibited an excellent resolution.Menthol concentration showed linear relationship within the range of 0.051-0.306 mg · ml-1(r =0.999 7).The recovery was 100.18% (RSD =2.26%,n =6).The content of menthol in Yangyin Qingfei syrups from the different manufacturers was various,while no difference was observed among the different batches from the same manufacturer.Conclusion:The method is simple,accurate and reproducible.It can be used in the determination of menthol in Yangyin Qingfei syrups.

  20. 毛细管柱气相色谱法测定风油精中主要成分的含量%Determination of Main Compositions in the Essential Balm by Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    陆俭洁

    2001-01-01

    The method of the capillary column with programmed temperature gas chromatography was used by the GC-900 gas chromatograph. Many kinds of compositions in the essential balm can be separated effectively by the method. The three main compositions that are camphor, menthol and methyl salicylate were quantified and satisfactory chromatogram was obtained. By the internal standard method, the recovery of determining the camphor, menthol, methyl salicylate are 106.29 %, 102.44 %, 98.38 % and RSD are 0.06 %, 2.62 % ,1.88 % respectively.%采用GC-900型气相色谱仪,毛细管程序升温法,将风油精中10多种成分进行了有效分离,测定风油精中樟脑、薄荷脑、水杨酸甲酯3种主要成分的含量,得出了较为理想的色谱图,用内标法测定樟脑的回收率为106.29 %,RSD为2.56 %;薄荷脑的回收率为102.44 %,RSD为1.52 %;水杨酸甲脂的回收率为98.38 %,RSD为1.35 %.

  1. Dosages d'hydrocarbures dans l'eau et le sédiment marins par infrarouge et chromatographie gazeuse sur colonne capillaire Hydrocarbon Titration in Water and Marine Sediments by Infrared Analysis and Gas Chromatography in a Capillary Column

    Directory of Open Access Journals (Sweden)

    Morel G.

    2006-11-01

    Full Text Available Nous avons étudié l'évolution des hydrocarbures pétroliers dans un site confiné, celui de l'Aber-Benoît (Finistère, à la suite de l'accident du super-pétrolier Amoco-Cadiz en mars 1978. Pour ce faire, plusieurs méthodes ont été mises en oeuvre, et tout particulièrement la chromato-graphie gazeuse sur colonne capillaire : le protocole analytique est décrit pour l'eau et pour le sédiment, après optimisation des techniques de filtration, de préconcentration et de fractionnement préalables à la mesure. Il est possible de travailler sur des échantillons de deux litres d'eau de mer ou de cinquante grammes de sédiment, avec des seuils de détection du niveau de la partie par trillion (ppt dans l'eau et de la centaine de ppt dans le sédiment. The evolution of petroleum hydrocarbons was analyzed in a confined site, at Aber-Benoît in the Finistère department, following the accident of the supertanker Amoco Cadiz in March 1978. To do this, several methods were developed, including, in particular, capillary coulumn as chromatography. The analytical procedure is described for water and sediment after optimization of filtering, preconcentrating and fractionating techniques prior to measuring. Analyses can be made with two liters of seawater or fifty grams of sediment, with detection thresholds in parts per trillion (ppt in water and the hundredth of a ppt in sediment.

  2. Innovative method of direct determination of the content of paraffins, naphthenes, aromatics and sulfur compounds by capillary high-resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    R. Baizhumanova

    2012-03-01

    Full Text Available Based on determination of individual Hydrocarbon (paraffins, naphthenes, aromatics and Sulphur components of fuels and their mixture on the thin bonded of absorber (the stationary phase is a 100-metre silica capillary column, containing 0.5μm film thickness of bonded dimethylpolysiloxane phase by means of the selective solvents (mobile phase combined with technique of ionization of separated compounds by Flame Ionization Detector (FID and Sulphur Chemiluminescence Detector (SCD.

  3. Water management in capillary gas chromatographic air monitoring systems

    Energy Technology Data Exchange (ETDEWEB)

    Tipler, A. [Perkin Elmer Corp., Norwalk, CT (United States). Fresh Aire Lab.

    1994-12-31

    Capillary gas chromatography is an excellent technique for the speciated quantitation of low-level volatile organic compounds (VOCs) in ambient air. Although GC detectors have excellent sensitivity, some sample pre-concentration will be necessary to enable detection of VOCs at sub-ppb levels. This process normally employs a cooled and/or adsorbent trap to retain the analytes from a large volume of sample air. For very volatile VOCs, a very retentive trap is used and this may also retain water present as vapor in the sample. This trapped water causes significant problems with the chromatography and detector operation and methods must be sought to remove it or eliminate its effects. This paper investigates the magnitude of the problem and examines the various alternatives for managing the trapped water. The application of some of these techniques is demonstrated in a method for the determination of volatile polar and non-polar toxic organic compounds in ambient air.

  4. 毛细管气相色谱法测定猪个体日产甲烷气体量方法研究%Method research to determinate daily methane production of a pig by capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    陈渠; 曹庆云; 周武艺; 廖新俤

    2012-01-01

    试验建立了毛细管气相色谱法测定猪个体日产甲烷气体量的方法.甲烷气体采集后采用气密注射器即可直接上机测试.采用HP-PLOT/Q毛细柱(30m×0.32mm×20μm),恒温方法分离,用氢火焰离子化检测器(FID)检测.结果表明:该方法实现了猪个体甲烷气体产量的直接快速测定,线性范围为14.29~142.86mg/m3,线性相关系数R2为0.9996,在3个添加浓度水平上的平均加标回收率为97.42%.该方法简便、准确、线性范围宽,可用于测定甲烷气体.%A capillary gas chromatography was developed for the determination of daily methane production of a pig. The sampled methane gas can be directly injected into the chromalographic instrument for assay using gastight syringe. The HP-PLOT/Q capillary column (30 m×0.32 mm×20 μm) and hydrogen flame ionization detector(FID) were used, the column temperature stayed at an even temperature. The results demonstrated that the direct and fast determination of daily methane production of a pig was fulfilled. The linear range of methane was 14.29-142.86 mg/m3 with a good linear relationship(R2=0.999 6), and the average recovery was 97.42% at three different concentration levels. The method was simple and accurate with wide linear range and could be used to determine methane gas.

  5. Characterization of cis- and trans-octadecenoic acid positional isomers in edible fat and oil using gas chromatography-flame ionisation detector equipped with highly polar ionic liquid capillary column.

    Science.gov (United States)

    Yoshinaga, Kazuaki; Asanuma, Masaharu; Mizobe, Hoyo; Kojima, Koichi; Nagai, Toshiharu; Beppu, Fumiaki; Gotoh, Naohiro

    2014-10-01

    In this study, the characterisation of all cis- and trans-octadecenoic acid (C18:1) positional isomers in partially hydrogenated vegetable oil (PHVO) and milk fat, which contain several cis- and trans-C18:1 positional isomers, was achieved by gas chromatography-flame ionisation detector equipped with a highly polar ionic liquid capillary column (SLB-IL111). Prior to analysis, the cis- and trans-C18:1 fractions in PHVO and milk fat were separated using a silver-ion cartridge. The resolution of all cis-C18:1 positional isomers was successfully accomplished at the optimal isothermal column temperature of 120 °C. Similarly, the positional isomers of trans-C18:1, except for trans-6-C18:1 and trans-7-C18:1, were separated at 120 °C. The resolution of trans-6-C18:1 and trans-7-C18:1 isomers was made possible by increasing the column temperature to 160 °C. This analytical method is suitable for determining the cis- and trans-C18:1 positional isomers in edible fats and oils.

  6. Determination of nanogram per liter concentrations of volatile organic compounds in water by capillary gas chromatography and selected ion monitoring mass spectrometry and its use to define groundwater flow directions in Edwards Aquifer, Texas

    Science.gov (United States)

    Buszka, P.M.; Rose, D.L.; Ozuna, G.B.; Groschen, G.E.

    1995-01-01

    A method has been developed to measure nanogram per liter amounts of selected volatile organic compounds (VOCs) including dichlorodifluoromethane, trichlorofluoromethane, cis-1,2-dichloroethene, trichloroethene, tetrachloroethene, and the isomers of dichlorobenzene in water. The method uses purge-and-trap techniques on a 100 mL sample, gas chromatography with a megabore capillary column, and electron impact, selected ion monitoring mass spectrometry. Minimum detection levels for these compounds ranged from 1 to 4 ng/L in water. Recoveries from organic-free distilled water and natural groundwater ranged from 70.5% for dichlorodifluoromethane to 107.8% for 1,4-dichlorobenzene. Precision was generally best for cis-1,2-dichloroethene, tetrachloroethene, and the dichlorobenzene isomers and worst for dichlorodifluoromethane and trichlorofluoromethane. Blank data indicated persistent, trace-level introduction of dichlorodifluoromethane, 1,4-dichlorobenzene, and tetrachloroemene to samples during storage and shipment at concentrations less than the method reporting limits. The largest concentrations of the selected VOCs in 27 water samples from the Edwards aquifer near San Antonio, TX, were from confined-zone wells near an abandoned landfill. The results defined a zone of water with no detectable VOCs in nearly all of the aquifer west of San Antonio and from part of the confined zone beneath San Antonio.

  7. Methods of analysis and quality-assurance practices of the U.S. Geological Survey organic laboratory, Sacramento, California; determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Crepeau, Kathryn L.; Domagalski, Joseph L.; Kuivila, Kathryn M.

    1994-01-01

    Analytical method and quality-assurance practices were developed for a study of the fate and transport of pesticides in the Sacramento-San Joaquin Delta and the Sacramento and San Joaquin River. Water samples were filtered to remove suspended parti- culate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide, and the pesticides were eluted with three 2-milliliter aliquots of hexane:diethyl ether (1:1). The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for analytes determined per 1,500-milliliter samples ranged from 0.006 to 0.047 microgram per liter. Recoveries ranged from 47 to 89 percent for 12 pesticides in organic-free, Sacramento River and San Joaquin River water samples fortified at 0.05 and 0.26 microgram per liter. The method was modified to improve the pesticide recovery by reducing the sample volume to 1,000 milliliters. Internal standards were added to improve quantitative precision and accuracy. The analysis also was expanded to include a total of 21 pesticides. The method detection limits for 1,000-milliliter samples ranged from 0.022 to 0.129 microgram per liter. Recoveries ranged from 38 to 128 percent for 21 pesticides in organic-free, Sacramento River and San Joaquin River water samples fortified at 0.10 and 0.75 microgram per liter.

  8. Determination of Four Active Components in Hongyao Strapping by Capillary Gas Chromatography%毛细管气相色谱法测定红药贴膏中4种活性成分的含量

    Institute of Scientific and Technical Information of China (English)

    张一鸣; 王洁; 胡明勋; 都增燕; 陈安家

    2011-01-01

    目的:建立毛细管气相色谱法同时测定红药贴膏中樟脑、薄荷脑、冰片和水杨酸甲酯的含量.方法:采用毛细管气相色谱法.色谱柱为PEG-20M石英毛细管柱(0.25 mm x 0.25 wm x 30 m),氢火焰离子检测器,检测器和气化室的温度均为200 ℃,柱温160℃,氮气为载气,正辛醇为内标物,用挥发油测定器蒸馏制备供试品溶液.结果:在该色谱条件下,樟脑、薄荷脑、冰片和水杨酸甲酯分离度和线性关系良好,回收率分别为99.8%,100.3%,99.5%,99.7%.结论:该方法简便、准确、专属性强、重复性好,可用于红药贴膏的质量控制.%Objective: To establish a method for determination of camphor, menthol, borneol and methylsalicylate in Hongyao strapping. Method:Capillary gas chromatography was adopted. The chromatography separation was carried out with PEG-20M capillary column(0.25 μm × 0. 25 mm × 30 m), using a flame ionization detector. The injector and detector temperature were set at 200 ℃. The column temperature was 160 ℃. n-Octanol was used as internal standard. The sample solution was prepared by distillation with essential oil collector. Result: The resolution and linearity of camphor, menthol, borneol and methylsalicylate were good under the chromatographic conditions. The average recoveries of camphor, menthol, borneol and methylsalicylate were 99.8%, 100. 3%,99.5% , 99.7%. Conclusion:This method is simple, sensitive, accurate and has good repeatability for controlling the quality of camphor, menthol, borneol and methylsalicylate in Hongyao strapping.

  9. Thermal expansion pump for capillary high-performance liquid chromatography.

    Science.gov (United States)

    Tao, Qian; Wu, Qian; Zhang, Xiangmin

    2010-02-01

    A thermal expansion pump (TEP) based on a principle of liquid thermal expansion for capillary high-performance liquid chromatography has been developed. The novel pump is capable of generating a continuous flow at high pressure for constant and stable delivery of binary solvents from nanoliters to microliters per minute without splitting. Theoretical equations for controlling fluidic output of this pump have been established and validated by a series of experiments. Factors affecting flow rate, such as density discrepancy, liquid compressibility, and mass loss in output, were taken into account. An assembly of the pump system employing two groups of thermal expansion pumps (TEPs) working in turns were fabricated, and a controlling strategy for the pump system to maintain a continuous delivery without pressure fluctuation even at switching points was also developed. Both isocratic and gradients of binary solvent delivery by the TEPs were performed. Reproducibility and standard deviation at different flow rates were determined. A capillary high-performance liquid chromatography (micro-HPLC) system consisting of the TEPs, an injection valve, a homemade packed capillary column (20 cm x 100 microm i.d. with 5 microm C18), and a laser-induced fluorescence detector was set up, and sample separations were carried out. Results of RSD = 4% for flow and RSD = 2% for retention times at 500 nL/min were achieved. Such a pump system has almost no moving parts except for the solvent switches. Its overall costs of manufacture and running are very low. It is proven that the TEPs system has great potential and competitive capabilities in capillary liquid chromatography.

  10. Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Wastewater Compounds by Polystyrene-Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Smith, Steven G.; Schroeder, Michael P.; Barber, Larry B.; Burkhardt, Mark R.

    2002-01-01

    A method for the determination of 67 compounds typically found in domestic and industrial wastewater is described. The method was developed in response to increasing concern over the impact of endocrine-disrupting chemicals in wastewater on aquatic organisms. This method also may be useful for evaluating the impact of combined sanitary and storm-sewer overflow on the water quality of urban streams. The method focuses on the determination of compounds that are an indicator of wastewater or that have been chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclicaromatic hydrocarbons, and high-use domestic pesticides. Water samples are filtered to remove suspended particulate matter and then are extracted by vacuum through disposable solid-phase cartridges that contain polystyrene-divinylbenzene resin. Cartridges are dried with nitrogen gas, and then sorbed compounds are eluted with dichloromethane-diethyl ether (4:1) and determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-water samples fortified at 4 micrograms per liter averaged 74 percent ? 7 percent relative standard deviation for all method compounds. Initial method detection limits for single-component compounds (excluding hormones and sterols) averaged 0.15 microgram per liter. Samples are preserved by filtration, the addition of 60 grams NaCl, and storage at 4 degrees Celsius. The laboratory has established a sample-holding time (prior to sample extraction) of 14 days from the date of sample collection until a statistically accepted method can be used to determine the effectiveness of these sample-preservation procedures.

  11. Determination of volatile and non-volatile products of milk fermentation processes using capillary zone electrophoresis and solid phase microextraction coupled to gas chromatography.

    Science.gov (United States)

    Ligor, Magdalena; Jarmalaviciene, Reda; Szumski, Michal; Maruska, Audrius; Buszewski, Boguslaw

    2008-08-01

    The aim of the investigations was to develop analytical methods for the determination of selected volatile and non-volatile organic compounds numbering among the final products of milk fermentation. The analyzed compounds were as follows: biacetyl and carboxylic acids (formic, acetic, citric, and lactic). The model yogurt was prepared under controlled conditions in our laboratory by addition of the selected bacteria (Lactobacillus bulgaricus and Streptococcus thermophilus) to the milk sample. The temperature, time, and stirring were controlled during the fermentation process. Factors considered in SPMPE-GC-FID method development included fiber exposure time, salt addition, temperature of extraction, and temperature of desorption. Various SPME fibers, for example with PDMS, CAR/PDMS, PA, and PDMS/DVB coatings, were tested to obtain the highest recovery of the investigated compounds extracted from yogurt samples. Based on these preliminary experiments, qualitative and quantitative analyses for the determination of biacetyl were performed by SPME-GC-FID. Moreover, a capillary zone electrophoresis method was developed for the determination of carboxylic acids in the yogurt samples. The buffer composition as well as deproteinization by acetonitrile were found to have a crucial effect on the analysis.

  12. Preparation and Separation Performance of Three New Gas Chromatography Capillary Columns Coated with Cyclodextrin Derivatives%环糊精衍生物涂渍毛细管柱的制备及分离性能

    Institute of Scientific and Technical Information of China (English)

    颜霞; 方智利; 林纯; 王国梁; 范军; 郑盛润; 贾成俊; 章伟光

    2013-01-01

    以3种环糊精衍生物分别涂覆在毛细管内壁制得气相色谱毛细管柱,以正十二烷为溶质,测得理论塔板数均在2800/m以上,柱效较高.研究了它们对一系列苯系物位置异构体的分离性能,探讨了硝基氯苯、硝基苯胺和苯二胺等化合物在不同柱上的拆分机理.底物分子和固定相之间的弱相互作用(如氢键、偶极相互作用和π-π堆积作用)等直接影响毛细管柱对底物的分离性能.对于苯二胺的位置异构体,在全对氯苯异氰酸酯化β-CD涂覆的毛细管柱(ACD)上的分离因子为1.88,在多叠氮β-CD衍生物涂覆的毛细管柱(NMCD)上的分离因子为1.41,但在单叠氮β-CD衍生物涂覆的毛细管柱(NSCD)上无法分开;对于硝基氯苯,在NMCD柱和ACD柱上的分离因子相近(前者为1.13/1.11;后者为1.08/1.15),在NSCD柱上则无分离趋势;对于硝基苯胺,在NMCD柱上无分离趋势.同时,苯环上不同取代基间电子效应则影响了异构体在气相色谱中出峰顺序.%Three kinds of capillary columns were obtained by coating cyclodextrin derivatives onto inner surface of fused capillary.According to the literature's method,all the theoretical plate numbers are over 2800/m by using n-dodecane,indicating that they have high column efficiencies.Then,separation and mechanism of isomeric benzene derivatives,such as nitrochlorobenzene,nitroaniline,and phenylenediamine by capillary column gas chromatography have been investigated in detail.The interactions such as hydrogen bonding,dipolar-dipolar attraction and π-π stacking between analytes and stationary phases have significant effect on the separation performances of these capillary columns.For phenylenediamine,separation factors on the heptakis (6-azido-6-deoxy-2,3-di-O-p-chlorophenylcarbamoylated)-b-CD (NMCD) and per(pchlorophenylcarbamoylated)-b-CD(ACD) columns are 1.41 and 1.88,respectively,however the positional isomers can not be separated on the NSCD column

  13. POLYMER-COATED FIBROUS MATERIALS AS THE STATIONARY PHASE IN PACKED CAPILLARY GAS CHROMATOGRAPHY AND THE APPLICATIONS FOR SAMPLE PREPARATION IN ENVIRONMENTAL ANALYSIS%聚合物涂层纤维材料为固定相填充毛细管气相色谱及其在样品预处理中的应用

    Institute of Scientific and Technical Information of China (English)

    SAITOYoshihiro; JINNOKiyokatsu

    2003-01-01

    Fibrous polymers having an excellent heat-resistance were successfully introduced as the stationary phase in capillary gas chromatography (GC) and the basic separation performance has been investigated. Poly(p-phenylene-26-benzobisoxazole); Zylon, fibers were selected as the stationary phase taking into account the chemical structure, heat resistance, solvent resistance and the physical strength. About 330 filaments of the polymer were packed longitudinally into fused-silica capillaries of 0.32 mm i.d., and the GC separation of several test mixtures, such as n-alkylbenzenes and n-alkanes was carried out with these fiber-packed capillary columns. From the results it has been demonstrated that the fiber-packed capillary columns have a great potential as the separation media for volatile compounds. Polymer coating onto the surface of the packed-filaments has been also studied, and the results clearly showed that the retentivity was significantly improved over a conventional capillary columns of the same length and that the selectivity can be tuned by selecting different types of coating materials selected for the purposes. The applications of polymer-coated fiber-packed capillary as a miniaturized sample preparation device was also investigated for the analysis of environmental pollutants in river water samples.

  14. Investigation of an alternating current plasma as an element selective atomic emission detector for high-resolution capillary gas chromatography and as a source for atomic absorption and atomic emission spectrometry

    Science.gov (United States)

    Ombaba, Jackson M.

    This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The device exhibits a stable signal because the plasma is self-seeding and reignites itself every half cycle. A tesla coil is not required to commence generation of the plasma if the ac voltage applied is greater than the breakdown voltage of the plasma-supporting gas. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (Mvutilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienyl manganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer (common room humidifier) was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were also considered. Figures of merits of selected elements both in absorption and emission modes are reported. The evaluation of a computer-aided optimization program, Drylab GC, using

  15. Separation of Aniline Derivatives by Micellar Electrokinetic Capillary Chromatography

    Institute of Scientific and Technical Information of China (English)

    Jun LI; Zhuo Bin YUAN

    2004-01-01

    A micellar electrokinetic capillary chromatography (MECC) was developed for the determination of aniline and 6 substituted anilines.The seven components were separated within 25 min in the buffer solution of 40 mmol/L sodium borate and 100 mmol/L SDS.It was found that the separation was dependent on operating voltage, pH value, borate and SDS concentrations.The analytical performance was examined in terms of linear response and reproducibility.Wastewater was determined by the established method.

  16. Determination of P-phenylenediamine in the Air of Workplace by Capillary Gas Chromatography%毛细管气相色谱测定工作场所空气中对苯二胺

    Institute of Scientific and Technical Information of China (English)

    谢碧俊; 杨长晓

    2011-01-01

    Objective To establish a method to determine p-phenylenediamine in the air of workplace by capillary gas chromatography. Methods The p-phenylenediamine in the air of workplace was sampled with silica gel tubes and eluted with ethanol, separated by SE - 54 capillary column and determined by gas chromatography under the optimal instrument conditions. The experimental study was carried out according to the requirements of Methods for Determination of Chemical Substances in the Air of Workplace. Results p-Phenylenediamine showed good linearity at the range of 0 - 1 120 μg/ml (r = 0. 999 6 ) . The limit of detection was 0. 39 μg/ml (s/n -3; injection volume, 1 μl) and the detectable concentrition of sample was 0. 13 mg/ m (3L of air sample). Samples of high, middle and low concentrations were re-determined for 6 times and the RSD was 0. 0% -0. 45% with the desorption efficiency at the range of 95. 2% to 96. 4% . Benzene, methylbenzene, xy-lene, acetone, diphenylamine, phenylamine, o-phenylenediamine, m-phenylenediamine, diphenyl and trieth-ylamine, which may coexist with p-phenylenediamine in the air of workplace, had no interference on the determination. Conclusion The method has the advantages of simple operation, rapid performance, high sensitivity and low detection limit, and coexisting substances have no interfering influence on the determination, so it is suitable to determine the p-phenylenediamine in the air of workplace.%目的 建立工作场所空气中对苯二胺毛细管气相色谱测定方法.方法 硅胶管采样,乙醇解吸,SE - 54毛细管色谱柱分离,在最佳仪器条件下用气相色谱仪测定,按照《工作场所空气中化学物质的测定方法》的要求,进行实验室方法研究.结果 对苯二胺在0~1120 μg/ml之间有良好的线性关系,相关系数0.9996.方法的最低检出浓度为0.39 μg/ml(进样1μl解吸液,以3倍噪音计算),样品最低检出浓度为0.13 mg/m3(采样体积以3L

  17. Determination of the Mercury Alkyl Mercuryalkylide in Municipal Sewage by Gas Chromatography Method Using DB-WAX Capillary Column%毛细管柱气相色谱法测定城市污水中烷基汞

    Institute of Scientific and Technical Information of China (English)

    张继蓉; 印成; 周金元

    2015-01-01

    A gas chromatography method using DB-WAX capillary column was established to determine the mercury alkyl mercuryalkylide in municipal sewage.On optimum condition , the measurement range was 0.10~1.00 mg/L, the correlation coefficient of methylmercury was 0.9998 , the correlation coefficient of ethylmercury was 0.9999.When 1 L water sample was taken , the detection limit of methylmercury was 6.9 ng/L, the detection limit of ethylmercury was 4.4 ng/L.Through the recovery of standard addition , the recovery rate of methylmercury and ethylmercury was in the ring of 90%~105%, the RSD was less than 1%.%建立了DB-WAX毛细管柱气相色谱法测定城市污水中烷基汞的方法。在优化条件下,测定范围为0.10~1.00 mg/L,甲基汞和乙基汞的相关系数分别为R=0.9998、0.9999。当水样取1 L时,甲基汞检出限为6.9 ng/L,乙基汞检出限为4.4 ng/L。通过基体加标回收,甲基汞和乙基汞的回收率均可控制在90%~105%之间,测定结果的RSD均<1%。

  18. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory : determination of organophosphate pesticides in whole water by continuous liquid-liquid extraction and capillary-column gas chromatography with flame photometric detection

    Science.gov (United States)

    Jha, Virendra K.; Wydoski, Duane S.

    2003-01-01

    A method for the isolation of 20 parent organophosphate pesticides and 5 organophosphate pesticide degradates from natural-water samples is described. Compounds are extracted from water samples with methylene chloride using a continuous liquid-liquid extractor for 6 hours. The solvent is evaporated using heat and a flow of nitrogen to a volume of 1 milliliter and solvent exchanged to ethyl acetate. Extracted compounds are determined by capillary-column gas chromatography with flame photometric detection. Single-operator derived method detection limits in three water-matrix samples ranged from 0.003 to 0.009 microgram per liter. Method performance was validated by spiking all compounds in three different matrices at three different concentrations. Eight replicates were analyzed at each concentration in each matrix. Mean recoveries of most method compounds spiked in surface-water samples ranged from 54 to 137 percent and those in ground-water samples ranged from 40 to 109 percent for all pesticides. Recoveries in reagent-water samples ranged from 42 to 104 percent for all pesticides. The only exception was O-ethyl-O-methyl-S-propylphosphorothioate, which had variable recovery in all three matrices ranging from 27 to 79 percent. As a result, the detected concentration of O-ethyl-O-methyl-S-propylphosphorothioate in samples is reported in this method with an estimated remark code. Based on the performance issue, two more compounds, disulfoton and ethion monoxon, also will be reported in this method with an estimated remark code. Estimated-value compounds, which are ?E-coded? in the data base, do not meet the performance criteria for unqualified quantification, but are retained in the method because the compounds are important owing to high use or potential environmental effects and because analytical performance has been consistent and reproducible.

  19. Determination of Parabens in cosmetics by capillary gas chromatography%毛细管气相色谱法测定化妆品中对羟基苯甲酸酯的含量

    Institute of Scientific and Technical Information of China (English)

    朱克旭; 汪海宣

    2014-01-01

    OBJECTIVE To establish a method to determine the content of methyl hydroxybenzoate and Ethyl p-Hydrobenzoate by capillary gas chromatography in the cosmetics.METHODS Direct-sample injection method was used with DB-17 capillary、FID detector and split ratio of 10∶1.RESULTS The linear for both of the preserva-tives was well in range of 10μg· mL-1 ~200μg· mL-1 ,the coefficient correlation was 0.9992 and 0.9993 respec-tively.The recovery for both of the preservatives was 95%~98%.CONCLUSION The method is easy and robust with high resolution and less time by standard curve method.%目的:建立毛细管气相色谱法测定化妆品中的对羟基苯甲酸甲酯和对羟基苯甲酸乙酯。方法采用溶液直接进样法测定,DB-17毛细管柱,FID检测器,分流比10∶1。结果两种防腐剂在10~200μg· mL -1浓度范围内呈良好线性关系,相关系数分别为0.9992、0.9993,两种化合物的加标回收率为95%~98%。结论本法耗时少,分离度高,用标准曲线法测定,方法简单可靠。

  20. 毛细管气相色谱法测定市售食用油中残留溶剂的研究%Determination of Residual Solvent Contents in Edible Oils by Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    黄韬睿; 王鑫

    2012-01-01

    6# solvent will residues in edible oils as the extraction solvent in process of Oil extraction.6# solvent has a lot of harm to quality of oil and health of human.Pressed oil should not contain 6# solvent because of the different process.So we can determine the quality of the pressed oil by detect the 6# solvent in the oil.In this research,Capillary Gas Chromatography detector is used to determine the residue of 6﹟ solvent in pressed oils which sold in Chengdu and Guangyuan market.The results of determine will provide a support in data to supervision of edible oils.%浸出法制油的过程中主要使用六号溶剂作为浸出溶剂,该方法难免造成六号溶剂在食用油中的残留,六号溶剂对食用油的品质以及人体健康都有诸多害处,而压榨油因为生产工艺不同,其中不应该含有六号溶剂的残留。顾可根据检测压榨油中是否含有六号溶剂判断压榨油中是否添加浸出油。本文建立了毛细管气相检测食用油中六号溶剂残留量的方法,并对成都和广元市场市售的压榨食用油进行了初步的检测,为两地食用油市场的监管提供初步的数据支持。

  1. A Robust Thermal Modulator for Comprehensive Two-Dimensional Gas Chromatography

    NARCIS (Netherlands)

    Geus, de H.J.; Boer, de J.

    1999-01-01

    In comprehensive two dimensional gas chromatography (GCxGC), two capillary columns are connected in series through an interface known as a 'thermal modulator'. This device transforms effluent from the first capillary column into a series of sharp injection-like chemical pulses suitable for high-spee

  2. Application of capillary gas chromatography-reaction interface/mass spectrometry to the selective detection of sup 13 C-, sup 15 N-, sup 2 H-, and sup 14 C-labeled drugs and their metabolites

    Energy Technology Data Exchange (ETDEWEB)

    Chace, D.H.

    1989-01-01

    A novel reaction interface/mass spectrometer (RIMS) technique has been applied to the selective detection of {sup 13}C-, {sup 15}N-, {sup 2}H-, and {sup 14}C-labeled phenytoin and its metabolites in urine following separation by capillary gas chromatography. The microwave-powered reaction interface converts materials from their original forms into small molecules whose mass spectra serve to identify and quantify the nuclides. The presence of each element is followed by monitoring the isotopic variants of CO{sub 2}, NO, H{sub 2}, or CH{sub 4} that are produced by the reaction interface. Chromatograms showing only enriched {sup 13}C and {sup 15}N were produced using the net {sup 13}CO{sub 2} or {sup 15}NO signal derived by subtracting the abundance of naturally occurring isotopes from the observed M + 1 signal. When hydrogen was used as a reactant gas, a selective chromatogram of {sup 2}H (D) was obtained by measuring HD at m/Z 3.0219, and a chromatogram showing {sup 14}C was obtained by measuring {sup 14}CH{sub 4} at m/Z 18.034 with a high resolution. For a stable isotope detection, metabolites representing less than 1.5% of the total labeled compounds could be detected in the chromatogram. Detection limits of 170 pCi/mL (34 pCi on column that is equivalent to 187 pg) of a {sup 14}C- labeled metabolite was detected. To identify many of these labeled peaks (metabolites), the chromatographic analysis was repeated with the reaction interface turned off and mass spectra obtained at the retention times found in the RIMS experiment. In addition to the ability of GC-RIMS to detect the presence of {sup 13}C-, {sup 15}N-, and {sup 2}H- (D), it can also quantify the level of enrichment. Enrichment of {sup 13}C and {sup 15}N is quantified by measuring the ratio of excess {sup 13}CO{sub 2} to total {sup 12}CO{sub 2} or excess {sup 15}NO to total {sup 14}NO.

  3. Determination of Thirteen Plasticizers in Food Plastic Packaging Materials by Capillary Column Gas Chromatography%食品包装材料中13种增塑剂的毛细管气相色谱法测定

    Institute of Scientific and Technical Information of China (English)

    马康; 汤福寿; 何雅娟; 刘菲

    2011-01-01

    A capillary column gas chromatographic method was developed for the separation and determination of thirteen plasticizers, including dimethyl phthalate acid ester(DMP), diethyl phthalate acid ester( DEP), dipropyl phthalate acid ester( DnPP), diisobutyl phthalate acid ester( DIBP), dibutyl phthalate acid ester( DBP), diamyl phthalate acid ester( DAP), bisphenol A( BIA), di-n-hexyl phthalate acid ester(DHP), butyl benzyl phthalate acid ester(BBP), di-2-ethylhexyl adipate (DEHA), di(2-ethylhexyl) phthalate acid ester(DEHP), dioctyl phthalate acid ester(DOP) and dinonyl phthalate acid ester(DNP) in plastic packaging materials for foodstuff. The analytes were extracted with hexane from samples by Soxhlet extraction technique, then purified by silica solid phase extraction. Three key factors such as rinse solvent, eluting solvent and eluting volume were optimized. Hexane and toluene ( 1: 1, by volume) were used as rinse solvents, 2 mL ethyl acetate was used as eluting solvent. After filtration, the eluate was determined by gas chromatography with flame ionization detector(GC/FID). The calibration curves of thirteen plasticizers were linear in the range of O. 1 - 1 000 mg/L with detection limits of 0. 005 - 0. 030 mg/L. The spiked recoveries ranged from 90% to 116% with relative standard deviations of 2. 2% -4. 9%. The method was successfully applied in the determination of plasticizers in plastic packaging materials for foodstuff.%建立了索氏提取、固相萃取净化浓缩、毛细管气相色谱法测定塑料食品包装材料中13种增塑剂的方法.优化了固相萃取淋洗剂、洗脱剂和洗脱剂体积等参数.样品经正己烷索氏提取后,用硅胶小柱净化浓缩.以正己烷-甲苯为淋洗剂,2 mL乙酸乙酯为洗脱剂.过滤后的洗脱液用气相色谱仪分析.结果显示,13种增塑剂在0.1~1000 mg/L范围内呈良好线性,检出限为0.005~O.030 mg/L.样品的加标回收率为90%~116%,相对标准偏差为2.2%~4.9%.

  4. Sol-gel multicapillary columns for gas-solid chromatography.

    Science.gov (United States)

    Sidelnikov, Vladimir N; Patrushev, Yuri V; Belov, Yuri P

    2006-01-06

    In this work, we report the method for the preparation of multicapillary columns (MCCs) for gas-solid chromatography. The porous layer adsorbent is formed on capillary walls by the hydrolysis of aluminum alkoxide in the presence of polypropylene glycol (PPG) and HCl. Porosity and selectivity of the adsorbent depend on reaction conditions and the concentration of PPG. Sol-gel MCCs are well suited for high-speed chromatographic analysis of light hydrocarbons by gas-solid chromatography. Nine-component mixtures of C1-C4 hydrocarbons are separated within 8-12 s. The efficiency of 25-30 cm long alumina sol-gel MCCs consisting of approximately 1400 capillaries of 40 microm diameter is up to 2500-3000 theoretical plates.

  5. Online comprehensive two-dimensional ion chromatography × capillary electrophoresis.

    Science.gov (United States)

    Ranjbar, Leila; Gaudry, Adam J; Breadmore, Michael C; Shellie, Robert A

    2015-09-01

    A comprehensively coupled online two-dimensional ion chromatography-capillary electrophoresis (IC × CE) system for quantitative analysis of inorganic anions and organic acids in water is introduced. The system employs an in-house built sequential injection-capillary electrophoresis instrument and a nonfocusing modulation interface comprising a tee-piece and a six-port two-position injection valve that allows comprehensive sampling of the IC effluent. High field strength (+2 kV/cm) enables rapid second-dimension separations in which each peak eluted from the first-dimension separation column is analyzed at least three times in the second dimension. The IC × CE approach has been successfully used to resolve a suite of haloacetic acids, dalapon, and common inorganic anions. Two-dimensional peak capacity for IC × CE was 498 with a peak production rate of 9 peaks/min. Linear calibration curves were obtained for all analytes from 5 to 225 ng/mL (except dibromoacetic acid (10-225 ng/mL) and tribromoacetic acid (25-225 ng/mL)). The developed approach was used to analyze a spiked tap water sample, with good measured recoveries (69-119%).

  6. 毛细管柱气相色谱法测定酱腌菜中环己基氨基磺酸钠%Determination of sodium cyclamate with capillary gas chromatography in pickled vegetables

    Institute of Scientific and Technical Information of China (English)

    李力军; 李鹏; 姜延国

    2011-01-01

    Objective:To determine the cyclamic sodium in foods in a rapid and accurate way.Methods:Use TR - 1 capillary column gas chromatography to determine the cyclamic sodium in pickled vegetables.Results: In the best chromatographic conditions, the result shows in the range of 1 μg ~ 5 μg as a good linear relationship ( r = 0.9998), and the detection limit was 4 ng.Under repeatability conditions, the absolute difference of two independent measurements was no more than 10% of the arithmetic mean.The actual measurement result was between 3.0% and 6.7%, and the recovery rate with added specimen was between 95.4% and 100.6%.Conclusion: This method is simple, fast, accurate and easy to operate to determine cyclamic sodium in vegetables and other foods.%目的:快速、准确地测定食品中的环己基氨基磺酸钠.方法:采用TR-1型毛细管柱气相色谱法测定酱腌菜中环己基氨基磺酸钠含量.结果:在最佳色谱条件下,结果在1μg~5μg范围内呈良好的线性关系(r=0.9998),检出限为4 ng.在重复性条件下获得的两次独立测定结果的绝对差值不超过算术平均值的10%,实际测定在3.0%~6.7%之间.加标回收率在95.4%~100.6%之间.结论:方法简单、快速、准确、易于操作,适用于酱腌菜等食品中环己基氨基磺酸钠的测定.

  7. Determination of volatile halohydrocarbons in drinking water by capillary column gas chromatography%毛细管柱气相色谱法测定生活饮用水中挥发性卤代烃

    Institute of Scientific and Technical Information of China (English)

    董玉英; 张瑞雨; 欧利华

    2013-01-01

    Objective: To establish a method for determination of seven volatile halohydrocarbons in drinking water. Methods: The seven volatile halohydrocarbons (chlorofrom, tetrachloromethane, trichloroethylene, bromodi-chloromethane, tetrachloroethylene, dibromochloromethane, bromoform) in drinking water were determined by head-space Gas Chromatography with DB - 624 capillary column. Results: Under the optimal experimental conditions, the recoveries of the seven volatile halohydrocarbons were in the range of 92.5% -102%, the relative standard deviation was between 1.20% ~4.61%, and the determination limit was between 0.01 μg/L ~ 1.00 μg/L. Conclusion: The developed methjod is sensitive, simple, rapid and accurate, and seven volatile halohydrocarbons in drinking water can be determined simultaneously.%目的:建立一种快速、准确测定生活饮用水中7种挥发性卤代烃的方法.方法:采用DB-624毛细管柱、顶空气相色谱法测定生活饮用水中三氯甲烷、四氯化碳、三氯乙烯、二氯一溴甲烷、四氯乙烯、一氯二溴甲烷及三溴甲烷.结果:在所选择的实验条件下,7种挥发性卤代烃的平均回收率在92.5%~102%之间,相对标准偏差(RSD)为1.20% ~4.61%,检出限为0.01 μg/L ~1.00 μg/L.结论:所建立的分析方法灵敏、简便、快速、准确,可同时测定生活饮用水中的7种挥发性卤代烃.

  8. Polymer-Coated Fibrous Packing Materials in Metal Capillary Gas Chromatography%聚合物涂层填充物在金属毛细管气相色谱中的应用

    Institute of Scientific and Technical Information of China (English)

    SAITO Yoshihiro; OGAWA Mitsuhiro; IMAIZUMI Motohiro; WADA Hiroo; JINNO Kiyokatsu

    2004-01-01

    Gas chromatography (GC) is one of the most versatile separation methods for volatile compounds, and a variety of polymeric materials as the stationary phases have been developed for various applications. In contrast to the successful applications and commercialization of the polymer-coated columns, the reports for the fibrous

  9. Rapid and high resolution capillary supercritical fluid chromatography (SFC) and SFC/MS of trichothecene mycotoxins.

    Science.gov (United States)

    Smith, R D; Udseth, H R; Wright, B W

    1985-05-01

    The potential application of capillary column supercritical fluid chromatography (SFC) and SFC/mass spectrometry (SFC/MS) for the separation and analysis of mycotoxins of the trichothecene group was examined. Trichothecenes present significant analytical problems for both gas and liquid chromatography with a major difficulty for the latter being the lack of sufficiently sensitive and selective detectors. Supercritical carbon dioxide mobile phases at temperatures up to 100 degrees C were used with deactivated fused silica columns coated with crosslinked stationary phases. Separations were obtained under pressure ramped conditions using long (15 m) 50-micron i.d. columns for several trichothecenes (diacetoxyscirpenol, deoxynivalenol, and T-2 toxin) and related higher molecular weight macrocyclic (roridin and verrucarin) trichothecenes. In addition, new rapid pressure programming techniques with short (less than 2m) 25- to 50-micron i.d. capillary columns were used to obtain fast separations in as little as 1 min. SFC/MS with ammonia chemical ionization provided high selectivity and sensitive detection (with approximately 1-pg detection limits) for trichothecene mixtures. The extension to complex sample matrices is discussed and the application of selective MS/MS detection is demonstrated.

  10. Speciation analysis by gas chromatography with plasma source spectrometric detection

    Science.gov (United States)

    Łobiński, Ryszard; Adams, Freddy C.

    State-of-the-art species-selective analysis by gas chromatography (GC) with plasma source spectrometric detection is discussed for organometal and organometalloid compounds. Various plasmas, inductively coupled plasma, microwave induced plasma, capacitatively coupled plasma, direct current plasma and alternating current plasma, are characterized and critically compared as sources of radiation for atomic emission spectrometry and sources of ions for mass spectrometry. Interfaces between gas chromatography (packed, wide-bore, capillary and multicapillary) and plasma source spectrometry are characterized. Particular emphasis is given to applications of GC with plasma source detection to real-world analytical problems, which are comprehensively reviewed. The use of plasmas for the acquisition of auxiliary molecular information such as empirical formulae and structural information is discussed. Recent developments relating to sample preparation and presentation to the hyphenated system are addressed. The most significant trends in speciation analysis are highlighted.

  11. Microfabricated planar glass gas chromatography with photoionization detection.

    Science.gov (United States)

    Lewis, Alastair C; Hamilton, Jacqueline F; Rhodes, Christopher N; Halliday, Jaydene; Bartle, Keith D; Homewood, Philip; Grenfell, Robin J P; Goody, Brian; Harling, Alice M; Brewer, Paul; Vargha, Gergely; Milton, Martin J T

    2010-01-29

    We report the development of a microfabricated gas chromatography system suitable for the separation of volatile organic compounds (VOCs) and compatible with use as a portable measurement device. Hydrofluoric acid etching of 95x95mm Schott B270 wafers has been used to give symmetrical hemi-spherical channels within a glass substrate. Two matching glass plates were subsequently cold bonded with the channels aligned; the flatness of the glass surfaces resulted in strong bonding through van der Waals forces. The device comprised gas fluidic interconnections, injection zone and 7.5 and 1.4m long, 320microm internal diameter capillaries. Optical microscopy confirmed the capillaries to have fully circular channel profiles. Direct column heating and cooling could be achieved using a combination of resistive heaters and Peltier devices. The low thermal conductivity of glass allowed for multiple uniform temperature zones to be achieved within a single glass chip. Temperature control over the range 10-200 degrees C was achieved with peak power demand of approximately 25W. The 7.5m capillary column was static coated with a 2microm film of non-polar dimethylpolysiloxane stationary phase. A standard FID and a modified lightweight 100mW photoionization detector (PID) were coupled to the column and performance tested with gas mixtures of monoaromatic and monoterpene species at the parts per million concentration level. The low power GC-PID device showed good performance for a small set of VOCs and sub ng detection sensitivity to monoaromatics.

  12. Determination of Nicotine and Cotinine in Urine and Hair by Capillary Gas Chromatography%尿液和头发中尼古丁和可替宁的毛细管气相色谱测定法

    Institute of Scientific and Technical Information of China (English)

    朱琳; 杨丽君; 孙丽艳

    2011-01-01

    目的 建立尿液和头发中尼古丁和可替宁的气相色谱标准检测方法.方法 尿液或头发样品用NaOH溶液完全消解后用三氯甲烷萃取,经毛细管柱分离,NPD检测器检测,保留时问定性,以二苯胺作为内标物进行定量.结果 尿液中尼古丁和可替宁的检测范围分别为0.017~5μg/ml和0.024~5μg/ml,重复测定相对标准偏差(RSD)分别为1.7%~2.1%和1.5%~2.8%,加标回收率分别为102%~104%和90%~106%,回归方程分别为y=2.508x+0.072,r=0.999 2和y=1.797x+0.050 9,r=0.999 6;头发中尼古丁的检测范围为0.017~4μg/ml,重复测定相对标准偏差(RSD)为0.87%~2.5%,加标回收率92.5%~96.1%,回归方程为y=2.456x-0.054 6,r=0.999 8.本方法测定尼古丁和可替宁时,在进样1μl条件下,检出限分别为0.005μg/ml和0.007μg/ml,测定下限分别为0.017和0.024 μg/ml.结论 本方法适合测定主动吸烟和被动吸烟者体内的尼古丁和可替宁含量,评估暴露者的烟草暴露剂量和程度.%Objective To establish a gas chromatography standard method for the determination of nicotine and cotinine in urine and hair. Methods The urine and hair samples were digested with NaOH, extracted with trachloromethane,separated by capillary column and determined with NPD detector, diphenylamine as the internal standard substance. Results The samples of nicotine and cotinine were injected at 1 lμl respectively, and the limits of detection were 0.005 μg/ml and 0.007 μg/ml, and limits of quantification were 0.017 μg/ml and 0.024 μg/ml respectively. The linear ranges of nicotine and cotinine in urine were 0.017-5 μg/ml and 0.024-5 μg/ml, the relative standard deviations(RSD) of determination were 1.7%2.1% and 1.5%-2.8%, the rates of recovery of spiked samples were in the range of 102%-104% and 90%-106%, and the regression equations were y=2.508x+O.072, r=0.999 2 and y=l.797x+O.050 9, r=0.999 6. The linear range of nicotine in hair was 0.017-4

  13. Análise de ácidos graxos não-esterificados de plasma humano por cromatografia gasosa capilar com injeção sem divisão de fluxo Analysis of non-esterified fatty acids in human plasma by capillary gas-chromatography with splitless injection

    Directory of Open Access Journals (Sweden)

    Jacqueline G. Ney

    2004-08-01

    Full Text Available The aim of the present work was to test the combination of non-esterified fatty acid (NEFA isolation using fumed silicon dioxide with capillary gas-chromatography (C-GC with splitless injection for the analysis of NEFAs in human plasma. Injection volume, solvent re-condensation and split purge flow-rate were the parameters evaluated for the analysis of fatty acid methyl esters by C-GC. The use of a solvent re-condensation technique, associated with 1.0 µL injection and a split purge flow rate of 80 mL/min resulted in satisfactory analysis of NEFAs. Fourteen fatty acids were identified in plasma samples, ranging from 2.03 to 184.0 µmol/L. The combination of both techniques proved useful for routine analyses of plasma NEFAs.

  14. Principles of Micellar Electrokinetic Capillary Chromatography Applied in Pharmaceutical Analysis

    OpenAIRE

    Árpád Gyéresi; Eleonora Mircia; Brigitta Simon; Aura Rusu; Gabriel Hancu

    2013-01-01

    Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve...

  15. Tunable secondary dimension selectivity in comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    J. Mommers; G. Pluimakers; J. Knooren; T. Dutriez; S. van der Wal

    2013-01-01

    In this paper two tunable two-dimensional gas chromatography setups are compared and described in which the secondary dimension consists of two different capillary columns coupled in series. In the first setup the selectivity of the second dimension can be tuned by adjusting the effective column len

  16. HD gas analysis with Gas Chromatography and Quadrupole Mass Spectrometer

    CERN Document Server

    Ohta, T; Didelez, J -P; Fujiwara, M; Fukuda, K; Kohri, H; Kunimatsu, T; Morisaki, C; Ono, S; Rouille, G; Tanaka, M; Ueda, K; Uraki, M; Utsuro, M; Wang, S Y; Yosoi, M

    2011-01-01

    A gas analyzer system has been developed to analyze Hydrogen-Deuteride (HD) gas for producing frozen-spin polarized HD targets, which are used for hadron photoproduction experiments at SPring-8. Small amounts of ortho-H$_{2}$ and para-D$_{2}$ gas mixtures ($\\sim$0.01%) in the purified HD gas are a key to realize a frozen-spin polarized target. In order to obtain reliable concentrations of these gas mixtures in the HD gas, we produced a new gas analyzer system combining two independent measurements with the gas chromatography and the QMS. The para-H$_{2}$, ortho-H$_{2}$, HD, and D$_{2}$ are separated using the retention time of the gas chromatography and the mass/charge. It is found that the new gas analyzer system can measure small concentrations of $\\sim$0.01% for the otho-H$_2$ and D$_2$ with good S/N ratios.

  17. Application of micellar electrokinetic capillary chromatography for routine analysis of different materials

    Directory of Open Access Journals (Sweden)

    Injac Rade

    2008-01-01

    Full Text Available Micellar electrokinetic capillary chromatography (MEKC has become a popular mode among the several capillary electro-migration techniques. Most drug analysis can be performed by using MEKC because of its wide applicability. Separation of very complex mixtures, determination of drugs in the biological materials, etc., can be successfully achieved by MEKC. This review surveys typical applications of MEKC analysis. Recent advances in MEKC, especially with solid-phase extraction and large-volume sample stacking, are described. Modes of electrokinetic chromatography including MEKC, a separation theory of MEKC, environmental friendly analysis, and selectivity manipulation in MEKC are also briefly mentioned.

  18. Capillary gas chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco

    Institute of Scientific and Technical Information of China (English)

    LIU Hong-cheng; LI Qi-wan; TANG Li-bin

    2007-01-01

    Simple procedures for extraction and chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco are described. The determination was carried out by capillary gas chromatography (GC) with electron capture detection (ECD) and confirmed by GC-MS. The mean recoveries and relative standard deviation (RSD) were 93.2%~112.9% and 3.5%~6.7%, respectively at levels ranging from 0.01 to 0.1 mg/kg. The limit of determination was 0.001 mg/kg. Tobacco samples in routine check were successfully analyzed using the proposed method.

  19. A Simple and Inexpensive Capillary Holder for Thin-Layer Chromatography

    Science.gov (United States)

    Pintea, Beniamin-Nicolae V.

    2011-01-01

    Thin-layer chromatography (TLC) is a widely used method of qualitative analysis in organic synthesis, as it uniquely combines low cost, rapidity, simplicity, versatility, small quantities of sample and low detection limits. The simplest and most economical method for the application of samples onto TLC plates is by hand, using glass capillaries.…

  20. Capillary liquid chromatography using laser-based and mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Sepaniak, M.J.; Cook, K.D.

    1990-01-01

    The DOE-supported research performed during the past year has mainly focused on investigating and minimizing three problems that limit the practical utility of these capillary electrokinetic separation techniques in chemical analysis. (1) Analyses are hindered by poor reproducibility. This is largely a result of complicated and irreproducible capillary wall-solute interactions that often result in adsorption and mobility changes. (2) While the (micellar electrokinetic capillary chromatography) (MECC) technique permits the separations of neutral solutes, hydrophobic compounds are difficult to separate and manipulation of capacity factors (k's) is critically important. (3) The very small solute band volumes require that on-column detection be performed (usually optical detection) and this seriously limits detectability. In addition to these projects, the electrokinetic equivalent of affinity chromatography and development of remote fiber-optic sensors to measure chemical carcinogens and other compounds have been investigated. 5 refs., 2 figs.

  1. Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

    OpenAIRE

    Joris Meurs

    2016-01-01

    This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC), gas chromatography (GC) and supercritical fluid chromatography (SFC). To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI) was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a p...

  2. Determination of Camphor and Menthol in Xiaozhongzhitong Tincture by Capillary Gas Chromatography%毛细管气相色谱法测定消肿止痛酊中樟脑与薄荷脑的含量

    Institute of Scientific and Technical Information of China (English)

    张晓霞; 陈安家; 张一鸣; 王洁; 李霞; 李进冉

    2009-01-01

    Objective To establish a method for GC determination of Camphor and Menthol in Xiaozhongzhitong Tincture.Methods Capillary GC was adopted.The internal standard method was employed with octanol as internal standard.The GC system consisted of a flame ionization detector,PEG-20M capillary column(30 m×0.25 mm×0.25 μm),nitrogen as the carrier gas;oven temperature 160℃,detector temperature 250℃,N2:3 ml/min,H2:30 ml/min,Air:300ml/min,made up(N2):30 ml/min.Results Camphor and Menthol could be separated well under the chromatographic conditions.The linear range of Camphor was 3.00~18.00 μg/ml (r=0.999 2),and the linear range of the Menthol was 3.20~19.20 μg/ml(r=0.999 5);the recovery of Camphor was 98.5%~101.5%,and the recovery of Menthol was 97.6%~101.7%.Conclusion The method is simple,sensitive,accurate and has good repeatability,and it can be used to control the quality of Xiaozhongzhitong Tincture.%目的 建立测定消肿止痛酊中樟脑和薄荷脑含量的方法.方法 采用毛细管气相色谱法.色谱柱为PEG-20M石英毛细管柱(30 m×0.25 mm×0.25 μm);载气为氮气;正辛醇为内标;柱温160℃;氢火焰离子检测器;检测器和气化室的温度均为250℃;N2流速3 ml/min;H2流速30 ml/min;空气流速300 ml/min;尾吹气N2流速30 ml/min.结果 樟脑、薄荷脑和正辛醇能达到良好分离;樟脑的线性范围3.00~18.00 μg/ml(r=0.999 2),薄荷脑的线性范围3.20~19.20 μg/ml(r=0.999 5);樟脑的回收率98.5%~101.5%,薄荷脑的回收率97.6%~101.7%.结论 方法简便、准确、专属性强、重复性好,可用于消肿止痛酊的质量控制.

  3. Characterization of sulfur and nitrogen compounds in Brazilian petroleum derivatives using ionic liquid capillary columns in comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection.

    Science.gov (United States)

    Cappelli Fontanive, Fernando; Souza-Silva, Érica Aparecida; Macedo da Silva, Juliana; Bastos Caramão, Elina; Alcaraz Zini, Claudia

    2016-08-26

    Diesel and naphtha samples were analyzed using ionic liquid (IL) columns to evaluate the best column set for the investigation of organic sulfur compounds (OSC) and nitrogen(N)-containing compounds analyses with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry detector (GC×GC/TOFMS). Employing a series of stationary phase sets, namely DB-5MS/DB-17, DB-17/DB-5MS, DB-5MS/IL-59, and IL-59/DB-5MS, the following parameters were systematically evaluated: number of tentatively identified OSC, 2D chromatographic space occupation, number of polyaromatic hydrocarbons (PAH) and OSC co-elutions, and percentage of asymmetric peaks. DB-5MS/IL-59 was chosen for OSC analysis, while IL59/DB-5MS was chosen for nitrogen compounds, as each stationary phase set provided the best chromatographic efficiency for these two classes of compounds, respectively. Most compounds were tentatively identified by Lee and Van den Dool and Kratz retention indexes, and spectra-matching to library. Whenever available, compounds were also positively identified via injection of authentic standards.

  4. Analysis of insecticidal proteins from Bacillus thuringiensis and recombinant Escherichia coli by capillary electrokinetic chromatography.

    Science.gov (United States)

    Luong, John H T; Male, Keith B; Mazza, Alberto; Masson, Luke; Brousseau, Roland

    2004-10-01

    Bacillus thuringiensis and recombinant Escherichia coli proteinaceous protoxins were subject to proteolysis and analyzed by capillary electrokinetic chromatography. Three resulting toxins (65 kDa) were baseline-resolved within 22 min using a 10 mM borate, pH 11 separation buffer consisting of 25 mM sodium dodecyl sulfate (SDS) and 30 mM phytic acid. The toxins displayed differential interactions with the SDS and phytic acid phases to effect their separation. The ion-pairing interaction between the analyte and phytic acid was also useful in preventing adsorption to the capillary walls and thus enhanced separation resolution and efficiency. The use of electrokinetic chromatography allows achievement of the separation in a significantly shorter time than conventional high-performance liquid chromatography (HPLC) using a diethylaminoethyl (DEAE) weak-anion exchanger.

  5. Demonstrating Chemical and Analytical Concepts in the Undergraduate Laboratory Using Capillary Electrophoresis and Micellar Electrokinetic Chromatography

    Science.gov (United States)

    Palmer, Christopher P.

    1999-11-01

    This paper describes instrumental analysis laboratory exercises that utilize capillary electrophoresis and micellar electrokinetic chromatography to demonstrate several analytical and chemical principles. Alkyl parabens (4-hydroxy alkyl benzoates), which are common ingredients in cosmetic formulations, are separated by capillary electrophoresis. The electrophoretic mobilities of the parabens can be explained on the basis of their relative size. 3-Hydroxy ethylbenzoate is also separated to demonstrate the effect of substituent position on the acid dissociation constant and the effect this has on electrophoretic mobility. Homologous series of alkyl benzoates and alkyl phthalates (common plasticizers) are separated by micellar electrokinetic chromatography at four surfactant concentrations. This exercise demonstrates the separation mechanism of micellar electrokinetic chromatography, the concept of chromatographic phase ratio, and the concepts of micelle formation. A photodiode array detector is used in both exercises to demonstrate the advantages and limitations of the detector and to demonstrate the effect of pH and substituent position on the spectra of the analytes.

  6. Determination of Free-Energy Relationships Using Gas Chromatography

    Science.gov (United States)

    Snow, Nicholas H.

    1996-06-01

    By performing a few straightforward analyses on a gas chromatograph, it is possible to calculate the free energy, enthalpy, and entropy changes that occur when a compound transfers between the mobile and stationary phases. The partition theory of chromatography allows this transfer to be expressed as a chemical equlibrium. By calculating the equilibrium constant for this reaction from chromatographic retention times, the standard free energy change may be determined, and from this, the standard enthalpy and entropy changes. Also, by calculating these values at several temperatures for structurally related compounds, it is possible to explore the relationship between chromatographic retention, standard free energy, and the structure of a compound. These calculations were performed for groups of homologous alcohols, acetates, and hydrocarbons on packed and capillary column gas chromatographs, using both polar and non-polar columns, and on computer simulation software. It is seen that for homologous compounds, the relationship between standard free energy change in partitioning and hydrocarbon chain length for this reaction is linear. It is also seen that gas chromatography represents a useful tool for the calculation and comparison of thermodynamic properties of compounds and that straightforward exercise of this type allows training of students in chromatographic analysis, basic partition theory, thermodynamic relationships, and linear free energy relationships.

  7. Feasibility of the preparation of silica monoliths for gas chromatography: fast separation of light hydrocarbons.

    Science.gov (United States)

    Azzouz, Imadeddine; Essoussi, Anouar; Fleury, Joachim; Haudebourg, Raphael; Thiebaut, Didier; Vial, Jerome

    2015-02-27

    The preparation conditions of silica monoliths for gas chromatography were investigated. Silica-based monolithic capillary columns based on sol-gel process were tested in the course of high-speed gas chromatographic separations of light hydrocarbons mixture (C1-C4). The impact of modifying the amount of porogen and/or catalyst on the monolith properties were studied. At the best precursor/catalyst/porogen ratio evaluated, a column efficiency of about 6500 theoretical plates per meter was reached with a very good resolution (4.3) for very light compounds (C1-C2). The test mixture was baseline separated on a 70cm column. To our knowledge for the first time a silica-based monolithic capillary column was able to separate light hydrocarbons from methane to n-butane at room temperature with a back pressure in the range of gas chromatography facilities (under 4.1bar).

  8. 毛细管气相色谱法测定佐米曲普坦中6种残留溶剂量%Determination of 6 Residual Organic Solvents in Zolmitriptan by Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    谢华; 刘峰; 周振兴

    2012-01-01

    目的:建立佐米曲普坦原料药中6种残留有机溶剂(甲醇、异丙醇、二氯甲烷、乙酸乙酯、二氧六环、甲苯)量的测定方法.方法:采用气相色谱法.色谱柱为Agilent DB-624毛细管柱,载气为氮气,氢火焰离子化检测器,程序升温,进样口温度为200℃,检测器温度为250℃,分流直接进样,外标法计算残留溶剂的量.结果:甲醇、异丙醇、二氯甲烷、乙酸乙酯、二氧六环、甲苯检测浓度的线性范围分别为9.07× 10-2~4.54、9.92× 10-2~4.96、1.35× 10-2~0.68、9.54×10-2~4.77、8.33×10-3~0.42、1.77×10-2~0.88 mg·nL-1(r=0.996 9~0.998 9);平均回收率为97.53%~103.49%,RSD均≤1.35%.结论:本方法简单准确、灵敏度好,可用于控制佐米曲普坦原料药中残留溶剂量.%OBJECTIVE: To develop a method for the determination of 6 residual organic solvents (methanol, isopropanol, methylene chloride, ethyl acetate, 1, 4-dioxane, methylbenzene) in zolmitriptan. METHODS: GC method was adopted. The determination was performed on a Agilent DB-624 capillary column with FID detector. The carrier gas was nitrogen gas. The injector temperature was 200 ℃ and the detector temperature was 250 ℃ by temperature programming. Through direct splitting sample introduction, the content of residual solvents was calculated by external standard method. RESULTS: The linear ranges of methanol, isopropanol, methylene chloride, ethyl acetate, 1,4-dioxane, methylbenzene were 9.07×10-2~4.54, 9.92×10-2~4.96, 1.35×10-2~ 0.68, 9.54×10-2~4.77, 8.33×10-3~0.42, 1.77×10-2~0.88 mg·mL-1 (r=0.996 9-0.998 9). The average recoveries were 97.53%~103.49% (all RSD≤1.35%). CONCLUSION: The method is simple, accurate and sensitive, and can be used for the detection of residual organic solvents in zolmitriptan.

  9. Cromatografia gasosa bidimensional abrangente (GC × GC Comprehensive two-dimensional gas chromatography (GC × GC

    Directory of Open Access Journals (Sweden)

    Marcio Pozzobon Pedroso

    2009-01-01

    Full Text Available This paper presents the fundamental principles, instrumentation and selected applications of comprehensive two-dimensional gas chromatography (GC × GC. In this technique, introduced in 1991, two capillary columns are coupled and proper modulating interfaces continuously collect the eluate from the first column, transferring it to the second column. The result is a geometric increment in the chromatographic resolution, ensuring separation of extremely complex mixtures in time periods shorter or comparable to those of analysis using conventional gas chromatography and with better detectabilities and sensitivities.

  10. 毛细管气相色谱法同时检测工作场所空气中三氯乙烯和四氯乙烯%Simultaneous Detection of Trichloroethylene and Tetrachloroethylene in the Air of workplace by Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    李玉京; 张鑫; 王颖

    2015-01-01

    A method was established for simultaneous determination of trichloroethylene, tetrachloroethylene in the atmosphere by solvent desorption capillary gas chromatography. After being collected by activated carbon cube and desorpted with carbon disulfide, samples of atmosphere were determined by capillary gas chromatography. Under the conditions of 1.5 L sampling volume and 1.0 mL desorption volume, the linear range of trichloroethylene, tetrachloroethylene in the air was 0–212,0–204μg/mL, respectively. The linear correlation coefficients were all more than 0.999 9. Therelative standard deviations were less than 2.5%(n=6). The detection limits were 0.90, 1.15μg/mL, respectively. The minimum detectable concentration was 0.6,0.8 mg/m3, respectively. The desorption efficiency was 96.1%–98.1%. The method is simple with good separation effect, good linear amd short detection time, which is suitable to determine trichloroethylene, tetrachloroethylene in the atmosphere.%建立大气中三氯乙烯、四氯乙烯的溶剂解吸毛细管气相色谱测定方法。大气样品用活性炭管采集后以二硫化碳解吸,再用毛细管气相色谱法进行测定。在采样体积为1.5 L,解吸体积为1.0 mL的条件下,空气中三氯乙烯、四氯乙烯的线性范围分别为0~212μg/mL,0~204μg/mL,线性相关系数均大于0.9999,测定结果的相对标准偏差均小于2.5%(n=6),最低检出限分别为0.90,1.15μg/mL,最低检出浓度分别为0.6,0.8 mg/m3,解吸效率为96.1%~98.1%。该法操作简便,分离效果好,检测时间短,适于空气中三氯乙烯和四氯乙烯的检测。

  11. Non-planar microfabricated gas chromatography column

    Science.gov (United States)

    Lewis, Patrick R.; Wheeler, David R.

    2007-09-25

    A non-planar microfabricated gas chromatography column comprises a planar substrate having a plurality of through holes, a top lid and a bottom lid bonded to opposite surfaces of the planar substrate, and inlet and outlet ports for injection of a sample gas and elution of separated analytes. A plurality of such planar substrates can be aligned and stacked to provide a longer column length having a small footprint. Furthermore, two or more separate channels can enable multi-channel or multi-dimensional gas chromatography. The through holes preferably have a circular cross section and can be coated with a stationary phase material or packed with a porous packing material. Importantly, uniform stationary phase coatings can be obtained and band broadening can be minimized with the circular channels. A heating or cooling element can be disposed on at least one of the lids to enable temperature programming of the column.

  12. Chromatography, solid-phase extraction, and capillary electrochromatography with MIPs.

    Science.gov (United States)

    Tóth, Blanka; Horvai, George

    2012-01-01

    Most analytical applications of molecularly imprinted polymers are based on their selective adsorption properties towards the template or its analogs. In chromatography, solid phase extraction and electrochromatography this adsorption is a dynamic process. The dynamic process combined with the nonlinear adsorption isotherm of the polymers and other factors results in complications which have limited the success of imprinted polymers. This chapter explains these problems and shows many examples of successful applications overcoming or avoiding the problems.

  13. DESIGN AND CALIBRATION OF A CAPILLARY FLOWMETER SET FOR MEASUREMENT OF GAS FLOWS

    Directory of Open Access Journals (Sweden)

    Menderes LEVENT

    1998-01-01

    Full Text Available In this study, design and calibration of a capillary flowmeter set was represented. The capillary flowmeters will be used for measurements of small gas flows having laminar flow regime. The gases (such as, nitrogen, argon, methane, hydrogen and carbon-dioxide supplied from high pressure gas bottles and passed through capillary flowmeters (1 to 3 at various times. Each capillary flowmeter was made of glass and calibrated with one or two gases. Outlet of the capillary flowmeters were connected to the needle valves which have been used for regulating gas flowrates of the capillary flowmeters. Gases individually passed to a bubble flowmeter, and residence time of gases are recorded by using a stop watch. Then, from collected experimental results actual gas flowrates through the capillary flowmeters are calculated by using Hagen-Poiseuille equation.

  14. Analysis of Surrogate Contaminants in Paper-plastic Food Packaging Material by Capillary Gas Chromatography%纸塑复合食品包装材料中模拟污染物的GC检测技术

    Institute of Scientific and Technical Information of China (English)

    黄秀玲; 刘志刚; 王志伟; 许文才; 刘全校

    2009-01-01

    A GC-FID method was established for the determination of photoinitiators (PIs) in paper-plastic packaging material 4015 which solved in 95% ethanol. The pre-treatment protocol for 1 -hydroxycyclohexyl-phenyl ketone and 2 ,2-dimethoxy-2-phenylacotophenone in 95% ethanol was introduced. The influencing factors such as chromatography column, injection mode and velocity of flow of carrier gas were discussed. The results showed that the peaks of two PIs and impurity from paper were completely separated. The linearity was good (0. 999 7 and 0. 999 8) with the detection thresholds of 0. 05mg/L and 0. 1 mg/L, respectively. The RSDs were less than 5% , and the average recovery for Pis in 95% ethanol was in the range of 94% - 107% and 93% - 102% , respectively.%建立了纸塑复合包装材料4015中的模拟墨成分1-羟基环己基苯基甲酮和2,2-二甲氧基-苯基甲酮在脂肪性食品模拟物95%乙醇的气相色谱-氢火焰离子化检测器检测条件,并介绍了体积分数95%乙醇的前处理方法,讨论了色谱柱、进样方式、载气流速对测定的影响.分析结果表明:该法可将2种光引发剂和纸中杂质完全分离,具有较好的线性(相关系数分别为0.999 7和0.999 8),最低检出限分别为0.05 mg/L和0.1 mg/L,测定结果的相对标准偏差均<5.0%,样品在95%乙醇中的平均回收率分别为94%-107%和93%-102%.

  15. Effect of Micelle Composition on Acidic Drugs Separation Behavior by Micellar Electrokinetic Capillary Chromatography

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Micellar electrokinetic capillary chromatography (MECC) separation of four acidic drugs similar in structure was studied. Both anionic surfactant sodium dodecyl sulfate (SDS) and nonionic surfactant Tween 20 were used to form single micelles and mixed micelles as pseudostationary phases. The effects of the composition of micellar solution on retention behaviors were studied. The results indicate that there is markedly different selectivity among SDS, Tween 20 and the mixed micelles systems.

  16. 静态顶空毛细管柱气相色谱法测定生活饮用水中三氯甲烷和四氯化碳%Determination on Trichloromethane and Carbon tetrachloride in Drinking Water by Static Headspace Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    纪增香

    2012-01-01

    建立了静态顶空毛细管柱气相色谱法测定生活饮用水中三氯甲烷和四氯化碳的方法。实验结果显示:三氯甲烷和四氯化碳在其测定范围内线性关系良好,相关系数为0.998~0.997,回收率为89.0%~107.0%。该方法简便、快速、可行。%To establish a static headspace capillary gas chromatography method for the determination of trichloromethane and carbon tetrachloride in drinking water.The results showed that the trichloromehane and carbon tetrachloride in the scope had a good linear relationship,the correlation coefficient were all 0.998~0.997,the recovery rate were 89%~107%.The method is simple,rapid and feasible.

  17. 吸附管采样-毛细管柱气相色谱法测定环境空气和工业废气中的丙酮%Determination of acetone in ambient air and exhaust air by tube adsorption and capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    李承

    2016-01-01

    文章建立了以活性炭为填料的吸附管采集环境空气或工业废气中的丙酮,CS2进行解吸,并用毛细管柱气相色谱进行定性定量的方法。结果表明该方法简单灵敏,线性范围良好,检出限低,精密度好,定性定量准确;经实际样品测定,完全能满足环境空气和工业废气中丙酮的监测要求。%The method of determination of acetone in ambient air and exhaust air was established in the pa-per, which was using activated charcoal tube adsorption/carbon disulfide desorption and determined by capillary gas chromatography. The method was simple and sensitive, it also had broad linear scale, low MDL, good precision, accuracy qualitative and quantitative accuracy. The method can satisfy the demand of monitoring of acetone in am-bient air and exhaust air via the sample test.

  18. Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

    Science.gov (United States)

    Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn M.

    2000-01-01

    A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

  19. Two-dimensional separation of ionic species by hyphenation of capillary ion chromatography × capillary electrophoresis-mass spectrometry.

    Science.gov (United States)

    Beutner, Andrea; Kochmann, Sven; Mark, Jonas Josef Peter; Matysik, Frank-Michael

    2015-03-17

    The separation of complex mixtures such as biological or environmental samples requires high peak capacities, which cannot be established with a single separation technique. Therefore, multidimensional systems are in demand. In this work, we present the hyphenation of the two most important (orthogonal) techniques in ion analysis, namely, ion chromatography (IC) and capillary electrophoresis (CE), in combination with mass spectrometry. A modulator was developed ensuring a well-controlled coupling of IC and CE separations. Proof-of-concept measurements were performed using a model system consisting of nucleotides and cyclic nucleotides. The data are presented in a multidimensional contour plot. Analyte stacking in the CE separation could be exploited on the basis of the fact that the suppressed IC effluent is pure water.

  20. Preparation and evaluation of bonded linear polymethacrylate stationary phases for open tubular capillary electrokinetic chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Z.J.; Remcho, V.T. [West Virginia Univ., Morgantown, WV (United States)

    1997-02-15

    A new procedure for the preparation of thick polymethacrylate films bonded in 25 {mu}m i.d. fused-silica capillaries is developed. The etched silica surface is first modified with an unsaturated organosilane, which is later incorporated into the polymer film. The capillary is then filled with a monomer solution, and polymerization is initiated by incubation at elevated temperature. This thermoinitiation method enables the use of ordinary polyimide-jacketed capillaries in preparing the columns. The effect of monomer concentration on the resulting polymer film was studied by open tubular capillary electrokinetic chromatography using p-hydroxybenzoates (parabens) as test solutes. Good separations were achieved using short capillaries. Run-to-run retention time reproducibility was excellent, with RSDs of 2% (n = 50) being representative. For the linear polymer films produced, retention of analytes increased as the monomer concentration increased to a certain value, at which point the capacity factors level off with further increases in monomer concentration. The electroosmotic flow velocity decreases with increasing monomer concentration. The efficiency for an unretained test probe (acetone) reaches 270 000 plates/m. 13 refs., 10 figs., 1 tab.

  1. Chiral Recognition and Enantioseparation Mechanisms in Capillary Electrokinetic Chromatography

    Science.gov (United States)

    Chankvetadze, Bezhan

    This chapter deals with the basic theory of enantiomeric separations in electrokinetic chromatography (EKC) in general and with the relationships between the recognition and the separation of enantiomers in EKC, in particular. It is important to note that the dependence between recognition and separation is not as straightforward in EKC as it is in chromatographic separation techniques. Therefore, a clear understanding of these dependences is very important for the explanation of experimentally observed results, as well as for a design of new powerful separation systems, technologies, and materials. Cyclodextrins (CDs) are mainly discussed as chiral selectors not only because the author has a long-term experience of working with these multifunctional macrocycles but also because CDs belong to the most widely used chiral selectors in EKC. In addition, these materials are quite well-characterized molecules of medium size. In addition, CDs are used for separation of enantiomers almost in all analytical separation techniques, as well as for determination of the enantiomeric excess in nonseparation techniques such as nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry. This chapter does not address applications of chiral EKC in chemistry, pharmaceutical and biomedical, environmental, and food analyses.

  2. GC内标法同时测定刺山柑果实中3种刺激性成分的含量%Determination of Three Irritant Constituents of Cappers spinoza with Capillary Gas Chromatography by Using Internal Standard Method

    Institute of Scientific and Technical Information of China (English)

    郭小娜; 陈文; 张华; 任全霞; 刘珊珊

    2012-01-01

    目的:建立毛细管气相色谱法同时测定刺山柑果实中3种刺激性成分(异硫氰酸异丙酯、异硫氰酸甲酯、异硫氰酸异丁酯)的方法.方法:采用挥发油提取器提取挥发油;以异硫氰酸丁酯为内标物,用TM-FFAP毛细管柱分离,火焰离子化检测器检测;以保留时间定性,内标法定量.结果:在所选的色谱条件下,上述成分在46 min内获得较好的分离;3种成分与内标物的峰面积比值与其浓度呈良好的线性关系(r>0.9991);样品加标平均回收率为85.9% ~ 104%,RSD 2.44% ~3.12%.结论:方法简单、准确,可同时测定刺山柑果实中3种刺激性成分的含量,为其质量控制提供依据.%Objective: A capillary gas chromatographic method for the simultaneous determination of three irritant constituents ( isopropyl isothiocyanate, methyl isothiocyanate, isobutyl isothiocyanate) in Cappers spinoza was developed. Method: The essential oil was extracted by steam distillation. Butyl isothiocyanate was selected as the internal standard substance. The contents of three irritant components was analyzed by gas chromatography using a TM-FFAP capillary column and a flame ionization detector. The retention time of the peak was applied for qualitative analysis, and the internal standard method was used for quantitative analysis. Result: Three components were well separated in 46 min. There were good linear relationships between peak area ratio on the mass concentration and correlation coefficents above 0. 999 1. The average recoveries for the added standards and the RSD were 85. 9%-104% and 2. 44%-3. 12%, respectively. Conclusion: This method is simple and accurate for the irritation determination of volatile substances of C. Spinoza.

  3. Permanent gas analysis using gas chromatography with vacuum ultraviolet detection.

    Science.gov (United States)

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Fan, Hui; Hildenbrand, Zacariah; Wong, Derek; Wetz, David; Schug, Kevin A

    2015-04-03

    The analysis of complex mixtures of permanent gases consisting of low molecular weight hydrocarbons, inert gases, and toxic species plays an increasingly important role in today's economy. A new gas chromatography detector based on vacuum ultraviolet (VUV) spectroscopy (GC-VUV), which simultaneously collects full scan (115-240 nm) VUV and UV absorption of eluting analytes, was applied to analyze mixtures of permanent gases. Sample mixtures ranged from off-gassing of decomposing Li-ion and Li-metal batteries to natural gas samples and water samples taken from private wells in close proximity to unconventional natural gas extraction. Gas chromatography separations were performed with a porous layer open tubular column. Components such as C1-C5 linear and branched hydrocarbons, water, oxygen, and nitrogen were separated and detected in natural gas and the headspace of natural gas-contaminated water samples. Of interest for the transport of lithium batteries were the detection of flammable and toxic gases, such as methane, ethylene, chloromethane, dimethyl ether, 1,3-butadiene, CS2, and methylproprionate, among others. Featured is the capability for deconvolution of co-eluting signals from different analytes.

  4. Retention models for programmed gas chromatography.

    Science.gov (United States)

    Castello, G; Moretti, P; Vezzani, S

    2009-03-06

    The models proposed by many authors for the prediction of retention times and temperatures, peak widths, retention indices and separation numbers in programmed temperature and pressure gas chromatography by starting from preliminary measurements of the retention in isothermal and isobaric conditions are reviewed. Several articles showing the correlation between retention data and thermodynamic parameters and the determination of the optimum programming rate are reported. The columns of different polarity used for the experimental measurement and the main equations, mathematical models and calculation procedures are listed. An empirical approach was used in the early models, followed by the application of thermodynamic considerations, iterative calculation procedures and statistical methods, based on increased computing power now available. Multiple column arrangements, simultaneous temperature and pressure programming, applications of two-dimensional and fast chromatography are summarised.

  5. 衍生化毛细管气相色谱法同时测定无糖食品中的多种糖醇类甜味剂%Determination of Sugar Alcohols Sweeteners in Sugar-free Food by Derivatization Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    张雅珩; 周围; 李斌

    2013-01-01

    A capillary gas chromatographic method for simultaneous determination of sugar alcohol sweeteners in sugar-free food was set up.The sugar alcohols were extracted from samples with water.Then these extracts were purified,dried and derived to sugar alcohol acetates in the presence of pyridine and acetic anhydride (1 ∶ 1,V/V) at the temperature of 90 ℃ for 20 min.Furthermore the derivation reaction products were separated by gas chromatography with the OV-101 (50 m×0.25 mm×O.33 μm) capillary column,then determined by flame ionization detector and characterized by gas chromatography-mass spectrometry.The derivatives of erythritol,xylitol,mannitol,sorbitol and maltitol could be effectively separated from common sugars on the optimum chromatographic condition.The linear regression equations between the concentrations of the sugar alcohols and their peak areas of the derivatives were established in the range of 0.01-1.6 g/L.The correlation coefficients were 0.9995-0.9999.The average recovery was in the range of 74.6%-113.4%.The relative standard deviation is in the range of 2.4%-8.6%.The results demonstrated that the method had the advantages such as simplicity,rapid speed and reliability.The detection limits and recoveries were suitable for the determination of sugar alcohols sweeteners in sugar-free food.%建立了一种同时测定无糖食品中多种糖醇类甜味剂的气相色谱定量分析方法.样品中的糖醇经水提取,净化、脱水后,在吡啶-乙酸酐(1∶1,V/V)存在条件下,于90℃反应20 min,生成的糖醇乙酸酯衍生物用OV-101毛细管色谱柱(50 m×0.25 mm×0.33 μm)分离,氢火焰离子化检测器(FID)进行测定及气相色谱-质谱结构鉴定.在优化的色谱分析条件下,实现了赤藓糖醇、木糖醇、甘露糖醇、山梨糖醇和麦芽糖醇衍生物的理想分离,并排除了常见糖类对糖醇测定的干扰.本方法在0.01 ~ 1.6 mg/mL范围内,对糖醇浓度与其衍生物峰面积进行

  6. Determination of common organic poisons in workplace air by programmed capillary gas chromatography%程序升温毛细管气相色谱法同时测定工作场所空气中常见有机毒物

    Institute of Scientific and Technical Information of China (English)

    刘战峰; 周凯

    2013-01-01

    Objective:To explore and establish a method for determination of n-hexane,benzene,toluene,acetone,ethyl acetate,butyl acetate,ethyl benzene,(p,m,o) xylene,styrene and other organic poison by gas chromatography.Method:With temperature programming,INNOWAX capillary column,carbon disulfide-solvent desorption-gas chromatography were involved for determination.Results:Under the established experimental conditions,the 11 kinds of poisonous substances were separated well,with the recovery of 86.0% ~101% and detection limit of 0.5 μg/ml ~ 1.0 μg/ml,r > 0.999.Conclusion:The method had the advantages of good linearity,high accuracy,easy operation and rapidity,so it can be applied to simultaneous determination of 11 kinds of common organic poisons in workplace.%目的:探索和建立一种同时测定工作场所空气中常见的正己烷、丙酮、乙酸乙酯、苯、甲苯、乙酸丁酯、乙苯、(对、间、邻)二甲苯、苯乙烯等11种有机毒物的气相色谱法.方法:采用程序升温,用INNOWAX毛细管柱,溶剂解吸-气相色谱法测定.结果:在所建立的实验条件下,11种毒物分离良好,加标回收率在86.0%~101%之间,方法检测限在0.5μg/ml ~ 1.3 μg/ml之间.在方法测定范围内相关系数均大于0.999.结论:该方法线性好,准确度较高,操作简便、快速,可同时测定作业场所中常见的11种共存有机毒物.

  7. Monitoring of cefepime in human serum and plasma by micellar electrokinetic capillary chromatography: Improvement of sample preparation and validation by liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Šestáková, Nela; Theurillat, Regula; Sendi, Parham; Thormann, Wolfgang

    2017-02-20

    Cefepime monitoring in deproteinized human serum and plasma by micellar electrokinetic capillary chromatography and liquid chromatography coupled to mass spectrometry in presence of other drugs is reported. For micellar electrokinetic capillary chromatography, sample preparation comprised dodecylsulfate protein precipitation at pH 4.5 using an increased buffer concentration compared to that of a previous assay and removal of hydrophobic compounds with dichloromethane. This provided robust conditions for cefepime analysis in the presence of sulfamethoxazole and thus enabled its determination in samples of patients that receive co-trimoxazole. The liquid chromatography assay is based upon use of a column with a pentafluorophenyl-propyl modified and multi-endcapped stationary phase and the coupling to electrospray ionization with a single quadrupole detector. The performances of both assays with multi-level internal calibration were assessed with calibration and control samples and both assays were determined to be robust. Cefepime levels monitored by micellar electrokinetic capillary chromatography in samples from patients that were treated with cefepime only and with cefepime and co-trimoxazole were found to compare well with those obtained by liquid chromatography coupled to mass spectrometry. Cefepime drug levels determined by micellar electrokinetic capillary chromatography could thereby be validated. This article is protected by copyright. All rights reserved.

  8. Gas Flow Dynamics in Inlet Capillaries: Evidence for non Laminar Conditions

    Science.gov (United States)

    Wißdorf, Walter; Müller, David; Brachthäuser, Yessica; Langner, Markus; Derpmann, Valerie; Klopotowski, Sebastian; Polaczek, Christine; Kersten, Hendrik; Brockmann, Klaus; Benter, Thorsten

    2016-09-01

    In this work, the characteristics of gas flow in inlet capillaries are examined. Such inlet capillaries are widely used as a first flow restriction stage in commercial atmospheric pressure ionization mass spectrometers. Contrary to the common assumption, we consider the gas flow in typical glass inlet capillaries with 0.5 to 0.6 mm inner diameters and lengths about 20 cm as transitional or turbulent. The measured volume flow of the choked turbulent gas stream in such capillaries is 0.8 L·min-1 to 1.6 L·min-1 under typical operation conditions, which is in good agreement to theoretically calculated values. Likewise, the change of the volume flow in dependence of the pressure difference along the capillary agrees well with a theoretical model for turbulent conditions as well as with exemplary measurements of the static pressure inside the capillary channel. However, the results for the volume flow of heated glass and metal inlet capillaries are neither in agreement with turbulent nor with laminar models. The velocity profile of the neutral gas in a quartz capillary with an inner diameter similar to commercial inlet capillaries was experimentally determined with spatially resolved ion transfer time measurements. The determined gas velocity profiles do not contradict the turbulent character of the flow. Finally, inducing disturbances of the gas flow by placing obstacles in the capillary channel is found to not change the flow characteristics significantly. In combination the findings suggest that laminar conditions inside inlet capillaries are not a valid primary explanation for the observed high ion transparency of inlet capillaries under common operation conditions.

  9. 活性炭超声萃取-毛细管柱气相色谱法测水中痕量丙烯酰胺%Determination of trace acrylamide in water by ultrasonic extraction of activated carbon capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    王峰慧; 汤建新; 魏巍

    2011-01-01

    建立了一种活性炭超声萃取-毛细管柱气相色谱联用的方法,对水中痕量丙烯酰胺进行定量分析.通过对乙酸乙酯液液萃取,Agilent ODS-C18固相萃取柱(500 mg,6 mL)萃取以及活性炭超声萃取这三种方法进行了比较与优化,实验结果表明活性炭超声萃取方法对大体积水样的萃取效果最佳,并通过精密度,重现性和加标回收率等实验得到了论证.该方法最低检测限达到0.05/μg/mL,灵敏度高,重现性好,适用于痕量丙烯酰胺的分析.%An ultrasonic extraction of activated carbon-capillary gas chromatography method is established for the determination of trace acrylamide in water by comparing and optimizing ethyl acetate liquid-liquid extraction, agilent ODS-C18 solid phase extraction column (500 mg, 6 mL) extraction with ultrasonic extraction of activated carbon. The results showed that ultrasonic extraction of activated carbon was the best for extraction of water samples generally, which was demonstrated through the precision, reproducibility and recovery experiments. The detection limit of the method was 0. 05 μg/mL.This method is desirable for high sensitivity and good reproducibility, and it can be applied to determine the trace acrylamide.

  10. Sub-critical Column and Capillary Chromatography with Water as Mobile Phase and Flame Ionization Detection

    Institute of Scientific and Technical Information of China (English)

    LuFeng; LiLing; SunPeng; WuYutian

    2001-01-01

    A sub-critical chromatography (SubWC) with water as mobile phase and FID detection system is employed to separate several alcohols with high or medium polarity, with pure water as the eluent. The flow rate gets up to 50 μ1-min-1 for packed column (1 mm i.d.) and 70 μ1-min-1 for capillary (50 μm i.d.). Increasing the temperatureup to 140℃, together with temperature programming, markedly improves the separation and peak shapes within short analysis time. Sub-critical state is guaranteed.

  11. Assessing gibberellins oxidase activity by anion exchange/hydrophobic polymer monolithic capillary liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Chen, Ming-Luan; Su, Xin; Xiong, Wei; Liu, Jiu-Feng; Wu, Yan; Feng, Yu-Qi; Yuan, Bi-Feng

    2013-01-01

    Bioactive gibberellins (GAs) play a key regulatory role in plant growth and development. In the biosynthesis of GAs, GA3-oxidase catalyzes the final step to produce bioactive GAs. Thus, the evaluation of GA3-oxidase activity is critical for elucidating the regulation mechanism of plant growth controlled by GAs. However, assessing catalytic activity of endogenous GA3-oxidase remains challenging. In the current study, we developed a capillary liquid chromatography--mass spectrometry (cLC-MS) method for the sensitive assay of in-vitro recombinant or endogenous GA3-oxidase by analyzing the catalytic substrates and products of GA3-oxidase (GA1, GA4, GA9, GA20). An anion exchange/hydrophobic poly([2-(methacryloyloxy)ethyl]trimethylammonium-co-divinylbenzene-co-ethylene glycol dimethacrylate)(META-co-DVB-co-EDMA) monolithic column was successfully prepared for the separation of all target GAs. The limits of detection (LODs, Signal/Noise = 3) of GAs were in the range of 0.62-0.90 fmol. We determined the kinetic parameters (K m) of recombinant GA3-oxidase in Escherichia coli (E. coli) cell lysates, which is consistent with previous reports. Furthermore, by using isotope labeled substrates, we successfully evaluated the activity of endogenous GA3-oxidase that converts GA9 to GA4 in four types of plant samples, which is, to the best of our knowledge, the first report for the quantification of the activity of endogenous GA3-oxidase in plant. Taken together, the method developed here provides a good solution for the evaluation of endogenous GA3-oxidase activity in plant, which may promote the in-depth study of the growth regulation mechanism governed by GAs in plant physiology.

  12. Assessing gibberellins oxidase activity by anion exchange/hydrophobic polymer monolithic capillary liquid chromatography-mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Ming-Luan Chen

    Full Text Available Bioactive gibberellins (GAs play a key regulatory role in plant growth and development. In the biosynthesis of GAs, GA3-oxidase catalyzes the final step to produce bioactive GAs. Thus, the evaluation of GA3-oxidase activity is critical for elucidating the regulation mechanism of plant growth controlled by GAs. However, assessing catalytic activity of endogenous GA3-oxidase remains challenging. In the current study, we developed a capillary liquid chromatography--mass spectrometry (cLC-MS method for the sensitive assay of in-vitro recombinant or endogenous GA3-oxidase by analyzing the catalytic substrates and products of GA3-oxidase (GA1, GA4, GA9, GA20. An anion exchange/hydrophobic poly([2-(methacryloyloxyethyl]trimethylammonium-co-divinylbenzene-co-ethylene glycol dimethacrylate(META-co-DVB-co-EDMA monolithic column was successfully prepared for the separation of all target GAs. The limits of detection (LODs, Signal/Noise = 3 of GAs were in the range of 0.62-0.90 fmol. We determined the kinetic parameters (K m of recombinant GA3-oxidase in Escherichia coli (E. coli cell lysates, which is consistent with previous reports. Furthermore, by using isotope labeled substrates, we successfully evaluated the activity of endogenous GA3-oxidase that converts GA9 to GA4 in four types of plant samples, which is, to the best of our knowledge, the first report for the quantification of the activity of endogenous GA3-oxidase in plant. Taken together, the method developed here provides a good solution for the evaluation of endogenous GA3-oxidase activity in plant, which may promote the in-depth study of the growth regulation mechanism governed by GAs in plant physiology.

  13. Physico-chemical characterization of liposomes and drug substance-liposome interactions in pharmaceutics using capillary electrophoresis and electrokinetic chromatography

    DEFF Research Database (Denmark)

    Franzen, Ulrik; Østergaard, Jesper

    2012-01-01

    Liposomes are self-assembled phospholipid vesicles and have numerous research and therapeutic applications. In the pharmaceutical and biomedical sciences liposomes find use as models of biological membranes, partitioning medium and as drug carriers. The present review addresses the use of capillary...... electrophoresis and liposome electrokinetic chromatography for the characterization of liposomes in a pharmaceutical context. Capillary electrophoretic techniques have been used for the measurement of electrophoretic mobility, which provides information on liposome surface charge, size and membrane permeability...... of liposomes. The use of liposome electrokinetic chromatography and capillary electrophoresis for determination of liposome/water partitioning and characterization of drug-liposome interactions is reviewed. A number of studies indicate that capillary electrophoresis may have a role in the characterization...

  14. Characterization of pulsed capillary channel gas puff target using EUV shadowgraphy

    Energy Technology Data Exchange (ETDEWEB)

    Wachulak, P.W., E-mail: wachulak@gmail.com; Bartnik, A.; Węgrzyński, Ł.; Fok, T.; Kostecki, J.; Szczurek, M.; Jarocki, R.; Fiedorowicz, H.

    2015-02-15

    Characterization measurements of a pulsed capillary channel gas puff target, developed for applications in laser-matter interaction experiments, are presented. The target is produced by pulsed injection of gas through a slit-shaped nozzle into a capillary channel and has been characterized by EUV radiography at 13.5 nm wavelength. Time dependent gas flow effects and flow shaping by capillary walls were visualized. Density measurements for argon were performed on axis for variable timing conditions and variable backing pressures. This target, due to its advantages, might be an interesting alternative for lower repetition rate and higher energy laser-matter interaction experiments.

  15. Comparison of monolithic capillary electrochromatography and micellar electrokinetic chromatography for the separation of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Salwiński, Aleksander; Delépée, Raphaël

    2014-05-01

    Atmospheric pollution of anthropic origin is recognized as a major risk factor for health, in particular for respiratory and cardio-vascular systems. Among these pollutants, polycyclic aromatic hydrocarbons (PAHs) are placed on the list of US Environmental Protection Agency (EPA) as 'priority' pollutants and four of them are assigned as potential carcinogens by The International Agency for Research on Cancer (IARC). In the present work two capillary techniques-micellar electrokinetic chromatography (MEKC) and monolithic capillary electrochromatography (CEC)-were compared for the separation of eleven PAHs. Both techniques compared in the present work are fully compatible with every standard apparatus of capillary electrophoresis. For MEKC, enhancement of selectivity and decrease of the separation window of eleven PAHs were obtained with methanol:borate 25 mM (20/80, v/v) running buffer containing 10 mM of hydroxypropylated γ-cyclodextrins with low SDS content (25 mM). In case of CEC, two acrylate-based monolithic stationary phases (MSPs) were evaluated for their application in the separation of eleven PAHs. The best MSP based on butyl acrylate was compared with MEKC in terms of sample capacity, PAHs elution order, LOQ, efficiency and effect of pH. Influence of the hydrophobicity of mobile phase on the PAHs elution order was also studied.

  16. Coating properties of a novel water stationary phase in capillary supercritical fluid chromatography.

    Science.gov (United States)

    Murakami, Jillian N; Thurbide, Kevin B

    2015-05-01

    The coating properties of a novel water stationary phase used in capillary supercritical fluid chromatography were investigated. The findings confirm that increasing the length or internal diameter of the type 316 stainless-steel column used provides a linear increase in the volume of stationary phase present. Under normal operating conditions, results indicate that about 4.9 ± 0.5 μL/m of water phase is deposited uniformly inside of a typical 250 μm internal diameter 316 stainless-steel column, which translates to an area coverage of about 6.3 ± 0.5 nL/mm(2) regardless of dimension. Efforts to increase the stationary phase volume present showed that etching the stainless-steel capillary wall using hydrofluoric acid was very effective for this. For instance, after five etching cycles, this volume doubled inside of both the type 304 and the type 316 stainless-steel columns examined. This in turn doubled analyte retention, while maintaining good peak shape and column efficiency. Overall, 316 stainless-steel columns were more resistant to etching than 304 stainless-steel columns. Results indicate that this approach could be useful to employ as a means of controlling the volume of water stationary phase that can be established inside of the stainless-steel columns used with this supercritical fluid chromatography technique.

  17. Simulating retention in gas-liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Martin, M.G.; Siepmann, J.I.; Schure, M.R.

    1999-12-16

    Accurate predictions of retention times, retention indices, and partition constants are a long sought-after goal for theoretical studies in chromatography. Configurational-bias Monte Carlo (CBMC) simulations in the Gibbs ensemble using the transferable potentials for phase equilibria-united atom (TraPPE-UA) force field have been carried out to obtain a microscopic picture of the partitioning of 10 alkane isomers between a helium vapor phase and a squalane liquid phase, a protypical gas-liquid chromatography system. The alkane solutes include some topological isomers that differ only in the arrangement of their building blocks (e.g., 2,5-dimethylhexane and 3,4-dimethylhexane), for which the prediction of the retention order is particularly difficult. The Kovats retention indices, a measure of the relative retention times, are calculated directly from the partition constants and are in good agreement with experimental values. The calculated Gibbs free energies of transfer for the normal alkanes conform to Martin's equation which is the basis of linear free energy relationships used in many process modeling packages. Analysis of radial distribution functions and the corresponding energy integrals does not yield evidence for specific retention structures and shows that the internal energy of solvation is not the main driving force for the separation of topological isomers in this system.

  18. Forensic potential of comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Sampat, A.; Lopatka, M.; Sjerps, M.; Vivo-Truyols, G.; Schoenmakers, P.; van Asten, A.

    2016-01-01

    In this study, the application of comprehensive two-dimensional (2D) gas chromatography (GC × GC) in forensic science is reviewed. The peer-reviewed publications on the forensic use of GC × GC and 2D gas chromatography with mass spectrometric detection (GC × GC-MS) have been studied in detail, not o

  19. 顶空气相色谱法测定大孔树脂提取物中的残留溶剂研究%Determination of residual solvents in macroporous resin extracts by Head-space capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    刘冬; 杨敬芝; 杜守颖; 张东明; 赵立敏; 陈雯

    2009-01-01

    目的:建立了测定大孔树脂淫羊藿提取物、栀子提取物以及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯残留有机溶剂含量的顶空气相色谱法.方法:采用顶空气相色谱法,FID检测器,以20%~50%二甲基亚砜为溶媒,顶空预热温度为90℃,预热时间为10 min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用DB-1交联毛细管柱(60m×0.32mm,1 μm),程序升温,实现了各组分的基线分离.结果:乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯在各自对应的浓度范围内,线性关系良好;乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯的最小检测限分别为2.72,0.22,0.03,0.03,0.28,0.33,0.03,0.31 μg·mL~(-1);加样回收率均在75%以上,精密度较好.结论:经方法学验证,该方法灵敏、准确、可靠,可适用于大孔树脂淫羊藿提取物、栀子提取物及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯等残留有机溶剂的测定.%Objective:This paper reports a Head-space GC method for determination of enthanol,hexane,benzene,toluene,methyl cyclohexane,xylene,styrene,divinyl benzene in macroporous resin extractions.Method:The analytical coluren was DB-1(60m×0.32mm,1μm).The injector temperature was 180℃ and the detector tempemture was 250℃.The column temperature was programmed raised.The carrier gas was nitrogen and the solvent was 20%-50% dimethyl sulfoxide.Results:The stand curve were linear for each solvents in the range of each consistencv.The average recoveries were all more than 75%.Conclusion:This method is simple,rapid and precise,it is suitable for measurement of residual solvents in macroporous resin extracts.

  20. Applications of resistive heating in gas chromatography: a review.

    Science.gov (United States)

    Jacobs, Matthew R; Hilder, Emily F; Shellie, Robert A

    2013-11-25

    Gas chromatography is widely applied to separate, identify, and quantify components of samples in a timely manner. Increasing demand for analytical throughput, instrument portability, environmental sustainability, and more economical analysis necessitates the development of new gas chromatography instrumentation. The applications of resistive column heating technologies have been espoused for nearly thirty years and resistively heated gas chromatography has been commercially available for the last ten years. Despite this lengthy period of existence, resistively heated gas chromatography has not been universally adopted. This low rate of adoption may be partially ascribed to the saturation of the market with older convection oven technology, coupled with other analytical challenges such as sampling, injection, detection and data processing occupying research. This article assesses the advantages and applications of resistive heating in gas chromatography and discusses practical considerations associated with adoption of this technology.

  1. Aspects of High-Resolution Gas Chromatography as Applied to the Analysis of Hydrocarbon Fuels and Other Complex Organic Mixtures. Volume 1

    Science.gov (United States)

    1985-02-01

    appendices were reviewed by Jerry Strange. Anita Cochran has been especially helpful in correcting my many grammar errors and has improved the readability of...Mechanism of Response of Flame lonization Detectors, In; Gas Chromatography, W. Brenner , J. E. Callen, and M. D. Weiss, eds.. Academic Press, New...T. Swanton, Performance of Coated Capillary Columns, In: Gas Chromatography, N. Brenner , J. E. Callen, and M. D. Weiss, eds.. Academic Press, New

  2. Determination of 5 Kinds of Residual Organic Solvents in Thyroid Tablets by Headspace Capillary Gas Chromatography%顶空毛细管气相色谱法测定甲状腺片中5种有机溶剂残留量

    Institute of Scientific and Technical Information of China (English)

    罗文艳; 段和祥

    2012-01-01

    OBJECTIVE: To establish a method for the content determination of 5 kinds of residual organic solvents in thyroid tablets, I.e. Methanol, ethanol, acetone, ether and ethyl acetate. METHODS: Headspace capillary gas chromatography was adopted. The residual organic solvents were separated on DB-1 capillary column with FID detector. The carried gas was nitrogen. The injector temperature and detector temperature were controlled at 200℃ and 250℃, respectively. The column temperature was raised by program. The sample was dissolved in dimethyl sulfoxide. The containers of head-space injector were in equilibrium at 100℃ for 30 min, and the splitting-ratio was 10:1. RESULTS: The measured solvents were separated completely (r ranged 0.999 6~0.999 9). The detection limits were 0.6 μg·mL-1, 2.0 μg·mL-1, 1.0 μg·mL-1, 0.2 μg·mL-1, 0.1 μg·mL-1, respectively. The average recovery rates were 98.6%~100.3% (RSD=0.53%~1.32%). The residual organic solvents of 3 batches of samples were within standard range. CONCLUSION: The established method is simple, rapid, sensitive and accurate. It is suitable for the content determination of residual organic solvents in thyroid tablets.%目的:建立测定甲状腺片中甲醇、乙醇、丙酮、乙醚、乙酸乙酯5种有机溶剂残留量的方法.方法:采用顶空毛细管气相色谱法.色谱柱为DB-1石英毛细管柱,载气为氮气,进样口温度为200℃,氢火焰离子化检测器温度为250℃,程序升温;顶空进样,顶空瓶温度为100℃,平衡时间为30min,分流比为10∶1,溶剂为二甲基亚砜.结果:甲醇、乙醇、丙酮、乙醚、乙酸乙酯5种有机溶剂分离较好;线性关系,为0.9996~0.9999,检测限分别为0.6、2.0、1.0、0.2、0.1μg·mL-1;平均回收率为98.6%~100.3%,RSD为0.53%~1.32%.3批样品中有机溶剂残留量均在合格范围内.结论:所建立的方法简便、快捷、灵敏度高,结果准确,适用于甲状腺片中有机溶剂残留量的检测.

  3. EFFECT OF SURFACTANT ON TWO-PHASE FLOW PATTERNS OF WATER-GAS IN CAPILLARY TUBES

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Flow patterns of liquid-gas two-phase flow were experimentally investigated. The experiments were carried out in both vertical and horizontal capillary tubes having inner diameters of 1.60 mm. The working liquid was the mixture of water and Sodium Dodecyl Benzoyl Sulfate (SDBS). The working gas was Nitrogen. For the water/SDBS mixture-gas flow in the vertical capillary tube, flow-pattern transitions occurred at lower flow velocities than those for the water-gas flow in the same tube. For the water/SDBS mixture-gas flow in the horizontal capillary tube, surface tension had little effect on the bubbly-intermittent transition and had only slight effect on the plug-slug and slug-annular transitions. However, surface tension had significant effect on the wavy stratified flow regime. The wavy stratified flow regime of water/SDBS mixture-gas flow expanded compared with that of water-gas.

  4. Vacuum ultraviolet detector for gas chromatography.

    Science.gov (United States)

    Schug, Kevin A; Sawicki, Ian; Carlton, Doug D; Fan, Hui; McNair, Harold M; Nimmo, John P; Kroll, Peter; Smuts, Jonathan; Walsh, Phillip; Harrison, Dale

    2014-08-19

    Analytical performance characteristics of a new vacuum ultraviolet (VUV) detector for gas chromatography (GC) are reported. GC-VUV was applied to hydrocarbons, fixed gases, polyaromatic hydrocarbons, fatty acids, pesticides, drugs, and estrogens. Applications were chosen to feature the sensitivity and universal detection capabilities of the VUV detector, especially for cases where mass spectrometry performance has been limited. Virtually all chemical species absorb and have unique gas phase absorption cross sections in the approximately 120-240 nm wavelength range monitored. Spectra are presented, along with the ability to use software for deconvolution of overlapping signals. Some comparisons with experimental synchrotron data and computed theoretical spectra show good agreement, although more work is needed on appropriate computational methods to match the simultaneous broadband electronic and vibronic excitation initiated by the deuterium lamp. Quantitative analysis is governed by Beer-Lambert Law relationships. Mass on-column detection limits reported for representatives of different classes of analytes ranged from 15 (benzene) to 246 pg (water). Linear range measured at peak absorption for benzene was 3-4 orders of magnitude. Importantly, where absorption cross sections are known for analytes, the VUV detector is capable of absolute determination (without calibration) of the number of molecules present in the flow cell in the absence of chemical interferences. This study sets the stage for application of GC-VUV technology across a wide breadth of research areas.

  5. On-line sample treatment - Capillary gas chromatography

    NARCIS (Netherlands)

    Goosens, EC; de Jong, D; de Jong, GJ; Brinkman, UAT

    1998-01-01

    Sample pretreatment is often the bottleneck of a trace level analytical procedure. In order to increase performance, increasing attention is therefore being devoted to combining sample pretreatment on-line with the separation technique that has to be used. In the present review, a variety of procedu

  6. Semi-targeted analysis of metabolites using capillary-flow ion chromatography coupled to high-resolution mass spectrometry.

    Science.gov (United States)

    Burgess, Karl; Creek, Darren; Dewsbury, Paul; Cook, Ken; Barrett, Michael P

    2011-11-30

    This work describes a novel application of capillary-flow ion chromatography mass spectrometry for metabolomic analysis, and comparison of the technique to octadecyl silica and hydrophilic interaction chromatography (HILIC)-based mass spectrometry. While liquid chromatography/mass spectrometry (LC/MS) is rapidly becoming the standard technique for metabolomic analysis, metabolomic samples are extremely heterogeneous, leading to a requirement for multiple methods of analysis and separation techniques to perform a 'global' metabolomic analysis. While C18 is suitable for hydrophobic metabolites and has been used extensively in pharmaceutical drug metabolism studies, HILIC is, in general, efficient at separating polar metabolites. Phosphorylated species and organic acids are challenging to analyse and effectively quantitate on both systems. There is therefore a requirement for an MS-compatible analytical technique that can separate negatively charged compounds, such as ion-exchange chromatography. Evaluation of capillary flow ion chromatography with electrolytic suppression was performed on a library of metabolite standards and was shown to effectively separate organic acids and sugar di- and tri-phosphates. Limits of detection for these compounds range from 0.01 to 100 pmol on-column. Application of capillary ion chromatography to a comparative analysis of energy metabolism in procyclic forms of the parasitic protozoan Trypanosoma brucei where cells were grown on glucose or proline as a carbon source was demonstrated to be more effective than HILIC for detection of the organic acids that comprise glucose central metabolism and the tricarboxylic acid (TCA) cycle.

  7. Determination of alkyl methanesulfonates in doxazosin mesylate by gas chromatography-mass spectrometer

    Directory of Open Access Journals (Sweden)

    C Sitaram

    2011-01-01

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

  8. Simultaneous determination of eleven preservatives in food by capillary column-gas chromatography after ultrasound-assisted dispersive liquid-liquid microextraction%超声分散液相微萃取-气相色谱法同时测定食品中11种防腐剂

    Institute of Scientific and Technical Information of China (English)

    杨金玲; 江阳; 薛勇; 孙成均

    2015-01-01

    目的:建立食品中11种防腐剂的超声分散液相微萃取-气相色谱法。方法样品经9∶1二氯甲烷‐乙酸乙酯超声分散液相微萃取,FFAP毛细管色谱柱分离、FID 检测器检测。结果方法线性范围为0.068~400μg/m l ,相关系数为0.9990~0.9999,回收率为84%~122%,相对标准偏差为3.11%~5.83%,方法检出限为0.026~0.23μg/m l。结论该法简便、高效、经济、环境友好,适于不同食品中11种防腐剂同时快速测定。%Objective To establish a method for simultaneous determination of eleven preservatives in foods by gas chromatography after ultrasound‐assisted dispersive liquid-liquid microextraction .Methods The target pre‐servatives in food samples were ultrasound‐assisted dispersive liquid-liquid microextracted ,and then they were separated with FFAP capillary column and detected with FID detector .Results Linear ranges of the method were between 0 .068 and 400μg/mL with correlation coefficients varying from 0 .9990 to 0 .9999 .Recoveries and rela‐tive standard deviations (RSDs)were in the range from 84% to 122% and from 3 .11% to 5 .83% ,respectively . The limitation of detection was in the range form 0 .026μg/ml to 0 .23μg/ml with enrichment factors ranging from 57 to 225 for all target compounds .Conclusion The method is simple ,efficient ,cheap ,eco‐friendly and is suitable for simultaneous determination of 11 preservatives in different foods .

  9. A validated capillary gas chromatography method for guaco (Mikania glomerata S. quality control and rastreability: from plant biomass to phytomedicines Método validado por cromatografia gasosa capilar para o controle de qualidade e rastreabilidade de guaco (Mikania glomerata S.: da matéria-prima ao fitoterápico

    Directory of Open Access Journals (Sweden)

    Paula C. P. Bueno

    2009-03-01

    Full Text Available This work describes a full validation of a capillary gas chromatography analytical methodology using internal standardization for the quantification of coumarin (1,2-benzopyrone in guaco (Mikania glomerata Spreng - Asteraceae products: syrup, plant and its extract, including the stability study of the phytomedicine. For the analysis, it was used an HP-5 capillary column (30 m x 0.32 mm x 0.25 µm, hydrogen at a flow rate of 1.8 mL/min and the increasing temperature gradient was: 100 ºC to 250 ºC, 15 ºC/min. The temperature of injector (split 1:20 and detector were kept at 250 ºC and 270 ºC, respectively. The retention times of the standards for the above conditions were 2.86 minutes for 1, 2, 3, 4-tetramethylbenzene, 4.45 min for piperonal (internal standards, and 5.36 minutes for coumarin. After extraction procedure, the recovery of coumarin determined for plant raw material was 101.6 %, while for syrup it was 100.8 %. Detection and quantification limits were 0.5 µg/mL and 1.5 µg/mL, respectively. Precision was determined for all samples and the results were lower than 2.5 %. The total amount of coumarin in plant raw material, its extract and syrup were 0.38% w/w, 1.33 mg/mL and 0.143 mg/mL, respectively.Este trabalho descreve a validação completa de metodologia analítica empregando cromatografia gasosa capilar com padronização interna para quantificação da cumarina (1,2-benzopirona em produtos contendo guaco (Mikania glomerata Spreng - Asteraceae: xarope, planta e extrato padronizado, além do estudo de estabilidade do fitoterápico em questão. Utilizou-se uma coluna capilar HP-5 (30 m x 0,32 mm x 0,25 µm, hidrogênio a 1,8 mL/min e rampa de temperatura de 100 ºC a 250 ºC, a 15 ºC/min. A temperatura do injetor (split 1:20 foi de 250 ºC, enquanto a do detector foi de 270 ºC. Os tempos de retenção dos padrões foram: 2,86 minutos para o 1, 2, 3, 4-tetrametilbenzeno, 4,45 minutos para o piperonal (padrões internos e 5

  10. Pseudo Peak Phenomena in Micellar Electrokinetic Capillary Chromatography by Using Ionic Surfactant

    Institute of Scientific and Technical Information of China (English)

    CHENGuan-hua; YANGGeng-liang; TIANYi-ling; CHENYi

    2003-01-01

    The origin of pseudo peak was studied by means of micellar electrokinetic capillary chromatography with cetyltrimethylaminium bormide as the pseudo stationary phase.It has been pointed that two peaks may appear for one component under certain conditions.Experiments showed that the relative areas of the two peaks of analyte depended on the time and the temperature of reaction between analyte and surfactant,and the concentration of surfactant in the sample solution.It means that the interaction between the analyte and the surfactant is a slow process,and a stable substance can be produced from the interaction.It is the substance and the analyte that may lead to the formation of two peaks.The fast interaction mechanism between the solute and the micellar should be queried from the experiment result.

  11. Pseudo Peak Phenomena in Micellar Electrokinetic Capillary Chromatography by Using Ionic Surfactant

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    The origin of pseudo peak was studied by means of micellar electrokinetic capillary chromatography with cetyltrimethylaminium bromide as the pseudo stationary phase. It has been pointed that two peaks may appear for one component under certain conditions. Experiments showed that the relative areas of the two peaks of analyte depended on the time and the temperature of reaction between analyte and surfactant, and the concentration of surfactant in the sample solution. It means that the interaction between the analyte and the surfactant is a slow process, and a stable substance can be produced from the interaction. It is the substance and the analyte that may lead to the formation of two peaks. The fast interaction mechanism between the solute and the micellar should be queried from the experiment result.

  12. Two-peak phenomena and formation origin in micellar electrokinetic capillary chromatography

    Institute of Scientific and Technical Information of China (English)

    CHEN; Guanhua(陈冠华); YANG; Gengliang(杨更亮); TIAN; Yiling(田益玲); CHEN; Yi(陈义)

    2003-01-01

    The formation origin of two peaks in micellar electrokinetic capillary chromatography by using cetyltrimethylaminium bromide (or sodium dodecyl sulfate) as pseudo stationary phase is studied. It is pointed out that two peaks may appear for one component in certain conditions. Experiments show that the relative areas of the two peaks of the corresponding component depend on the time and temperature of reaction between the analyte and the surfactant, and the concentration of surfactant in the sample solution. One of the two peaks increase with the increase of surfactant concentration in the sample solution while reverse for another peak. Temperature can accelerate the reaction process. This means that the interaction between analyte and surfactant is a slow process, and a stable substance can be produced from the interaction and leads to the formation of two peaks. The standpoint is confirmed by the infrared and nuclear magnetic resonance spectra of the product from the reaction between cetyltrimethylaminium bromide and m-hydroxyl benzoic acid.

  13. Analysis of Soft Drinks: UV Spectrophotometry, Liquid Chromatography, and Capillary Electrophoresis

    Science.gov (United States)

    McDevitt, Valerie L.; Rodriguez, Alejandra; Williams, Kathryn R.

    1998-05-01

    Instrumental analysis students analyze commercial soft drinks in three successive laboratory experiments. First, UV multicomponent analysis is used to determine caffeine and benzoic acid in Mello YelloTM using the spectrophotometer's software and manually by the simultaneous equations method. The following week, caffeine, benzoic acid and aspartame are determined in a variety of soft drinks by reversed-phase liquid chromatography using 45% methanol/55% aqueous phosphate, pH 3.0, as the mobile phase. In the third experiment, the same samples are analyzed by capillary electrophoresis using a pH 9.4 borate buffer. Students also determine the minimum detection limits for all three compounds by both LC and CE. The experiments demonstrate the analytical use and limitations of the three instruments. The reports and prelab quizzes also stress the importance of the chemistry of the three compounds, especially the relationships of acid/base behavior and polarity to the LC and CE separations.

  14. Using contemporary liquid chromatography theory and technology to improve capillary gradient ion-exchange separations.

    Science.gov (United States)

    Wouters, Bert; Broeckhoven, Ken; Wouters, Sam; Bruggink, Cees; Agroskin, Yury; Pohl, Christopher A; Eeltink, Sebastiaan

    2014-11-28

    The gradient-performance limits of capillary ion chromatography have been assessed at maximum system pressure (34.5 MPa) using capillary columns packed with 4.1 μm macroporous anion-exchange particles coated with 65 nm positively-charged nanobeads. In analogy to the van-Deemter curve, the gradient performance was assessed applying different flow rates, while decreasing the gradient time inversely proportional to the increase in flow rate in order to maintain the same retention properties. The gradient kinetic-performance limits were determined at maximum system pressure, applying tG/t0=5, 10, and 20. In addition, the effect of retention on peak width was assessed in gradient mode for mono-, di-, and trivalent inorganic anions. The peak width of late-eluting ions can be significantly reduced by using concave gradient, resulting in better detection sensitivity. A signal enhancement factor of 8 was measured for a late-eluting ion when applying a concave instead of a linear gradient. For the analysis of a complex anion mixture, a coupled column with a total length of 1.05 m was operated at the kinetic-performance limit applying a linear 250 min gradient (tG/t0=10). The peak capacity varied between 200 and 380 depending on analyte retention, and hence on charge and size of the ion.

  15. Stereospecific micellar electrokinetic chromatography assay of methionine sulfoxide reductase activity employing a multiple layer coated capillary.

    Science.gov (United States)

    Zhu, Qingfu; El-Mergawy, Rabab G; Heinemann, Stefan H; Schönherr, Roland; Jáč, Pavel; Scriba, Gerhard K E

    2013-09-01

    A micellar electrokinetic chromatography method for the analysis of the l-methionine sulfoxide diastereomers employing a successive multiple ionic-polymer layer coated fused-silica capillary was developed and validated in order to investigate the stereospecificity of methionine sulfoxide reductases. The capillary coating consisted of a first layer of hexadimethrine and a second layer of dextran sulfate providing a stable strong cathodic EOF and consequently highly repeatable analyte migration times. The methionine sulfoxide diastereomers, methionine as product as well as β-alanine as internal standard were derivatized by dabsyl chloride and separated using a 35 mM sodium phosphate buffer, pH 8.0, containing 25 mM SDS as BGE and a separation voltage of 25 kV. The method was validated in the range of 0.15-2.0 mM with respect to linearity and precision. The LODs of the analytes ranged between 0.04 and 0.10 mM. The assay was subsequently applied to determine the stereospecificity of methionine sulfoxide reductases as well as the enzyme kinetics of human methionine sulfoxide reductase A. Monitoring the decrease of the l-methionine-(S)-sulfoxide Km = 411.8 ± 33.8 μM and Vmax = 307.5 ± 10.8 μM/min were determined.

  16. Flow rate dependent extra-column variance from injection in capillary liquid chromatography.

    Science.gov (United States)

    Aggarwal, Pankaj; Liu, Kun; Sharma, Sonika; Lawson, John S; Dennis Tolley, H; Lee, Milton L

    2015-02-01

    Efficiency and resolution in capillary liquid chromatography (LC) can be significantly affected by extra-column band broadening, especially for isocratic separations. This is particularly a concern in evaluating column bed structure using non-retained test compounds. The band broadening due to an injector supplied with a commercially available capillary LC system was characterized from experimental measurements. The extra-column variance from the injection valve was found to have an extra-column contribution independent of the injection volume, showing an exponential dependence on flow rate. The overall extra-column variance from the injection valve was found to vary from 34 to 23 nL. A new mathematical model was derived that explains this exponential contribution of extra-column variance on chromatographic performance. The chromatographic efficiency was compromised by ∼130% for a non-retained analyte because of injection valve dead volume. The measured chromatographic efficiency was greatly improved when a new nano-flow pumping system with integrated injection valve was used.

  17. Sheath liquid effects in capillary high-performance liquid chromatography-electrospray mass spectrometry of oligonucleotides.

    Science.gov (United States)

    Huber, C G; Krajete, A

    2000-02-18

    Fused-silica capillary columns of 200 microm inner diameter were packed with micropellicular, octadecylated, 2.3 microm poly(styrene-divinylbenzene) particles and applied to the separation of oligonucleotides by ion-pair reversed-phase high-performance liquid chromatography. Oligonucleotides were eluted at 50 degrees C with gradients of 3-13% acetonitrile in 50 mM triethylammonium bicarbonate. Addition of sheath liquid to the column effluent allowed the detection of oligonucleotides by electrospray ionization mass spectrometry using full-scan data acquisition with a detectability comparable to that obtained with UV detection. The signal-to-noise ratios with different sheath liquids increased in the order isopropanolcapillary ion-pair reversed-phase high-performance liquid chromatography-electrospray ionization mass spectrometry was

  18. Gas chromatography using resistive heating technology.

    Science.gov (United States)

    Wang, Anzi; Tolley, H Dennis; Lee, Milton L

    2012-10-26

    Air bath ovens are standard in conventional gas chromatography (GC) instruments because of their simplicity and reliability for column temperature control. However, their low heating rates, high power consumption and bulky size are in conflict with the increasing demands for fast separation and portable instrumentation. The deficiencies of air bath ovens can be eliminated using resistive heating technology, as the column is conductively heated by compact resistive heaters with low thermal mass. Resistive heating methods were employed in the early years of GC history, and they are emerging again as instrumentation is becoming more compact and sophisticated. Numerous designs have been tested and some have been successfully commercialized. Development of portable GC systems, including lab-on-a-chip devices, greatly benefits from the use of small, low-power resistive heating hardware. High speed GC separations using conventional instruments also can be best achieved with resistive heating modules. Despite some of its own inherent disadvantages, including efficiency loss, complex manufacturing and inconvenient column maintenance, resistive heating is expected to rapidly become a mature technology and even replace oven heating in the not-to-distant future.

  19. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

    Science.gov (United States)

    Belisle, A.A.; Swineford, D.M.

    1988-01-01

    A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

  20. Capillary ion-exchange chromatography with nanogram sensitivity for the analysis of monoclonal antibodies.

    Science.gov (United States)

    Rea, Jennifer C; Freistadt, Benny S; McDonald, Daniel; Farnan, Dell; Wang, Yajun Jennifer

    2015-12-11

    Ion-exchange chromatography (IEC) is widely used for profiling the charge heterogeneity of proteins, including monoclonal antibodies (mAbs). Despite good resolving power and robustness, ionic strength-based ion-exchange separations are generally product specific and can be time consuming to develop. In addition, conventional analytical scale ion-exchange separations require tens of micrograms of mAbs for each injection, amounts that are often unavailable in sample-limited applications. We report the development of a capillary IEC (c-IEC) methodology for the analysis of nanogram amounts of mAb charge variants. Several key modifications were made to a commercially available liquid chromatography system to perform c-IEC for charge variant analysis of mAbs with nanogram sensitivity. We demonstrate the method for multiple monoclonal antibodies, including antibody fragments, on different columns from different manufacturers. Relative standard deviations of <10% were achieved for relative peak areas of main peak, acidic and basic regions, which are common regions of interest for quantifying monoclonal antibody charge variants using IEC. The results herein demonstrate the excellent sensitivity of this c-IEC characterization method, which can be used for analyzing charge variants in sample-limited applications, such as early-stage candidate screening and in vivo studies.

  1. Mixed Stationary Liquid Phases for Gas-Liquid Chromatography.

    Science.gov (United States)

    Koury, Albert M.; Parcher, Jon F.

    1979-01-01

    Describes a laboratory technique for use in an undergraduate instrumental analysis course that, using the interpretation of window diagrams, prepares a mixed liquid phase column for gas-liquid chromatography. A detailed procedure is provided. (BT)

  2. Prepared polymethacrylate-based monoliths for the separation of cations by non-suppressed capillary ion chromatography.

    Science.gov (United States)

    Li, Jing; Zhu, Yan

    2014-01-01

    This paper describes a novel analytical system for non-suppressed capillary ion chromatography. Methacrylate monolithic columns were prepared from silanized fused-silica capillaries of 320 µm i.d. by in situ polymerization of glycidyl methacrylate and ethylene dimethacrylate in the presence of 1,4-butanediol, 1-propanol and water as the porogen solvents. The introduction of cation-exchange sites was achieved by sulfonating the matrix with sodium sulfite to produce total cation-exchange capacities in the range of 45-105 μequiv/mL for a 25 cm column. The conditions (concentrations of sodium sulfite solution, reacting time and modified flow rate) of sulfonation were optimized. The hydrodynamic and chromatographic performances were estimated. Coupled with a conductivity detector, a capillary ion chromatography system was set up with the prepared column. Finally, the resultant column was used for the separations of five common univalent cations (Li(+), Na(+), NH4(+), K(+) and Cs(+)) using methanesulfonic acid as the eluent and four divalent cations (Mg(2+), Ca(2+), Sr(2+) and Ba(2+)) by non-suppressed capillary ion chromatography; the chromatographic parameters were further researched.

  3. Fabrication and modeling of narrow capillaries for vacuum system gas inlets

    DEFF Research Database (Denmark)

    Quaade, Ulrich; Jensen, Søren; Hansen, Ole

    2005-01-01

    Micrometer-sized cylindrical capillaries with well-controlled dimensions are fabricated using deep reactive ion etching. The flow through the capillaries is experimentally characterized for varying pressures, temperatures, and diameters. For the parameters used, it is shown that the Knudsen numbe...... is in the intermediate flow regime, and Knudsen's expression for the flow fit the data well. The flow properties of the capillaries make them ideal for introducing gas into vacuum systems and in particular mass spectrometers. ©2005 American Institute of Physics...

  4. Intrinsic advantages of packed capillaries over narrow-bore columns in very high-pressure gradient liquid chromatography.

    Science.gov (United States)

    Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

    2016-06-17

    250μm×100mm fused silica glass capillaries were packed with 1.8μm high-strength silica (HSS) fully porous particles. They were prepared without bulky stainless steel endfittings and metal frits, which both generate significant sample dispersion. The isocratic efficiencies and gradient peak capacities of these prototype capillary columns were measured for small molecules (n-alkanophenones) using a home-made ultra-low dispersive micro-HPLC instrument. Their resolution power was compared to that of standard 2.1mm×100mm very high-pressure liquid chromatography (vHPLC) narrow-bore columns packed with the same particles. The results show that, for the same column efficiency (25000 plates) and gradient steepness (0.04min(-1)), the peak capacity of the 250μm i.d. capillary columns is systematically 15-20% higher than that of the 2.1mm i.d. narrow-bore columns. A validated model of gradient chromatography enabled one to predict accurately the observed peak capacities of the capillary columns for non-linear solvation strength retention behavior and under isothermal conditions. Thermodynamics applied to the eluent quantified the temperature difference for the thermal gradients in both capillary and narrow-bore columns. Experimental data revealed that the gradient peak capacity is more affected by viscous heating than the column efficiency. Unlike across 2.1mm i.d. columns, the changes in eluent composition across the 250μm i.d. columns during the gradient is rapidly relaxed by transverse dispersion. The combination of (1) the absence of viscous heating and (2) the high uniformity of the eluent composition across the diameter of capillary columns explains the intrinsic advantage of capillary over narrow-bore columns in gradient vHPLC.

  5. Wall modified photonic crystal fibre capillaries as porous layer open tubular columns for in-capillary micro-extraction and capillary chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Kazarian, Artaches A. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); W.M. Keck FT-ICR-MS Laboratory, Department of Chemistry, North Carolina State University, Raleigh, NC (United States); Sanz Rodriguez, Estrella; Deverell, Jeremy A. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); McCord, James; Muddiman, David C. [W.M. Keck FT-ICR-MS Laboratory, Department of Chemistry, North Carolina State University, Raleigh, NC (United States); Paull, Brett, E-mail: Brett.Paull@utas.edu.au [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); ARC Centre of Excellence for Electromaterials Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia)

    2016-01-28

    Wall modified photonic crystal fibre capillary columns for in-capillary micro-extraction and liquid chromatographic separations is presented. Columns contained 126 internal parallel 4 μm channels, each containing a wall bonded porous monolithic type polystyrene-divinylbenzene layer in open tubular column format (PLOT). Modification longitudinal homogeneity was monitored using scanning contactless conductivity detection and scanning electron microscopy. The multichannel open tubular capillary column showed channel diameter and polymer layer consistency of 4.2 ± 0.1 μm and 0.26 ± 0.02 μm respectively, and modification of 100% of the parallel channels with the monolithic polymer. The modified multi-channel capillaries were applied to the in-capillary micro-extraction of water samples. 500 μL of water samples containing single μg L{sup −1} levels of polyaromatic hydrocarbons were extracted at a flow rate of 10 μL min{sup −1}, and eluted in 50 μL of acetonitrile for analysis using HPLC with fluorescence detection. HPLC LODs were 0.08, 0.02 and 0.05 μg L{sup −1} for acenaphthene, anthracene and pyrene, respectively, with extraction recoveries of between 77 and 103%. The modified capillaries were also investigated briefly for direct application to liquid chromatographic separations, with the retention and elution of a standard protein (cytochrome c) under isocratic conditions demonstrated, proving chromatographic potential of the new column format, with run-to-run retention time reproducibility of below 1%. - Highlights: • Novel PS-DVB modified photonic crystal fibres for in-capillary micro-extraction. • New method for micro-extraction of PAHs and HPLC-FL detection at sub-ppb levels. • Demonstration of PS-DVB modified photonic crystal fibres for capillary bioseparations.

  6. Detection of ergot (Claviceps purpurea) in a dairy feed component by gas chromatography and mass spectrometry.

    Science.gov (United States)

    Mantle, P G

    1996-11-01

    A dairy feed that contained barley malt screenings caused hyperthermia in dairy cattle. The feed was suspected of containing ergot and was subsequently analyzed to determine the ricinoleate component, a special and prominent feature of oil-rich ergot tissue. Triglyceride oil was extracted by organic solvents from the dairy feed, and the oil was saponified to release fatty acids. Ricinoleate, as a methyl ester, was selectively resolved from other fatty acids by silica gel chromatography and was analyzed by capillary gas chromatography coupled with chemical ionization mass spectrometry, which demonstrated the presence of the methyl ricinoleate molecule and proved that the feed contained ergot. The methodology may be refined to monitor for ergot in powdered dairy feed more routinely.

  7. Analytical potential of mid-infrared detection in capillary electrophoresis and liquid chromatography: A review

    Energy Technology Data Exchange (ETDEWEB)

    Kuligowski, Julia; Quintas, Guillermo; Guardia, Miguel de la [Department of Analytical Chemistry, Universitat de Valencia, Edifici Jeroni Munoz, 50th Dr. Moliner, 46100 Burjassot (Spain); Lendl, Bernhard, E-mail: blendl@mail.zserv.tuwien.ac.at [Institute of Chemical Technologies and Analytics, Vienna University of Technology, Getreidemarkt 9-164, A-1060 Vienna (Austria)

    2010-10-29

    Literature published in the last decade concerning the use of mid-infrared spectrometry as a detection system in separation techniques employing a liquid mobile phase is reviewed. In addition to the continued use of isocratic liquid chromatographic (LC) techniques, advances in chemometric data evaluation techniques now allow the use of gradient techniques on a routine basis, thus significantly broadening the range of possible applications of LC-IR. The general trend towards miniaturized separation systems was also followed for mid-IR detection where two key developments are of special importance. Firstly, concerning on-line detection the advent of micro-fabricated flow-cells with inner volumes of only a few nL for transmission as well as attenuated total reflection measurements enabled on-line mid-IR detection in capillary LC and opened the path for the first successful realization of on-line mid-IR detection in capillary zone electrophoresis as well as micellar electrokinetic chromatography. Secondly, concerning off-line detection the use of micro-flow through dispensers now enables to concentrate eluting analytes on dried spots sized a few tens of micrometers, thus matching the dimensions for sensitive detection by mid-IR microscopy. Finally in an attempt to increase detection sensitivity of on-line mid-IR detection, mid-IR quantum cascade lasers have been used. Applications cover the field of food analysis, environmental analysis and the characterization of explosives among others. Best detection sensitivities for on-line and off-line detection have been achieved in miniaturized systems and are in the order of 50 ng and 2 ng on column, respectively.

  8. Differentiation between naproxen, naproxen-protein conjugates, and naproxen-lysine in plasma via micellar electrokinetic capillary chromatography : a new approach in the bioanalysis of drug targeting preparations

    NARCIS (Netherlands)

    Albrecht, C.; Reichen, J; Visser, Jan; Meijer, D.K F; Thormann, W

    1997-01-01

    Pharmacotherapy through the targeting of drugs is a promising new approach that requires adequate analytical methods capable of differentiating between the free drug the drug carrier, and metabolites. Using micellar electrokinetic capillary chromatography (MECC), we report the separation of naproxen

  9. Analysis of reducing carbohydrates by reductive tryptamine derivatization prior to micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Andersen, Keld E; Bjergegaard, Charlotte; Sørensen, Hilmer

    2003-12-03

    A micellar electrokinetic capillary chromatography method for determination of low molecular weight carbohydrates (dp 1-2) with an unbound carbonyl group as in aldoses or other reducing carbohydrates has been developed. Reductive amination of aldoses on the carbonyl group using tryptamine introduced a chromophor system to the carbohydrates enabling their sensitive UV detection at 220 nm and identification based on the indole group using diode array detection. Twelve carbohydrates including pentoses (d-ribose, l-arabinose, and d-xylose), hexoses (d-glucose, d-mannose, and d-galactose), deoxy sugars (l-rhamnose and l-fucose), uronic acids (d-glucuronic acid and d-galacturonic acid), and disaccharides (cellobiose and melibiose) are included in the study, using d-thyminose (2-deoxy-d-ribose) as the internal standard. Detection of all 12 carbohydrates is performed within 30 min. Linearity with correlation coefficients from 0.9864 to 0.9992 was found in the concentration range of 25-2500 micromol/L for all carbohydrates; the relative standard deviation on the migration times was between 0.27 and 0.80 min, and limits of quantification and limits of determination were in the picomole range.

  10. Quantitative analysis of flavonoids and phenolic acids in Arnica montana L. by micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Ganzera, Markus; Egger, Christoph; Zidorn, Christian; Stuppner, Hermann

    2008-05-01

    Arnica montana preparations have been used in Europe for centuries to treat skin disorders. Among the biologically active ingredients in the flower heads of the plant are sequiterpenes, flavonoids and phenolic acids. For the simultaneous determination of compounds belonging to the latter two groups a micellar electrokinetic capillary chromatography (MEKC) method was developed and validated. By using an electrolyte solution containing 50 mM borax, 25 mM sodium dodecyl sulfate and 30% of acetonitrile the separation of seven flavonoids and four caffeic acid derivatives was feasible in less than 20 min. The optimized system was validated for repeatability (sigma(rel) or = 0.9996), and then successfully applied to assay several plant samples. In all of them the most dominant flavonoid was found to be quercetin 3-O-glucuronic acid, whereas 3,5-dicaffeoylquinic acid was the major phenolic acid; the total content of flavonoids and phenolic acids varied in the samples from 0.60 to 1.70%, and 1.03 to 2.24%, respectively.

  11. Ionic liquid-based zwitterionic organic polymer monolithic column for capillary hydrophilic interaction chromatography.

    Science.gov (United States)

    Wang, Tingting; Chen, Yihui; Ma, Junfeng; Zhang, Xiaodan; Zhang, Lihua; Zhang, Yukui

    2015-08-21

    In the current study, a novel ionic liquid-based zwitterionic organic polymer monolithic column was developed by copolymerizing 1-vinyl-3-(butyl-4-sulfonate) imidazolium, acrylamide and N,N'-methylenebisacrylamide in a quaternary porogenic solvent consisting of formamide, dimethyl sulphoxide, polyethylene glycol 8000 and polyethylene glycol 10,000 for capillary hydrophilic interaction chromatography. The monolithic stationary phase was optimized by adjusting the amount of monomer in the polymerization solution along with the composition of porogenic solvent. The optimized monolith exhibited excellent selectivity and favorable retention for nucleosides and benzoic acid derivatives. The primary factors affecting the separation efficiency of the monolithic column (including acetonitrile content, pH, and buffer salt concentration in the mobile phase) have been thoroughly evaluated. Excellent reproducibility of the retention times for five nucleosides was achieved, with relative standard deviations of run-to-run (n = 3), column-to-column (n = 3) and batch-to-batch (n = 3) in the range of 0.18-0.48%, 2.33-4.20% and 3.07-6.50%, respectively.

  12. Wall modified photonic crystal fibre capillaries as porous layer open tubular columns for in-capillary micro-extraction and capillary chromatography.

    Science.gov (United States)

    Kazarian, Artaches A; Sanz Rodriguez, Estrella; Deverell, Jeremy A; McCord, James; Muddiman, David C; Paull, Brett

    2016-01-28

    Wall modified photonic crystal fibre capillary columns for in-capillary micro-extraction and liquid chromatographic separations is presented. Columns contained 126 internal parallel 4 μm channels, each containing a wall bonded porous monolithic type polystyrene-divinylbenzene layer in open tubular column format (PLOT). Modification longitudinal homogeneity was monitored using scanning contactless conductivity detection and scanning electron microscopy. The multichannel open tubular capillary column showed channel diameter and polymer layer consistency of 4.2 ± 0.1 μm and 0.26 ± 0.02 μm respectively, and modification of 100% of the parallel channels with the monolithic polymer. The modified multi-channel capillaries were applied to the in-capillary micro-extraction of water samples. 500 μL of water samples containing single μg L(-1) levels of polyaromatic hydrocarbons were extracted at a flow rate of 10 μL min(-1), and eluted in 50 μL of acetonitrile for analysis using HPLC with fluorescence detection. HPLC LODs were 0.08, 0.02 and 0.05 μg L(-1) for acenaphthene, anthracene and pyrene, respectively, with extraction recoveries of between 77 and 103%. The modified capillaries were also investigated briefly for direct application to liquid chromatographic separations, with the retention and elution of a standard protein (cytochrome c) under isocratic conditions demonstrated, proving chromatographic potential of the new column format, with run-to-run retention time reproducibility of below 1%.

  13. A sensitive gas chromatography detector based on atmospheric pressure chemical ionization by a dielectric barrier discharge.

    Science.gov (United States)

    Kirk, Ansgar T; Last, Torben; Zimmermann, Stefan

    2017-02-03

    In this work, we present a novel concept for a gas chromatography detector utilizing an atmospheric pressure chemical ionization which is initialized by a dielectric barrier discharge. In general, such a detector can be simple and low-cost, while achieving extremely good limits of detection. However, it is non-selective apart from the use of chemical dopants. Here, a demonstrator manufactured entirely from fused silica capillaries and printed circuit boards is shown. It has a size of 75×60×25mm(3) and utilizes only 2W of power in total. Unlike other known discharge detectors, which require high-purity helium, this detector can theoretically be operated using any gas able to form stable ion species. Here, purified air is used. With this setup, limits of detection in the low parts-per-billion range have been obtained for acetone.

  14. Comparison of silanization/hydrosilation and organosilanization modification procedures on etched capillaries for electrokinetic chromatography.

    Science.gov (United States)

    Matyska, Maria T; Pesek, Joseph J

    2005-06-24

    Etched capillaries for use in open tubular electrochromatography are modified by silanization/hydrosilation and organosilanization. The migration behavior of both types of capillaries is evaluated with small basic molecules, peptides and proteins. Comparisons of peak symmetry and efficiency are used to measure the effectiveness of the two methods for modifying the etched surface. From this information, the suitability of each method for use with etched capillaries can be determined.

  15. The development of a weak anion micro-capillary film for protein chromatography.

    Science.gov (United States)

    Kouyoumdjian, A J M; Lazar, R A; Slater, N K H

    2016-10-14

    In this study, the surface of a microporous walled micro-capillary film (MMCF) was modified into a weak anion exchanger by coupling cyanuric chloride and 2-diethylaminoethylamine (DEAE) to the ethylene-vinyl alcohol (EVOH) matrix. Fourier transform infrared spectroscopy (FTIR) measurements of modified and unmodified MMCFs confirmed the addition of a triazine ring and DEAE onto the membrane. Binding of bovine serum albumin (BSA) at pH 7.2 was found to follow a Langmuir isotherm with a maximum equilibrium binding of 12.4mg BSA/mL adsorbent and 8.2mg BSA/mL adsorbent under static and flow conditions, respectively. The ion exchange capacity, determined by Mohr's titration of chlorine atoms displaced from the functionalised surface, was found to be 195±21μmol Cl(-)/mL of adsorber, comparable to commercial ion exchangers. BSA adsorption onto the ion exchanger was strongly pH-dependant, with an observed reduction in binding above pH 8.2. Frontal experiments of a BSA (5mg/mL) and lysozyme (5mg/mL) mixture demonstrated successful separation of BSA from lysozyme at more than 97% purity as verified by sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE). Separation between similarly charged anionic molecules was also achieved using BSA (5mg/mL) and herring sperm DNA (0.25mg/mL). BSA was extracted at 100% purity, demonstrating the ability of MMCF-DEAE to remove significant DNA contamination from a protein solution. These experiments highlight the potential for MMCFs to be used for fast protein purification in preparative chromatography application.

  16. High-Throughput Proteomics Using High Efficiency Multiple-Capillary Liquid Chromatography With On-Line High-Performance ESI FTICR Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Yufeng (BATTELLE (PACIFIC NW LAB)); Tolic, Nikola (BATTELLE (PACIFIC NW LAB)); Zhao, Rui (ASSOC WESTERN UNIVERSITY); Pasa Tolic, Ljiljana (BATTELLE (PACIFIC NW LAB)); Li, Lingjun (Illinois Univ Of-Urbana/Champa); Berger, Scott J.(ASSOC WESTERN UNIVERSITY); Harkewicz, Richard (BATTELLE (PACIFIC NW LAB)); Anderson, Gordon A.(BATTELLE (PACIFIC NW LAB)); Belov, Mikhail E.(BATTELLE (PACIFIC NW LAB)); Smith, Richard D.(BATTELLE (PACIFIC NW LAB))

    2000-12-01

    We report on the design and application of a high-efficiency multiple-capillary liquid chromatography (LC) system for high-throughput proteome analysis. The multiple-capillary LC system was operated at the pressure of 10,000 psi using commercial LC pumps to deliver the mobile phase and newly developed passive feedback valves to switch the mobile phase flow and introduce samples. The multiple-capillary LC system was composed of several serially connected dual-capillary column devices. The dual-capillary column approach was designed to eliminate the time delay for regeneration (or equilibrium) of the capillary column after its use under the mobile phase gradient condition (i.e. one capillary column was used in separation and the other was washed using mobile phase A). The serially connected dual-capillary columns and ESI sources were operated independently, and could be used for either''backup'' operation or with other mass spectrometer(s). This high-efficiency multiple-capillary LC system uses switching valves for all operations and is highly amenable to automation. The separations efficiency of dual-capillary column device, optimal capillary dimensions (column length and packed particle size), suitable mobile phases for electrospray, and the capillary re-generation were investigated. A high magnetic field (11.5 tesla) Fourier transform ion cyclotron resonance (FTICR) mass spectrometer was coupled on-line with this high-efficiency multiple-capillary LC system through an electrospray ionization source. The capillary LC provided a peak capacity of {approx}600, and the 2-D capillary LC-FTICR provided a combined resolving power of > 6 x 10 7 polypeptide isotopic distributions. For yeast cellular tryptic digests, > 100,000 polypeptides were typically detected, and {approx}1,000 proteins can be characterized in a single run.

  17. Application of a low impedance contactless conductometric detector for the determination of inorganic cations in capillary monolithic column chromatography.

    Science.gov (United States)

    Shen, Dazhong; Li, Dongdong; Yang, Xiuwen; Zhu, Yan; Dong, Jianfeng; Kang, Qi

    2011-03-15

    Poly(glycidyl methacrylate) cation exchange monolithic column was prepared in fused-silica capillaries of 320 μm i.d. by thermally initiated radical polymerization and utilized in capillary ion chromatography. With 15 mM methanesulfonic acid as the mobile phase, the separations of a mixture of inorganic cations (Li(+), Na(+), NH(4)(+), K(+)) was tested by using a capacitively coupled contactless conductivity detector (C(4)D) and a low impedance C(4)D (LIC(4)D). The LIC(4)D is the series combination of a C(4)D and a quartz crystal resonator. At the resonant frequency of the series combination, the capacitor impedance from capillary wall was offset by the inductance impedance from the quartz crystal resonator. A minimum impedance was obtained in the impedance-frequency curve of the combination. The responses of the C(4)D and LIC(4)D were analyzed based on an equivalent circuit model. It was shown that the sensitivity of the C(4)D to the change in analyte concentration is rather poor due to the high ratio of the impedance from the capillary wall capacitor to the solution impedance. The LIC(4)D has the similar sensitivity as a contact conductivity detector but a much smaller cell volume. The on-column detection model was realized by LiC(4)D without preparation of optical detection window in monolithic column.

  18. Pressurized nano-liquid-junction interface for coupling capillary electrochromatography and nano-liquid chromatography with mass spectrometry.

    Science.gov (United States)

    D'Orazio, Giovanni; Fanali, Salvatore

    2013-11-22

    A new nano-liquid-junction interface for coupling both capillary electrochromatography (CEC) or nano-liquid chromatography (nano-LC) with mass spectrometry (MS) was studied. The interface was a small T piece of polymeric material where capillary column and tip capillary were positioned at 180° while the third exit (at 90°) was occupied by a capillary delivering a liquid-assisting spray ionization for CEC experiments or by the electrode for the high voltage spray for nano-LC. Experiments were carried out analyzing mixtures of some organophosphorus pesticides (OPPs) or anti-inflammatory and related acidic drugs with MS detection in positive or negative ion mode, respectively. Analyzed OPPs compounds were baseline resolved utilizing the novel interface in both nano-LC and CEC obtaining good sensitivity and repeatability. For CEC-MS, the limits of detection ranged between 0.03 and 6.80 μg/mL and the intra-day repeatability was RSD interface was easy to handle and good reproducibility, between 2.5 and 3.5% for the retention time and interface was installed by two different analysts. Furthermore, it could be used for both CEC and nano-LC.

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

    Energy Technology Data Exchange (ETDEWEB)

    Masada, Y.

    1976-01-01

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

  20. Development of a thermal desorption modulator for gas chromatography

    NARCIS (Netherlands)

    Geus, H.J.; Boer, de J.; Brinkman, U.A.Th.

    1997-01-01

    The separation space in gas chromatography can be enhanced dramatically by the comprehensive coupling of two independent separation dimensions. An interface between the two columns must accumulate analytes eluting from the first dimension, focus them and at the appropriate moment transfer them to th

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

    Science.gov (United States)

    Gochman, Nathan; And Others

    1979-01-01

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

  2. Optimization strategies for separation of sulfadiazines using Box-Behnken design by liquid chromatography and capillary electrophoresis

    Institute of Scientific and Technical Information of China (English)

    GONG Wen-jun; ZHANG Yu-ping; ZHANG Yi-Jun; XU Guang-ri; WEI Xin-jun; LEE Kwang-pill

    2007-01-01

    Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35 ℃ and 1.0 mL/min, respectively.Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.

  3. Effect of Surface Forces on the Gas Flow in Nanosize Capillaries

    Science.gov (United States)

    Roldughin, V. I.; Zhdanov, V. M.

    2005-05-01

    The flow of gas in ultrafine capillary under the action of temperature gradient is considered with allowance for the action of surface forces. It is shown that the presence of surface forces considerably increases the effect of thermal transpiration compared to the classical value determined in a free molecular regime of gas flow. The coefficient responsible for the mechanocaloric effect for the case of gas flow under the pressure gradient was also determined using Onsager relation for the kinetic coefficients calculated with accownt of the effect of surface forces.

  4. Gas chromatography-vacuum ultraviolet spectroscopy for multiclass pesticide identification.

    Science.gov (United States)

    Fan, Hui; Smuts, Jonathan; Walsh, Phillip; Harrison, Dale; Schug, Kevin A

    2015-04-10

    A new vacuum ultraviolet detector for gas chromatography was recently developed and applied to multiclass pesticide identification. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 pesticides across different classes were recorded. These pesticides display rich gas phase absorption features across various classes. Even for isomeric compounds, such as hexachlorocyclohexane (HCH) isomers, the VUV absorption spectra are unique and can be easily differentiated. Also demonstrated is the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV provides both qualitative and quantitative information. It offers high specificity, sensitivity (pg on-column detection limits), and a fast data acquisition rate, making it a powerful tool for multiclass pesticide screening when combined with gas chromatography.

  5. Application of mass spectrometer-inverse gas chromatography to study polymer-solvent diffusivity and solubility.

    Science.gov (United States)

    Galdámez, J Román; Danner, Ronald P; Duda, J Larry

    2007-07-20

    The application of a mass spectrometer detector in capillary column inverse gas chromatography is shown to be a valuable tool in the measurement of diffusion and solubility in polymer-solvent systems. The component specific detector provides excellent results for binary polymer-solvent systems, but it is particularly valuable because it can be readily applied to multicomponent systems. Results for a number of infinitely dilute solvents in poly(vinyl acetate) (PVAc) are reported over a range of temperature from 60 to 150 degrees C. Results are also reported for finite concentrations of toluene and methanol in PVAc from 60 to 110 degrees C. Finally, the technique was applied to study the effect of finite concentrations of toluene on the diffusion coefficients of THF and cyclohexane in PVAc. The experimental data compare well with literature values for both infinite and finite concentrations, indicating that the experimental protocol described in this work is sound.

  6. Elemental speciation analysis by multicapillary gas chromatography with microwave-induced plasma atomic spectrometric detection.

    Science.gov (United States)

    Rodriguez Pereiro, I; Schmitt, V O; Lobiński, R

    1997-12-01

    Multicapillary column gas chromatography (MC-GC)/microwave-induced plasma atomic emission spectrometry (MIP AES) was developed for fast speciation analysis of organotin compounds in the environment. Ethylated butyltin compounds could be separated isothermally within less than 30 s (instead of ∼5-10 min) without sacrificing either the resolution or the sample capacity of conventional capillary GC with oven temperature gradient programming. Careful optimization of the pressure and temperature GC program allowed a comprehensive organotin speciation analysis including phenyltin compounds within less than 2.5 min, increasing the sample throughput 6-fold. Compatibility of MC-GC with an MIP atomic emission detector (MIP-AED) was discussed. MC-GC/MIP-AES was validated for the analysis of sediment (PACS-1 and BCR 462) and biological (NIES11) certified reference materials.

  7. 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.

  8. Gas chromatography-olfactometry analysis of the volatile compounds of two commercial Irish beef meats

    NARCIS (Netherlands)

    Machiels, D.; Ruth, van S.M.; Posthumus, M.A.; Istasse, L.

    2003-01-01

    The volatile flavour compounds of two commercial Irish beef meats (labelled as conventional and organic) were evaluated by gas chromatography-olfactometry and were identified by gas chromatography-mass spectrometry. The volatile compounds were isolated in a model mouth system. Gas chromatography-olf

  9. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  10. [Chiral separation of drugs based on macrocyclic antibiotics using HPLC, supercritical fluid chromatography (SFC) and capillary electrochromatography (CEC)].

    Science.gov (United States)

    Dungelová, J; Lehotay, J; Rojkovicová, T; Cizmárik, J

    2003-05-01

    Separation of enantiomers by means of high-performance liquid chromatography (HPLC), supercritical fluid chromatography (SFC), and capillary electrochromatography (CEC) is of great importance in pharmaceutical analyses. In recent years, separation of various types of racemates employs most frequently chiral stationary phases based on macrocyclic antibiotics. This class of chiral selectors includes vancomycin, teikoplanin, ristocetin A, teikoplanin without saccharide components, avoparcin, etc. The review paper describes the properties of selected antibiotics, the effect of chromatographic conditions on enantioselectivity (effect of the composition of the mobile phase, effect of pH of the mobile phase, effect of temperature), and the study of possible mechanisms of interaction, which play an important role in the separation of enantiomers. Examples of the use of macrocyclic antibiotics in the separation of various compounds by means of the HPLC, SFC, and CEC methods follow.

  11. HOT ELUENT CAPILLARY LIQUID CHROMATOGRAPHY USING ZIRCONIA AND TITANIA BASED STATIONARY PHASES. (R825344)

    Science.gov (United States)

    AbstractHigh speed capillary liquid chromatographic separations using a simple home made system constructed from readily available inexpensive components have been studied. Using thermally stable zirconia and titania based packing, the separation of eight alkylbenzene...

  12. Evaluation of new ionic liquids as high stability selective stationary phases in gas chromatography.

    Science.gov (United States)

    González Álvarez, Jaime; Blanco Gomis, Domingo; Arias Abrodo, Pilar; Díaz Llorente, Daniel; Busto, Eduardo; Ríos Lombardía, Nicolás; Gotor Fernández, Vicente; Gutiérrez Álvarez, María Dolores

    2011-05-01

    Two ionic liquids (ILs), namely (S,S)-1-butyl-3-(2'-hydroxy-cyclohexyl)-3H-imidazol-1-ium tetrafluoroborate and (S,S)-1-butyl-3-(2'-acetyl-cyclohexyl)-3H-imidazol-1-ium tetrafluoroborate have been employed as stationary phases in capillary gas chromatography. These new phases exhibit a column efficiency of 1,600 and 2,100 plates m(-1) for IL 1 and IL 2, respectively, a wide operating temperature range and good thermal stability (bleeding temperature of 250 °C for IL 1 and 160 °C for IL 2). Inverse gas chromatography (GC) analyses were used to study the solvation properties of these ILs through a linear solvation energy model. The application of these ILs as new GC stationary phases was studied. These stationary phases exhibited unique selectivity for many organic substances, such as alkanes, ketones, esters, and aromatic compounds. The efficient separation of several mixtures containing compounds of different polarities and the good separation of fatty acid methyl esters (FAMEs) and cis/trans isomers indicate that these ILs may be applicable as a new type of GC stationary phases.

  13. Gas Chromatography Method of Cleaning Validation Process for 2-Propanol Residue Determination in Pharmaceutical Manufacturing Equipment

    Directory of Open Access Journals (Sweden)

    Łukasz Czubak

    2014-07-01

    Full Text Available Cleaning validation is an integral operation of good manufacturing practice in pharmaceutical industry. The aim of this study was to validate simple analytical method for detection of 2-propanol residue in equipment, which is likely contaminated with 2-propanol, usually used in the production area. The gas chromatography with flame ionization detection (GC-FID method was validated on a GC system using DB-FFAP capillary column at the flow rate of 4.9 mL/min. The calibration curve was linear over concentration range from 2.8µg/mL to 110.7µg/mL with a correlation coefficient equal to 0.99981. The detection limit (LOD and quantitation limit (LOQ were 1.1µg/mL and 2.8µg/mL, respectively. The simplicity of gas chromatography method makes it useful for routine analysis of 2-propanol residue and is an alternative to corresponding methods.

  14. Quality assurance of commercial beeswax. Part I. Gas chromatography-electron impact ionization mass spectrometry of hydrocarbons and monoesters.

    Science.gov (United States)

    Jiménez, J J; Bernal, J L; Aumente, S; del Nozal, Ma J; Martín, Ma T; Bernal, J

    2004-01-23

    The use of low-temperature capillary gas chromatography coupled to electron impact mass spectrometry for the characterization of crude beeswaxes yielded by Apis mellifera is described. The system allows the identification of a great number of compounds, some of them not reported till now in beeswax, such as a family of ethyl esters, tetracosyl oleate, and several saturated and unsaturated hydrocarbons. The information acquired makes possible the differentiation between pure beeswax and some foundation beeswax samples where mixture of pure beeswax with another substances is suspected.

  15. Analysis of microdialysate monoamines, including noradrenaline, dopamine and serotonin, using capillary ultra-high performance liquid chromatography and electrochemical detection.

    Science.gov (United States)

    Ferry, Barbara; Gifu, Elena-Patricia; Sandu, Ioana; Denoroy, Luc; Parrot, Sandrine

    2014-03-01

    Electrochemical methods are very often used to detect catecholamine and indolamine neurotransmitters separated by conventional reverse-phase high performance liquid chromatography (HPLC). The present paper presents the development of a chromatographic method to detect monoamines present in low-volume brain dialysis samples using a capillary column filled with sub-2μm particles. Several parameters (repeatability, linearity, accuracy, limit of detection) for this new ultrahigh performance liquid chromatography (UHPLC) method with electrochemical detection were examined after optimization of the analytical conditions. Noradrenaline, adrenaline, serotonin, dopamine and its metabolite 3-methoxytyramine were separated in 1μL of injected sample volume; they were detected above concentrations of 0.5-1nmol/L, with 2.1-9.5% accuracy and intra-assay repeatability equal to or less than 6%. The final method was applied to very low volume dialysates from rat brain containing monoamine traces. The study demonstrates that capillary UHPLC with electrochemical detection is suitable for monitoring dialysate monoamines collected at high sampling rate.

  16. Comparison of chiral separation of basic drugs in capillary electrophoresis and liquid chromatography using neutral and negatively charged cyclodextrins.

    Science.gov (United States)

    Kwaterczak, Arkadiusz; Duszczyk, Kazimiera; Bielejewska, Anna

    2009-07-10

    Liquid chromatography (LC) and capillary electrophoresis (CE) are very widely used as chiral separation methods. In this publication we try to find if the results obtained in CE and LC with the chiral selector added to the electrolyte and the mobile phase, respectively, can be used as tools for studying weak stereoselective interactions, and how this information can be useful for optimizing chiral separation processes. The manuscript presents a systematic comparison of chiral discrimination of model compounds in HPLC and CE using neutral and negatively charged cyclodextrins. The enantiomeric separation of basic chiral pharmaceuticals such as pheniramine, brompheniramine, metoxyphenamine, cyclopentolate, doxylamine and ketamine was investigated in capillary electrophoresis (CE) and liquid chromatography (HPLC) using negatively charged sulfated-beta-cyclodextrin (S-beta-CD) and neutral cyclodextrins (CDs). The apparent stability constants between the model compounds and cyclodextrins were estimated in both techniques. We discuss the influence of the stability constant and K1/K2 ratio of the investigated complexes on chiral separation obtained in both techniques.

  17. Direct measurement of the capillary pressure characteristics of water-air-gas diffusion layer systems for PEM fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Gostick, Jeff T.; Ioannidis, Marios A.; Fowler, Michael W.; Pritzker, Mark D. [Department of Chemical Engineering, University of Waterloo, 200 University Avenue West, Waterloo, ON (Canada)

    2008-10-15

    A method and apparatus for measuring the relationship between air-water capillary pressure and water saturation in PEMFC gas diffusion layers (GDL) is described. Capillary pressure data for water injection and withdrawal from typical GDL materials are obtained, which demonstrate permanent hysteresis between water intrusion and water withdrawal. Capillary pressure, defined as the difference between the water and gas pressures at equilibrium, is positive during water injection and negative during water withdrawal. The results contribute to the understanding of liquid water behavior in GDL materials which is necessary for the development of effective PEMFC water management strategies. (author)

  18. Simultaneous determination of caffeine, paracetamol, and ibuprofen in pharmaceutical formulations by high-performance liquid chromatography with UV detection and by capillary electrophoresis with conductivity detection.

    Science.gov (United States)

    Cunha, Rafael R; Chaves, Sandro C; Ribeiro, Michelle M A C; Torres, Lívia M F C; Muñoz, Rodrigo A A; Dos Santos, Wallans T P; Richter, Eduardo M

    2015-05-01

    Paracetamol, caffeine and ibuprofen are found in over-the-counter pharmaceutical formulations. In this work, we propose two new methods for simultaneous determination of paracetamol, caffeine and ibuprofen in pharmaceutical formulations. One method is based on high-performance liquid chromatography with diode-array detection and the other on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation by high-performance liquid chromatography with diode-array detection was achieved on a C18 column (250×4.6 mm(2), 5 μm) with a gradient mobile phase comprising 20-100% acetonitrile in 40 mmol L(-1) phosphate buffer pH 7.0. The separation by capillary electrophoresis with capacitively coupled contactless conductivity detection was achieved on a fused-silica capillary (40 cm length, 50 μm i.d.) using 10 mmol L(-1) 3,4-dimethoxycinnamate and 10 mmol L(-1) β-alanine with pH adjustment to 10.4 with lithium hydroxide as background electrolyte. The determination of all three pharmaceuticals was carried out in 9.6 min by liquid chromatography and in 2.2 min by capillary electrophoresis. Detection limits for caffeine, paracetamol and ibuprofen were 4.4, 0.7, and 3.4 μmol L(-1) by liquid chromatography and 39, 32, and 49 μmol L(-1) by capillary electrophoresis, respectively. Recovery values for spiked samples were between 92-107% for both proposed methods.

  19. A capillary liquid chromatography method for benzalkonium chloride determination as a component or contaminant in mixtures of biocides.

    Science.gov (United States)

    Prieto-Blanco, M C; Argente-García, A; Campíns-Falcó, P

    2016-01-29

    A method for quantifying benzalkonium chloride (BAK), an alkyl dimethyl benzyl ammonium compound, in several biocides formulations is proposed. A tertiary amine like N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine (TA) and a straight-chain alkyl ammonium compound like trimethyl-tetradecyl ammonium chloride (TMTDAC), have been employed as trade surfactants besides BAK. Two capillary analytical columns with different polarities are tested: inertsil CN-3 capillary column (150mm×0.5mm i.d., 3μm particle diameter) and a non endcapped Zorbax C18 capillary column (35mm×0.5mm i.d., 5μm particle diameter). This latter column provided the best separation of the BAK homologues in less than 12min using acetonitrile:acetate buffer (50mM, pH 5) 85:15 at 20μLmin(-1). The proposed method combines on-line in-tube solid-phase microextraction (IT-SPME) coupled to capillary liquid chromatography (CapLC) and UV diode array detection. Matrix effect was present when TA were in excess to BAK. If TMTDAC is the co-biocide, matrix effect is always present. A decreasing of analytical response mainly for C12-BAK homologue was found using both chromatographic columns. The charged amount of mixture in the system was the most important parameter for obtaining reliable results. 1mL was the on line processed sample volume optimum for concentrations lower than 35μgmL(-1) of total surfactants. LODs were 0.03μgmL(-1) and 0.006μgmL(-1) for C12-BAK and C14-BAK, respectively. This method is also of use to evaluate the unwanted presence of BAK in biocide formulations due to industrial processes.

  20. Reducing Mechanical Formation Damage by Minimizing Interfacial Tension and Capillary Pressure in Tight Gas

    Science.gov (United States)

    Ahmed, Arshad; Talib Shuker, Muhannad; Rehman, Khalil; Bahrami, Hassan; Memon, Muhammad Khan

    2013-12-01

    Tight gas reservoirs incur problems and significant damage caused by low permeability during drilling, completion, stimulation and production. They require advanced improvement techniques to achieve flow gas at optimum rates. Water blocking damage (phase Trapping/retention of fluids) is a form of mechanical formation damage mechanism, which is caused by filtrate invasion in drilling operations mostly in fracturing. Water blocking has a noticeable impact on formation damage in gas reservoirs which tends to decrease relative permeability near the wellbore. Proper evaluation of damage and the factors which influence its severity is essential to optimize well productivity. Reliable data regarding interfacial tension between gas and water is required in order to minimize mechanical formation damage potential and to optimize gas production. This study was based on the laboratory experiments of interfacial tension by rising drop method between gas-brine, gas-condensate and gas-brine. The results showed gas condensate has low interfacial tension value 6 - 11 dynes/cm when compared to gas-brine and gas- diesel which were 44 - 58 dynes/cm and 14 - 19 dynes/cm respectively. In this way, the capillary pressure of brine-gas system was estimated as 0.488 psi, therefore diesel-gas system was noticed about 0.164 psi and 0.098 psi for condensate-gas system. A forecast model was used by using IFT values to predict the phase trapping which shows less severe phase trapping damage in case of condensate than diesel and brine. A reservoir simulation study was also carried out in order to better understand the effect of hysteresis on well productivity and flow efficiency affected due to water blocking damage in tight gas reservoirs.

  1. Determination of Vinyl Chloride at ug/l. Level in Water by Gas Chromatography

    Science.gov (United States)

    Bellar, Thomas A.; And Others

    1976-01-01

    A quantitative method for the determination of vinyl chloride in water is presented. Vinyl chloride is transfered to the gas phase by bubbling inert gas through the water. After concentration on silica gel or Carbosieve-B, determination is by gas chromatography. Confirmation of vinyl chloride is by gas chromatography-mass spectrometry. (Author/BT)

  2. The Use of Gas Chromatography for Biogas Analysis

    Science.gov (United States)

    Andersen, Amanda; Seeley, John; Aurandt, Jennifer

    2010-04-01

    Energy from natural gas accounts for 24 percent of energy consumed in the US. Natural gas is a robust form of energy which is rich in methane content and is low in impurities. This quality suggests that it is a very clean and safe gas; it can be used in providing heat, a source for cooking, and in powering vehicles. The downside is that it is a non-renewable resource. On the contrary, methane rich gas that is produced by the breakdown of organic material in an anaerobic environment, called biogas, is a renewable energy source. This research focuses on the gas analysis portion of the creation of the anaerobic digestion and verification laboratory where content and forensic analysis of biogas is performed. Gas Chromatography is implemented as the optimal analytical tool for quantifying the components of the biogas including methane, carbon dioxide, hydrogen sulfide and siloxanes. In addition, the problems associated with the undesirable components are discussed. Anaerobic digestion of primary sludge has consistently produced about 55 percent methane; future goals of this research include studying different substrates to increase the methane yield and decrease levels of impurities in the gas.

  3. Capillary liquid chromatography separations using non-porous pillar array columns

    NARCIS (Netherlands)

    Malsche, de D.M.W.; Bruyne, de S.; Beek, op de J.; Sandra, P.; Gardeniers, J.G.E.; Desmet, G.; Lynen, F.

    2012-01-01

    We report on a series of explorative experiments wherein a non-porous pillar array column (NP-PAC) is coupled to a commercial capillary LC instrument. The performance of the system was evaluated by both non-retained and retained experiments using several types of samples. In order to minimize interf

  4. Determination of alcohol in Yangyinqingfei Syrup from 10 manufactories by capillary gas chromatography%毛细管柱气相色谱法测定10个厂家养阴清肺糖浆中乙醇的含量

    Institute of Scientific and Technical Information of China (English)

    姜姗; 倪健; 黄淑惠; 李晋凯; 冯丽君

    2011-01-01

    目的:建立测定养阴清肺糖浆中乙醇含量的方法,对10个厂家糖浆中乙醇含量进行比较.方法:采用毛细管柱气相色谱法(GC),色谱条件:DM-WAX毛细管柱(30m×0.25mm×0.25μm);进样口温度180C;程序升温;载气为氮气,流速5.0mL/min;FID检测器.结果:乙醇与内标物正丙醇分离效果理想,线性关系良好(r=0.998),精密度、重复性、稳定性、加样回收率均符合要求.测得的10个厂家的乙醇含量分别为:0.40%、14.63%、8.86%、10.72%、10.49%、11.05%、10.67%、9.12%、12.09%、11.07%.结论:本方法柱效高,方法简单、准确、重现性好,可用于测定养阴清肺糖浆中乙醇的含量.不同厂家生产的糖浆中乙醇含量有差异,有的不符合标准规定的要求,说明在产品生产质量控制方面还有待提高.%Objective: To establish a method for determining alcohol in Yangyinqingfei Syrup. To compare the content of alcohol in Yangyingqingfei Syrup from 10 manufactories. Methods: Capillary GC was adopted with DM-WAX ( 30m×0.25mm ×0.25μm ) capillary column; The injector and detector temperature were at 180℃; The column temperature was programmed to rise; Nitrogen was the carrier gas, the speed of flow was 5.0mL/min; Detector was the FID. Results: The alcohol and n-propanol acted as the internal standand exhibited an excellent separatability. Alcohol concentration showed good relationships(r=0.998).Precision, repeatability, stability and recovery all met the requirement. The content of alcohol measured from 10 manufactories were 0.40%, 14.63%, 8.86%, 10.72%, 10.49%, 11.05%, 10.67%, 9.12%, 12.09% and 11.07%. Conclusion: The method was highly efficient, simple, accurate and reproducible. It could be used for determination of alcohol in Yangyinqingfei Syrup. There were differences in the content of alcohol measured from different manufactories, some of them could not meet the ministerial standands, which showed that it remained to be improved

  5. a Diffusivity Model for Gas Diffusion in Dry Porous Media Composed of Converging-Diverging Capillaries

    Science.gov (United States)

    Wang, Shifang; Wu, Tao; Deng, Yongju; Zheng, Qiusha; Zheng, Qian

    2016-08-01

    Gas diffusion in dry porous media has been a hot topic in several areas of technology for many years. In this paper, a diffusivity model for gas diffusion in dry porous media is developed based on fractal theory and Fick’s law, which incorporates the effects of converging-diverging pores and tortuous characteristics of capillaries as well as Knudsen diffusion. The effective gas diffusivity model is expressed as a function of the fluctuation amplitude of the capillary cross-section size variations, the porosity, the pore area fractal dimension and the tortuosity fractal dimension. The results show that the relative diffusivity decreases with the increase of the fluctuation amplitude and increases with the increase of pore area fractal dimension. To verify the validity of the present model, the relative diffusivity from the proposed fractal model is compared with the existing experimental data as well as two available models of Bruggeman and Shou. Our proposed diffusivity model with pore converging-diverging effect included is in good agreement with reported experimental data.

  6. [Development of a droplet-interfaced high performance liquid chromatography-capillary electrophoresis two dimensional separation platform].

    Science.gov (United States)

    Ye, Linquan; Wu, Qingshi; Dai, Simin; Xiao, Zhiliang; Zhang, Bo

    2011-09-01

    Proteomics demands high resolution multidimensional separation techniques due to its extremely high complexity. Droplet microfluidics provides a series of unique advantages in manipulating micro and nanolitre samples, such as micro-volume operation, limited diffusion and none cross-contaminating, therefore has the potential to be an ideal interface strategy for multidimensional separation. Using the microchips of different structures, functions such as "droplet generation" and "oil depletion" can be realized. Based on these functions, samples can be transferred from continuous flow to segmented flow and then back to continuous flow. In this way, different separation modes can be combined. In this study, droplet technology was utilized as a novel interface strategy in combining high performance liquid chromatography (HPLC) and capillary electrophoresis (CE). Using tryptic peptides mixture as a sample, this two dimensional HPLC-CE system provided high resolution separation with a peak capacity over 3000. This proof-of-principle study has demonstrated the usefulness of droplet interface technology in multidimensional separation.

  7. Capillary ion chromatography-mass spectrometry for simultaneous determination of glucosylglycerol and sucrose in intracellular extracts of cyanobacteria.

    Science.gov (United States)

    Fa, Yun; Liang, Wenhui; Cui, He; Duan, Yangkai; Yang, Menglong; Gao, Jun; Liu, Huizhou

    2015-09-15

    A capillary ion chromatography-mass spectrometry (MS) method was proposed to determine glucosylglycerol (GG), sucrose, and five other carbohydrates. MS conditions and make-up flow parameters were optimized. This method is accurate and sensitive for simultaneous analysis of carbohydrates, with mean correlation coefficients of determination greater than 0.99, relative standard deviation of 0.91-2.81% for eight replicates, and average spiked recoveries of 97.3-104.9%. Limits of detection of sodium adduct were obtained with MS detection in selected ion mode for GG (0.006mg/L), sucrose (0.02mg/L), and other carbohydrates (0.03mg/L). This method was successfully applied to determine GG and sucrose in intracellular extracts of salt-stressed cyanobacteria.

  8. Quantitative analysis of [Dmt(1)]DALDA in ovine plasma by capillary liquid chromatography-nanospray ion-trap mass spectrometry.

    Science.gov (United States)

    Wan, Haibao; Umstot, Edward S; Szeto, Hazel H; Schiller, Peter W; Desiderio, Dominic M

    2004-04-15

    The synthetic opioid peptide analog Dmt-D-Arg-Phe-Lys-NH(2) ([Dmt(1)]DALDA; [Dmt= 2',6'-dimethyltyrosine) is a highly potent and selective mu opioid-receptor agonist. A very sensitive and robust capillary liquid chromatography/nanospray ion-trap (IT) mass spectrometry method has been developed to quantify [Dmt(1)]DALDA in ovine plasma, using deuterated [Dmt(1)]DALDA as the internal standard. The standard MS/MS spectra of d(0)- and d(5)-[Dmt(1)]DALDA were obtained, and the collision energy was experimentally optimized to 25%. The product ion [ M + 2H-NH(3)](2+) (m/z 312.2) was used to identify and to quantify the synthetic opioid peptide analog in ovine plasma samples. The MS/MS detection sensitivity for [Dmt(1)]DALDA was 625 amol. A calibration curve was constructed, and quantitative analysis was performed on a series of ovine plasma samples.

  9. Determination of caffeine and associated compounds in food, beverages, natural products, pharmaceuticals, and cosmetics by micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Injac, Rade; Srdjenovic, Branislava; Prijatelj, Matevz; Boskovic, Marija; Karljikovic-Rajic, Katarina; Strukelj, Borut

    2008-02-01

    A method is described for quantitating caffeine, theobromine, theophylline, paracetamol, propyphenazone, acetylsalicylic acid, salicylic acid, and codeine phosphate in corresponding real samples of food, beverages, natural products, pharmaceuticals, and cosmetic preparations by micellar electrokinetic capillary chromatography. The separation is carried out at 25 degrees C and 25 kV, using a 20 mM phosphate buffer (pH 9.0), 80 mM sodium dodecyl sulfate, and 7.5% (v/v) acetonitrile. UV detection is at 210 nm. The method is shown to be specific, accurate (recoveries over the range 98.9-101.2%), linear over the tested range (correlation coefficients>or=0.9993), and precise (relative standard deviation below 2.1%). The method is applied for the quantitative analysis of these compounds in different foods, beverages, natural products, pharmaceuticals, and cosmetic products.

  10. Rapid "one-pot" preparation of polymeric monolith via photo-initiated thiol-acrylate polymerization for capillary liquid chromatography.

    Science.gov (United States)

    Bai, Jingyao; Wang, Hongwei; Ou, Junjie; Liu, Zhongshan; Shen, Yehua; Zou, Hanfa

    2016-06-21

    A facile approach was exploited for fast preparation of polymer-based monoliths in UV-transparent fused-silica capillaries via "one-pot" photo-initiated thiol-acrylate polymerization reaction of dipentaerythritolpenta-/hexaacrylate (DPEPA) and 1-octadecanethiol (ODT) in the presence of porogenic solvents (1-butanol and ethylene glycol). Due to relative insensitivity of oxygen inhibition in thiol-ene free-radical polymerization, the polymerization could be performed within 5 min. The effects of composition of prepolymerization solution on the morphology and permeability of poly(ODT-co-DPEPA) monoliths were investigated in detail by adjusting the content of monomer and binary porogen ratio. The physical properties of poly(ODT-co-DPEPA) monoliths were characterized by Fourier transform infrared spectroscopy (FT-IR), mercury intrusion porosimetry (MIP) and nitrogen adsorption/desorption measurement. The evaluation of chromatographic performance was carried out by capillary liquid chromatography (cLC). The results indicated that the poly(ODT-co-DPEPA) monolith was homogeneous and permeable, and also possessed a typical reversed-phase retention mechanism in cLC with high efficiency (∼75,000 N m(-1)) for separation of alkylbenzenes. Eventually, the further separation of tryptic digest of proteins by cLC tandem mass spectrometry (cLC-MS/MS) demonstrated its potential in the analysis of biological samples.

  11. [Separation of cefoperazone and its S-isomer and other related substances by micellar electrokinetic capillary chromatography].

    Science.gov (United States)

    Zhang, Huiwen; Hu, Changqin; Xu, Mingzhe; Li, Yaping; Hang, Taijun

    2007-09-01

    The separation of cefoperazone, its S-isomer, impurity A and other unknown related substances by micellar electrokinetic capillary chromatography (MECC) using sodium dodecyl sulphate (SDS) as the micellar phase was investigated. The effects of pH, concentration of phosphate buffer solution, SDS micelle concentration, methanol volume fraction, applied voltage and temperature on the separation were studied. It was found that the migration of these compounds was affected by these factors, especially by pH of the solution. The elution, as well as the migration time and separation efficiency of cefoperazone, its S-isomer, impurity A and other related substances changed with the acidity of the solution. The optimized separation conditions consisted of a running buffer of 70 mmol/L sodium phosphate buffer, at pH 6.5, containing 100 mmol/L SDS, with an applied voltage of 15 kV and a temperature of 25 degrees C. An uncoated fused-silica capillary of 51.0 cm x 75 microm (42.5 cm of effective length) was used. The sample was injected into the column by pressure (5 kPa) for 5 s. The detection wavelength was set at 254 nm. Twenty-eight impurities in cefoperazone sodium could be detected. Cefoperazone sodium and the degradation products could be separated well. The method was applied to separate and determine cefoperazone and its related substances successfully.

  12. Direct determination of lignin peroxidase released from Phanerochaete chrysosporium by in-capillary enzyme assay using micellar electrokinetic chromatography.

    Science.gov (United States)

    Harada, Airi; Sasaki, Keiko; Kaneta, Takashi

    2016-04-01

    Here we describe the application of an in-capillary enzyme assay using micellar electrokinetic chromatography (MEKC) in the determination of enzyme activity in a crude culture medium containing lignin peroxidase released from Phanerochaete chrysosporium (P. chrysosporium). The method consists of a plug-plug reaction between lignin peroxidase and its substrate, veratryl alcohol, the separation of the product, veratraldehyde, from the other components including the enzyme and the culture medium, and the determination of the enzyme activity from the peak area of veratraldehyde produced by the plug-plug reaction. This method is more sensitive than conventional spectrophotometry since the background originates from the enzyme and the culture medium can be removed via MEKC separation. Veratraldehyde was separated at -10kV in a background electrolyte containing 50mM tartrate buffer (pH 2.5) and 50mM sodium dodecyl sulfate (SDS) after a plug-plug reaction in the capillary for 5min. The calibration curve of veratraldehyde was linear up to 4pmol (500μM) with a limit to quantification of 0.026pmol (3.2μM) (SN=10). The activity of lignin peroxidase was directly measured from the peak area of veratraldehyde. The activity of lignin peroxidase released from P. chrysosporium into the medium for 7 days was successfully determined to be 3.40UL(-1).

  13. Determination of eight triazine herbicide residues in cereal and vegetable by micellar electrokinetic capillary chromatography with on-line sweeping.

    Science.gov (United States)

    Fang, Rou; Chen, Guan-hua; Yi, Ling-xiao; Shao, Yu-xiu; Zhang, Li; Cai, Qing-hong; Xiao, Jing

    2014-02-15

    A new method was developed for the determination of eight triazine herbicide residues in cereal and vegetable samples by on-line sweeping technique in micellar electrokinetic capillary chromatography (MEKC). Some factors affecting analyte enrichment and separation efficiency were examined. The optimum buffer was composed of 25 mM borate, 15 mM phosphate, 40 mM sodium dodecylsulfate (SDS) and 3% (v/v) of 1-propanol at pH 6.5. The separation voltage was 20 kV and the sample was injected at 0.5 psi for 240 s. The detection wavelength was set at 220 nm with the capillary temperature being at 25 °C. Under the optimized conditions, the enrichment factors were achieved from 479 to 610. The limits of detection (LODs, S/N = 3) ranged from 0.02 to 0.04 ng/g and the limits of quantification (LOQs) of eight triazine herbicides were all 0.1 ng/g. The average recoveries of spiked samples were 82.8-96.8%. This method has been successfully applied to the determination of the triazine herbicide residues in cereal and vegetable samples.

  14. Gas-liquid chromatography in lunar organic analysis.

    Science.gov (United States)

    Gehrke, C. W.

    1972-01-01

    Gas-liquid chromatography (GLC) is a powerful and sensitive method for the separation and detection of organic compounds at nanogram levels. The primary requirement for successful analyses is that the compounds of interest must be volatile under the chromatographic conditions employed. Nonvolatile organic compounds must be converted to volatile derivatives prior to analysis. The derivatives of choice must be both amenable to chromatographic separation and be relatively stable. The condition of volatility necessitates the development of efficient derivatization reactions for important groups of compounds as amino acids, carbohydrates, nucleosides, etc. Trimethylsilylation and trifluoroacetylation represent specific areas of recent prominence. Some relevant practical aspects of GLC are discussed.

  15. Enhanced resolution of Mentha piperita volatile fraction using a novel medium-polarity ionic liquid gas chromatography stationary phase.

    Science.gov (United States)

    Ragonese, Carla; Sciarrone, Danilo; Grasso, Elisa; Dugo, Paola; Mondello, Luigi

    2016-02-01

    The evaluation of a novel medium-polarity ionic-liquid-based gas chromatography column, SLB-IL60, towards the analysis of a complex essential oil, namely, a peppermint essential oil sample, is reported. The SLB-IL60 30 m column was subjected to bleeding measurements, by means of conventional gas chromatography with mass spectrometry. The SLB-IL60 column was then evaluated in the analysis of pure standard compounds, chosen as typical constituents of peppermint essential oil. Resolution and peak symmetry (expressed as tailing factors at 10% of peak height) were measured and the results were compared to those obtained on the most widely used columns in such an application, namely a medium-polarity [100% poly(ethyleneglycol)] stationary phase, and an apolar 5% diphenyl/95% dimethyl siloxane. The final part of the evaluation was dedicated to the gas chromatography with mass spectrometry analysis of a peppermint essential oil sample and again the data were compared to those obtained on the 100% poly(ethyleneglycol) and the 5% diphenyl/95% dimethyl siloxane phase. Linear retention indices were determined for all the identified components on the ionic liquid capillary.

  16. Micellar electrokinetic capillary chromatography determination of alginic acid in pharmaceutical formulations after treatment with alginate lyase and UV detection.

    Science.gov (United States)

    Volpi, Nicola

    2008-09-01

    A new highly specific and sensitive capillary electrophoresis method (electrokinetic chromatography with SDS) for the determination of the total alginic acid (AA) content in pharmaceutical formulations is described by means of capillary electrophoresis at 230 nm after treatment with alginate lyase [4.2.2.3] and separation of unsaturated products, Delta-oligomers (DeltaHexA-[HexA](n)), in particular, DP3 (DeltaHexA-HexA-HexA) and DP4 (DeltaHexA-HexA-HexA-HexA). Using a buffer constituted with 10 mM sodium borate and 50 mM SDS at pH 9.0, micellar electrokinetic capillary chromatography was able to determine with very high resolution the AA Delta-oligomers produced by the action of the lyase (mainly DP3 and DP4) as one single species. The intra- and inter-day variations (CV%) were between 6.3 and 9.1 for migration time and between 2.5 and 5.7 for peak area, respectively. The calibration curve showed good linearity for the examined concentration range (60-360 ng) with an average correlation coefficient greater than 0.980. The lowest detection limit and the lowest quantitation limit of the method were 15 ng (0.25 mg/mL) and 40 ng (0.67 mg/mL), respectively. The intra- and inter-day variations in terms of CV% were 5.5 and 8.6%, respectively, and the intra- and inter-day accuracy was estimated to range from 4.1 to 8.9%, while the percent recoveries of AA were calculated to be 102, 97 and 93% for different AA amounts. Variations in temperatures, voltage and buffer composition in comparison with adopted conditions within a 10% limit do not modify the electrophoresis results. The evaluation of AA was performed in both solid and liquid pharmaceutical formulations also in the presence of other ingredients, in particular, aluminium, sodium and potassium bicarbonate, and emulsifying and flavouring agents. The quantitative results obtained were 101.2+/-3.4% of AA content in tablets and 98.4+/-2.8% in liquid formulation, in total conformity with the label claims.

  17. Review of recent developments and applications in low-pressure (vacuum outlet) gas chromatography.

    Science.gov (United States)

    Sapozhnikova, Yelena; Lehotay, Steven J

    2015-10-29

    The concept of low pressure (LP) vacuum outlet gas chromatography (GC) was introduced more than 50 years ago, but it was not until the 2000s that its theoretical applicability to fast analysis of GC-amenable chemicals was realized. In practice, LPGC is implemented by placing the outlet of a short, wide (typically 10-15 m, 0.53 mm inner diameter) analytical column under vacuum conditions, which speeds the separation by reducing viscosity of the carrier gas, thereby leading to a higher optimal flow rate for the most separation efficiency. To keep the inlet at normal operating pressures, the analytical column is commonly coupled to a short, narrow uncoated restriction capillary that also acts as a guard column. The faster separations in LPGC usually result in worse separation efficiency relative to conventional GC, but selective detection usually overcomes this drawback. Mass spectrometry (MS) provides highly selective and sensitive universal detection, and nearly all GC-MS instruments provide vacuum outlet conditions for implementation of LPGC-MS(/MS) without need for adaptations. In addition to higher sample throughput, LPGC provides other benefits, including lower detection limits, less chance of analyte degradation, reduced peak tailing, increased sample loadability, and more ruggedness without overly narrow peaks that would necessitate excessively fast data acquisition rates. This critical review summarizes recent developments in the application of LPGC with MS and other detectors in the analysis of pesticides, environmental contaminants, explosives, phytosterols, and other semi-volatile compounds.

  18. High performance mini-gas chromatography-flame ionization detector system based on micro gas chromatography column

    Science.gov (United States)

    Zhu, Xiaofeng; Sun, Jianhai; Ning, Zhanwu; Zhang, Yanni; Liu, Jinhua

    2016-04-01

    Monitoring Volatile organic compounds (VOCs) was a very important measure for preventing environmental pollution, therefore, a mini gas chromatography (GC) flame ionization detector (FID) system integrated with a mini H2 generator and a micro GC column was developed for environmental VOC monitoring. In addition, the mini H2 generator was able to make the system explode from far away due to the abandoned use of a high pressure H2 source. The experimental result indicates that the fabricated mini GC FID system demonstrated high repeatability and very good linear response, and was able to rapidly monitor complicated environmental VOC samples.

  19. Determination of panaxadiol and panaxatriol in ginseng and its preparations by capillary supercritical fluid chromatography (SFC).

    Science.gov (United States)

    Li, Y H; Li, X L; Hong, L; Liu, J Y; Zhang, M Y

    1992-01-01

    Capillary supercritical fluid chromatographic (SFC) method has been developed for the determination of panaxadiol and panaxatriol in ginseng and its preparations. 0.1 g ginseng or an appropriate amount of its preparations was hydrolysed by 15% H2SO4 in an ethanol:water (1:1 v/v) solution for 4 h followed by 15% NaOH for 0.5 h. The mixture was extracted by cyclohexane. The cyclohexane extracts were purified by a partition column and concentrated by an adsorption column and then analysed by SFC. Methyltestosterone was used as the internal standard.

  20. Solid-phase microcolumn extraction and gas chromatography-mass spectrometry identification of volatile organic compounds emitted by paper.

    Science.gov (United States)

    Hrivnák, Ján; Tölgyessy, Peter; Figedyová, Sona; Katuscák, Svetozár

    2009-11-15

    A rapid non-destructive sampling technique for the analysis of volatile organic compounds (VOCs) emitted by paper sheets is described. A capillary, which is connected to a microcolumn packed with Tenax TA, is inserted between two sheets at the centre of a paper stack encapsulated inside a PET/Al/PE composite foil. The other end of the microcolumn is connected to a gas-tight syringe and an appropriate volume of gaseous phase is aspirated. The microcolumn is then thermally desorbed in a modified GC inlet (modification is presented) and analysed by gas chromatography-mass spectrometry (GC-MS). In the chromatogram from the analysis of artificially aged paper sample 21 compounds were identified. Advantages of the method including the short sampling time (1 min), simplicity and economic aspect are discussed.

  1. Analysis of red inks by micellar electrokinetic capillary chromatography with laser-induced fluorescence detection.

    Science.gov (United States)

    Król, Małgorzata; Gondko, Klaudia; Kula, Agnieszka; Kościelniak, Paweł

    2016-01-01

    A combination of MEKC with a--highly sensitive but not commonly used--LIF detector was tested regarding the possibility of differentiation of red inks. The separation process was conducted in a fused silica capillary (id 50 μm, 60/50 cm total/effective length) in BGE consisting of 40 mM sodium borate, 20 mM SDS and 10% v/v ACN with 30 kV applied. The optimized temperature of storage and capillary was 10 and 25°C, respectively. The samples were prepared using 20 dots (ø 0.5 mm), extracted in 35 μL BGE and diluted with 30 μL of water. The proposed method showed excellent repeatability and reproducibility (RSD (tm ) < 0.8 and < 2.5%, respectively). It was applied to group identification and differentiation of different brands, models, and batches of red printing, stamp, and pen inks. It was demonstrated that differentiation can be performed effectively on the basis of migration times and ratios of peak areas. The high efficiency of the developed method was indicated by discriminating power ranging from 87.3 to 98.8%, for stamp and pen inks, respectively. The results showed that the proposed procedure can be valuable for an objective examination of the red parts of questioned documents.

  2. 毛细管气相色谱法同时检测丙酸氯倍他索原料药中4种有机溶剂残留量%Simultaneous Determination of 4 Kinds of Residual Organic Solvents in Clobetasol Propionate by Capillary Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    李春燕; 屠婕红; 傅应华

    2011-01-01

    OBJECTIVE: To establish the method for the content determination of 4 kinds of residμal organic solvents (metha-nol, ethanol, N, JV-dimethylformamide, dimethylsμlfoxide) in clobetasol propionate. METHODS: The residμal solvents in beclo-metasone dipropionate were separated on HP-INNOWAX capillary colμmn. 1,6-dioxane was μsed as solvent. The carried gas was nitrogen at flow rate of 1.0 Ml-min-1. The programmed colμmn temperatμre was set as follows: maintained at 60 ℃ for 5 min and raised to 160 ℃ at the rate of 30 t ·min-1 followed by holding for 5 min. The injector temperatμre and FID detector temperatμre were controlled at 160 t and 250 X., respectively. The splitting-ratio was 5.0:1. Hydrogen was μse as fμel gas at flow rate of 30 Ml'inin-1 with air as combμstion-sμpporting gas at flow rate of 450 Ml-min-1. The makeμp gas was nitrogen at flow rate of 25 Ml-min-1. The injection volμme was 1 Μl. The contents of 4 kinds of residμal solvents in 5 batches of samples were determined μnder same condition. RESULTS: Methanol, ethanol, JV.JV-dimethylforrnamide, dimethylsμlfoxide in clobetasol propionate were completely separated. The linear ranges were 0.02 - 1.0 g-L-1 (r= 1.000). Average recovery rates were 97.6% -102.5% (RSD< 2.88%). The minimμm qμantitative concentrations were 0.60 μg·Ml-1,0.98 μg"Ml-1,0.38 μg·Ml-1, 0.85 μg-Ml-1,respectively. Methanol was foμnd in 1 batch of sample and ethanol was foμnd in 2 batches of samples. No organic solvent was foμnd in other batches of samples. CONCLUSIONS: The established method is proved to be accμrate and sensitive. It can be μsed for simμltaneoμs determination of 4 kinds of residμal organic solvents in clobetasol dipropionate.%目的:建立丙酸氯倍他索原料药中4种有机溶剂(甲醇、乙醇、N,N-二甲基甲酰胺、二甲亚砜)残留量的检测方法.方法:采用毛细管气相色谱法.色谱柱为HP-INNOWAX石英毛细管柱;溶剂为1,6-二氧六

  3. Solvent-resistant sol-gel polydimethyldiphenylsiloxane coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2008-09-26

    A sol-gel polydimethyldiphenylsiloxane (PDMDPS) coating was developed for capillary microextraction on-line hyphenated with high-performance liquid chromatography (HPLC). This coating was created using methyltrimethoxysilane (MTMS) as the sol-gel precursor and di-hydroxy-terminated PDMDPS as the sol-gel active polymer. The methyl and phenyl groups on the sol-gel active polymer and the methyl groups on the sol-gel precursor ultimately turned into pendant groups providing the ability to extract non-polar analytes. A 40-cm segment of 0.25 mm I.D. fused silica capillary containing the sol-gel PDMDPS coating was installed as an external sampling loop in an HPLC injection port. Aqueous samples containing polycyclic aromatic hydrocarbons (PAHs), aromatic compounds, ketones, and aldehydes were passed through this capillary wherein the analytes were extracted by the sol-gel coating. The extracted analytes were then transferred to the HPLC column using isocratic or gradient elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for non-polar (e.g., polycyclic aromatic hydrocarbons and aromatic compounds) as well as moderately polar compounds, such as aromatic amines, ketones, and aldehydes. The test results indicate that PDMDPS can be successfully immobilized into a sol-gel network and that the resulting solvent-resistant sol-gel organic-inorganic hybrid coating can be effectively used for on-line hyphenation of capillary microextraction with high-performance liquid chromatography. The test results also indicate that the sol-gel PDMDPS coated capillary is resistant to high-temperature solvents, making it suitable for applications in high-temperature HPLC. To the best of our knowledge, this is the first report on the creation of a silica-based sol-gel PDMDPS coating used in capillary microextraction on-line hyphenated to HPLC.

  4. Signal-Pressure Curves of Cascaded Four-Wave Mixing in Gas-Filled Capillary by fs Pulses

    Institute of Scientific and Technical Information of China (English)

    CHEN Bao-Zhen; HUANG Zu-Qia

    2005-01-01

    The theoretical framework for the cascaded four waves mixing (CFWM) in gas-filled capillary by fs pulses is constructed. Based on the theoretical framework, the signal-pressure curves (SPC) of the CFWM in gas-filled capillary by fs pulses are calculated. With a comparison between the theoretical and experimental SPC we have discussed the influence of the walk-off and Phase modulation on the SPC. At the same time, we have discussed the possible origin of the first three peaks of the SPC.

  5. 管内固相微萃取-气相色谱法在线联用技术用于水样中的痕量分析%On-Line Coupling of In-Tube Solid Phase Microextraction to Capillary Gas Chromatography for Trace Analysis of Aqueous Samples

    Institute of Scientific and Technical Information of China (English)

    关亚风; 王涵文; 刘文民

    2004-01-01

    Since the development of solid phase microextraction ( SPME ) method, many modifications have been made to improve the availability and application of the technique The in-tube SPME (ITSPME) was emerged and employed in high performance liquid chromatography (HPLC)

  6. Chemical Discrimination in Turbulent Gas Mixtures with MOX Sensors Validated by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jordi Fonollosa

    2014-10-01

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

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

    Science.gov (United States)

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

    2014-10-16

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

  8. [A simple preparation method of an electric heating apparatus for heating capillary chromatographic columns and its application in liquid chromatography-mass spectrometry system].

    Science.gov (United States)

    Jin, Zuyao; Lü, Yayao; Zhou, Shanshan; Hao, Feiran; Fu, Bin; Ying, Wantao; Qian, Xiaohong; Zhang, Yangjun

    2015-06-01

    For deep coverage of proteome, especially in performing qualitative identification and quantitative analysis of low-abundance proteins, the most commonly used method is the application of a longer capillary chromatographic column or a capillary column packed with smaller particle sizes. However, this causes another problem, the very high back pressure which results in liquid leaks in some connection parts in a liquid chromatograph. To solve this problem, an electric heating apparatus was developed to raise the temperature of a capillary column for reducing its back pressure, which was further applied in a capillary high performance liquid chromatography-tandem mass spectrometry system (cHPLC-MS/MS), and evaluated in the terms of chromatographic column back pressure and chromatographic column efficiency using bovine serum albumin (BSA) tryptic digests and yeast tryptic digests, separately. The results showed that at the optimum current, our electric heating apparatus could reduce the column pressure of a capillary column packed with 3 µm packing materials by at least 50% during the separation of BSA tryptic digestion and yeast tryptic digestion, compared with that without electric heating. The column efficiency was also increased slightly. This suggested that the electric heating apparatus can significantly reduce the column pressure, which provides an efficient way to use capillary chromatographic columns packed with smaller sizes of particles at a lower pressure.

  9. Determination of Five Organic Acids in Radix Isatidis by Column Partition Chromatography and Capillary Zone Electrophoresis

    Institute of Scientific and Technical Information of China (English)

    CHAIYi-fen; JISong-gang; ZHANGGuo-qing; LIUChang-hai

    2003-01-01

    Aim To determine five organic acids in Radix lsatidis. Method The extraction method and the column partition chromatographic conditiom were studied. Then a capillary zone dectrophorefic method was set up for the determina-tion. Results The linear ranges of quinazolinone acid, n-anthranilic acid, benzoic acid, salicylic acid, and syringic acid were 5.52 - 92.0μg·mL-1 , 5.12 - 102μg·mL-1 , 2.28 - 84.4μg·mL-1, 4.78 - 159 μg·mL-1, and 1.74- 87.0μg·mL-1 respectively. Conclusion The established method is accurate and simple.

  10. Gas-bubble snap-off under pressure driven flow in constricted noncircular capillaries

    Energy Technology Data Exchange (ETDEWEB)

    Kovscek, A.R.; Radke, C.J.

    1996-04-01

    A model for snap-off of a gas thread in a constricted cornered pore is developed. The time for wetting liquid to accumulate at a pore throat into an unstable collar is examined, as for the resulting pore-spanning lens to be displaced from the pore so that snap-off is the time may repeat. A comer-flow hydrodynamic analysis for the accumulation rate of wetting liquid due to both gradients in interfacial curvature and in applied liquid-phase pressure reveals that wetting-phase pressure gradients significantly increase the frequency of liquid accumulation for snap-off as compared to liquid rearrangement driven only by differences in pore-wall curvature. For moderate and large pressure gradients, the frequency of accumulation increases linearly with pressure gradient because of the increased rate of wetting liquid flow along pore comers. Pore topology is important to the theory, for pores with relatively small throats connected to large bodies demonstrate excellent ability to snapoff gas threads even when the initial capillary pressure is high or equivalently when the liquid saturation is low. A macroscopic momentum balance across the lens resulting from snap-off reveals that lens displacement rates are not linear with the imposed pressure drop. Instead, the frequency of lens displacement scales with powers between 0.5 and 0.6 for pores with dimensionless constriction radii between 0.15 and 0.40. Statistical percolation arguments are employed to form a generation rate expression and connect pore-level foam generation events to macroscopic pressure gradients in porous media. The rate of foam generation by capillary snap-off increases linearly with the liquid-phase pressure gradient and according to a power-law relationship with respect to the imposed gas-phase pressure gradient.

  11. Determinations of gas-liquid partition coefficients using capillary chromatographic columns. Alkanols in squalane.

    Science.gov (United States)

    Tascon, Marcos; Romero, Lílian M; Acquaviva, Agustín; Keunchkarian, Sonia; Castells, Cecilia

    2013-06-14

    This study focused on an investigation into the experimental quantities inherent in the determination of partition coefficients from gas-liquid chromatographic measurements through the use of capillary columns. We prepared several squalane - (2,6,10,15,19,23-hexamethyltetracosane) - containing columns with very precisely known phase ratios and determined solute retention and hold-up times at 30, 40, 50 and 60°C. We calculated infinite dilution partition coefficients from the slopes of the linear regression of retention factors as a function of the reciprocal of the phase ratio by means of fundamental chromatographic equations. In order to minimize gas-solid and liquid-solid interface contributions to retention, the surface of the capillary inner wall was pretreated to guarantee a uniform coat of stationary phase. The validity of the proposed approach was first tested by estimating the partition coefficients of n-alkanes between n-pentane and n-nonane, for which compounds data from the literature were available. Then partition coefficients of sixteen aliphatic alcohols in squalane were determined at those four temperatures. We deliberately chose these highly challenging systems: alcohols in the reference paraffinic stationary phase. These solutes exhibited adsorption in the gas-liquid interface that contributed to retention. The corresponding adsorption constant values were estimated. We fully discuss here the uncertainties associated with each experimental measurement and how these fundamental determinations can be performed precisely by circumventing the main drawbacks. The proposed strategy is reliable and much simpler than the classical chromatographic method employing packed columns.

  12. Liquid chromatography-gas chromatography interfacing using microbore high-performance liquid chromatography with a bundled capillary stream splitter

    Energy Technology Data Exchange (ETDEWEB)

    Raglione, T.V.; Hartwick, R.A.

    1986-11-01

    An on-line LC-GC system is presented. HPLC peak volume reduction was accomplished through the use of microbore (1.0 mm) columns. Further volume reduction was accomplished by use of a novel bundled multicapillary stream splitter between the LC detector and the GC. Applications of the system for the separation of solvent-refined coal samples are presented. Reproducibilities of the direct and split systems were 13% and 9% relative standard deviation, respectively.

  13. Real-Time Gas Identification by Analyzing the Transient Response of Capillary-Attached Conductive Gas Sensor

    Directory of Open Access Journals (Sweden)

    Behzad Bahraminejad

    2010-05-01

    Full Text Available In this study, the ability of the Capillary-attached conductive gas sensor (CGS in real-time gas identification was investigated. The structure of the prototype fabricated CGS is presented. Portions were selected from the beginning of the CGS transient response including the first 11 samples to the first 100 samples. Different feature extraction and classification methods were applied on the selected portions. Validation of methods was evaluated to study the ability of an early portion of the CGS transient response in target gas (TG identification. Experimental results proved that applying extracted features from an early part of the CGS transient response along with a classifier can distinguish short-chain alcohols from each other perfectly. Decreasing time of exposition in the interaction between target gas and sensing element improved the reliability of the sensor. Classification rate was also improved and time of identification was decreased. Moreover, the results indicated the optimum interval of the early transient response of the CGS for selecting portions to achieve the best classification rates.

  14. Surface Characterization of Glass Fiber by Inverse Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    HUANG Xiaohua; LI Bin; SHI Baoli; GUO Xuefei; JIA Lina

    2008-01-01

    The surface properties of glass fiber were quantificationally analyzed by inverse gas chromatography (IGC). Five n-alkanes (C6, C7, C8, C9, and C10) were chosen as apolar probes to characterize the dispersive component of surface free energy. Trichloromethane (CHCl3), acetone,and tetrahydrofuran (THF) were chosen as polar probes to detect the Lewis acid-base parameters. It is found that the dispersive components of free energy are 32.3, 30.5, 27.5, and 26.9 Mj/m2 at 70,80, 90, and 100 ℃, respectively. The Lewis acidic number Ka of the glass fiber is 0.512 4, and the basic number Kb is 2.862. The results mean the glass fiber is a Lewis basic material.

  15. Hansen solubility parameters for polyethylene glycols by inverse gas chromatography.

    Science.gov (United States)

    Adamska, Katarzyna; Voelkel, Adam

    2006-11-03

    Inverse gas chromatography (IGC) has been applied to determine solubility parameter and its components for nonionic surfactants--polyethylene glycols (PEG) of different molecular weight. Flory-Huggins interaction parameter (chi) and solubility parameter (delta(2)) were calculated according to DiPaola-Baranyi and Guillet method from experimentally collected retention data for the series of carefully selected test solutes. The Hansen's three-dimensional solubility parameters concept was applied to determine components (delta(d), delta(p), delta(h)) of corrected solubility parameter (delta(T)). The molecular weight and temperature of measurement influence the solubility parameter data, estimated from the slope, intercept and total solubility parameter. The solubility parameters calculated from the intercept are lower than those calculated from the slope. Temperature and structural dependences of the entopic factor (chi(S)) are presented and discussed.

  16. Feedlot lamb meat fatty acids profile characterization employing gas chromatography

    Directory of Open Access Journals (Sweden)

    M.I. Cruz-Gonzalez

    2014-06-01

    Full Text Available Fat is an important constituent in diet, not only as an energy source, but for its essential fatty acids associated to fats in foods, considering that some polyunsaturated fatty acids like linoleic, linolenic and arachidonic cannot be synthesized by superior animals like humans. Scientific evidence show that the fatty acids ingest can affect the thrombotic tendency, cardiac rhythm, endothelial function systematic inflammation, insulin sensibility and oxidative stress. Samples from 21 ovine crossbreds from Pelibuey, Blackbelly, Dorper and Katahadin (40 kg average weight feed with corn based balanced diets were taken from loin area 18 h after refrigeration. Saturated and polyunsaturated fatty acids levels were analyzed by gas chromatography. Results in this work showed that the healthy fatty acids levels are higher as compared to saturated fatty acids levels, indicating that this meat can influence consumer’s buying choice decision regarded to their health.

  17. Estimation of brassylic acid by gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mohammed J. Nasrullah, Erica N. Pfarr, Pooja Thapliyal, Nicholas S. Dusek, Kristofer L. Schiele, Christy Gallagher-Lein, and James A. Bahr

    2010-10-29

    The main focus of this work is to estimate Brassylic Acid (BA) using gas chromatography-mass spectrometry (GC-MS). BA is a product obtained from the oxidative cleavage of Erucic Acid (EA). BA has various applications for making nylons and high performance polymers. BA is a 13 carbon compound with two carboxylic acid functional groups at the terminal end. BA has a long hydrocarbon chain that makes the molecule less sensitive to some of the characterization techniques. Although BA can be characterized by NMR, both the starting material (EA) and products BA and nonanoic acid (NA) have peaks at similar {delta}, ppm values. Hence it becomes difficult for the quick estimation of BA during its synthesis.

  18. Use of a MicroStrip Gas Chamber conductive capillary plate for time-resolved X-ray area detection

    CERN Document Server

    Ochi, A; Nishi, Y; Nishi, Y; Nagayoshi, T; Ohashi, Y; Uekusa, H; Toyokawa, H

    2002-01-01

    The stable operation of MicroStrip Gas Chamber (MSGC) was successfully performed using glass capillary plate as an intermediate gas multiplier. Detection area of 95 mm sup 2 was available and fine position resolution of 90 mu m using digital readout was attained. A charge-up problem of capillary plate under intense radiation source was perfectly removed by surface conductivity inside of capillaries. The quantitative measurements using MSGC is now available in X-ray imaging. This paper also presents novel applications of X-ray diffraction studies and their preliminary results using an MSGC. Rapid measurements for X-ray crystallography of the order of a few tens of seconds were attained successfully.

  19. Identification of Cyclopentenyl Fatty Acids by Gas Liquid Chromatography and Mass Spectrometry

    DEFF Research Database (Denmark)

    Shukla, V. K. S.; Abdel-Moety, E. M.; Larsen, Elfinn;

    1979-01-01

    The straight chain fatty acids and the cyclopentenyl fatty acids present in the lipids of Hydnocarpus wightiana seeds were separated as their pyrrolidides by means of gas chromatography. A gas chromatography-mass spectrometry system confirmed the complete separation and permitted the identification...

  20. Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Sepaniak, M.J.; Cook, K.D.

    1992-09-01

    In the years following the 1986 seminal paper (J. Chromatogr. Sci., 24, 347-352) describing modern capillary zone electrophoresis (CZE), the prominence of capillary electrokinetic separation techniques has grown. A related electrochromatographic technique is micellar electrokinetic capillary chromatography (MECC). This report presents a brief synopsis of research efforts during the current 3-year period. In addition to a description of analytical separations-based research, results of efforts to develop and expand spectrometric detection for the techniques is reviewed. Laser fluorometric detection schemes have been successfully advanced. Mass spectrometric research was less fruitful, largely owing to personnel limitations. A regenerable fiber optic sensor was developed that can be used to remotely monitor chemical carcinogens, etc. (DLC)

  1. Evaluation of Aroma in Oriental Tobaccos as Based On Valeric Acid Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Dagnon S

    2014-12-01

    Full Text Available Levels of valeric acids (isovaleric and 3-methylvaleric in leaves and smoke of different tobacco types were quantified by capillary gas chromatography (GC using flame ionization detector (FID. The aroma characteristics of the smoke were scored by sensory evaluation. It was found that leaves of Oriental and burley tobaccos contain higher amounts of both valeric acid derivatives than Virginia tobaccos containing isovaleric acid but no 3-methylvaleric acid. Strong correlation between the aroma and pleasantness scores of smoke and the content of valeric acids in the leaves of Oriental tobaccos was observed, while it was not the case for leaves of Virginia and burley tobaccos. In all tobacco types no correlation between smoking characteristics and the content of valeric acids in the smoke was established. Regression models involving leaf isovaleric acid were developed that can be used to evaluate aroma and pleasantness of smoke in Oriental tobaccos. The data obtained allow the following conclusions to be drawn: a 3-methylvaleric acid may be a chemical marker to distinguish Virginia tobaccos from Oriental and burley tobaccos; b isovaleric acid content in leaves of Oriental tobaccos may be used for objective aroma evaluation that can be exploited for breeding and market purposes.

  2. Characterization of 22 Vibrio species by gas chromatography analysis of their cellular fatty acids.

    Science.gov (United States)

    Urdaci, M C; Marchand, M; Grimont, P A

    1990-05-01

    The cellular fatty acid compositions of 51 Vibrio strains belonging to 22 species as well as five Aeromonas strains were determined by using capillary gas-liquid chromatography (GLC). The major fatty acids were most often hexadecenoic, hexadecanoic and octadecenoic acids. Heptadecenoic acid was present in significant amounts in V. alginolyticus, V. natriegens, V. parahaemolyticus and "Vibrio navarrensis". Twenty fatty acids including branched and hydroxy acids were detected in the genus Vibrio. Quantitative results were treated by principal component analysis to display groups of strains. The first three components (accounting for 69% of the variance) showed the type strains of V. fischeri, V. ordalii, V. damsela, V. mediterranei, V. tubiashii, V. campbellii, V. pelagius, V. gazogenes, and V. nereis to be unclustered. V. alginolyticus (4 strains) and V. parahaemolyticus (4 strains) showed some overlap and the type strain of V. natriegens was in their neighborhood. V. harveyi (4 strains) formed a cluster and V. vulnificus was in its vicinity. V. cholerae (5 strains) overlapped with V. diazotrophicus (3 strains) and was close to the type strain of V. mimicus and V. anguillarum. V. metschnikovii (3 strains) clustered with the type strain of V. cincinnatiensis. A decision tree was devised for the identification of Vibrio species based on qualitative characteristics of fatty acid patterns. However, the following three groups, V. alginolyticus-V. parahaemolyticus-V. natriegens, V. metschnikovii-V. cincinnatiensis and V. cholerae-V. mimicus could not be split into such a decision tree.

  3. QUANTITATIVE DETERMINATION OF FATTY ACIDS IN INFANT FORMULA BY GAS CHROMATOGRAPHY WITHOUT DERIVATIZATION

    Directory of Open Access Journals (Sweden)

    M. R. Oveisi

    2006-08-01

    Full Text Available Fatty acids play important roles in biological systems and the newborns fatty acids requirements are covered only by the milk. It is of particular interest to qualify the content of the fatty acids in the milk. This study was performed to determine the levels of some fatty acids in the infant formulas and also to describe a method without derivatization for the fatty acids analysis and applying it to the control of infant formulas. Free fatty acids were produced by adding isopropanol- KOH to milk fat extract and heating it to saponify and acidify by H2SO4. Free fatty acids were extracted and were quantified by capillary gas chromatography on a fused silica column (AT-1000 and flame ionization detector. The average experimental values of lauric, palmitic, stearic and linoleic fatty acids contents of twenty infant formulas were 6.47, 16.52, 2.11 and 14.56 g/100g, respectively. The obtained experimental values of lauric and linoleic fatty acids contents of twenty infant formulas were in good agreement with the values proposed by standards of codex alimentary.

  4. [Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

    Science.gov (United States)

    Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

    2014-05-01

    A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

  5. Authentication of beeswax (Apis mellifera) by high-temperature gas chromatography and chemometric analysis.

    Science.gov (United States)

    Maia, Miguel; Nunes, Fernando M

    2013-01-15

    Chemical characterization and authentication of beeswax of Apis mellifera was performed by high temperature capillary gas chromatography coupled to electron impact mass spectrometry or to flame ionisation detection and chemometric analysis. Many major components (>50) of beeswax, odd and even hydrocarbons, oleofin, palmitate, oleate and hydroxypalmitate monoesters were detected, and for the first time palmitate and oleate monoesters esterified with 1-octadecanol and 1-eicosanol are reported to be present in beeswax. Unsupervised pattern recognition procedures, cluster analysis and principal component analysis, were used to find data patterns and successfully differentiate authentic and paraffin adulterated beeswax based on the chemical profile obtained. Independent assessment of beeswax quality and performance of the unsupervised classification methods were performed using classical analytical parameters. The discrimination power of the chemometric unsupervised methods for detection of paraffin adulterated beeswax was superior to the discriminating power of classical analytical parameters. Using linear discriminant analysis, classification rules for authentic and paraffin adulterated beeswax samples were developed. The model was validated by leave-one-out cross validation and showed good recognition and prediction abilities, 100% and 99%, respectively.

  6. Determination of fluvalinate residues in beeswax by gas chromatography with electron-capture detection.

    Science.gov (United States)

    Tsigouri, A; Menkissoglu-Spiroudi, U; Thrasyvoulou, A T; Diamantidis, G C

    2000-01-01

    A simple, rapid, and accurate method is described for the determination of residual fluvalinate in beeswax. The procedure consists of partitioning on a disposable column of diatomaceous earth (Extrelut), followed by chromatographic cleanup on a Florisil cartridge. The final extract is analyzed by capillary gas chromatography with electron-capture detection (GC-ECD). Briefly, wax samples were dissolved in n-hexane, and the solutions were sonicated and transferred to Extrelut columns. The fluvalinate was extracted with acetonitrile, and a portion of the extract was cleaned up on a Florisil cartridge. The fluvalinate was eluted with diethyl ether-n-hexane (1 + 1) and directly determined by GC-ECD. Recoveries from wax samples spiked at 5 fortification levels (100-1500 microg/kg) ranged from 77.4 to 87.3%, with coefficients of variation of 5.12-8.31%. The overall recovery of the method was 81.4 +/- 3.2%, and the limit of determination was 100 microg/kg.

  7. Improved sensitivity gas chromatography-mass spectrometry determination of parabens in waters using ionic liquids.

    Science.gov (United States)

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2016-01-01

    A new procedure for the introduction of ionic liquid samples in gas chromatography (GC) is proposed. This procedure, based on microvial insert thermal desorption, allows the direct analysis of the compounds preconcentrated by ionic liquid based liquid-liquid microextraction (IL-LLME) using the combination of a thermal desorption unit (TDU) and a programmed temperature vaporization injector (PTV). Two different IL-LLME methodologies, one based on the formation of a microdroplet emulsion by dispersive liquid-liquid microextraction (DLLME) and other through ultrasound-assisted emulsification microextraction (USAEME) were studied and evaluated. IL-DLLME proved advantageous and consequently, it was adopted for preconcentration purposes. This easy to apply approach was used for the determination of five parabens (methyl-, ethyl-, propyl-, butyl- and isobutyl paraben) in swimming pool waters, after in situ acetylation. The optimized conditions of TDU/PTV allowed the analytes contained in 20 µL of the enriched IL to be transferred to the capillary column. Quantification of the samples was carried out against aqueous standards, and quantification limits of between 4.3 and 8.1 ng L(-1) were obtained, depending on the compound. Concentrations of between 9 and 47 ng L(-1) for some analytes were obtained in the analysis of ten samples.

  8. Application of finite inverse gas chromatography in hypromellose acetate succinate-water-acetone systems.

    Science.gov (United States)

    Chiu, Sheng-Wei; Sturm, Derek R; Moser, Justin D; Danner, Ronald P

    2016-09-30

    A modification of a GC was developed to investigate both infinitely dilute and finite concentrations of solvents in polymers. Thermodynamic properties of hypromellose acetate succinate (HPMCAS-L)-acetone-water systems are important for the optimization of spray-drying processes used in pharmaceutical manufacturing of solid dispersion formulations. These properties, at temperatures below the glass transition temperature, were investigated using capillary column inverse gas chromatography (CCIGC). Water was much less soluble in the HPMCAS-L than acetone. Experiments were also conducted at infinitely dilute concentrations of one of the solvents in HPMCAS-L that was already saturated with the other solvent. Overall the partitioning of the water was not significantly affected by the presence of either water or acetone in the polymer. The acetone partition coefficient decreased as either acetone or water was added to the HPMCAS-L. A representation of the HPMCAS-L structure in terms of UNIFAC groups has been developed. With these groups, the UNIFAC-vdw-FV model did a reasonable job of predicting the phase equilibria in the binary and ternary systems. The Flory-Huggins correlation with fitted interaction parameters represented the data well.

  9. Rapid determination of acrylamide contaminant in conventional fried foods by gas chromatography with electron capture detector.

    Science.gov (United States)

    Zhang, Yu; Dong, Yi; Ren, Yiping; Zhang, Ying

    2006-05-26

    Gas chromatography coupled with electron capture detector (GC-ECD) was successfully developed and applied for the rapid determination of acrylamide in conventional fried foods, such as potato crisps, potato chips, and fried chicken wings. The method included defatting with n-hexane, extraction with aqueous solution of sodium chloride (NaCl), derivatization with potassium bromate (KBrO3) and potassium bromide (KBr), and liquid-liquid extraction with ethyl acetate. The final acrylamide extract was analyzed by GC-ECD for quantification and by GC-MS for confirmation. The chromatographic analysis was performed on the HP-INNOWax capillary column, and good retention and peak response of acrylamide were achieved under the optimal conditions (numbers of theoretical plates N = 83,815). The limit of detection (LOD) was estimated to be 0.1 microg kg(-1) on the basis of ECD technique. Recoveries of acrylamide from conventional samples spiked at levels of 150, 500 and 1000 microg kg(-1) (n = 4 for each level) ranged between 87 and 97% with relative standard deviations (RSD) of less than 4%. Furthermore, the GC-ECD method showed that no clean-up steps of acrylamide derivative would be performed prior to injection and was slightly more sensitive than the MS/MS-based methods. Validation and quantification results demonstrated that this method should be regarded as a new, low-cost, and robust alternative for conventional investigation of acrylamide.

  10. Determination of terpenes in tequila by solid phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Peña-Alvarez, Araceli; Capella, Santiago; Juárez, Rocío; Labastida, Carmen

    2006-11-17

    Solid phase microextraction and capillary gas chromatography-mass spectrometry were used for the determination of seven terpenes in tequila. The method was selected based on the following parameters: coating selection (PA, PDMS, CW/DVB, and PDMS/DVB), extraction temperature, addition of salt, and extraction time profile. The extraction conditions were: PDMS/DVB fiber, Headspace, 100% NaCl, 25 degrees C extraction temperature, 30 min extraction time and stirring at 1200 rpm. The calibration curves (50-1000 ng/ml) for the terpenes followed linear relationships with correlation coefficients (r) greater than 0.99, except for trans,trans-farnesol (r = 0.98). RSD values were smaller than 10% confirmed that the technique was precise. Samples from 18 different trade brands of "Aged" tequila analyzed with the developed method showed the same terpenes in different concentrations. The analytical procedure used is selective, robust (more than 100 analyses with the same fiber), fast and of low-cost.

  11. Use of an accelerometer and a microphone as gas detectors in the online quantitative detection of hydrogen released from ammonia borane by gas chromatography.

    Science.gov (United States)

    He, Yi-San; Chen, Kuan-Fu; Lin, Chien-Hung; Lin, Min-Tsung; Chen, Chien-Chung; Lin, Cheng-Huang

    2013-03-19

    The use of an accelerometer as a gas detector in gas chromatography (GC) is described for the first time. A milli-whistle was connected to the outlet of the GC capillary. When the eluted and GC carrier gases pass through the capillary and milli-whistle, a sound is produced. After a fast Fourier transform (FFT), the sound wave generated from the milli-whistle is picked up by a microphone and the resulting vibration of the milli-whistle body can be recorded by an accelerometer. The release of hydrogen gas, as the result of thermal energy, from ammonia borane (NH3BH3), which has been suggested as a storage medium for hydrogen, was selected as the model sample. The findings show that the frequencies generated, either by sound or by the vibration from the whistle body, were identical. The concentration levels of the released hydrogen gas can be determined online, based on the frequency changes. Ammonia borane was placed in a brass reservoir, heated continually, and the released hydrogen gas was directly injected into the GC inlet at 0.5 min intervals, using a home-built electromagnetic pulse injector. The concentration of hydrogen for each injection can be calculated immediately. When the ammonia borane was encapsulated within a polycarbonate (PC) microtube array membrane, the temperature required for the release of hydrogen can be decreased, which would make such a material more convenient for use. The findings indicate that 1.0 mg of ammonia borane can produce hydrogen in the range of 1.0-1.25 mL, in the temperature range of 85-115 °C.

  12. Analysis of odour compounds from scented consumer products using gas chromatography-mass spectrometry and gas chromatography-olfactometry.

    Science.gov (United States)

    Bartsch, Jennifer; Uhde, Erik; Salthammer, Tunga

    2016-01-21

    Scented consumer products are being bought in increasing amounts and gaining more popularity. There is, however, relatively little information available about their ingredients, emissions and allergenic potential. Frequently, a mixture of different fragrance substances and not solely an individual substance contributes to the overall desired smell. The aim of this study was to investigate the odorous volatile organic compounds (OVOCs) in consumer products containing fragrances. Over 44 products were selected: various scented candles, printing products with different scent types and other products types particularly meant to be used indoors. Measurements were carried out in a desiccator. Air samples were collected on thermal desorption tubes to determine the released fragrance substances by means of gas chromatography-mass spectrometry (GC-MS). Moreover, gas chromatography-olfactometry (GC-O) was used to obtain sensory data and to ensure no important odorant was overlooked. Using both methods it was possible to distinguish between odour active and inactive compounds and subsequently to identify almost 300 different odorants across all scented products. Besides the advantage of differentiation, as the human nose is a very sensitive detector, GC-O was found to be a useful tool for detecting traces and chosen target compounds. One focus in this study lay on the 26 EU-regulated fragrance allergens to prove their relevance in scented consumer goods. In total, 18 of them were identified, with at least one substance being present in almost every product. Benzyl alcohol, cinnamaldehyde, citronellol, eugenol, linalool and limonene were the prevalently detected allergens. Particularly linalool and limonene were observed in over 50% of the products. In addition, eugenol appeared to be one of the most frequently detected compounds in trace-level concentrations in the candle emissions.

  13. Capillary Electrophoresis in the Analysis of Polyunsaturated Fatty Acids

    Directory of Open Access Journals (Sweden)

    Gabriel Hancu

    2015-12-01

    Full Text Available The aim of this study to inventory the main electrophoretic methods for identification and quantitative determination of fatty acids from different biological matrices. Critical analysis of electrophoretic methods reported in the literature show that the determination of polyunsaturated fatty acids can be made by: capillary zone electrophoresis, micellar electrokinetic chromatography and microemulsion electrokinetic chromatography using different detection systems such as ultraviolet diode array detection, laser induced fluorescence or mass – spectrometry. Capillary electrophoresis is a fast, low-cost technique used for polyunsaturated fatty acids analysis although their determination is mostly based on gas chromatography.

  14. Analysis of water from the Space Shuttle and Mir Space Station by ion chromatography and capillary electrophoresis

    Science.gov (United States)

    Orta, D.; Mudgett, P. D.; Ding, L.; Drybread, M.; Schultz, J. R.; Sauer, R. L.

    1998-01-01

    Drinking water and condensate samples collected from the US Space Shuttle and the Russian Mir Space Station are analyzed routinely at the NASA-Johnson Space Center as part of an ongoing effort to verify water quality and monitor the environment of the spacecraft. Water quality monitoring is particularly important for the Mir water supply because approximately half of the water consumed is recovered from humidity condensate. Drinking water on Shuttle is derived from the fuel cells. Because there is little equipment on board the spacecraft for monitoring the water quality, samples collected by the crew are transported to Earth on Shuttle or Soyuz vehicles, and analyzed exhaustively. As part of the test battery, anions and cations are measured by ion chromatography, and carboxylates and amines by capillary electrophoresis. Analytical data from Shuttle water samples collected before and after several missions, and Mir condensate and potable recovered water samples representing several recent missions are presented and discussed. Results show that Shuttle water is of distilled quality, and Mir recovered water contains various levels of minerals imparted during the recovery processes as designed. Organic ions are rarely detected in potable water samples, but were present in humidity condensate samples.

  15. Facile preparation of organic-silica hybrid monolith for capillary hydrophilic liquid chromatography based on "thiol-ene" click chemistry.

    Science.gov (United States)

    Chen, Ming-Luan; Zhang, Jun; Zhang, Zheng; Yuan, Bi-Feng; Yu, Qiong-Wei; Feng, Yu-Qi

    2013-04-05

    In this work, a one-step approach to facile preparation of organic-inorganic hybrid monoliths was successfully developed. After vinyl-end organic monomers and azobisisobutyronitrile (AIBN) were mixed with hydrolyzed tetramethoxysilane (TMOS) and 3-mercaptopropyltrimethoxysilane (MPTMS), the homogeneous mixture was introduced into a fused-silica capillary for simultaneous polycondensation and "thiol-ene" click reaction to form the organic-silica hybrid monoliths. By employing this strategy, two types of organic-silica hybrid monoliths with positively charged quaternary ammonium and amide groups were prepared, respectively. The functional groups were successfully introduced onto the monoliths during the sol-gel process with "thiol-ene" click reaction, which was demonstrated by ζ-potential assessment, energy dispersive X-ray spectroscopy (EDX), and Fourier transform infrared (FT-IR) spectroscopy. The porous structure of the prepared monolithic columns was examined by scanning electron microscopy (SEM), nitrogen adsorption-desorption measurement, and mercury intrusion porosimetry. These results indicate the prepared organic-silica hybrid monoliths possess homogeneous column bed, large specific surface area, good mechanical stability, and excellent permeability. The prepared monolithic columns were then applied for anion-exchange/hydrophilic interaction liquid chromatography. Different types of analytes, including benzoic acids, inorganic ions, nucleosides, and nucleotides, were well separated with high column efficiency around 80,000-130,000 plates/m. Taken together, we present a facile and universal strategy to prepare organic-silica hybrid monoliths with a variety of organic monomers using one-step approach.

  16. Optimization of micellar electrokinetic capillary chromatography method using central composite design for the analysis of components in Yangwei granule

    Institute of Scientific and Technical Information of China (English)

    Shu-fang WANG; Hai-yan FANG; Hai-bin QU

    2011-01-01

    Central composite design (CCD), together with multiple linear regression, was successfully used to optimize the electrophoretic buffer system of micellar electrokinetic capillary chromatography (MEKC) for the determination of albiflorin, paeoniflorin, liquiritin, and glycyrrhizic acid in the traditional Chinese medicine (TCM) prescription,Yangwei granule. Concentrations of sodium deoxycholate (SDC) and borate, and proportions of ammonia, acetonitrile,and methanol were optimized. The total resolutions of peaks between the analytes and their adjacent peaks in real samples were integrated into the evaluation index of separation efficiency. The optimum electrophoretic buffer contained 80 mmol/L SDC, 20 mmol/L borate, 5% (v/v) methanol, 0.5% (v/v) ammonia, and 5% (v/v) acetonitrile. The correlation coefficients (R2) between the peak areas and the corresponding concentrations of analytes were greater than 0.9956. The limits of detection (LODs) (S/N=3) of the analytes were 0.97-4.00 μg/mi. The results indicate the superiority of CCD in optimizing the separation conditions of complex samples such as TCM prescriptions.

  17. Capillary ion chromatography with on-column focusing for ultra-trace analysis of methanesulfonate and inorganic anions in limited volume Antarctic ice core samples.

    Science.gov (United States)

    Rodriguez, Estrella Sanz; Poynter, Sam; Curran, Mark; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

    2015-08-28

    Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with anions, including fluoride, methanesulfonate, chloride, sulfate and nitrate anions. Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak.

  18. Analysis of Critical Permeabilty, Capillary Pressure and Electrical Properties for Mesaverde Tight Gas Sandstones from Western U.S. Basins

    Energy Technology Data Exchange (ETDEWEB)

    Alan Byrnes; Robert Cluff; John Webb; John Victorine; Ken Stalder; Daniel Osburn; Andrew Knoderer; Owen Metheny; Troy Hommertzheim; Joshua Byrnes; Daniel Krygowski; Stefani Whittaker

    2008-06-30

    Although prediction of future natural gas supply is complicated by uncertainty in such variables as demand, liquefied natural gas supply price and availability, coalbed methane and gas shale development rate, and pipeline availability, all U.S. Energy Information Administration gas supply estimates to date have predicted that Unconventional gas sources will be the dominant source of U.S. natural gas supply for at least the next two decades (Fig. 1.1; the period of estimation). Among the Unconventional gas supply sources, Tight Gas Sandstones (TGS) will represent 50-70% of the Unconventional gas supply in this time period (Fig. 1.2). Rocky Mountain TGS are estimated to be approximately 70% of the total TGS resource base (USEIA, 2005) and the Mesaverde Group (Mesaverde) sandstones represent the principal gas productive sandstone unit in the largest Western U.S. TGS basins including the basins that are the focus of this study (Washakie, Uinta, Piceance, northern Greater Green River, Wind River, Powder River). Industry assessment of the regional gas resource, projection of future gas supply, and exploration programs require an understanding of reservoir properties and accurate tools for formation evaluation. The goal of this study is to provide petrophysical formation evaluation tools related to relative permeability, capillary pressure, electrical properties and algorithms for wireline log analysis. Detailed and accurate moveable gas-in-place resource assessment is most critical in marginal gas plays and there is need for quantitative tools for definition of limits on gas producibility due to technology and rock physics and for defining water saturation. The results of this study address fundamental questions concerning: (1) gas storage; (2) gas flow; (3) capillary pressure; (4) electrical properties; (5) facies and upscaling issues; (6) wireline log interpretation algorithms; and (7) providing a web-accessible database of advanced rock properties. The following text

  19. Carbon monoxide measurement by gas chromatography; Mesure du monoxyde de carbone par chromatographie en phase gazeuse

    Energy Technology Data Exchange (ETDEWEB)

    Gros, V.; Sarda-Esteve, R.; Bonsang, B.; Ramonet, M.

    1998-09-01

    Although carbon monoxide (CO) is present in trace quantities in the atmosphere (0.1 ppm -or parts per million in volume- on average), the study of this gas is important. Indeed, its impact on human can be dangerous at high level of concentration on the hand and it constitutes one of the main precursor of ozone in presence of concentration on the one hand and it constitutes one of the main precursor of ozone in presence of other pollutants on the other hand. Finally, CO affects the levels of several important greenhouse gases, through its reaction with hydroxyl radicals (OH). CO is measured in the atmosphere since the mid 60's by various methods. Among them, gas chromatography has the advantage to combine a low detection limit with a high precision. This report details the improvements made on the measurement analyser which allowed to perform automatic CO measurements in remote areas with low mixing ratios of carbon monoxide. This report describes some quality tests and the results of various applications. (authors)

  20. [Determination of chemical components of volatile oil from Cuminum cyminum L. by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Yan, Jian-hui; Tang, Ke-wen; Zhong, Ming; Deng, Ning-hua

    2002-11-01

    Volatile oil was extracted from Cuminum cyminum L. by using steam distillation. More than sixty peaks were separated and 49 compounds were identified by gas chromatography-mass spectrometry (GC-MS). The relative amounts of the components were determined by area normalization method. Among the 49 compounds identified, there were 16 hydrocarbons and 32 oxygenated compounds. The main compnents were cuminal and safranal (accounting for 32.26% and 24.46% respectively in the components identified). The other nine compounds with contents all over 1%, were monterpenes, sesquiterpenes, aromatic aldehydes and aromatic oxides etc. The other components with relatively small amounts were chiefly terpenes, terpenols, terpenals, terpenones, terpene esters and aromatic compounds. It is good to separate polar and apolar components in the volatile oil from Cuminum cyminum L. on the GC capillary column of moderate polarity.

  1. Capillary electrophoresis and column chromatography in biomedical chiral amino acid analysis.

    Science.gov (United States)

    Waldhier, Magdalena C; Gruber, Michael A; Dettmer, Katja; Oefner, Peter J

    2009-06-01

    Free amino acids are typically quantified as the sum of their enantiomers, because in terrestrial organisms they mainly exist in the left-handed form. However, with increasing understanding of the biological significance of right-handed amino acids interest in enantioselective quantification of amino acids has steadily increased. Initially, electrophoretic and chromatographic methods using chiral (pseudo)-stationary phases or chiral eluents were applied to the separation of amino acid enantiomers. Later, derivatization of amino acids prior to chromatography with chiral reagents gained in popularity, because the diastereomers formed can be resolved on conventional reversed-phase columns. Novel multi-interaction chiral columns turned attention back to direct chiral chromatographic methods. Hyphenation to mass spectrometry has increasingly replaced optical detection because of superior selectivity, although this has not obviated the need for baseline resolution of amino acid enantiomers. Despite the progress made, enantioselective separation and quantification of amino acids remains an analytical challenge owing to frequently incomplete resolution of all naturally occurring enantiomers and insufficient sensitivity for the determination of the trace amounts of D-amino acids typically found in biological fluids and tissues.

  2. Chromatography.

    Science.gov (United States)

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  3. Gas chromatography coupled with atomic absorption spectrometry — a sensitive instrumentation for mercury speciation

    Science.gov (United States)

    Emteborg, Håkan; Sinemus, Hans-Werner; Radziuk, Bernard; Baxter, Douglas C.; Frech, Wolfgang

    1996-07-01

    New instrumentation for the speciation of mercury is described, and is applied to the analysis of natural water samples. The separation of mercury species is effected using gas chromatography of derivatized mercury species on a widebore capillary column. The solvent is vented using a bypass valve and the separated mercury species are pyrolysed on-line at 800°C for production of mercury atoms. These are then detected by atomic absorption spectrometry (AAS) at the 253.7 and 184.9 nm lines simultaneously in a quartz cuvette. The use of the 184.9 nm line provides a more than five-fold increase in sensitivity compared with the conventional 253.7 nm line and an absolute detection limit of 0.5 pg of mercury. The dynamic range of the combined analytical lines provides a linear response over more than three orders of magnitude. A number of organic compounds not containing mercury are also detected following pyrolysis, especially at the 184.9 nm line. These background species must not co-elute at the retention times for methyl- and inorganic mercury, as otherwise a positive interference would result. By maximizing the chromatographic resolution and minimizing the band broadening in the cuvette by use of a make-up gas, the retention times of interest are freed from co-eluting background peaks. The instrumentation has been applied to the determination of ng l -1 concentrations of methyl- and inorganic mercury in Lake Constance, Germany and within the Lake Constance drinking water supply organization, Bodenseewasserversorgung (BWV). The accuracy for the sum of methyl- and inorganic mercury has been assessed by comparison with an independent method for total mercury based on AAS detection implemented at BWV. Relative detection limits using 1 litre water samples and 15 ml injections of the final hexane extract were 0.03 ng l -1 for methylmercury and 0.4 ng l -1 for inorganic mercury based on the 3j criterion.

  4. Fully Automated Portable Comprehensive 2-Dimensional Gas Chromatography Device.

    Science.gov (United States)

    Lee, Jiwon; Zhou, Menglian; Zhu, Hongbo; Nidetz, Robert; Kurabayashi, Katsuo; Fan, Xudong

    2016-10-06

    We developed a fully automated portable 2-dimensional (2-D) gas chromatography (GC x GC) device, which had a dimension of 60 cm × 50 cm × 10 cm and weight less than 5 kg. The device incorporated a micropreconcentrator/injector, commercial columns, micro-Deans switches, microthermal injectors, microphotoionization detectors, data acquisition cards, and power supplies, as well as computer control and user interface. It employed multiple channels (4 channels) in the second dimension ((2)D) to increase the (2)D separation time (up to 32 s) and hence (2)D peak capacity. In addition, a nondestructive flow-through vapor detector was installed at the end of the (1)D column to monitor the eluent from (1)D and assist in reconstructing (1)D elution peaks. With the information obtained jointly from the (1)D and (2)D detectors, (1)D elution peaks could be reconstructed with significantly improved (1)D resolution. In this Article, we first discuss the details of the system operating principle and the algorithm to reconstruct (1)D elution peaks, followed by the description and characterization of each component. Finally, 2-D separation of 50 analytes, including alkane (C6-C12), alkene, alcohol, aldehyde, ketone, cycloalkane, and aromatic hydrocarbon, in 14 min is demonstrated, showing the peak capacity of 430-530 and the peak capacity production of 40-80/min.

  5. [Determination of dimethyl ether correction factors in gas chromatography with TCD and FID].

    Science.gov (United States)

    Chen, J; Zhang, L; Yang, L; Cai, G

    1997-05-01

    Dimethyl ether (DME) correction factors in gas chromatography with thermal conductivity detector (TCD) and flame ionization detector (FID) by using H2 as carrier gas were determined in this work. The homemade DME gas was quantitatively absorbed in ice-cold water. With ethanol as standard, the aqueous mixture was injected into a gas chromatograph, equipped with serially-connected TCD and FID. The weight correction factors of DME based on methanol were 0.86 and 0.55 for TCD and FID respectively. The result for TCD was also confirmed by calculation based on the stoichiometrical transformation of methanol into DME in reaction gas chromatography.

  6. Photopolymerization of acrylamide as a new functionalization way of silica monoliths for hydrophilic interaction chromatography and coated silica capillaries for capillary electrophoresis.

    Science.gov (United States)

    El-Debs, R; Marechal, A; Dugas, V; Demesmay, C

    2014-01-24

    A simple, rapid and localizable photochemical process for the preparation of hydrophilic coated capillary and silica-based monolithic capillary columns is described. The process involves the free radical polymerization of acrylamide monomers onto acrylate pre-activated silica surface triggered by UV photoinitiation. The experimental conditions (monomer content, time of irradiation) were optimized on silica monolithic columns by monitoring the evolution of the chromatographic properties (retention, permeability, efficiency) in HILIC mode using a set of nucleosides as test solutes. Compared to thermal polymerization process, the photoinitiation allows the preparation of highly retentive and efficient HILIC monolithic columns in less than 10min of irradiation. This process was then successfully applied to the surface coating of fused silica capillary walls. In addition to its relative high stability and ability to reduce the electroosmotic flow, this polyacrylamide coating is localizable. Benefits of this localizable photochemical process are highlighted through the conception of an in-line integrated bimodal microseparation tool combining a SPE preconcentration step on a photografted silica monolith and an electrokinetic separation step in a polyacrylamide photopolymerized capillary section. Two neuropeptides are used as model solutes to illustrate the suitability of this approach.

  7. Fluorescent polymer coated capillaries as optofluidic refractometric sensors.

    Science.gov (United States)

    Rowland, Kristopher J; François, Alexandre; Hoffmann, Peter; Monro, Tanya M

    2013-05-06

    A capillary microresonator platform for refractometric sensing is demonstrated by coating the interior of thick-walled silica capillaries with a sub-wavelength layer of high refractive index, dye-doped polymer. No intermediate processing, such as etching or tapering, of the capillary is required. Side illumination and detection of the polymer layer reveals a fluorescence spectrum that is periodically modulated by whispering gallery mode resonances within the layer. Using a Fourier technique to calculate the spectral resonance shifts, the fabricated capillary resonators exhibited refractometric sensitivities up to approximately 30 nm/RIU upon flowing aqueous glucose through them. These sensors could be readily integrated with existing biological and chemical separation platforms such as capillary electrophoresis and gas chromatography where such thick walled capillaries are routinely used with polymer coatings. A review of the modelling required to calculate whispering gallery eigenmodes of such inverted cylindrical resonators is also presented.

  8. [Determination of partition coefficient of dissolved gases in transformer oil using phase ratio variation method and static headspace gas chromatography].

    Science.gov (United States)

    Zhao, Jinghong; Wang, Hailong; Liu, Wenmin; Zhou, Yansheng; Guan, Yafeng

    2004-05-01

    The partition coefficients of dissolved gases in transformer oil were determined using a phase ratio variation method and static headspace gas chromatography (GC). A pressure balancing and gas volume-metering device was connected to the vent of a sample loop on a six-port injection valve of the GC. The gas phase sample from the headspace vial of 25 mL was transferred to an 80 microL sample-loop through a fused silica capillary of 0.53 mm i.d., and then separated and determined quantitatively by GC. A 2 m x 1 mm i.d. GDX502 micro-packed column was used for the separation. Five different gas-liquid volume ratios in the headspace vials were measured at different equilibrium concentrations. The partition coefficients of hydrocarbon gases including methane, acetylene, ethylene, ethane and propane dissolved in transformer oil were determined by using linear regression analysis at 20 degrees C and 50 degrees C separately. The errors between the real values and regression values from experimental data were less than 4.14% except methane. Fundamental data for on-line measurement of dissolved gases in transformer oil are provided by GC.

  9. Sol-gel methyl coating in capillary microextraction hyphenated on-line with high-performance liquid chromatography Counterintuitive extraction behavior for polar analytes.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2008-07-18

    A sol-gel coating with anchored methyl groups was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). This was accomplished by using methyltrimethoxysilane as the sol-gel precursor. The methyl group on the sol-gel precursor ultimately turned into a pendant group on the created sol-gel coating and was primarily responsible for the extraction of nonpolar analytes. A 40-cm segment of 0.25mm I.D. fused silica capillary containing the sol-gel methyl coating on the inner surface was installed as a sampling loop in an HPLC injection port. The analytes were extracted by the coating when an aqueous sample containing the analytes was passed through this capillary. The extracted analytes were then transferred to the HPLC column using isocratic elution with an acetonitrile/water mobile phase. This capillary demonstrated excellent extraction capability for polycyclic aromatic hydrocarbons and ketones. Unexpectedly, this coating also provided good extraction for polar analytes, including aromatic phenols, alcohols, and amines. Considering the fact that the methyl group is nonpolar in nature, such an extraction behavior of sol-gel methyl coating toward polar analytes is counterintuitive. Thus, sol-gel sorbents with short alkyl side chains have the potential to offer a polymer-free alternative to traditional sol-gel capillary microextraction (CME) media commonly prepared with the use of polymers in the sol solution. Elimination of polymers from the sol-gel coating solution is conducive to improving thermal stability and solvent tolerance of the created sol-gel extracting phase. This also makes the preparation of sol-gel coatings facile and cost-effective. Possessing excellent solvent stability, such sol-gel coatings offer the opportunity for effective on-line hyphenation of capillary microextraction with HPLC and other liquid-phase separation techniques that employ organo-aqueous mobile phases.

  10. A microfluidic-based enzymatic assay for bioactivity screening combined with capillary liquid chromatography and mass spectrometry.

    Science.gov (United States)

    de Boer, Arjen R; Bruyneel, Ben; Krabbe, Johannes G; Lingeman, Henk; Niessen, Wilfried M A; Irth, Hubertus

    2005-11-01

    The design and implementation of a continuous-flow microfluidic assay for the screening of (complex) mixtures for bioactive compounds is described. The microfluidic chip featured two microreactors (1.6 and 2.4 microL) in which an enzyme inhibition and a substrate conversion reaction were performed, respectively. Enzyme inhibition was detected by continuously monitoring the products formed in the enzyme-substrate reaction by electrospray ionization mass spectrometry (ESI-MS). In order to enable the screening of mixtures of compounds, the chip-based assay was coupled on-line to capillary reversed-phase high-performance liquid chromatography (HPLC) with the HPLC column being operated either in isocratic or gradient elution mode. In order to improve the detection limits of the current method, sample preconcentration based on a micro on-line solid-phase extraction column was employed. The use of electrospray MS allowed the simultaneous detection of chemical (MS spectra) and biological parameters (enzyme inhibition) of ligands eluting from the HPLC column. The present system was optimized and validated using the protease cathepsin B as enzyme of choice. Inhibition of cathepsin B is detected by monitoring three product traces, obtained by cleavage of the substrate. The two microreactors provided 32 and 36 s reaction time, respectively, which resulted in sufficient assay dynamics to enable the screening of bioactive compounds. The total flow rate was 4 microL min-1, which a 25-fold decrease was compared with a macro-scale system described earlier. Detection limits of 0.17-2.6 micromol L-1 were obtained for the screening of inhibitors, which is comparable to either microtiter plate assays or continuous-flow assays described in the literature.

  11. A High Position Resolution X-ray Detector: an Edge on Illuminated Capillary Plate Combined with a Gas Amplification Structure

    CERN Document Server

    Iacobaeus, C; Lund-Jensen, B; Ostling, J; Pavlopoulos, P; Peskov, Vladimir; Tokanai, F

    2006-01-01

    We have developed and successfully tested a prototype of a new type of high position resolution hybrid X-ray detector. It contains a thin wall lead glass capillary plate converter of X-rays combined with a microgap parallel-plate avalanche chamber filled with gas at 1 atm. The operation of these converters was studied in a wide range of X-ray energies (from 6 to 60 keV) at incident angles varying from 0-90 degree. The detection efficiency, depending on the geometry, photon energy, incident angle and the mode of operation, was between 5-30 percent in a single step mode and up to 50 percent in a multi-layered combination. Depending on the capillary geometry, the position resolution achieved was between 0.050-0.250 mm in digital form and was practically independent of the photon energy or gas mixture. The usual lead glass capillary plates operated without noticeable charging up effects at counting rates of 50 Hz/mm2, and hydrogen treated capillaries up to 10E5 Hz/mm2. The developed detector may open new possibil...

  12. Direct determination of melamine in dairy products by gas chromatography/mass spectrometry with coupled column separation

    Energy Technology Data Exchange (ETDEWEB)

    Xu Xiaomin [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou, 310028 (China); Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051 (China); Ren Yiping [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051 (China); Zhu Yun [Xinjiang Uygur Autonomous Region Center for Disease Control and Prevention, Urumchi, 830002 (China); Cai Zengxuan; Han Jianlong; Huang Baifen [Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051 (China); Zhu Yan, E-mail: zhuyan@zju.edu.cn [Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou, 310028 (China)

    2009-09-14

    A coupled capillary column system was developed for the qualitative and quantitative determination of melamine with isotope internal standard in dairy products by gas chromatography/mass spectrometry (GC/MS) without derivatization. A 30 m of DB-5ms ((5%-phenyl)-methylpolysiloxane, 0.25 mm i.d., 0.25 {mu}m df) coupled with a 1.5 m of Innowax (polyethylene glycol, 0.32 mm i.d., 0.25 {mu}m df) by a quartz capillary column connector was introduced as separation column. Three advantages were discussed for the coupled system. The sample was fortified with a ring-labeled {sup 13}C{sub 3}{sup 15}N{sub 3}-melamine as an isotope internal standard and extracted by 1% of trichloroacetic acid aqueous solution. 2.2% of lead acetate solution was then added to deposit protein in the sample matrix. After purification by cation exchange cartridge, the sample solution was directly injected and detected by GC/MS. A six-point calibration curve ranging from 0.05 to 2 mg kg{sup -1} of melamine in sample was used to establish instrument response. The recovery was 93.9-102% with relative standard deviation from 3.1 to 8.7% when isotope internal standard used. The calculated method detection limit was 0.01 mg kg{sup -1}.

  13. A Chemical Detector for Gas Chromatography Using Pulsed Discharge Emission Spectroscopy on a Microchip

    Science.gov (United States)

    Luo, X.; Zhu, W.; Mitra, B.; Liu, J.; Liu, T.; Fan, X.; Gianchandani, Y.

    2011-12-01

    There is increasing interest in miniaturized systems for chemical analysis in harsh environments. Chemical detection by emission spectroscopy of on-chip microdischarges [1-3] can be performed at >200°C [4], suggesting utility inspace exploration, volcanic monitoring, and oil well monitoring. This abstract describes the first use of pulsed microdischarge spectroscopy for gas chromatography (GC).This effort supports NASA interests in monitoring closed-loop life support systems for spacecraft. The microdischarge occurs on a 1cm2 glass chip (Fig. 1a), with thin-film Ni electrodes separated by 160μm. A glass lid with a grooved gas-flow channel, and inlet/outlet capillary tubes are epoxy-sealed to the chip. Located downstream of the 1.7m-long, RTX-1-coated, GC separation column, the microdischarge chip is read by a spectrometer. In a typical experiment (Fig. 1b), a mixture of acetone 3.6μg, 1-hexanol 2.8μg and nitrobenzene 3.0μg, is injected, with He carrier gas at 1.56sccm, through the GC. Acetone elutes quickly while nitrobenzene is slower. Microdischarges are triggered at 0.5Hz for 6 min., and 0.04Hz thereafter. Each microdischarge consumes ≈8mJ; the average power is ≈1.14mW. The spectrum (Fig. 1b, inset) shows that the 388nm peak, representing CN/CH fragments [5], is enhanced by carbon compounds. Its strength relative to the 588nm peak of He provides a chromatogram. Fig. 1b also shows a benchmark result from a commercial flame ionization detector (FID). The differences in elution time are attributed to differences in the gas flow paths for the two detectors [1]. REFERENCES [1] Eijkel et al, Anal. Chem, 2000 [2] Mitra et al, IEEE Trans Plasma Sci, 2008 [3] Mitra et al, IEEE Sensors, 2008 [4] Wright et al, APL, 2009 [5] Pearse et al, The Identification of Molecular Spectra, 1963

  14. Steroid monochloroacetates : Physical-chemical characteristics and use in gas-liquid chromatography

    NARCIS (Netherlands)

    Molen, H.J. van der; Groen, D.; Maas, J.H. van der

    1965-01-01

    Synthesis and physical-chemical characteristics (melting points, infrared-, visible- and ultraviolet spectra, paper-,thin-layer- and gas-liquid Chromatographie behaviour) of monochloroacetate derivatives of steroids representing the androstane-, pregnane-, estrane- and cholestane series are describe

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

    DEFF Research Database (Denmark)

    Nielsen, Kristian Fog; Thrane, Ulf

    2001-01-01

    The paper presents a fast method for trichothecene profiling and chemotaxonomic studies in species of Fusarium, Stachybotrys, Trichoderma and Memnoniella. Micro scale extracted crude Fusarium extracts were derivatised using pentafluoropropionic anhydride and analysed by gas chromatography...

  16. VACUUM DISTILLATION COUPLED WITH GAS CHROMATOGRAPHY/MASS SPECTROMETRY FOR THE ANALYSIS OF ENVIRONMENTAL SAMPLES

    Science.gov (United States)

    A procedure is presented that uses a vacuum distillation/gas chromatography/mass spectrometry system for analysis of problematic matrices of volatile organic compounds. The procedure compensates for matrix effects and provides both analytical results and confidence intervals from...

  17. Analysis of chemical signals in red fire ants by gas chromatography and pattern recognition techniques

    Science.gov (United States)

    The combination of gas chromatography and pattern recognition (GC/PR) analysis is a powerful tool for investigating complicated biological problems. Clustering, mapping, discriminant development, etc. are necessary to analyze realistically large chromatographic data sets and to seek meaningful relat...

  18. Capillary gas chromatographic analysis of nerve agents using large volume injections. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Deinum, T.; Nieuwenhuy, C.

    1994-11-01

    The procedure developed at TNO-Prins Maurits Laboratory (TNO-PML) for the verification of intact organophosphorus chemical warfare agents in water samples was improved. The last step in this procedure, the laborious and non-reproducible transfer of an ethyl acetate extract onto a Tenax-adsorption tube followed by thermal desorption of the Tenax-tube, was replaced by large volume injection of the extract onto a capillary gas chromatographic system. The parameters controlling the injection of a large volume of an extract (200 ul) were investigated and optimized. As ethyl acetate caused severe problems, potential new solvents were evaluated. With the improved procedure, the nerve agents sarin, tabun, soman, diisopropyl fluorophosphate (DFP) and VX could be determined in freshly prepared water samples at pg/ml (ppt) levels. The fate of the nerve agents under study in water at two pH`s (4.8 and 6) was investigated. For VX, the pH should be adjusted before extraction. Moreover, it is worthwhile to acidify water samples to diminish hydrolysis.

  19. Monolithic silica-based capillary reversed-phase liquid chromatography/electrospray mass spectrometry for plant metabolomics

    NARCIS (Netherlands)

    Tolstikov, V.V.; Lommen, A.; Nakanishi, K.; Tanaka, N.; Fiehn, O.

    2003-01-01

    Application of C18 monolithic silica capillary columns in HPLC coupled to ion trap mass spectrometry detection was studied for probing the metabolome of the model plant Arabidopsis thaliana. It could be shown that the use of a long capillary column is an easy and effective approach to reduce ionizat

  20. [Development of methods for determining acrylamide in food products by gas-liquid chromatography].

    Science.gov (United States)

    Bessonov, V V; Malinkin, A D; Perederiaev, O I; Bogachuk, M N; Volkovich, S V; Medvedev, Iu V

    2011-01-01

    The method of determination of acrylamide in various food (milk powder, potato chips, instant coffee) by gas-liquid chromatography after pre-bromination was developed. Studies have shown the possibility of using bromination of acrylamide to give it the necessary properties for better extraction, purification and detection. Also revealed the possibility of qualitative and quantitative determine a acrylamide in food by gas-liquid chromatography with detection by electron capture detector.

  1. [Determination of residual organic solvents in flunixin meglumine raw material by headspace gas chromatography].

    Science.gov (United States)

    Hu, Huilian

    2012-01-01

    A method for the determination of five kinds of residual organic solvents in flunixin meglumine raw material was developed by headspace gas chromatography. An HP-FFAP capillary column (30 m x 0.32 mm x 1.0 microm), a flame ionization detector and the external standard method were used for the separation and quantitative analysis. The effects of equilibrium temperature and equilibrium time on the determination of residual organic solvents were investigated. The good results were obtained in the equilibrium temperature of 90 degrees C and equilibrium time of 30 min. The standard curves were linear in the range of 0.40-7.93 mg/L (r = 0.999 8) for ethyl acetate, 7.32-146.48 mg/L (r = 0.999 6) for methanol, 4.53-90.61 mg/L (r = 0.999 9) for isopropanol, 3.62-72.32 mg/L (r = 0.999 8) for ethanol and 2.31-46.24 mg/L (r = 0.999 6) for acetonitrile. The recoveries for the five residual organic solvents were between 95.96% and 100.31% with relative standard deviations (RSDs) (n = 6) of 1.97%-3.28%. The detection limits of ethyl acetate, methanol, isopropanol, ethanol and acetonitrile were 0.08, 0.9, 0.2, 0.4 and 0.3 mg/L, respectively. The proposed method was successfully applied to analyze the residual organic solvents in the real sample of flunixin meglumine raw material. The results showed that only isopropanol and ethanol were found in the sample with the contents of 177.44 microg/g and 69.32 microg/g, respectively. The method is rapid, sensitive and accurate for the content determination of residual solvents in flunixin meglumine raw material.

  2. ICSH recommendations for assessing automated high-performance liquid chromatography and capillary electrophoresis equipment for the quantitation of HbA2.

    Science.gov (United States)

    Stephens, A D; Colah, R; Fucharoen, S; Hoyer, J; Keren, D; McFarlane, A; Perrett, D; Wild, B J

    2015-10-01

    Automated high performance liquid chromatography and Capillary electrophoresis are used to quantitate the proportion of Hemoglobin A2 (HbA2 ) in blood samples order to enable screening and diagnosis of carriers of β-thalassemia. Since there is only a very small difference in HbA2 levels between people who are carriers and people who are not carriers such analyses need to be both precise and accurate. This paper examines the different parameters of such equipment and discusses how they should be assessed.

  3. HPLC separation and GC-MS identification of the polar components of coal liquids. [High pressure liquid chromatography, gas chromatography-mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Satoh, M.; Tanabe, K.; Uchino, H.; Yokoyama, S.; Sanada, Y.

    1984-01-01

    The polar components in the 200-400 C fraction of Akabira coal liquids were separated by high pressure liquid chromatography using an amine-based column. By varying the CHCl/sub 3/ concentration in the solvent, basic, neutral and acid fractions were obtained. These were then investigated separately using infrared spectroscopy, flame ionization detection-gas chromatography and gas chromatography-mass spectroscopy. The basic fraction contained alkyltetrahydroquinolines, the neutral fraction, alkylphenols and alkylcarbazoles; and the acid fraction, alkylphenols. 15 references.

  4. Fast filtration sampling protocol for mammalian suspension cells tailored for phosphometabolome profiling by capillary ion chromatography - tandem mass spectrometry.

    Science.gov (United States)

    Kvitvang, Hans F N; Bruheim, Per

    2015-08-15

    Capillary ion chromatography (capIC) is the premium separation technology for low molecular phosphometabolites and nucleotides in biological extracts. Removal of excessive amounts of salt during sample preparation stages is a prerequisite to enable high quality capIC separation in combination with reproducible and sensitive MS detection. Existing sampling protocols for mammalian cells used for GC-MS and LC-MS metabolic profiling can therefore not be directly applied to capIC separations. Here, the development of a fast filtration sampling protocol for mammalian suspension cells tailored for quantitative profiling of the phosphometabolome on capIC-MS/MS is presented. The whole procedure from sampling the culture to transfer of filter to quenching and extraction solution takes less than 10s. To prevent leakage it is critical that a low vacuum pressure is applied, and satisfactorily reproducibility was only obtained by usage of a vacuum pressure controlling device. A vacuum of 60mbar was optimal for filtration of multiple myeloma Jjn-3 cell cultures through 5μm polyvinylidene (PVDF) filters. A quick deionized water (DI-water) rinse step prior to extraction was tested, and significantly higher metabolite yields were obtained during capIC-MS/MS analyses in this extract compared to extracts prepared by saline and reduced saline (25%) washing steps only. In addition, chromatographic performance was dramatically improved. Thus, it was verified that a quick DI-water rinse is tolerated by the cells and can be included as the final stage during filtration. Over 30 metabolites were quantitated in JJN-3 cell extracts by using the optimized sampling protocol with subsequent capIC-MS/MS analysis, and up to 2 million cells can be used in a single filtration step for the chosen filter and vacuum pressure. The technical set-up is also highly advantageous for microbial metabolome filtration protocols after optimization of vacuum pressure and washing solutions, and the reduced salt

  5. Determination of lysergic acid diethylamide (LSD) in mouse blood by capillary electrophoresis/ fluorescence spectroscopy with sweeping techniques in micellar electrokinetic chromatography.

    Science.gov (United States)

    Fang, Ching; Liu, Ju-Tsung; Chou, Shiu-Huey; Lin, Cheng-Huang

    2003-03-01

    The separation and on-line concentration of lysergic acid diethylamide (LSD) in mouse blood was achieved by means of capillary electrophoresis/fluorescence spectroscopy using sodium dodecyl sulfate (SDS) as the surfactant. Techniques involving on-line sample concentration, including sweeping micellar electrokinetic chromatography (sweeping-MEKC) and cation-selective exhaustive injection-sweep-micellar electrokinetic chromatography (CSEI-sweep-MEKC) were applied; the optimum on-line concentration and separation conditions were determined. In the analysis of an actual sample, LSD was found in a blood sample from a test mouse (0.1 mg LSD fed to a 20 g mouse; approximately 1/10 to the value of LD(50)). As a result, 120 and 30 ng/mL of LSD was detected at 20 and 60 min, respectively, after ingestion of the doses.

  6. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    Science.gov (United States)

    Miller, C. J.; Elias, G.; Schmitt, N. C.; Rae, C.

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify trace levels of the military explosives, RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol and filtered using no additional sample cleanup of the sample extract prior to analysis. The filtered methanol extracts were injected directly into several different column types and analyzed by high performance liquid chromatography using ultraviolet detection and/or gas chromatography using electron capture detection. This paper describes general screening methods that were used to determine the presence of explosives (RDX, TNT, and PETN) in unknown samples of denim, colored flannel, vinyl and canvas in addition to techniques that have been optimized for quantification of each explosive from the substrate extracts.

  7. Analysis of pesticide residues in tobacco with online size exclusion chromatography with gas chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Guo, Weiyun; Bian, Zhaoyang; Tang, Gangling; Wang, Deguo; Li, Guanghui; Wang, Jianlong

    2016-07-01

    An ultrasensitive method for the simultaneous analysis of pesticides residues in tobacco was developed with online size exclusion chromatography with gas chromatography and tandem mass spectrometry. Tobacco samples were extracted with the solvent mixture of cyclohexane and acetone (7:3, v/v) and centrifuged. Then, the supernatant liquors were injected directly into the online size exclusion chromatography with gas chromatography and tandem mass spectrometry without any other purification procedures after being filtered with a 0.22 μm organic phase filter. The matrix interferences were effectively removed and recoveries of most pesticides were in the range of 72-121%. Especially, for chlorothalonil, the analysis efficiency of this method was much more favorable than that of the general method, in which dispersive solid-phase extraction was used as an additional purified procedure. In addition, the limits of quantitation of this method were from 1 to 50 μg/kg. Therefore, a rapid, cost-effective, labor-saving method was proposed in the present work, which was suitable for the analysis of 41 pesticide residues in tobacco.

  8. Isotope Fractionation in Methane Reactions Studied by Gas Chromatography and Liquid Scintillation

    DEFF Research Database (Denmark)

    Andersen, Bertel Lohmann; Bidoglio, G.; Leip, A.

    1997-01-01

    Determination of C-14-marked methane by gas chromatography and liquid scintillation counting is shown to be useful in studies of isotope effects. Data on the specific activity is used to separate the contributions of (CH4)-C-14, and (CH4)-C-12 to the gas-chromatographic peak area. As an application...

  9. Capillary gas chromatographic analysis of alditol acetates of neutral and amino sugars in bacterial cell walls.

    Science.gov (United States)

    Fox, A; Morgan, S L; Hudson, J R; Zhu, Z T; Lau, P Y

    1983-02-18

    Several improvements in the preparation of alditol acetates of neutral and amino sugars and in the preparation of glass capillary columns for their separation are described. Modifications in sample preparation permitted the simultaneous processing of multiple samples and eliminated extraneous background peaks. Efficient and inert columns were tailor-made for the separation of alditol acetates of neutral and amino sugars by leaching glass capillaries with aqueous hydrochloric acid and dynamically coating with SP-2330.

  10. Investigation of Pinus mugo essential oil oxygenated fraction by combined use of gas chromatography and dry column chromatography.

    Science.gov (United States)

    A, M B; Coran, S A; Giannellini, V; Vincieri, F F; Moneti, G

    1981-09-01

    The oxygenated compounds of Pinus mugo Turra essential oil were investigated by a combination of GC and dry column chromatography (DCC) coordinated by GC data processing. The collected data resulted in a bar graph ("normalized" gas chromatogram) giving the RRT's and relative amounts of 68 components; 38 of them were identified by MS and IR. The described procedure may be used for essential oil analysis in general.

  11. Quantitative analysis of trace-level benzene, toluene, ethylbenzene, and xylene in cellulose acetate tow using headspace heart-cutting multidimensional gas chromatography with mass spectrometry.

    Science.gov (United States)

    Ji, Xiaorong; Zhang, Jing; Guo, Yinlong

    2016-06-01

    This study describes a method for the quantification of trace-level benzene, toluene, ethylbenzene, and xylene in cellulose acetate tow by heart-cutting multidimensional gas chromatography with mass spectrometry in selected ion monitoring mode. As the major volatile component in cellulose acetate tow samples, acetone would be overloaded when attempting to perform a high-resolution separation to analyze trace benzene, toluene, ethylbenzene, and xylene. With heart-cutting technology, a larger volume injection was achieved and acetone was easily cut off by employing a capillary column with inner diameter of 0.32 mm in the primary gas chromatography. Only benzene, toluene, ethylbenzene, and xylene were directed to the secondary column to result in an effective separation. The matrix interference was minimized and the peak shapes were greatly improved. Finally, quantitative analysis of benzene, toluene, ethylbenzene, and xylene was performed using an isotopically labeled internal standard. The headspace multidimensional gas chromatography mass spectrometry system was proved to be a powerful tool for analyzing trace volatile organic compounds in complex samples.

  12. Determination of anions using monolithic capillary column ion chromatography with end-to-end differential contactless conductometric detectors under resonance approach.

    Science.gov (United States)

    Zhang, Zhenli; Li, Dongdong; Liu, Xueyong; Subhani, Qamar; Zhu, Yan; Kang, Qi; Shen, Dazhong

    2012-06-21

    An end-to-end differential measurement approach with capacitively coupled contactless conductivity detection (C(4)D) was applied to anion-exchange monolithic capillary column ion chromatography. The column was prepared by thermally initiated radical polymerization of poly(glycidyl methacrylate) in a fused-silica capillary of 320 μm i.d. and modified by quaternary ammonium latex surface coating. Two C(4)Ds were placed near both ends of the capillary column and the output difference between them was measured. With 15 mM potassium hydrogen phthalate used as the eluent, good separation of a mixture of inorganic anions (F(-), Cl(-), NO(2)(-), NO(3)(-)) was achieved. The detection limits of conventional C(4)D are 1.6, 0.28, 0.53, and 0.47 mg L(-1) for F(-), Cl(-), NO(2)(-), and NO(3)(-), respectively. To further enhance the sensitivity, the capacitive impedance from C(4)D was neutralized by an inductive impedance from a piezoelectric resonator. An increase in sensitivity by a factor of 7-8 was achieved in the resonating C(4)D in comparison with the conventional C(4)D. The detection limits of the resonating C(4)D are 0.23, 0.041, 0.065, and 0.059 mg L(-1) for F(-), Cl(-), NO(2)(-), and NO(3)(-), respectively. The response of the resonating C(4)D was analyzed based on an equivalent circuit model.

  13. Recent advances in capillary scale ion chromatography technology%毛细管离子色谱分析系统研究进展

    Institute of Scientific and Technical Information of China (English)

    杨丙成; 刁雪芳

    2012-01-01

    Ion chromatography (IC) has been a well-established technique for the analysis of ionic samples. The aqueous solution used for IC eluent is well suited for bioanalysis in relative to common liquid chromatography. This is especially true for capillary ion chromatography (CIC) due to its advantage of small sample needed. CIC is generally divided into three categories including open tubular, packed and monolithic. In this review, the recent progress of CIC is summarized based on the development of several key components associated with packed column-based system. The development of open tubular ion chromatography is also reviewed.%离子色谱是目前分析离子型样品的成熟技术,其水相工作介质的特点相对于液相色谱更适合于生物样品的分析.毛细管离子色谱(CIC)由于其节省样品的特点在生物分析方面的优势更为明显.CIC大体上可分为开管型、填充柱型和整体柱型3种类型.本文以填充型CIC几大关键部件技术发展为主线,综述了近年来CIC的研究进展.

  14. Determination of n-alkanes contamination in soil samples by micro gas chromatography functionalized by multi-walled carbon nanotubes.

    Science.gov (United States)

    Li, Yubo; Zhang, Runzhou; Wang, Tao; Wang, Yonghuan; Xu, Tianbai; Li, Lingfeng; Zhao, Weijun; Dong, Shurong; Wang, Xiaozhi; Luo, Jikui

    2016-09-01

    A new method for separation of 11 n-alkanes: octane, o-nonane, n-decane, n-undecane, n-dodecane, n-tridecane, n-tetradecane, n-pentdecne, n-hexadecath, heptadecane, n-octadecane in soil samples was developed. Kuderna-Danish (K.D.) concentrator enrichment prior to ultrasonic extraction and the silicone chromatography column purification and with gas chromatography flame ionization detection (GC-FID) could be used for n-alkanes determination. The micro channels of open tubular column were fabricated onto a silicon wafer to replace the quartz capillary chromatographic column. The column structure and analysis parameters that affected the column separation were investigated and optimized. Under optimal conditions, the extract reagent was centrifuged and collected. A silicone chromatography column and a K.D. concentrator were used for further clean-up and enrichment. Using this method, the limits of detection (LOD) and limits of quantification (LOQ) were obtained in the range of 0.03-0.15 and 0.1-0.5 mg kg(-1) in soil samples, respectively. The relative standard deviation (RSD) was under 12%. The optimized procedure that presented good analytical performance (with recoveries ranging from 56.5% to 89.2%), was successfully applied to determine n-alkane content in farmland soil samples adjacent to a highway. The results showed that the MWCNTs-functionalized column is capable of separating the alkane contaminations with high resolution in about 3 min, which is much shorter than that of GC-MS and other conventional analytical methods, demonstrating its great potential for rapid analysis.

  15. Measurement of abscisic acid and gibberellins by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Okamoto, Masanori; Hanada, Atsushi; Kamiya, Yuji; Yamaguchi, Shinjiro; Nambara, Eiji

    2009-01-01

    Gas chromatography-mass spectrometry (GC-MS)-based analysis is an accurate and sensitive method to quantify plant hormones. This method is commonly used for analysis of low-molecular-weight compounds, such as abscisic acid (ABA), gibberellins (GAs), auxins, and brassinosteroids. Procedures are composed of four major steps: extraction, fractionation, derivatization, and detection. Here, we describe a protocol for quantification of ABA and GAs.

  16. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Greyce Kelly Steinhorst Alcantara

    2016-01-01

    Full Text Available Levetiracetam (LEV is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time, the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.

  17. Comprehensive two-dimensional gas chromatography coupled with fast sulphur-chemiluminescence detection: implications of detector electronics.

    Science.gov (United States)

    Blomberg, Jan; Riemersma, Toby; van Zuijlen, Manfred; Chaabani, Hassan

    2004-09-24

    Within the petrochemical industry, there has been a growing interest in methods capable of providing detailed information on the distribution of sulphur-containing compounds in various product streams, going down to the level of separating and quantifying individual sulphur species. Since no single capillary gas chromatographic column is able to perform this separation, a refuge to multi-dimensional separation techniques has to be taken. In this respect, comprehensive two-dimensional gas chromatography (GC x GC) coupled with sulphur chemiluminescence detection (SCD) has shown to be highly promising. It has been suggested, however, that the detector volume of an SCD restricts its potential to keep up with the fast second-dimension separations of contemporary GC x GC. In this paper, we will demonstrate that the lack of speed of the SCD does not originate from its physical dimensions, but is largely determined by the speed of the electronics used. Additionally, some typical examples will be presented to illustrate the potential of GC x GC coupled with fast SCD.

  18. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    2016-01-01

    Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient's plasma sample using less than 550 μL of organic solvent. PMID:27830105

  19. Direct comparison of capillary electrophoresis and capillary liquid chromatography hyphenated to collision-cell inductively coupled plasma mass spectrometry for the investigation of Cd-, Cu- and Zn-containing metalloproteins.

    Science.gov (United States)

    Montes-Bayon, Maria; Pröfrock, Daniel; Sanz-Medel, Alfredo; Prange, Andreas

    2006-05-05

    Capillary liquid chromatography (cLC) and capillary electrophoresis (CE) have been critically compared for the separation of metalloproteins when using collision-cell inductively coupled plasma mass spectrometry (ICP-CC-MS) as detection system. For cLC separation, the selected column was a C8 (0.3 mm I.D.) and the separation conditions involved a gradient up to 80% methanol in 10mM ammonium acetate buffer (pH 7.4). The low flow rate used (3 microL min(-1)) permitted the utilization of a high methanol content maintaining the sensitivity along the whole chromatographic run. For this purpose, a new low-flow interface has been developed based on a total consumption nebulizer. Similarly, CE has been studied as separation technique using a 75 microm I.D. fused silica capillary and a running buffer of 20 mM Tris-HNO3 (pH 7.4) and working at 30 kV. Metallothionein (mixture of MT-I and -II) and superoxide dismutase (SOD) have been used as protein models in order to evaluate the separation/detection capabilities using the same injection volumes in both systems (20 nL). For both hybrid systems, separation parameters such as retention factor, numbers of theoretical plates, tailing factor and resolution have been critically compared. Also, the analytical performance characteristics of both hybrid systems have been evaluated and tested by analyzing the Cu-, Zn-species present in red blood cell extracts in order to explore more adequate separation methodology for the analysis of metalloproteins in complex matrices.

  20. DETERMINATION OF ACRYLAMIDE IN FOOD BY GAS AND LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

    OpenAIRE

    Michaela Vieriková; Miriam Vlčáková

    2010-01-01

     Acrylamide in food was determined by gas chromatography - mass spectrometry (GC-MS) after bromination of acrylamide and underivatized acrylamide was quantified by ultra performance liquid chromatography -mass spectrometry (UPLC-MS). Two different sample preparation methods were used and optimised. The GC-MS method was used for various food matrices like breads, potato crisps, potato crackers, french fries. The UPLC-MS method was used for analysis of coffee. The limit of detect...

  1. Adsorption and displacement effects in the gas-chromatography of metal beta-diketonates.

    Science.gov (United States)

    Uden, P C; Jenkins, C R

    1969-07-01

    A detailed study of the gas chromatography of the aluminium(III), chromium(III) and iron(III) beta-diketonates has shown that their elution and separation characteristics arise from a number of adsorptive effects. Conditions of optimal peak shape for individual compounds are established by varying Chromatographie parameters, and the adsorption of one metal chelate on a column and its subsequent displacement by another chelate are investigated. The chromatography of iron(III) beta-diketonates is seen to be further complicated by gradual elution of a portion of the chelate before the rest of the sample.

  2. Sol-gel germania triblock polymer coatings of exceptional pH stability in capillary microextraction online-coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Triplett, Judy; Malik, Abdul

    2010-05-15

    For the first time, a germania-based sol-gel coating was used in capillary microextraction (CME) in combination with high-performance liquid chromatography (HPLC). A hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), was covalently bonded into a sol-gel germania matrix in the course of its creation from an alkoxide precursor via hydrolytic polycondensation reactions. A thin layer of this in situ-created sol-gel hybrid material was covalently anchored to the inner walls of a 0.25 mm i.d. fused silica capillary to produce a sol-gel germania triblock polymeric sorbent in the form of a highly stable surface coating. Such a coating served as an effective extracting phase for the preconcentration of a wide range of polar and nonpolar analytes (e.g., alcohols, amines, ketones, phenols, and polycyclic aromatic hydrocarbons) with nanomolar and picomolar detection limits. Most significantly, the sol-gel germania triblock polymer coating demonstrated impressive resistance to extreme pH conditions, surviving 5 days of continuous exposure to 1.0 M HCl (pH approximately 0.0) or 1.0 M NaOH (pH approximately 14.0), practically without any changes in performance. This shows the suitability of sol-gel germania hybrid organic-inorganic hybrid materials for use as sorbents or stationary phases under extreme pH conditions, often needed in a variety of separation and sample preparation techniques and applications, including ion chromatography, hydrophobic interaction chromatography, proteomics, HPLC with electrochemical detection, isoelectric focusing, and extraction of acidic and basic analytes.

  3. Characterization of aroma-active compounds in three Chinese Moutai liquors by gas chromatography-olfactometry, gas chromatography-mass spectrometry and sensory evaluation.

    Science.gov (United States)

    Niu, Yunwei; Chen, Xiaomei; Xiao, Zuobing; Ma, Ning; Zhu, Jiancai

    2017-04-01

    The aroma-active compounds in three Chinese Moutai liquors, aged 1 year, 15 years and 30 years were investigated in this study. The aroma compounds were analysed by gas chromatography-olfactometry (GC-O) coupled with gas chromatography-mass spectrometry (GC-MS). A total of 79 aroma compounds were identified. Aroma extract dilution analysis (AEDA) was further employed to identify the aroma-active compounds. A total of 35 aroma-active compounds with flavour dilution (FD) values ≧ 64 simultaneously in three Chinese Moutai liquors were quantitated. Among them, ethyl acetate, ethyl lactate and acetic acid appeared with the highest concentrations. They were all >1000 mg/L. Then, the relationships between the aroma-active compounds and seven sensory attributes were studied.

  4. Prediction of capillary gas chromatographic retention times of fatty acid methyl esters in human blood using MLR, PLS and back-propagation artificial neural networks.

    Science.gov (United States)

    Gupta, Vinod Kumar; Khani, Hadi; Ahmadi-Roudi, Behzad; Mirakhorli, Shima; Fereyduni, Ehsan; Agarwal, Shilpi

    2011-01-15

    Quantitative structure-retention relationship (QSRR) models correlating the retention times of fatty acid methyl esters in high resolution capillary gas chromatography and their structures were developed based on non-linear and linear modeling methods. Genetic algorithm (GA) was used for the selection of the variables that resulted in the best-fitted models. Gravitational index (G2), number of cis double bond (NcDB) and number of trans double bond (NtDB) were selected among a large number of descriptors. The selected descriptors were considered as inputs for artificial neural networks (ANNs) with three different weights update functions including Levenberg-Marquardt backpropagation network (LM-ANN), BFGS (Broyden, Fletcher, Goldfarb, and Shanno) quasi-Newton backpropagation (BFG-ANN) and conjugate gradient backpropagation with Polak-Ribiére updates (CGP-ANN). Computational result indicates that the LM-ANN method has better predictive power than the other methods. The model was also tested successfully for external validation criteria. Standard error for the training set using LM-ANN was SE=0.932 with correlation coefficient R=0.996. For the prediction and validation sets, standard error was SE=0.645 and SE=0.445 and correlation coefficient was R=0.999 and R=0.999, respectively. The accuracy of 3-2-1 LM-ANN model was illustrated using leave multiple out-cross validations (LMO-CVs) and Y-randomization.

  5. Identification of Explosives from Porous Materials: Applications Using Reverse Phase High Performance Liquid Chromatography and Gas Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    C.J. Miller; G. Elias; N.C. Schmitt; C. Rae

    2010-06-01

    High performance liquid chromatography and gas chromatography techniques are well documented and widely used for the detection of trace explosives from organic solvents. These techniques were modified to specifically identify and quantify explosives extracted from various materials taken from people who had recently handled explosives. Documented techniques were modified to specifically detect and quantify RDX, TNT, and PETN from denim, colored flannel, vinyl, and canvas extracted in methanol using no sample cleanup prior to analysis. The methanol extracts were injected directly into several different column types and analyzed by HPLC-UV and/or GC-ECD. This paper describes general screening methods that were used to determine the presence of explosives in unknown samples and techniques that have been optimized for quantification of each explosive from the substrate extracts.

  6. Analyzing salvia divinorum and its active ingredient salvinorin a utilizing thin layer chromatography and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Jermain, John D; Evans, Hiram K

    2009-05-01

    In recent years, Salvia divinorum has become a major focus by state legislatures throughout the United States looking to prohibit the sale of the psychoactive plant. After researching testing procedures presented in the literature and those employed by crime laboratories throughout the country, it was decided that thin layer chromatography (TLC) and gas chromatography/mass spectrometry (GC/MS) were the methods to use to analyze plant material for salvinorin A. With TLC, salvinorin A was detected from extracted plant material and was easily distinguishable from 13 other Salvia species as well as Cannabis sativa L. (marijuana). When using GC/MS, salvinorin A was best extracted from plant material with chloroform at ambient temperature when using a nonpolar solvent and acetone at ambient temperature when using a polar solvent. By utilizing these techniques, criminalists are now able to confirm the presence of salvinorin A in a submitted plant material suspected to be Salvia divinorum.

  7. Separation performance of guanidinium-based ionic liquids as stationary phases for gas chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Lu, Kai; Qi, Meiling; Fu, Ruonong

    2013-02-08

    Room temperature ionic liquids (RTILs) as stationary phases for gas chromatography (GC) have made great achievements in both research and applications over the last decades. Until now, all of the RTIL stationary phases reported have involved imidazolium, ammonium, pyrrolidinium, and phosphonium-based RTILs, and however, no publications are available using guanidinium-based ionic liquids (GBILs) as GC stationary phases except two preliminary reports from our group. In the present work, three hexaalkyl GBILs stationary phases, namely N, N,N',N'-tetramethyl-N″, N″-dioctylguanidinum hexafluophosphate (DOTMG-PF(6)), N,N,N',N'-tetramethyl-N″, N″-dioctylguanidinium bis (trifluoromethylsulfonyl) imide (DOTMG-NTf(2)), and N,N,N',N'-tetraoctyl-N″, N″-dimethylguanidinium bis (trifluoromethylsulfonyl) imide (TODMG-NTf(2)), were synthesized and used as stationary phases for GC separation after they were statically coated onto the inner walls of fused-silica capillary columns. The evaluation of DOTMG-PF(6) and TODMG-NTf(2) as GC stationary phases is reported here for the first time, whereas additional results on the DOTMG-NTf(2) stationary phase are added here on the basis of our previous report. In this work, McReynolds constants and Abraham solvation system constants are used to evaluate the average polarity and the solvation properties of the GBILs stationary phases for GC separation, respectively. The results show that the GBILs stationary phases exhibit medium polarity with an average polarity of 293-390, and that the major molecular interactions of the GBILs with analytes are dipole/polarizable interactions, H-bond basicity and dispersion forces, etc. After this, the separation performance and thermal stability of the GBILs stationary phases were evaluated, showing that these stationary phases achieve excellent separation for analytes of great variety covering hydrocarbons, alcohols, esters, aldehydes, ketones, amines, amides and aromatics, and exhibit

  8. Pyrolysis-Gas Chromatography/Mass Spectrometry of Thermoplastic Polymers

    Science.gov (United States)

    1988-04-01

    was operated in the splitless mode. Nitrogen was used as a makeup gas in the FID. The makeup gas was required since the GC was designed for use with... nitrogen and sulfur are present in the polymer, oxides of sulfur and nitrogen will also be formed. In most instances, the conditions required for the...chronic or irreversible tissue damage, or narcosis of sufficient degree to increase the likelihood of accidental injury or reduce work efficiency. 4.0

  9. Evaluation of three gas chromatography and two direct mass spectrometry techniques for aroma analysis of dried red bell peppers

    NARCIS (Netherlands)

    Ruth, van S.M.; Boscaini, E.; Mayr, D.; Pugh, J.; Posthumus, M.A.

    2003-01-01

    Three gas chromatography methods and two direct mass spectrometry techniques were compared for the analysis of the aroma of rehydrated diced red bell peppers. Gas chromatography methods included systems with olfactometry detection (GC-O), flame ionisation detection (GC-FID) and mass spectrometry (GC

  10. Highly sensitive assay for the measurement of serotonin in microdialysates using capillary high-performance liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Parrot, Sandrine; Lambás-Señas, Laura; Sentenac, Sabine; Denoroy, Luc; Renaud, Bernard

    2007-05-01

    A highly sensitive isocratic capillary high-performance liquid chromatographic (HPLC) method with electrochemical detection (ED) for the simultaneous measurement of serotonin (5-hydroxytryptamine, 5-HT) and its metabolite 5-hydroxyindole-3-acetic acid (5-HIAA) in microdialysates has been developed using a 0.5 mm i.d. capillary column and a 11-nL detection cell. This method, validated on both pharmacological and analytical bases, can be performed using injection volumes as low as 1 microL. The limits of detection were 5.6 x 10(-11)mol/L and 3.0 x 10(-9)mol/L for 5-HT and 5-HIAA. Several applications of the present method are given on microdialysates from rodent brain and human spinal cord.

  11. Analysis of phenolic compounds in Spanish Albrariño and Portuguese Alvarinho and Loureiro wines by capillary zone electrophoresis and high-performance liquid chromatography.

    Science.gov (United States)

    Andrade, P B; Oliveira, B M; Seabra, R M; Ferreira, M A; Ferreres, F; García-Viguera, C

    2001-05-01

    The concentration of different phenolic compounds was measured in Spanish Albariño and Portuguese Alvarinho and Loureiro white wines by capillary zone electrophoresis (CZE), in order to characterize them. Although all samples presented the same qualitative pattern (characterized by tyrosol; (-)-epicatechin; syringic acid; ferulic acid; p-coumaric acid; caffeic acid, gallic acid; 3,4-dihydroxybenzoic acid; cis-coumaroyl tartaric acid (COUTA); trans-COUTA; trans-caffeoyl tartaric acid (CAFTA), and hydroxycinnamic esters), some quantitative differences were observed. When samples were analyzed by high-performance liquid chromatography (HPLC), in order to compare the results obtained by both techniques, no significant qualitative or quantitative differences were obtained. Nevertheless, CZE proved to be a more convenient technique for the routinary analyses of these wines, due to better separation of the different compounds, better peak shapes, and higher speed than HPLC.

  12. Characterization of fruit products by capillary zone electrophoresis and liquid chromatography using the compositional profiles of polyphenols: application to authentication of natural extracts.

    Science.gov (United States)

    Navarro, Meritxell; Núñez, Oscar; Saurina, Javier; Hernández-Cassou, Santiago; Puignou, Lluis

    2014-02-01

    Capillary zone electrophoresis (CZE) and high performance liquid chromatography (HPLC) were applied to the authentication of fruit products based on the compositional profiles of polyphenols. Various sample treatments were used to maximize the overall recovery of polyphenols or specific fractions, such as phenolic acids or anthocyanins. The resulting CZE and HPLC data were treated with Principal Component Analysis (PCA) showing that samples were mainly clustered according to the fruit of origin, with cranberry- and grape-based products clearly separated in groups. A possible adulterated cranberry extract was analyzed more deeply by high resolution mass spectrometry (HRMS) in order to identify the presence of A-type proanthocyanidins, which are characteristic and more abundant in cranberry-based products. In accordance with PCA interpretation, HRMS results indicated that the suspicious sample was not a cranberry-based product, allowing us to validate and demonstrate the suitability of both CZE- and HPLC-proposed methods for the characterization of fruit-based products.

  13. Simultaneous determination of gaseous and particulate carbonyls in air by coupling micellar electrokinetic capillary chromatography with molecular imprinting solid-phase extraction.

    Science.gov (United States)

    Sun, Hui; Lai, Jia-Ping; Fung, Ying Sing

    2014-09-05

    A novel method coupling molecular imprinting solid-phase extraction (MISPE) and micellar electrokinetic capillary chromatography (MEKC) was developed to enable the hourly determination of low level of ambient carbonyls, and study their partition between gaseous phase and particulate phase. With 2,4-dinitroaniline (DNAN) as dummy imprinting template, the unreacted 2,4-Dinitrophenylhydrazine (DNPH) in sampling solution could be removed effectively using MISPE, and an average recovery of 97±5.3% (n=5) for the carbonyl-DNPH derivatives was achieved. Owing to the high enrichment due to sample clean-up, and the improvement of MEKC separation efficiency, many low abundant carbonyls could be detected by hourly in the field study.

  14. Preparation and evaluation of packed capillary columns for the separation of nucleic acids by ion-pair reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Oberacher, H; Krajete, A; Parson, W; Huber, C G

    2000-09-29

    Oligonucleotides and double stranded DNA fragments were separated in 200 microm I.D. capillary columns packed with micropellicular, octadecylated, 2.1 microm poly(styrene-divinylbenzene) particles by ion-pair reversed-phase high-performance liquid chromatography (IP-RP-HPLC). Both the length and the diameter of the connecting capillaries (150 x 0.020 mm I.D.) as well as the detection volume (3 nl) had to be kept to a minimum in order to maintain the high efficiency of this chromatographic separation system with peak widths at half height in the range of a few seconds. Three different types of frits, namely sintered silica particles, sintered octadecylsilica particles, and monolithic poly(styrene-divinylbenzene) (PS-DVB) frits were evaluated with respect to their influence on chromatographic performance. Best performance for the separation of oligonucleotides and long DNA fragments was observed with the PS-DVB frits, whereas the short DNA fragments were optimally resolved in columns terminated by octadecylsilica frits. The maximum loading capacity of 60 x 0.20 mm I.D. columns ranged from 20 fmol (7.7 ng) for a 587 base pair DNA fragment to 500 fmol (2.4 ng) for a 16-mer oligonucleotide. Lower mass- and concentration detection limits in the low femtomol and low nanomol per liter range, respectively, make capillary IP-RP-HPLC with UV absorbance detection highly attractive for the separation and characterization of minute amounts of synthetic oligonucleotides, DNA restriction fragments, and short tandem repeat sequences amplified by polymerase chain reaction.

  15. Simultaneous determination of bromate, chlorite and haloacetic acids by two-dimensional matrix elimination ion chromatography with coupled conventional and capillary columns.

    Science.gov (United States)

    Teh, Hui Boon; Li, Sam Fong Yau

    2015-02-27

    A new, highly sensitive and reliable two-dimensional matrix elimination ion chromatography (IC) method was developed for simultaneous detection of bromate, chlorite and five haloacetic acids. This method combined the conventional IC in first dimension with capillary IC in the second dimension coupled with suppressed conductivity detection. The first dimension utilizes a high capacity column to partially resolve matrix from target analytes. By optimizing the cut window, the target analytes were selectively cut and trapped in a trap column through the use of a six-port valve, while the separated matrix were diverted to waste. The trapped target analytes were delivered on to the capillary column for further separation and detection. Temperature programming was used to improve selectivity in second dimension column to obtain complete resolution of the target analytes. Compared to the performance of one-dimensional IC, the two-dimensional approach resulted in a significant increase in sensitivity for all target analytes with limit of detection ranging from 0.30 to 0.64μg/L and provided more reliable analysis due to second column confirmation. Good linearity was obtained for all the target analytes with correlation coefficients >0.998. The proposed method was successfully applied to the determination of oxyhalides and haloacetic acids in various matrices with recoveries ranging from 90 to 116% and RSD less than 6.1%. The method allows direct injection of samples and the use of columns with different selectivity, thus significantly reduces the level of false positive results. The method is fully automated and simple, making it practical for routine monitoring of water quality. The satisfactory results also demonstrated that the two-dimensional matrix elimination method coupled with capillary IC is a promising approach for detection of trace substances in complex matrices.

  16. Hyphenated and comprehensive liquid chromatography × gas chromatography-mass spectrometry for the identification of Mycobacterium tuberculosis.

    Science.gov (United States)

    Mourão, Marta P B; Denekamp, Ilse; Kuijper, Sjoukje; Kolk, Arend H J; Janssen, Hans-Gerd

    2016-03-25

    Tuberculosis is one of the world's most emerging public health problems, particularly in developing countries. Chromatography based methods have been used to tackle this epidemic by focusing on biomarker detection. Unfortunately, interferences from lipids in the sputum matrix, particularly cholesterol, adversely affect the identification and detection of the marker compounds. The present contribution describes the serial combination of normal phase liquid chromatography (NPLC) with thermally assisted hydrolysis and methylation followed by gas chromatography-mass spectrometry (THM-GC-MS) to overcome the difficulties of biomarker evaluation. The in-series combination consists of an LC analysis where fractions are collected and then transferred to the THM-GC-MS system. This was either done with comprehensive coupling, transferring all the fractions, or with hyphenated interfacing, i.e. off-line multi heart-cutting, transferring only selected fractions. Owing to the high sensitivity and selectivity of LC as a sample pre-treatment method, and to the high specificity of the MS as a detector, this analytical approach, NPLC × THM-GC-MS, is extremely sensitive. The results obtained indicate that this analytical set-up is able to detect down to 1 × 10(3) mycobacteria/mL of Mycobacterium tuberculosis strain 124, spiked in blank sputum samples. It is a powerful analytical tool and also has great potential for full automation. If further studies demonstrate its usefulness when applied blind in real sputum specimens, this technique could compete with the current smear microscopy in the early diagnosis of tuberculosis.

  17. Comparative study of multi walled carbon nanotubes-based electrodes in micellar media and their application to micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Chicharro, Manuel; Arribas, Alberto Sánchez; Moreno, Mónica; Bermejo, Esperanza; Zapardiel, Antonio

    2007-12-15

    This work reports on a comparative study of the electrochemical performance of carbon nanotubes-based electrodes in micellar media and their application for amperometric detection in micellar electrokinetic capillary chromatography (MEKC) separations. These electrodes were prepared in two different ways: immobilization of a layer of carbon nanotubes dispersed in polyethylenimine (PEI), ethanol or Nafion onto glassy carbon electrodes or preparation of paste electrodes using mineral oil as binder. Scanning electron microscopy (SEM) was employed for surface morphology characterization while cyclic voltammetry of background electrolyte was used for capacitance estimation. The amperometric responses to hydrogen peroxide, amitrol, diuron and 2,3-dichlorophenol (2,3CP) in the presence and in the absence of sodium dodecylsulphate (SDS) were studied by flow injection analysis (FIA), demonstrating that the electrocatalytic activity, background current and electroanalytical performance were strongly dependent on the electrodes preparation procedure. Glassy carbon electrodes modified with carbon nanotubes dispersed in PEI (GC/(CNT/PEI)) displayed the most adequate performance in micellar media, maintaining good electrocatalytic properties combined with acceptable background currents and resistance to passivation. The advantages of using GC/(CNT/PEI) as detectors in capillary electrophoresis were illustrated for the MEKC separations of phenolic pollutants (phenol, 3-chlorophenol, 2,3-dichlorophenol and 4-nitrophenol) and herbicides (amitrol, asulam, diuron, fenuron, monuron and chlortoluron).

  18. Monolithic metal-organic framework MIL-53(Al)-polymethacrylate composite column for the reversed-phase capillary liquid chromatography separation of small aromatics.

    Science.gov (United States)

    Yusuf, Kareem; Badjah-Hadj-Ahmed, Ahmed Yacine; Aqel, Ahmad; ALOthman, Zeid Abdullah

    2016-03-01

    A monolithic capillary column containing a composite of metal-organic framework MIL-53(Al) incorporated into hexyl methacrylate-co-ethylene dimethacrylate was prepared to enhance the separation of mixtures of small aromatic compounds by using capillary liquid chromatography. The addition of 10 mg/mL MIL-53(Al) microparticles increased the micropore content in the monolithic matrix and increased the Brunauer-Emmett-Teller surface area from 26.92 to 85.12 m(2) /g. The presence of 1,4-benzenedicarboxylate moieties within the structure of MIL-53(Al) as an organic linker greatly influenced the separation of aromatic mixtures through π-π interactions. High-resolution separation was obtained for a series of alkylbenzenes (with resolution factors in the range 0.96-1.75) in less than 8 min, with 14 710 plates/m efficiency for propylbenzene, using a binary polar mobile phase of water/acetonitrile in isocratic mode. A reversed-phase separation mechanism was indicated by the increased retention factor and resolution as the water percentage in the mobile phase increased. A stability study on the composite column showed excellent mechanical stability under various conditions. The higher resolution and faster separation observed at increased temperature indicated an exothermic separation, whereas the negative values for the free energy change of transfer indicated a spontaneous process.

  19. Evaluation of the combination of micellar electrokinetic capillary chromatography with sweeping and cation selective exhaustive injection for the determination of 5-nitroimidazoles in egg samples.

    Science.gov (United States)

    Airado-Rodríguez, Diego; Hernández-Mesa, Maykel; García-Campaña, Ana M; Cruces-Blanco, Carmen

    2016-12-15

    A methodology is presented for the sensitive determination of nitromidazole residues in egg by means of micellar electrokinetic capillary chromatography in combination with cation selective exhaustive injection and ultraviolet detection. Six compounds have been considered and the separation has been achieved in less than 12min in a 61.5-cm effective length capillary with 50-μm internal diameter. Phosphate buffer 44mM pH 2.5, containing 8% tetrahydrofurane and 123mM sodium dodecyl sulfate was employed as running buffer. Solid phase extraction has been employed for sample clean-up. The methodology has been successfully validated in hen eggs, obtaining method detection limits in the range of 2.1-5.0ng/g. Precision was studied in terms of repeatability and intermediate precision, with relative standard deviations lower than 18.0%. Recoveries were calculated in quail eggs and a commercial pasteurized egg white product, reaching over 70% for most of the considered 5-nitroimidazoles.

  20. Evaluation of the oxidative deoxyribonucleic acid damage biomarker 8-hydroxy-2'-deoxyguanosine in the urine of leukemic children by micellar electrokinetic capillary chromatography.

    Science.gov (United States)

    Zhang, Pingping; Lian, Kaoqi; Wu, Xiaoli; Yao, Min; Lu, Xin; Kang, Weijun; Jiang, Lingling

    2014-04-04

    Determining the level of urinary 8-hydroxy-2'-deoxyguanosine (8-OHdG), an oxidative DNA damage biomarker, is vital to the study of clinical pathogenesis and drug toxicity. The principal limitation of capillary electrophoresis (CE) with UV detection is its low sensitivity. To overcome this shortcoming, we developed a micellar electrokinetic capillary chromatography (MEKC) with solid-phase extraction (SPE) for urinary 8-OHdG analysis. The sensitivity of MEKC-UV was improved using a reasonable UV system, injection mode, and SPE. The parameters affecting MEKC and SPE were also optimized. The calibration curve was linear within the range from 1 to 500 μg L(-1). The limits of detection and quantification were 0.27 μg L(-1) and 0.82 μg L(-1), respectively. Interday and intraday precision were both <5.6%. The recovery of 8-OHdG in urine ranged from 94.5% to 103.2%. This method was used to measure urinary 8-OHdG from eight normal children, eight newly diagnosed leukemic children, and eight leukemic children undergoing chemotherapy. The results show that the proposed method can be used to assess oxidative stress in patients and the side effects of chemotherapeutic drugs by measuring urinary 8-OHdG.

  1. High-resolution gas chromatography/mass spectrometry method for characterization and quantitative analysis of ginkgolic acids in Ginkgo biloba plants, extracts, and dietary supplements.

    Science.gov (United States)

    Wang, Mei; Zhao, Jianping; Avula, Bharathi; Wang, Yan-Hong; Avonto, Cristina; Chittiboyina, Amar G; Wylie, Philip L; Parcher, Jon F; Khan, Ikhlas A

    2014-12-17

    A high-resolution gas chromatography/mass spectrometry (GC/MS) with selected ion monitor method focusing on the characterization and quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba L. plant materials, extracts, and commercial products was developed and validated. The method involved sample extraction with (1:1) methanol and 10% formic acid, liquid-liquid extraction with n-hexane, and derivatization with trimethylsulfonium hydroxide (TMSH). Separation of two saturated (C13:0 and C15:0) and six unsaturated ginkgolic acid methyl esters with different positional double bonds (C15:1 Δ8 and Δ10, C17:1 Δ8, Δ10, and Δ12, and C17:2) was achieved on a very polar (88% cyanopropyl) aryl-polysiloxane HP-88 capillary GC column. The double bond positions in the GAs were determined by ozonolysis. The developed GC/MS method was validated according to ICH guidelines, and the quantitation results were verified by comparison with a standard high-performance liquid chromatography method. Nineteen G. biloba authenticated and commercial plant samples and 21 dietary supplements purported to contain G. biloba leaf extracts were analyzed. Finally, the presence of the marker compounds, terpene trilactones and flavonol glycosides for Ginkgo biloba in the dietary supplements was determined by UHPLC/MS and used to confirm the presence of G. biloba leaf extracts in all of the botanical dietary supplements.

  2. Comprehensive two-dimensional gas chromatography for the analysis of organohalogenated micro-contaminants

    NARCIS (Netherlands)

    Korytar, P.; Haglund, P.; Boer, de J.; Brinkman, U.A.Th.

    2006-01-01

    We explain the principles of comprehensive two-dimensional gas chromatography (GC × GC), and discuss key instrumental aspects - with emphasis on column combinations and mass spectrometric detection. As the main item of interest, we review the potential of GC × GC for the analysis of organohalogenate

  3. The Separation and Identification of Straight Chain Hydrocarbons: An Experiment Using Gas-Liquid Chromatography.

    Science.gov (United States)

    Benson, G. A.

    1982-01-01

    An experiment using gas-liquid chromatography is discussed, introducing the student to concept of dead volume and its measurement, idea and use of an internal reference compound, and to linear relationship existing between measurements of a separation on two different stationary phases. (Author/SK)

  4. Gas chromatography-mass spectrometric assay for propofol in cerebrospinal fluid of traumatic brain patients

    NARCIS (Netherlands)

    Peeters, Mariska Y. M.; Kuiper, Hiltjo; Greijdanus, Ben; van der Naalt, Joukje; Knibbe, Catherijne A. J.; Uges, Donald R. A.

    2007-01-01

    A sensitive gas chromatography-mass spectrometry method for measuring propofol in cerebrospinal fluid is described, validated and applied to four patients after traumatic brain injury. The limit of quantitation was 2 mu g/L using a volume of 0.5 mL. The inter- and intra-assay coefficients of variati

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

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

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

  6. Quantitative analysis of target components by comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Mispelaar, V.G. van; Tas, A.C.; Smilde, A.K.; Schoenmakers, P.J.; Asten, A.C. van

    2003-01-01

    Quantitative analysis using comprehensive two-dimensional (2D) gas chromatography (GC) is still rarely reported. This is largely due to a lack of suitable software. The objective of the present study is to generate quantitative results from a large GC x GC data set, consisting of 32 chromatograms. I

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

    Science.gov (United States)

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

    2013-01-01

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

  8. Planar gas chromatography column on aluminum plate with multi-walled carbon nanotubes as stationary phase

    Science.gov (United States)

    Platonov, I. A.; Platonov, V. I.; Pavelyev, V. S.

    2016-04-01

    The high selectivity of the adsorption layer for low-boiling alkanes is shown, the separation factor (α) couple iso-butane / butane is 1.9 at a column temperature of 50 °C.The paper presents sorption and selective properties of planar gas chromatography column on aluminum plate with multi-walled carbon nanotubes as the stationary phase.

  9. Chiral gas chromatography for the determination of 1,2-O-isopropylidene-sn-glycerol stereoisomers

    NARCIS (Netherlands)

    Dröge, M.J; Bos, R.; Woerdenbag, H.J.; Quax, Wim; Droge, MJ

    2003-01-01

    A stereospecific gas chromatography (GC) method using a (6-O-tButyldimethylsilyl-2,3-di-O-methyl)-beta-cyclodextrin as the chiral stationary phase has been developed and validated for the determination of the enantiomers of 1,2-O-isopropylidene-sn-glycerol (IPG), an important chiral synthon, in kine

  10. Impurity profiling of trinitrotoluene using vacuum-outlet gas chromatography-mass spectrometry

    NARCIS (Netherlands)

    Brust, H.; Willemse, S.; Zeng, T.; Asten, A. van; Koeberg, M.; Heijden, A.E.D.M. van der; Bolck, A.; Schoenmakers, P.

    2014-01-01

    In this work, a reliable and robust vacuum-outlet gas chromatography-mass spectrometry (GC-MS) method is introduced for the identification and quantification of impurities in trinitrotoluene (TNT). Vacuum-outlet GC-MS allows for short analysis times the analysis of impurities in TNT was performed in

  11. Composition of carbonaceous smoke particles from prescribed burning of a Canadian boreal forest: 1. Organic aerosol characterization by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Mazurek, M.A.; Laterza, C.; Newman, L.; Daum, P. [Brookhaven National Lab., Upton, NY (United States); Cofer, W.R. III; Levine, J.S. [National Aeronautics and Space Administration, Hampton, VA (United States). Langley Research Center; Winstead, E.L. [Science Applications International Corporation, Hampton, VA (United States)

    1995-06-01

    In this study we examine the molecular organic constituents (C8 to C40 lipid compounds) collected as smoke particles from a Canadian boreal forest prescribed burn. Of special interest are (1) the molecular identity of polar organic aerosols, and (2) the amount of polar organic matter relative to the total mass of aerosol particulate carbon. Organic extracts of smoke aerosol particles show complex distributions of the lipid compounds when analyzed by capillary gas chromatography/mass spectrometry. The molecular constituents present as smoke aerosol are grouped into non-polar (hydrocarbons) and polar {minus}2 oxygen atoms) subtractions. The dominant chemical species found in the boreal forest smoke aerosol are unaltered resin compounds (C20 terpenes) which are abundant in unburned conifer wood, plus thermally altered wood lignins and other polar aromatic hydrocarbons. Our results show that smoke aerosols contain molecular tracers which are related to the biofuel consumed. These smoke tracers can be related structurally back to the consumed softwood and hardwood vegetation. In addition, combustion of boreal forest materials produces smoke aerosol particles that are both oxygen-rich and chemically complex, yielding a carbonaceous aerosol matrix that is enriched in polar substances. As a consequence, emissions of carbonaceous smoke particles from large-scale combustion of boreal forest land may have a disproportionate effect on regional atmospheric chemistry and on cloud microphysical processes.

  12. Comprehensive two-dimensional gas chromatography in combination with rapid scanning quadrupole mass spectrometry in perfume analysis.

    Science.gov (United States)

    Mondello, Luigi; Casillia, Alessandro; Tranchida, Peter Quinto; Dugo, Giovanni; Dugo, Paola

    2005-03-01

    Single column gas chromatography (GC) in combination with a flame ionization detector (FID) and/or a mass spectrometer is routinely employed in the determination of perfume profiles. The latter are to be considered medium to highly complex matrices and, as such, can only be partially separated even on long capillaries. Inevitably, several monodimensional peaks are the result of two or more overlapping components, often hindering reliable identification and quantitation. The present investigation is based on the use of a comprehensive GC (GC x GC) method, in vacuum outlet conditions, for the near to complete resolution of a complex perfume sample. A rapid scanning quadrupole mass spectrometry (qMS) system, employed for the assignment of GC x GC peaks, supplied high quality mass spectra. The validity of the three-dimensional (3D) GC x GC-qMS application was measured and compared to that of GC-qMS analysis on the same matrix. Peak identification, in all applications, was achieved through MS spectra library matching and the interactive use of linear retention indices (LRI).

  13. Atmospheric Pressure Chemical Ionization Gas Chromatography Mass Spectrometry for the Analysis of Selected Emerging Brominated Flame Retardants in Foods

    Science.gov (United States)

    Lv, Surong; Niu, Yumin; Zhang, Jing; Shao, Bing; Du, Zhenxia

    2017-03-01

    Emerging brominated flame retardants (eBFRs) other than polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs) and their derivatives in foods have been in focus in recent years due to their increasing production volumes, indefinite information on toxicities and the lack of data on occurrence in environments, foods as well as humans. In this study, gas chromatography was coupled to an atmospheric pressure chemical ionization-tandem mass spectrometry (APGC-MS/MS) for the analysis of six eBFRs in pork, chicken, egg, milk and fish. A short section of unpacked capillary column coupled to the end of the analytical column was applied to improve the chromatographic behaviors of high boiling point compounds. The method was comprehensively validated with method limit of quantification (mLOQ) lower than 8 pg/g wet weight (w.w.). Samples from Chinese Total Diet study were quantified following the validated APGC-MS/MS method. 2,3,4,5-pentabromo-6-ethylbenzene (PBEB), hexabromobenzene (HBB), pentabromotoluene (PBT) and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) were most frequently detected in samples. The highest concentration was found in fish with 351.9 pg/g w.w. of PBT. This is the first report on the presence of PBT in food samples with non-ignorable concentrations and detection rate.

  14. Detection and quantification of cocoa butter equivalents in cocoa butter and plain chocolate by gas liquid chromatography of triacylglycerols.

    Science.gov (United States)

    Buchgraber, Manuela; Senaldi, Chiara; Ulberth, Franz; Anklam, Elke

    2004-01-01

    The development and in-house testing of a method for the detection and quantification of cocoa butter equivalents in cocoa butter and plain chocolate is described. A database consisting of the triacylglycerol profile of 74 genuine cocoa butter and 75 cocoa butter equivalent samples obtained by high-resolution capillary gas liquid chromatography was created, using a certified cocoa butter reference material (IRMM-801) for calibration purposes. Based on these data, a large number of cocoa butter/cocoa butter equivalent mixtures were arithmetically simulated. By subjecting the data set to various statistical tools, reliable models for both detection (univariate regression model) and quantification (multivariate model) were elaborated. Validation data sets consisting of a large number of samples (n = 4050 for detection, n = 1050 for quantification) were used to test the models. Excluding pure illipé fat samples from the data set, the detection limit was determined between 1 and 3% foreign fat in cocoa butter. Recalculated for a chocolate with a fat content of 30%, these figures are equal to 0.3-0.9% cocoa butter equivalent. For quantification, the average error for prediction was estimated to be 1.1% cocoa butter equivalent in cocoa butter, without prior knowledge of the materials used in the blend corresponding to 0.3% in chocolate (fat content 30%). The advantage of the approach is that by using IRMM-801 for calibration, the established mathematical decision rules can be transferred to every testing laboratory.

  15. Quantitation of volatile oils in ground cumin by supercritical fluid extraction and gas chromatography with flame ionization detection.

    Science.gov (United States)

    Heikes, D L; Scott, B; Gorzovalitis, N A

    2001-01-01

    Ground cumin is used as a flavoring agent in a number of ethnic cuisines. The chemical entities, which primarily establish its characteristically pungent flavor, are found in the volatile oil of cumin. Fixed oils and carbohydrates tend to round out the harshness of the volatile oil components. However, the quantity of volatile oil is commonly the measure of the quality of this spice. For several decades, the spice industry has used a classical distillation procedure for the determination of volatile oil in cumin and other spices. However, the method is cumbersome and requires nearly 8 h to complete. Supercritical fluid extraction with capillary gas chromatography-flame ionization detection is utilized in the formulation of a rapid, accurate, and specific method for the determination of volatile oil in ground cumin. Samples are extracted in a static-dynamic mode with CO2 at 550 bar and 100 degrees C. Toluene is used as a static modifier addition. The extracted volatile oil, collected in toluene, is analyzed directly using tetradecane as the internal standard. Integration is performed as grouped peaks to include all chemical entities found in cumin volatile oil recovered from the official distillation procedure. Results from this procedure compare favorably with those obtained by the official procedure (coefficient of correlation = 0.995, 24 samples).

  16. Rapid determination of pesticide residues in herbs using selective pressurized liquid extraction and fast gas chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Du, Gang; Xiao, Yao; Yang, Hua-Rong; Wang, Li; Song, Yue-Lin; Wang, Yi-Tao

    2012-08-01

    A selective pressurized liquid extraction and gas chromatography coupled with triple quadrupole mass spectrometer method was developed for simultaneous determination of 52 pesticide residues in medicine and food dual-purpose herbs. The developed extraction method integrated extraction and cleanup processes for sample preparation. The sorbents, 5 g Florisil and 100 mg graphitized carbon black, were placed inside the extraction cell to remove matrix interferences. Optimized conditions of selective pressurized liquid extraction were ethyl acetate as extraction solvent, 120°C of extraction temperature, 6 min of static extraction time, 50% of flush volume extracted for two cycles. An ultra inert capillary GC-MS HP-5 UI column (20 m × 0.18 mm id, 0.18 μm) and column backflush system were used for the analysis. Multiple-reaction monitoring was employed for the quantitative analysis with electron ionization mode. All calibration curves showed good linearity (r(2) > 0.995) within the test ranges. The average recoveries of most pesticides were from 81 to 118%. The validated method was successfully applied for the determination of pesticide residues in four herbs. The results indicate that selective pressurized liquid extraction and GC-MS/MS is a sensitive and reliable analytical method for the simultaneous determination of multiple pesticide residues in herbs.

  17. [Determination of gomisin A (TJN-101) and its metabolite in rat serum by gas chromatography-mass spectrometry].

    Science.gov (United States)

    Matsuzaki, Y; Ishibashi, E; Koguchi, S; Wakui, Y; Takeda, S; Aburada, M; Oyama, T

    1991-10-01

    Gomisin A (TJN-101) is one of the lignan components isolated from Schisandra Fruits. A high sensitive and precise method for the determination of TJN-101 and its major metabolite (Met. B) in the rat serum was developed by selected ion monitoring (SIM) with gas chromatography-mass spectrometry (GC/MS) using a fused silica capillary column (SPB-1, Supelco). A 100 microliter serum sample was used for the solid phase extraction. The calibration curves of TJN-101 and Met.B both showed a good linearity between 2.0 and 2000.0 ng/ml. The analytical precision (intra-assay, C.V. less than 4.7%), recoveries (98.4 +/- 10.1%), and detection limit (2 ng/ml) of TJN-101 indicated that this system was suited for the determination of TJN-101 in biological fluid. In case of Met.B, the same results as TJN-101, were obtained. After oral administration of TJN-101 at a dose of 10 mg/kg to male rats, the average values of the maximal serum concentration of TJN-101 and Met.B were 1446.1 +/- 131.8 and 317.4 +/- 18.5 ng/ml, respectively. The serum concentrations of these substances could be monitored sufficiently for 8 h after dosing.

  18. Role of capillary electrophoresis in the fight against doping in sports.

    Science.gov (United States)

    Harrison, Christopher R

    2013-08-06

    At present the role of capillary electrophoresis in the detection of doping agents in athletes is, for the most part, nonexistent. More traditional techniques, namely gas and liquid chromatography with mass spectrometric detection, remain the gold standard of antidoping tests. This Feature will investigate the in-roads that capillary electrophoresis has made, the limitations that the technique suffers from, and where the technique may grow into being a key tool for antidoping analysis.

  19. High-temperature solvent stability of sol-gel germania triblock polymer coatings in capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Malik, Abdul

    2010-09-10

    Germania-based sol-gel organic-inorganic hybrid coatings were prepared for on-line coupling of capillary microextraction with high-performance liquid chromatography. For this, a germania-based sol-gel precursor, tetra-n-butoxygermane and a hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide) were used. These sol-gel germania triblock polymer coatings were chemically anchored to the inner walls of a fused silica capillary (0.25 mm I.D.) in course of its evolution from the sol solution. Scanning electron microscopy images of the sol-gel germania triblock polymer coating were obtained to estimate the coating thickness. For the first time, the analyte distribution constants between a sol-gel germania organic-inorganic hybrid coating and the samples (K(cs)) were determined. For a variety of analytes from different chemical classes, including polycyclic aromatic hydrocarbons (PAHs), ketones, alcohols, phenols and amines, the K(cs) values ranged from 8.1 x 10(1) to 5.6 x 10(4). Also, for the first time, the stability of the sol-gel germania-based coating in high-temperature reversed-phase solvent environment was evaluated. The sol-gel germania triblock polymer coatings were capable of surviving exposure to high-temperature solvent conditions (200 degrees C) with little change in extraction capabilities. This demonstrates that sol-gel germania triblock polymer hybrid materials might be suitable for further applications in high-temperature HPLC. The reproducibility of the method for preparation of the sol-gel germania triblock polymer coatings was also evaluated, and the capillary-to-capillary RSD values ranged from 5.3 to 6.5%. The use of higher flow rates in extraction was found to significantly reduce the time required (from 30-40 to 10-15 min) to reach equilibrium between the sol-gel germania triblock polymer coating and the analytes in the sample solution.

  20. Polymethacrylate monolithic and hybrid particle-monolithic columns for reversed-phase and hydrophilic interaction capillary liquid chromatography.

    Science.gov (United States)

    Jandera, Pavel; Urban, Jirí; Skeríková, Veronika; Langmaier, Pavel; Kubícková, Romana; Planeta, Josef

    2010-01-01

    We prepared hybrid particle-monolithic polymethacrylate columns for micro-HPLC by in situ polymerization in fused silica capillaries pre-packed with 3-5microm C(18) and aminopropyl silica bonded particles, using polymerization mixtures based on laurylmethacrylate-ethylene dimethacrylate (co)polymers for the reversed-phase (RP) mode and [2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl) zwitterionic (co)polymers for the hydrophilic interaction (HILIC) mode. The hybrid particle-monolithic columns showed reduced porosity and hold-up volumes, approximately 2-2.5 times lower in comparison to the pure monolithic columns prepared in the whole volume of empty capillaries. The elution volumes of sample compounds are also generally lower in comparison to packed or pure monolithic columns. The efficiency and permeability of the hybrid columns are intermediate in between the properties of the reference pure monolithic and particle-packed columns. The chemistries of the embedded solid particles and of the interparticle monolithic moiety in the hybrid capillary columns contribute to the retention to various degrees, affecting the selectivity of separation. Some hybrid columns provided improved separations of proteins in comparison to the reference particle-packed columns in the reversed-phase mode. Zwitterionic hybrid particle-monolithic columns show dual mode retention HILIC/RP behaviour depending on the composition of the mobile phase and allow separations of polar compounds such as phenolic acids in the HILIC mode at lower concentrations of acetonitrile and, often in shorter analysis time in comparison to particle-packed and full-volume monolithic columns.

  1. Metal-Organic Framework Thin Films as Stationary Phases in Microfabricated Gas-Chromatography Columns.

    Energy Technology Data Exchange (ETDEWEB)

    Read, Douglas [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sillerud, Colin Halliday [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-01-01

    The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

  2. Determination of iron, copper and aluminium by gas-liquid chromatography.

    Science.gov (United States)

    Moshier, R W; Schwarberg, J E

    1966-03-01

    Gas chromatography has been utilised in the analysis of two National Bureau of Standard alloys for quantitative determination of aluminium, iron and copper. In the analysis of N.B.S. 162a the relative mean errors were 3.13% for aluminium, 2.06% for iron and -1.72% for copper and for N.B.S. 164a the relative mean errors were -1.39%, -0.19% and -0.89% for aluminium, iron and copper, respectively. The procedure for analysis involves solution of the alloy, conversion of the metal ions to trifluoroacetylacetonates by solvent extraction and, finally, complete separation of the metal chelates and quantitative determination by gas chromatography using a column containing Gas Pack F coated with Tissuemat E, a polyethylene wax. Other metals present in the N.B.S. samples did not interfere with the determination of aluminium, iron and copper.

  3. Development of gas chromatography analysis of fatty acids in marine organisms.

    Science.gov (United States)

    Tang, Baokun; Row, Kyung Ho

    2013-08-01

    The gas chromatographic analysis of fatty acids has attracted considerable interest. In this analysis, the common derivatives of fatty acids, such as fatty acid methyl esters, can be detected using a flame ionization detector and the mass spectra can indicate the true structure of fatty acids. This paper reviews gas chromatographic methods for obtaining fatty acids from marine organisms. The stationary phase and detector for applications in gas chromatography are discussed. This article also reviews the components of fatty acids in marine animals, marine plants and marine microorganisms.

  4. Partition coefficients of organic compounds in new imidazolium based ionic liquids using inverse gas chromatography.

    Science.gov (United States)

    Revelli, Anne-Laure; Mutelet, Fabrice; Jaubert, Jean-Noël

    2009-06-05

    Partition coefficients of organic compounds in four ionic liquids: 1-ethanol-3-methylimidazolium tetrafluoroborate, 1-ethanol-3-methylimidazolium hexafluorophosphate, 1,3-dimethylimidazolium dimethylphosphate and 1-ethyl-3-methylimidazolium diethylphosphate were measured using inverse gas chromatography from 303.3 to 332.55K. The influence of gas-liquid and gas-solid interfacial adsorption of different solutes on ionic liquids was also studied. Most of the polar solutes were retained largely by partition while light hydrocarbons were retained predominantly by interfacial adsorption on the ionic liquids studied in this work. The solvation characteristics of the ionic liquids were evaluated using the Abraham solvation parameter model.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2001-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Kenneth Paul Roberts

    2002-06-27

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

  7. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

  8. Identification of intact long-chain p-hydroxycinnamate esters in leaf fibers of abaca (Musa textilis) using gas chromatography/mass spectrometry.

    Science.gov (United States)

    del Río, José C; Rodríguez, Isabel M; Gutiérrez, Ana

    2004-01-01

    The study of acetone-extractable components from the leaf fibers of the non-wood plant abaca (Musa textilis) resulted in the isolation and identification of series of intact hydroxycinnamate esters consisting of ferulic and p-coumaric acids esterified to long-chain fatty alcohols (C20 to C28) and omega-hydroxyfatty acids (C22 to C28). These series of compounds were characterized by high-temperature gas chromatography/mass spectrometry (GC/MS) using capillary columns (12 m length) with thin films that allowed the analysis of intact (i.e., without prior saponification) hydroxycinnamate esters. Characterization of intact individual compounds was achieved based on the mass spectra obtained by GC/MS of the underivatized compounds and their methyl and/or trimethylsilyl ether derivatives.

  9. Estado da arte da cromatografia gasosa de alta resolução e alta temperatura State of the art of high temperature high resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    Alberto dos Santos Pereira

    2000-06-01

    Full Text Available The developments in stationary phase synthesis and capillary column technology, have opened new perspectives in analysis of high molecular mass compounds (³600 daltons and thermolabile organic compounds by High Temperature High Resolution Gas Chromatography (HT-HRGC. HT-HRGC is a new analytical borderline and its application to the analysis of high molecular mass compounds is still in its infancy. The apolar and medium polar gum phases can now be operated at temperatures up to 400-480ºC, being used for the analysis of n-alcanes up to C-100, lipids, oligosaccharides, industrial resins, polyglycerols, cyclodextrins, porphyrins, etc. This technique should play a leading role as a powerful tool, for many different analysis types, in multidisciplinary fields of Science.

  10. Determination of musty odorants, 2-methylisoborneol and geosmin, in environmental water by headspace solid-phase microextraction and gas chromatography--mass spectrometry.

    Science.gov (United States)

    Saito, Keita; Okamura, Kota; Kataoka, Hiroyuki

    2008-04-01

    A simple and sensitive method for the determination of musty odorants, 2-methylisoborneol (MIB) and geosmin (GSM), in environmental water was developed by headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry. MIB and GSM were separated within 10 min using a DB-1 capillary column and detected in the selective ion monitoring mode. HS-SPME using a polydimethylsiloxane/divinylbenzene fiber provided effective sample enrichment, and was carried out by fiber exposition at 70 degrees C for 30 min. Using this method, the calibration curves of MIB and GSM were linear in the range of 0-500 pg/mL, with a correlation coefficient above 0.9977 (n=24). The detection limits (S/N=3) of MIB and GSM were 0.9 and 0.6 pg/mL, respectively. This method was successfully applied to the analysis of environmental water samples without interference peaks.

  11. Determination of methyl tert-butyl ether (MTBE) in Chinese fuels by gas chromatography/mass spectrometry and gas chromatography/flame ionization detector

    Institute of Scientific and Technical Information of China (English)

    LIU Jie-min; CHENG Wei; WEN Mei-juan; JIANG Gui-bin

    2004-01-01

    A method was developed to determine the concentration of methyl tert-butyl ether(MTBE) in gasoline,diesel and heating oil by gas chromatography(GC) with mass spectrometry(GC-MS) or flame ionization detection (FID). The diluted gasoline was directly injected into the GC, and the complete separation of MTBE from co-eluting hydrocarbons was not required. GC/MS or GC/FID method can be used to analyze MTBE in different concentration range and have good consistency.

  12. Enantioseparation of ofloxacin in urine by capillary electrokinetic chromatography using charged cyclodextrins as chiral selectors and assessment of enantioconversion

    NARCIS (Netherlands)

    Mol, R; de Zeeuw, R.A; de Jong, G.J.; Ensing, K

    2001-01-01

    A method was developed for the enantioseparation of ofloxacin, a member of the fluoroquinolones, using an anionic cyclodextrin-derivative with or without combination with a neutral cyclodextrin-derivative, as the chiral selector (s) in an electrokinetic chromatography system. The best results were o

  13. Gas and high-performance liquid chromatography of phenols

    Energy Technology Data Exchange (ETDEWEB)

    Tesarova, E.; Pacakova, V.

    1983-05-01

    Gas (GC) and high-performance liquid chromatographic (HPLC) methods in the analysis of phenols are reviewed. Among the great number of phenolic compounds analyzed, alkylphenols, chlorophenols, dihydroxy-and trihydroxy-benzenes and biphenols are chiefly considered. The advantages and drawbacks of the methods are discussed. Relationships between the structural characteristics of phenols, the stationary phase structure, the mobile phase composition and the retention data are treated. Typical examples of the conditions for GC and HPLC analysis are summarized in tables. 276 references

  14. Determination of free fatty acids and triglycerides by gas chromatography using selective esterification reactions.

    Science.gov (United States)

    Kail, Brian W; Link, Dirk D; Morreale, Bryan D

    2012-01-01

    A method for selectively determining both free fatty acids (FFA) and triacylglycerides (TAGs) in biological oils was investigated and optimized using gas chromatography after esterification of the target species to their corresponding fatty acid methyl esters (FAMEs). The method used acid catalyzed esterification in methanolic solutions under conditions of varying severity to achieve complete conversion of more reactive FFAs while preserving the concentration of TAGs. Complete conversion of both free acids and glycerides to corresponding FAMEs was found to require more rigorous reaction conditions involving heating to 120°C for up to 2 h. Method validation was provided using gas chromatography-flame ionization detection, gas chromatography-mass spectrometry, and liquid chromatography-mass spectrometry. The method improves on existing methods because it allows the total esterified lipid to be broken down by FAMEs contributed by FFA compared to FAMEs from both FFA and TAGs. Single and mixed-component solutions of pure fatty acids and triglycerides, as well as a sesame oil sample to simulate a complex biological oil, were used to optimize the methodologies. Key parameters that were investigated included: HCl-to-oil ratio, temperature and reaction time. Pure free fatty acids were found to esterify under reasonably mild conditions (10 min at 50°C with a 2.1:1 HCl to fatty acid ratio) with 97.6 ± 2.3% recovery as FAMEs, while triglycerides were largely unaffected under these reaction conditions. The optimized protocol demonstrated that it is possible to use esterification reactions to selectively determine the free acid content, total lipid content, and hence, glyceride content in biological oils. This protocol also allows gas chromatography analysis of FAMEs as a more ideal analyte than glyceride species in their native state.

  15. Direct analysis of fluoxetine and norfluoxetine in plasma by gas chromatography with nitrogen-phosphorus detection.

    Science.gov (United States)

    Fontanille, P; Jourdil, N; Villier, C; Bessard, G

    1997-05-09

    A quantitative method for the simultaneous GC resolution and detection of fluoxetine and his metabolite norfluoxetine in human plasma was developed. The procedure required 1.0 ml of plasma, extraction with a mixed organic solvent and injection into a capillary gas chromatograph with an OV-1 fused-silica column coupled to a nitrogen-phosphorus detector. The calibration curves were linear over the range 5-3000 ng/ml. The detection limits were 0.3 and 2 ng/ml for fluoxetine and norfluoxetine, respectively. The assay is suitable for routine analysis.

  16. Determination of phenoxy acid herbicides in water by electron-capture and microcoulometric gas chromatography

    Science.gov (United States)

    Goerlitz, D.F.; Lamar, William L.

    1967-01-01

    A sensitive gas chromatographic method using microcoulometric titration and electron-capture detection for the analysis of 2,4-D, silvex, 2,4,5-T, and other phenoxy acid herbicides in water is described. The herbicides are extracted from unfiltered water samples (800-1,000 ml) by use of ethyl ether ; then the herbicides are concentrated and esterilied. To allow the analyst a choice, two esterilication procedures--using either boron trifluoride-methanol or diazomethane--are evaluated. Microcoulometric gas chromatography is specific for the detection of halogenated compounds such as the phenoxy acid herbicides whereas it does not respond to nonhalogenated components. Microcoulometric gas chromatography requires care and patience. It is not convenient for rapid screening of l-liter samples that contain less than 1 microgram of the herbicide. Although electroncapture gas chromatography is less selective and more critically affected by interfering substances, it is, nevertheless, convenient and more sensitive than microcoulometric gas chromatography. Two different liquid phases are used in the gas chromatographic columns--DC-200 silicone in one column and QF-1 silicone in the other. The performance of both columns is improved by the addition of Carbowax 20M. The Gas Chrom Q support is coated with the liquid phases by the 'frontal-analysis' technique. The practical lower limits for measurement of the phenoxy acid herbicides in water primarily depend upon the sample size, interferences present, anal instrumentation used. With l-liter samples of water, the practical lower limits of measurement are 10 ppt (parts per trillion) for 2,4-D and 2 ppt for silvex and 2,4,5-T when electron-capture detection is used, and approximately 20 ppt for each herbicide when analyzed by microcoulometric-titration gas chromatography. Recoveries of the herbicides immediately after addition to unfiltered water samples averaged 92 percent for 2,4-D, 90 percent for silvex, and 98 percent for 2

  17. Qualitative Gas Chromatography-Mass Spectrometry Analyses Using Amines as Chemical Ionization Reagent Gases

    Science.gov (United States)

    Little, James L.; Howard, Adam S.

    2013-12-01

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

  18. Characterisation of beeswax in works of art by gas chromatography-mass spectrometry and pyrolysis-gas chromatography-mass spectrometry procedures.

    Science.gov (United States)

    Bonaduce, Ilaria; Colombini, Maria Perla

    2004-03-05

    Pyrolysis (Py) with in situ derivatisation with hexamethyldisilazane-gas chroma-break tography-mass spectrometry (GC-MS) and a gas chromatography-mass spectrometry procedure based on microwave-assisted saponification were used to identify the organic components in small sized beeswax samples. With the latter procedure quantitative recoveries can be made and hydrocarbons, alcohols and omega-1-diols in the neutral fraction, and fatty acids and omega-1-hydroxy acids in the acidic fraction can be efficiently separated and detected. Both procedures were used to characterise a wax anatomic sculpture "The Plague" (1691-1694) by Gaetano Zumbo, resulting in the identification of beeswax and a Pinaceae resin. The GC-MS analysis brought to light some essential differences in beeswax composition between the raw material and the old modelled wax thus giving some clear indications about the recipe used by the sculptor.

  19. Determination of Hydrocarbon Group-Type of Diesel Fuels by Gas Chromatography with Vacuum Ultraviolet Detection.

    Science.gov (United States)

    Weber, Brandon M; Walsh, Phillip; Harynuk, James J

    2016-06-07

    A GC-vacuum ultraviolet (UV) method to perform group-type separations of diesel range fuels was developed. The method relies on an ionic liquid column to separate diesel samples into saturates, mono-, di-, and polyaromatics by gas chromatography, with selective detection via vacuum UV absorption spectroscopy. Vacuum UV detection was necessary to solve a coelution between saturates and monoaromatics. The method was used to measure group-type composition of 10 oilsands-derived Synfuel light diesel samples, 3 Syncrude light gas oils, and 1 quality control sample. The gas chromatography (GC)-vacuum UV results for the Synfuel samples were similar (absolute % error of 0.8) to historical results from the supercritical fluid chromatography (SFC) analysis. For the light gas oils, discrepancies were noted between SFC results and GC-vacuum UV results; however, these samples are known to be challenging to quantify by SFC-flame ionization detector (FID) due to incomplete resolution between the saturate/monoaromatic and/or monoaromatic/diaromatic group types when applied to samples heavier than diesel (i.e., having a larger fraction of higher molecular weight species). The quality control sample also performed well when comparing both methods (absolute % error of 0.2) and the results agreed within error for saturates, mono- and polyaromatics.

  20. Cyclopentadiene evolution during pyrolysis-gas chromatography of PMR polyimides

    Science.gov (United States)

    Alston, William B.; Gluyas, Richard E.; Snyder, William J.

    1992-01-01

    The effect of formulated molecular weight (FMW), extent of cure, and cumulative aging on the amount of cyclopentadiene (CPD) evolved from Polymerization of Monomeric Reactants (PMR) polyimides were investigated by pyrolysis-gas chromotography (PY-GC). The PMR polyimides are additional crosslinked resins formed from an aromatic diamine, a diester of an aromatic tetracarboxylic acid and a monoester of 5-norbornene-2, 3-dicarboxylic acid. The PY-GC results were related to the degree of crosslinking and to the thermo-oxidative stability (weight loss) of PMR polyimides. Thus, PY-GC has shown to be a valid technique for the characterization of PMR polyimide resins and composites via correlation of the CPD evolved versus the thermal history of the PMR sample.

  1. [Quantitative analysis of butachlor, oxadiazon and simetryn by gas chromatography].

    Science.gov (United States)

    Liu, F; Mu, W; Wang, J

    1999-03-01

    The quantitative analysis of the ingredients in 26% B-O-S (butachlor, oxadiazon and simetryn) emulsion by gas chromatographic method was carried out with a 5% SE-30 on Chromosorb AW DMCS, 2 m x 3 mm i.d., glass column at column temperature of 210 degrees C and detector temperature of 230 degrees C. The internal standard is di-n-butyl sebacate. The retentions of simetryn, internal standard, butachlor and oxadiazon were 6.5, 8.3, 9.9 and 11.9 min respectively. This method has a recovery of 98.62%-100.77% and the coefficients of variation of this analysis of butachlor, oxadiazon and simetryn were 0.46%, 0.32% and 0.57% respectively. All coefficients of linear correlation were higher than 0.999.

  2. Analysis of volatile organic compounds in pleural effusions by headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry.

    Science.gov (United States)

    Huang, Zhongping; Zhang, Jie; Zhang, Peipei; Wang, Hong; Pan, Zaifa; Wang, Lili

    2016-07-01

    Headspace solid-phase microextraction coupled with cryotrap gas chromatography and mass spectrometry was applied to the analysis of volatile organic compounds in pleural effusions. The highly volatile organic compounds were separated successfully with high sensitivity by the employment of a cryotrap device, with the construction of a cold column head by freezing a segment of metal capillary with liquid nitrogen. A total of 76 volatile organic compounds were identified in 50 pleural effusion samples (20 malignant effusions and 30 benign effusions). Among them, 34 more volatile organic compounds were detected with the retention time less than 8 min, by comparing with the normal headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry method. Furthermore, 24 volatile organic compounds with high occurrence frequency in pleural effusion samples, 18 of which with the retention time less than 8 min, were selected for the comparative analysis. The results of average peak area comparison and box-plot analysis showed that except for cyclohexanone, 2-ethyl-1-hexanol, and tetramethylbenzene, which have been reported as potential cancer biomarkers, cyclohexanol, dichloromethane, ethyl acetate, n-heptane, ethylbenzene, and xylene also had differential expression between malignant and benign effusions. Therefore, the proposed approach was valuable for the comprehensive characterization of volatile organic compounds in pleural effusions.

  3. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses.

    Science.gov (United States)

    Muthukrishnan, Suriyavathana; Palanisamy, Subha; Subramanian, Senthilkumar; Selvaraj, Sumathi; Mari, Kavitha Rani; Kuppulingam, Ramalingam

    2016-08-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy) tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases.

  4. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    Directory of Open Access Journals (Sweden)

    Suriyavathana Muthukrishnan

    2016-08-01

    Full Text Available Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV were identified by using high-performance liquid chromatography (HPLC and gas chromatography-mass spectroscopy (GC-MS analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases.

  5. Straightforward and rapid determination of sulfadoxine and sulfamethoxazole in capillary blood on sampling paper with liquid chromatography and UV detection.

    Science.gov (United States)

    Lindkvist, J; Malm, M; Bergqvist, Y

    2009-04-01

    A method for the determination of sulfadoxine and sulfamethoxazole in capillary blood on sampling paper has been developed and validated. The method is straightforward with minimal sample preparation, and is suitable for rural settings. Separation of sulfadoxine, sulfamethoxazole and internal standard was performed using a Purospher STAR RP-18 endcapped LC column (150x4.6mm) with a mobile phase consisting of acetonitrile:sodium acetate buffer pH 5.2, I=0.1 (1:2, v/v). For sulfadoxine, the within-day precision was 5.3% at 15micromol/l and 3.7% at 600micromol/l, while for sulfamethoxazole it was 5.7% at 15micromol/l and 3.8% at 600micromol/l. The lower limit of quantification was determined to 5micromol/l and precision was 5.5% and 5.0% for sulfadoxine and sulfamethoxazole, respectively.

  6. Off-odor compounds produced in cork by isolated bacteria and fungi: a gas chromatography-mass spectrometry and gas chromatography-olfactometry study.

    Science.gov (United States)

    Prat, Chantal; Trias, Rosalia; Culleré, Laura; Escudero, Ana; Anticó, Enriqueta; Bañeras, Lluís

    2009-08-26

    The risk of development of specific olfactory profiles in cork was evaluated after inoculation of cork granules and agglomerated and natural cork stoppers with isolated bacteria and fungi. The highest incidence of off-odor development was found in assays when fungi were inoculated. Cork granules with musty-earthy, musty-earthy-TCA, and vegetative deviations were inspected by gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). Sixteen odor zones were clearly recognized in the GC-O analyses. Among these, octanal, 2-methoxy-3,5-dimethylpyrazine (MDMP), Z-2-nonenal, 2-methylisoborneol, 2,4,6-trichloroanisole (TCA), geosmin, and guaiacol were the most significant odorants and helped in the discrimination of sensory deviations. Only TCA and guaiacol were detected above their respective detection limits by HS-SPME-GC-MS. The fungi Cryptococcus sp. isolate F020, Rhodotorula sp. isolate F025, Penicillium glabrum isolate F001, and Pennicillium variabile F003A and the bacterium Pseudomonas jessenii isolate A1 were found to produce TCA to a greater extent. Additionally, 13 of 38 isolated microorganisms (2 bacteria and 11 fungi) proved able to produce unpleasant musty-earthy or vegetative odors that were not related to a significant TCA accumulation.

  7. Elucidation of the aroma compositions of Zhenjiang aromatic vinegar using comprehensive two dimensional gas chromatography coupled to time-of-flight mass spectrometry and gas chromatography-olfactometry.

    Science.gov (United States)

    Zhou, Zhilei; Liu, Shuangping; Kong, Xiangwei; Ji, Zhongwei; Han, Xiao; Wu, Jianfeng; Mao, Jian

    2017-03-03

    In this work, a method to characterize the aroma compounds of Zhenjiang aromatic vinegar (ZAV) was developed using comprehensive two dimensional gas chromatography (GC×GC) coupled with time-of-flight mass spectrometry (TOFMS) and gas chromatography olfactometry (GC-O). The column combination was optimized and good separation was achieved. Structured chromatograms of furans and pyrazines were obtained and discussed. A total of 360 compounds were tentatively identified based on mass spectrum match factors, structured chromatogram and linear retention indices comparison. The most abundant class in number was ketones. A large number of esters, furans and derivatives, aldehydes and alcohols were also detected. The odor-active components were identified by comparison of the reported odor of the identified compounds with the odor of corresponding GC-O region. The odorants of methanethiol, 2-methyl-propanal, 2-methyl-butanal/3-methyl-butanal, octanal, 1-octen-3-one, dimethyl trisulfide, trimethyl-pyrazine, acetic acid, 3-(methylthio)-propanal, furfural, benzeneacetaldehyde, 3-methyl-butanoic acid/2-methyl-butanoic acid and phenethyl acetate were suspected to be the most potent. About half of them were identified as significant aroma constituents in ZAV for the first time. Their contribution to specific sensory attribute of ZAJ was also studied. The results indicated that the presented method is suitable for characterization of ZAV aroma constituents. This study also enriches our knowledge on the components and aroma of ZAV.

  8. Identification of volatiles from pineapple (Ananas comosus L.) pulp by comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Pedroso, Marcio P; Ferreira, Ernesto C; Hantao, Leandro W; Bogusz, Stanislau; Augusto, Fabio

    2011-07-01

    Combining qualitative data from the chromatographic structure of 2-D gas chromatography with flame ionization detection (GC×GC-FID) and that from gas chromatography-mass spectrometry (GC/MS) should result in a more accurate assignment of the peak identities than the simple analysis by GC/MS, where coelution of analytes is unavoidable in highly complex samples (rendering spectra unsuitable for qualitative purposes) or for compounds in very low concentrations. Using data from GC×GC-FID combined with GC/MS can reveal coelutions that were not detected by mass spectra deconvolution software. In addition, some compounds can be identified according to the structure of the GC×GC-FID chromatogram. In this article, the volatile fractions of fresh and dehydrated pineapple pulp were evaluated. The extraction of the volatiles was performed by dynamic headspace extraction coupled to solid-phase microextraction (DHS-SPME), a technique appropriate for slurries or solid matrices. Extracted analytes were then analyzed by GC×GC-FID and GC/MS. The results obtained using both techniques were combined to improve compound identifications.

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

    DEFF Research Database (Denmark)

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

    1980-01-01

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

  10. Analysis of trapped gas in 1E34 detonators by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Warner, D.K.; Back, P.S.; Barnhart, B.V.

    1980-05-14

    A method was developed to extract and then analyze gas trapped in thermally aged 1E34 detonators. This gas was extracted into an evacuated volume and injected into a gas chromatograph for separation and quantitative analysis. To effect this gas extraction, a device was designed for puncturing the detonator cup and capturing the effused gas. Limited testing of five detonators in this device shows amounts of gas ranging from about 0.5 X 10 {sup -7} to 12 X 10 {sup - 7} moles.

  11. Isotope Ratio Monitoring Gas Chromatography Mass Spectrometry (IRM-GCMS)

    Science.gov (United States)

    Freeman, K. H.; Ricci, S. A.; Studley, A.; Hayes, J. M.

    1989-01-01

    On Earth, the C-13 content of organic compounds is depleted by roughly 13 to 23 permil from atmospheric carbon dioxide. This difference is largely due to isotope effects associated with the fixation of inorganic carbon by photosynthetic organisms. If life once existed on Mars, then it is reasonable to expect to observe a similar fractionation. Although the strongly oxidizing conditions on the surface of Mars make preservation of ancient organic material unlikely, carbon-isotope evidence for the existence of life on Mars may still be preserved. Carbon depleted in C-13 could be preserved either in organic compounds within buried sediments, or in carbonate minerals produced by the oxidation of organic material. A technique is introduced for rapid and precise measurement of the C-13 contents of individual organic compounds. A gas chromatograph is coupled to an isotope-ratio mass spectrometer through a combustion interface, enabling on-line isotopic analysis of isolated compounds. The isotope ratios are determined by integration of ion currents over the course of each chromatographic peak. Software incorporates automatic peak determination, corrections for background, and deconvolution of overlapped peaks. Overall performance of the instrument was evaluated by the analysis of a mixture of high purity n-alkanes of know isotopic composition. Isotopic values measured via IRM-GCMS averaged withing 0.55 permil of their conventionally measured values.

  12. Dynamic headspace gas chromatography of volatile compounds in milk.

    Science.gov (United States)

    Urbach, G

    1987-08-28

    A method is described for investigating volatile compounds in milk. The volatiles are removed from milk by a stream of helium swept at 100 ml/min over the surface of the milk at 70 degrees C. They are trapped on 40 mg of NIOSH charcoal and then desorbed by heat and re-trapped on the front of a chromatographic column of Tenax-GC coated with 1% OV-275, the column being maintained at room temperature during trapping. An amount of 40 mg NIOSH charcoal under these conditions traps over 90% of the total quantity of the lowest boiling compounds swept from the milk, such as acetaldehyde and ethanol, and retains 100% of the total quantity of acetone, propanol and higher boiling compounds from the gas stream. The volume of milk and its temperature affect the ratios of volatiles collected and these factors are useful in increasing the proportion of a volatile of particular interest. The addition of potassium carbonate increases the yield of volatiles from 100 ml aqueous phase but not from 10 ml.

  13. Determination of Fatty Acid in Asparagus by Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Zehra HAJRULAI-MUSLIU

    2016-05-01

    Full Text Available Asparagus contain a lot of macronutrients and micronutrients including folate, dietary fibre (soluble and insoluble and phenolic compounds. Also asparagus is a good source of unsaturated linoleic and linolenic fatty acids which are precursors for Eicosapentanoic acid (EPA and Docosahexanoic acid (DHA. Unsaturated fatty acids have important biological effects and they have important role in human health. The objective of this study was to analyze fatty acid composition of asparagus as a potential source of linoleic and linolenic acid - a precursor for EPA and DHA. For this reason we analyzed fifty seven samples of asparagus collected from the local market. We used AOAC 996.06 method and analyses were performed with gas chromatograph with flame-ionization detector (GC-FID. The highest concentration of fatty acid in the asparagus was linoleic acid (C18:2n6 which content in asparagus is 25.620±1.0%. Also, asparagus is good source of -linolenic fatty acid (C18:3n3 and content of this fatty acid in asparagus is 8.840±0.3%. The omega-6 to omega-3 (n6/n3 ratio in asparagus was 3.19. Polyunsaturated fatty acids (PUFAs were higher than monounsaturated fatty acids (MUFAs, and from saturated fatty acids, palmitic acid was most frequent with 24.324±1.0%. From our study we can conclude that asparagus is very good source of unsaturated fatty acids, especially linoleic and linolenic fatty acids.

  14. Preparation of hybrid monolithic columns via "one-pot" photoinitiated thiol-acrylate polymerization for retention-independent performance in capillary liquid chromatography.

    Science.gov (United States)

    Zhang, Haiyang; Ou, Junjie; Liu, Zhongshan; Wang, Hongwei; Wei, Yinmao; Zou, Hanfa

    2015-09-01

    A novel "one-pot" approach was developed for ultrarapid preparation of various hybrid monolithic columns in UV-transparent fused-silica capillaries via photoinitiated thiol-acrylate polymerization of an acrylopropyl polyhedral oligomertic silsesquioxane (acryl-POSS) and a monothiol monomer (1-octadecanethiol or sodium 3-mercapto-1-propanesulfonate) within 5 min, in which the acrylate not only homopolymerizes, but also couples with the thiol. This unique combination of two types of free-radical reaction mechanisms offers a simple way to fabricate various acrylate-based hybrid monoliths. The physical characterization, including scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, and thermal gravimetric analysis was performed. The results indicated that the monothiol monomers were successfully incorporated into acryl-POSS-based hybrid monoliths. The column efficiencies for alkylbenzenes on the C18-functionalized hybrid monolithic column reached to 60 000-73 500 plates/m at the velocity of 0.33 mm/s in capillary liquid chromatography, which was far higher than that of previously reported POSS-based columns prepared via thermal-initiated free-radical polymerization without adding any thiol monomers. By plotting the plate height (H) of the alkylbenzenes versus the linear velocity (u) of the mobile phase, the results revealed a retention-independent efficient performance of small molecules in the isocratic elution. These results indicated that more homogeneous hybrid monoliths formed via photoinitiated thiol-acrylate polymerization; particularly, the use of the multifunctional cross-linker possibly prevented the generation of gel-like micropores, reducing mass transfer resistance (C-term). Another sulfonate-containing hybrid monolithic column also exhibited hydrophobicity and ion-exchange mechanism, and the dynamic binding capacity was calculated as 71.1 ng/cm (75 μm i.d.).

  15. Assessment of capillary anion exchange ion chromatography tandem mass spectrometry for the quantitative profiling of the phosphometabolome and organic acids in biological extracts.

    Science.gov (United States)

    Kvitvang, Hans F N; Kristiansen, Kåre A; Bruheim, Per

    2014-11-28

    Metabolic profiling has become an important tool in biological research, and the chromatographic separation of metabolites coupled with mass spectrometric detection is the most frequently used approach for such studies. The establishment of robust chromatographic methods for comprehensive coverage of the anionic metabolite pool is especially challenging. In this study, the development of a capillary ion exchange chromatography (capIC) - negative ESI tandem mass spectrometry (MS/MS) workflow for the quantitative profiling of the phosphometabolome (e.g., sugar phosphates and nucleotides) is presented. The chromatographic separation and MS/MS conditions were optimized, and the precision of repetitive injections and accuracy in terms of error percentage to true concentration were assessed. The precision is excellent for a capillary flow system with an average CV% of 8.5% for a 50-fmol standard injection and in the lower 2.4-4.4% range for higher concentrations (500-7,500 fmol). The limit of detection (LOD) ranges from 1 to 100 nM (5-500 fmol injected on column), and the limit of quantitation (LOQ) ranges from 1 to 500 nM (5-2,500 fmol injected on column). A fast gradient method with the injection of 50% methanol in water between analytical samples is needed to eliminate carry-over and ensure optimal re-equilibration of the column. Finally, the quantitative applicability of the system was tested on real biological matrices using the constant-volume standard addition method (SAM). Extracts of the human kidney Hek293 cell line were spiked with increasing concentrations of standards to determine the concentration of each metabolite in the sample. Forty-four metabolites were detected with an average uncertainty of 4.1%. Thus, the capIC-MS/MS method exhibits excellent selectivity, sensitivity and precision for the quantitative profiling of the phosphometabolome.

  16. Differentiation of mint (Mentha haplocalyx Briq.) from different regions in China using gas and liquid chromatography.

    Science.gov (United States)

    Dong, Wenjiang; Ni, Yongnian; Kokot, Serge

    2015-02-01

    In this study, complex substances such as Mint (Mentha haplocalyx Briq.) samples from different growing regions in China were analyzed for phenolic compounds by high-performance liquid chromatography with diode array detection and for the volatile aroma compounds by gas chromatography with mass spectrometry. Chemometrics methods, e.g. principal component analysis, back-propagation artificial neural networks, and partial least squares discriminant analysis, were applied to resolve complex chromatographic profiles of Mint samples. A total of 49 aroma components and 23 phenolic compounds were identified in 79 Mint samples. Principal component analysis score plots from gas chromatography with mass spectrometry and high-performance liquid chromatography with diode array detection data sets showed a clear distinction among Mint from three different regions in China. Classification results showed that satisfactory performance of prediction ability for back-propagation artificial neural networks and partial least squares discriminant analysis. The major compounds that contributed to the discrimination were chlorogenic acid, unknown 3, kaempherol 7-O-rutinoside, salvianolic acid L, hesperidin, diosmetin, unknown 6 and pebrellin in Mint according to regression coefficients of the partial least squares discriminant analysis model. This study indicated that the proposed strategy could provide a simple and rapid technique to distinguish clearly complex profiles from samples such as Mint.

  17. Measuring fuel contamination using high speed gas chromatography and cone penetration techniques

    Energy Technology Data Exchange (ETDEWEB)

    Farrington, S.P.; Bratton, W.L. [Applied Research Associates, Inc., South Royalton, VT (United States); Akard, M.L. [Chromatofast, Inc., Ann Arbor, MI (United States)] [and others

    1995-10-01

    Decision processes during characterization and cleanup of hazardous waste sites are greatly retarded by the turnaround time and expense incurred through the use of conventional sampling and laboratory analyses. Furthermore, conventional soil and groundwater sampling procedures present many opportunities for loss of volatile organic compounds (VOC) by exposing sample media to the atmosphere during transfers between and among sampling devices and containers. While on-site analysis by conventional gas chromatography can reduce analytical turnaround time, time-consuming sample preparation procedures are still often required, and the potential for loss of VOC is not reduced. This report describes the development of a high speed gas chromatography and cone penetration testing system which can detect and measure subsurface fuel contamination in situ during the cone penetration process.

  18. Polymeric imidazolium ionic liquids as valuable stationary phases in gas chromatography: chemical synthesis and full characterization.

    Science.gov (United States)

    González-Álvarez, Jaime; Blanco-Gomis, Domingo; Arias-Abrodo, Pilar; Díaz-Llorente, Daniel; Ríos-Lombardía, Nicolás; Busto, Eduardo; Gotor-Fernández, Vicente; Gutiérrez-Álvarez, María Dolores

    2012-04-06

    Seven new functionalized polymerizable ionic liquids were chemically prepared, and later applied for the preparation of polymeric stationary phases in gas chromatography. These coated GC columns, which exhibited good thermal stabilities (240-300°C) and very high efficiencies (3120-4200 plates/m), have been characterized using the Abraham solvation parameter model. The chromatographic behavior of these polymeric IL columns has been deeply studied observing excellent selectivities in the separation of many organic substances such as alkanes, ketones, alcohols, amines or esters in mixtures of polar and non polar solvents or fragrances. Remarkably, the challenging separation of xylene isomers has been possible using a bis(trifluoromethylsulfonyl)amide based imidazolium IL coated column as a gas chromatography stationary phase.

  19. [Determination of aromatics in light petroleum products by comprehensive two-dimensional gas chromatography].

    Science.gov (United States)

    Li, Yanyan

    2006-07-01

    In recent years, comprehensive two-dimensional gas chromatography (GC x GC) have been used widely, and the applications of this technique to many fields have already been reported. In the standard method of oil analysis, the concentrations of aromatics and naphthalene hydrocarbons in light petroleum products must be detected by more than two methods. Mono-aromatics, di-aromatics etc. in light petroleum products were detected only by comprehensive two-dimensional gas chromatography. After the proper selection of column system and optimization of chromatographic conditions, the method can achieve the group separations of paraffins, olefins, naphthenes, aromatics with 1 to 2 rings and some target components in light petroleum products with good reproducibility and good precision. The recoveries of standard compounds were 89.5% - 106.1%, and the relative standard deviations of repeatedly detecting the components were all lower than 5.8%. It took only 30 min to finish a determination.

  20. Simultaneous determination of carbohydrates and simmondsins in jojoba seed meal (Simmondsia chinensis) by gas chromatography.

    Science.gov (United States)

    Lein, Sabine; Van Boven, Maurits; Holser, Ron; Decuypere, Eddy; Flo, Gerda; Lievens, Sylvia; Cokelaere, Marnix

    2002-11-22

    Separate methods for the analyses of soluble carbohydrates in different plants and simmondsins in jojoba seed meal are described. A reliable gas chromatographic procedure for the simultaneous quantification of D-pinitol, myo-inositoL sucrose, 5-alpha-D-galactopyranosyl-D-pinitol. 2-alpha-D-galactopyranosyl-D-pinitol, simmondsin, 4-demethylsimmondsin, 5-demethylsimmondsin and 4,5-didemethylsimmondsin as trimethylsilyl derivatives in jojoba seed meal has been developed. The study of different extraction mixtures allowed for the quantitative recovery of the 9 analytes by a mixture of methanol-water (80:20, v/v) in the concentration range between 0.1 and 4%. Comparison of the separation parameters on three different capillary stationary phases with MS detection allowed for the choice of the optimal gas chromatographic conditions for baseline separation of the analytes.

  1. Quantitative Analysis and Fingerprint Profiles for Quality Control of Fructus Schisandrae by Gas Chromatography: Mass Spectrometry

    OpenAIRE

    Yong-Gang Xia; Bing-You Yang; Jun Liang; Qi Yang; Di Wang; Hai-Xue Kuang

    2014-01-01

    This paper describes a simple, rapid, and effective quality assessment method for Fructus Schisandrae by gas chromatography-mass spectrum (GC-MS). The method was established by using specific lignan fingerprint profiles and quantitation of characteristic compounds in this herbal medicine. The GC-MS fingerprints of 15 batches of Schisandra samples from different regions of China showed similar lignan profiles. Five peaks were selected as characteristic peaks, and all of these were identified b...

  2. Influence of ripening stages of tomatoes in the analysis of pesticides by gas chromatography

    OpenAIRE

    Sousa,Flaviane A. de; Neves,Antônio A.; Maria Eliana L. R. Queiroz; Heleno,Fernanda F.; Teófilo, Reinaldo F.; Pinho,Gevany P.

    2014-01-01

    Some parameters of tomato fruits ripening such as color, pH, ºBrix, acidity and lycopene and β-carotene content were evaluated during the ripening of fruits. Five pesticides were quantified in organic extracts derived from tomatoes at different stages of maturation. The solid-liquid extraction technique with partition at low temperature (SLE-PLT) was used to obtain these organic extracts. The matrix effect of tomato was calculated from the results of analysis by gas chromatography with e...

  3. Determination of diclofenac concentrations in human plasma using a sensitive gas chromatography mass spectrometry method

    OpenAIRE

    2016-01-01

    Background A gas chromatography mass spectrometry (GCMS) method for the determination of diclofenac in human plasma has been developed and validated. Results This method utilizes hexane which is a relatively less toxic extraction solvent compared to heptane and benzene. In addition, phosphoric acid and acetone were added to the samples as deproteination agents, which increased the recovery of diclofenac. These revised processes allow clean extraction and near-quantitative recovery of analyte ...

  4. Determination of diclofenac concentrations in human plasma using a sensitive gas chromatography mass spectrometry method

    OpenAIRE

    Shah, Iltaf; Barker, James; Naughton, Declan P; Barton, Stephen J.; Ashraf, Syed Salman

    2016-01-01

    Background\\ud A gas chromatography mass spectrometry (GCMS) method for the determination of diclofenac in human plasma has been developed and validated.\\ud \\ud Results\\ud This method utilizes hexane which is a relatively less toxic extraction solvent compared to heptane and benzene. In addition, phosphoric acid and acetone were added to the samples as deproteination agents, which increased the recovery of diclofenac. These revised processes allow clean extraction and near-quantitative recover...

  5. Evaluation of noni (Morinda citrifolia) volatile profile by dynamic headspace and gas chromatography-mass spectrometry

    OpenAIRE

    Sousa, A.; M. A. SOUZA NETO; GARRUTI, D. dos S.; Sousa, J. A.; BRITO, E. S. de

    2010-01-01

    Noni is a fruit that has interested the scientific community due to its medicinal and functional activities. Different products that contain noni are already in the market, but their consumption could be impaired by their distinctive unpleasant aroma and flavor. The aim of this work was to evaluate the noni pulp volatile profile by dynamic headspace and gas chromatography-mass spectrometry. Thirty seven volatile compounds were detected, mainly alcohols (63.3%), esters (26.9%), cetones (7.4%),...

  6. H2S Analysis in Biological Samples Using Gas Chromatography with Sulfur Chemiluminescence Detection

    OpenAIRE

    Vitvitsky, Victor; Banerjee, Ruma

    2015-01-01

    Hydrogen sulfide (H2S) is a metabolite and signaling molecule in biological tissues that regulates many physiological processes. Reliable and sensitive methods for H2S analysis are necessary for a better understanding of H2S biology and for the pharmacological modulation of H2S levels in vivo. In this chapter, we describe the use of gas chromatography coupled to sulfur chemiluminescence detection to measure the rates of H2S production and degradation by tissue homogenates at physiologically r...

  7. Measurement of Infinite Diluted Activity Coefficient of Solvents in Polymer by Inverse Gas Chromatography Method

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    @@1 INTRODUCTION Due to its short experimental time, little sample needed, suitable for broad temperature range, inverse gas chromatography (IGC) has been widely used to measure variety of properties of polymer systems, such as the intinite diluted activity coefficients of solvent in polymer, the glass transition temperature of polymer and the surface properties of polymer[1-5], etc. Those data have been used to develop the group contribution method for the prediction of thermodynamic proper-ties of polymer solution[6].

  8. Isotope-Dilution Mass Spectrometry for Quantification of Urinary Active Androgens Separated by Gas Chromatography

    OpenAIRE

    Su Hyeon Lee; Man Ho Choi; Won-Yong Lee; Bong Chul Chung

    2010-01-01

    Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methodsare needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry(GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which areclinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with β-glucur...

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

    OpenAIRE

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

    2011-01-01

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

  10. Characterization by Gas Chromatography-Mass Spectrometry of Commercially Available Thinner in the City of Cartagena

    OpenAIRE

    2013-01-01

    Thinner is a widely used product in the industry of paints, lubricants and adhesives. Its composition varies according to its use and quality. However, its chronic exposure is a concern, because it can affect major organs such as lungs, liver, kidney and the adrenal glands. This study characterizes the composition of several thinner samples commercially available in the city of Cartagena. Twelve samples were collected in different stores, these were then analyzed through gas chromatography co...

  11. Analysis of Phenolic Antioxidants in Navy Mobility Fuels by Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    2013-06-19

    methyl phenol ECD Electrochemical detector GC-MS Gas chromatography with mass selective detection HT Hydrotreated HPLC High Performance...Antioxidants are often used to meet military storage stability requirements and are required in hydrotreated and alternative fuels. It is often necessary to...constituents to be quantifiable by this method. The single column method was successfully employed to measure TTBP depletion in hydrotreated Jet A fuels

  12. Analysis of 23 polycyclic aromatic hydrocarbons in smokeless tobacco by gas chromatography-mass spectrometry

    OpenAIRE

    Stepanov, Irina; Villalta, Peter W.; Knezevich, Aleksandar; Jensen, Joni; Hatsukami, Dorothy; Hecht, Stephen S.

    2010-01-01

    Smokeless tobacco contains 28 known carcinogens and causes precancerous oral lesions and oral and pancreatic cancer. A recent study conducted by our research team identified 8 different polycyclic aromatic hydrocarbons (PAH) in U.S. moist snuff, encouraging further investigations of this group of toxicants and carcinogens in smokeless tobacco products. In this study, we developed a gas chromatography-mass spectrometry method that allows simultaneous analysis of 23 various PAH in smokeless tob...

  13. Ethanol as Internal Standard for Quantitative Determination of Volatile Compounds in Spirit Drinks by Gas Chromatography

    CERN Document Server

    Charapitsa, Siarhei V; Kulevich, Nikita V; Makoed, Nicolai M; Mazanik, Arkadzi L; Sytova, Svetlana N

    2012-01-01

    The new methodical approach of using ethanol as internal standard in gas chromatographic analysis of volatile compounds in spirit drinks in daily practice of testing laboratories is proposed. This method provides determination of volatile compounds concentrations in spirit drinks directly expressed in milligrams per liter (mg/L) of absolute alcohol according to official methods without measuring of alcohol strength of analyzed sample. The experimental demonstration of this method for determination of volatile compounds in spirit drinks by gas chromatography is described. Its validation was carried out by comparison with experimental results obtained by internal standard method and external standard method.

  14. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    Science.gov (United States)

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents.

  15. Application of the standard addition method for the determination of acrylamide in heat-processed starchy foods by gas chromatography with electron capture detector.

    Science.gov (United States)

    Zhu, Yonghong; Li, Genrong; Duan, Yunpeng; Chen, Shiqi; Zhang, Chun; Li, Yanfei

    2008-08-15

    A gas chromatography electron capture detector (GC-ECD) using the standard addition method was developed for the determination of acrylamide in heat-processed foods. The method entails extraction of acrylamide with water, filtration, defatting with n-hexane, derivatization with hydrobromic acid and saturated bromine-water, and liquid-liquid extraction with ethyl acetate. The sample pretreatment required no SPE clean-up and concentration steps prior to injection. The final extract was analyzed by GC-ECD. The chromatographic analysis was performed on polar columns, e.g. Supelcowax-10 capillary column, and good retention and peak response of the analyte were achieved under the optimal conditions. The qualification of the analyte was by identifying the peak with same retention time as standard compound 2,3-DBPA and confirmed by GC-MS. GC-MS analysis confirmed that 2,3-DBPA was converted to 2-BPA nearly completely on the polar capillary column, whether or not treated with triethylamine. A four-point standard addition protocol was used to quantify acrylamide in food samples. The limit of detection (LOD) was estimated to be 0.6μg/kg on the basis of ECD technique. Validation and quantification results demonstrated that the method should be regarded as a low-cost, convenient, and reliable alternative for conventional investigation of acrylamide.

  16. Determination of Sodium of Soy Sauce by Gas Chromatography%气相色谱法测定酱油中甜蜜素含量的探讨

    Institute of Scientific and Technical Information of China (English)

    洪晓峰

    2012-01-01

    本文建立了毛细管气相色谱法测定酱油中甜蜜素含量的分析方法。采用RTX—WAX毛细管色谱柱和氢火焰检测器测定,外标法定量。【结果】样品加标平均回收率为93.7%-99.3%,相对标准偏差(RsD)为2.5%-4.7%。实验结果表明,该方法简便、快速,适合酱油甜蜜素含量的测定。%The article established the analysis of using gas capillary chromatography to determine the content of sodium cyclamate in soy sauce. This analysis adopt RTX-WAX capillary column and hydrogen flame detector to determine, and external standard. The average spiked recoveries of 93.7%-99.3%,the relatine standard deviation(RSD)is 2.5%-4.7%.It is show our that this method is simple,fast, is suit for the determination of sodium cyclamate sauce.

  17. Microgravity Compatible Gas-Liquid Separation using Capillary Pressure Gradients Project

    Data.gov (United States)

    National Aeronautics and Space Administration — An innovative microgravity and hypogravity compatible Gas-Liquid Separator (GLS) is proposed. This novel GLS consists of an ordered array of variable sized water...

  18. Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

    NARCIS (Netherlands)

    Koster, E.H M; Hofman, N.S K; de Jong, G.J.

    1998-01-01

    Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic stre

  19. Comprehensive verification of new method "Ethanol as Internal Standard" for determination of volatile compounds in alcohol products by gas chromatography

    CERN Document Server

    Charapitsa, Siarhei V; Markovsky, Mikhail G; Yakuba, Yurii F; Kotov, Yurii N

    2014-01-01

    Recently proposed new method "Ethanol as Internal Standard" for determination of volatile compounds in alcohol products by gas chromatography is investigated from different sides. Results of experimental study from three different laboratories from Belarus and Russian Federation are presented.

  20. Multiphase Transport in Porous Media: Gas-Liquid Separation Using Capillary Pressure Gradients International Space Station (ISS) Flight Experiment Development

    Science.gov (United States)

    Wheeler, Richard R., Jr.; Holtsnider, John T.; Dahl, Roger W.; Deeks, Dalton; Javanovic, Goran N.; Parker, James M.; Ehlert, Jim

    2013-01-01

    Advances in the understanding of multiphase flow characteristics under variable gravity conditions will ultimately lead to improved and as of yet unknown process designs for advanced space missions. Such novel processes will be of paramount importance to the success of future manned space exploration as we venture into our solar system and beyond. In addition, because of the ubiquitous nature and vital importance of biological and environmental processes involving airwater mixtures, knowledge gained about fundamental interactions and the governing properties of these mixtures will clearly benefit the quality of life here on our home planet. The techniques addressed in the current research involving multiphase transport in porous media and gas-liquid phase separation using capillary pressure gradients are also a logical candidate for a future International Space Station (ISS) flight experiment. Importantly, the novel and potentially very accurate Lattice-Boltzmann (LB) modeling of multiphase transport in porous media developed in this work offers significantly improved predictions of real world fluid physics phenomena, thereby promoting advanced process designs for both space and terrestrial applications.This 3-year research effort has culminated in the design and testing of a zero-g demonstration prototype. Both the hydrophilic (glass) and hydrophobic (Teflon) media Capillary Pressure Gradient (CPG) cartridges prepared during the second years work were evaluated. Results obtained from ground testing at 1-g were compared to those obtained at reduced gravities spanning Martian (13-g), Lunar (16-g) and zero-g. These comparisons clearly demonstrate the relative strength of the CPG phenomena and the efficacy of its application to meet NASAs unique gas-liquid separation (GLS) requirements in non-terrestrial environments.LB modeling software, developed concurrently with the zero-g test effort, was shown to accurately reproduce observed CPG driven gas-liquid separation

  1. Determination of some individual chlorobiphenyls in eel-fat with capillary gaschromatography: collaborative study

    NARCIS (Netherlands)

    Tuinstra, L.G.M.T.; Roos, A.H.; Werdmuller, G.A.

    1984-01-01

    A method for the determination of six individual chlorobiphenyls in eel-fat, based on saponification of the sample and determination with capillary gas chromatography, was studied collaboratively. Eleven laboratories submitted analytical results in duplo of six individual chlorbiphenyls on two sampl

  2. Characterization of poly(4-vinylpyridine 1-oxide) by free-solution capillary electrophoresis and micellar electrokinetic chromatography.

    Science.gov (United States)

    Beneito-Cambra, Miriam; Herrero-Martínez, José M; Ramis-Ramos, Guillermo

    2008-08-01

    The migration characteristics of poly(4-vinylpyridine 1-oxide) (PVP-NO) in phosphate buffers of acidic pH (20 mM H3PO4 or NaH2PO4) have been studied using both free-solution capillary electrophoresis (FSCE) and MEKC. To inhibit adsorption, 250 mM o-phosphoethanolamine (2-aminoethyl dihydrogen phosphate) was used. In FSCE, PVP-NO showed a narrow peak and a broader band, both having anionic behavior. These peak and band were attributed to the free and aggregated or micellized PVP-NO forms, respectively. According to surface tension measurements, the CMC of SDS in the BGE was 1.8 and 0.48 mM in the absence and in the presence of 1000 microg/mL PVP-NO, respectively, and the association of the polymer with SDS was completed at 9.7 mM SDS. Using MEKC, a narrow peak and a broader band also appeared at SDS concentrations of ca. 1 mM, and their intensity increased with the SDS concentration. These peak and band were attributed to the formation of mixed micelles constituted by both free PVP-NO/SDS and aggregated PVP-NO/SDS, respectively. The determination of PVP-NO by FSCE in commercial additives for laundry was demonstrated.

  3. Determination of pore size distributions in capillary-channeled polymer fiber stationary phases by inverse size-exclusion chromatography and implications for fast protein separations.

    Science.gov (United States)

    Wang, Zhengxin; Marcus, R Kenneth

    2014-07-18

    Capillary-channeled polymer (C-CP) fibers have been utilized as liquid chromatography stationary phases, primarily for biomacromolecule separations on the analytical and preparative scales. The collinear packing of the eight-channeled C-CP fibers provides for very efficient flow, allowing operation at high linear velocity (u>100mm s(-1)) and low backpressure (transport properties, there must not be mass transfer limitations as would be imposed by having an appreciably porous phase, wherein solute diffusion limits the overall mass transport rates. To better understand the physical nano-/micro- structure of C-CP fibers, inverse size exclusion chromatography (iSEC) has been employed to determine the pore size distribution (PSD) within C-CP fibers. A diversity of test species (from metal ions to large proteins) was used as probes under non-retaining conditions to obtain a response curve reflecting the apparent partition coefficient (Kd) versus hydrodynamic radii (rm). A mean pore radius (rp) of 4.2nm with standard deviation (sp) of ±1.1nm was calculated by fitting the Kd versus rm data to model equations with a Gaussian pore size distribution, and a pore radius of 4.0±0.1nm was calculated based on a log-normal distribution. The derived mean pore radius is much smaller than traditional support materials, with the standard deviation showing a relatively uniform pore distribution. van Deemter plots were analyzed to provide practical confirmation of the structural implications. Large molecules (e.g., proteins) that are fully excluded from pores have no significant C-terms in the van Deemter plots whereas small molecules that can access the pore volumes display appreciable C-terms, as expected. Fitting of retention data to the Knox equation suggests that the columns operate with a characteristic particle diameter (dp) of ∼53μm.

  4. The role of the gas/plasma plume and self-focusing in a gas-filled capillary discharge waveguide for high-power laser-plasma applications

    CERN Document Server

    Ciocarlan, C.; Islam, M. R.; Ersfeld, B.; Abuazoum, S.; Wilson, R.; Aniculaesei, C.; Welsh, G. H.; Vieux, G.; Jaroszynski, D. A.; 10.1063/1.4822333

    2013-01-01

    The role of the gas/plasma plume at the entrance of a gas-filled capillary discharge plasma waveguide in increasing the laser intensity has been investigated. Distinction is made between neutral gas and hot plasma plumes that, respectively, develop before and after discharge breakdown. Time-averaged measurements show that the on-axis plasma density of a fully expanded plasma plume over this region is similar to that inside the waveguide. Above the critical power, relativistic and ponderomotive selffocusing lead to an increase in the intensity, which can be nearly a factor of 2 compared with the case without a plume. When used as a laser plasma wakefield accelerator, the enhancement of intensity can lead to prompt electron injection very close to the entrance of the waveguide. Self-focusing occurs within two Rayleigh lengths of the waveguide entrance plane in the region, where the laser beam is converging. Analytical theory and numerical simulations show that, for a density of 3.01018 cm3, the peak normalized...

  5. 气相色谱法及气相色谱-质谱法测定调味品中的对羟基苯甲酸酯%Determination of Parabens in Condiment by Gas Chromatography and Gas Chromatography Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    高杨; 郑玉山

    2014-01-01

    建立了调味品中对羟基苯甲酸乙酯及对羟基苯甲酸丙酯的气相色谱及气相色谱-质谱联用的测定方法。比较了四种不同气相色谱柱的分离效果,最终确定了气相色谱法使用SE-30毛细柱,气质联用法使用DB-5 ms毛细柱对提取物进行分析,并对两种结果进行比较。结果表明:运用气相色谱法和气相色谱-质谱联用法测定调味品中的对羟基苯甲酸酯的含量,气相法的回收率在85.9%~94.7%之间,气质法的回收率在84.5%~92.3%之间;两种方法的 RSD 值均小于10%,方法检出限均在0.001 g/kg 以下;实际检测中准确度高,重现性好,具有很好的应用效果,是调味品中对羟基苯甲酸酯检测的有效方法。%A method is developed for the determination of parabens in condiment by Gas Chromatogra-phy and Gas Chromatography Tandem Mass Spectrometry.The separation effect of four different gas chromatographic columns is compared.The best separation effect is confirmed by using SE-30 capil-lary column and DB-5ms capillary column.The recovery range is from 85.9% to 94.7% by Gas Chro-matography,and the recovery range is from 84.5% to 92.3% by Gas Chromatography Tandem Mass Spectrometry.The RSDs are all less than 10% and the detection limits are all under 0.001 mg/kg. The accuracy,reliability and sensitivity of the method makes it availably used for the determination of parabens in condiment.

  6. Measurement of choline and choline metabolite concentrations using high-pressure liquid chromatography and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Pomfret, E A; daCosta, K A; Schurman, L L; Zeisel, S H

    1989-07-01

    We have developed a reproducible and sensitive procedure for the isolation and measurement of choline, phosphocholine, glycerophosphocholine, phosphatidylcholine, lysophosphatidylcholine and acetylcholine in a single 100-mg sample of biological tissue. Tissues were spiked with 14C-methyl- and 2H-methyl- or 15N-choline labeled internal standards for each compound. They were extracted with chloroform/methanol/water and the aqueous and organic phases were dried. The organic phase was resuspended in chloroform/methanol (1/1, v/v) and an aliquot was applied to a silica-gel thin-layer chromatography plate. The plate was developed in chloroform/methanol/water (65/30/4, v/v). Segments which cochromatographed with external standards of phosphatidylcholine and lysophosphatidylcholine were stained, scraped, and hydrolyzed in 6 M methanolic-HCl at 80 degrees C for 60 min, liberating free choline. The aqueous phase was resuspended in methanol/water and injected onto a silica HPLC column. Choline and its metabolites were eluted using a binary nonlinear gradient of acetonitrile/ethanol/acetic acid/1 M ammonium acetate/water/0.1 M sodium phosphate (800/68/2/3/127/10, v/v changing to 400/68/44/88/400/10, v/v). Peaks were detected with an on-line radiometric detector, collected, and dried under vacuum. Each choline ester was digested in 6 M HCl at 80 degrees C to form choline. Choline was then converted to the propionyl ester and demethylated with sodium benzenethiolate. This volatile derivative was then isolated using gas chromatography and measured with a mass selective detector. Deuterated internal standards were used to correct for variations in recovery. Choline, glycerophosphocholine, phosphocholine, phosphatidylcholine, lysophosphatidylcholine, and acetylcholine were measured in rat liver, heart, muscle, kidney, plasma, red blood cells, and brain and in human plasma.(ABSTRACT TRUNCATED AT 250 WORDS)

  7. Determination of alkyl amines in atmospheric aerosol particles: a comparison of gas chromatography-mass spectrometry and ion chromatography approaches

    Directory of Open Access Journals (Sweden)

    R.-J. Huang

    2014-03-01

    Full Text Available In recent years low molecular weight alkyl amines have been recognized to play an important role in particle formation and growth in the lower atmosphere. However, major uncertainties are associated with their atmospheric processes, sources and sinks, mostly due to the lack of ambient measurements and the difficulties in accurate quantification of alkyl amines at trace level. In this study, we present the evaluation and optimization of two analytical approaches, i.e., gas chromatography-mass spectrometry (GC-MS and ion chromatography (IC, for the determination of alkyl amines in aerosol particles. Alkyl amines were converted to carbamates through derivatization with isobutyl chloroformate for GC-MS determination. A set of parameters affecting the analytical performances of the GC-MS approach, including reagent amount, reaction time and pH value, was evaluated and optimized. The accuracy is 84.3–99.1%, and the limits of detection obtained are 1.8–3.9 pg. For the IC approach, a solid phase extraction (SPE column was used to separate alkyl amines from interfering cations before IC analysis. 1–2% (v/v of acetone (or 2–4% (v/v of acetonitrile was added to the eluent to improve the separation of alkyl amines on the IC column. The limits of detection obtained are 2.1–15.9 ng and the accuracy is 55.1–103.4%. The lower accuracy can be attributed to evaporation losses of amines during the sample concentration procedure. Measurements of ambient aerosol particle samples collected in Hong Kong show that the GC-MS approach is superior to the IC approach for the quantification of primary and secondary alkyl amines due to its lower detection limits and higher accuracy.

  8. Measurements of interfacial dynamics of gas-liquid displacement in a capillary

    Science.gov (United States)

    Yan, Changfei; Qiu, Huihe

    2016-06-01

    Measurement of liquid film thickness in gas-liquid plug/slug flows is a challenging task. A novel laser interference method for measuring the interfacial film thickness of gas-liquid displacement in a plug flow has been developed. This novel technique utilizes light scattering from different liquid/gas interfaces in forming interference fringes. The interference fringes are used for calculating the film thickness. A set of simultaneous equations is derived based on geometrical optics. The experiment set up is not complex and is easy to install. The fringes are recorded by a charge-coupled device high speed camera and the image data are calculated using fast Fourier transform (FFT) and a non-linear least squares Levenberg-Marquardt algorithm. The uncertainty of this measurement technique is quite small (0.3 μm) and the entire film thickness profile can be measured at the same time.

  9. Sensitive determination of parabens in human urine and serum using methacrylate monoliths and reversed-phase capillary liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Carrasco-Correa, Enrique Javier; Vela-Soria, Fernando; Ballesteros, Oscar; Ramis-Ramos, Guillermo; Herrero-Martínez, José Manuel

    2015-01-30

    A method for the determination of parabens in human urine and serum by capillary liquid chromatography (cLC) with UV-Vis and mass spectrometry (MS) detection using methacrylate ester-based monolithic columns has been developed. The influence of composition of polymerization mixture was studied. The optimum monolith was obtained with butyl methacrylate monomer at 60/40% (wt/wt) butyl methacrylate/ethylene dimethacrylate ratio and 50wt% porogens (composed of 36wt% of 1,4-butanediol, 54wt% 1-propanol and 10wt% water). Baseline resolution of analytes was achieved through a mobile phase of acetonitrile/water in gradient elution mode. Additionally, dispersive liquid-liquid microextraction (DLLME) was combined with both cLC-UV-Vis and cLC-MS to achieve the determination of parabens in human urine and serum samples with very low limits of detection. Satisfactory intra- and inter-day repeatabilities were obtained in UV-Vis and MS detection, although the latter provided lower detection limits (up to 300-fold) than the UV-Vis detection. Recoveries for the target analytes from spiked biological samples ranged from 95.2% to 106.7%. The proposed methodology for the ultra-low determination of parabens in human urine and serum samples is simple and fast, the consumption of reagents is very low, and very small samples can be analyzed.

  10. Approaching over 10 000-fold sensitivity increase in chiral capillary electrophoresis: Cation-selective exhaustive injection and sweeping cyclodextrin-modified micellar electrokinetic chromatography.

    Science.gov (United States)

    Mikuma, Toshiyasu; Iwata, Yuko T; Miyaguchi, Hajime; Kuwayama, Kenji; Tsujikawa, Kenji; Kanamori, Tatsuyuki; Kanazawa, Hideko; Inoue, Hiroyuki

    2016-11-01

    A novel and simple method that combines an online concentration technique with an enantioseparation technique for capillary electrophoresis-namely, cation-selective exhaustive injection and sweeping cyclodextrin-modified micellar electrokinetic chromatography (CSEI-sweeping CD-modified MEKC)-realizes the effective enantioseparation of cationic analytes while keeping a significant increase of detection sensitivity. This technique consists of a slight modification of the basic CSEI-sweeping MEKC. The main idea is to simply add an anionic CD as a chiral selector into the micellar buffer including sodium dodecyl sulfate, but not to change any other buffers in order to preserve the online concentration mechanism. When applied to analysis of the street drug, methamphetamine, the method achieved not only a baseline enantioseparation but also limits of detection (LODs; S/N = 3) of 70-90 pg/mL (ppt) for each isomer. This translates to a more than 10 000-fold improvement compared to the LODs by the usual injection method. The present technique, which was made from a slight modification of CSEI-sweeping MEKC, would give an attractive approach that is applicable to almost any analytes for which CSEI-sweeping MEKC is applicable; all that is required is the selection of an appropriate anionic CD to be added to the micellar buffer.

  11. A micellar electrokinetic chromatography-mass spectrometry approach using in-capillary diastereomeric derivatization for fully automatized chiral analysis of amino acids.

    Science.gov (United States)

    Moldovan, Radu-Cristian; Bodoki, Ede; Kacsó, Timea; Servais, Anne-Catherine; Crommen, Jacques; Oprean, Radu; Fillet, Marianne

    2016-10-07

    In the context of bioanalytical method development, process automatization is nowadays a necessity in order to save time, improve method reliability and reduce costs. For the first time, a fully automatized micellar electrokinetic chromatography-mass spectrometry (MEKC-MS) method with in-capillary derivatization was developed for the chiral analysis of d- and l-amino acids using (-)-1-(9-fluorenyl) ethyl chloroformate (FLEC) as labeling reagent. The derivatization procedure was optimized using an experimental design approach leading to the following conditions: sample and FLEC plugs in a 2:1 ratio (15s, 30mbar: 7.5s, 30mbar) followed by 15min of mixing using a voltage of 0.1kV. The formed diastereomers were then separated using a background electrolyte (BGE) consisting of 150mM ammonium perfluorooctanoate (APFO) (pH=9.5) and detected by mass spectrometry (MS). Complete chiral resolution was obtained for 8 amino acids, while partial separation was achieved for 6 other amino acid pairs. The method showed good reproducibility and linearity in the low micromolar concentration range. The applicability of the method to biological samples was tested by analyzing artificial cerebrospinal fluid (aCSF) samples.

  12. Monolithic poly (SPE-co-BVPE) capillary columns as a novel hydrophilic interaction liquid chromatography stationary phase for the separation of polar analytes.

    Science.gov (United States)

    Foo, Hsiao Ching; Heaton, James; Smith, Norman W; Stanley, Shawn

    2012-10-15

    A novel hydrophilic interaction liquid chromatography (HILIC) stationary phase was prepared by the co-polymerisation of zwitterionic N,N'-dimethyl-N-methacryloxyethyl-N-(3-sulfopropyl) ammonium betaine (SPE) and the crosslinker 1,2-bis(p-vinylphenyl) ethane (BVPE) in the presence of the porogens, toluene and methanol. Monolithic columns were produced by carrying out the α,α'-azoisobutyronitrile (AIBN) initiated reaction for 1, 2, 4, 8 and 12 h inside a 200 μm i.d. fused silica capillary at 75°C (water bath). The optimum polymerisation time was shown to be 2 h, as this resulted in good porosity, due to enlarged flow-channels and the presence of a higher proportion of mesopores provided a relatively larger surface area than the other columns. The chromatographic properties of the optimised poly (SPE-co-BVPE) monolithic column were evaluated with test mixtures containing both basic and neutral compounds in the HILIC gradient separation mode. This produced relatively sharp peaks (average peak width at half height=0.1 min) with average asymmetry factors of 1.4 and baseline resolution was obtained for all the compounds. Using the isocratic separation of the test mixture, the number of theoretical plates (N) per metre calculated was between 26,888 and 35,930 by using average values obtained for triplicate injections of the compounds thiourea, toluene and acrylamide.

  13. Monitoring subcellular biotransformation of N-L-leucyldoxorubicin by micellar electrokinetic capillary chromatography coupled to laser-induced fluorescence detection.

    Science.gov (United States)

    Satori, Chad P; Meyer, Brandon; Arriaga, Edgar A

    2014-04-01

    Development of prodrugs is a promising alternative to address cytotoxicity and nonspecificity of common anticancer agents. N-L-leucyldoxorubicin (LeuDox) is a prodrug that is biotransformed to the anticancer drug doxorubicin (Dox) in the extracellular space; however, its biotransformation may also occur intracellularly in endocytic organelles. Such organelle-specific biotransformation is yet to be determined. In this study, magnetically enriched endocytic organelle fractions from human uterine sarcoma cells were treated with LeuDox. Micellar electrokinetic chromatography with laser-induced fluorescence detection (MEKC-LIF) was used to determine that 10% of LeuDox was biotransformed to Dox, accounting for ~43% of the biotransformation occurring in the post-nuclear fraction. This finding suggests that endocytic organelles also participate in the intracellular biotransformation of LeuDox to Dox.

  14. Verification of capillary pressure functions and relative permeability equations for gas production

    Energy Technology Data Exchange (ETDEWEB)

    Jang, Jaewon [Arizona State Univ., Tempe, AZ (United States)

    2016-10-25

    The understanding of multiphase fluid flow in porous media is of great importance in many fields such as enhanced oil recovery, hydrology, CO2 sequestration, contaminants cleanup and natural gas production from hydrate bearing sediments. However, there are many unanswered questions about the key parameters that characterize gas and water flows in porous media. The characteristics of multiphase fluid flow in porous media such as water retention curve, relative permeability, preferential fluid flow patterns and fluid-particle interaction should be taken into consideration for a fundamental understanding of the behavior of pore scale systems.

  15. Enantiomeric separation and quantification of ephedrine-type alkaloids in herbal materials by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Wang, Min; Marriott, Philip J; Chan, Wing-Hong; Lee, Albert W M; Huie, Carmen W

    2006-04-21

    The separation of ephedrine-type alkaloids and their enantiomers in raw herbs and commercial herbal products was investigated by carrying out enantioselective separation in the first-dimension column (containing beta-cyclodextrin as the chiral selector) of a comprehensive two-dimensional gas chromatography (GC x GC) system, whereas a polar polyethylene glycol capillary column was used for separation in the second dimension. Naturally occurring ephedrine-type alkaloids and their synthetic analogues (enantiomeric counterparts) were adequately resolved from each other, as well as from potential interference species in the sample matrix using GC x GC, whereas single column GC analysis was unable to separate all the alkaloids of interest. Detection limits in the order of 0.1-1.3 microg/mL and linearity of calibration with R(2)>or=0.999 over approximately the range of 0.5-100 microg/mL for the quantitative determination of various ephedrine-type alkaloids were obtained. The commercial herbal products tested contained mostly (-)-ephedrine, (+)-pseudoephedrine, (-)-N-methylephedrine and (-)-norephedrine, with concentrations in the range of 40-2100, 0-1,300, 15-300 and 0-30 microg/g of the product, respectively, and repeatability of analysis was generally in the range of 1-5%. The present GCxGC method is effective and useful for the determination of the dosage levels of the principle ephedrine-type alkaloids in commercial health supplements and complex raw herb formulations, as well the differentiation of ephedrine-containing products that were derived from natural plant or synthetic sources, e.g., simply by visualizing the presence or absence of the enantiomeric pairs of (+/-) ephedrine and (+/-)-N-methylephedrine in the GC x GC chromatograms.

  16. Sensitive method for the determination of roxarsone using solid-phase microextraction with multi-detector gas chromatography.

    Science.gov (United States)

    Roerdink, Aaron R; Aldstadt, Joseph H

    2004-11-19

    We describe the development, optimization, and application of a novel method for the unequivocal identification and quantification of roxarsone (3-nitro-4-hydroxyphenylarsonic acid, 3-NHPAA) at low microg L(-1) levels. The method is based on capillary gas-liquid chromatography with parallel quadrupole ion-trap mass spectrometric (QIT-MS) and pulsed flame photometric detection (PFPD). The sensitive method couples the arsenic specificity of PFPD with the high selectivity of molecular MS for the determination of roxarsone, dimethylarsenic acid (DMAA), and monomethylarsonic acid (MMAA) in complex matrices. Analytes were derivatized based on the approach we previously reported [B. Szostek, J.H. Aldstadt, J. Chromatogr. A 807 (1998) 253 and D.R. Killelea, J.H. Aldstadt, J. Chromatogr. A 918 (2001) 169] for the reaction of organoarsenicals with 1,3-propanedithiol (PDT). The cyclic dithiaarsenolines formed were extracted from the sample matrix in the liquid phase by solid-phase microextraction (SPME). The optimized SPME conditions employed a 65 microm polydimethlysiloxane-divinylbenzene (PDMS-DVB) fiber, extraction temperature of 70 degrees C and fiber equilibration time of 15.0 min. The mass spectrum of the dithiaarsenoline of roxarsone showed a base peak that corresponded to the predicted structure at m/z 319 and the tell-tale peak of an arsenic compound derivatized with PDT at m/z 181. Further peaks at m/z 149 and 228 were observed and found to be unique to roxarsone, formed by an interesting internal rearrangement of the ONOH functionality. A linear calibration model was prepared for roxarsone over an environmentally relevant range (0.0-100 microg L(-1)) and a detection limit of 2.69 microg L(-1) (3sigma) was observed. The method was applied to several fortified environmental surface water samples (50 microg L(-1)) where the average recovery for roxarsone was 103+/-10.9%.

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

    Directory of Open Access Journals (Sweden)

    Michael Phillips

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

  18. Multiresidue analysis of 50 pesticides in grape, pomegranate, and mango by gas chromatography-ion trap mass spectrometry.

    Science.gov (United States)

    Savant, Rahul H; Banerjee, Kaushik; Utture, Sagar C; Patil, Sangram H; Dasgupta, Soma; Ghaste, Manoj S; Adsule, Pandurang G

    2010-02-10

    A selective and sensitive multiresidue analysis method is reported for simultaneous determination of 50 pesticides of different chemical classes in three commercially important fruits of different nature viz. grape, pomegranate, and mango. The sample preparation method involves extraction of a 10 g sample with 10 mL of ethyl acetate; cleanup by dispersive solid phase extraction with primary secondary amine (PSA, 25 mg) for grape and PSA + graphitized carbon black (25 + 5 mg) for pomegranate and mango; and determination by gas chromatography-ion trap mass spectrometry through multiple reaction monitoring (MRM). Sample preparation under acidified (pH 4) and cold (<4 degrees C) conditions, use of PTV-large volume injection (20 microL) through multibaffled liner and chromatographic separation on a short 10 m VF-5MS capillary column gave a satisfactory response for all of the analytes including relatively unstable compounds such as captan, captafol, folpet, endrine, and iprodione within 31.8 min. The limit of quantification (LOQ) of most of the compounds was

  19. Capillary high-performance liquid chromatography/mass spectrometric analysis of proteins from affinity-purified plasma membrane.

    Science.gov (United States)

    Zhao, Yingxin; Zhang, Wei; White, Michael A; Zhao, Yingming

    2003-08-01

    Proteomics analysis of plasma membranes is a potentially powerful strategy for the discovery of proteins involved in membrane remodeling under diverse cellular environments and identification of disease-specific membrane markers. A key factor for successful analysis is the preparation of plasma membrane fractions with low contamination from subcellular organelles. Here we report the characterization of plasma membrane prepared by an affinity-purification method, which involves biotinylation of cell-surface proteins and subsequent affinity enrichment with strepavidin beads. Western blotting analysis showed this method was able to achieve a 1600-fold relative enrichment of plasma membrane versus mitochondria and a 400-fold relative enrichment versus endoplasmic reticulum, two major contaminants in plasma membrane fractions prepared by conventional ultracentrifugation methods. Capillary-HPLC/MS analysis of 30 microg of affinity-purified plasma membrane proteins led to the identification of 918 unique proteins, which include 16.4% integral plasma membrane proteins and 45.5% cytosol proteins (including 8.6% membrane-associated proteins). Notable among the identified membrane proteins include 30 members of ras superfamily, receptors (e.g., EGF receptor, integrins), and signaling molecules. The low number of endoplasmic reticulum and mitochondria proteins (approximately 3.3% of the total) suggests the plasma membrane preparation has minimum contamination from these organelles. Given the importance of integral membrane proteins for drug design and membrane-associated proteins in the regulation cellular behaviors, the described approach will help expedite the characterization of plasma membrane subproteomes, identify signaling molecules, and discover therapeutic membrane-protein targets in diseases.

  20. Identification and measurement of chlorinated organic pesticides in water by electron-capture gas chromatography

    Science.gov (United States)

    Lamar, William L.; Goerlitz, Donald F.; Law, LeRoy M.

    1965-01-01

    Pesticides, in minute quantities, may affect the regimen of streams, and because they may concentrate in sediments, aquatic organisms, and edible aquatic foods, their detection and their measurement in the parts-per-trillion range are considered essential. In 1964 the U.S. Geological Survey at Menlo Park, Calif., began research on methods for monitoring pesticides in water. Two systems were selected--electron-capture gas chromatography and microcoulometric-titration gas chromatography. Studies on these systems are now in progress. This report provides current information on the development and application of an electron-capture gas chromatographic procedure. This method is a convenient and extremely sensitive procedure for the detection and measurement of organic pesticides having high electron affinities, notably the chlorinated organic pesticides. The electron-affinity detector is extremely sensitive to these substances but it is not as sensitive to many other compounds. By this method, the chlorinated organic pesticide may be determined on a sample of convenient size in concentrations as low as the parts-per-trillion range. To insure greater accuracy in the identifications, the pesticides reported were separated and identified by their retention times on two different types of gas chromatographic columns.

  1. Gas Phase Chromatography of some Group 4, 5, and 6 Halides

    Energy Technology Data Exchange (ETDEWEB)

    Sylwester, Eric Robert [Univ. of California, Berkeley, CA (United States)

    1998-10-01

    Gas phase chromatography using The Heavy Element Volatility Instrument (HEVI) and the On Line Gas Apparatus (OLGA III) was used to determine volatilities of ZrBr4, HfBr4, RfBr4, NbBr5, TaOBr3, HaCl5, WBr6, FrBr, and BiBr3. Short-lived isotopes of Zr, Hf, Rf, Nb, Ta, Ha, W, and Bi were produced via compound nucleus reactions at the 88-Inch Cyclotron at Lawrence Berkeley National Laboratory and transported to the experimental apparatus using a He gas transport system. The isotopes were halogenated, separated from the other reaction products, and their volatilities determined by isothermal gas phase chromatography. Adsorption Enthalpy (ΔHa) values for these compounds were calculated using a Monte Carlo simulation program modeling the gas phase chromatography column. All bromides showed lower volatility than molecules of similar molecular structures formed as chlorides, but followed similar trends by central element. Tantalum was observed to form the oxybromide, analogous to the formation of the oxychloride under the same conditions. For the group 4 elements, the following order in volatility and ΔHa was observed: RfBr4 > ZrBr4 > HfBr4. The ΔHa values determined for the group 4, 5, and 6 halides are in general agreement with other experimental data and theoretical predictions. Preliminary experiments were performed on Me-bromides. A new measurement of the half-life of 261Rf was performed. 261Rf was produced via the 248Cm(18O, 5n) reaction and observed with a half-life of 74-6+7 seconds, in excellent agreement with the previous measurement of 78-6+11 seconds. We recommend a new half-life of 75±7 seconds for 261Rf based on these two measurements. Preliminary studies in transforming HEVI from an isothermal (constant

  2. Capillary seal capacity of cenozoic mudstone caprocks of shallow gas occurrences, dutch offshore

    NARCIS (Netherlands)

    Verweij, J.M.; Daza Cajigal, V.; Bruin, G. de; Geel, K.

    2014-01-01

    The seals of the shallow gas occurrences in the northern offshore of the Netherlands are formed by siliciclastic intra-delta mudstones of Plio-Pleistocene age. There are no publicly available measured values of the seal capacity of these Plio-Pleistocene caprock mudstones. We developed, tested and a

  3. Effect of the interface on separation in multicapillary gas chromatography-based hyphenated techniques for speciation analysis of organometallic compounds.

    Science.gov (United States)

    Jitaru, Petru; Birzu, Adrian; Mocanu, Raluca; Adams, Freddy C

    2005-08-01

    This paper reports the effect of transfer line (TL) internal diameter (i.d.) on gas chromatographic separation characteristics such as efficiency and speed, when a multicapillary (MC) column is used for speciation analysis of mercury. Five different TL consisting of fused-silica capillaries with 0.15, 0.20, 0.25, 0.32, and 0.53 mm i.d. are compared. The separation efficiency and total chromatographic run time are critically affected by the i.d. of the TL. Narrow capillaries (i.d. or =35 psig) and wide TL (> or =0.25 mm i.d.).

  4. [The rapid analysis of polychlorinated quaterphenyls in blood using different diameter capillary column with the high-resolution gas chromatograph high-resolution mass spectrometer].

    Science.gov (United States)

    Yasutake, Daisuke; Ashizuka, Yuki; Hori, Tsuguhide; Kurokawa, Youichi; Kajiwara, Jumboku; Hirata, Teruaki; Ishiguro, Yasuhisa; Iida, Takao; Uchi, Hiroshi; Furue, Masutaka

    2011-04-01

    The polychlorinated quaterphenyl (PCQ) concentrations in blood are important discriminative parameters in yusho patient. In this study, a rapid analytical method for PCQ using different diameter capillary column (rapid-Rtx65TG) with high-resolution gas chromatograph high-resolution mass spectrometer (HRGC/HRMS) instead of the gas chromatograph electron capture detector (ECD/GC) was developed. Using different diameter capillary columns, the analysis time of the HRGC/HRMS was drastically shortened, and the detection sensitivity was improved. In the rapid-Rtx65TG column, a small-bore capillary column (length 1m, I.D. 0.1mm) was connected with the inlet side of the GC, and behind that column, a large-bore capillary column (length 15mm, I.D. 0.53mm) for octadecachloroquaterphenyl (ODCQ) analysis was connected. In the HRGC/HRMS measurement of ODCQ by the rapid-Rtx65TG column, the minimum limit of detection for the apparatus was 0.4 pg, and the minimum limit of determination for the blood was 0.008 ppb. On ECD/GC in the conventional method and HRGC/HRMS in this study, the PCQ concentration in blood including yusho patients and yusho suspected persons was almost equivalent.

  5. Quantification of the plant-derived hallucinogen Salvinorin A in conventional and non-conventional biological fluids by gas chromatography/mass spectrometry after Salvia divinorum smoking.

    Science.gov (United States)

    Pichini, Simona; Abanades, Sergio; Farré, Magí; Pellegrini, Manuela; Marchei, Emilia; Pacifici, Roberta; Torre, Rafael de la; Zuccaro, Piergiorgio

    2005-01-01

    A gas chromatography method with mass spectrometric detection is described for the determination of Salvinorin A, the main active ingredient of the hallucinogenic mint Salvia divinorum. The method was validated in plasma, urine, saliva and sweat using 17-alpha-methyltestosterone as internal standard. The analytes were extracted from biological matrices with chloroform/isopropanol (9:1, v/v). Chromatography was performed on a 5% phenyl methyl silicone capillary column and analytes were determined in the selected ion monitoring mode. The method was validated over the concentration range 0.015-5 microg/mL plasma, urine and saliva and 0.01-5 microg/patch in the case of sweat. Mean recoveries ranged between 77.1 and 92.7% for Salvinorin A in different biological matrices, with precision and accuracy always better than 15%. The method was applied to the analysis of urine, saliva and sweat from two consumers after smoking 75 mg plant leaves to verify the presence of the active ingredient of S. divinorum in human biological fluids as a biomarker of plant consumption. Salvinorin A was detected in urine (2.4 and 10.9 ng/mL) and saliva (11.1 and 25.0 ng/mL), but not in sweat patches from consumers.

  6. Pyrolysis-gas chromatography-mass spectrometry for studying N-vinyl-2-pyrrolidone-co-vinyl acetate copolymers and their dissolution behaviour.

    Science.gov (United States)

    Chojnacka, Aleksandra; Ghaffar, Abdul; Feilden, Andrew; Treacher, Kevin; Janssen, Hans-Gerd; Schoenmakers, Peter

    2011-11-14

    Knowledge on the solubility behaviour and dissolution rate of speciality and commodity polymers is very important for the use of such materials in high-tech applications. We have developed methods for the quantification and characterization of dissolved copolymers of N-vinyl-2-pyrrolidone (VP) and vinyl acetate (VA) during dissolution in water. The methods are based on pyrolysis (Py) performed in a programmed-temperature vaporization injector with subsequent identification and quantification of the components in the pyrolysate using capillary gas chromatography-mass spectrometry (GC-MS). By injecting large volumes and applying cryo-focussing at the top of the column, low detection limits could be achieved. The monomer ratio was found to have the greatest effect on the dissolution rate of the PVP-co-VA copolymers. The material with the highest amount of VA (50%) dissolves significantly slower than the other grades. Size-exclusion chromatography (SEC) and Py-GC-MS were used to measure molecular weights and average chemical compositions, respectively. Combined off-line SEC//Py-GC-MS was used to determine the copolymer composition (VP/VA ratio), as a function of the molecular weight for the pure polymers. In the dissolution experiments, a constant VP/VA ratio across the dissolution curve was observed for all copolymers analysed. This suggests a random distribution of the two monomers over the molecules.

  7. Poly(ethylene oxide)-bonded stationary phase for separation of inorganic anions in capillary ion chromatography.

    Science.gov (United States)

    Linda, Roza; Lim, Lee Wah; Takeuchi, Toyohide

    2013-06-14

    A tosylated-poly(ethylene oxide) (PEO) reagent was reacted with primary amino groups of an aminopropylsilica packing material (TSKgel NH2-60) in acetonitrile to form PEO-bonded stationary phase. The reaction was a single and simple step reaction. The prepared stationary phase was able to separate inorganic anions. The retention behavior of six common inorganic anions on the prepared stationary phase was examined under various eluent conditions in order to clarify its separation/retention mechanism. The elution order of the tested anions was iodate, bromate, bromide, nitrate, iodide, and thiocyanate, which was similar as observed in common ion chromatography. The retention of inorganic anions could be manipulated by ion exchange interaction which is expected that the eluent cation is coordinated among the PEO chains and it works as the anion-exchange site. Cations and anions of the eluent therefore affected the retention of sample anions. We demonstrated that the retention of the analyte anions decreased with increasing eluent concentration. The repeatability of retention time for the six anions was satisfactory on this column with relative standard deviation values from 1.1 to 4.3% when 10mM sodium chloride was used as the eluent. Compared with the unmodified TSKgel NH2-60, the prepared stationary phase retained inorganic anions more strongly and the selectivity was also improved. The present stationary phase was applied for the determination of inorganic anions contained in various water samples.

  8. Simultaneous and Rapid Determination of Main Lignans in Different Parts of Schisandra Sphenanthera by Micellar Electrokinetic Capillary Chromatography

    Directory of Open Access Journals (Sweden)

    Ming Guan

    2011-05-01

    Full Text Available Lignans are imporant active ingredients of Schisandra sphenanthera. A micellar electrokinetic chromatography method was developed for the simultaneous determination of eight lignans – schizandrin, schisandrol B, schisantherin A, schisanhenol, anwulignan, deoxyschizandrin, schizandrin B and schizandrin C – in different parts of S. sphenanthera. The key factors for separation and determination were studied and the best analysis conditions were obtained using a background electrolyte of 10 mM phosphate-37.5 mM SDS-35% v/v acetonitrile (pH 8.0 at the separation voltage of 28 kV and detection at 214 nm, whereby the plant samples could be analyzed within 9.0 min. Analysis yielded good reproducibility (RSD between 1.19-2.28% and good recovery (between 92.2-103.8%. The detection limits (LOD and limit of quantification (LOQ were within 0.4-1.2 mg/L and 1.5-4.0 mg/L. This method is promising to improve the quality control of different parts of S. sphenanthera.

  9. Complete elution of vacuum gas oil resins by comprehensive high-temperature two-dimensional gas chromatography.

    Science.gov (United States)

    Boursier, Laure; Souchon, Vincent; Dartiguelongue, Cyril; Ponthus, Jérémie; Courtiade, Marion; Thiébaut, Didier

    2013-03-08

    The development of efficient conversion processes requires extended knowledge on vacuum gas oils (VGOs). Among these processes, hydrocracking is certainly one of the best suited to meet the increasing demand on high quality diesel fuels. Most of refractory and inhibiting compounds towards hydrocracking and especially nitrogen containing compounds are contained in a fraction of the VGO called the resin fraction, which corresponds to the most polar fraction of a VGO obtained by liquid chromatography (LC) fractionation on a silica column. However, the lack of resolution observed through existing analytical methods does not allow a detailed characterization of these fractions. A recent study showed that comprehensive high temperature two-dimensional gas chromatography (HT-GC×GC) methods could be optimized in order to elute heavy compounds. This method was implemented for the analysis of VGO resin fractions and complete elution was reached. Firstly, the method was validated through repeatability, accuracy, linearity and response factors calculations. Four VGO resin fractions were analyzed and their HT-GC×GC simulated distillation curves were compared to their GC simulated distillation (GC-SimDist) curves. This comparison showed that the method allows complete elution of most of the analyzed VGO resin fractions. However, a detailed characterization of these fractions is not yet obtained due to the very large number of heteroatomic and aromatic species that a flame ionization detector can detect. Current work aims at increasing the selectivity of GC×GC by using heteroatom selective detectors in order to improve the characterization of such products.

  10. Application of high-temperature gas chromatography to the analysis of used frying fats

    Energy Technology Data Exchange (ETDEWEB)

    Aguirre, M.; Marmesat, S.; Ruiz Mendez, M. V.; Dobarganes, M. C.

    2010-07-01

    The determination of polar compounds is the most commonly applied technique in the analysis of used frying fats and oils. High-temperature gas chromatography allows for a quantitative determination of oxidized monomeric FAME and dimeric FAME thus giving extra information on oil degradation starting from the fraction of polar compounds. Polar compounds are trans esterified and methyl esters are separated in a VF-5ht Ultimetal column (150 degree centigrade -held for 5 min- rising at 5 degree centigrade min-1 to 370 degree centigrade and held for 5 min) using methyl tricosanoate as internal standard. Results are compared with those obtained by more complex alternative methodology using high-performance size-exclusion chromatography. (Author)

  11. A salting out-acetonitrile homogeneous extraction coupled with gas chromatography-mass spectrometry method for the simultaneous determination of thirteen N-nitrosamines in skin care cosmetics.

    Science.gov (United States)

    Dong, Hao; Guo, Xindong; Xian, Yanping; Luo, Haiying; Wang, Bin; Wu, Yuluan

    2015-11-27

    A sensitive gas chromatography-mass spectrometry method was established for the simultaneous determination of thirteen N-nitrosamines (NAs) in skin care cosmetics. The cosmetics samples were firstly dispersed by water and subsequently extracted and purified using salting out-acetonitrile homogeneous extraction method. Finally, the extracting solution was concentrated by slow nitrogen gas blowing. All of the samples were separated by INNOWAX capillary chromatographic column, and detected by selected ion monitoring (SIM) mode of gas chromatography-mass spectrometry (GC-MS) and quantified by isotope internal standard method. The method was validated for linearity and range, accuracy, precision and sensitivity. Under the optimized condition, the calibration curves were linear over the selected concentration ranges of 2-500μg/L for all the thirteen analytes, with calculated coefficients of determination (R(2)) of greater than 0.996. The limits of detection (LODs) and the limits of quantitation (LOQs) of the method were 3-15μg/kg and 10-50μg/kg, respectively. Recoveries were calculated at three levels of concentration spiked in two kinds of cosmetics (skin care cream and water). The values were found between 93.8% and 121.0% with relative standard deviation (RSD) values of 2.5-7.2% for intra-day precision (n=6) and 3.3-6.7% for inter-day precision (n=5). The method was successfully applied to analyze twenty-two cosmetics samples and N-nitrosodimethylamine (NDMA) was detected in one sample with the concentration of 207μg/kg.

  12. Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

    Science.gov (United States)

    Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

    2016-03-01

    A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples.

  13. Macroporous polymer monoliths as second dimension columns in comprehensive two-dimensional gas chromatography: a feasibility study

    NARCIS (Netherlands)

    D. Peroni; R.J. Vonk; W. van Egmond; H.-G. Janssen

    2012-01-01

    When the typical column combinations are used, comprehensive two-dimensional gas chromatography (GC × GC) suffers from the impossibility to operate both dimensions at their optimum carrier gas velocities at the same time. This as a result of the flow mismatch caused by the different dimensions of th

  14. Comparison of the quantification of caffeine in human plasma by gas chromatography and ELISA

    Directory of Open Access Journals (Sweden)

    A.B. Carregaro

    2001-06-01

    Full Text Available In the present study we evaluated the precision of the ELISA method to quantify caffeine in human plasma and compared the results with those obtained by gas chromatography. A total of 58 samples were analyzed by gas chromatography using a nitrogen-phosphorus detector and routine techniques. For the ELISA test, the samples were diluted to obtain a concentration corresponding to 50% of the absorbance of the standard curve. To determine whether the proximity between the I50 of the standard curve and that of the sample would bring about a more precise result, the samples were divided into three blocks according to the criterion of difference, in modulus, of the I50 of the standard curve and of the I50 of the sample. The samples were classified into three groups. The first was composed of 20 samples with I50 up to 1.5 ng/ml, the second consisted of 21 samples with I50 ranging from 1.51 to 3 ng/ml, and the third of 17 samples with I50 ranging from 3.01 to 13 ng/ml. The determination coefficient (R² = 0.999 showed that the data obtained by gas chromatography represented a reliable basis. The results obtained by ELISA were also reliable, with an estimated Pearson correlation coefficient of 0.82 between the two methods. This coefficient for the different groups (0.88, 0.79 and 0.49 for groups 1, 2 and 3, respectively showed greater reliability for the test with dilutions closer to I50.

  15. Theoretical Description of the Third Order Parametric Wave Mixing in a Gas-Filled Capillary of Femto-Second Laser Pulse

    Institute of Scientific and Technical Information of China (English)

    CHEN Bao-Zhen; HUANG Zu-Qia

    2004-01-01

    The theoretical signal-pressure curves are calculated from approximate analytical solutions of the coupledequations describing the third order parametric wave mixing in a gas-filled capillary of femto-second laser pulses. Thecomparison with the corresponding experimental curves suggests that the following three factors exert important influ-ences on the degree of fitting between the theoretical and experimental results: the walk-off, the phase modulation, andthe third order harmonic of idler pulse.

  16. 高柱容量毛细管气相色谱柱研究进展%Progress of High Column Capacity Capillary Column

    Institute of Scientific and Technical Information of China (English)

    周阳; 吴波; 高尧华; 刘磊; 牛娜

    2012-01-01

    随着分析技术和色谱技术的发展,作为气相色谱仪的核心―毛细管柱的制备改进工作取得了丰富的研究成果。本文综述了近年来毛细管气相色谱柱,主要包括大口径、厚液膜毛细管柱、微填充柱、集束毛细管柱、环形毛细管柱及纤维填充柱,在柱容量改进方面的工作及其应用进展。%With the development of analysis and chromatography technology, the preparation of capillary gas chromatography column, as the core of capillary gas chromatography, has obtained abundant research achievements. In this paper, the progress on the development of capillary gas chromatography column capacity and its applications, mainly including those on wide-bore capillary column, micro-packed column, multicapillary column, annular capillary column and fiber packed capillary column, were reviewed.

  17. Simultaneous determination of aliphatic hydrocarbons, PCBs and PCTs in pork liver by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez-Barros, C. [Dept. de Quimica Analitica, Nutricion y Bromatologia, Area Nutricion y Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Alvarez Pineiro, M.E. [Inst. de Investigacion y Analisis Alimentarios, Lab. de Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Simal Lozano, J. [Dept. de Quimica Analitica, Nutricion y Bromatologia, Area Nutricion y Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain); Lage Yusty, M.A. [Inst. de Investigacion y Analisis Alimentarios, Lab. de Bromatologia, Facultad de Farmacia, Santiago de Compostela (Spain)

    1996-10-01

    A multicomponent extraction/concentration procedure has been developed for the enrichment of PCBs, PCTs and aliphatic hydrocarbons (pristane, C{sub 18}, C{sub 19}, C{sub 20}, C{sub 22}, C{sub 24}, C{sub 28}, C{sub 32} and C{sub 36}) in pork liver. These components of the enriched extract were then simultaneously determined by gas chromatography. Mean recoveries ranged from 81.5% for pristane to 93% for PCBs; CV % (0.9-6.7) indicated the method to be both precise and reproducible. (orig.)

  18. Acid-base and surface energy characterization of grafted polyethylene using inverse gas chromatography.

    Science.gov (United States)

    Uhlmann, Petra; Schneider, Steffen

    2002-09-06

    For a specific design of interfaces, i.e. in composites and blends, it is essential to know the surface thermodynamics of the components. Polyethylene grafted with maleic anhydride and maleic anhydride-styrene mixtures, respectively, was the component of interest of our investigations. Inverse gas chromatography (IGC) at infinite dilution was shown to be an appropriate method to evaluate the dispersive and acid-base surface characteristics although there is an influence of bulk absorption and morphology when performing IGC above the glass transition temperature of the polymer.

  19. Identification of petroleum distillates from fire debris using multidimensional gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Jayatilaka, A. (Dept. of Chemistry, Wayne State Univ., Detroit, MI (United States)); Poole, C.F. (Dept. of Chemistry, Wayne State Univ., Detroit, MI (United States))

    1994-08-01

    A method for identifying petroleum distillates (accelerants) in fire debris samples by dynamic headspace analysis and multidimensional gas chromatography is described. The method relies on the separation of target compounds characteristic of different petroleum distillate classes from interfering co-eluting and matrix components. A relatively non-polar column is used to characterize the volatility distribution of the sample and heartcutting to a second polar column of certain fractions to separate target compounds from interferences unresolved on the first column. The method is demonstrated for the identification of gasoline, kerosene, charcoal lighter fluid, and paint thinners in simulated arson samples. (orig.)

  20. Screening of Brazilian fruit aromas using solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Augusto, F; Valente, A L; dos Santos Tada, E; Rivellino, S R

    2000-03-17

    Manual headspace solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) was used for the qualitative analysis of the aromas of four native Brazilian fruits: cupuassu (Theobroma grandiflorum, Spreng.), cajá (Spondias lutea. L.), siriguela (Spondias purpurea, L.) and graviola (Anona reticulata, L). Industrialized pulps of these fruits were used as samples, and extractions with SPME fibers coated with polydimethylsiloxane, polyacrylate, Carbowax and Carboxen were carried out. The analytes identified included several alcohols, esters, carbonyl compounds and terpernoids. The highest amounts extracted, evaluated from the sum of peak areas, were achieved using the Carboxen fiber.

  1. Determination of Surface Energy of Natural Zeolite by Inverse Gas Chromatography

    Science.gov (United States)

    Bilgiç, Ceyda; Karakehya, Naile

    2016-10-01

    In this study, surface energy of natural zeolite was investigated using inverse gas chromatography (IGC). Purified zeolite was prepared from natural zeolite applying decantation and centrifugation process together. For IGC studies, retention time of n-octane, n-nonane and n-decane were measured at infinite dilution conditions, between 250 and 280 °C. Dispersive component of the surface energy (γd S)of purified zeolite was calculated. γd S values calculated using Schultz et al methods decrease with temperature.

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

  3. Analysis of the citric acid cycle intermediates using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kombu, Rajan S; Brunengraber, Henri; Puchowicz, Michelle A

    2011-01-01

    Researchers view analysis of the citric acid cycle (CAC) intermediates as a metabolomic approach to identifying unexpected correlations between apparently related and unrelated pathways of metabolism. Relationships of the CAC intermediates, as measured by their concentrations and relative ratios, offer useful information to understanding interrelationships between the CAC and metabolic pathways under various physiological and pathological conditions. This chapter presents a relatively simple method that is sensitive for simultaneously measuring concentrations of CAC intermediates (relative and absolute) and other related intermediates of energy metabolism using gas chromatography-mass spectrometry.

  4. Identification of a flunixin metabolite in camel by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Wasfi, I A; Hadi, A A; Alkatheeri, N A; Barezaiq, I M; ElGhazali, M; Boni, N S; Zorob, O

    1998-05-29

    A flunixin metabolite, a hydroxylated product, has been identified in camel urine and plasma samples using gas chromatography-mass spectrometry (GC-MS) and GC-MS-MS in the electron impact and chemical ionization modes. Its major fragmentation pattern has been verified by GC-MS-MS in daughter ion and parent ion scan modes. The method could detect flunixin and its metabolite in camel urine after a single intravenous dose of 2.2 mg of flunixin/kg body weight for 96 and 48 h, respectively, which increases the reliability of antidoping control analysis.

  5. [Characterization of aromatic hydrocarbons in heavy gas oil using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry].

    Science.gov (United States)

    Guo, Kun; Zhou, Jian; Liu, Zelong

    2012-02-01

    An analytical method for separating and identifying the aromatic hydrocarbons in heavy gas oil using comprehensive two-dimensional gas chromatography (GC x GC) coupled to time-of-flight mass spectrometry (TOF MS) was established. The two-dimensional distribution by ring number of the aromatic hydrocarbons was obtained. Besides phenanthrene and methyl-phenanthrene, many other polycyclic aromatic hydrocarbons (PAHs) such as pyrene and benzo [a] anthracene were identified by using the retention times, standard mass spectra or literature reports. The method was successfully applied to the hydrotreating process of heavy gas oil and the hydrotreated products of phenanthrene, pyrene were identified. This method provided technical support for the characterization of aromatic hydrocarbons in heavy gas oil and the investigation of hydrogenation mechanism of polycyclic aromatic hydrocarbons. Compared with the conventional method, gas chromatography coupled to mass spectrometry (GC-MS), the GC x GC-TOF MS method illustrated the obvious advantages for heavy gas oil analysis.

  6. [Evaluation of inverse gas chromatography (IGC) methods to measure astragaloside solubility parameter from Buyang Huanwu decoction].

    Science.gov (United States)

    Tang, Yu; Hu, Chao; Liao, Qiong; Liu, Wen-long; Yang, Yan-tao; He, Hong; He, Fu-yuan

    2015-01-01

    The solubility parameter determination of astrageloside from Buyang Huanwu decoction with inverse gas chromatography (IGC) method evaluation was investigated in this paper. Di-n-octyl phthalate Kwai alternative sample was used to carry out methodological study. The accuracy of the measured correlation coefficient was 0.992 1. Experimental precision measured by IGC experiments showed that the results were accurate and reliable. The sample was uniformly coated on the surface of an inert carrier and N2 gas was carrier gas, a variety of polar solvents such as isopropanol, toluene, acetone, chloroform, cyclohexane as probes. TCD detector temperature was 150 degrees C, gas room temperature was 120 degrees C. Similar headspace method was used whichever over 1 μL gas into the GC measurement, Retention time t(R), t(0) and all the parameters of air and probes molecules within the column were tested. Astragaloside solubility parameter was (21.02 ± 2.4) [J x cm(-3)] ½, literature value was 19.24 [J x cm(-3)] ½, and relevant coefficient was 0.984 5. IGC method is effective and accurate to measure ingredients solubility parameter.

  7. Ultra-high-stability, pH-resistant sol-gel titania poly(tetrahydrofuran) coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Segro, Scott S; Cabezas, Yaniel; Malik, Abdul

    2009-05-15

    A sol-gel titania poly(tetrahydrofuran) (poly-THF) coating was developed for capillary microextraction hyphenated on-line with high-performance liquid chromatography (HPLC). Poly-THF was covalently bonded to the sol-gel titania network which, in turn, became chemically anchored to the inner surface of a 0.25mm I.D. fused silica capillary. For sample preconcentration, a 38-cm segment of the sol-gel titania poly-THF coated capillary was installed on an HPLC injection port as a sampling loop. Aqueous samples containing a variety of analytes were passed through the capillary and, during this process, the analytes were extracted by the sol-gel titania poly-THF coating on the inner surface of the capillary. Using isocratic and gradient elution with acetonitrile/water mobile phases, the extracted analytes were desorbed into the on-line coupled HPLC column for separation and UV detection. The sol-gel titania poly-THF coating was especially efficient in extracting polar analytes, such as underivatized phenols, alcohols, amines, and aromatic carboxylic acids. In addition, this coating was capable of extracting moderately polar and nonpolar analytes, such as ketones and polycyclic aromatic hydrocarbons. The sol-gel titania poly-THF coated capillary was also able to extract polypeptides at pH values near their respective isoelectric points. Extraction of these compounds can be important for environmental and biomedical applications. The observed extraction behavior can be attributed to the polar and nonpolar moieties in the poly-THF structure. This coating was found to be stable under extremely low and high pH conditions-even after 18h of exposure to 1M HCl (pH approximately 0.0) and 1M NaOH (pH approximately 14.0).

  8. Combination of capillary micellar liquid chromatography with on-chip microfluidic chemiluminescence detection for direct analysis of buspirone in human plasma.

    Science.gov (United States)

    Al Lawati, Haider A J; Kadavilpparampu, Afsal Mohammed; Suliman, FakhrEldin O

    2014-09-01

    Microfluidic based chemiluminescence (CL) detector having novel channel design for enhanced mixing has been developed and investigated in terms of its applicability with micellar mode of liquid chromatography (MLC). The newly developed detector was found to be highly sensitive and an alternative detection technique to combine with capillary MLC. This combination was successfully employed for direct detection of a model analyte using Ru(III)-peroxydisulphate CL system. The selected analyte, buspirone hydrochloride (BUS), was detected selectively at therapeutic concentration levels in human plasma without any sample pretreatment. By incorporating eight flow split units within the spiral channel of microfluidic chip, an enhancement of 140% in CL emission was observed. We also evaluated the effect of non- ionic surfactant, Brij-35, which used as mobile phase modifier in MLC, on CL emission. The CL signal was improved by 52% compared to aqueous-organic mobile phase combinations. Various parameters influencing the micellar chromatographic performance and the CL emission were optimized. This allowed highly sensitive analysis of BUS with limit of detection (LOD) of 0.27 ng mL(-1) (3σ/s) and limit of quantification (LOQ) of 0.89 ng mL(-1) (10σ/s). The analyte recovery from human plasma at three different concentration level ranges from 88% to 96% (RSD 1.9-5.3%). The direct analysis of BUS in human plasma was achieved within 6 min. Therefore, combining microfluidic CL detection with micellar mode of separation is an efficient, cost-effective and highly sensitive technique that can utilize MLC in its full capacity for various bioanalytical procedures.

  9. [Rapid determination of pesticide multiresidues in porphyra by dispersive solid-phase extraction coupled with online gel permeation chromatography-gas chromatography-mass spectrometry].

    Science.gov (United States)

    Sun, Xiaojie; Guo, Mengmeng; Wang, Suyue; Tan, Zhijun; Li, Zhaoxin; Zhai, Yuxiu

    2014-10-01

    A rapid method for the simultaneous identification and quantification of pesticide multiresidues in porphyra was developed using gel permeation chromatography (GPC) coupled to gas chromatography-mass spectrometry (GPC-GC/MS). Nineteen pesticides (organochlorines, organophosphoruses, triazines and pyrethroids) were selected as the target analytes. The pretreatment method was applied consisting of organic solvent extraction followed by dispersive solid-phase extraction with graphitized carbon black (GCB) and primary secondary amine (PSA) adsorbents. GPC was also employed online to remove the large molecules such as pigments and lipids. The quantitative analysis was carried out by external standard method using gas chromatography coupled with mass spectrometry in selective ion monitoring (SIM) mode. Moreover, a large volume of sample was allowed to be injected using the program of GPC programmed-temperature vaporizer of gas chromatography to improve the sensitivity of measurements. The results showed that the calibration curves were linear (r > 0.995) in the range of 10-1,000 μg/L for all the pesticides. The limits of detection (LODs) for the pesticides in porphyra were from 0.005 to 0.03 mg/kg, and the average recoveries were between 70% and 120%. The advantages of the method are simple, sensitive and shorter operation time for analysis of pesticide residues in porphyra samples.

  10. Dosage direct des alcools dans les carburols par chromatographie en phase gazeuse Direct Gas Chromatographie Determination of Alcohols in Gasolines Blended by Oxygenated Compounds

    Directory of Open Access Journals (Sweden)

    Petroff N.

    2006-11-01

    Full Text Available Dans cette étude, on décrit une méthode de chromatographie en phase gazeuse utilisant une colonne remplie ; elle permet de doser, sans préfractionnement, les alcools jusqu'aux butanols dans les carburols (carburants additionnés de composés oxygénés. La phase stationnaire sélectionnée est le glycérol. This report describes a gas chromatographie method using a packed column. It allows the direct determination of alcohols up to butanols in gasolines blended with oxygenated compounds without prefractionation. Glycerol has been selected as stationary phase.

  11. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle L.; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  12. ANALYSIS OF PENTACHLOROPHENOL IN WATER BY PURGE AND TRAP CONCENTRATOR COUPLED TO GAS CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    HuixiaLan; YuancaiChen; ZhonghaoChen

    2004-01-01

    It is convenient and time saving to analyze pentachlorophenol (PCP) in water by purge and trap concentrator coupled to gas chromatography that avoids employing a great deal of organic solvent. In this paper, the appropriate purge and trap conditions of PCP are determined: the trapped sorbent is TenaxGC; the purge gas is pure nitrogen and purge flow is 40ml/min; the purge time is 30min. A series of standard PCP water samples 5, 10, 50, 100, 200, 400, 800, 1000ppb are analyzed in order to obtain standard curve, and the linear regressive equation obtained is Y=109.65X-687.72, which correlation coefficient r is 0.9949. The precision of the method is determined with 0.5ppb PCP water sample, and the standard deviation measured is 3%. The detection limit for PCP is 0.2ppb.

  13. Determination of Water Content of Water-soluble Paints by Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    顾润南; 钦维民; 肖舸

    2003-01-01

    This paper describes the determination of water content of water-soluble paints by gas chromatography. The water in paints is extracted by dimethyl formamide (DMF) as a solvent.Isopropanol is used as an internal standard. The mixture is separated by low-speed centrifugation.Then a 1-uL sample of the supernatant from the prepared solution is injected into the gas chromatograph. The water content is determined by internal standard calibration curve. The rate of recovery of added standard of this method is more than 98%. Relative mean deviation is less than 3‰.The linearity of calibration curve is good and relativity coefficient is higher than 0.998.

  14. A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

    2003-01-01

    A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

  15. Determination of Free Fatty Acids and Triglycerides by Gas Chromatography Using Selective Esterification Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kail, Brian W; Link, Dirk D; Morreale, Bryan D

    2012-11-01

    A method for selectively determining both free fatty acids (FFA) and triacylglycerides (TAGs) in biological oils was investigated and optimized using gas chromatography after esterification of the target species to their corresponding fatty acid methyl esters (FAMEs). The method used acid catalyzed esterification in methanolic solutions under conditions of varying severity to achieve complete conversion of more reactive FFAs while preserving the concentration of TAGs. Complete conversion of both free acids and glycerides to corresponding FAMEs was found to require more rigorous reaction conditions involving heating to 120°C for up to 2 h. Method validation was provided using gas chromatography–flame ionization detection, gas chromatography–mass spectrometry, and liquid chromatography–mass spectrometry. The method improves on existing methods because it allows the total esterified lipid to be broken down by FAMEs contributed by FFA compared to FAMEs from both FFA and TAGs. Single and mixed-component solutions of pure fatty acids and triglycerides, as well as a sesame oil sample to simulate a complex biological oil, were used to optimize the methodologies. Key parameters that were investigated included: HCl-to-oil ratio, temperature and reaction time. Pure free fatty acids were found to esterify under reasonably mild conditions (10 min at 50°C with a 2.1:1 HCl to fatty acid ratio) with 97.6 ± 2.3% recovery as FAMEs, while triglycerides were largely unaffected under these reaction conditions. The optimized protocol demonstrated that it is possible to use esterification reactions to selectively determine the free acid content, total lipid content, and hence, glyceride content in biological oils. This protocol also allows gas chromatography analysis of FAMEs as a more ideal analyte than glyceride species in their native state.

  16. Pseudo-absolute quantitative analysis using gas chromatography - Vacuum ultraviolet spectroscopy - A tutorial.

    Science.gov (United States)

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Qiu, Changling; McNair, Harold M; Schug, Kevin A

    2017-02-08

    The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120-240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method.

  17. DETERMINATION OF PERMEATION PROPERTIES OF GAS THROUGH POLYMER MEMBRANE BY GAS CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    JIN Xigao; FU Xiucheng; ZHAN Yongjian; QIAN Renyuan

    1987-01-01

    An apparatus constructed for measuring permeation properties of polymer membranes using a mixture of gases is described. A gas chromatographic system was applied to determine the individual transport characteristics of component gases without a vacuum line. This paper also discusses some experimental factors effecting the precision of measurement. The results show that there is a linear relationship between the permeation time and the volume of the gas permeated through the membrane within certain permeation period, which depends on the permeation rate (from 10-4 to 10-7 cm3 (STP)/cm2.sec. cmHg) of the membrane. The reproducibility has been found to be good with a relative standard deviation of 3.5%. This method is more sensitive, considerably faster and more convenient for determining both the permeability coefficient and the separation factor of a polymer membrane from a chromat ogram using mixed penetrant gases.

  18. In situ search for organics by gas chromatography analysis: new derivatization / thermochemolysis approach

    Science.gov (United States)

    Geffroy, Claude; Buch, Arnaud; David, Marc; Aissat, Lyes; El Mufleh, Amel; Papot, S.; Sternberg, Robert

    Many organic molecules are present in interstellar clouds and might be carried to the early Earth by comets and meteorites during the heavy bombardment phase in the first few hundred million years of the solar system. It has been suggested that extraterrestrial organic material may well represent an important part of the organic material available for the origin of life. Until samples, brought by future space missions, are available on Earth, in situ measurements are one of the way to get unaltered and non-contaminated samples for analysis. The analytical technique has to be robust, sensitive and non-specific due to the large scope of targets molecules. The only currently flight qualified technique of analysis of organic molecules in space is gas chromatography (Viking, Cassini-Huygens, SAM-MSL, COSAC-Rosetta). The main objective of this work is to present a new approach with multi step analysis using derivatisation and thermochemolysis reagents for a one pot in situ analysis of volatile and refractory organics in surface or sub-surface samples (Mars, comets).Indeed, no single technology enables to identify all organic compounds because naturally occurring molecules have different polarities, molecular weights, being extractible or recalcitrant, bonded trapped or adsorbed on minerals. Thus, we propose to wider the scope of chemical reagent already validated for in situ wet chemistry such as MTBSTFA (Rodier et al. 2001, 2002), DMF-DMA (Rodier et al. 2002), or TMAH (Rodier et al, 2005, Geffroy-Rodier et al; 2009) to analyze enantiomers of amino acids, carbohydrates and lipids in a one pot several steps sub system using a multi reagent and multi step approach. Thus using a new derivatizing agent, we successfully identified twenty one amino acids including twelve of the twenty proteinic amino acids without inhibiting following multi step thermochemolysis. *Geffroy-Rodier C, Grasset L, Sternberg R. Buch A. Amblès A. (2009) Thermochemolysis in search for organics in

  19. Comprehensive two-dimensional gas chromatography for characterizing mineral oils in foods and distinguishing them from synthetic hydrocarbons.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2015-01-02

    Many foods are contaminated by hydrocarbons of mineral oil or synthetic origin. High performance liquid chromatography on-line coupled with gas chromatography and flame ionization detection (HPLC-GC-FID) is a powerful tool for the quantitative determination, but it would often be desirable to obtain more information about the type of hydrocarbons in order to identify the source of the contamination and specify pertinent legislation. Comprehensive two-dimensional gas chromatography (GC×GC) is shown to produce plots distinguishing mineral oil saturated hydrocarbons (MOSH) from polymer oligomeric saturated hydrocarbons (POSH) and characterizing the degree of raffination of a mineral oil. The first dimension separation occurred on a phenyl methyl polysiloxane, the second on a dimethyl polysiloxane. Mass spectrometry (MS) was used for identification, FID for quantitative determination. This shows the substantial advances in chromatography to characterize complex hydrocarbon mixtures even as contaminants in food.

  20. Determination of toxaphene enantiomers by comprehensive two-dimensional gas chromatography with electron-capture detection.

    Science.gov (United States)

    Bordajandi, Luisa R; Ramos, Lourdes; González, María José

    2006-09-01

    Comprehensive two-dimensional gas chromatography with micro electron-capture detection (GC x GC-microECD) has been evaluated for the enantioseparation of five chiral toxaphenes typically found in real-life samples (Parlar 26, 32, 40, 44 and 50). From the two enantioselective beta-cyclodextrin-based columns evaluated as first dimension column, BGB-176SE and BGB-172, the latter provided the best results and was further combined with three non-enantioselective columns in the second dimension: HT-8, BPX-50 and Supelcowax-10. The combination BGB-172 x BPX-50 was finally selected because it provided a complete separation among all enantiomers. A satisfactory repeatability and reproducibility of the retention times in both the first and the second dimension were observed for all target compounds (RSDs below 0.8%, n = 4). Linear responses in the tested range of 10-200 pg/microl and limits of detection in the range of 2-6 pg/microl were obtained. The repeatability and reproducibility at a concentration of 100 pg/microl, evaluated as the RSDs calculated for the enantiomeric fraction (EF), was better than 11% (n = 4) in all instances. The feasibility of the method developed for real-life analyses was illustrated by the determination of the enantiomeric ratios and concentration levels of the test compounds in four commercial fish oil samples. These results were compared to those obtained by heart-cut multidimensional gas chromatography using the same enantioselective column.

  1. Separation of cis- and trans-Asarone from Acorus tatarinowii by Preparative Gas Chromatography

    Directory of Open Access Journals (Sweden)

    H. L. Zuo

    2012-01-01

    Full Text Available A preparative gas chromatography (pGC method was developed for the separation of isomers (cis- and trans-asarone from essential oil of Acorus tatarinowii. The oil was primarily fractionated by silica gel chromatography using different ratios of petroleum ether and ethyl acetate as gradient elution solvents. And then the fraction that contains mixture of the isomers was further separated by pGC. The compounds were separated on a stainless steel column packed with 10% OV-101 (3 m × 6 mm, i.d., and then the effluent was split into two gas flows. One percent of the effluent passed to the flame ionization detector (FID for detection and the remaining 99% was directed to the fraction collector. Two isomers were collected after 90 single injections (5 uL with the yield of 178 mg and 82 mg, respectively. Furthermore, the structures of the obtained compounds were identified as cis- and trans-asarone by 1H- and 13C-NMR spectra, respectively.

  2. [Determination of residual glycol ethers in leather and leather products by gas chromatography/mass spectrometry].

    Science.gov (United States)

    Wang, Ghengyun; Zhang, Weiya; Li, Lixia; Shen, Yalei; Lin, Junfeng; Xie, Tangtang; Chu, Naiqing

    2014-08-01

    An effective method was established for the simultaneous determination of residual glycol ethers in leather and leather products by gas chromatography/mass spectrometry. Glycol ethers in leather and leather products were ultrasonically extracted at 45 °C, using ethyl acetate as the extraction solvent. The extracts were purified by solid phase extraction (SPE) columns, and then analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode. The content of each analyte was calibrated by external standard method. The limit of detection of ethylene glycol ethyl ether (EGEE) was 0. 10 mg/kg under the condition of signal to noise (S/N) of 3 and the limits of the other 11 glycol ethers were all less than 0.05 mg/kg. The spiked recoveries varied from 81. 2% to 95. 5% at three different spiked levels with the relative standard deviations (RSDs) ranged from 1.4% to 6. 6%. The proposed method is simple, rapid and accurate, with the limits of detection much less than the requirements of the Regulation Concerning Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) of European Union. It is applicable to the determination of residual glycol ethers in leather and leather products, and provides a reference for the relevant testing standards.

  3. Method Development and Validation for Determining 1,3-Butadiene in Human Blood by Gas Chromatography-Mass Spectrometry and Head-Space Gas Chromatography%Method Development and Validation for Determining1,3-Butadiene in Human Blood by Gas Chromatography-Mass Spectrometry and Head-Space Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    ZHANG Su-jing; SHEN Bao-hua; ZHUO Xian-yi

    2013-01-01

    To develop a simple,validated method for identifying and quantifying 1,3-butadiene (BD) in human blood by gas chromatography-mass spectrometry (GC-MS) and head-space gas chromatography (HS-GC).BD was identified by GC-MS and HS-GC,and quantified by HS-GC.The method showed that BD had a good linearity from 50 to 500 μg/mL (r>0.99).The limits of detection and quantification were 10 μg/mL and 50 μg/mL,respectively.Both the intra-day precision and inter-day precision were <6.08%,and the accuracy was 96.98%-103.81%.The method was applied to an actual case,and the concentration of BD in the case was 242 μg/mL in human blood.This simple method is found to be useful for the routine forensic analysis of acute exposure to BD.

  4. Quantification of residual solvents in antibody drug conjugates using gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Medley, Colin D., E-mail: medley.colin@gene.com [Genentech Inc., Small Molecule Pharmaceutical Sciences, 1 DNA Way, South San Francisco, CA 94080 (United States); Kay, Jacob [Research Pharmaceutical Services, 520 Virginia Dr. Fort, Washington, PA (United States); Li, Yi; Gruenhagen, Jason; Yehl, Peter; Chetwyn, Nik P. [Genentech Inc., Small Molecule Pharmaceutical Sciences, 1 DNA Way, South San Francisco, CA 94080 (United States)

    2014-11-19

    Highlights: • Sensitive residual solvents detection in ADCs. • 125 ppm QL for common conjugation solvents. • Generic and validatable method. - Abstract: The detection and quantification of residual solvents present in clinical and commercial pharmaceutical products is necessary from both patient safety and regulatory perspectives. Head-space gas chromatography is routinely used for quantitation of residual solvents for small molecule APIs produced through synthetic processes; however residual solvent analysis is generally not needed for protein based pharmaceuticals produced through cultured cell lines where solvents are not introduced. In contrast, antibody drug conjugates and other protein conjugates where a drug or other molecule is covalently bound to a protein typically use solvents such as N,N-dimethylacetamide (DMA), N,N‑dimethylformamide (DMF), dimethyl sulfoxide (DMSO), or propylene glycol (PG) to dissolve the hydrophobic small molecule drug for conjugation to the protein. The levels of the solvent remaining following the conjugation step are therefore important to patient safety as these parental drug products are introduced directly into the patients bloodstream. We have developed a rapid sample preparation followed by a gas chromatography separation for the detection and quantification of several solvents typically used in these conjugation reactions. This generic method has been validated and can be easily implemented for use in quality control testing for clinical or commercial bioconjugated products.

  5. Method for determination of methyl tert-butyl ether in gasoline by gas chromatography.

    Science.gov (United States)

    Achten, C; Püttmann, W

    2001-03-02

    A simple method for the determination of methyl tert-butyl ether (MTBE) in gasoline has been developed. The separation of MTBE from other analytes was controlled by the use of gas chromatography-mass spectrometry in the full scan mode using the characteristic primary, secondary and tertiary ions m/z 73, 57 and 43. The sample mass spectrum did not show any superimposition of other analytes. The separation from the common gasoline component 2-methylpentane was sufficient for reliable quantitation. An application of the developed conditions using gas chromatography with flame ionization detection was performed by the analysis of regular, euro super, super premium unleaded and 'Optimax' gasoline from petrol stations in the area of Frankfurt/Main, Germany. Regular unleaded gasoline shows an average MTBE content of 0.4% (w/w), whereas the MTBE content in euro super gasoline varies between 0.4 and 4.2% (w/w). The blending of MTBE to super premium has increased from 8.2% (w/w) in 1998 to 9.8% (w/w) on average in 1999. The recently introduced gasoline 'Optimax' shows an average MTBE content of 11.9% (w/w). The presented method might also be used for the analysis of other ethers, such as ethyl tert-butyl ether, which requires the use of another internal standard.

  6. Determination of endogenous ethanol in blood and breath by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jones, A W; Mårdh, G; Anggård, E

    1983-01-01

    We describe methods for the determination of endogenous ethanol in biological specimens from healthy abstaining subjects. The analytical methods were headspace gas chromatography (GC) for plasma samples and gas chromatography-mass spectometry (GC/MS) with deuterium labelled species 2H3-ethanol and 2H5-ethanol as internal standards for breath analysis. Ethanol in rebreathed air was about 10% higher than in directly analysed end-expired alveolar air. Known volumes of rebreathed air were passed through a liquid-N2 freeze trap and the volatile constituents of breath were concentrated prior to analysis by GC or GC/MS. Besides endogenous ethanol, peaks were seen on the chromatograms for methanol, acetone and acetaldehyde as well as several as yet unidentified substances. The endogenous alcohols ethanol and methanol were confirmed from their mass chromatograms and the GC/MS profile also indicated the presence of endogenous propan-1-ol. The concentration of endogenous ethanol in plasma showed wide inter-subject variations ranging from below detection limits to 1.6 micrograms/ml (34.8 mumol/l) and with mean +/- SD of 0.39 +/- 0.45 micrograms/ml (8.5 +/- 9.8 mumol/l). We aim to characterise further the role of endogenous ethanol with the main focus on dynamic aspects such as the rate of formation and turnover.

  7. Water Determination in Solid Pharmaceutical Products Utilizing Ionic Liquids and Headspace Gas Chromatography.

    Science.gov (United States)

    Frink, Lillian A; Armstrong, Daniel W

    2016-08-01

    A rapid, accurate, and precise headspace gas chromatographic (HSGC) analytical method was developed for the detection and quantification of water in drug products. The analysis is able to be performed in 10 min and automated. The HSGC method used an ionic liquid (IL) based open tubular capillary gas chromatographic column to increase the ruggedness of this method and provide improved peak shapes for water. Due to the ionic liquids low vapor pressure, unique physiochemical properties, and high thermal stability, they also make idea solvents for HSGC. Unlike Karl Fischer titration methods, this HSGC method is not affected by side reactions. The developed method was shown to be broadly applicable. The water content in 12 different samples was found to range from 1%-7% water. The use of HSGC was highly sensitive and only required 10 mg of sample. In addition, it was found to have greater precision and accuracy than Karl Fischer titration and greater precision and speed than loss on drying.

  8. Simultaneous assessment of cholesterol absorption and synthesis in humans using on-line gas chromatography/ combustion and gas chromatography/pyrolysis/isotope-ratio mass spectrometry.

    Science.gov (United States)

    Gremaud, G; Piguet, C; Baumgartner, M; Pouteau, E; Decarli, B; Berger, A; Fay, L B

    2001-01-01

    A number of dietary components and drugs are known to inhibit the absorption of dietary and biliary cholesterol, but at the same time can compensate by increasing cholesterol synthesis. It is, therefore, necessary to have a convenient and accurate method to assess both parameters simultaneously. Hence, we validated such a method in humans using on-line gas chromatography(GC)/combustion and GC/pyrolysis/isotope-ratio mass spectrometry (IRMS). Cholesterol absorption was measured using the ratio of [(13)C]cholesterol (injected intravenously) to [(18)O]cholesterol (administered orally). Simultaneously, cholesterol synthesis was measured using the deuterium incorporation method. Our methodology was applied to 12 mildly hypercholesterolemic men that were given a diet providing 2685 +/- 178 Kcal/day (mean +/- SD) and 255 +/- 8 mg cholesterol per day. Cholesterol fractional synthesis rates ranged from 5.0 to 10.5% pool/day and averaged 7.36% +/- 1.78% pool/day (668 +/- 133 mg/day). Cholesterol absorption ranged from 36.5-79.9% with an average value of 50.8 +/- 15.4%. These values are in agreement with already known data obtained with mildly hypercholesterolemic Caucasian males placed on a diet similar to the one used for this study. However, our combined IRMS method has the advantage over existing methods that it enables simultaneous measurement of cholesterol absorption and synthesis in humans, and is therefore an important research tool for studying the impact of dietary treatments on cholesterol parameters.

  9. Capillary sample

    Science.gov (United States)

    ... several times a day using capillary blood sampling. Disadvantages to capillary blood sampling include: Only a limited ... do not constitute endorsements of those other sites. Copyright 1997-2017, A.D.A.M., Inc. Duplication ...

  10. Purge efficiency in the determination of trihalomethanes in water by purge-and-trap gas chromatography.

    Science.gov (United States)

    Ruiz-Bevia, Francisco; Fernandez-Torres, Maria J; Blasco-Alemany, Maria P

    2009-01-26

    Purge-and-trap gas chromatography-mass spectrometry (PT-GC-MS) has become an accepted method for the analysis of trihalomethanes (THMs) in water. The purge-and-trap technique is based on an efficient transfer of volatile organic compounds from the liquid (contained in the purge chamber) to the gaseous phase by bubbling with an inert gas. The aim of this work was to study the purge system's efficiency by means of several consecutive purge cycles lasting 11 min each of the same liquid sample. The concentration range chosen of THMs was very wide [5-200 microg L(-1)]. The inert gas flow rate was 40 mL min(-1), and experiments were performed at temperatures of 25, 35 and 50 degrees C. Bromoform (CHBr(3)), the least volatile compound, needed 19 cycles to be purged quantitatively at a concentration of 200 microg L(-1) and only 7 cycles at 5 microg L(-1) for a 25 mL sample at 25 degrees C. Chloroform (CHCl(3)), the most volatile compound, required 4 cycles to be fully extracted at 200 microg L(-1) and 2 at 5 microg L(-1). Finally, Novak's theoretical model, based on the distribution constant between gas and liquid phases, was used to correlate the THMs purging extraction data.

  11. Aroma characterization of chinese rice wine by gas chromatography-olfactometry, chemical quantitative analysis, and aroma reconstitution.

    Science.gov (United States)

    Chen, Shuang; Xu, Yan; Qian, Michael C

    2013-11-27

    The aroma profile of Chinese rice wine was investigated in this study. The volatile compounds in a traditional Chinese rice wine were extracted using Lichrolut EN and further separated by silica gel normal phase chromatography. Seventy-three aroma-active compounds were identified by gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). In addition to acids, esters, and alcohols, benzaldehyde, vanillin, geosmin, and γ-nonalactone were identified to be potentially important to Chinse rice wine. The concentration of these aroma-active compounds in the Chinese rice wine was further quantitated by combination of four different methods, including headsapce-gas chromatography, solid phase microextraction-gas chromatography (SPME)-GC-MS, solid-phase extraction-GC-MS, and SPME-GC-pulsed flame photometric detection (PFPD). Quantitative results showed that 34 aroma compounds were at concentrations higher than their corresponding odor thresholds. On the basis of the odor activity values (OAVs), vanillin, dimethyl trisulfide, β-phenylethyl alcohol, guaiacol, geosmin, and benzaldehyde could be responsible for the unique aroma of Chinese rice wine. An aroma reconstitution model prepared by mixing 34 aroma compounds with OAVs > 1 in an odorless Chinese rice wine matrix showed a good similarity to the aroma of the original Chinese rice wine.

  12. The use of gas chromatography/matrix isolation infrared spectroscopy (GC/MIIR) and supercritical fluid chromatography (SFC) for waste characterization

    Energy Technology Data Exchange (ETDEWEB)

    Raphaelian, L.A.; Green, D.W.

    1987-01-01

    In processes involving coal and other fossil fuels, wastes are generated that are normally biologically or chemically treated before disposal. To assist in determining the best treatment for obtaining material suitable for disposal, a knowledge of the chemical composition of the wastes is required. Typically, these wastes contain a complex mixture of organic compounds. One objective of this project is to enhance the capabilities of analyzing complex mixtures by using gas chromatography/matrix isolation infrared spectroscopy. The second objective is to simplify the mixtures found in solid wastes into less complex mixtures so that a better separation can be made by the gas chromatograph portion of GC/MS and GC/MIIR. The technique used for this is supercritical fluid chromatography.

  13. Analysis of the venom of the Sydney funnel-web spider, Atrax robustus using gas chromatography mass spectrometry.

    Science.gov (United States)

    Duffield, P H; Duffield, A M; Carroll, P R; Morgans, D

    1979-03-01

    Thirteen compounds have been identified using gas chromatography mass spectrometry in the venom of the Sydney funnel-web spider, Atrax robustus. The compounds were identified as their trimethylsilyl or pentafluoropropionate derivatives and were citric acid, lactic acid, phosphoric acid, glycerol, urea, glucose, gamma-aminobutyric acid, glycine, spermidine, spermine, tyramine and octopamine. Female venom contained trace quantities of 5-methyoxytryptamine which was not detected in male venom. Quantitative determination of tyramine and octopamine was achieved using chemical ionization (CH4) gas chromatography mass spectrometry and deuterated internal standards.

  14. Rapid tandem-column micro-gas chromatography based on optofluidic ring resonators with multi-point on-column detection.

    Science.gov (United States)

    Sun, Yuze; Liu, Jing; Howard, Daniel J; Frye-Mason, Greg; Thompson, Aaron K; Ja, Shiou-jyh; Fan, Xudong

    2010-01-01

    We demonstrated a novel tandem-column micro-gas chromatography (microGC) based on optofluidic ring resonator (OFRR). The OFRR is a thin-walled fused silica capillary whose interior surface is coated with a polymeric stationary phase. The circular cross section of the OFRR forms the micro-ring resonator and supports whispering gallery modes (WGMs). Via tapered optical fibers in contact with the OFRR, the WGM can be excited externally at any positions along the OFRR capillary, thus enabling multi-point, on-column, real-time detection of vapor molecules flowing through the OFRR. In the present OFRR-based tandem-column-based microGC implementation, a 180 cm long conventional GC column coated with a nonpolar stationary phase was followed by a relatively short OFRR column coated with a polar phase. Two detection positions, one at the inlet of the OFRR and the other a few centimeters downstream, were used to monitor the separation achieved by the first and the second column, respectively. Owing to the multi-point on-column detection that provides complementary retention time information on each chemical compound, co-eluted analytes can be well separated and identified on at least one detection channel and no modulation is needed at the interface of tandem columns. Separation and detection of twelve analytes with various volatilities and polarities within four minutes were demonstrated. In addition, the chromatograms obtained from three different locations along the OFRR column demonstrated the system's capability of on-column monitoring of the separation process for the target analyte in a vapor mixture. Our results will lead to the development of a rapid, simple, and portable microGC system with significantly improved selectivity and chemical identification capabilities.

  15. Detailed analysis of petroleum cuts by multidimensional gas chromatography; Analyse detaillee de coupes petrolieres par chromatographie en phase gazeuse multidimensionnelle

    Energy Technology Data Exchange (ETDEWEB)

    Vendeuvre, C.

    2006-01-15

    The limitations of petroleum resources implying a better valorisation of crude oil through the optimisation of production, refinery and petrochemistry processes, as well as the environmental regulations have strengthened the necessity of more detailed characterisation of petroleum products. In order to take up this challenge, efficient analytical tools have to be developed. This work demonstrates that comprehensive two-dimensional gas chromatography (GCxGC) constitutes a major advance compared to GC owing to its improved resolution power and to the structured chromatograms indicating the polarity and the volatility of hydrocarbons. The principle of GCxGC is based on the analysis of a whole sample in two independent dimensions of separation achieved using two GC columns of different selectivities; between the two columns a modulator device samples, focuses and re-injects small portions of the effluent from the first column into the second one. Since its introduction in 1991, GCxGC has known a rapid growth and has received a wide acceptance by the analytical science community. The competitive situation has considerably evolved during this thesis with the introduction of commercial systems and the two first sessions of an international symposium dedicated to this technique (Volendam, 2003 and Atlanta, 2004). The key points of the thesis concern the development of a GCxGC prototype system using dual jets CO{sub 2} technology and a data processing program; the evaluation of a retention model allowing a rational choice of operating conditions; and the application of this technique to various and complex issues. Thus, effluents from petrochemistry, refinery or pollution areas have been analysed according to the chemical classes of hydrocarbons and to their number of carbon atoms; a new method for obtaining distillation curves for each chemical group was also presented. Furthermore, the hyphenation of GCxGC with a specific sulphur detector revealed a great interest for

  16. Gas chromatographic separation of fatty acid esters of cholesterol and phytosterols on an ionic liquid capillary column.

    Science.gov (United States)

    Hammann, Simon; Vetter, Walter

    2015-12-15

    Steryl esters are high molecular weight compounds (600-700g/mol) regularly present as a minor lipid class in animal and plant lipids. Different sterol backbones (e.g., cholesterol, β-sitosterol and brassicasterol) which can be esterified with various fatty acids can result in highly complex steryl ester patterns in food samples. The gas chromatographic (GC) analysis of intact steryl esters is challenging, since high elution temperatures are required for their elution. On nonpolar GC phases, steryl esters with fatty acids with differing degree of unsaturation (e.g., oleate and linoleate) cannot be separated and there are only few polar columns available with sufficient temperature stability. In this study, we used gas chromatography with mass spectrometry (GC/MS) and analyzed intact steryl esters on a commercial room temperature ionic liquid (RTIL) column which was shortened to a length of 12m. The column separated the steryl esters both by total carbon number and by degree of unsaturation of the fatty acid. For instance, cholesteryl esters with stearic acid (18:0), oleic acid (18:1n-9), linoleic acid (18:2n-6) and α-linolenic acid (18:3n-3) could be resolved (R≥1.3) from each other. By analysis of synthesized standard substances, the elution orders for different steryl backbones and different fatty acids on a given sterol backbone could be determined. Analysis of spreads and plant oils allowed to determine retention times for 37 steryl esters, although a few co-elutions were observed. The ionic liquid column proved to be well-suited for the analysis of intact steryl esters.

  17. Quantification of Triacylglycerol Molecular Species in Edible Fats and Oils by Gas Chromatography-Flame Ionization Detector Using Correction Factors.

    Science.gov (United States)

    Yoshinaga, Kazuaki; Obi, Junji; Nagai, Toshiharu; Iioka, Hiroyuki; Yoshida, Akihiko; Beppu, Fumiaki; Gotoh, Naohiro

    2017-03-01

    In the present study, the resolution parameters and correction factors (CFs) of triacylglycerol (TAG) standards were estimated by gas chromatography-flame ionization detector (GC-FID) to achieve the precise quantification of the TAG composition in edible fats and oils. Forty seven TAG standards comprising capric acid, lauric acid, myristic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, stearic acid, oleic acid, linoleic acid, and/or linolenic acid were analyzed, and the CFs of these TAGs were obtained against tripentadecanoyl glycerol as the internal standard. The capillary column was Ultra ALLOY(+)-65 (30 m × 0.25 mm i.d., 0.10 μm thickness) and the column temperature was programmed to rise from 250°C to 360°C at 4°C/min and then hold for 25 min. The limit of detection (LOD) and limit of quantification (LOQ) values of the TAG standards were > 0.10 mg and > 0.32 mg per 100 mg fat and oil, respectively, except for LnLnLn, and the LOD and LOQ values of LnLnLn were 0.55 mg and 1.84 mg per 100 mg fat and oil, respectively. The CFs of TAG standards decreased with increasing total acyl carbon number and degree of desaturation of TAG molecules. Also, there were no remarkable differences in the CFs between TAG positional isomers such as 1-palmitoyl-2-oleoyl-3-stearoyl-rac-glycerol, 1-stearoyl-2-palmitoyl-3-oleoyl-rac-glycerol, and 1-palmitoyl-2-stearoyl-3-oleoyl-rac-glycerol, which cannot be separated by GC-FID. Furthermore, this method was able to predict the CFs of heterogeneous (AAB- and ABC-type) TAGs from the CFs of homogenous (AAA-, BBB-, and CCC-type) TAGs. In addition, the TAG composition in cocoa butter, palm oil, and canola oil was determined using CFs, and the results were found to be in good agreement with those reported in the literature. Therefore, the GC-FID method using CFs can be successfully used for the quantification of TAG molecular species in natural fats and oils.

  18. Online capillary solid-phase microextraction coupled liquid chromatography-mass spectrometry for analysis of chiral secondary alcohol products in yeast catalyzed stereoselective reduction cell culture.

    Science.gov (United States)

    Cheng, Cheanyeh; Nian, Yu-Chuan

    2015-02-06

    An online solid-phase microextraction coupled liquid chromatography-electrospray ionization-ion trap mass spectrometry was developed for the analysis of trace R- and S-4-phenyl-2-butanol (R- and S-pbol) in salt rich cell culture of Saccharomyces cerevisiae catalyzed stereoselective reduction of 4-pheny-2-butanone (pbone). A Supel-Q PLOT capillary column was used for the extraction and deionized distilled water was used as the extraction mobile phase. The extraction flow rate and extraction time were at 0.1 mL min(-1) and 0.95 min, respectively. The three target analytes, pbone, R-pbol, and S-4-pbol, were desorbed and eluted by the mobile phase of water/methanol/isopropanol (55/25/20, v/v/v) with a flow rate of 0.5 mL min(-1) and analyzed by a chiral column. The mass spectrometric detection of the three target analytes was in positive ion mode with the signal [M+Na](+). The matrix-matched external standard calibration curves with linear concentration range between 0 and 50 μg mL(-1) were used for quantitative analysis. The linear regression correlation coefficients (r(2)) of the standard calibration curves were between 0.9950 and 0.9961. The yeast mediated reduction was performed with a recation culture of yeast incubation culture/glycerol (70/30, v/v) for 4 days. This biotransformation possessed 82.3% yield and 92.9% S-enantomeric excess. The limit of detection (LOD)/limit of quantification (LOQ) for pbone, R-pbol, and S-pbol was 0.02/0.067, 0.01/0.033, and 0.01/0.033 μg mL(-1), respectively. The intra-day and inter-day precisions from repeated measurements were 10.8-21.1% and 11.6-18.7%, respectively. The analysis accuracy from spike recovery was 84-91%.

  19. Temperature-assisted on-column solute focusing: a general method to reduce pre-column dispersion in capillary high performance liquid chromatography.

    Science.gov (United States)

    Groskreutz, Stephen R; Weber, Stephen G

    2014-08-01

    Solvent-based on-column focusing is a powerful and well known approach for reducing the impact of pre-column dispersion in liquid chromatography. Here we describe an orthogonal temperature-based approach to focusing called temperature-assisted on-column solute focusing (TASF). TASF is founded on the same principles as the more commonly used solvent-based method wherein transient conditions are created that lead to high solute retention at the column inlet. Combining the low thermal mass of capillary columns and the temperature dependence of solute retention TASF is used effectively to compress injection bands at the head of the column through the transient reduction in column temperature to 5°C for a defined 7mm segment of a 6cm long 150μm I.D. column. Following the 30s focusing time, the column temperature is increased rapidly to the separation temperature of 60°C releasing the focused band of analytes. We developed a model to simulate TASF separations based on solute retention enthalpies, focusing temperature, focusing time, and column parameters. This model guides the systematic study of the influence of sample injection volume on column performance. All samples have solvent compositions matching the mobile phase. Over the 45-1050nL injection volume range evaluated, TASF reduces the peak width for all solutes with k' greater than or equal to 2.5, relative to controls. Peak widths resulting from injection volumes up to 1.3 times the column fluid volume with TASF are less than 5% larger than peak widths from a 45nL injection without TASF (0.07 times the column liquid volume). The TASF approach reduced concentration detection limits by a factor of 12.5 relative to a small volume injection for low concentration samples. TASF is orthogonal to the solvent focusing method. Thus, it can be used where on-column focusing is required, but where implementation of solvent-based focusing is difficult.

  20. 阳离子交换毛细管整体柱的制备及其在毛细管离子色谱中的应用%Preparation and Application of Cation-exchange Capillary Monolithic Column in Capillary Ion Chromatography

    Institute of Scientific and Technical Information of China (English)

    李晶; 朱岩

    2013-01-01

    Polymer-based cation exchange capillary monolithic column was prepared for capillary ion chromatography (CIC) by radical polymerization in a 320-μm-i. d. fused-silica capillary tube, taking glycidyl methacrylate ( GMA ) as the functional monomer, ethylene dimethacrylate ( EDMA) as the cross-linking agent and in the presence of 1 ,4-butanediol, 1-propanol and water as the porogen solvents and azobisisobutyronitrile (AIBN) as a suitable initiator. Introduction of cation exchange sites was achieved by reacting with Na2SO3. Coupled with the prepared cation exchange capillary monolithic column, a capillary ion chromatography system was constructed with a pump (in μL/min level) , a capillary detection cell and a UV detector, on which more chromatographic characteristics were further studied. With the CIC system, 9 common univalent and divalent cations (Li+ , Na+ , NH4+ , K+ , Cs+ , Mg2+, Ca2+ , Sr2+, Ba2+) were successfully separated and determined by flow rate gradient. Another interesting separation of cations and melamine was also tested on the prepared column.%以甲基丙烯酸缩水甘油酯(GMA)为功能单体,亚乙基二甲基丙烯酸酯(EDMA)为交联剂,偶氮二异丁腈(AIBN)为自由基引发剂,在三元致孔剂(正丙醇,1,4-丁二醇,水)的存在下,在320μm内径的弹性石英毛细管柱内制备得到带有环氧功能基团的聚合物整体柱基质;利用Na2SO3对其改性,制备得到磺酸基型阳离子交换毛细管整体柱.采用微流泵、毛细管检测池和紫外检测器构建了毛细管离子色谱系统,并对所制备的整体柱的流体力学参数、色谱性能参数进行评价;采用流速梯度洗脱的方式实现9种常见阳离子(Li+,Na+,NH4+,K+,Cs+,Mg2+,Ca2+,Sr2+,Ba2+)的分离分析;此色谱系统还可应用于牛奶中阳离子和三聚氰胺的分离检测.