Sample records for gas-liquid chromatography analysis

  1. Gas-liquid chromatography in lunar organic analysis.

    NASA Technical Reports Server (NTRS)

    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.

  2. Analysis of chemically synthesized oleoylethanolamide by gas–liquid chromatography

    Microsoft Academic Search

    Clémentine Thabuis; Delphine Tissot-Favre; Jean-Baptiste Bezelgues; Jean-Charles Martin; Cristina Cruz-Hernandez; Fabiola Dionisi; Frédéric Destaillats

    2008-01-01

    Oleoylethanolamide (OEA) is known to potentially have beneficial biological effects on weight management by controlling food intake and activating lipid catabolism. In biological fluids, OEA and other endogenously biosynthesized fatty acid ethanolamides are usually analyzed by liquid chromatography–mass spectrometry (LC–MS). The present study provides analytical method to routinely assess the quality of OEA prepared for biological studies by gas–liquid chromatography

  3. Quantitative Fatty Acid Analysis of Milk Fat by Gas-Liquid Chromatography

    Microsoft Academic Search

    L. M. Smith

    1961-01-01

    A procedure was developed for quantitative analysis of the fatty acids of milk fat. Methyl esters of the acids were prepared by methanolysis, extracted with ethyl chloride, and separated by gas-liquid chromatography (GLC), with diethylene glycol succinate as liquid phase. Known mixtures of methyl esters were used in determining factors for correction of peak areas for losses from evaporation of

  4. Quantitative fatty acid analysis of vegetable oils by gas-liquid chromatography

    Microsoft Academic Search

    B. M. Craig; N. L. Murty

    1959-01-01

    Summary  The fatty acid composition of a number of vegetable oils and of two synthetic mixtures of methyl esters are compared by gas-liquid\\u000a chromatography and by standard methods. The calculated iodine values from G.L.P.C. results are in good agreement with measured\\u000a iodine values and are indicative of the reliability of the G.L.P.C. values. Standard methods gave lower values for linoleic\\u000a acid

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

    ERIC Educational Resources Information Center

    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)

  6. The identification and quantitative analysis of abscisic acid in plant extracts by gas-liquid chromatography

    Microsoft Academic Search

    J. R. Lenton; V. M. Perry; P. F. Saunders

    1971-01-01

    New techniques are described which permit the quantitative analysis of microgram quantities of abscisic acid in plant extracts by gas chromatography. Presumptive methyl abscisate peaks on gas chromatograms are positively identified by photosensitised isomerisation to methyl 2-trans-abscisate. Losses of abscisic acid during pre-purification are corrected by using 2-trans-abscisic acid as an internal standard.

  7. Application of gas-liquid chromatography to the analysis of essential oils. Part XVII. Fingerprinting of essential oils by temperature-programmed gas-liquid chromatography using capillary columns with non-polar stationary phases. Analytical methods committee.

    PubMed

    1997-10-01

    Problems in obtaining reproducible results when 'fingerprinting' essential oils by temperature-programmed gas-liquid chromatography have been reported on in Parts VII and VIII of this series. Those reports were concerned with the general problems and the use of packed columns. This report is concerned with the use of capillary columns and non-polar stationary phases. A collaborative study using capillary columns with non-polar stationary phases has resulted in a method which specifies the 'g-pack value' of a column and gives reproducible relative retention indices for the test compounds limonene, acetophenone, linalol, naphthalene, linalyl acetate and cinnamyl alcohol. The method has been applied successfully to the examination of oil of rosemary. A recommended method is given for the reproducible temperature-programmed gas-liquid chromatographic fingerprinting of essential oils using capillary columns with non-polar stationary phases. PMID:9463975

  8. Analysis of fats and oils by gas-liquid chromatography and by ultraviolet spectrophotometry

    Microsoft Academic Search

    S. F. Herb; Paul Magidman; R. W. Riemenschneider

    1960-01-01

    Summary  \\u000a \\u000a \\u000a \\u000a 1. \\u000a \\u000a Known mixtures of pure fatty acid methyl esters and a number of fats and oils as their methyl esters have been analyzed by\\u000a conventional GLC with thermal conductivity detectors.\\u000a \\u000a \\u000a \\u000a \\u000a 2. \\u000a \\u000a Percentage of fatty acid distribution determined by GLC agreed well with known percentages in model mixtures and with analysis\\u000a by the spectrophotometric method for fats and oils.\\u000a \\u000a \\u000a \\u000a \\u000a 3. 

  9. Occurrence of mixtures of geometrical isomers of conjugated octadecatrienoic acids in some seed oils: Analysis by open-tubular gas liquid chromatography and high performance liquid chromatography

    Microsoft Academic Search

    Toru Takagi; Yutaka Itabashi

    1981-01-01

    Analytical methods to obtain the detailed compositions of the fatty acids in oils containing more than one conjugated octadecatrienoic\\u000a acid by open-tubular gas liquid chromatography (GLC) and by reversed-phase high performance liquid chromatography (HPLC) were\\u000a established. Effective GLC separations ofcis,trans,trans-9,11,13-octadecatrienoic acid (ctt-9,11,13–18?3),ctc-9,11,13–18?3,ttc-9,11,13–18?3,ttt-9,11,13–18?3,ttc-8,10,12–18?3, andttt-8,10,12–18?3 were obtained with an opentubular column coated with the nonpolar liquid phase OV-1 using an instrument having

  10. Gas-liquid chromatographic analysis of cyclopropenoid fatty acids

    Microsoft Academic Search

    E. L. Schneider; Sook P. Loke; D. T. Hopkins

    1968-01-01

    A method is described for the analysis of cyclopropenoid fatty acids in oils. The method consists of reacting the methyl esters\\u000a of the cyclopropenoid fatty acids with silver nitrate in methanol to form ether and ketone derivatives. The derivatives formed\\u000a from the cyclopropenoid fatty acids are separated from the methyl esters of the normal fatty acids by gas-liquid chromatography\\u000a on

  11. Detection of Griseofulvin and Dechlorogriseofulvin by Thin-Layer Chromatography and Gas-Liquid Chromatography

    PubMed Central

    Cole, R. J.; Kirksey, J. W.; Holaday, C. E.

    1970-01-01

    A rapid and accurate method is described for the determination of griseofulvin and dechlorogriseofulvin extracted from Penicillium urticae with chloroform. Thinlayer chromatography was used to tentatively identify griseofulvin or dechlorogriseofulvin, or both. Two gas-liquid chromatographic systems provided additional qualitative information and simultaneous quantitation of the individual compounds. PMID:5415206

  12. Identification of polychlorinated styrene compounds in heron tissues by gas-liquid chromatography-mass spectrometry.

    PubMed

    Reichel, W L; Prouty, R M; Gay, M L

    1977-01-01

    Unknown compounds detected in Ardea herodias tissues are identified by gas-liquid chromatography-mass spectrometry as residues of octachlorostyrene. Heptachlorostyrene and hexachlorostyrene were tentatively identified. PMID:833106

  13. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory Instruments § 862.2250 Gas liquid chromatography...

  14. Preparation of pure microbiological samples for pyrolysis gas-liquid chromatography studies

    NASA Technical Reports Server (NTRS)

    Oxborrow, G. S.; Fields, N. D.; Puleo, J. R.

    1976-01-01

    Bacterial samples were prepared for pyrolysis gas-liquid chromatography using cells grown on membrane filters. Pyrochromatograms were reproducible when cells harvested from the filters were pyrolyzed without being washed.

  15. Fecal short-chain fatty acid (SCFA) analysis by capillary gas-liquid

    Microsoft Academic Search

    Wolfgang M Scheppach; Claudia E Fabian; Heinrich W Kasper

    A new method is described for short-chain fatty acid (SCFA) analysis in stool samples. After sample purification by acid vacuum transfer and concentration by alkaline freeze- drying, SCFAs were measured by gas-liquid chromatography using a capillary column. Peak resolution and reproducibility were superior to SCFA analysis on a conventional glass column. With this new technique SCFA were quantitated in stool

  16. Fatty acids of cows' milk. A. Techniques employed in supplementing gas-liquid chromatography for identification of fatty acids

    Microsoft Academic Search

    Paul Magidman; S. F. Herb; R. A. Barford; R. W. Riemenschneider

    1962-01-01

    Milk fat methyl esters were subjected to distillation and silicic acid column chromatography to provide fractions of less\\u000a complexity for gas-liquid chromatographic analysis. It was still necessary however to employ supplemental techniques for identification.\\u000a Chromatograms were obtained with polyester columns of different polarity on all the fractions and necessary reference samples.\\u000a While many of the components were identified in the

  17. The Separation and Identification of Straight Chain Hydrocarbons: An Experiment Using Gas-Liquid Chromatography.

    ERIC Educational Resources Information Center

    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)

  18. Correlation of gas liquid chromatographie volatiles with flavor intensity scores of stored sunflower oils

    Microsoft Academic Search

    W. H. Morrison; B. G. Lyon; J. A. Robertson

    1981-01-01

    Samples of sunflower salad oil from seed produced in the northern United States containing butylated hydroxyanisole, butylated\\u000a hydroxytoluene, tert-butylhydroquinone and propyl gallate were stored in flintglass and amber bottles in the presence and\\u000a absence of light for 16 wk. Using Dupuy’s direct gas liquid chromatography method, correlations were made between pentane\\u000a and flavor intensity scores and total volatiles and flavor

  19. Determination of cis and trans -Octadecenoic acids in margarines by gas liquid chromatography-infrared spectrophotometry

    Microsoft Academic Search

    W. M. N. Ratnayake; R. Hollywood; E. O'Grady; J. L. Beare-Rogers

    1990-01-01

    A combined capillary gas liquid chromatography (GLC) and infrared spectrophotometry (IR) method is described for the determination\\u000a ofcis andtrans-octadecenoic acids in margarines made from partially hydrogenated vegetable oils. The totaltrans-unsaturation of margarine fatty acid methyl esters determined by IR, with methyl elaidate as the external standard, was correlated\\u000a to the capillary GLC weight percentages of the componenttrans fatty acid methyl

  20. Gas-liquid chromatography of triglycerides from erucic acid oils and fish oils

    Microsoft Academic Search

    R. D. Harlow; Carter Litchfield; Raymond Reiser

    1966-01-01

    By critically selecting optimum operating conditions, quantitative gas-liquid chromatography of triglycerides has been extended\\u000a to molecules containing substantial amounts of C20, C22, and C24 fatty acids. The triglycerides of four erucic acid oils (water cress, rapessed, nasturtium, andLunaria annua) and two fully hydrogenated fish oils (menhaden and tuna) have been quantitatively analyzed by this technique. The average\\u000a fatty acid chain

  1. Arabidopsis thaliana Polar Glycerolipid Profiling by Thin Layer Chromatography (TLC) Coupled with Gas-Liquid Chromatography (GLC)

    PubMed Central

    Wang, Zhen; Benning, Christoph

    2011-01-01

    Biological membranes separate cells from the environment. From a single cell to multicellular plants and animals, glycerolipids, such as phosphatidylcholine or phosphatidylethanolamine, form bilayer membranes which act as both boundaries and interfaces for chemical exchange between cells and their surroundings. Unlike animals, plant cells have a special organelle for photosynthesis, the chloroplast. The intricate membrane system of the chloroplast contains unique glycerolipids, namely glycolipids lacking phosphorus: monogalactosyldiacylglycerol (MGDG), digalactosyldiacylglycerol (DGDG), sulfoquinovosyldiacylglycerol (SQDG)4. The roles of these lipids are beyond simply structural. These glycolipids and other glycerolipids were found in the crystal structures of photosystem I and II indicating the involvement of glycerolipids in photosynthesis8,11. During phosphate starvation, DGDG is transferred to extraplastidic membranes to compensate the loss of phospholipids9,12. Much of our knowledge of the biosynthesis and function of these lipids has been derived from a combination of genetic and biochemical studies with Arabidopsis thaliana14. During these studies, a simple procedure for the analysis of polar lipids has been essential for the screening and analysis of lipid mutants and will be outlined in detail. A leaf lipid extract is first separated by thin layer chromatography (TLC) and glycerolipids are stained reversibly with iodine vapor. The individual lipids are scraped from the TLC plate and converted to fatty acyl methylesters (FAMEs), which are analyzed by gas-liquid chromatography coupled with flame ionization detection (FID-GLC) (Figure 1). This method has been proven to be a reliable tool for mutant screening. For example, the tgd1,2,3,4 endoplasmic reticulum-to-plastid lipid trafficking mutants were discovered based on the accumulation of an abnormal galactoglycerolipid: trigalactosyldiacylglycerol (TGDG) and a decrease in the relative amount of 18:3 (carbons : double bonds) fatty acyl groups in membrane lipids 3,13,18,20. This method is also applicable for determining enzymatic activities of proteins using lipids as substrate6. PMID:21445048

  2. Detection of Clostridium difficile in faeces by direct gas liquid chromatography.

    PubMed Central

    Levett, P N

    1984-01-01

    Stool specimens examined for the presence of Clostridium difficile and its cytotoxin were screened by gas liquid chromatography for the presence of volatile fatty acids and p-cresol. Twenty seven of 110 (25%) stools yielded C difficile or cytotoxin; iso-valeric acid was detected in 63/110 (57%) and iso-caproic acid in 18/110 (16%) stools. Para-cresol was found in 24/71 (34%) stools examined. Iso-valeric acid was detected in 85% of stools positive for C difficile, whereas iso-caproic acid (41%) and p-cresol (52%) were found in much lower numbers of C difficile-positive stools. It is concluded that gas chromatographic detection of volatile fatty acids or p-cresol in faeces are not satisfactory screening tests for the presence of C difficile. PMID:6693575

  3. Ionic liquids as novel stationary phases in gas liquid chromatography: inverse or normal isotope effect?

    PubMed

    Schmarr, Hans-Georg; Slabizki, Petra; Müntnich, Sabrina; Metzger, Carmen; Gracia-Moreno, Elisa

    2012-12-28

    The separation of deuterated and non-deuterated compounds in gas liquid partitioning chromatography (GLC) on silicone type stationary phase usually results in the inverse isotope effect. With ionic liquids (ILs) as stationary phase, however, this may show a totally different nature. The inverse isotope effect, in which heavier (deuterated) isotopic compounds (isotopologues) elute earlier, is to be expected when van der Waals (London) dispersion forces play a dominant role in the solute-stationary phase interaction. Such (apolar) interactions seem to play only a minor role when ILs are the stationary phases, leading to only a marginal inverse isotope effect, e.g. for the separation of 2,4,6-trichloroanisole and its [(2)H(5)]-isotopologue on 1,12-di(tripropylphosphonium) dodecane bis(trifluoromethansulfonyl) amide (commercialized as SLB-IL59, Supelco). Indeed, with the most polar stationary phase available (commercialized as SLB-IL111; Supelco), this separation showed a normal isotope effect. Further examples are presented and the nature of the isotope effect observed is discussed. PMID:23200305

  4. Identification of monoacyl- and monoalkylglycerols by gas-liquid chromatography-mass spectrometry using polar siloxane liquid phases

    Microsoft Academic Search

    J. J. Myher; L. Marai; A. Kuksis

    A comparative study was made of the spectra ob- tained after gas-liquid chromatography-mass spectrometry of the trimethylsilyl ethers of 1- and 2-monoacyl- and monoalkyl- glycerols. The glycerol derivatives were resolved on the basis of positional substitution and the degree of unsaturation on Silar- 5CP (a cyanopropylphenylsiloxane) liquid phase, and the peaks were examined in a Varian MAT CH-5 single-focusing mass

  5. Gas-liquid chromatography technique for detection of hippurate hydrolysis and conversion of fumarate to succinate by microorganisms.

    PubMed Central

    Kodaka, H; Lombard, G L; Dowell, V R

    1982-01-01

    A gas-liquid chromatography technique which allows simultaneous detection of hippuric acid (N-benzoylglycine) hydrolysis and conversion of fumaric acid to succinic acid by microorganisms uses a new medium, hippurate-formate-fumarate broth, and a gas chromatograph equipped with a thermal conductivity detector. This technique gave more reproducible results than other tests used in the study for detecting hippurate hydrolysis and also gave consistent results in detecting succinic acid produced from utilization of fumaric acid. PMID:7153346

  6. Norleucine-tyrosine broth for rapid identification of Clostridium difficile by gas-liquid chromatography.

    PubMed Central

    Nunez-Montiel, O L; Thompson, F S; Dowell, V R

    1983-01-01

    A new medium, norleucine-tyrosine (NT) broth, was developed for rapid identification of Clostridium difficile on the basis of caproic acid and p-cresol production. The NT broth consists of 0.5% Trypticase (BBL Microbiology Systems, Cockeysville, Md.), 0.5% yeast extract (Difco Laboratories, Detroit), 0.2% L-norleucine and 0.2% L-tyrosine (wt/vol; final concentrations), and a mixture of salts. The procedure for demonstrating caproic acid and p-cresol production involves extracting NT broth cultures with ether or chloroform and analyzing the extracts with a gas-liquid chromatograph equipped with a thermal conductivity detector, as is customary for analysis of volatile fatty acids. A total of 120 strains of C. difficile from diverse geographic locations were tested by this procedure, and they all produced caproic acid and p-cresol in NT broth. No other Clostridium species or other microorganisms tested have been found to produce both products in NT broth. PMID:6833488

  7. Determination of topanol antioxidants in methacrylates using capillary gas-liquid chromatography.

    PubMed

    Smith, I D; Waters, D G

    1992-04-10

    This paper presents a method to identify and determine topanol A and topanol O antioxidants in methylmethacrylate and 11-bromoundecylmethacrylate. The method is both simple and rapid. Analysis is performed on a 10 m x 0.53 mm I.D. HP-1 capillary gas chromatography column with a temperature gradient and a high carrier gas flow-rate (16.5 ml/min). Quantitation is by internal standardisation. Validation of the method is described for both topanols at concentrations of approximately 50 ppm in methylmethacrylate and 250 ppm in 11-bromoundecylmethacrylate. PMID:1400842

  8. DETERMINATION OF THE INSECT GROWTH REGULATOR METHOPRENE IN NATURAL WATERS BY CAPILLARY GAS-LIQUID CHROMATOGRAPHY

    EPA Science Inventory

    Residues of methoprene were measured in natural waters by capillary as liquid chromatography (GLG). Methoprene was extracted in the field by liquid-liquid partitioning with dichloromethane, transPorted to the laboratory, and extracted a second time with hexane. The extracts were ...

  9. Gas-liquid chromatographic analysis of monoglycerides as their trimethylsilyl ether derivatives

    Microsoft Academic Search

    R. D. Wood; P. K. Raju; Raymond Reiser

    1965-01-01

    A quantitative method is described for the rapid gas-liquid chromatographic analysis of monoglycerides of long chain fatty\\u000a acids as their trimethylsilyl (TMS) ether derivatives. The TMS derivatives are formed rapidly and quantitatively at room temp\\u000a without isomerization. The TMS derivatives of 1- and 2-monoglycerides may be separated on polyester columns, which can also\\u000a be used for the analysis of methyl

  10. Simulating Retention in Gas-Liquid Chromatography: Benzene, Toluene, and Xylene Solutes

    SciTech Connect

    WICK,COLLIN D.; MARTIN,MARCUS G.; SIEPMANN, J. ILJA; SCHURE,MARK R.

    2000-07-12

    Accurate predictions of retention times, retention indices, and partition constants are a long sought-after goal for theoretical studies in chromatography. Although advances in computational chemistry have improved the understanding of molecular interactions, little attention has been focused on chromatography, let alone calculations of retention properties. Configurational-bias Monte Carlo simulations in the isobaric-isothermal Gibbs ensemble were used to investigate the partitioning of benzene, toluene, and the three xylene isomers between a squalane liquid phase and a helium vapor phase. The united-atom representation of the TraPPE (Transferable Potentials for Phase Equilibria) force field was used for all solutes and squalane. The Gibbs free energies of transfer and Kovats retention indices of the solutes were calculated directly from the partition constants (which were averaged over several independent simulations). While the calculated Kovats indices of benzene and toluene at T = 403 K are significantly higher than their experimental counterparts, much better agreement is found for the xylene isomers at T = 365 K.

  11. Studies of stools from pseudomembranous colitis, rotaviral, and other diarrheal syndromes by frequency-pulsed electron capture gas-liquid chromatography.

    PubMed

    Brooks, J B; Nunez-Montiel, O L; Basta, M T; Hierholzer, J C

    1984-09-01

    Thirty-five patients with various diarrheal syndromes and 22 controls were studied. All stool samples were carefully cultured for Clostridium difficile, using selective isolation media. Cytotoxin assays with proper antitoxin neutralization were done in MRC-5 cells. The stool samples were extracted four times, three times at pH 2 and once at pH 10, using CHCl3 or ether. Derivatizations of extracts were done with trichloroethanol, heptafluorobutyric anhydride, and heptafluorobutyric anhydride-ethanol, and all derivatives were analyzed by frequency-pulsed electron capture gas-liquid chromatography (FPEC-GLC). A dedicated computer was used to assist in both qualitative and quantitative data analysis. Isocaproic acid (iC6) was always found in stool from which C. difficile was isolated and was absent in C. difficile-negative specimens. p-Cresol was found frequently in both persons with pseudomembranous colitis and controls. Tryptamine was found in stool containing C. bifermentans. The FPEC-GLC profiles of persons with acute diarrhea were very different from those of normal persons. Diarrhea associated with adenovirus and rotavirus, Klebsiella spp., and Escherichia spp. showed different FPEC-GLC patterns. Stools from well persons consistently contained full-scale peaks of pyruvic, acetic, propionic, isobutyric, butyric, isovaleric, and valeric acids. In rotavirus stools isobutyric, isovaleric, and valeric acids were reduced in quantity from those found in control stools, whereas propionic and butyric acids were increased. PMID:6490836

  12. Studies of stools from pseudomembranous colitis, rotaviral, and other diarrheal syndromes by frequency-pulsed electron capture gas-liquid chromatography.

    PubMed Central

    Brooks, J B; Nunez-Montiel, O L; Basta, M T; Hierholzer, J C

    1984-01-01

    Thirty-five patients with various diarrheal syndromes and 22 controls were studied. All stool samples were carefully cultured for Clostridium difficile, using selective isolation media. Cytotoxin assays with proper antitoxin neutralization were done in MRC-5 cells. The stool samples were extracted four times, three times at pH 2 and once at pH 10, using CHCl3 or ether. Derivatizations of extracts were done with trichloroethanol, heptafluorobutyric anhydride, and heptafluorobutyric anhydride-ethanol, and all derivatives were analyzed by frequency-pulsed electron capture gas-liquid chromatography (FPEC-GLC). A dedicated computer was used to assist in both qualitative and quantitative data analysis. Isocaproic acid (iC6) was always found in stool from which C. difficile was isolated and was absent in C. difficile-negative specimens. p-Cresol was found frequently in both persons with pseudomembranous colitis and controls. Tryptamine was found in stool containing C. bifermentans. The FPEC-GLC profiles of persons with acute diarrhea were very different from those of normal persons. Diarrhea associated with adenovirus and rotavirus, Klebsiella spp., and Escherichia spp. showed different FPEC-GLC patterns. Stools from well persons consistently contained full-scale peaks of pyruvic, acetic, propionic, isobutyric, butyric, isovaleric, and valeric acids. In rotavirus stools isobutyric, isovaleric, and valeric acids were reduced in quantity from those found in control stools, whereas propionic and butyric acids were increased. PMID:6490836

  13. Retention in gas-liquid chromatography with a polyethylene oxide stationary phase: molecular simulation and experiment.

    PubMed

    Sun, Li; Siepmann, J Ilja; Klotz, Wendy L; Schure, Mark R

    2006-09-01

    Configurational-bias Monte Carlo simulations in the isobaric-isothermal Gibbs ensemble were carried out to investigate the partitioning of normal alkanes, primary and secondary alcohols, symmetric alkyl ethers and arenes between a helium vapor phase and a polyethylene oxide stationary phase (M(W)=382 g mol(-1)). The united-atom version of the transferable potentials for phase equilibria force field was used to model all solutes, polyethylene oxide and helium. The Gibbs free energies of transfer and Kovats retention indices of the solutes were calculated directly from the partition constants at two different temperatures, 353 and 393 K. Chromatographic experiments on a Carbowax 20M retentive phase were performed for the same set of solutes and temperatures ranging from 333 to 413 K. The predicted retention indices for alcohols, ethers and arenes are overestimated by about 120, 70 and 20 retention index units, respectively, pointing to an overestimation of the first-order electrostatic interactions in the model system. Molecular-level analysis shows that hydrogen-bonding and dipole-dipole interactions lead to orientational ordering for the alcohol and ether analytes, whereas the weaker dipole-quadrupole interactions for the arene solutes are not sufficient to induce orientational ordering. The retention indices of alcohols and ethers decrease with increasing temperature because of the large entropic cost of hydrogen-bonding and orientational ordering. In contrast, the retention indices for arenes increase with increasing temperature because the entropic cost of cavity formation is smaller for arenes than for comparable alkanes. PMID:16814798

  14. Simultaneous determination of amitriptyline, nortriptyline and four hydroxylated metabolites in serum by capillary gas-liquid chromatography with nitrogen-phosphorus-selective detection

    Microsoft Academic Search

    S. Ulrich; T. Isensee; U. Pester

    1996-01-01

    A method for the simultaneous quantification of the antidepressant drug amitriptyline, its demethylated metabolite nortriptyline and four hydroxy metabolites (E-10-hydroxyamitriptyline, Z-10-hydroxyamitriptyline, E-10-hydroxynortriptyline, Z-10-hydroxynortriptyline) in human serum or plasma has been developed. The method is based on a three-step liquid-liquid extraction followed by gas-liquid chromatography (split-splitless injection, HP-5, 25 m×0.2 mm I.D., 0.33 ?m capillary) with nitrogen phosphorus-selective detection (GLC-NPD). The

  15. Radiometric studies with gas-liquid and thin-layer chromatography for rapid demonstration of hemin dependence and characterization of Mycobacterium haemophilum

    SciTech Connect

    Damato, J.J.; Collins, M.T.

    1984-09-01

    Eight isolates of Mycobacterium haemophilum were evaluated by radiometric methods to determine whether this test system could support the growth of these organisms as well as demonstrate their growth requirements for iron complexes such as hemin, ferric ammonium citrate, and blood. In addition, gas-liquid and thin-layer chromatography were evaluated to determine whether these procedures could further differentiate M. haemophilum from other mycobacteria. During the initial 24 to 48 h, there was no significant difference between the radiometric test broths containing iron complexes and control broths without iron supplementation. After 48 h, the test growth index readings rapidly increased, and control broth readings leveled off and declined. The mean growth index reading of the test broths after 6 days of incubation was 100 times that of the controls. The mean incubation time with supplemented 7H10 agar was 17 days. The use of radiometric media resulted in the demonstration of hemin dependence by M. haemophilum significantly earlier than with 7H10 agar. Of the three supplements studied, whole blood provided the greatest growth rate, followed by ferric ammonium citrate and hemin. When 12 species of mycobacteria other than M. haemophilum were radiometrically evaluated, no isolate demonstrated an iron complex requirement. Gas-liquid and thin-layer chromatography procedures were able to rapidly differentiate M. haemophilum from the other 12 Mycobacterium species.

  16. Frequency-pulsed electron capture gas-liquid chromatographic analysis of metabolites produced by Clostridium difficile in broth enriched with amino acids.

    PubMed Central

    Brooks, J B; Nunez-Montiel, O L; Wycoff, B J; Moss, C W

    1984-01-01

    Clostridium difficile strain CDC A-567 was cultured in Trypticase (BBL Microbiology Systems)-yeast-salt broth supplemented with 0.2% L-leucine, L-norleucine, L-isoleucine, L-tyrosine, or L-tryptophan. Four extractions were done on the spent medium, three at pH 2 and one at pH 10, using CHCL3 or ether. Derivatizations were done with trichloroethanol, heptafluorobutyric anhydride, and heptafluorobutyric anhydride-ethanol. All samples were analyzed with frequency-pulsed electron capture gas-liquid chromatography. A dedicated computer was used to assist in data analysis. C. difficile produced both short-chain and aromatic acids in Trypticase-yeast-salt broth; hydroxy acids were also detected. p-Cresol, indoleacetic acid, 4-methylthio-2-hydroxybutyric acid, and some unidentified alcohols were observed. The basic chloroform extraction contained cadaverine and putrescine. Leucine, norleucine, and isoleucine influenced the production of C5 and C6 acids and alcohols. L-Tyrosine underwent successive degradation to produce p-cresol and aromatic acids as final products. Tryptophan increased the production of indoleacetic, indolepropionic, and indolebutyric acids. Isocaproic acid was produced in relatively high concentrations regardless of medium substitution. The consistent production of iC6 under various substrate conditions indicates that the production of this compound might be consistent enough in vitro to form the basis of a rapid test for detection of C. difficile in stool specimens by frequency-pulsed electron capture gas-liquid chromatography. PMID:6490835

  17. Simultaneous determination of amitriptyline, nortriptyline and four hydroxylated metabolites in serum by capillary gas-liquid chromatography with nitrogen-phosphorus-selective detection.

    PubMed

    Ulrich, S; Isensee, T; Pester, U

    1996-10-11

    A method for the simultaneous quantification of the antidepressant drug amitriptyline, its demethylated metabolite nortriptyline and four hydroxy metabolites (E-10-hydroxyamitriptyline, Z-10-hydroxyamitriptyline, E-10-hydroxynortriptyline, Z-10-hydroxynortriptyline) in human serum or plasma has been developed. The method is based on a three-step liquid-liquid extraction followed by gas-liquid chromatography (split-splitless injection, HP-5, 25 m x 0.2 mm I.D., 0.33 microns capillary) with nitrogen-phosphorus-selective detection (GLC-NPD). The limits of detection are 1.5 ng/ml for amitriptyline, nortriptyline, E-10-hydroxyamitriptyline and Z-10-hydroxyamitriptyline and 3 ng/ml for E-10-hydroxynortiptyline and Z-10-hydroxynortriptyline. The within-day and between-day precision is between 6 and 15% at three concentrations (low, moderate and high) for amitriptyline, nortriptyline and E-10-hydroxy metabolites. At low concentrations of 10 ng/ml, the precision of the assay of the Z-10-hydroxy metabolites has been found to be up to 19%. Accuracy is between 91 and 115% for all analytes. The performance of the assay of the hydroxy metabolites is mainly determined by the cleanness and the deactivation of the quartz insert of the injector port. Therefore, every day a freshly cleaned and deactivated insert was used. PMID:8930756

  18. Effect of cavitation on the properties of coal-tar pitch as studied by gas-liquid chromatography

    SciTech Connect

    M.I. Baikenov; T.B. Omarbekov; S.K. Amerkhanova (and others) [Buketov State University, Karaganda (Kazakhstan)

    2008-02-15

    The applicability of the cavitation-wave effect to coal-tar pitch processing is considered. The results of the GLC analysis of the test material before and after rotor-pulsation cavitation treatment are given. The organic matter of coal-tar pitch was found to degrade upon cavitation; as a result of this, the yields of light and medium fractions considerably increased. 5 refs., 2 figs., 4 tabs.

  19. Analysis of finit in urine sample using thin layer chromatography.

    PubMed

    Jaiswal, A K; Lal, Nand

    2012-01-01

    Finit is a common insecticide generally used to control a variety of insects in homes. Routinely it is analysed by Gas Liquid Chromatography (GLC) and High Performance Liquid Chromatography (HPLC). An attempt has been made to develop a new method for analysis of finit in urine samples using Thin Layer Chromatography (TLC) technique which is inexpensive, accurate and non-destructive. Finit was extracted from urine using solvent extraction methods and then identified on the TLC plates. For detection on developed plates, palladium chloride, silver nitrate, iodine vapour and bromophenol blue were used which successfully increased the sensitivity without dispensing with the simplicity of the method. The method developed is simple, inexpensive, accurate and non-destructive that allows for sensitive and reproducible analysis of finit. PMID:23741873

  20. Chromatographie analysis of seed oils. Fatty acid composition of castor oil

    Microsoft Academic Search

    R. G. Binder; T. H. Applewhite; G. O. Kohler; L. A. Goldblatt

    1962-01-01

    The fatty acid composition of a number of domestic and foreign castor oils was determined by consecutive column and gas-liquid\\u000a Chromatographic analysis. After saponification of the oils and removal of the unsaponifiables, the nonhydroxy, monohydroxy,\\u000a and dihydroxy acids were fractionated by partition chromatography on silicic acid. The amount of acid in each fraction was\\u000a determined by titration or weighing. Gravimetric

  1. Quantitative Analysis of Urine Vapor and Breath by Gas-Liquid Partition Chromatography

    Microsoft Academic Search

    Linus Pauling; Arthur B. Robinson; Roy Teranishi; Paul Cary

    1971-01-01

    When a human being is placed for several days on a completely defined diet, consisting almost entirely of small molecules that are absorbed from the stomach into the blood, intestinal flora disappear because of lack of nutrition. By this technique, the composition of body fluids can be made constant (standard deviation about 10%) after a few days, permitting significant quantitative

  2. Boolean logic analysis for flow regime recognition of gas-liquid horizontal flow

    NASA Astrophysics Data System (ADS)

    Ramskill, Nicholas P.; Wang, Mi

    2011-10-01

    In order to develop a flowmeter for the accurate measurement of multiphase flows, it is of the utmost importance to correctly identify the flow regime present to enable the selection of the optimal method for metering. In this study, the horizontal flow of air and water in a pipeline was studied under a multitude of conditions using electrical resistance tomography but the flow regimes that are presented in this paper have been limited to plug and bubble air-water flows. This study proposes a novel method for recognition of the prevalent flow regime using only a fraction of the data, thus rendering the analysis more efficient. By considering the average conductivity of five zones along the central axis of the tomogram, key features can be identified, thus enabling the recognition of the prevalent flow regime. Boolean logic and frequency spectrum analysis has been applied for flow regime recognition. Visualization of the flow using the reconstructed images provides a qualitative comparison between different flow regimes. Application of the Boolean logic scheme enables a quantitative comparison of the flow patterns, thus reducing the subjectivity in the identification of the prevalent flow regime.

  3. Gas-liquid chromatographic and gas-liquid-mass spectometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

    USGS Publications Warehouse

    Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.

    1981-01-01

    A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

  4. Analysis of essential oils, using capillary chromatography

    Microsoft Academic Search

    V. N. Paukov; B. A. Rudenko; V. F. Kucherov

    1968-01-01

    1.The possibility of using capillary chromatography for a complete analysis of essential oils without preliminary separation into fractions was demonstrated.2.The relative retainable volumes and Kovach indices of a number of components of the essential oils of fennel, geranium, and coriander were determined.3.All the components of the essential oils of fennel, coriander, and geranium detected in capillary chromatography were identified.

  5. Supersonic Gas-Liquid Cleaning System

    NASA Technical Reports Server (NTRS)

    Kinney, Frank

    1996-01-01

    The Supersonic Gas-Liquid Cleaning System Research Project consisted mainly of a feasibility study, including theoretical and engineering analysis, of a proof-of-concept prototype of this particular cleaning system developed by NASA-KSC. The cleaning system utilizes gas-liquid supersonic nozzles to generate high impingement velocities at the surface of the device to be cleaned. The cleaning fluid being accelerated to these high velocities may consist of any solvent or liquid, including water. Compressed air or any inert gas is used to provide the conveying medium for the liquid, as well as substantially reduce the total amount of liquid needed to perform adequate surface cleaning and cleanliness verification. This type of aqueous cleaning system is considered to be an excellent way of conducting cleaning and cleanliness verification operations as replacements for the use of CFC 113 which must be discontinued by 1995. To utilize this particular cleaning system in various cleaning applications for both the Space Program and the commercial market, it is essential that the cleaning system, especially the supersonic nozzle, be characterized for such applications. This characterization consisted of performing theoretical and engineering analysis, identifying desirable modifications/extensions to the basic concept, evaluating effects of variations in operating parameters, and optimizing hardware design for specific applications.

  6. Chromatography.

    ERIC Educational Resources Information Center

    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)

  7. Chromatography coupled atomic fluorescence spectrometry for mercury species analysis

    Microsoft Academic Search

    Juan Chen; Xiaoping Yu; Yafei Guo; Tianlong Deng

    2011-01-01

    Pretreatment and determination for mercury species based on coupled chromatography techniques especially the combination of liquid chromatography with atomic fluorescence spectrometry were reviewed in this paper with 17 references, and the new trends for trace and ultra-trace of mercury species analysis in the future was also carried out. Keywords-Envionment, pretreatment, mercury speciation analysis; liquid chromatography, atomic fluorescence spectrometry. I. INTRODUCTION

  8. Advances in gas-liquid flows 1990

    SciTech Connect

    Kim, J.M. (Texas Univ., Austin, TX (United States). Nuclear Reactor Lab.); Rohatgi, U.S. (Brookhaven National Lab., Upton, NY (United States)); Hashemi, A. (Lockheed Missiles and Space Company (US))

    1990-01-01

    Gas-liquid two-phase flows commonly occur in nature and industrial applications. Rain, clouds, geysers, and waterfalls are examples of natural gas-liquid flow phenomena, whereas industrial applications can be found in nuclear reactors, steam generators, boilers, condensers, evaporators, fuel atomization, heat pipes, electronic equipment cooling, petroleum engineering, chemical process engineering, and many others. The household-variety phenomena such as garden sprinklers, shower, whirlpool bath, dripping faucet, boiling tea pot, and bubbling beer provide daily experience of gas-liquid flows. The papers presented in this volume reflect the variety and richness of gas-liquid two-phase flow and the increasing role it plays in modern technology. This volume contains papers dealing with some recent development in gas-liquid flow science and technology, covering basic gas-liquid flows, measurements and instrumentation, cavitation and flashing flows, countercurrent flow and flooding, flow in various components and geometries liquid metals and thermocapillary effects, heat transfer, nonlinear phenomena, instability, and other special and general topics related to gas-liquid flows.

  9. Detection and data analysis in size exclusion chromatography

    SciTech Connect

    Provder, T. (ed.)

    1987-01-01

    Specific topics covered in this symposium on site exclusion chromatography are of interest under the broad topic of energy research. namely, the chemical analysis of siloxanes as the chemical analysis of coal liquids.

  10. Chromatography

    NSDL National Science Digital Library

    WGBH Boston

    2002-01-01

    In this activity, explore chromatography and the various colors that make up the ink in markers. Use this activity to investigate cohesion and adhesion. The online version of this activity is set up so that learners solve a mystery.

  11. ANALYSIS OF TECHNICAL CHLORDANE BY GAS CHROMATOGRAPHY MASS SPECTROMETRY

    EPA Science Inventory

    The composition of technical chlordane has been investigated by combined gas chromatography/mass spectrometry, employing a column commonly used for pesticide residue analysis. Partial or complete structure identification have been assigned to some 45 individual constituents. Many...

  12. Minimizing liquid contaminants in natural gas liquids

    SciTech Connect

    Brown, R.L. [Pall Industrial Process Filtration, East Hills, NY (United States); Wines, T.H. [Pall Scientific and Laboratory Services, Port Washington, NY (United States); Williamson, K.M. [Pall Process Equipment Development, Cortland, NY (United States)

    1996-12-31

    In processing natural gas liquids, significant contamination occurs with liquid dispersions and emulsions. Natural gas liquids (NGL) and liquid petroleum gas (LPG) streams are treated with caustic to remove residual organic sulfur compounds such as mercaptans and with amines to remove hydrogen sulfide. In both cases a liquid/liquid contactor is used. Significant amounts of the caustic or amine can be carried over into the product stream in process units that are running at rates above design capacity, are treating high sulfur feed stocks, or have other operational problems. The carried over liquid results in off-spec products, excessive loses of caustic or amine, and can cause operating problems in downstream processes. In addition, water is a significant contaminant which can cause LPG and natural gasoline to be off-specification. This paper discusses a new technique for separating very stable liquid dispersions of caustic, amine, or water from natural gas liquids using liquid/liquid cartridge coalescers constructed with specially formulated polymer and fluoropolymer medium with enhanced surface properties. In addition, factors influencing the coalescer mechanism will be discussed including interfacial tension, concentration of surface active compounds, steric repulsion, and electrostatic charge affects. Results from field tests, operating data from commercial installations, and economic benefits will also be presented.

  13. Targeted analysis of glycomics liquid chromatography\\/mass spectrometry data

    Microsoft Academic Search

    Jonathan M. Dreyfuss; Christopher Jacobs; Yevgeniy Gindin; Gary Benson; Gregory O. Staples; Joseph Zaia

    2011-01-01

    Hydrophilic interaction chromatography (HILIC) liquid chromatography\\/mass spectrometry (LC\\/MS) is appropriate for all native\\u000a and reductively aminated glycan classes. HILIC carries the advantage that retention times vary predictably according to oligosaccharide\\u000a composition. Chromatographic conditions are compatible with sensitive and reproducible glycomics analysis of large numbers\\u000a of samples. The data are extremely useful for quantitative profiling of glycans expressed in biological tissues.

  14. Gas-liquid flow and heat transfer

    SciTech Connect

    Hewitt, G.F.; Whalley, P.B.

    1984-01-01

    This book covers almost the total field of gas-liquid flow and heat transfer, reviewing and collating recent information. Contents (partial): Introduction. Regimes of flow. General analytical and empirical relationships in two phase flow. Interfacial waves. Creation and behaviour of entrained droplets. Bubble flow. Plug flow. Hydrodynamics of co-current vertical annular flow. Hydrodynamics and limits of counter-current flows. Stratified wavy and slug flow in horizontal tubes. Hydrodynamics of annular flows in nonvertical channels and complex. Introduction to two phase heat transfer. Heat transfer in annular flow. Burnout. Post burnout heat transfer. Rewetting and reflooding. Experimental techniques.

  15. Phytanic acid: measurement of plasma concentrations by gas-liquid chromatography-mass spectrometry analysis and associations with diet and other plasma fatty acids.

    PubMed

    Allen, Naomi E; Grace, Philip B; Ginn, Annette; Travis, Ruth C; Roddam, Andrew W; Appleby, Paul N; Key, Timothy

    2008-03-01

    Epidemiological data suggest that a diet rich in animal foods may be associated with an increased risk of several cancers, including cancers of the prostate, colorectum and breast, but the possible mechanism is unclear. It is hypothesised that phytanic acid, a C20 branched-chain fatty acid found predominantly in foods from ruminant animals, may be involved in early cancer development because it has been shown to up regulate activity of alpha-methylacyl-coenzyme A racemase, an enzyme commonly found to be over-expressed in tumour cells compared with normal tissue. However, little is known about the distribution of plasma phytanic acid concentrations or its dietary determinants in the general population. The primary aim of the present cross-sectional study was to determine circulating phytanic acid concentrations among ninety-six meat-eating, lacto-ovo-vegetarian and vegan women, aged 20-69 years, recruited into the Oxford component of the European Prospective Investigation into Cancer and Nutrition (EPIC-Oxford). Meat-eaters had, on average, a 6.7-fold higher geometric mean plasma phytanic acid concentration than the vegans (5.77 v. 0.86 micromol/l; P < 0.0001) and a 47 % higher mean concentration than the vegetarians (5.77 v. 3.93 micromol/l; P = 0.016). The strongest determinant of plasma phytanic acid concentration appeared to be dairy fat intake (r 0.68; P < 0.0001); phytanic acid levels were not associated with age or other lifestyle factors. These data show that a diet high in fat from dairy products is associated with increased plasma phytanic acid concentration, which may play a role in cancer development. PMID:17868488

  16. Identification of the Botanical Origin of Commercial Pine Nuts Responsible for Dysgeusia by Gas-Liquid Chromatography Analysis of Fatty Acid Profile

    PubMed Central

    Destaillats, Frédéric; Cruz-Hernandez, Cristina; Giuffrida, Francesca; Dionisi, Fabiola; Mostin, Martine; Verstegen, Geert

    2011-01-01

    Over the last 10 years, complaints were increasingly reported from consumers that experienced dysgeusia following the consumption of pine nuts. In the present study, pine nuts samples (N = 16) from consumers that reported dysgeusia have been analyzed to identify the botanical origin of critical pine nuts samples. The fatty acid composition of the samples was performed, and diagnostic index values were used to identify the botanical origin of the samples. Pinus armandii nuts were identified in all the samples pure or in mixture with P. koraiensis nuts. P. armandii is not reported as edible pine nuts by the Food and Agriculture Organization (FAO). This study confirmed that consumption of P. armandii nuts may lead to dysgeusia. Based on the present study and previous work, we advise import companies to trade pine nuts from traditionally recognized species such as P. pinea, P. sibirica, P. koraiensis, or P. gerardiana. PMID:21559093

  17. Supersonic gas-liquid cleaning system

    NASA Technical Reports Server (NTRS)

    Caimi, Raoul E. B.; Thaxton, Eric A.

    1994-01-01

    A system to perform cleaning and cleanliness verification is being developed to replace solvent flush methods using CFC 113 for fluid system components. The system is designed for two purposes: internal and external cleaning and verification. External cleaning is performed with the nozzle mounted at the end of a wand similar to a conventional pressure washer. Internal cleaning is performed with a variety of fixtures designed for specific applications. Internal cleaning includes tubes, pipes, flex hoses, and active fluid components such as valves and regulators. The system uses gas-liquid supersonic nozzles to generate high impingement velocities at the surface of the object to be cleaned. Compressed air or any inert gas may be used to provide the conveying medium for the liquid. The converging-diverging nozzles accelerate the gas-liquid mixture to supersonic velocities. The liquid being accelerated may be any solvent including water. This system may be used commercially to replace CFC and other solvent cleaning methods widely used to remove dust, dirt, flux, and lubricants. In addition, cleanliness verification can be performed without the solvents which are typically involved. This paper will present the technical details of the system, the results achieved during testing at KSC, and future applications for this system.

  18. Determination of microbial fatty acid profiles at femtomolar levels in human urine and the initial marine microfouling community by capillary gas chromatography-chemical ionization mass spectrometry with negative ion detection

    Microsoft Academic Search

    Goran Odham; Anders Tunlid; Gunilla Westerdahl; Lennart Larsson; James B. Guckert; David C. White

    1985-01-01

    Summary Room temperature esterification with the electron capturing pentafluorobenzyl bromide in glass capillaries, with analysis by capillary gas-liquid chromatography coupled with chemical ionization mass spectrometry and negative ion detection in the selected ion mode, allowed detection and identification of fatty acids from micro- bial biofilms at the femtomolar level. This sensitivity was achieved without loss of specificity of the mass

  19. Gas-Liquid Processing in Microchannels

    SciTech Connect

    TeGrotenhuis, Ward E.; Stenkamp, Victoria S.; Twitchell, Alvin

    2005-09-01

    Processing gases and liquids together in microchannels having at least one dimension <1 mm has unique advantages for rapid heat and mass transfer. One approach for managing the two phases is to use porous structures as wicks within microchannels to segregate the liquid phase from the gas phase. Gas-liquid processing is accomplished by providing a gas flow path and inducing flow of the liquid phase through or along the wick under an induced pressure gradient. A variety of unit operations are enabled, including phase separation, partial condensation, absorption, desorption, and distillation. Results are reported of an investigation of microchannel phase separation in a transparent, single-channel device. Next, heat exchange is integrated with the microchannel wick approach to create a partial condenser that also separates the condensate. Finally, the scale-up to a multi-channel phase separator is described.

  20. Gas-liquid chromatographic determination of 3-trifluoromethyl-4-nitrophenol residues in fish

    USGS Publications Warehouse

    Allen, J.L.; Sills, J.B.

    1974-01-01

    A procedure for the determination of 3-mftuormethyl-4-nitrophenol (TFM) in fish tissues is described. Homogenized tissues are extracted with hexane-ethyl ether; the extract is cleaned up by partitioning the TFM from the extracting solvent into O.IN NaOB, acidifying the aqueous solution, and partitioning again with hexaneethyl ether. The TFM is methylated with diazomethane and analyzed by gas-liquid chromatography, using electron capture detection. Recoveries ranged from 75 to 1000/., from fish muscles that were spiked with 0.01-2.00 JA#g TFM/g.

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

    NASA Astrophysics Data System (ADS)

    ?obi?ski, 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.

  2. Energy Recovery By Direct Contact Gas-Liquid Heat Exchange 

    E-print Network

    Fair, J. R.; Bravo, J. L.

    1988-01-01

    Energy from hot gas discharge streams can be recovered by transfer directly to a coolant liquid in one of several available gas-liquid contacting devices. The design of the device is central to the theme of this paper, ...

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

    PubMed

    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. PMID:24312804

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

    PubMed Central

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

    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. PMID:24312804

  5. Isothermal Gas-liquid Flow Using the Lattice Boltzmann Method

    E-print Network

    Kim, Donghoon

    2012-10-19

    ISOTHERMAL GAS-LIQUID FLOW USING THE LATTICE BOLTZMANN METHOD A Thesis by DONGHOON KIM Submitted to the Office of Graduate Studies of Texas A&M University in partial fulfillment of the requirements for the degree... of MASTER OF SCIENCE August 2011 Major Subject: Nuclear Engineering ISOTHERMAL GAS-LIQUID FLOW USING THE LATTICE BOLTZMANN METHOD A Thesis by DONGHOON KIM Submitted to the Office of Graduate Studies of Texas A&M University...

  6. Numerical modelling of gas–liquid flow in stirred tanks

    Microsoft Academic Search

    M. P. Schwarz; G. M. Evans

    2005-01-01

    A numerical modelling method is presented for gas–liquid flow in mechanically stirred tanks. In this method, the tank is represented by a mesh which explicitly includes the impeller geometry, with impeller motion treated by the multiple frames of reference or sliding mesh methods. Gas–liquid flow is modelled using an ensemble-averaged form of the Eulerian two-fluid equations. This leads to an

  7. Group type analysis of asphalt by column liquid chromatography

    SciTech Connect

    Zhang, C.; Yang, J.; Xue, Y.; Li, Y. [Chinese Academy of Science, Taiyuan (China)

    2008-07-01

    An improved analysis method for characterization of asphalt was established. The method is based on column chromatography technique. The asphalts were separated into four groups: saturates, aromatics, resins, and asphaltenes, quantitatively. About 0.1 g of sample was required in each analysis. About 20 mL of n-heptanes was used to separate out saturates first. Then about 35 mL of n-heptanes/dichloromethane (.5, v/v) mixture was used to separate out aromatics. About 30 mL of dichloromethane/tetrahydrofuran (1/3, v/v) mixture was used to separate out resin. The quality of the separation was confirmed by infrared spectra (IR) and {sup 1}H NMR analysis. The model compounds, tetracosan for saturates, dibenz(o)anthracen for aromatics, and acetanilide for resins were used for verification. The IR and {sup 1}H NMR analysis of the prepared fractions from the column liquid chromatography were in good agreement that of pure reagents.

  8. Cellular fatty acid analysis as a potential tool for predicting mosquitocidal activity of Bacillus sphaericus strains.

    PubMed Central

    Frachon, E; Hamon, S; Nicolas, L; de Barjac, H

    1991-01-01

    Gas-liquid chromatography of fatty acid methyl esters and numerical analysis were carried out with 114 Bacillus sphaericus strains. Since only two clusters harbored mosquitocidal strains, this technique could be developed in screening programs to limit bioassays on mosquito larvae. It also allows differentiation of highly homologous strains. PMID:1781697

  9. Injector design guidelines for gas/liquid propellant systems

    NASA Technical Reports Server (NTRS)

    Falk, A. Y.; Burick, R. J.

    1973-01-01

    Injector design guidelines are provided for gas/liquid propellant systems. Information was obtained from a 30-month applied research program encompassing an analytical, design, and experimental effort to relate injector design parameters to simultaneous attainment of high performance and component (injector/thrust chamber) compatibility for gas/liquid space storable propellants. The gas/liquid propellant combination studied was FLOX (82.6% F2)/ ambient temperature gaseous methane. Design criteria that provide for simultaneous attainment of high performance and chamber compatibility are presented for both injector types. Parametric data are presented that are applicable for the design of circular coaxial and like-doublet injectors that operate with design parameters similar to those employed. However, caution should be exercised when applying these data to propellant combinations whose elements operate in ranges considerably different from those employed in this study.

  10. Modified electrokinetic sample injection method in chromatography and electrophoresis analysis

    DOEpatents

    Davidson, J. Courtney (Livermore, CA); Balch, Joseph W. (Livermore, CA)

    2001-01-01

    A sample injection method for horizontal configured multiple chromatography or electrophoresis units, each containing a number of separation/analysis channels, that enables efficient introduction of analyte samples. This method for loading when taken in conjunction with horizontal microchannels allows much reduced sample volumes and a means of sample stacking to greatly reduce the concentration of the sample. This reduction in the amount of sample can lead to great cost savings in sample preparation, particularly in massively parallel applications such as DNA sequencing. The essence of this method is in preparation of the input of the separation channel, the physical sample introduction, and subsequent removal of excess material. By this method, sample volumes of 100 nanoliter to 2 microliters have been used successfully, compared to the typical 5 microliters of sample required by the prior separation/analysis method.

  11. Partial wetting gas-liquid segmented flow microreactor.

    PubMed

    Kazemi Oskooei, S Ali; Sinton, David

    2010-07-01

    A microfluidic reactor strategy for reducing plug-to-plug transport in gas-liquid segmented flow microfluidic reactors is presented. The segmented flow is generated in a wetting portion of the chip that transitions downstream to a partially wetting reaction channel that serves to disconnect the liquid plugs. The resulting residence time distributions show little dependence on channel length, and over 60% narrowing in residence time distribution as compared to an otherwise similar reactor. This partial wetting strategy mitigates a central limitation (plug-to-plug dispersion) while preserving the many attractive features of gas-liquid segmented flow reactors. PMID:20383398

  12. Investigation on a gas-liquid ejector using three-dimensional CFD model

    NASA Astrophysics Data System (ADS)

    Kang, S. H.; Song, X. G.; Park, Y. C.

    2012-11-01

    This paper is focusing on the numeral study of a gas-liquid ejector used for ballast water treatment. The gasliquid ejector is investigated through steady three-dimensional multiphase CFD analysis with commercial software ANSYS-CFX 13.0. Water as the primary fluid is driven through the driving nozzle and air is ejected into as the second gas instead of the ozone in real application. Several turbulence models such as Standard k-? model, RNG k-? model, SST model and k-? model, and different mesh size and compared extensively with the experimental results to eliminate the influence of the auxiliary system, turbulence models and mesh generation. The appropriate numerical model in terms of the best combination of turbulence model and mesh size are used in the subsequent research the study the influence of the operating condition such as the driving pressure/velocity and the back pressure of the ejector on its performance. The results provide deep insight on the influence of various factors on the performance of gas-liquid ejector. And the proposed numerical model will be very helpful in the further design optimization of the gas-liquid ejectors.

  13. An improved method for analysis of biomass sugars and galacturonic acid by anion exchange chromatography

    Technology Transfer Automated Retrieval System (TEKTRAN)

    While the most accurate method for analysis of sugars in biomass is based on gas chromatography of trimethylsilane or alditol acetate derivitives of sugars, the derivation method is time consuming and laborious. In comparison, sample preparation for sugar analysis using liquid chromatography is a si...

  14. Analysis of soybean lecithin by thin layer and analytical liquid chromatography

    Microsoft Academic Search

    W. L. Erdahl; A. Stolyhwo; O. S. Privett

    1973-01-01

    The application of thin layer and analytical liquid chromatography to the analysis of two samples of commercial soybean lecithins\\u000a is described. A combination of column chromatography and quantitative thin layer chromatography showed that these products\\u000a consisted of ca. 82% mixture of the major phospholipids of soybeans, phosphatidyl choline, phosphatidyl ethanolamine, and\\u000a phosphatidyl inositol. The remainder of these products contained essentially

  15. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...Factors for Petroleum Products and Natural Gas Liquids 1 2 MM Table MM-1...Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column... Other Petroleum Products and Natural Gas Liquids Aviation Gasoline...

  16. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...Factors for Petroleum Products and Natural Gas Liquids 1 2 MM Table MM-1...Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column... Other Petroleum Products and Natural Gas Liquids Aviation Gasoline...

  17. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...Factors for Petroleum Products and Natural Gas Liquids 1 2 MM Table MM-1...Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column... Other Petroleum Products and Natural Gas Liquids Aviation Gasoline...

  18. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...Factors for Petroleum Products and Natural Gas Liquids 1 2 MM Table MM-1...Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column... Other Petroleum Products and Natural Gas Liquids Aviation Gasoline...

  19. Thin-layer chromatography-densitometry and liquid chromatography analysis of alkaloids in leaves of Papaver somniferum under stress conditions.

    PubMed

    Szabó, Beata; Lakatos, Agnes; Kõszegi, Tamás; Kátay, György; Botz, L

    2005-01-01

    The effect of stress conditions on the concentrations of secondary metabolites were examined during various developmental stages of Papaver somniferum plants. P. somniferum plants were grown in laboratory conditions (Budakalász). The experiment consisted of 22 treatments. Significantly different alkaloid contents can be observed under different stress conditions. In general, the alkaloid contents of plants are very low; therefore, a highly sensitive and reliable method has to be developed for analysis. The amount of alkaloids was measured by 2 separation and detection techniques. Accuracy of the thin-layer chromatography method for quantitative analysis is limited. Without purification of samples the background is too noisy. Column liquid chromatography is a sensitive and relatively inexpensive method that allows precise quantitative determination of the alkaloid content. PMID:16386012

  20. Analysis of anions in aqueous samples by ion chromatography and capillary electrophoresis

    Microsoft Academic Search

    S. L. Tamisier-Karolak; I. Le Potier; O. Barlet; M. Czok

    1999-01-01

    The object of this study is the comparison of two methods for the quantitative analysis of anions in aqueous samples: ion chromatography with conductimetric detection, and capillary zone electrophoresis with indirect photometric detection. The comparison includes modeling of experimental peaks as well as statistical validation criteria according to the recommendations of the International Conference on Harmonisation. In ion chromatography, peak

  1. An improved method for analysis of biomass sugars and galacturonic acid by anion exchange chromatography

    Microsoft Academic Search

    Wilbur Widmer

    2010-01-01

    The most accurate analysis method for sugars in biomass, based on gas chromatography, requires a time consuming and laborious\\u000a sample derivatation to trimethylsilanes or alditol acetates. In comparison, sample preparations for sugar analysis by liquid\\u000a chromatography are simple water dilutions. However, HPLC methods either require long analysis times, use of expensive solvents,\\u000a or do not give good resolution of sugars.

  2. US crude oil, natural gas, and natural gas liquids reserves

    SciTech Connect

    Not Available

    1990-10-05

    This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1989, and production volumes for the year 1989 for the total United States and for selected states and state sub-divisions. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), its two major components (nonassociated and associated-dissolved gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, two components of natural gas liquids, lease condensate and natural gas plant liquids, have their reserves and production reported separately. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. 28 refs., 9 figs., 15 tabs.

  3. Hydrocarbon Gas Liquids (HGL): Recent Market Trends and Issues

    EIA Publications

    2014-01-01

    Over the past five years, rapid growth in U.S. onshore natural gas and oil production has led to increased volumes of natural gas plant liquids (NGPL) and liquefied refinery gases (LRG). The increasing economic importance of these volumes, as a result of their significant growth in production, has revealed the need for better data accuracy and transparency to improve the quality of historical data and projections for supply, demand, and prices of these liquids, co-products, and competing products. To reduce confusion in terminology and improve its presentation of data, EIA has worked with industry and federal and state governments to clarify gas liquid terminology and has developed the term Hydrocarbon Gas Liquids, or HGL.

  4. Optimum design of space storable gas/liquid coaxial injectors.

    NASA Technical Reports Server (NTRS)

    Burick, R. J.

    1972-01-01

    Review of the results of a program of single-element, cold-flow/hot-fire experiments performed for the purpose of establishing design criteria for a high-performance gas/liquid (FLOX/CH4) coaxial injector. The approach and the techniques employed resulted in the direct design of an injector that met or exceeded the performance and chamber compatibility goals of the program without any need for the traditional 'cut-and-try' development methods.

  5. Computational fluid dynamics applied to gas-liquid contactors

    Microsoft Academic Search

    E. Delnoij; J. A. M. Kuipers; W. P. M. van Swaaij

    1997-01-01

    In this paper a ‘hierarchy of models’ is discussed to study the fluid dynamic behaviour of gas-liquid bubble columns. This ‘hierarchy of models’ consists of a Eulerian-Eulerian two fluid model, a Eulerian-Lagrangian discrete bubble model and a Volume Tracking or Marker Particle model. These models will be briefly reviewed and their advantages and disadvantages will be highlighted. In addition, a

  6. Chromatographic analysis of olopatadine in hydrophilic interaction liquid chromatography.

    PubMed

    Maksi?, Jelena; Jovanovi?, Marko; Raki?, Tijana; Popovi?, Igor; Ivanovi?, Darko; Jan?i?-Stojanovi?, Biljana

    2015-01-01

    In this paper, chromatographic analysis of active substance olopatadine hydrochloride, which is used in eye drops as antihistaminic agent, and its impurity E isomer by hydrophilic interaction liquid chromatography (HILIC) and application of design of experiments (DoE) methodology are presented. In addition, benzalkonium chloride is very often used as a preservative in eye drops. Therefore, the evaluation of its chromatographic behavior in HILIC was carried out as well. In order to estimate chromatographic behavior and set optimal chromatographic conditions, DoE methodology was applied. After the selection of important chromatographic factors, Box-Behnken design was utilized, and on the basis of the obtained models factor effects were examined. Then, multi-objective robust optimization is performed aiming to obtain chromatographic conditions that comply with several quality criteria simultaneously: adequate and robust separation of critical peak pair and maximum retention of the first eluting peak. The optimal conditions are identified by using grid point search methodology. The experimental verification confirmed the adequacy of the defined optimal conditions. Finally, under optimal chromatographic conditions, the method was validated and applicability of the proposed method was confirmed. PMID:25300592

  7. Analysis of anions in beer using ion chromatography.

    PubMed

    Bruce, Jonathan

    2002-01-01

    The majority of anions found in beer are a consequence of impurities derived from the water used during the brewing process. The process of beer manufacture consists of malting, brewing and fermentation followed by maturation before filtration and finally storage. Strict quality control is required because the presence of certain anions outside strictly defined tolerance limits can affect the flavour characteristics of the finished product. The anions present were quantified using the technique of ion chromatography with the Metrohm modular system following sample preparation. The analysis produced a result of the order 200 mg l(-1) for chloride, phosphate and sulphate and around 20 mg l(-1) for nitrate. If the chloride level exceeds 250 mg l(-1), then the sweetness of the beer is enhanced, but yeast flocculation can be hindered. An excess of sulphate can give a sharp, dry edge to hopped beers and excessive amounts of nitrate have been found to harm the yeast metabolism after conversion to the nitrite form. As water is a primary ingredient within beer, its quality and type is a fundamental factor in establishing many of the distinctive regional beers that can be found in the United Kingdom and is thus monitored carefully. PMID:18924733

  8. PETN homolog analysis and large-scale preparation of pure PETN homologs by high-performance liquid chromatography (HPLC)

    Microsoft Academic Search

    B. V. Barnhart; R. J. Schumacher

    2009-01-01

    A reverse-phase, high-performance, liquid chromatography (HPLC) technique was developed for the analysis of PETN and related nitrate esters to replace or supplement the subjective thin-layer chromatography (TLC) method currently in use.

  9. Industrial application of green chromatography - II. Separation and analysis of preservatives in skincare products using subcritical water chromatography.

    PubMed

    Yang, Y; Kapalavavi, B; Gujjar, L; Hadrous, S; Marple, R; Gamsky, C

    2012-10-01

    Several high-temperature liquid chromatography (HTLC) and subcritical water chromatography (SBWC) methods have been successfully developed in this study for separation and analysis of preservatives contained in Olay skincare creams. Efficient separation and quantitative analysis of preservatives have been achieved on four commercially available ZirChrom and Waters XBridge columns at temperatures ranging from 100 to 200°C. The quantification results obtained by both HTLC and SBWC methods developed for preservatives analysis are accurate and reproducible. A large number of replicate HTLC and SBWC runs also indicate no significant system building-up or interference for skincare cream analysis. Compared with traditional HPLC separation carried out at ambient temperature, the HTLC methods can save up to 90% methanol required in the HPLC mobile phase. However, the SBWC methods developed in this project completely eliminated the use of toxic organic solvents required in the HPLC mobile phase, thus saving a significant amount of money and making the environment greener. Although both homemade and commercial systems can accomplish SBWC separations, the SBWC methods using the commercial system for preservative analysis are recommended for industrial applications because they can be directly applied in industrial plant settings. PMID:22762371

  10. QUANTITATIVE ANALYSIS OF 68 POLAR COMPOUNDS FROM TEN CHEMICAL CLASSES BY DIRECT AQUEOUS INJECTION GAS CHROMATOGRAPHY

    EPA Science Inventory

    Porous polymer packings have been used successfully in many applications of direct aqueous injection gas chromatography. The authors have expanded the use of aqueous injection to the quantitative analysis of 68 alcohols, acetates, ketones, ethers, sulfides, aldehydes, diols, dion...

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

    EPA Science Inventory

    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...

  12. DYNAMIC MODELING STRATEGY FOR FLOW REGIME TRANSITION IN GAS-LIQUID TWO-PHASE FLOWS

    SciTech Connect

    X. Wang; X. Sun; H. Zhao

    2011-09-01

    In modeling gas-liquid two-phase flows, the concept of flow regime has been used to characterize the global interfacial structure of the flows. Nearly all constitutive relations that provide closures to the interfacial transfers in two-phase flow models, such as the two-fluid model, are often flow regime dependent. Currently, the determination of the flow regimes is primarily based on flow regime maps or transition criteria, which are developed for steady-state, fully-developed flows and widely applied in nuclear reactor system safety analysis codes, such as RELAP5. As two-phase flows are observed to be dynamic in nature (fully-developed two-phase flows generally do not exist in real applications), it is of importance to model the flow regime transition dynamically for more accurate predictions of two-phase flows. The present work aims to develop a dynamic modeling strategy for determining flow regimes in gas-liquid two-phase flows through the introduction of interfacial area transport equations (IATEs) within the framework of a two-fluid model. The IATE is a transport equation that models the interfacial area concentration by considering the creation and destruction of the interfacial area, such as the fluid particle (bubble or liquid droplet) disintegration, boiling and evaporation; and fluid particle coalescence and condensation, respectively. For the flow regimes beyond bubbly flows, a two-group IATE has been proposed, in which bubbles are divided into two groups based on their size and shape (which are correlated), namely small bubbles and large bubbles. A preliminary approach to dynamically identifying the flow regimes is provided, in which discriminators are based on the predicted information, such as the void fraction and interfacial area concentration of small bubble and large bubble groups. This method is expected to be applied to computer codes to improve their predictive capabilities of gas-liquid two-phase flows, in particular for the applications in which flow regime transition occurs.

  13. Analysis of global components in Ganoderma using liquid chromatography system with multiple columns and detectors.

    PubMed

    Qian, Zhengming; Zhao, Jing; Li, Deqiang; Hu, Dejun; Li, Shaoping

    2012-10-01

    In present study, a multiple columns and detectors liquid chromatography system for analysis of global components in traditional Chinese medicines was developed. The liquid chromatography system was consist of three columns, including size exclusion chromatography column, hydrophilic interaction chromatography column, and reversed phase chromatography column, and three detectors, such as diode array detector, evaporative light scattering detector, and mass spectrometry detector, based on column switching technique. The developed multiple columns and detectors liquid chromatography system was successfully applied to the analysis of global components, including macromolecular (polysaccharides), high (nucleosides and sugars)-, and low (triterpenes)-polarity small molecular compounds in Ganoderma, a well-known Chinese medicinal mushroom. As a result, one macromolecular chromatographic peak was found in two Ganoderma species, 19 components were identified in Ganoderma lucidum (two sugars, three nucleosides, and 14 triterpenes), and four components (two sugars and two nucleosides) were identified in Ganoderma sinense. The developed multiple columns and detectors liquid chromatography system was helpful to understand comprehensive chemical characters in TCMs. PMID:23007922

  14. High-Performance Liquid Chromatography Analysis of Spectrin Oligomerization

    Microsoft Academic Search

    Lars Löfvenberg; Lars Backman

    2001-01-01

    Gel filtration chromatography has been used to analyze the oligomerization of human erythrocyte spectrin. By applying an exponentially modified Gaussian function we have been able to resolve overlapping elution peaks. From these peaks it was possible to calculate the equilibrium composition of each spectrin concentration and thus also the dissociation constants describing the oligomeric process. The determined dissociation constants for

  15. ORGANIC WATER POLLUTANT ANALYSIS BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    Gas chromatography-mass spectrometry is a widely used technique for the identification of organic chemicals in water. This paper describes the gas chromatograph-mass spectrometer system, the preparation and separation of samples, the selection of ionizing processes, the integrati...

  16. Engineering aspects of gas-liquid catalytic reactions

    SciTech Connect

    Carra, S.; Santacesaria, E.

    1980-01-01

    A review of factors which affect selectivity and product yield in gas absorption with liquid-phase catalytic reaction and which must be considered in reactor design covers the chemistry and kinetics of homolytic and heterolytic oxidation reactions in the production, e.g., of acetic acid from butane catalyzed by cobalt acetate in a sparged reactor, hydroformylation, carbonylation, hydrogenation, and acid-base catalysis; mass transfer, phase equilibria, and the effect of the chemical reaction on mass transfer rates in gas-liquid reaction systems; modeling of reactors in which the gas is the dispersed phase, including stirred tank and bubble column reactors; and modeling of distillation with catalytic reaction.

  17. Surfactant effects on heat transfer at gas/liquid interfaces

    NASA Astrophysics Data System (ADS)

    Lopez, J. M.; Hirsa, A. H.

    2000-01-01

    A formulation of a canonical model to elucidate the interplay and competition between three primary sources of heat and mass transfer in non-isothermal systems with gas/liquid interfaces is presented. The nonlinear interaction between (i) buoyancy driven flow in the bulk, (ii) thermal Marangoni flow at the gas/liquid interface, and (iii) surfactant Marangoni flow at the interface is considered. A numerical model of the Navier-Stokes and energy equations is being developed for a simple, axisymmetric flow geometry. The boundary conditions for the Navier-Stokes equations are functions of the intrinsic viscoelastic properties of the interface, specifically the surface tension and the surface viscosities. A flow geometry which is amenable to both experiments and computations for elucidating the separate effects of the three mechanisms consists of an annular region bounded by a stationary inner and an outer cylinder and floor, and a free surface. The flow is driven by the temperature difference between the inner and outer cylinder which are set independently, and the floor is insulated. The predictions of the model for earth-g can be compared to laboratory measurements of the velocity field, and the surface temperature distribution. The predictions of the model for arbitrary gravity may be subsequently tested in the microgravity environment. .

  18. Preparative optical chromatography with external collection and analysis.

    PubMed

    Hart, Sean J; Terray, Alex; Arnold, Jonathan; Leski, Tomasz A

    2008-11-10

    Optical chromatography, used for particle separation, involves loosely focusing a laser into a fluid flowing opposite the direction of laser propagation. When microscopic particles in the flow path encounter this beam they are trapped axially along the beam and are pushed upstream from the laser focal point to rest at a point where the optical and fluid forces on the particle balance. Because optical and fluid forces are sensitive to differences in the physical and chemical properties of a particle, separations are possible. An optical chromatography beam which completely fills a fluid channel can operate as an optically tunable filter for the preparative separation of polymeric/colloidal and biological samples. We show how the technique can be used to separate injected samples containing large numbers of colloids. The power of optical chromatographic separations is illustrated through combination with epi-fluorescence microscopy and sample purification for real-time polymerase chain reaction (RT-PCR) detection of Bacillus anthracis spores. PMID:19581966

  19. High-performance liquid chromatography analysis of spectrin oligomerization.

    PubMed

    Löfvenberg, L; Backman, L

    2001-05-15

    Gel filtration chromatography has been used to analyze the oligomerization of human erythrocyte spectrin. By applying an exponentially modified Gaussian function we have been able to resolve overlapping elution peaks. From these peaks it was possible to calculate the equilibrium composition of each spectrin concentration and thus also the dissociation constants describing the oligomeric process. The determined dissociation constants for tetramer formation (1.3 microM) and for hexamer formation (24 microM) agree well with other measurements. PMID:11355854

  20. Analysis of post-harvest fungicides by micellar electrokinetic chromatography

    Microsoft Academic Search

    R. Rodr??guez; Y. Picó; J. Mañes

    2001-01-01

    A method based on solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC) was developed for the simultaneous determination of carbendazim, imazalil, methylthiophanate, O-phenylphenol, prochloraz, procimidone, thiabendazole and triadimefon residues in grape, lettuce, orange and tomato. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the type and concentration of surfactant and the methanol content in

  1. Analysis of non-saponifiable lipids by super-/subcritical-fluid chromatography.

    PubMed

    Lesellier, E

    2001-11-30

    Because of the particular properties of carbon dioxide or carbon dioxide/modifier mobile phases, super- or subcritical-fluid chromatography (SFC) can be an alternative to more classical chromatographic methods such as gas chromatography (GC) or high-performance liquid chromatography (HPLC) for the separation of unsaponifiable lipids. These fluids can also be helpful in the extraction and/or the concentration steps of sterols, tocopherols or carotenoids from complex samples. Supercritical extraction, off-line prefractionation or semi-preparative supercritical fluid chromatography, carried out before the analysis are described. The effects on separation of analytical parameters such as pressure, nature of and modifier percentage or stationary phase nature are also reported. The performance of capillary, packed or capillary packed columns is discussed, as well as the consequences of their use (choice of stationary phases, type of coupled detector). Numerous examples of fine separations are reported. PMID:11761001

  2. The application of a non-thermal plasma generated by gas-liquid gliding arc discharge in sterilization

    NASA Astrophysics Data System (ADS)

    Du, Chang Ming; Wang, Jing; Zhang, Lu; Xia Li, Hong; Liu, Hui; Xiong, Ya

    2012-01-01

    Gliding arc discharge has been investigated in recent years as an innovative physicochemical technique for contaminated water treatment at atmospheric pressure and ambient temperature. In this study we tested a gas-liquid gliding arc discharge reactor, the bacterial suspension of which was treated circularly. When the bacterial suspension was passed through the electrodes and circulated at defined flow rates, almost 100% of the bacteria were killed in less than 3.0 min. Experimental results showed that it is possible to achieve an abatement of 7.0 decimal logarithm units within only 30 s. Circulation flow rates and types of feeding gas caused a certain impact on bacteria inactivation, but the influences are not obvious. So, under the promise of sterilization effect, industrial applications can select their appropriate operating conditions. All inactivation curves presented the same three-phase profile showing an apparent sterilization effect. Analysis of the scanning electron microscope images of bacterial cells supports the speculation that the gas-liquid gliding arc discharge plasma is acting under various mechanisms driven essentially by oxidation and the effect of electric field. These results enhance the possibility of applying gas-liquid gliding arc discharge decontamination systems to disinfect bacterial-contaminated water. Furthermore, correlational research indicates the potential applications of this technology in rapid sterilization of medical devices, spacecraft and food.

  3. On The Validity of the Assumed PDF Method for Modeling Binary Mixing/Reaction of Evaporated Vapor in GAS/Liquid-Droplet Turbulent Shear Flow

    NASA Technical Reports Server (NTRS)

    Miller, R. S.; Bellan, J.

    1997-01-01

    An Investigation of the statistical description of binary mixing and/or reaction between a carrier gas and an evaporated vapor species in two-phase gas-liquid turbulent flows is perfomed through both theroetical analysis and comparisons with results from direct numerical simulations (DNS) of a two-phase mixing layer.

  4. Gas-liquid chromatographic determination of chlorinated norbornene derivatives in fish.

    PubMed

    Yurawecz, M P; Roach, J A

    1978-01-01

    1,2,3,4,7,7-Hexachloro-2,5-norbornadiene (I), 1,2,3,4,5-endo,7,7-heptachloro-2-norbornene (II), and 1,2,3,4,7,7-hexachloro-5,6-endo-epoxy-2-norbornene (III) have been identified as contaminants in Mississippi River fish by combined gas-liquid chromatography (GLC)-mass spectrometry. The method used to determine residues of these compounds, which are associated with production of the pesticide endrin, is similar to the AOAC multiresidue method for chlorinated pesticides. The residues are extracted from the sample with acetonitrile, transferred to petroleum ether, and chromatographed on a Florisil column. Compounds I and II are eluted from the Florisil with petroleum ether and compound III is eluted with ethyl ether-petroleum ether (6 + 94). The concentrated eluates are analyzed by using electron capture GLC. The method provides adequate recoveries of all 3 chlorinated norbornene derivatives and allows quantitation at or below the 0.05 ppm level in fish with a 20 mg sample equivalent injection. PMID:621191

  5. Mass Accommodation and Chemical Reaction at Gas-Liquid Interfaces

    NASA Astrophysics Data System (ADS)

    Kolb, C. E.; Williams, L. R.; Jayne, J. T.; Worsnop, D. R.; Davidovits, P.

    2006-12-01

    The uptake of trace gases by liquid surfaces is an important process that initiates the heterogeneous chemistry of liquid aerosol particles and cloud droplets. We have recently reviewed the available experimental data for liquid aqueous and aqueous/organic surfaces (1). The review highlights some inconsistencies among experimental results and between experimental results and molecular dynamics simulations. Some of these inconsistencies will be evaluated and discussed in terms of the physics of liquid interfaces, the limitations of various experimental techniques and the disparate scales of laboratory experiments and current molecular simulations (1, 2). 1. Davidovits, P., Kolb, C. E., Williams, L. R., Jayne, J. T., Worsnop, D. R., 2006, Mass Accommodation and Chemical Reactions at Gas Liquid Interfaces, Chem. Rev. 106, 1323-1354. 2. Garrett, B. C., Schenter, G. K., Morita, A., 2006, Molecular Simulations of Molecules across the Liquid/Vapor Interface of Water, Chem. Rev. 106, 1355-1374.

  6. CARBON DIOXIDE SEPARATION BY PHASE ENHANCED GAS-LIQUID ABSORPTION

    SciTech Connect

    Liang Hu

    2004-09-30

    A new process called phase enhanced gas-liquid absorption has been developed in its early stage. It was found that adding another phase into the absorption system of gas/aqueous phase could enhance the absorption rate. A system with three phases was studied. In the system, gas phase was carbon dioxide. Two liquid phases were used. One was organic phase. Another was aqueous phase. By addition of organic phase into the absorption system of CO{sub 2}-aqueous phase, the absorption rate of CO{sub 2} was increased significantly. CO{sub 2} finally accumulated into aqueous phase. The experimental results proved that (1) Absorption rate of carbon dioxide was enhanced by adding organic phase into gas aqueous phase system; (2) Organic phase played the role of transportation of gas solute (CO{sub 2}). Carbon dioxide finally accumulated into aqueous phase.

  7. Decomposition of phenol by hybrid gas\\/liquid electrical discharge reactors with zeolite catalysts

    Microsoft Academic Search

    Hrvoje Kuši?; Natalija Koprivanac; Bruce R. Locke

    2005-01-01

    Application of hybrid gas\\/liquid electrical discharge reactors and a liquid phase direct electrical discharge reactor for degradation of phenol in the presence and absence of zeolites have been investigated. Hybrid gas\\/liquid electrical discharges involve simultaneous high voltage electrical discharges in water and in the gas phase above the water surface leading to the additional OH radicals in the liquid phase

  8. A variational approach to motion of triple junction of gas, liquid and solid

    E-print Network

    Soatto, Stefano

    A variational approach to motion of triple junction of gas, liquid and solid Kensuke Yokoia;b;c;1 a to deal with motion of triple junctions of gas, liquid (or two kinds of uid) and solid based on the level set method [1{4]. In Eulerian framework, to simulate interaction between a moving solid object

  9. Design of a Gas-Liquid Unbaffled Stirred Tank with a Concave Blade Impeller

    NASA Astrophysics Data System (ADS)

    Devi, T. T.; Kumar, Bimlesh

    2015-01-01

    Experimental investigation of unbaffled multiphase (gas-liquid) stirred tanks is conducted with the use of a concave blade impeller to analyze mass transfer, gassed power, and gas holdup. The experiments are carried out with various impeller diameter to tank diameter ratios and impeller clearances. The design criterion for the mass transfer rate is proposed, and its prediction capability is found to be satisfactory. The results show that the gassed power is dependent on the impeller diameter to tank diameter ratio and impeller clearance. The design criteria for gassed power to ungassed power ratio and gas holdup are also introduced. Multiphase modeling is done by employing the computational fluid dynamics (CFD) techniques to observe the characteristic flow pattern transition and to carry out a qualitative analysis of the mass transfer rate.

  10. Asymptotic stability of the compressible gas-liquid model with well-formation interaction and gravity

    NASA Astrophysics Data System (ADS)

    Evje, Steinar; Liu, Qingqing; Zhu, Changjiang

    2014-11-01

    In this paper we are concerned with the initial-boundary value problem of the compressible gas-liquid model with well-formation interaction and gravity. The asymptotic behavior of solutions to steady states is established. Also the time-decay rates of perturbed solutions in the sense of L? norm are obtained under some suitable assumptions on the initial date, if ?>1 (associated with pressure law of gas) and ??(0,?/2]?(0,?-??)?(0,?+?/?3] where ? characterizes the viscosity coefficient and ? describes the mass decay rate at the boundary. A main purpose of this work is to clarify the role played by the well-reservoir interaction term. The analysis demonstrates that it is essential to take into account information about sign as well as size of the interaction term in order to obtain time-independent estimates when it operates in combination with gravity.

  11. COMPARATIVE EVALUATION OF GC/MS (GAS CHROMATOGRAPHY/MASS SPECTROMETRY) DATA ANALYSIS PROCESSING

    EPA Science Inventory

    Mass spectra obtained by fused silica capillary gas chromatography/mass spectrometry/data system (GC/MS/DS) analysis of mixtures of organic chemicals adsorbed on Tenax GC cartridges was subjected to manual and automated interpretative techniques. Synthetic mixtures (85 chemicals ...

  12. ANALYSIS OF NITRITE IN NO2 DIFFUSION TUBES USING ION CHROMATOGRAPHY

    EPA Science Inventory

    An analytical method was developed for the analysis of the NO2 collected by a passive diffusion controlled atmospheric sampling device. The method measured the total amount of nitrite ion using ion chromatography. The precision obtained under field conditions, defined as twice th...

  13. Analysis and Identification of Acid-Base Indicator Dyes by Thin-Layer Chromatography

    ERIC Educational Resources Information Center

    Clark, Daniel D.

    2007-01-01

    Thin-layer chromatography (TLC) is a very simple and effective technique that is used by chemists by different purposes, including the monitoring of the progress of a reaction. TLC can also be easily used for the analysis and identification of various acid-base indicator dyes.

  14. ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

    EPA Science Inventory

    A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

  15. GAS CHROMATOGRAPHY/MATRIX ISOLATION - INFRARED SPECTROMETRY FOR AIR SAMPLE ANALYSIS

    EPA Science Inventory

    This report describes the application of gas chromatography/matrix- solation infrared (GC/MI-IR) spectrometry to the analysIs of environmental air sample extracts. Samples that were analyzed include extracts from woodsmoke-impacted air, XAD-2 blanks, indoor air, and carpet sample...

  16. A multivariate statistical analysis approach to analyze gas chromatography-olfactometry data of tangerine hybrids

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Gas chromatography (GC) hyphenated with olfactometry (O) when a human subject smells the effluent of the GC is a useful technique to identify aroma activity of volatile compounds in a food. Many techniques have been developed, based on olfactory thresholds (CHARM analysis, AEDA), or based on psychop...

  17. Third-order gas-liquid phase transition and the nature of Andrews critical Tian Ma and Shouhong Wang

    E-print Network

    Wang, Shouhong

    Third-order gas-liquid phase transition and the nature of Andrews critical point Tian Ma-order gas-liquid phase transition and the nature of Andrews critical point Tian Ma1 and Shouhong Wang2 1 is to study the nature of the Andrews critical point in the gas-liquid transition in a physical

  18. Displacement chromatography as first separating step in online two-dimensional liquid chromatography coupled to mass spectrometry analysis of a complex protein sample--the proteome of neutrophils.

    PubMed

    Trusch, Maria; Tillack, Kati; Kwiatkowski, Marcel; Bertsch, Andreas; Ahrends, Robert; Kohlbacher, Oliver; Martin, Roland; Sospedra, Mireia; Schlüter, Hartmut

    2012-04-01

    Displacement chromatography provides some advantages over elution chromatography such as the opportunity to enrich trace amounts of molecules and to elute molecules in highest concentrations achievable with liquid chromatography. In a previous study we demonstrated that displacement chromatography is a well-suited alternative to gradient elution in an offline two-dimensional (2D-)LC-MS approach for the analysis of proteomes. In this study we present a method for applying displacement chromatography in an online 2D-LC-MS system including a cation exchange (CEX) column and a reversed phase column. We circumvented the problem of determining the sample capacity of the CEX column by repeated injection (pulses) of sample aliquots monitored by an LC-MS analysis of each flow-through fraction of the CEX column. Elution of tryptic peptides from the CEX column was achieved by repeated injection (pulses) of the displacer spermine. Pulsed displacer injections offer the advantage through physical separation of preventing post-column mixing of already separated compounds. As a proof of principle we analyzed the cytosolic proteome of human neutrophils. PMID:22391494

  19. Analysis of phytosterols and phytostanols in enriched dairy products by Fast gas chromatography with mass spectrometry.

    PubMed

    Inchingolo, Raffaella; Cardenia, Vladimiro; Rodriguez-Estrada, Maria Teresa

    2014-10-01

    A Fast gas chromatography and mass spectrometry method for plant sterols/stanols analysis was developed, using a short capillary gas chromatography column (10 m × 0.1 mm internal diameter × 0.1 ?m film thickness) coated with 5% diphenyl-polysiloxane. A silylated mixture of the main plant sterols/stanols standards (?-sitosterol, campesterol, stigmasterol, campestanol, sitostanol) was well separated in 1.5 min, with a good peak resolution (>1.4, determined on a critical chromatographic peak pair (?-sitosterol and sitostanol)), repeatability (<13%), and sensitivity (<0.017 ng/mL). The suitability of this Fast chromatography method was tested on plant sterols/stanols-enriched dairy products (yogurt and milk), which were subjected to lipid extraction, cold saponification, and silylation prior to injection. The analytical performance (sensitivity < 0.256 ng/mL and repeatability < 10.36%) and significant reduction of the analysis time and consumables demonstrate that Fast gas chromatography-mass spectrometry method could be also employed for the plant sterols/stanols analysis in functional dairy products. PMID:25069661

  20. Multiresidue analysis of pesticides in soil by gas chromatography with nitrogen-phosphorus detection and gas chromatography mass spectrometry.

    PubMed

    Fenoll, José; Hellín, Pilar; Marín, Cristóbal; Martínez, Carmen M; Flores, Pilar

    2005-10-01

    A rapid multiresidue method for the simultaneous determination of 25 fungicides and insecticides in soil was developed. Soil samples are extracted by sonication with a water-acetonitrile mixture, and the pesticides are partitioned into dichloromethane. Final determination was made by gas chromatography (GC) with nitrogen-phosphorus detection (NPD). Confirmation analysis of pesticides was carried out by GC-MS in the selected ion monitoring (SIM) mode. The identification of compounds was based on retention time and on comparison of the primary and secondary ions. The average recovery by the GC-NPD method obtained for these compounds varied from 68.5% to 112.1% with a relative standard deviation between 1.8% and 6.2%. The GC-NPD method presents good linearity over the range assayed 50-2000 microg/L, and the detection limit for the pesticides studied varied from 0.1 to 10.4 microg/kg. The proposed method was used to determine pesticide levels in soil samples from experimental greenhouse pepper cultivation. PMID:16190613

  1. NASA Li/CF(x) cell problem analysis: Anion exchange chromatography analysis

    NASA Astrophysics Data System (ADS)

    Bytella, Joseph

    1991-05-01

    An analysis was made of wiper samples used to wipe down lithium/chlorine fluorine battery components and production equipment. These components and equipment were potentially exposed to thionyl chloride vapors. In the presence of moisture, thionyl chloride decomposes to sulfur dioxide and hydrogen chloride. The wiper samples were analyzed for soluble chlorides and fluorides by anion exchange chromatography. During the examination of the test chromatographs, fluoride contamination was discovered in wiper samples from the test equipment. An analytical method to determine fluoride was developed. The first 3 extracts from the potentially exposed and clean wiper samples were tested, and the total fluoride from both groups determined. A comparison of the results from both groups was made to determine the extent of fluoride contamination.

  2. Analysis of waterborne paints by gas chromatography–mass spectrometry with a temperature-programmable pyrolyzer

    Microsoft Academic Search

    Sadao Nakamura; Masahiko Takino; Shigeki Daishima

    2001-01-01

    Gas chromatography–mass spectrometry (GC–MS) with a temperature-programmable pyrolyzer was used for the analysis of waterborne paints. Evolved gas analysis (EGA) profiles of the waterborne paints were obtained by this temperature-programmed pyrolysis directly coupled with MS via a deactivated metal capillary tube. The EGA profile suggested the optimal thermal desorption conditions for solvents and additives and the subsequent optimal pyrolysis temperature

  3. Analysis of sugars in environmental samples by gas chromatography–mass spectrometry

    Microsoft Academic Search

    Patricia M. Medeiros; Bernd R. T. Simoneit

    2007-01-01

    Many environmental samples contain complex mixtures of organic compounds with different sources, polarities and reactivities. This study reports a method for the analysis of both polar\\/water-soluble and apolar organic compounds in several kinds of environmental samples. The analytical method consists of extraction with a mixture of dichloromethane:methanol (2:1, v\\/v), silylation using BSTFA (N,O-bis-(trimethylsilyl)trifluoroacetamide) and analysis by gas chromatography–mass spectrometry (GC–MS),

  4. Insecticide Residues in Baby Food, Animal Feed, and Vegetables by Gas Liquid Chromatography

    Microsoft Academic Search

    I. Mukherjee; M. Gopal

    1996-01-01

    India is among a few developing countries where organochlorines are still used for controlling pests due to economic constraints. DDT and HCH are still used for controlling pests of public, health especially malaria vector. The residues of these pesticides are known to find their way into milk and milk products (Mukherjee and Gopal 1992a). In our earlier publication (Mukherjee and

  5. Headspace profiles of modified atmosphere packaged fresh red snapper (Lutjanus campechanus) by gas liquid chromatography

    E-print Network

    Scorah, Craig Darrell Allen

    1988-01-01

    thanks is given to the author's big brother, Mr. Todd Scorah, for his encouragement to keep going when the deck was stacked against me. Sincere thanks is given to Ms. Veronica Rosas, for all the time she gave-up and the effort she put into the typing...

  6. Headspace profiles of modified atmosphere packaged fresh red snapper (Lutjanus campechanus) by gas liquid chromatography 

    E-print Network

    Scorah, Craig Darrell Allen

    1988-01-01

    by CRAIG DARRELL ALLEN SCORAH Approved as to style and content by: Gunnar Finne ( o-Ch ' an of Committee) Carl Vander ant (Co ? Chairman of o ittee) Leon Russell, Jr. (Member) aries W. Dill (Member) Gary C. Smith (Head of Department) May 1988... Finne R d pp* )L~t' ~h) f'll t p k g d polyethylene barrier pouches backflushed with air and C02 enriched atmospheres were stored at 4 C and 15 C. At regular time intervals, the headspace within the packages was analyzed for atmospheric composition...

  7. Amino acid composition of single seeds and cotyledons of some brassica species by gas liquid chromatography

    Microsoft Academic Search

    L.-A. Appelqvist; Baboo M. Nair

    1977-01-01

    There are considerable differences in amino acid pattern between the seed coat and the embryo (separated after 5 h of imbibition in water) but only minor differences between the various embryonic parts, the hypocotyl, the inner and outer cotyledons. Thus, the seed coat is high in proline and hydroxyproline and relatively low in glutamic acid. No change in amino acid

  8. Use of gas liquid chromatography for monitoring the fatty acid composition of canadian rapeseed

    Microsoft Academic Search

    J. K. Daun; P. B. Mazur; C. J. Marek

    1983-01-01

    Since 1972, Canadian rapeseed has been changing from high erucic acid types to low erucic acid types. In 1970, the Canadian\\u000a Grain Commission instituted a program to monitor the fatty acid composition of rapeseed at the farm level, in railway carlot\\u000a shipments and in export cargo shipments. Initially, in order to process up to 20,000 samples per year, a combined

  9. Quantitative Aging Pattern in Mouse Urine Vapor as Measured by Gas-Liquid Chromatography

    NASA Technical Reports Server (NTRS)

    Robinson, Arthur B.; Dirren, Henri; Sheets, Alan; Miquel, Jaime; Lundgren, Paul R.

    1975-01-01

    We have discovered a quantitative aging pattern in mouse urine vapor. The diagnostic power of the pattern has been found to be high. We hope that this pattern will eventually allow quantitative estimates of physiological age and some insight into the biochemistry of aging.

  10. Determination of physicochemical properties of some fatty acid methyl esters by gas liquid chromatography

    Microsoft Academic Search

    Sajid Husain; P. Nageswara Sarma; G. Y. S. K. Swamy; K. Sita Devi

    1993-01-01

    Physicochemical data such as vapor pressures (p0), heats of vaporization (?Hv), activity coefficents at infinite dilution (??) and excess partial molar entropy (?S\\u000a e\\u000a 0\\u000a ) are considered important for conducting unit processes and designing reactor equipment. Scanty information regarding such\\u000a data is available in the literature for the higher fatty acid methyl esters. The objective of this research was

  11. A Multidimensional Chromatography Technology for In-depth Phosphoproteome Analysis

    Microsoft Academic Search

    Claudio P. Albuquerque; Marcus B. Smolka; Samuel H. Payne; Vineet Bafna; Jimmy Eng; Huilin Zhou

    2008-01-01

    Protein phosphorylation is a post-translational modifica- tion widely used to regulate cellular responses. Recent studies showed that global phosphorylation analysis could be used to study signaling pathways and to identify targets of protein kinases in cells. A key objective of global phosphorylation analysis is to obtain an in-depth mapping of low abundance protein phosphorylation in cells; this necessitates the use

  12. Analysis of organic/inorganic analytes in environmental samples by packed capillary chromatography

    SciTech Connect

    Burford, M.D.; Robson, M.M.; Mitchell, S.C. [Univ. of Leeds (United Kingdom)] [and others

    1995-12-31

    Recent progress in the development of techniques for packing of high efficiency capillary columns has enabled the concept of unified chromatography to be realised. Packed capillary columns offer the advantages of both packed column (high loading capacity, wide range of stationary phases) and capillary column (speed of analysis, high resolution) techniques to produce a versatile and efficient analytical procedure. For the detailed investigation of fossil fuel and environmental samples the rapid growth of packed capillary chromatography offers the unique opportunity to analyse both organic and inorganic components as the column can be operated in both gas chromatography (GC) and supercritical fluid chromatography (SFC) modes. In this study, the use of packing capillary columns, prepared in-house is investigated for both high pressure GC and SFC using helium and CO{sub 2} as the mobile phase respectively. Several spiked and real world samples have been used to demonstrate the potential of packed capillary columns in the analysis of organic and inorganic analytes in fuel and environmental samples.

  13. Carbohydrate Analysis of Bradyrhizobial (NC 92) Lipopolysaccharides by High Performance-Anion Exchange Chromatography with Pulsed Amperometric Detection

    Microsoft Academic Search

    Hasi Das; Vani Jayaraman; Indranil Bhattacharya

    1999-01-01

    Composition analysis of monosaccharides of Sepharose 4B purified NC 92 LPS and the polysaccharides fractions from Sephadex G-50 chromatography was performed by high performance anion exchange chromatography using pulsed amperometric detection. Rhamnose, mannose, galactose and glucose are present in a substantial amount in the purified LPS (Pk I). High molecular weight purified polysaccharides (PS I) obtained after sephadex gel filtration

  14. Argentation high performance liquid chromatography on-line coupled to gas chromatography for the analysis of monounsaturated polyolefin oligomers in packaging materials and foods.

    PubMed

    Lommatzsch, Martin; Biedermann, Maurus; Simat, Thomas J; Grob, Koni

    2015-07-10

    Multidimensional chromatography based on two-dimensional high performance liquid chromatography on-line coupled to gas chromatography (on-line HPLC-HPLC-GC) enables the separate analysis of saturated, monounsaturated and aromatic hydrocarbons in packaging materials like polyolefins or paperboard and their migrates into foods. Since normal-phase HPLC on silica gel did not preseparate saturated from monounsaturated hydrocarbons, a separation step on a normal-phase HPLC column treated in the laboratory with an optimized amount of silver nitrate was added. The preparation of this HPLC column and the instrumental set-up are described, followed by examples showing the potential of the method. In a preliminary investigation of 11 polyolefin granulates for food contact up to 40% monounsaturated hydrocarbons among the oligomers C16-35 were determined. PMID:26037318

  15. SUPERCRITICAL FLUID CHROMATOGRAPHY FOR HIGH MOLECULAR WEIGHT ORGANIC ANALYSIS

    EPA Science Inventory

    The report describes a preliminary application of supercritical fluid mass spectrometry (MS) techniques to the analysis of a middle distillate fuel, an emission particulate extract, and the emission particulates themselves. These techniques include capillary column supercritical ...

  16. A Management Tool for Analyzing CHP Natural Gas Liquids Recovery System 

    E-print Network

    Olsen, C.; Kozman, T. A.; Lee, J.

    2008-01-01

    The objective of this research is to develop a management tool for analyzing combined heat and power (CHP) natural gas liquids (NGL) recovery systems. The methodology is developed around the central ideas of product recovery, possible recovery...

  17. Upward Gas-Liquid Flow in Concentric and Eccentric Annular Spaces 

    E-print Network

    Cavalcanti de Sousa, Pedro

    2013-12-09

    A limited amount of work exists on upward gas-liquid flow in annular spaces. This is a common scenario in drilling operations, especially in underbalanced drilling, and in high-production wells. To carry out this study, a ...

  18. The application of chromatography to the analysis of pharmaceutical creams

    Microsoft Academic Search

    F. J. van de Vaart; A. W. M. Indemans; A. Hulshoff; O. A. Lake

    1982-01-01

    The application of GLC, HPLC and TLC to the analysis of pharmaceutical creams is discussed with special attention to sample clean-up. The results of the determination of hydrocortisone acetate, salicylic acid, benzoic acid, diethyl stilbestrol, chloramphenicol, diphenhydramine HCl, tretinoin and some cream base components by reversed phase HPLC are given.

  19. The identification of mycoplasma species by gas chromatography 

    E-print Network

    Shult, Milton Donald

    1969-01-01

    method to identify myco- plasma at the species level because of their minimal bio- chemical activity and their pleomorphism . Recent reports have indicated that the use of gas-liquid chromatography of cellular components is feasible...THE IDENTIFICATION OF MYCOPLASMA SPECIES BY GAS CHROMATOGRAPHY A Thesis MILTON DONALD SHULT& JR. Submitted to the Graduate College of Texas AFM University in partial fulfillment of the requirement for the degree of MASTER OF SCIENCE May 1969...

  20. CFD simulation of mixing in tall gas–liquid stirred vessel: Role of local flow patterns

    Microsoft Academic Search

    A. R. Khopkar; G. R. Kasat; A. B. Pandit; V. V. Ranade

    2006-01-01

    In this work, we have used the computational fluid dynamics (CFD)-based models to investigate the gas–liquid flows generated by three down-pumping pitched blade turbines. A two-fluid model along with the standard k–? turbulence model was used to simulate the dispersed gas–liquid flow in a stirred vessel. Appropriate drag corrections to account for bulk turbulence [Khopkar and Ranade, 2005. CFD simulation

  1. Microporous hydrophobic hollow fiber modules for gas-liquid phase separation in microgravity

    Microsoft Academic Search

    Gary Noyes

    1993-01-01

    Gas-liquid interphase mass transfer operations, such as gas-liquid phase separation, gas absorption into liquid or dissolved gas separation from liquid, gas humidification and drying via liquid contact, and evaporative cooling are readily accomplished on the Earth with settling\\/spray chambers, packed towers, or bubble columns. This paper reports on gas-water mass transfer tests performed utilizing microporous hydrophobic Hollow Fiber Modules (HFMs)

  2. Reuse of spent natural gas liquid sweetening solutions

    SciTech Connect

    Hahn, W.J.; McKim, M.N.; Smith, L.S.

    1995-12-01

    Partially spent caustic solutions from natural gas liquids (NGL) sweetening processes can be used as reagent for sulfur dioxide (SO{sub 2}) scrubbing facilities, reducing the costs for purchasing scrubber reagent and eliminating the costs and liabilities associated with waste disposal. This paper discusses: (1) the characteristics of typical spent NGL sweetening solutions, (2) State and Federal regulations governing the disposal of these solutions as wastes, (3) the operational variables affecting reuse of these solutions in SO{sub 2} scrubbers, (4) field and laboratory analytical data from a pilot project conducted to evaluate the reuse of a partially spent NGL sweetening solution as SO{sub 2} scrubber reagent, and (5) economic data from the pilot project. For the pilot project, a partially spent caustic NGL sweetening solution was used in place of soda ash solution as reagent in a SO{sub 2} scrubber serving two steam generators burning sour gas. Emissions testing of the scrubber demonstrated that the solution provided effective removal of oxides of sulfur (SO{sub x}) in both gaseous and particulate phases to meet permitted limits. Data from the pilot project is used in the paper to: (1) quantify SO{sub 2} scrubber performance with partially spent caustic solutions in terms of SO{sub x} removal efficiency, (2) identify the necessary modifications in scrubber operation (reagent feed rate, scrubber liquor pH and specific gravity, blowdown rate) to achieve acceptable performance using partially spent caustic solutions, and (3) describe the effect that the use of partially spent caustic solutions has on physical and chemical properties of scrubber liquor.

  3. Quantitative analysis of food fatty acids by capillary gas chromatography

    Microsoft Academic Search

    H. T. Slover; E. Lanza

    1979-01-01

    The superior efficiency of capillary columns is desirable for the gas chromatographic analysis of complex mixtures of fatty\\u000a acids, but there have been some reservations regarding quantitation and reproducibility. This paper discusses the use of wall-coated\\u000a glass capillary columns in a semiautomated system for the determination of food fatty acids. Glass columns coated with SP2340\\u000a were used for extended periods

  4. Analysis of oxyhalides in water by ion chromatography–ionspray mass spectrometry

    Microsoft Academic Search

    L Charles; D Pépin

    1998-01-01

    A sensitive method for analyzing chlorite, chlorate, bromate and iodate in water by ion chromatography (IC) coupled with ionspray tandem mass spectrometry (IS-MS–MS) has been developed. Prior to analysis, samples were subjected to off-line sample clean-up with Ba, Ag and H-form resins to remove sulfate, chloride and hydrogencarbonate, respectively. Oxyhalides in the purified samples were concentrated and separated on a

  5. Targeted multidimensional gas chromatography for the quantitative analysis of suspected allergens in fragrance products

    Microsoft Academic Search

    Michael S. Dunn; Natalie Vulic; Robert A. Shellie; Simon Whitehead; Paul Morrison; Philip J. Marriott

    2006-01-01

    Two approaches are described and compared for the analysis of suspected allergens (SAs) in fragrance products, which are defined by the Scientific Committee of Cosmetics and Non-Food Products (SCCNFP). The first consists of a comprehensive two-dimensional gas chromatography (GC×GC) experiment using both a “conventional” non-polar\\/polar column combination and an “inverse” polar\\/non-polar column set. The second approach uses a targeted multidimensional

  6. RECENT ADVANCES IN ULTRA-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY FOR THE ANALYSIS OF TRADITIONAL CHINESE MEDICINE

    PubMed Central

    Huang, Huilian; Liu, Min; Chen, Pei

    2014-01-01

    Traditional Chinese medicine has been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra-high performance liquid chromatography (UHPLC) is a relatively new technique offering new possibilities. This paper reviews recent developments in UHPLC in the separation and identification, fingerprinting, quantification, and metabolism of traditional Chinese medicine. Recently, the combination of UHPLC with MS has improved the efficiency of the analysis of these materials. PMID:25045170

  7. Rapid Analysis of Multiresidual Pesticides in Agricultural Products by Gas Chromatography-mass Spectrometry

    Microsoft Academic Search

    Libin Liu; Hashi Yuki; Yaping Qin; Haixia Zhou; Jinming Lin

    2006-01-01

    A method for the rapid analysis of multiresidual pesticides in agricultural products using gas chromatography-mass spectrometry (GC\\/MS) was introduced. The matrix solid-phase dispersion (MSPD) technique with slight modification was employed to minimize the matrix interferences. To calculate the recovery, 97 target pesticides were spiked into a range of foods including potato, cabbage, carrot, apple, orange, cucumber, and rice. The combination

  8. Analysis of formose sugar and formaldehyde by high-performance liquid chromatography

    Microsoft Academic Search

    Senad Novalin

    2009-01-01

    Formose sugar and formaldehyde (HCHO) were analyzed using high-performance liquid chromatography (HPLC) utilizing a CarboPac PA1 column (Dionex) and pulsed amperometric detection. This HPLC system was unsuitable for the analysis of formose sugar and HCHO and thus reducing sugars and unconverted HCHO were determined by endowing them with charges through a derivatization method using 2,4-dinitrophenylhydrazine. The separation and detection of

  9. Nitric oxide in biological fluids: analysis of nitrite and nitrate by high-performance ion chromatography

    Microsoft Academic Search

    Steven A. Everett; Madeleine F. Dennis; Gillian M. Tozer; Vivien E. Prise; Peter Wardman; Michael R. L. Stratford

    1995-01-01

    The analysis of nitric oxide-derived nitrite and nitrate ions in biological fluids represents a proven strategy for determining nitric oxide participation in a diverse range of physiological and pathophysiological processes in vivo. In this article we describe a versatile method for the simultaneous measurement of NO2? and NO3? anions in both plasma and isolated tumour models based on anion-exchange chromatography

  10. Ultraperformance liquid chromatography with electrospray ionization ion trap mass spectrometry for chondroitin disaccharide analysis

    Microsoft Academic Search

    Kemal Solakyildirim; Zhenqing Zhang; Robert J. Linhardt

    2010-01-01

    Chondroitin sulfate (CS) has an important role in cell division, in the central nervous system, and in joint-related pathologies such as osteoarthritis. Due to the complex chemical structure and biological importance of CS, simple, sensitive, high resolution, and robust analytical methods are needed for the analysis of CS disaccharides and oligosaccharides. An ion-pairing, reversed-phase, ultraperformance liquid chromatography (IPRP–UPLC) separation, coupled

  11. CRC handbook of chromatography

    SciTech Connect

    Qureshi, M.

    1986-01-01

    This book provides technology for routine analysis or developing new methods of chromatography or organic materials. In this book Section 1 presents the principles, techniques, quantitative determinations and detection methods used in chromatographic analysis. In the major part of the book, Section 2 summarizes data in voluminous tabular/graphic form on paper, thin layer, liquid and gas chromatography. Section 3 lists important books on electrophoreses, gel permeation chromatography, and ion exchange, in addition to the other forms of chromatography.

  12. Analysis of gossypol by high performance liquid chromatography.

    PubMed

    Wang, M Z

    1987-06-01

    Several high performance liquid chromatographic methods for the analysis of gossypol in different kinds of sample were developed. (1) Pure gossypol: separation on C18 column with MeOH/H2O/CHCl3 (70:30:40) containing 0.1% H3PO4 as mobile phase or on SO3H column with MeOH/citrate buffer (pH 6.3) (55:45) as mobile phase was recommended. With these systems, minute amounts of contaminants difficult to separate by other HPLC systems could be determined. (2) Plant material: acetone was selected as the extraction solvent. After evaporation of acetone from the extract, the residue was redissolved in 1% HOAc in CHCl3. An aliquot of this solution was chromatographed and quantified by peak area method. The mean recovery of pure gossypol added to plant material was 91.1 +/- 1.1% (S.D.). (3) Plasma sample: a HPLC method with electrochemical detector was developed. A plasma sample with glutathione as protective agent and gossypol dimethyl ether as internal standard was introduced on to a C18 pre-column. By using column-switching technique, a certain part of the eluate containing gossypol and gossypol dimethyl ether was subjected to a C8 analytical column for further separation. MeOH/citrate buffer (pH 3.2) (80:20) was used as the mobile phase. The optimum potential for detection was +0.6 V vs. Ag-AgCl. The assay sensitivity was 5 ng/ml. This method is sensitive and selective, suitable for clinical pharmacokinetic studies. PMID:3626590

  13. Supercritical fluid chromatography with photodiode array detection for pesticide analysis in papaya and avocado samples.

    PubMed

    Pano-Farias, Norma S; Ceballos-Magaña, Silvia G; Gonzalez, Jorge; Jurado, José M; Muñiz-Valencia, Roberto

    2015-04-01

    To improve the analysis of pesticides in complex food matrices with economic importance, alternative chromatographic techniques, such as supercritical fluid chromatography, can be used. Supercritical fluid chromatography has barely been applied for pesticide analysis in food matrices. In this paper, an analytical method using supercritical fluid chromatography coupled to a photodiode array detection has been established for the first time for the quantification of pesticides in papaya and avocado. The extraction of methyl parathion, atrazine, ametryn, carbofuran, and carbaryl was performed through the quick, easy, cheap, effective, rugged, and safe methodology. The method was validated using papaya and avocado samples. For papaya, the correlation coefficient values were higher than 0.99; limits of detection and quantification ranged from 130-380 and 220-640 ?g/kg, respectively; recovery values ranged from 72.8-94.6%; precision was lower than 3%. For avocado, limit of detection values were ?450 ?g/kg; precision was lower than 11%; recoveries ranged from 50.0-94.2%. Method feasibility was tested for lime, banana, mango, and melon samples. Our results demonstrate that the proposed method is applicable to methyl parathion, atrazine, ametryn, and carbaryl, toxics pesticides used worldwide. The methodology presented in this work could be applicable to other fruits. PMID:25641906

  14. Emerging liquid chromatography-mass spectrometry technologies improving dried blood spot analysis.

    PubMed

    Rao, Ramisetti Nageswara

    2014-08-01

    Dried blood spots (DBS), a micro blood sampling technique, has recently gained interest in drug discovery and development due to its inherent advantages over the conventional whole blood, plasma or serum sample collection. Since the regulatory authorities have agreed to the use of blood as an acceptable biological matrix for drug exposure measurements, its applications have been extended not only to therapeutic drug monitoring but also to toxicokinetic and pharmacokinetic studies. The pharmaceutical industry is keen to promote DBS as a prominent tool in bioanalytical applications due to the financial, ethical and organizational issues involved in clinical trials. This could be accomplished due to the latest advances in modern analytical technology, particularly liquid chromatography-mass spectrometry. The present review discusses some of the emerging liquid chromatography-mass spectrometry technologies in improving DBS analysis for its innovative applications in the development of new drugs. PMID:24697571

  15. Analysis of antimycin A by reversed-phase liquid chromatography/nuclear magnetic-resonance spectrometry

    USGS Publications Warehouse

    Ha, Steven T.K.; Wilkins, Charles L.; Abidi, Sharon L.

    1989-01-01

    A mixture of closely related streptomyces fermentation products, antimycin A, Is separated, and the components are identified by using reversed-phase high-performance liquid chromatography with directly linked 400-MHz proton nuclear magnetic resonance detection. Analyses of mixtures of three amino acids, alanine, glycine, and valine, are used to determine optimal measurement conditions. Sensitivity increases of as much as a factor of 3 are achieved, at the expense of some loss in chromatographic resolution, by use of an 80-?L NMR cell, Instead of a smaller 14-?L cell. Analysis of the antimycin A mixture, using the optimal analytical high performance liquid chromatography/nuclear magnetic resonance conditions, reveals it to consist of at least 10 closely related components.

  16. Evaluation of high-efficiency gas-liquid contactors for natural gas processing. Semi-annual report, April--September 1994

    SciTech Connect

    NONE

    1994-11-01

    Objective was to ensure reliable supply of high-quality natural gas by reducing the cost of treating subquality natural gas containing H{sub 2}O, CO{sub 2}, H{sub 2}S and/or trace quantities of other gaseous impurities by applying high-efficiency rotating and structured packing gas liquid contactors. The work included analysis of base case residence time, viscosity studies on low pressure rotary contactor system, and surface tension studies on the contactor.

  17. Modeling of closed-loop recycling liquid-liquid chromatography: Analytical solutions and model analysis.

    PubMed

    Kostanyan, Artak E

    2015-08-01

    In closed-loop recycling (CLR) chromatography, the effluent from the outlet of a column is directly returned into the column through the sample feed line and continuously recycled until the required separation is reached. To select optimal operating conditions for the separation of a given feed mixture, an appropriate mathematical description of the process is required. This work is concerned with the analysis of models for the CLR separations. Due to the effect of counteracting mechanisms on separation of solutes, analytical solutions of the models could be helpful to understand and optimize chromatographic processes. The objective of this work was to develop analytical expressions to describe the CLR counter-current (liquid-liquid) chromatography (CCC). The equilibrium dispersion and cell models were used to describe the transport and separation of solutes inside a CLR CCC column. The Laplace transformation is applied to solve the model equations. Several possible CLR chromatography methods for the binary and complex mixture separations are simulated. PMID:26116190

  18. Gas–liquid flow generated by a Rushton turbine in stirred vessel: CARPT\\/CT measurements and CFD simulations

    Microsoft Academic Search

    A. R. Khopkar; A. R. Rammohan; V. V. Ranade; M. P. Dudukovic

    2005-01-01

    In this work, computer-automated radioactive particle tracking (CARPT), computed tomography (CT) and computational fluid dynamic (CFD) based models were used to investigate gas–liquid flow generated by a Rushton turbine. CARPT and CT measurements were carried out in a gas–liquid stirred vessel operating in two different flow regimes and captured the quantitative Eulerian information of gas–liquid flow. The CARPT data was

  19. High GVF and low pressure gas–liquid two-phase flow measurement based on dual-cone flowmeter

    Microsoft Academic Search

    Fusheng Zhang; Feng Dong; Chao Tan

    2010-01-01

    Parameter measurement of gas–liquid two-phase flows with a high gas volume fraction (GVF) has received great attention in the research field of multiphase flow. The cone meter, as a new proposed differential pressure (DP) meter, is increasingly being applied in flowrate measurement of gas–liquid two-phase flow. A dual-parameter measurement method of gas–liquid two-phase flow based on a dual-cone meter is

  20. Qualitative and quantitative analysis of vetiver essential oils by comprehensive two-dimensional gas chromatography and comprehensive two-dimensional gas chromatography/mass spectrometry.

    PubMed

    Filippi, Jean-Jacques; Belhassen, Emilie; Baldovini, Nicolas; Brevard, Hugues; Meierhenrich, Uwe J

    2013-05-01

    Vetiver essential oils (VEO) are important raw ingredients used in perfume industry, entering the formula of numerous modern fragrances. Vetiver oils are considered to be among the most complex essential oils, resulting most of the time in highly coeluted chromatograms whatever the analytical technique. In this context, conventional gas chromatography has failed to provide a routine tool for the accurate qualitative and quantitative analysis of their constituents. Applying comprehensive two-dimensional gas chromatography techniques (GC×GC-FID/MS) afforded the mean to separate efficiently vetiver oil constituents in order to identify them in a more reliable way. Moreover, this is the first time that a complete true quantitation of each constituent is carried out on such complex oils by means of internal calibration. Finally, we have studied the influence of the injection mode on the determined chemical composition, and showed that several alcohols underwent dehydration under defined chromatographic conditions (splitless mode) usually recommended for quantitation purposes. PMID:23522261

  1. Rapid analysis of cholesterol-elevating compounds in coffee brews by off-line high-performance liquid chromatography/high-resolution gas chromatography.

    PubMed

    Ruiz del Castillo, M L; Herraiz, M; Blanch, G P

    1999-04-01

    A new method is proposed to analyze the cholesterol-elevating cafestol and kahweol which allows their rapid and reliable determination in different coffee brews. The method involves the preseparation of the sample by high-performance liquid chromatography, the collection of the selected fraction, and its subsequent analysis by high-resolution gas chromatography using a programmed temperature vaporizer operated in the split mode as sampling system. Under the experimental conditions investigated, recoveries as high as 87% (cafestol) and 94% (kahweol) were achieved while detection limits equal to 0.06 and 0.04 ppm for cafestol and kahweol, respectively, were obtained. Examples are given comparing levels of cafestol and kahweol resulting from the same ground roasted coffee by different brewing methods, which show the lowest values for brews prepared from coffee bags. PMID:10564010

  2. Carbohydrate analysis by high-performance anion-exchange chromatography with pulsed amperometric detection: The potential is still growing

    Microsoft Academic Search

    Tommaso R. I. Cataldi; Cristiana Campa; Giuseppe E. De Benedetto

    2000-01-01

    This article reviews recent advances of carbohydrate analysis by high-performance anion-exchange chromatography with pulsed\\u000a amperometric detection. Starting from the paper of Dennis C. Johnson [1] in which the great analytical promise of such a technique\\u000a was anticipated, a multitude of exciting new research possibilities have recently emerged. The great attractiveness of high-performance\\u000a anion-exchange chromatography is largely due to its compatibility

  3. Green chromatography.

    PubMed

    P?otka, Justyna; Tobiszewski, Marek; Sulej, Anna Maria; Kupska, Magdalena; Górecki, Tadeusz; Namie?nik, Jacek

    2013-09-13

    Analysis of organic compounds in samples characterized by different composition of the matrix is very important in many areas. A vast majority of organic compound determinations are performed using gas or liquid chromatographic methods. It is thus very important that these methods have negligible environmental impact. Chromatographic techniques have the potential to be greener at all steps of the analysis, from sample collection and preparation to separation and final determination. The paper summarizes the approaches used to accomplish the goals of green chromatography. While complete elimination of sample preparation would be an ideal approach, it is not always practical. Solventless extraction techniques offer a very good alternative. Where solvents must be used, the focus should be on the minimization of their consumption. The approaches used to make chromatographic separations greener differ depending on the type of chromatography. In gas chromatography it is advisable to move away from using helium as the carrier gas because it is a non-renewable resource. GC separations using low thermal mass technology can be greener because of energy savings offered by this technology. In liquid chromatography the focus should be on the reduction of solvent consumption and replacement of toxic and environmentally hazardous solvents with more benign alternatives. Multidimensional separation techniques have the potential to make the analysis greener in both GC and LC. The environmental impact of the method is often determined by the location of the instrument with respect to the sample collection point. PMID:23932374

  4. Fluorescence analysis of p-hydroxymethamphetamine in urine by thin-layer chromatography.

    PubMed

    Kato, Noriyuki; Kubo, Hiroaki; Homma, Hiroshi

    2005-09-01

    A highly-sensitive analytical method for the detection of p-hydroxymethamphetamine (pOHMA) in urine is presented. The proposed method combines liquid-liquid extraction with acetonitrile and solid-phase extraction by thin-layer chromatography (TLC) with oxidation using potassium hexacyanoferrate(III) and sodium hydroxide to detect the fluorophor of pOHMA. The detection limit for pOHMA is 10 ng (n = 3). The analysis of pOHMA in forensic samples is successfully performed, without interference from endogenous fluorophors, yielding concentrations in the appropriate range for methamphetamine abusers. PMID:16363483

  5. Microwave-assisted derivatization procedures for gas chromatography\\/mass spectrometry analysis

    Microsoft Academic Search

    Sandra L. Söderholm; Markus Damm; C. Oliver Kappe

    2010-01-01

    In this review, published applications of microwave-assisted derivatization procedures for gas chromatography\\/mass spectrometry\\u000a (GC\\/MS) are summarized. Among the broad range of analytical techniques available, GC\\/MS is still the method of choice for\\u000a most high-throughput screening procedures in forensic\\/clinical toxicology, doping control and food and environmental analysis.\\u000a Despite the many advantages of the GC\\/MS method, time-consuming derivatization steps are often required

  6. Separation of carbamazepine and five metabolites, and analysis in human plasma by micellar electrokinetic capillary chromatography

    Microsoft Academic Search

    Maria Augusta Raggi; Vincenzo Pucci; Alessandra Maurizio; Jan Muzikar; Ernst Kenndler

    2002-01-01

    A rapid and feasible method was developed for the analysis of carbamazepine and its five metabolites (10,11-dihydro-10,11-epoxycarbamazepine, 10,11-dihydro-10,11-dihydroxycarbamazepine, 10,11-dihydro-10-hydroxycarbamazepine, 2-hydroxycarbamazepine and 3-hydroxycarbamazepine) in human plasma. Separation of the analytes is based on micellar electrokinetic chromatography, in untreated fused-silica capillary (48.5\\/40.0 cm length, 50 ?m I.D.) with phosphate buffer (30 mM, pH 8.00) as background electrolyte, containing 50 mM sodium dodecylsulfate,

  7. Analysis of corticosteroids by high performance liquid chromatography-electrospray mass spectrometry.

    PubMed

    Panusa, Alessia; Ottaviani, Monica; Picardo, Mauro; Camera, Emanuela; Gagliardi, Luigi; Chimenti, Paola; Granese, Arianna; Tonelli, Domenica

    2004-08-01

    A high performance liquid chromatography electrospray mass spectrometry (HPLC-ESI-MS) method, for the detection of corticosteroids in cosmetics has been developed. A water-acetonitrile linear gradient on a C-18 reversed-phase column was found to be suitable in separating triamcinolone and its main derivatives, which greatly differ in lipophilicity. Detection was performed in negative electrospray ionisation mode. Good correlation between peaks areas and solutions concentration was found in the range 0.05-10.0 micro g ml(-1) and the detection limits resulted in the range of 20-45 pg injected. The method was successfully applied to the analysis of real samples of shampoo. PMID:15284915

  8. Dynamic and spectroscopic characteristics of atmospheric gliding arc in gas-liquid two-phase flow

    SciTech Connect

    Tu, X. [Center for Surface Chemistry and Catalysis, Katholieke Universiteit Leuven, Heverlee 3001 (Belgium); Yu, L.; Yan, J. H.; Cen, K. F. [State Key Laboratory of Clean Energy Utilization, Zhejiang University, Hangzhou 310027 (China); Cheron, B. G. [CNRS UMR 6614-CORIA, Saint Etienne du Rouvray 76801 (France)

    2009-11-15

    In this study, an atmospheric alternating-current gliding arc device in gas-liquid two-phase flow has been developed for the purpose of waste water degradation. The dynamic behavior of the gas-liquid gliding arc is investigated through the oscillations of electrical signals, while the spatial evolution of the arc column is analyzed by high speed photography. Different arc breakdown regimes are reported, and the restrike mode is identified as the typical fluctuation characteristic of the hybrid gliding arc in air-water mixture. Optical emission spectroscopy is employed to investigate the active species generated in the gas-liquid plasma. The axial evolution of the OH (309 nm) intensity is determined, while the rotational and vibrational temperatures of the OH are obtained by a comparison between the experimental and simulated spectra. The significant discrepancy between the rotational and translational temperatures has also been discussed.

  9. Multiresidue analysis of 30 organochlorine pesticides in milk and milk powder by gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry.

    PubMed

    Zheng, Guocan; Han, Chao; Liu, Yi; Wang, Jing; Zhu, Meiwen; Wang, Chengjun; Shen, Yan

    2014-10-01

    A method for simultaneous determination of the 30 organochlorine pesticides (OCP) in milk and milk powder samples has been developed. Prior to the gas chromatography-tandem mass spectrometric analysis, the residual OCP in samples were extracted with n-hexane and acetone mixture (1/1, vol/vol) and cleaned up by gel permeation chromatography and solid phase extraction. Selected reaction monitoring mode was used for gas chromatography-tandem mass spectrometric data acquisition to identify and quantify the OCP. To avoid the matrix effects, matrix-matched calibration solutions ranging from 2 to 50 ng/mL were used to record the calibration curve. Limits of quantification of all OCP were 0.8 ?g/kg. With the exception of endrin, limits of quantification are signi?cantly lower than maximum residue limits set by the European Union and China. The average recoveries were in the range of 70.1 to 114.7% at 3 spiked concentration levels (0.8, 2.0, and 10.0 ?g/kg) with residual standard deviation lower than 12.9%. The developed method was successfully applied to analyze the OCP in commercial milk products. PMID:25087035

  10. Basic Principles of Chromatography

    NASA Astrophysics Data System (ADS)

    Ismail, Baraem; Nielsen, S. Suzanne

    Chromatography has a great impact on all areas of analysis and, therefore, on the progress of science in general. Chromatography differs from other methods of separation in that a wide variety of materials, equipment, and techniques can be used. [Readers are referred to references (1-19) for general and specific information on chromatography.]. This chapter will focus on the principles of chromatography, mainly liquid chromatography (LC). Detailed principles and applications of gas chromatography (GC) will be discussed in Chap. 29. In view of its widespread use and applications, high-performance liquid chromatography (HPLC) will be discussed in a separate chapter (Chap. 28). The general principles of extraction are first described as a basis for understanding chromatography.

  11. Analysis of macrolide antibiotics, using liquid chromatography-mass spectrometry, in food, biological and environmental matrices.

    PubMed

    Wang, Jian

    2009-01-01

    Macrolides are a group of antibiotics that have been widely used in human medical and veterinary practices. Analysis of macrolides and related compounds in food, biological, and environmental matrices continue to be the focus of scientists for the reasons of food safety, pharmacokinetic studies, and environmental concerns. This article presents an overview on the primary biological properties of macrolides and their associated analytical issues, including extraction, liquid chromatography-mass spectrometry (LC-MS), method validation, and measurement uncertainty. The main techniques that have been used to extract macrolides from various matrices are solid-phase extraction and liquid-liquid extraction. Conventional liquid chromatography (LC) with C18 columns plays a dominant role for the determination of macrolides, whereas ultra-performance liquid chromatography (UPLC) along with sub-2 microm particle C18 columns reduces run time and improves sensitivity. Mass spectrometry (MS), serving as a universal detection technique, has replaced ultraviolet (UV), fluorometric, and electrochemical detection for multi-macrolide analysis. The triple-quadrupole (QqQ), quadrupole ion trap (QIT), triple-quadrupole linear ion trap, time-of-flight (TOF), and quadrupole time-of-flight (QqTOF) mass spectrometers are current choices for the determination of macrolides, including quantification, confirmation, identification of their degradation products or metabolites, and structural elucidation. LC or UPLC coupled to a triple-quadrupole mass spectrometer operated in the multiple-reaction monitoring (MRM) mode (LC/MS/MS) is the first choice for quantification. UPLC-TOF or UPLC-QqTOF has been recognized as an emerging technique for accurate mass measurement and unequivocal identification of macrolides and their related compounds. PMID:18785191

  12. Sensitive headspace gas chromatography analysis of free and conjugated 1-methoxy-2-propanol in urine.

    PubMed

    Tomicic, Catherine; Berode, Michèle

    2010-04-01

    Glycol ethers still continue to be a workplace hazard due to their important use on an industrial scale. Currently, chronic occupational exposures to low levels of xenobiotics become increasingly relevant. Thus, sensitive analytical methods for detecting biomarkers of exposure are of interest in the field of occupational exposure assessment. 1-Methoxy-2-propanol (1M2P) is one of the dominant glycol ethers and the unmetabolized urinary fraction has been identified to be a good biological indicator of exposure. An existing analytical method including a solid-phase extraction and derivatization before GC/FID analysis is available but presents some disadvantages. We present here an alternative method for the determination of urinary 1M2P based on the headspace gas chromatography technique. We determined the 1M2P values by the direct headspace method for 47 samples that had previously been assayed by the solid-phase extraction and derivatization gas chromatography procedure. An inter-method comparison based on a Bland-Altman analysis showed that both techniques can be used interchangeably. The alternative method showed a tenfold lower limit of detection (0.1 mg/L) as well as good accuracy and precision which were determined by several urinary 1M2P analyses carried out on a series of urine samples obtained from a human volunteer study. The within- and between-run precisions were generally about 10%, which corresponds to the usual injection variability. We observed that the differences between the results obtained with both methods are not clinically relevant in comparison to the current biological exposure index of urinary 1M2P. Accordingly, the headspace gas chromatography technique turned out to be a more sensitive, accurate, and simple method for the determination of urinary 1M2P. PMID:20155252

  13. Analysis of Total Human Urinary Glycosaminoglycan Disaccharides by Liquid Chromatography-Tandem Mass Spectrometry.

    PubMed

    Sun, Xiaojun; Li, Lingyun; Overdier, Katherine H; Ammons, Lee Anne; Douglas, Ivor S; Burlew, Clay Cothren; Zhang, Fuming; Schmidt, Eric P; Chi, Lianli; Linhardt, Robert J

    2015-06-16

    The determination of complex analytes, present at low concentrations, in biological fluids poses a difficult challenge. This study relies on an optimized method of recovery, enzymatic treatment, and disaccharide analysis by liquid chromatography-tandem mass spectrometry to rapidly determine low concentrations of glycosaminoglycans in human urine. The approach utilizes multiple reaction monitoring (MRM) of glycosaminoglycan disaccharides obtained from treating urine samples with recombinant heparin lyases and chondroitin lyase. This rapid and sensitive method allows the analysis of glycosaminoglycan content and disaccharide composition in urine samples having concentrations 10- to 100-fold lower than those typically analyzed from patients with metabolic diseases, such as mucopolysaccharidosis. The current method facilitates the analysis low (ng/mL) levels of urinary glycosaminoglycans present in healthy individuals and in patients with pathological conditions, such as inflammation and cancers, that can subtly alter glycosaminoglycan content and composition. PMID:26005898

  14. Enantiomeric analysis of limonene and carvone by direct introduction of aromatic plants into multidimensional gas chromatography.

    PubMed

    Barba, C; Toledano, R M; Santa-María, G; Herraiz, M; Martínez, R M

    2013-03-15

    Analysis of chiral compounds in complex mixtures is achieved by multidimensional gas chromatography using heptakis-(2,3,6-tri-O-methyl)-?-cyclodextrin stationary phase as the main column of the system to separate specific selected cuts containing components unresolved in the first dimension. The proposed procedure allows rapid analysis of both solid and liquid matrices by direct introduction, into the programmed temperature vaporizer (PTV) of a gas chromatograph, of either the plant material or the essential oil, respectively. A comparison between enantiomeric excesses data obtained, from plant leaves (or plant seeds) and the corresponding essential oils, by direct injection (i.e., without sample pretreatment or concentration step) into the multidimensional system is also included. Reported data demonstrate that no racemization occurs during analysis as identical enantiomeric excesses are obtained in both cases for specific chiral compounds. PMID:23598101

  15. A Laboratory Experiment in Pharmaceutical Analysis: Analysis of Diazepam Tablets by High Pressure Liquid Chromatography

    ERIC Educational Resources Information Center

    Bailey, Leonard

    1978-01-01

    The experiment described was developed for the third-year course in inorganic and analytical pharmaceutical chemistry to provide students with "hands-on" experience with high pressure liquid chromatography. Assay procedures are given along with experimental parameters and student results. (LBH)

  16. Application of displacement chromatography for the analysis of a lipid raft proteome.

    PubMed

    Trusch, Maria; Böhlick, Alexandra; Hildebrand, Diana; Lichtner, Björn; Bertsch, Andreas; Kohlbacher, Oliver; Bachmann, Sebastian; Schlüter, Hartmut

    2010-02-01

    Defining membrane proteomes is fundamental to understand the role of membrane proteins in biological processes and to find new targets for drug development. Usually multidimensional chromatography using step or gradient elution is applied for the separation of tryptic peptides of membrane proteins prior to their mass spectrometric analysis. Displacement chromatography (DC) offers several advantages that are helpful for proteome analysis. However, DC has so far been applied for proteomic investigations only in few cases. In this study we therefore applied DC in a multidimensional LC-MS approach for the separation and identification of membrane proteins located in cholesterol-enriched membrane microdomains (lipid rafts) obtained from rat kidney by density gradient centrifugation. The tryptic peptides were separated on a cation-exchange column in the displacement mode with spermine used as displacer. Fractions obtained from DC were analyzed using an HPLC-chip system coupled to an electrospray-ionization ion-trap mass spectrometer. This procedure yielded more than 400 highly significant peptide spectrum matches and led to the identification of more than 140 reliable protein hits within an established rat kidney lipid raft proteome. The majority of identified proteins were membrane proteins. In sum, our results demonstrate that DC is a suitable alternative to gradient elution separations for the identification of proteins via a multidimensional LC-MS approach. PMID:20015709

  17. Injectors for capillary gas chromatography and their application to environmental analysis.

    PubMed

    Bailey, Renata

    2005-11-01

    The application of different injectors in capillary gas chromatography (GC) analysis of semi-volatile organic contaminants in environmental samples prepared in organic solvents is reviewed. The injectors examined include a split/splitless injector in splitless mode (SS), cold on-column (COC), and programmable temperature vaporizer (PTV) and adaptations of these injector designs. Key issues when selecting an injector include properties of the analyte, such as potential for thermal degradation or discrimination of high boiling point compounds within the injector, and the ability of the GC systems to handle large volume injections (LVI) primarily to lower detection limits and allow direct coupling with sample preparation techniques such as at-line or on-line solid phase extraction (SPE). LVI also require consideration of matrix interference issues. This review examines only injector chamber modifications that are feasible with a standard GC configuration, however some modifications to the chromatographic system to extend the range of applicability of gas chromatography analysis for environmental samples are also noted. PMID:16252052

  18. High performance thin layer chromatography (HPTLC) and high performance liquid chromatography (HPLC) for the qualitative and quantitative analysis of Calendula officinalis-advantages and limitations.

    PubMed

    Loescher, Christine M; Morton, David W; Razic, Slavica; Agatonovic-Kustrin, Snezana

    2014-09-01

    Chromatography techniques such as HPTLC and HPLC are commonly used to produce a chemical fingerprint of a plant to allow identification and quantify the main constituents within the plant. The aims of this study were to compare HPTLC and HPLC, for qualitative and quantitative analysis of the major constituents of Calendula officinalis and to investigate the effect of different extraction techniques on the C. officinalis extract composition from different parts of the plant. The results found HPTLC to be effective for qualitative analysis, however, HPLC was found to be more accurate for quantitative analysis. A combination of the two methods may be useful in a quality control setting as it would allow rapid qualitative analysis of herbal material while maintaining accurate quantification of extract composition. PMID:24880991

  19. Limiting activity coefficients and gas-liquid partition coefficients of various solutes in piperidinium ionic liquids: measurements and LSER calculations.

    PubMed

    Paduszy?ski, Kamil; Doma?ska, Urszula

    2011-06-30

    This paper is a continuation of our systematic investigations on piperidinium ionic liquids and presents new data on activity coefficients at infinite dilution for 43 solutes: linear and branched alkanes, cycloalkanes, alkenes, alkynes, benzene, alkylbenzenes, alcohols, water, thiophene, tetrahyrdofuran (THF), methyl tert-butyl ether (MTBE), linear ethers, acetone, and linear ketones in the ionic liquid 1-butyl-1-methyl-piperidinium bis(trifluoromethylsulfonyl)imide, [BMPIP][NTf2]. The data were determined by gas-liquid chromatography (GLC) at temperatures from 308.15 to 358.15 K. These values were compared to those previously published for the bis-(trifluoromethylsulfonyl)imide-based ionic liquids. The partial molar excess enthalpies ?H1(E,?) and entropies ?S1(E,?) at infinite dilution were calculated from the experimental ?13(?) values obtained over the temperature range. The values of the selectivities for different separation problems were calculated from ?13(?) and compared to literature values for N-methyl-2-pyrrolidinone (NMP), sulfolane, and additional ionic liquids. Experimental limiting activity coefficients were used to calculate gas-IL partition coefficients of solutes, K(L). The modeling with specific linear solvation energy relationship (LSER) equations was performed for data obtained in this work and those reported earlier for 1-butyl-1-methylpiperidinium thiocyanate, [BMPIP][SCN]. PMID:21634373

  20. Direct numerical simulation of reactive absorption in gas–liquid flow on structured packing using interface capturing method

    Microsoft Academic Search

    Y. Haroun; D. Legendre; L. Raynal

    2010-01-01

    Direct numerical simulations are performed in order to study physical and reactive absorption in gas–liquid flow on structured packing. The volume of fluid method is used to capture the gas-liquid interface motion. The mass transport is computed by additional chemical species concentration transport equation with adequate modelling of solubility and chemical reaction. The numerical difficulties arise in imposing jump discontinuity

  1. Improving sensitivity in chiral supercritical fluid chromatography for analysis of active pharmaceutical ingredients.

    PubMed

    Helmy, Roy; Biba, Mirlinda; Zang, Jia; Mao, Bing; Fogelman, Kimber; Vlachos, Vaso; Hosek, Paul; Welch, Christopher J

    2007-11-01

    Despite its status as the preferred method for routine enantiopurity analysis in pharmaceutical research, supercritical fluid chromatography (SFC) has historically been unsuited for the accurate and precise measurements required for release testing of active pharmaceutical ingredients (APIs) under current good manufacturing processes (cGMPs). Insufficient signal to noise, as compared to HPLC, has heretofore been the major limitation of the chiral SFC approach. We herein describe an investigation into the fundamental limitations and sources of noise in the SFC approach, identifying thermal, electronic, and mechanical sources of noise within the flow cell as key parameters contributing to reduced sensitivity. A variety of instrument modifications are explored, ultimately leading to the development of a new and improved flow cell and other instrument modifications that allow suitable sensitivity and accuracy to carry out GMP release testing for enantiopurity analysis using SFC. PMID:17722016

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

    PubMed

    Czy?ewska, Urszula; Kono?czuk, Joanna; Teul, Joanna; Dr?gowski, Pawe?; Pawlak-Morka, Renata; Sura?y?ski, Arkadiusz; Miltyk, Wojciech

    2015-05-01

    Propolis is a resin that is collected by honeybees from various plant sources. Due to its pharmacological properties, it is used in commercial production of nutritional supplements in pharmaceutical industry. In this study, gas chromatography-mass spectrometry was applied for quality control analysis of the three commercial specimens containing aqueous-alcoholic extracts of bee propolis. More than 230 constituents were detected in analyzed products, including flavonoids, chalcones, cinnamic acids and their esters, phenylpropenoid glycerides, and phenylpropenoid sesquiterpenoids. An allergenic benzyl cinnamate ester was also identified in all tested samples. This analytical method allows to evaluate biological activity and potential allergenic components of bee glue simultaneously. Studies on chemical composition of propolis samples may provide new approach to quality and safety control analysis in production of propolis supplementary specimens. PMID:25198412

  3. Design of a cyclone separator for the separation of gas-liquid mixtures

    Microsoft Academic Search

    A. S. Zhikharev; A. M. Kutepov; V. V. Solov'ev

    1985-01-01

    A procedure has been developed at the MIKhMe for the design of a hollow cyclone separator with a rectangular tangential inlet of the gas-liquid mixture near the bottom. The procedure is based on the results of theoretical and experimental investigations of the cyclone and allows one to determine the geometrical dimensions and the operating regime of the cyclone which corresponds

  4. Degradation of phenol in water using a gas–liquid phase pulsed discharge plasma reactor

    Microsoft Academic Search

    Jie Li; Masayuki Sato; Takayuki Ohshima

    2007-01-01

    In this paper, a gas–liquid phase pulsed discharge plasma reactor was used to dispose phenol in aqueous solutions. The effect of pulsed peak voltage and energy, solution conductivity, solution pH, and additive gas varieties on degradation efficiency of phenol was reviewed in the research. The observed results showed that degradation efficiency of phenol increased with the increase of pulsed peak

  5. Dynamic digital speckle interferometry applied to optical diagnosis of gas-liquid phase change

    Microsoft Academic Search

    Yaozu Song; Hongling Zhang; Wei Zhang; Tianfeng Jiao

    2001-01-01

    In this paper, a Dynamic Digital Speckle Interferometry (DDSI) applied to optical diagnosis of gas-liquid phase change is proposed. The basic principle and experimental system of the DDSI are presented. This technology of flow optical diagnosis has the following three main advantages. First, DDSI uses a CCD camera as record device of a specklegram and a microcomputer, which processes the

  6. Upward Gas-Liquid Flow in Concentric and Eccentric Annular Spaces

    E-print Network

    Cavalcanti de Sousa, Pedro

    2013-12-09

    A limited amount of work exists on upward gas-liquid flow in annular spaces. This is a common scenario in drilling operations, especially in underbalanced drilling, and in high-production wells. To carry out this study, a 40-meter high laboratory...

  7. Flow injection turbidimetric determination of total organic carbon with a gas–liquid transfer microreactor

    Microsoft Academic Search

    José Neri Gottfried Paniz; Érico M. M Flores; Valderi L Dressler; Ayrton F Martins

    2001-01-01

    A procedure for the determination of total organic carbon (TOC) and its fractions in industrial effluent samples is proposed. A flow injection system using a gas–liquid transfer microreactor was developed, and adapted to a turbidimetric spectrophotometer. Samples were decomposed into glass vials in a microwave oven and a fraction of the CO2 was injected into a carrier gas and pumped

  8. Triple-channel microreactor for biphasic gas-liquid reactions: Photosensitized oxygenations.

    PubMed

    Maurya, Ram Awatar; Park, Chan Pil; Kim, Dong-Pyo

    2011-01-01

    A triple-channel microreactor fabricated by means of a soft-lithography technique was devised for efficient biphasic gas-liquid reactions. The excellent performance of the microreactor was demonstrated by carrying out photosensitized oxygenations of ?-terpinene, citronellol, and allyl alcohols. PMID:21915221

  9. Modelling of the dynamics of a low-speed gas-liquid heat engine

    Microsoft Academic Search

    C. M. P. Cunha; J. A. R. Parise

    1992-01-01

    This paper deals with the simulation model of a gas-liquid heat engine which is characterized by very low speeds (1-3 rpm) and relatively high torque. The engine operates according to the Minto Thermal Wheel' principle. It is based on the conversion of thermal energy from the heat source, through gas expansion, into mechanical work, by means of the fall of

  10. Research on Gas-liquid Flow Rate Optimization in Foam Drilling

    NASA Astrophysics Data System (ADS)

    Gao, B. K.; Sun, D. G.; Jia, Z. G.; Huang, Z. Q.

    2010-03-01

    With the advantages of less gas consumption, higher carrying rocks ability, lower leakage and higher penetration rate, foam drilling is widely used today in petroleum industry. In the process of foam underbalanced drilling, the mixture of gas, liquid and cuttings flows upwards through the annular, so it is a typical gas-liquid-solid multi-phase flow. In order to protect the reservoir and avoid borehole wall collapsing during foam drilling, it is crucial to ensure that the bottom hole pressure is lower than the formation pressure and higher than the formation collapse pressure, and in the mean time, foam drilling fluid in the whole wellbore should be in the best foam quality stage in order to have sufficient capacity to carry cuttings. In this paper, main relations between bottom hole pressure and gas-liquid injecting rate are analyzed with the underbalanced multiphase flow models. And in order to obtain precise flow pattern and flow pressure, the whole well bore is spatial meshed and iterative method is used. So, a convenient safety window expressed by gas-liquid injecting rate is obtained instead of that by bottom hole pressure. Finally, a foam drilling example from a block in Yemen is presented; the drilling results show that this method is reliable and practical.

  11. Calculation of interfacial flows and surfactant redistribution as a gas/liquid interface moves between two parallel plates

    NASA Astrophysics Data System (ADS)

    Wassmuth, Fred; Laidlaw, W. G.; Coombe, D. A.

    1993-07-01

    The hydrodynamic equations governing the evolution of the interface of a gas/liquid ``bubble'' as it moves through the space between two plates are solved using a finite difference algorithm defined on a moving deforming surface grid. Particular attention is paid to the redistribution of surfactant as the bubble deforms on squeezing through a constriction. The surfactant redistribution, the surface tangential flows, and the surface normal velocity depend on factors such as bulk viscosity, the bulk/surface surfactant exchange rate, the surface tension dependence on surfactant concentration, and the bulk velocity pattern. Zones of surfactant depletion just behind the bubble front and an accumulation near the bubble front are observed; there are also depletion and accumulation zones associated with the constriction. A variety of other effects are investigated and a detailed analysis permits the generation of schematic representations of the interplay of the coupled bulk and surface hydrodynamic equations for the system.

  12. Doping control analysis of metamfepramone and two major metabolites using liquid chromatography-tandem mass spectrometry.

    PubMed

    Thevis, Mario; Sigmund, Gerd; Thomas, Andreas; Gougoulidis, Vassilios; Rodchenkov, Grigory; Schänzer, Wilhelm

    2009-01-01

    The sympathomimetic agent metamfepramone (2-dimethylamino-1-phenylpropan-1-one, dimethylpropion) is widely used for the treatment of the common cold or hypotonic conditions. Due to its stimulating properties and its rapid metabolism resulting in major degradation products such as methylpseudoephedrine and methcathinone, it has been considered relevant for doping controls by the World Anti-Doping Agency (WADA). The rapid degradation of the active drug complicates the detection of metamfepramone itself but the metabolites methylpseudoephedrine and methcathinone can be monitored, and the finding of the latter in particular allows the inference of a metamfepramone administration. In order to improve sports drug testing procedures, metamfepramone, methylpseudoephedrine and methcathinone were characterized using electrospray ionization-high resolution/high accuracy mass spectrometry, and a method employing liquid chromatography/tandem mass spectrometry was established that allowed the analysis of these three analytes by direct injection of 2 microL of urine specimens. The assay was validated with regard to specificity, lower limits of detection (2-10 ng mL(-1)), intraday and interday precision (3-17%) and ion suppression/enhancement effects. The developed procedure has been used to verify or falsify suspicious signals observed in routine screening procedures based on gas chromatography/mass spectrometry and yielded an adverse analytical finding concerning a metamfepramone administration in an authentic doping control sample. Although the active drug was not detected, the indicative metabolites methylpseudoephedrine and methcathinone were considered sufficient to infer the application of the prohibited drug. PMID:19661559

  13. On-line liquid chromatography-gas chromatography: A novel approach for the analysis of phytosterol oxidation products in enriched foods.

    PubMed

    Scholz, Birgit; Wocheslander, Stefan; Lander, Vera; Engel, Karl-Heinz

    2015-05-29

    A novel methodology for the automated qualitative and quantitative determination of phytosterol oxidation products in enriched foods via on-line liquid chromatography-gas chromatography (LC-GC) was established. The approach is based on the LC pre-separation of acetylated phytosterols and their corresponding oxides using silica as stationary phase and a mixture of n-hexane/methyl tert-butyl ether/isopropanol as eluent. Two LC-fractions containing (i) 5,6-epoxy- and 7-hydroxyphytosterols, and (ii) 7-ketophytosterols are transferred on-line to the GC for the analysis of their individual compositions on a medium polar trifluoropropylmethyl polysiloxane capillary column. Thus, conventionally employed laborious off-line purification and enrichment steps can be avoided. Validation data, including recovery, repeatability, and reproducibility of the method, were elaborated using an enriched margarine as example. The margarine was subjected to a heating procedure in order to exemplarily monitor the formation of phytosterol oxidation products. Quantification was performed using on-line LC-GC-FID, identification of the analytes was based on on-line LC-GC-MS. The developed approach offers a new possibility for the reliable and fast analysis of phytosterol oxidation products in enriched foods. PMID:25890442

  14. Rapid and Sensitive PCR-Dipstick DNA Chromatography for Multiplex Analysis of the Oral Microbiota

    PubMed Central

    Niwa, Kousuke; Kawase, Mitsuo; Tanner, Anne C. R.; Takahashi, Nobuhiro

    2014-01-01

    A complex of species has been associated with dental caries under the ecological hypothesis. This study aimed to develop a rapid, sensitive PCR-dipstick DNA chromatography assay that could be read by eye for multiplex and semiquantitative analysis of plaque bacteria. Parallel oligonucleotides were immobilized on a dipstick strip for multiplex analysis of target DNA sequences of the caries-associated bacteria, Streptococcus mutans, Streptococcus sobrinus, Scardovia wiggsiae, Actinomyces species, and Veillonella parvula. Streptavidin-coated blue-colored latex microspheres were to generate signal. Target DNA amplicons with an oligonucleotide-tagged terminus and a biotinylated terminus were coupled with latex beads through a streptavidin-biotin interaction and then hybridized with complementary oligonucleotides on the strip. The accumulation of captured latex beads on the test and control lines produced blue bands, enabling visual detection with the naked eye. The PCR-dipstick DNA chromatography detected quantities as low as 100?pg of DNA amplicons and demonstrated 10- to 1000-fold higher sensitivity than PCR-agarose gel electrophoresis, depending on the target bacterial species. Semiquantification of bacteria was performed by obtaining a series of chromatograms using serial 10-fold dilution of PCR-amplified DNA extracted from dental plaque samples. The assay time was less than 3?h. The semiquantification procedure revealed the relative amounts of each test species in dental plaque samples, indicating that this disposable device has great potential in analysis of microbial composition in the oral cavity and intestinal tract, as well as in point-of-care diagnosis of microbiota-associated diseases. PMID:25485279

  15. Analysis of vitamin D and its metabolites using thermospray liquid chromatography/mass spectrometry.

    PubMed

    Watson, D; Setchell, K D; Ross, R

    1991-07-01

    A new method is described for the analysis of vitamin D and its metabolites utilizing thermospray (TSP) mass spectrometry as an on-line detector for high performance liquid chromatography. Ionization conditions were optimized for use with isocratic reversed phase chromatography. TSP mass spectrometry was employed in series with a UV absorbance detector to facilitate comparisons between the two methods of detection. Positive ion TSP mass spectra were recorded for vitamin D2, vitamin D3, 25-hydroxyvitamin D3 (25(OH)D3), 1,25-dihydroxyvitamin D3 (1,25(OH)2D3) and 24,25-dihydroxyvitamin D3 (24,25(OH)2D3). The spectra contained protonated molecular ions, ammonium adduct ions and fragment ions due to the loss of one or more molecules of water. A comparison of quantitative precision was made by determining UV absorbance and TSP standard curves for vitamin D3 using two different methods: (1) External standard method with post-column (post UV detector) addition of ammonium acetate. (2) As (1) but using the method of internal standards with a closely eluting internal standard (vitamin D2). In each case the quantitative precision (correlation coefficient) for UV absorbance detection was superior owing to intrinsic instability of the TSP ion beam. A stable isotopically labelled internal standard was employed in the development of an assay for 1,25(OH)2D3. The assay was used to quantify in vitro enzymic conversion of 25(OH)D3 to 1,25(OH)2D3 in guinea pig and sheep renal mitochondrial incubations. TSP LC/MS was also applied to analysis of an extract of human blood plasma in which D3 and each of its principal metabolites were identified in a single analysis. PMID:1655127

  16. Circulating ultrasound-assisted extraction, countercurrent chromatography, and liquid chromatography for the simultaneous extraction, isolation, and analysis of the constituents of Uncaria tomentosa.

    PubMed

    Zhang, Yuchi; Liu, Chunming; Qi, Yanjuan; Li, Sainan; Pan, Yan; Li, Yuchun

    2015-04-01

    A hyphenated automated technique for the online extraction, isolation, analysis, and identification of natural organic compounds was established. Circulating ultrasound-assisted extraction (CUAE) was coupled with countercurrent chromatography (CCC), high performance liquid chromatography (HPLC), and a diode array detector (DAD). This approach was applied to the fractionation and purification of alkaloids from Uncaria tomentosa. A biphasic solvent system of chloroform-methanol-water (6:4:5, v:v:v) was used for the CUAE and CCC separation of compounds from 500 g of U. tomentosa. Two CUAE/CCC/HPLC/DAD modes were established. Either the upper aqueous phase or the lower organic phase of the solvent system could be used as the extraction solvent. The target compounds were extracted by CUAE, and the extract was pumped into a sample loop before being directly injected into the CCC column, or pre-purified using a flash chromatography column before injection. The target compounds were eluted using either the organic or aqueous phase of the solvent system and the fractions were monitored using a UV detector. The target fractions were collected by a sample loop via a six-port valve, and analyzed by HPLC/DAD for purity and structural identification. This system isolated of 8.2mg, 7.4 mg, and 12.9 mg of rhynchophylline, corynoxine, and corynoxine B with HPLC purities of 96.15%, 95.34%, and 95.49%, respectively via the first mode; and isolated 26.6 mg, 24.6 mg, and 45.3mg of rhynchophylline, corynoxine, and corynoxine B with a HPLC purities of 98.22%, 97.18%, and 97.93% via the second mode. PMID:25725954

  17. [Quantitative analysis of (-)-epigallocatechin gallate in tea leaves by high-performance liquid chromatography].

    PubMed

    Sakata, I; Ikeuchi, M; Maruyama, I; Okuda, T

    1991-12-01

    The quantitative analysis of (-)-epigallocatechin gallate (EGCG) in tea (Camellia sinensis L.) was performed by high-performance liquid chromatography (HPLC) with a C-18 reversed-phase column. EGCG was then eluted within 20 min by using methanol-water-acetic acid (20:75:5 (v/v/v)) as an eluent. As an internal standard, tryptophan was used. The content of EGCG in five kinds of green tea (sencha, gyokuro, bancha, matsucha and oolong tea) and in a cup of those was determined by both the extraction method with 50% (v/v) methanol and the infusion method with water. The largest amount of EGCG was obtained from matsucha by the extraction method, or from sencha by the infusion method. Furthermore, EGCG contents in various parts of the tea plant were examined. The first leaf had the highest concentration of EGCG, and the concentration of EGCG decreased with the aging of the leaf. PMID:1806661

  18. Analysis of anthocyanins in powdered berry extracts by planar chromatography linked with bioassay and mass spectrometry.

    PubMed

    Cretu, Georgiana C; Morlock, Gertrud E

    2014-03-01

    Major anthocyanins were extracted with acidified methanol and characterised in powdered berry extracts of bilberry, blueberry, chokeberry, açai berry and cranberry by HPTLC-Vis-MS for the first time. A combined 2-step normal phase separation was applied, first for separation of anthocyanins and secondly of anthocyanidins. Documentation was performed under white light illumination (transmission mode). In the powdered berry extracts, especially the 3-glucosides of delphinidin, cyanidin, malvidin and peonidin, further cyanidin glycosides and respective anthocyanidins were found. Calibration data revealed a good correlation, with r between 0.9988 and 0.9999. The repeatability of the sample analysis (n=3) was ?3.6%. Based on the results obtained, this method can be used for rapid routine quality control of powdered berry extracts. For confirmation of the results or characterisation of unknown anthocyanin zones, mass spectra were recorded. Chromatography was directly linked to the effect using DPPH(?) reagent and luminescent Aliivibrio fischeri bioassay. PMID:24176320

  19. Mycolic Acid Analysis by High-Performance Liquid Chromatography for Identification of Mycobacterium Species

    PubMed Central

    Butler, W. Ray; Guthertz, Linda S.

    2001-01-01

    Mycobacterium tuberculosis is the etiologic agent of tuberculosis and can be accurately detected by laboratories using commercial genetic tests. Nontuberculosis mycobacteria (NTM) causing other mycobacterioses can be difficult to identify. The identification processes are confounded by an increasing diversity of newly characterized NTM species. The ubiquitous nature of NTM, combined with their potential to be opportunistic pathogens in immunocompromised as well as nonimmunodeficient patients, further complicates the problem of their identification. Since clinical case management varies depending on the etiologic agent, laboratories must identify the species in a timely manner. However, only a few identification methods can detect the species diversity within the Mycobacterium genus. Over the last decade, high-performance liquid chromatography analysis of the mycolic acids has become an accepted method for identification of mycobacteria. In this review, we assess its development and usefulness as an identification technique for Mycobacterium species. PMID:11585782

  20. High performance size exclusion chromatography (IX) bulk and component analysis of silanol groups in polydimethylsiloxanes

    SciTech Connect

    Kohn, E.

    1985-01-01

    Methods for the bulk and molecular weight component analysis of hydroxyl groups attached to silicon in polydimethylsiloxanes of the Sylgard type have been developed. The infrared (ir) absorbance band of the silanol adduct produced by hydrogen bonding with 1,4-dioxane is used. The determination of hydroxyl content as a function of molecular weight employs an on-line size exclusion chromatography-infrared (SEC-IR) technique. Interference by vinyl or phenyl groups in the sample or by traces of water in the solvent was negligible, but water or compounds containing other types of hydroxyl groups interfered. Sensitivity of the method is about 10 ..mu..g of the silanol, as OH in the polydimethylsiloxane. Primary calibration was by proton nuclear magnetic resonance (PNMR) at a high concentration of hydroxyl groups.

  1. [Quantitative analysis of deacylgymnemic acid by high-performance liquid chromatography].

    PubMed

    Suzuki, K; Ishihara, S; Uchida, M; Komoda, Y

    1993-04-01

    A method of the quantitative analysis was established for the determination of deacylgymnemic acid (DAGA) in the alkaline hydrolysate of the sample containing gymnemic acids which are ingredients of Gymnema sylvestre R. BR. leaves, by means of high-performance liquid chromatography. This method was used for comparing the contents of gymnemic acids in various samples. The amount of gymnemic acids analyzed as DAGA in 70% ethanol extract of dry leaves was about twice that in hot water extract. The commercial health-supplemental foods of five companies were investigated for the contents of gymnemic acids as DAGA and there were large differences from 38 to 251 mg in the dosage per day recommended by each company. PMID:8492295

  2. Routine analysis of plasma busulfan by gas chromatography-mass fragmentography.

    PubMed

    Lai, W K; Pang, C P; Law, L K; Wong, R; Li, C K; Yuen, P M

    1998-12-01

    Busulfan (BU) is a widely used alkylating agent for antineoplastic therapy and marrow ablation in preparation for bone marrow transplantation (BMT). High-dose BU often leads to successful preparation and low relapse but is associated with veno-occlusive disease of liver. We established a protocol to determine postdosage plasma BU concentrations by gas chromatography-mass fragmentography in an attempt to relate clinical outcome to plasma BU concentrations. We used nonisotopic pusulfan as the internal standard. After extraction into ethyl acetate, BU and pusulfan were iodinated into 1, 4-diiodobutane and 1,5-diiodopentane, respectively. Gas chromatography-mass spectrometry (GC-MS) analysis was carried out on an Hewlett-Packard (HP) 5890II gas chromatograph with a 30-m 100% methyl silicon narrow bore, fused-silica capillary column interfaced with an HP 5970A mass spectrometer. Helium was the carrier gas. The sample molecules were identified by total ion monitoring and quantified by selective ion monitoring of m/z 183 and 197. The calibration curve was linear to 4 mg/L. The limit of quantification was 0.04 mg/L, and the analytical recovery was approximately 97%. The within-day and between-day imprecision (CV) was <6% and 9%, respectively. In a preliminary study of 12 children, the BU areas under the BU-time curve were 616-949 micromol. min/L after the first dose and 793-1143 micromol. min/L after the fifth dose. We conclude that the GC-MS procedure is suitable for routine analysis of plasma BU. PMID:9836718

  3. Electrophoretic concentration and sweeping-micellar electrokinetic chromatography analysis of cationic drugs in water samples.

    PubMed

    Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

    2015-07-01

    Sample preparation by electrophoretic concentration, followed by analysis using sweeping-micellar electrokinetic chromatography, was studied as a green and simple analytical strategy for the trace analysis of cationic drugs in water samples. Electrophoretic concentration was conducted using 50mmol/L ammonium acetate at pH 5 as acceptor electrolyte. Electrophoretic concentration was performed at 1.0kV for 50min and 0.5kV and 15min for purified and 10-fold diluted waste water samples, respectively. Sweeping-micellar electrokinetic chromatography was with 100mmol/L sodium phosphate at pH 2, 100mmol/L sodium dodecyl sulfate and 27.5%-v/v acetonitrile as separation electrolyte. The separation voltage was -20kV, UV-detection was at 200nm, and the acidified concentrate was injected for 36s at 1bar (or 72% of the total capillary length, 60cm). Both purified water and 10-fold diluted waste water exhibited a linear range of two orders of concentration magnitude. The coefficient of determination, and intra- and interday repeatability were 0.991-0.997, 2.5-6.2, and 4.4-9.7%RSD (n=6), respectively, for purified water. The values were 0.991-0.997, 3.4-7.1, and 8.7-9.8%RSD (n=6), correspondingly, for 10-fold diluted waste water. The method detection limit was in the range from 0.04-0.09 to 1.20-6.97ng/mL for purified and undiluted waste water, respectively. PMID:26008596

  4. Comparison of ultra-high performance supercritical fluid chromatography and ultra-high performance liquid chromatography for the analysis of pharmaceutical compounds.

    PubMed

    Grand-Guillaume Perrenoud, Alexandre; Veuthey, Jean-Luc; Guillarme, Davy

    2012-11-30

    Currently, columns packed with sub-2 ?m particles are widely employed in liquid chromatography but are scarcely used in supercritical fluid chromatography. The goal of the present study was to compare the performance, possibilities and limitations of both ultra-high performance liquid chromatography (UHPLC) and ultra-high performance supercritical fluid chromatography (UHPSFC) using columns packed with sub-2 ?m particles. For this purpose, a kinetic evaluation was first performed, and van Deemter curves and pressure plots were constructed and compared for columns packed with hybrid silica stationary phases composed of 1.7 and 3.5 ?m particles. As expected, the kinetic performance of the UHPSFC method was significantly better than that of the UHPLC. Indeed, the h(min) values were in the same range with both strategies and were between 2.2 and 2.8, but u(opt) was increased by a factor of >4 in UHPSFC conditions. Another obvious advantage of UHPSFC over UHPLC is related to the generated backpressure, which is significantly lower in the presence of a supercritical or subcritical fluid. However, the upper pressure limit of the UHPSFC system was only ?400 bar vs. ?1000 bar in the UHPLC system, which prevents the use of highly organic mobile phases at high flow rates in UHPSFC. Second, the impact of reducing the particle size (from 3.5 to 1.7 ?m) was evaluated in both UHPLC and UHPSFC conditions. The effect of frictional heating on the selectivity was demonstrated in UHPLC and that of fluid density or decompression cooling was highlighted in UHPSFC. However, in both cases, a change in selectivity was observed for only a limited number of compounds. Third, various types of column chemistries packed with 1.7 ?m particles were evaluated in both UHPLC and UHPSFC conditions using a model mixture of acidic, neutral and basic compounds. It has been shown that more drastic changes in selectivity were obtained using UHPSFC columns compared to those obtained by changing UHPLC columns. In addition, there was a good complementarity between the two separation modes. Finally, by combining the use of small particles with supercritical fluids as a mobile phase, it was possible to achieve the analysis of pharmaceutical compounds in less than 1 min or to attain a peak capacity of more than 250 in approximately 40 min, both with a high degree of repeatability. PMID:23092872

  5. Separation of Caffeine from Beverages and Analysis Using Thin-Layer Chromatography and Gas Chromatography-Mass Spectrometry

    ERIC Educational Resources Information Center

    Torres y Torres, Janelle L.; Hiley, Shauna L.; Lorimor, Steven P.; Rhoad, Jonathan S.; Caldwell, Benjamin D.; Zweerink, Gerald L.; Ducey, Michael

    2015-01-01

    The Characterization and Analysis of a Product (CAP) project is used to introduce first-semester general chemistry students to chemical instrumentation through the analysis of caffeine-containing beverage products. Some examples of these products have included coffee, tea, and energy drinks. Students perform at least three instrumental experiments…

  6. RAPID ANALYSIS OF CYANURIC ACID IN SWIMMING POOL WATERS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY USING POROUS GRAPHITIC CARBON

    EPA Science Inventory

    An innovative approach is presented for reducing analysis times of cynuric acid in swimming pool waters by high performance liquid chromatography (HPLC). The HPLC method exploits the unique selectivity of porous graphitic carbon (PGC) to fully resolve within 10 minutes cyanuric ...

  7. RAPID ANALYSIS OF CYNANURIC ACID IN SWIMMING POOL WATERS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY USING POROUS GRAPHITIC CARBON COLUMN

    EPA Science Inventory

    An innovative approach is presented for reducing analysis times of cyanuric acid in swimming pool waters by high performance liquid chromatography (HPLC). The HPLC method exploits the unique selectivity of porous graphitic carbon (PGC) to fully resolve cyanuric acid from other p...

  8. Liquid chromatography\\/time-of-flight\\/mass spectrometry (LC\\/TOF\\/MS) for the analysis of emerging contaminants

    Microsoft Academic Search

    E. Michael Thurman

    2003-01-01

    In this review, we focus on the importance of unequivocally detecting emerging contaminants, as well as establishing their presence in the environment by accurate mass spectrometric measurement techniques. The environmental issue of emerging contaminants is tied to the analysis of wastewater samples using the new analytical methods of the last decade, especially liquid chromatography coupled to tandem mass spectrometry (LC\\/MS\\/MS)

  9. ANALYSIS OF OCTYL- AND NONYLPHENOL AND THEIR ETHOXYLATES IN WATER AND SEDIMENTS BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A quantitative method for the analysis of octyl- and nonylphenol, and their ethoxylates (1 to 5) in water and sediment is presented. Extraction procedures are based on solid-phase extraction techniques. Identification and quantitation of the analytes is done by liquid chromatography coupled to tan...

  10. Improvements of a combined size exclusion chromatography and solid phase extraction approach for the clean-up of marine sediment samples for trace analysis of pesticides

    Microsoft Academic Search

    K. Bester; Heinrich Hühnerfuss

    1997-01-01

    Two methods based on gel permeation chromatography (GPC) [size exclusion chromatography] for the analysis of traces (ng\\/kg)\\u000a of nitrogen and phosphorus containing pesticides (like triazines or phosphothionates) from marine sediment samples are compared:\\u000a A macro GPC with Biobeads SX-3 and a chromatography on a high-performance (HP-GPC) column with UV-detection. Results for eight\\u000a triazine herbicides, two triazine metabolites, the phenylurea derivative

  11. Applying Chromatography.

    ERIC Educational Resources Information Center

    Klein, Jessie W.; Patev, Paul

    1998-01-01

    Presents three experiments to introduce students to different kinds of chromatography: (1) paper chromatography; (2) gel filtration chromatography; and (3) reverse-phase liquid chromatography. Written in the form of a laboratory manual, explanations of each of the techniques, materials needed, procedures, and a glossary are included. (PVD)

  12. Analysis of drugs of abuse in wastewater by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    PubMed

    van Nuijs, Alexander L N; Tarcomnicu, Isabela; Bervoets, Lieven; Blust, Ronny; Jorens, Philippe G; Neels, Hugo; Covaci, Adrian

    2009-10-01

    The simultaneous analysis of nine drugs of abuse (DOAs) and their metabolites (amphetamine, methamphetamine, methylenedioxymethamphetamine, methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine, cocaine, benzoylecgonine, ecgonine methyl ester and 6-monoacetylmorphine) in wastewater based on hydrophilic interaction liquid chromatography (HILIC) coupled to tandem mass spectrometry (MS/MS) was optimised and validated. For each analyte, the deuterated analogue was used for quantification. The separation by HILIC showed good performance for all compounds, especially for the hydrophilic compounds, which elute early (amphetamine-like stimulants) or show no retention (ecgonine methyl ester) in reversed-phase liquid chromatography. Sample preparation based on solid-phase extraction was optimised by comparing Oasis HLB and Oasis MCX sorbents for various parameters such as sample pH, amount of sorbent bed and washing solvent. The method was validated for each compound by assessing the following parameters (following International Conference on Harmonisation guidelines): specificity, limit of quantification (LOQ), linearity, accuracy, precision, recovery and matrix effects. LOQs were 2 ng/L for 6-monoacetylmorphine, ecgonine methyl ester and amphetamine and 1 ng/L for the rest of the compounds, corresponding with the lowest point in the calibration curve. Except for 6-monoacetylmorphine, all compounds were detected from 1 to 819 ng/L in influent wastewater samples (n = 12) collected from 11 different wastewater treatment plants across Belgium. The presence of ecgonine methyl ester in wastewater could be demonstrated for the first time. In the future, the new HILIC-MS/MS method will be applied to assess the use of DOAs in Belgium using the "sewage epidemiology" approach. PMID:19685341

  13. Native fluorescent detection with sequential injection chromatography for doping control analysis

    PubMed Central

    2013-01-01

    Background Sequential injection chromatography (SIC) is a young, ten years old, separation technique. It was proposed with the benefits of reagent-saving, rapid analysis, system miniaturization and simplicity. SIC with UV detection has proven to be efficient mostly for pharmaceutical analysis. In the current study, a stand-alone multi-wavelength fluorescence (FL) detector was coupled to an SIC system. The hyphenation was exploited for developing an SIC-FL method for the separation and quantification of amiloride (AML) and furosemide (FSM) in human urine and tablet formulation. Results AML and FSM were detected using excitation maxima at 380 and 270 nm, respectively, and emission maxima at 413 and 470 nm, respectively. The separation was accomplished in less than 2.0 min into a C18 monolithic column (50?×?4.6 nm) with a mobile phase containing 25 mmol/L phosphate buffer (pH 4.0): acetonitrile: (35:65, v/v). The detection limits were found to be 12 and 470 ng/mL for AML and FSM, respectively. Conclusions The proposed SIC-FL method features satisfactory sensitivity for AML and FSM in urine samples for the minimum required performance limits recommended by the World Anti-Doping Agency, besides a downscaled consumption of reagents and high rapidity for industrial-scale analysis of pharmaceutical preparations. PMID:23985079

  14. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    NASA Astrophysics Data System (ADS)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

  15. Identification of Dactylopius cochineal species with high-performance liquid chromatography and multivariate data analysis.

    PubMed

    Serrano, Ana; Sousa, Micaela; Hallett, Jessica; Simmonds, Monique S J; Nesbitt, Mark; Lopes, João A

    2013-10-21

    Identification of American cochineal species (Dactylopius genus) can provide important information for the study of historical works of art, entomology, cosmetics, pharmaceuticals and foods. In this study, validated species of Dactylopius, including the domesticated cochineal D. coccus, were analysed by high-performance liquid chromatography with a diode array detector (HPLC-DAD) and submitted to multivariate data analysis, in order to discriminate the species and hence construct a reference library for a wide range of applications. Principal components analysis (PCA) and partial least squares discriminant analysis (PLSDA) models successfully provided accurate species classifications. This library was then applied to the identification of 72 historical insect specimens of unidentified species, mostly dating from the 19th century, and belonging to the Economic Botany Collection, Royal Botanic Gardens, Kew, England. With this approach it was possible to identify anomalies in how insects were labelled historically, as several of them were revealed not to be cochineal. Nevertheless, more than 85% of the collection was determined to be species of Dactylopius and the majority of the specimens were identified as D. coccus. These results have shown that HPLC-DAD, in combination with suitable chemometric methods, is a powerful approach for discriminating related cochineal species. PMID:23961534

  16. Denaturing high-performance liquid chromatography using the WAVE DNA fragment analysis system.

    PubMed

    Donohoe, Elizabeth

    2005-01-01

    Denaturing high-performance liquid chromatography (DHPLC) is a chromatographic mutation analysis technique that is based on temperature-dependent separation of DNA containing mismatched base pairs from polymerase chain reaction (PCR)-amplified DNA fragments. The WAVE system, developed for DHPLC analysis, allows for unattended analysis of 96 samples directly from a PCR plate under a number of different conditions. It utilizes a Peltier cooling platform to maintain sample integrity. Sample detection is achieved via UV absorbance at 260 nm, thereby avoiding the cost, safety, variability, or waste disposal issues associated with radioisotopic, enzyme-linked, or fluorescence detection systems. There are four key aspects to successfully detecting mutations on the WAVE: (1) PCR primer design, (2) PCR protocol, (3) separation gradient, and (4) separation temperature. Provided these procedures are carried out correctly, almost 100% detection of single-nucleotide polymorphisms (SNPs) and small deletion/insertion mutations can be achieved. For this reason, DHPLC is a powerful tool for identifying mutations in candidate genes for hypertension. PMID:16028684

  17. The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

    PubMed

    Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

    2014-03-01

    In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. PMID:24412698

  18. Glycomic Analysis by Glycoprotein Immobilization for Glycan Extraction and Liquid Chromatography on Microfluidic Chip

    PubMed Central

    Yang, Shuang; Eshghi, Shadi Toghi; Chiu, Hanching; DeVoe, Don L.; Zhang, Hui

    2013-01-01

    Glycosylation is one of the most common protein modifications and profoundly regulates many biological processes. Aberrant glycosylation is reported to associate with diseases such as cancers, human immunodeficiency virus, and immune disorders. It is considerably important to study protein glycosylation and the associated glycans for diagnostics and disease prognostics. Unlike other protein modifications, glycans attached to proteins are enormously complex. Therefore, the comprehensive analysis of glycans from biological or clinical samples is an unmet technical challenge. Development of the high-throughput method will facilitate the glycomics analysis. In this study, we developed a novel method for the high-throughput analysis of N-glycans from glycoproteins using glycoprotein immobilization for glycan extraction (GIG) coupled with liquid chromatography (LC) in an integrated microfluidic platform (chipLC). The separated glycans were then analyzed by mass spectrometry. Briefly, proteins were first immobilized on a solid support. Glycans on immobilized glycoproteins were modified on solid phase to increase the detection and structure analysis. N-Glycans were then enzymatically released and subsequentially separated by porous graphitized carbon particles packed in the same device. By applying the GIG-chipLC for glycomic analysis of human sera, we identified N-glycans with 148 distinct N-glycan masses. The platform was used to analyze N-glycans from mouse heart tissue and serum. The extracted N-glycans from tissues indicated that unique unsialylated N-glycans were detected in tissues that were missing from the proximal or distal serum, whereas common N-glycans from tissues and serum have mature and sialylated structures. The GIG-chipLC provides a simple and robust platform for glycomic analysis of complex biological and clinical samples. PMID:24111616

  19. Two-column sequential injection chromatography--new approach for fast and effective analysis and its comparison with gradient elution chromatography.

    PubMed

    Chocholous, Petr; Satínský, Dalibor; Sklenárová, Hana; Solich, Petr

    2010-05-23

    This work presents novel approach in low-pressure chromatography flow systems--two-column Sequential Injection Chromatography (2-C SIC) and its comparison with gradient elution chromatography on the same instrument. The system was equipped with two different chromatographic columns (connected to selection valve in parallel design) for isocratic separation and determination of all components in composed anti-inflammatory pharmaceutical preparation (tablets). The sample was first injected on the first column of length 30 mm where less retained analytes were separated and then the sample was injected on the second column of length 10 mm where more retained analytes were separated. The SIC system was based on a commercial SIChrom manifold (8-port high-pressure selection valve and medium-pressure syringe pump with 4 mL reservoir) (FIAlab, USA) with two commercially available monolithic columns the "first column" Chromolith Flash RP-18e (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.) and the "second column" Chromolith RP-18e (10 mm x 4.6 mm i.d.) and CCD UV-vis detector USB 4000 with micro-volume 1.0 cm Z flow cell. Two mobile phases were used for analysis (one for each column). The mobile phase 1 used for elution of paracetamol, caffeine and salicylic acid (internal standard) was acetonitrile/water (10:90, v/v, the water part of pH 3.5 adjusted with acetic acid), flow rate was 0.9 mL min(-1) (volume 3.0 mL of mobile phase per analysis). The mobile phase 2 used for elution of propyphenazone was acetonitrile/water (30:70, v/v); flow rate was 1.2 mL min(-1) (volume 1.5 mL of mobile phase per analysis). Absorbance was monitored at 210 nm. Samples were prepared by dissolving of one tablet in 30% acetonitrile and 10 microL of filtered supernatant was injected on each column (2 x 10 microL). The chromatographic resolution between all compounds was >1.45 and analysis time was 5.5 min under the optimal conditions. Limits of detection were determined at 0.4 microg mL(-1) for paracetamol, at 0.5 microg mL(-1) for caffeine and at 0.7 microg mL(-1) for propyphenazone. The new two-column chromatographic set-up developed as an alternative approach to gradient elution chromatography shows evident advantages (time and solvent reduction more than one-third) as compared with single-column gradient SIC method with Chromolith Flash RP-18 (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.). PMID:20457303

  20. [Analysis of triacylglycerol composition of perilla oil by combination of non-aqueous reversed-phase high performance liquid chromatography with gas chromatography].

    PubMed

    Cui, K; Ding, X; Xiao, G; Dai, J

    1997-11-01

    Perilla oil was verified to be a rich source of polyunsaturated fatty acid (PUFA). Its linolenic content is 64.82%, the highest in the plants. Its triacylglycerol (TAG) components were isolated and identified first time in this paper by a combination of non-aqueous reversed-phase high performance liquid chromatography (RP-HPLC) with gas chromatography (GC). The TAG of perilla oil were isolated by HPLC with a Zorbax ODS column (5 microm, 4.6 mm i.d. x 250 mm; Dupont, Inc) and differential refractometer. The eluent was acetone/acetonitrile (80:20, V/V) with flow rate of 1.0 mL/min. The TAG component acyl groups were converted to fatty acid methyl esters (FAME). The acyl constituents for each TAG were determined by GC analysis. Gas chromatography of FAMEs was performed with a AC20 Carbowax 20M column (30 m x 0.32 mm i.d.). Detector and injection port temperatures were 260 degrees C. Column temperature was programmed from 120 degrees C, 1 min initially hold, then 8 degrees C/min to 220 degrees C and finally hold for 10 min. Nitrogen was the carrier gas. FAMEs peaks were identified by comparison of their retention times with those of standards. The retention times of the palmitic, stearic, oleic, linoleic, n-nonadecanoic acid (internal standard) and linolenic FAMEs were 10.7, 13.0, 13.3, 13.8, 14.2 and 14.7 min respectively. Five main components were determined. They were LnLnLn (34.10%), LnLnL (13.22%), LnLL (6.22%), LnLnO (11.38%) and LnLnP (9.17%). The TAG contents were corrected from their fatty acids content. The combination of non-aqueous RP-HPLC with GC is a simple and rapid method for the analysis of oil TAG structure and is also very helpful for the identification of oil quality. PMID:15739324

  1. US crude oil, natural gas, and natural gas liquids reserves, 1992 annual report

    SciTech Connect

    Not Available

    1993-10-18

    This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1992, as well as production volumes for the United States, and selected States and State subdivisions for the year 1992. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), its two major components (nonassociated and associated-dissolved gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, two components of natural gas liquids, lease condensate and natural gas plant liquids, have their reserves and production data presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1992 is provided.

  2. Efficient gas-liquid contact using microfluidic membrane devices with staggered herringbone mixers.

    PubMed

    Femmer, Tim; Eggersdorfer, Max L; Kuehne, Alexander J C; Wessling, Matthias

    2015-07-14

    We describe a novel membrane based gas-liquid-contacting device with increased mass transport and reduced pressure loss by combining a membrane with a staggered herringbone static mixer. Herringbone structures are imposed on the microfluidic channel geometry via soft lithography, acting as mixers which introduce secondary flows at the membrane interface. Such flows include Dean vortices and Taylor flows generating effective mixing while improving mass transport and preventing concentration polarization in microfluidic channels. Furthermore, our static herringbone mixer membranes effectively reduce pressure losses leading to devices with enhanced transfer properties for microfluidic gas-liquid contact. We investigate the red blood cell distribution to tailor our devices towards miniaturised extracorporeal membrane oxygenation and improved comfort of patients with lung insufficiencies. PMID:26087992

  3. U.S. crude oil, natural gas, and natural gas liquids reserves 1997 annual report

    SciTech Connect

    Wood, John H.; Grape, Steven G.; Green, Rhonda S.

    1998-12-01

    This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1997, as well as production volumes for the US and selected States and State subdivisions for the year 1997. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), nonassociated gas and associated-dissolved gas (which are the two major types of wet natural gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, reserve estimates for two types of natural gas liquids, lease condensate and natural gas plant liquids, are presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1997 is provided. 21 figs., 16 tabs.

  4. Analysis of free and esterified sterols in fats and oils by flash chromatography, gas chromatography and electrospray tandem mass spectrometry

    Microsoft Academic Search

    Paavo Kalo; Tiia Kuuranne

    2001-01-01

    A method for the analysis of free and esterified sterols has been developed. Fat or oil samples were separated on solid-phase extraction silica gel columns into a sterol ester fraction, a fraction of triacylglycerols, and a free sterol fraction containing partial acylglycerols and residual triacylglycerols. Sterol esters and acylglycerols of the free sterol fraction were transesterified to methyl esters. The

  5. Determination of the pressure at the gas-liquid interface using acoustic speed measurements 

    E-print Network

    Heggelund, Dag Gustav

    1988-01-01

    measurements. A method for calculating the specific gravity of a gas mixture given acoustic velocity has been developed. The method can be employed to accounts for changing specific gravity of the gas mixture with depth. The method employed is based.... The method has been applied to field data to demonstrate its use in determining the pressure at the gas- liquid interface, and in estimating the specific gravity of the gas mixture from well sounder measurements. Uniqueness problems associated with minima...

  6. A review of two-phase gas–liquid adiabatic flow characteristics in micro-channels

    Microsoft Academic Search

    Sira Saisorn; Somchai Wongwises

    2008-01-01

    A literature review of recent research on two-phase flow in micro-channels is provided in this article. Researches on the micro-hydrodynamics concerned with two-phase gas–liquid adiabatic flow characteristics in both circular and non-circular micro-channels are discussed. This review aims to survey and identify new findings obtained from this attractive area, which may contribute to optimum design and process control of high

  7. A MULTILOOP SENSOR FOR THE FLOWRATE MEASUREMENT OF GAS-LIQUID TWO-PHASE FLOW

    Microsoft Academic Search

    Xie Dailiang; Liang Guowei; Wang Fang

    A multi-loop flowmeter is designed for the flowrate measurement of the gas-liquid two-phase flow. The differential pressure signals can be collected from the multi- loop sensor at different positions. The total flowrate measurement model is established according to the average differential pressure value obtained from the optimal position. The time serial of the signals is obtained by using the high

  8. Computational model and simulations of gas-liquid-solid three-phase interactions

    NASA Astrophysics Data System (ADS)

    Zhang, Lucy; Wang, Chu

    2013-11-01

    A computational technique to model three-phase (gas-liquid-solid) interactions is proposed in this study. This numerical algorithm couples a connectivity-free front-tracking method that treats gas-liquid multi-fluid interface to the immersed finite element method that treats fully-coupled fluid-solid interactions. The numerical framework is based on a non-boundary-fitted meshing technique where the background grid is fixed where no mesh-updating or re-meshing is required. An indicator function is used to identify the gas from the liquid, and the fluid (gas or liquid) from the solid. Several 2-D and 3-D validation cases are demonstrated to show the accuracy and the robustness of the method. A computational technique to model three-phase (gas-liquid-solid) interactions is proposed in this study. This numerical algorithm couples a connectivity-free front-tracking method that treats gas-liquid multi-fluid interface to the immersed finite element method that treats fully-coupled fluid-solid interactions. The numerical framework is based on a non-boundary-fitted meshing technique where the background grid is fixed where no mesh-updating or re-meshing is required. An indicator function is used to identify the gas from the liquid, and the fluid (gas or liquid) from the solid. Several 2-D and 3-D validation cases are demonstrated to show the accuracy and the robustness of the method. Funding from NRC and CCNI computational facility at Rensselaer Polytechnic Institute are greatly acknowledged.

  9. Gas chromatography mass spectrometry computer analysis of volatile halogenated hydrocarbons in man and his environment--A multimedia environmental study.

    PubMed

    Barkley, J; Bunch, J; Bursey, J T; Castillo, N; Cooper, S D; Davis, J M; Erickson, M D; Harris, B S; Kirkpatrick, M; Michael, L C; Parks, S P; Pellizzari, E D; Ray, M; Smith, D; Tomer, K B; Wagner, R; Zweidinger, R A

    1980-04-01

    As part of a study to make a comparative analysis of selected halogenated compounds in man and the environmental media, a quantitative gas chromatography mass spectrometric analysis of the levels of the halogenated compounds found in the breath, blood and urine of an exposed population (Old Love Canal area, Niagara, New York) and their immediate environment (air and water) was undertaken. In addition, levels of halogenated hydrocarbons in air samples taken in the general Buffalo, Niagara Falls area were determined. PMID:7448328

  10. Analysis of psilocybin and psilocin in Psilocybe subcubensis GUZMÁN by ion mobility spectrometry and gas chromatography–mass spectrometry

    Microsoft Academic Search

    Thomas Keller; Andrea Schneider; Priska Regenscheit; Richard Dirnhofer; Thomas Rücker; Jürgen Jaspers; Wolfgang Kisser

    1999-01-01

    A new method has been developed for the rapid analysis of psilocybin and\\/or psilocin in fungus material using ion mobility spectrometry. Quantitative analysis was performed by gas chromatography–mass spectrometry after a simple one-step extraction involving homogenization of the dried fruit bodies of fungi in chloroform and derivatization with MSTFA. The proposed methods resulted in rapid procedures useful in analyzing psychotropic

  11. Applications of supercritical fluid chromatography-mass spectrometry in the analysis of fossil fuels

    Microsoft Academic Search

    E. K. Chess; H. T. Kalinoski; B. W. Wright; H. R. Udseth; R. D. Smith

    1987-01-01

    Because the physical properties of a supercritical fluid (e.g., low viscosity, high diffusivity, and reasonable solubility, etc.) impart characteristics to the supercritical mobile phase intermediate to those of a liquid and a gas, SFC has allowed the separation of some components of complex mixtures that were not separable by gas chromatography or high performance liquid chromatography. The application of SFC-MS

  12. Recent advances in ultra-high performance liquid chromatography for the analysis of traditional chinese medicine

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Traditional Chinese medicines (TCMs) have been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra Performance Liquid Chromatography (UHPLC) is a relatively new technique offering new possibilities in liquid chromatography. This paper reviews recen...

  13. US crude oil, natural gas, and natural gas liquids reserves 1996 annual report

    SciTech Connect

    NONE

    1997-12-01

    The EIA annual reserves report series is the only source of comprehensive domestic proved reserves estimates. This publication is used by the Congress, Federal and State agencies, industry, and other interested parties to obtain accurate estimates of the Nation`s proved reserves of crude oil, natural gas, and natural gas liquids. These data are essential to the development, implementation, and evaluation of energy policy and legislation. This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1996, as well as production volumes for the US and selected States and State subdivisions for the year 1996. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), nonassociated gas and associated-dissolved gas (which are the two major types of wet natural gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, reserve estimates for two types of natural gas liquids, lease condensate and natural gas plant liquids, are presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1996 is provided. 21 figs., 16 tabs.

  14. Cavitation and gas-liquid flow in fluid machinery and devices. FED-Volume 190

    SciTech Connect

    O`Hern, T.J.; Kim, J.H.; Morgan, W.B.; Furuya, O. [eds.

    1994-12-31

    Cavitation and gas-liquid two-phase flow have remained important areas in many industrial applications and constantly provided challenges for academic researchers and industrial practitioners alike. Cavitation and two-phase flow commonly occur in fluid machinery such as pumps, propellers, and fluid devices such as orifices, valves, and diffusers. Cavitation not only degrades the performance of these machines and devices but deteriorates the materials. Gas-liquid two-phase flow has also been known to degrade the performance of pumps and propellers and can often induce an instability. The industrial applications of cavitation and two-phase flow can be found in power plants, ship propellers, hydrofoils, and aerospace equipment, to name but a few. The papers presented in this volume reflect the variety and richness of cavitation and gas-liquid two-phase flow in various flow transporting components and the increasing role they play in modern and conventional technologies. Separate abstracts were prepared for 35 papers in this book.

  15. U.S. crude oil, natural gas, and natural gas liquids reserves 1995 annual report

    SciTech Connect

    NONE

    1996-11-01

    The EIA annual reserves report series is the only source of comprehensive domestic proved reserves estimates. This publication is used by the Congress, Federal and State agencies, industry, and other interested parties to obtain accurate estimates of the Nation`s proved reserves of crude oil, natural gas, and natural gas liquids. These data are essential to the development, implementation, and evaluation of energy policy and legislation. This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1995, as well as production volumes for the US and selected States and State subdivisions for the year 1995. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), nonassociated gas and associated-dissolved gas (which are the two major types of wet natural gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, reserve estimates for two types of natural gas liquids, lease condensate and natural gas plant liquids, are presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1995 is provided. 21 figs., 16 tabs.

  16. Microporous hydrophobic hollow fiber modules for gas-liquid phase separation in microgravity

    NASA Astrophysics Data System (ADS)

    Noyes, Gary

    Gas-liquid interphase mass transfer operations, such as gas-liquid phase separation, gas absorption into liquid or dissolved gas separation from liquid, gas humidification and drying via liquid contact, and evaporative cooling are readily accomplished on the Earth with settling/spray chambers, packed towers, or bubble columns. This paper reports on gas-water mass transfer tests performed utilizing microporous hydrophobic Hollow Fiber Modules (HFMs) of the type currently employed as blood oxygenators in heart-lung machines. In these HFMs, gases are transferrred to and from water or other hydrophilic liquids through the microporous fiber walls; liquid water does not enter the pores of the highly hydrophobic wall material. The experiments included air-water phase separation, absorption of oxygen and carbon dioxide into water and separation of these dissolved gases from water, air humidification and drying by contact with temperature-controlled water, and controlled evaporation of water into a vacuum. In each of these experiments, a small, light HFM sucessfully performed the mass tranfer function, with no leakage of liquid water through the porous walls of the hollow fibers, even with high pressure across the fiber wall for extended periods of time. These results demonstrate that gas-liquid mass transfer unit operations on hydrophilic liquids, implemented with microporous hydrophobic HFM technology, are ready for use in microgravity fluid processing systems.

  17. A parametric study for high-efficiency gas-liquid separator design

    NASA Astrophysics Data System (ADS)

    Nagdewe, S.; Kwoon, J. K.; Kim, H. D.; Kim, D. S.; Kwak, K. M.; Setoguchi, Toshiaki

    2008-09-01

    A gas liquid centrifugal separator is widely used in industry on account of its simple geometry and little maintenance. These separators have considerable advantages over filters, scrubbers or precipitators in term of compact design, lower pressure drop and higher capacity. A gas liquid centrifugal separator is a device that utilizes centrifugal forces and low pressure caused by rotational motion to separate liquid from gas by density differences. Efficient and reliable separation is required for the optimum operation. These separators are often operated at less than peak efficiency due to the entrainment of separated liquid through an outlet pipe which is closely associated with the very complicated flow phenomena involved. Design parameters such as length of the separation space, vane exit angle, inlet to outlet diameter ratio, models for separation efficiency and pressure drop as a function of physical dimensions are not available in literature. This leaves the designer with very little to go on except known designs and experimentation. The aim of present study is to perform a parametric study to get higher efficiency for gas-liquid separator. A parametric study has been carried out with the help of CFD tools to analyze a separation performance of a centrifugal separator by varying the length of separator space. The best design parameters are analyzed based upon obtained results, tangential velocities, vortices, total pressure losses. From the present study several attempts are made to improve the performance of conventional centrifugal separators.

  18. Microwave-assisted derivatization procedures for gas chromatography/mass spectrometry analysis.

    PubMed

    Söderholm, Sandra L; Damm, Markus; Kappe, C Oliver

    2010-11-01

    In this review, published applications of microwave-assisted derivatization procedures for gas chromatography/mass spectrometry (GC/MS) are summarized. Among the broad range of analytical techniques available, GC/MS is still the method of choice for most high-throughput screening procedures in forensic/clinical toxicology, doping control and food and environmental analysis. Despite the many advantages of the GC/MS method, time-consuming derivatization steps are often required in order to obtain desirable chromatographic characteristics or to improve the stability and detectability of the target analytes. These derivatization processes typically require reaction times from 30 min up to several hours at elevated temperature. In contrast, microwave protocols have demonstrated to be able to reduce the time required for derivatization to a few minutes, and can thus very effectively shorten the overall analysis time, in particular when carried out in a high-throughput format. Herein, the literature in this field is summarized and recent experimental techniques for performing parallel GC/MS derivatization protocols are discussed. PMID:20225067

  19. Global Analysis of the Membrane Subproteome of Pseudomonas aeruginosa using Liquid Chromatography-Tandem Mass Spectrometry

    SciTech Connect

    Blonder, Josip; Goshe, Michael B.; Xiao, Wenzhong; Camp, David G.; Wingerd, Mark A.; Davis, Ronald W.; Smith, Richard D.

    2004-05-30

    Pseudomonas aeruginosa is one of the most significant opportunistic bacterial pathogens in humans causing infections and premature death in patients with cystic fibrosis, AIDS, severe burns, organ transplants or cancer. Liquid chromatography coupled online with tandem mass spectrometry (LC-MS/MS) was used for the large-scale proteomic analysis of the P. aeruginosa membrane subproteome. Concomitantly, an affinity labeling technique, using iodoacetyl-PEO biotin to tag cysteinyl-containing proteins, permitted the enrichment and detection of lower abundance membrane proteins. The application of these approaches resulted in the identification of 786 proteins. A total of 333 proteins (42%) had a minimum of one transmembrane domain (TMD; ranging from 1 to 14) and 195 proteins were classified as hydrophobic based on their positive GRAVY values (ranging from 0.01 to 1.32). Key integral inner and outer membrane proteins involved in adaptation and antibiotic resistance were conclusively identified, including the detection of 53% of all predicted opr-type porins (outer integral membrane proteins) and all the components of the mexA-mexB-oprM transmembrane protein complex. This work represents the most comprehensive qualitative proteomic analysis of the membrane subproteome of P. aeruginosa and for prokaryotes in general to date.

  20. Phthalate analysis by gas chromatography-mass spectrometry: blank problems related to the syringe needle.

    PubMed

    Marega, Milena; Grob, Konrad; Moret, Sabrina; Conte, Lanfranco

    2013-01-18

    For the analysis of the most commonly encountered phthalates by gas chromatography-mass spectrometry (GC-MS), absorption of phthalates from the laboratory air on the outer wall of the syringe needle is shown to be an important contribution to the blank problems. It was investigated for programmed temperature vapourizing (PTV) injection. Cleaning of the needle in automated injection is of modest efficiency, since the needle cannot be immersed deeply enough into the wash vial. Two approaches were studied to minimize the transfer into the column: (i) cleaning of the needle in the injector prior to splitless injection by inserting the needle in split mode while the precolumn is backflushed, which presupposes a high injector temperature to be efficient; (ii) injection under conditions minimizing thermal desorption from the needle wall, i.e. fast injection at low injector temperature (e.g. 40 °C). Both approaches resulted in blank levels of around 0.1 pg for diisobutyl phthalate (DIBP) and dibutyl phthalate (DBP), and of around 1 pg for di(2-ethylhexyl) phthalate (DEHP). They could be useful tools in existing or future methods for the analysis of phthalates or other compounds causing blank problems through contamination of the laboratory air. PMID:23265992

  1. Application of high-performance ion-exchange chromatography to the analysis of cytosolic glucocorticoid receptor.

    PubMed

    Denis, M; Guendouz, F; Blanchardie, P; Bernard, S; Lustenberger, P

    1988-01-01

    The use of high-performance ion-exchange chromatography (HPIEC) on a Mono Q column was investigated for the analysis of glucocorticoid receptor. In the presence of 10 mM sodium molybdate, both liganded and unliganded glucocorticoid receptor were eluted as a single and sharp peak (0.32 M NaCl). In the absence of molybdate and after exposure to heat and salt, another peak of specifically bound radioactivity was eluted with 0.08 M NaCl. When HPIEC was performed in the absence of molybdate, two molecular forms of the liganded receptor were detected which eluted with 0.08 M NaCl (Stokes' radius Rs = 5.1 nm, s20,w = 4.6 S, calculated mol. wt Mr approximately 100,000) and 0.32 M NaCl (Rs = 7.3 nm, S20,w = 9.0 S, calculated Mr approximately 280,000). Analysis of both forms with mini-columns of DNA-Ultrogel, DEAE-Trisacryl and hydroxylapatite (HA-Ultrogel) confirmed the identity of the two peaks with transformed and non-transformed glucocorticoid-receptor complexes. These results suggest that HPIEC may provide a useful tool for the rapid resolution and quantification of receptor molecular forms. PMID:3386254

  2. Analysis and purification of IgG4 bispecific antibodies by a mixed-mode chromatography.

    PubMed

    Yang, Xiaoyu; Zhang, Ying; Wang, Fengqiang; Wang, Larry Jin; Richardson, Daisy; Shameem, Mohammed; Ambrogelly, Alexandre

    2015-09-01

    Therapeutic non-hinge-modified IgG4 molecules form bispecific hybrid antibodies with endogenous human IgG4 molecules via a process known as Fab-arm exchange (or called half molecule exchange). Analysis of the bispecific hybrids is critical for studies of half molecule exchange. A number of analytical methods are available to detect IgG4 hybrids. These methods mostly necessitate labeling or alteration of the model IgG4 molecules, or rely on time-consuming immunoassays and mass spectrometry. In addition, these methods do not allow isolation of hybrid antibodies. We report here the only analytical method to date that relies on chromatographic separation for detection of hybrids formed from intact antibodies in their native forms using pembrolizumab as an example. This method employs a mixed-mode chromatography using a Sepax Zenix SEC-300 column to separate a bispecific hybrid from the parental antibodies. The simultaneous quantitative monitoring of the newly formed hybrid and parental antibodies was achieved by UV absorption and/or protein fluorescence. The bispecific hybrid antibodies were purified with the same method for further biochemical characterization. The method has allowed monitoring of half molecule exchange between a human serum IgG4 and a tested IgG4 molecule, and has been implemented for the analysis of in vitro as well as in vivo samples. PMID:26091837

  3. Surface-sampling and analysis of TATP by swabbing and gas chromatography/mass spectrometry.

    PubMed

    Romolo, Francesco Saverio; Cassioli, Luigi; Grossi, Silvana; Cinelli, Giuseppe; Russo, Mario Vincenzo

    2013-01-10

    The method of sample recovery for trace detection and identification of explosives plays a critical role in several criminal investigations. After bombing, there can be difficulties in sending big objects to a laboratory for analysis. Traces can also be searched for on large surfaces, on hands of suspects or on surfaces where the explosive was placed during preparatory phases (e.g. places where an IED was assembled, vehicles used for transportation, etc.). In this work, triacetone triperoxide (TATP) was synthesized from commercial precursors following reported methods. Several portions of about 6mg of TATP were then spread on different surfaces (e.g. floors, tables, etc.) or used in handling tests. Three different swabbing systems were used: a commercial swab, pre-wetted with propan-2-ol (isopropanol) and water (7:3), dry paper swabs, and cotton swabs wetted with propan-2-ol. Paper and commercial swabs were also used to sample a metal plate, where a small charge of about 4g of TATP was detonated. Swabs were sealed in small glass jars with screw caps and Parafilm(®) M and sent to the laboratory for analysis. Swabs were extracted and analysed several weeks later by gas chromatography/mass spectrometry. All the three systems gave positive results, but wetted swabs collected higher amounts of TATP. The developed procedure showed its suitability for use in real cases, allowing TATP detection in several simulations, including a situation in which people wash their hands after handling the explosive. PMID:23219697

  4. Analysis of formose sugar and formaldehyde by high-performance liquid chromatography.

    PubMed

    Iqbal, Md Zafar; Novalin, Senad

    2009-06-26

    Formose sugar and formaldehyde (HCHO) were analyzed using high-performance liquid chromatography (HPLC) utilizing a CarboPac PA1 column (Dionex) and pulsed amperometric detection. This HPLC system was unsuitable for the analysis of formose sugar and HCHO and thus reducing sugars and unconverted HCHO were determined by endowing them with charges through a derivatization method using 2,4-dinitrophenylhydrazine. The separation and detection of compounds were performed by three Chromolith RP-C18 columns (Merck) and diode array detection, at a wavelength of 360 nm ultraviolet light, respectively. Lower sugars (except HCHO) showed some instabilities when the derivatized samples were kept for the extended periods of time. For C(5) and consecutive higher sugars, a certain derivatization time was necessary. In the present case (formose reaction with partial HCHO conversion), approximately 18 h may be a reasonable compromise for the derivatization reaction. A derivatization agent to compound mole ratio of up to 100:1 was required to complete the derivatization of C(4) and higher sugars. However, the analysis of C(4) and consecutive higher sugars is problematic for example due to overlapping of peaks or branched-chain sugars. PMID:19446299

  5. Proteomic Analysis of the Organ of Corti Using Nanoscale Liquid Chromatography Coupled with Tandem Mass Spectrometry

    PubMed Central

    Peng, Hong; Liu, Miao; Pecka, Jason; Beisel, Kirk W.; Ding, Shi-Jian

    2012-01-01

    The organ of Corti (OC) in the cochlea plays an essential role in auditory signal transduction in the inner ear. For its minute size and trace amount of proteins, the identification of the molecules in pathophysiologic processes in the bone-encapsulated OC requires both delicate separation and a highly sensitive analytical tool. Previously, we reported the development of a high resolution metal-free nanoscale liquid chromatography system for highly sensitive phosphoproteomic analysis. Here this system was coupled with a LTQ-Orbitrap XL mass spectrometer to investigate the OC proteome from normal hearing FVB/N male mice. A total of 628 proteins were identified from six replicates of single LC-MS/MS analysis, with a false discovery rate of 1% using the decoy database approach by the OMSSA search engine. This is currently the largest proteome dataset for the OC. A total of 11 proteins, including cochlin, myosin VI, and myosin IX, were identified that when defective are associated with hearing impairment or loss. This study demonstrated the effectiveness of our nanoLC-MS/MS platform for sensitive identification of hearing loss-associated proteins from minute amount of tissue samples. PMID:22942697

  6. In situ Analysis of Organic Compounds on Mars using Chemical Derivatization and Gas Chromatography Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Glavin, D. P.; Buch, A.; Cabane, M.; Coll, P.; Navarro-Gonzalez, R.; Mahaffy, P. R.

    2005-01-01

    One of the core science objectives of NASA's 2009 Mars Science Laboratory (MSL) mission is to determine the past or present habitability of Mars. The search for key organic compounds relevant to terrestrial life will be an important part of that assessment. We have developed a protocol for the analysis of amino acids and carboxylic acids in Mars analogue materials using gas chromatography mass spectrometry (GCMS). As shown, a variety of carboxylic acids were readily identified in soil collected from the Atacama Desert in Chile at part-per-billion levels by GCMS after extraction and chemical derivatization using the reagent N,N-tert.-butyl (dimethylsilyl) trifluoroacetamide (MTBSTFA). Several derivatized amino acids including glycine and alanine were also detected by GCMS in the Atacama soil at lower concentrations (chromatogram not shown). Lacking derivatization capability, the Viking pyrolysis GCMS instruments could not have detected amino acids and carboxylic acids, since these non-volatile compounds require chemical transformation into volatile species that are stable in a GC column. We are currently optimizing the chemical extraction and derivatization technique for in situ GCMS analysis on Mars. Laboratory results of analyses of Atacama Desert samples and other Mars analogue materials using this protocol will be presented.

  7. Analysis of the Glycoproteome of Toxoplasma gondii using Lectin Affinity Chromatography and Tandem Mass Spectrometry

    PubMed Central

    Luo, Qilie; Upadhya, Rajendra; Zhang, Hong; Madrid-Aliste, Carlos; Nieves, Edward; Kim, Kami; Angeletti, Ruth Hogue; Weiss, Louis M.

    2011-01-01

    Glycoproteins are involved in many important molecular recognition processes including invasion, adhesion, differentiation, and development. To identify the glycoproteins of Toxoplasma gondii, a proteomic analysis was undertaken. T. gondii proteins were prepared and fractioned using lectin affinity chromatography. The proteins in each fraction were then separated using SDS-PAGE and identified by tryptic in gel digestion followed by tandem mass spectrometry. Utilizing these methods 132 proteins were identified. Among the identified proteins were 17 surface proteins, 9 microneme proteins, 15 rhoptry proteins, 11 heat shock proteins (HSP), and 32 hypothetical proteins. Several proteins had 1 to 5 transmembrane domains (TMD) with some being as large as 608.3 kDa. Both lectin-fluorescence labeling and lectin blotting were employed to confirm the presence of carbohydrates on the surface or cytoplasm of T. gondii parasites. PCR demonstrated that selected hypothetical proteins were expressed in T. gondii tachyzoites. This is data provides a large scale analysis of the T. gondii glycoproteome. Studies of the function of glycosylation of these proteins may help elucidate mechanism(s) involved in invasion improving drug therapy as well as identify glycoproteins that may prove to be useful as vaccine candidates. PMID:21920448

  8. EVALUATION OF GEL PERMEATION CHROMATOGRAPHY FOR CLEAN UP OF HUMAN ADIPOSE TISSUE SAMPLES FOR GC/MS ANALYSIS OF PESTICIDES AND OTHER CHEMICALS

    EPA Science Inventory

    Gel permeation chromatography (GPC) has been evaluated for clean up of human adipose tissue sample extracts in preparation for confirmatory analysis by gas chromatography-mass spectrometry (GC/MS). Studies were conducted with standard solutions, fortified chicken fat, and actual ...

  9. Expanding the operational envelope of compact cylindrical cyclone gas/liquid separators using a variable inlet-slot configuration 

    E-print Network

    Uvwo, Ighofasan

    2006-04-12

    Despite the numerous advantages associated with using compact cylindrical cyclone gas/liquid separators, particularly for upstream production operations, the lack of a full understanding of the complex hydrodynamic process ...

  10. Targeted multidimensional gas chromatography for the quantitative analysis of suspected allergens in fragrance products.

    PubMed

    Dunn, Michael S; Vulic, Natalie; Shellie, Robert A; Whitehead, Simon; Morrison, Paul; Marriott, Philip J

    2006-10-13

    Two approaches are described and compared for the analysis of suspected allergens (SAs) in fragrance products, which are defined by the Scientific Committee of Cosmetics and Non-Food Products (SCCNFP). The first consists of a comprehensive two-dimensional gas chromatography (GC x GC) experiment using both a "conventional" non-polar/polar column combination and an "inverse" polar/non-polar column set. The second approach uses a targeted multidimensional gas chromatography (MDGC) system employing a Deans type pneumatic switch and a longitudinally modulated cryogenic system (LMCS). It was found that the conventional and inverse column sets complement each other well, providing identification of SAs present. Compounds well retained on the second dimension of one column set were the first to be eluted from the other. In some instances SAs co-eluting with matrix components on the second dimension for a given column set were clearly resolved on the other, although this has the disadvantage of requiring two analytical runs. Targeted MDGC with a non-polar/polar column set, successfully separated all SAs identified within a fragrance product. The instrument is set up in a similar fashion to a GC x GC system though with longer second dimension ((2)D) column, a cryogenic trap at the beginning of the second column, and a pneumatic switch coupling both columns. The data are easier to process than for a GC x GC experiment. The targeted MDGC method has the capacity to deliver far greater efficiency to targeted regions of a primary separation than a GC x GC experiment, whilst still maintaining overall run times similar to those of a conventional one-dimensional (1D) GC experiment. Cryogenic focussing at the beginning of the (2)D column delivers enhanced sensitivity, accurate (2)D retention times and narrow peak widths; these are responsible for an increased resolution obtained from the fast, relatively short (approximately 5 m) (2)D column. The two column set GC x GC analysis provided a quick and effective means to qualitatively determine the presence of six SAs in a commercially available air freshener, however all were not adequately resolved from matrix components. In contrast, quantitation was straightforward using the targeted MDGC method. PMID:16934274

  11. Analysis of free and esterified sterols in fats and oils by flash chromatography, gas chromatography and electrospray tandem mass spectrometry.

    PubMed

    Kalo, P; Kuuranne, T

    2001-11-23

    A method for the analysis of free and esterified sterols has been developed. Fat or oil samples were separated on solid-phase extraction silica gel columns into a sterol ester fraction, a fraction of triacylglycerols, and a free sterol fraction containing partial acylglycerols and residual triacylglycerols. Sterol esters and acylglycerols of the free sterol fraction were transesterified to methyl esters. The fatty acid methyl esters from sterol ester fraction and the free sterols from sterol ester fraction and free sterol fraction were determined by GLC. Precursor ion electrospray MS-MS of sterol fragment ions of sterol ester fractions were recorded and used for determination of sterol ester proportions in butterfat and vegetable oil samples. PMID:11762776

  12. Comprehensive thin layer chromatography×gas chromatography using headspace sampling modulation-A case study on fatty acid composition analysis.

    PubMed

    Križman, Mitja; Pušar, Alenka

    2015-07-31

    The recently developed comprehensive TLC×GC technique using headspace sampling is presented. The main advantage of this approach, as demonstrated in lipid analysis, is the possibility to include a transesterification step of glycerides into fatty acid methyl ester derivatives (FAME) because no particular constraints in terms of operational time between TLC and GC are present. Besides being a relatively low-cost solution, TLC×GC by means of headspace sampling provides many benefits in terms of flexibility of separation conditions and modulation sampling width. The technique provides over two orders of magnitude of linear range with TLC sample loads of about 1mg with good reproducibility and accuracy, as demonstrated by multiple headspace extraction (MHE) tests. The technique is a viable alternative to the established but more expensive HPLC×GC technique. The useful range of TLC×GC in terms of analyte volatility can be further extended with a future development of devices based on thermal desorption. PMID:26100575

  13. Pitfalls encountered during quantitative determination of 3-alkyl-2-methoxypyrazines in grape must and wine using gas chromatography-mass spectrometry with stable isotope dilution analysis. Comprehensive two-dimensional gas chromatography-mass spectrometry and on-line liquid chromatography-multidimensional gas chromatography-mass spectrometry as potential loopholes.

    PubMed

    Schmarr, Hans-Georg; Ganss, Sebastian; Koschinski, Stefan; Fischer, Ulrich; Riehle, Carmen; Kinnart, Julian; Potouridis, Theodoros; Kutyrev, Maria

    2010-10-22

    The analysis of 3-alkyl-2-methoxypyrazines in Vitis vinifera grape must or wine at the low nanogram per liter level failed in several situations when applying a one-dimensional gas chromatographic analysis with mass spectrometric detection (GC-MS). Sample preparation methods such as headspace solid phase microextraction or solid phase extraction were convenient procedures, however lacking extraction selectivity for complex matrices. Analysis by comprehensive two-dimensional gas chromatography with mass spectrometric detection clearly demonstrated the potential for co-elution in such matrices and the risk for erroneous results when applying one-dimensional GC-MS. In one example, matrix problems would have been a challenge even for a comprehensive two-dimensional chromatographic approach with MS detection (GC×GC-MS). A solution to matrix problems was found by protonating the 3-alkyl-2-methoxypyrazines in acidic pH and sample clean-up using solid phase extraction with a mixed-mode polymeric cation-exchange sorbent. Quantification was performed by a stable isotope dilution assay, following analysis by on-line coupled high performance liquid chromatography with multidimensional gas chromatography and detection with mass spectrometry (on-line LC-MDGC-MS). This new approach allowed trace-level analysis of 3-alkyl-2-methoxypyrazines in grape musts and wines and is described for V. vinifera Sauvignon blanc, following 3-alkyl-2-methoxypyrazines concentrations during ripening and in the processed wines. PMID:20637469

  14. Qualitative and quantitative analysis of pyrolysis oil by gas chromatography with flame ionization detection and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry.

    PubMed

    Sfetsas, Themistoklis; Michailof, Chrysa; Lappas, Angelos; Li, Qiangyi; Kneale, Brian

    2011-05-27

    Pyrolysis oils have attracted a lot of interest, as they are liquid energy carriers and general sources of chemicals. In this work, gas chromatography with flame ionization detector (GC-FID) and two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) techniques were used to provide both qualitative and quantitative results of the analysis of three different pyrolysis oils. The chromatographic methods and parameters were optimized and solvent choice and separation restrictions are discussed. Pyrolysis oil samples were diluted in suitable organic solvent and were analyzed by GC×GC-TOFMS. An average of 300 compounds were detected and identified in all three samples using the ChromaToF (Leco) software. The deconvoluted spectra were compared with the NIST software library for correct matching. Group type classification was performed by use of the ChromaToF software. The quantification of 11 selected compounds was performed by means of a multiple-point external calibration curve. Afterwards, the pyrolysis oils were extracted with water, and the aqueous phase was analyzed both by GC-FID and, after proper change of solvent, by GC×GC-TOFMS. As previously, the selected compounds were quantified by both techniques, by means of multiple point external calibration curves. The parameters of the calibration curves were calculated by weighted linear regression analysis. The limit of detection, limit of quantitation and linearity range for each standard compound with each method are presented. The potency of GC×GC-TOFMS for an efficient mapping of the pyrolysis oil is undisputable, and the possibility of using it for quantification as well has been demonstrated. On the other hand, the GC-FID analysis provides reliable results that allow for a rapid screening of the pyrolysis oil. To the best of our knowledge, very few papers have been reported with quantification attempts on pyrolysis oil samples using GC×GC-TOFMS most of which make use of the internal standard method. This work provides the ground for further analysis of pyrolysis oils of diverse sources for a rational design of both their production and utilization process. PMID:21036362

  15. Combined size exclusion chromatography, supercritical fluid chromatography and electrospray ionization mass spectrometry for the analysis of complex aliphatic polyesters.

    PubMed

    Pretorius, Nadine O; Willemse, Chandré M; de Villiers, André; Pasch, Harald

    2014-02-21

    Aliphatic polyesters are complex products of polycondensation that are distributed regarding the degree of polycondensation, the end group functionality and the molecular topology. To address the molecular heterogeneity of polyesters based on phthalic acid and propylene glycol, for the first time the combination of SEC, SFC and ESI-MS have been used. In a first set of experiments, samples were fractionated by SEC and the collected fractions analyzed by SFC for a tentative assignment of the degrees of polycondensation. More conclusive results were obtained by semi-preparative SFC fractionation of the bulk samples and the subsequent analysis of the collected fractions by ESI-MS. The ESI-MS spectra of the SFC fractions provided detailed information on the presence of linear and cyclic oligomers, their degrees of polycondensation and their end groups. Information on the presence of propylene oxide oligomers was also obtained and it was shown how they were inserted in the polymer structures. Compared to previous work, the present approach provides significantly more detailed information on the molecular complexity of aliphatic polyesters. This is mainly due to the fact that SFC has been used as the second chromatographic dimension which is known to have superior separation capabilities. PMID:24472839

  16. Transport evaluation of a gas-liquid scrubber. [Five-tray, single-bubble-cap, single-downcomer, gas liquid contactor

    SciTech Connect

    Brodner, A.J.; Bistline, J.E.; Weber, S.E.

    1982-10-01

    The hydraulics and the mass-transfer behavior of a five-tray, single-bubble-cap, single-downcomer, gas-liquid contactor were studied for use as a gas scrubber. Flooding was not observed at the maximum available liquid and gas flow rates of 0.32 and 464 L/min, respectively. The maximum liquid entrainment was 33% at a gross liquid flow rate of 0.05 L/min. The Murphree-tray efficiencies for absorption of CO/sub 2/ (5000 ppM in air) into demineralized water ranged from 0.14 to 0.74 for volumetric liquid-to-gas ratios of 4 x 10/sup -4/ and 2 x 10/sup -4/, respectively, for k/sub L/a values ranging from 0.088 to 0.36 min/sup -1/. 12 figures, 10 tables.

  17. A rapid analysis of plasma/serum ethylene and propylene glycol by headspace gas chromatography.

    PubMed

    Ehlers, Alexandra; Morris, Cory; Krasowski, Matthew D

    2013-12-01

    A rapid headspace-gas chromatography (HS-GC) method was developed for the analysis of ethylene glycol and propylene glycol in plasma and serum specimens using 1,3-propanediol as the internal standard. The method employed a single-step derivitization using phenylboronic acid, was linear to 200 mg/dL and had a lower limit of quantitation of 1 mg/dL suitable for clinical analyses. The analytical method described allows for laboratories with HS-GC instrumentation to analyze ethanol, methanol, isopropanol, ethylene glycol, and propylene glycol on a single instrument with rapid switch-over from alcohols to glycols analysis. In addition to the novel HS-GC method, a retrospective analysis of patient specimens containing ethylene glycol and propylene glycol was also described. A total of 36 patients ingested ethylene glycol, including 3 patients who presented with two separate admissions for ethylene glycol toxicity. Laboratory studies on presentation to hospital for these patients showed both osmolal and anion gap in 13 patients, osmolal but not anion gap in 13 patients, anion but not osmolal gap in 8 patients, and 1 patient with neither an osmolal nor anion gap. Acidosis on arterial blood gas was present in 13 cases. Only one fatality was seen; this was a patient with initial serum ethylene glycol concentration of 1282 mg/dL who died on third day of hospitalization. Propylene glycol was common in patients being managed for toxic ingestions, and was often attributed to iatrogenic administration of propylene glycol-containing medications such as activated charcoal and intravenous lorazepam. In six patients, propylene glycol contributed to an abnormally high osmolal gap. The common presence of propylene glycol in hospitalized patients emphasizes the importance of being able to identify both ethylene glycol and propylene glycol by chromatographic methods. PMID:23741644

  18. A study of the analytical behaviour of selected synthetic and naturally occurring quinolines using electrospray ionisation ion trap mass spectrometry, liquid chromatography and gas chromatography and the construction of an appropriate database for quinoline characterisation

    Microsoft Academic Search

    F. O’Donnell; V. N. Ramachandran; W. F. Smyth; C. J. Hack; E. Patton

    2006-01-01

    Mass spectral fragmentation of quinoline alkaloids of significance in plants has been investigated using electrospray ionisation ion trap mass spectrometry (ESI–MSn) with a view to characterisation of molecules of unknown structure isolated from these natural sources. This investigation has led to the generation of an appropriate database incorporating data from ESI–MSn and also from gas liquid chromatography (GLC) and liquid

  19. Comprehensive analysis of lipids in biological systems by liquid chromatography-mass spectrometry.

    PubMed

    Cajka, Tomas; Fiehn, Oliver

    2014-10-01

    Liquid chromatography-mass spectrometry (LC-MS)-based lipidomics has been a subject of dramatic developments over the past decade. This review focuses on state of the art in LC-MS-based lipidomics, covering all the steps of global lipidomic profiling. On the basis of review of 185 original papers and application notes, we can conclude that typical LC-MS-based lipidomics methods involve: (1) extraction using chloroform/MeOH or MTBE/MeOH protocols, both with addition of internal standards covering each lipid class; (2) separation of lipids using short microbore columns with sub-2-?m or 2.6-2.8-?m (fused-core) particle size with C18 or C8 sorbent with analysis time <30 min; (3) electrospray ionization in positive- and negative-ion modes with full spectra acquisition using high-resolution MS with capability to MS/MS. Phospholipids (phosphatidylcholines, phosphatidylethanolamines, phosphatidylinositols, phosphatidylserines, phosphatidylglycerols) followed by sphingomyelins, di- and tri-acylglycerols, and ceramides were the most frequently targeted lipid species. PMID:25309011

  20. Sources of Variability in Chlorophyll Analysis by Fluorometry and by High Performance Liquid Chromatography. Chapter 22

    NASA Technical Reports Server (NTRS)

    VanHeukelem, Laurie; Thomas, Crystal S.; Glibert, Patricia M.

    2001-01-01

    The need for accurate determination of chlorophyll a (chl a) is of interest for numerous reasons. From the need for ground-truth data for remote sensing to pigment detection for laboratory experimentation, it is essential to know the accuracy of the analyses and the factors potentially contributing to variability and error. Numerous methods and instrument techniques are currently employed in the analyses of chl a. These methods range from spectrophotometric quantification, to fluorometric analysis and determination by high performance liquid chromatography. Even within the application of HPLC techniques, methods vary. Here we provide the results of a comparison among methods and provide some guidance for improving the accuracy of these analyses. These results are based on a round-robin conducted among numerous investigators, including several in the Sensor Intercomparison and Merger for Biological and Interdisciplinary Oceanic Studies (SIMBIOS) and HyCODE Programs. Our purpose here is not to present the full results of the laboratory intercalibration; those results will be presented elsewhere. Rather, here we highlight some of the major factors that may contribute to the variability observed. Specifically, we aim to assess the comparability of chl a analyses performed by fluorometry and HPLC, and we identify several factors in the analyses which may contribute disproportionately to this variability.

  1. Quantitative analysis of mitragynine in human urine by high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Lu, Shijun; Tran, Buu N; Nelsen, Jamie L; Aldous, Kenneth M

    2009-08-15

    Mitragynine is the primary active alkaloid extracted from the leaves of Mitragyna speciosa Korth, a plant that originates in South-East Asia and is commonly known as kratom in Thailand. Kratom has been used for many centuries for their medicinal and psychoactive qualities, which are comparable to that of opiate-based drugs. Kratom abuse can lead to a detectable content of mitragynine residue in urine. Ultra trace amount of mitragynine in human urine was determined by a high performance liquid chromatography coupled to an electrospray tandem mass spectrometry (HPLC-ESI/MS/MS). Mitragynine was extracted by methyl t-butyl ether (MTBE) and separated on a HILIC column. The ESI/MS/MS was accomplished using a triple quadrupole mass spectrometer in positive ion detection and multiple reactions monitoring (MRM) mode. Ajmalicine, a mitragynine's structure analog was selected as internal standard (IS) for method development. Quality control (QC) performed at three levels 0.1, 1 and 5 ng/ml of mitragynine in urine gave mean recoveries of 90, 109, and 98% with average relative standard deviation of 22, 12 and 16%, respectively. The regression linearity of mitragynine calibration ranged from 0.01 to 5.0 ng/ml was achieved with correlation coefficient greater than 0.995. A detection limit of 0.02 ng/ml and high precision data within-day and between days analysis were obtained. PMID:19577523

  2. The analysis of black powder substitutes containing ascorbic acid by ion chromatography/mass spectrometry.

    PubMed

    Lang, Gui-hua Lisa; Boyle, Katherine M

    2009-11-01

    Black powder substitutes containing ascorbic acid are a group of low explosives that utilize ascorbic acid as the fuel. The analysis of these powders is complicated by the degradation of ascorbic acid which occurs rapidly in solution and may also occur as the powder ages. Aqueous extracts of both intact powders and postblast residues were analyzed by an existing ion chromatography/mass spectrometry (IC/MS) method used at the Bureau of Alcohol, Tobacco, Firearms and Explosives. Results have shown that while ascorbic acid itself is not detected in this method, its diagnostic degradation products (threonic acid, monohydrated diketogulonic acid, and oxalic acid) can be identified. In addition, anions from the inorganic oxidizers (perchlorate and nitrate) and combustion products such as chloride, chlorate, and nitrite, can be identified within the same experiment. While this IC/MS method shows promise, future modifications are necessary because of limitations in identifying threonate in postblast residues, as well as coeluting compounds observed in postblast residues. PMID:19732276

  3. Qualitative and quantitative environmental analysis by capillary column gas chromatography/lightpipe Fourier transform infrared spectrometry

    SciTech Connect

    Gurka, D.F.; Pyle, S.M.

    1988-08-01

    A new state-of-art commercial gas chromatography/Fourier transform infrared (GC/FT-IR) lightpipe-containing system has been evaluated for its applicability to qualitative and quantitative environmental analysis of typical environmental contaminants. This system exhibited minimum identifiable quantities, for many compounds, in the 10-50-ng range. On a wide-bore capillary column, quantitation curves generated from chromatogram peak areas were linear over the 10-250-ng range. The mean correlation coefficient for 38 quantitation calibration curves on 24 standards was 0.976. The selectivity of the new system was evaluated with standards, soil, and still-bottom samples. It was demonstrated with 27 standards that no discernible loss in identification selectivity occurred when a narrow-band infrared detector (spectral cutoff 750 cm/sup -1/) was used in place of a midband detector (cutoff 700 cm/sup -1/). This allows the meaningful utilization of the extra sensitivity associated with narrower frequency range infrared detectors.

  4. Optimised determination of clobazam in human plasma with extraction and high-performance liquid chromatography analysis.

    PubMed

    Bolner, A; Tagliaro, F; Lomeo, A

    2001-01-01

    The analysis of clobazam by high-performance liquid chromatography and UV detection is described herein. After adding an internal standard, 600 microl of plasma were extracted under basic conditions onto disposable cartridges packed with celite. The organic extract was then evaporated to dryness and the residue reconstituted in 200 microl of mobile phase. A 20 microl aliquot was injected into chromatograph. The HPLC system was equipped with an Ultrasphere C8 analytical column coupled with an UV detector set at 235 nm. The mobile phase was an acetate buffer 20 mM, pH 5.5, containing acetonitrile and triethylamine 70:30:0.01 (v/v); the flow-rate was 1.8 ml/min. Using this method, clobazam can be detected with a sensitivity limit of 6 ng/ml and the RSD% intra- and inter-assay were lower than 5%. For its ruggedness and reliability, the proposed method is particularly suitable for therapeutic drug monitoring in epilepsy. PMID:11204219

  5. [Serum metabolomics analysis on benign prostate hyperplasia in mice based on liquid chromatography-mass spectrometry].

    PubMed

    Geng, Yue; Sun, Fengxia; Ma, Yu; Deng, Ligang; Lü, Jianyun; Li, Teng; Wang, Congcong

    2014-12-01

    Benign prostatic hyperplasia (BPH) increasingly becomes a common factor affecting the quality of life of aging men. Its pathogenesis has not yet been fully elucidated. Ultra-high pressure liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) was employed to detect the changes of serum metabolites in normal mice, benign prostatic hyperplasia model mice and BPH model mice with finasteride intervention. The serum metabolite profiles of the three groups of mice were analyzed. Partial least squares-discriminant analysis (PLS-DA) was used for group differentiation and biomarker selection. The results showed good distinction among the three groups of mice serum metabolite spectra. Three potential biomarkers, 1-hexadecanoyl-SN-glycero-3-phosphocholine, 1-O-hexadecyl-2-O-acetyl-sn-glyceryl-3-phosphorylcholine and (Z)-13-docosenamide, were discovered and identified. They all indicated the occurrence of benign prostatic hypertrophy is closely related to the disorders of lipid metabolism. Coinpared with the control group, the contents of the first two substances were significantly increased in the serum of BPH model mice, and significantly decreased after intervened by finasteride. The contents of (Z)-13-docosenamide decreased significantly in the serum of model group, and increased after intervened by finasteride. Compared with the control group, the contents of three biomarkers in finasteride group did not recover completely and had significant differences. This study is conductive to open new avenues of diagnosis and medical treatment for BPH. PMID:25902635

  6. Quantitative analysis of eight testosterone metabolites using column switching and liquid chromatography/tandem mass spectrometry.

    PubMed

    Magnusson, Mats O; Sandström, Rikard

    2004-01-01

    The rate at which testosterone is metabolized to different singly hydroxylated metabolites has been widely used as an in vitro marker for activity of different CYP450 enzymes. The interest in extra-hepatic metabolism, e.g. due to metabolism in the gut wall, has increased during the last decade. Measurement of extra-hepatic enzyme activity using testosterone as a substrate requires a highly sensitive analytical method. A new liquid chromatography/electrospray tandem mass spectrometry (LC/MS/MS) method, using column switching for online cleaning and desalting of samples, was developed and validated for analysis of 2alpha-, 2beta-, 6alpha-, 6beta-, 7alpha-, 16alpha-, and 16beta-hydroxytestosterone and androstenedione. The samples were injected on a SB-CN column and detection was performed using MS/MS. The limits of quantification ranged from 0.3 to 3.33 nM for the different metabolites. The validated method was used to quantify the enzyme activity in rat intestine mucosa. The formation rates of 16alpha-, 16beta-hydroxytestosterone and androstenedione were quantified, and 2beta-and 6beta-hydroxytestosterone were formed above the limits of detection. PMID:15150832

  7. Simple and rapid analysis of methyldibromo glutaronitrile in cosmetic products by gas chromatography mass spectrometry.

    PubMed

    Pellegrini, Manuela; Bossù, Elena; Rotolo, Maria Concetta; Pacifici, Roberta; Pichini, Simona

    2011-12-15

    A simple and rapid gas chromatography (GC) method with mass spectrometry (MS) detection has been developed for the determination of methyldibromo glutaronitrile (MDBGN) in cosmetic products. The presence of this preservative in commercial cosmetic samples is prohibited since 2007 because of its allergenic properties. The analyzed products were opportunely diluted in methanol and MDBGN was separated by fused silica capillary column and detected by electron impact (EI)-MS in positive ionization mode with a total run time of 7 min. The assay was validated in the range 0.005-0.100 mg MDBGN per g of examined product with good determination coefficients (r(2)?0.99) for the calibration curves. At three concentrations spanning the linear dynamic range of the calibration curves, mean recoveries were always higher than 95% for MDBGN in the tested cosmetics. This method was successfully applied to the analysis of cleansing gels, shampoo and solar waters to disclose the eventual presence of MDBGN illegally added in cosmetic products. PMID:21871753

  8. Analysis of Fluconazole in Human Urine Sample by High Performance Liquid Chromatography Method

    NASA Astrophysics Data System (ADS)

    Hermawan, D.; Ali, N. A. Md; Ibrahim, W. A. Wan; Sanagi, M. M.

    2013-04-01

    A method for determination of fluconazole, antifungal drug in human urine by using reversed-phased high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detector was developed. Optimization HPLC conditions were carried out by changing the flow rate and composition of mobile phase. The optimum separation conditions at a flow rate 0.85 mL/min with a composition of mobile phase containing methanol:water (70:30, v/v) with UV detection at a wavelength 254 nm was able to analyze fluconazole within 3 min. The excellent linearity was obtained in the range of concentration 1 to 10 ?g/mL with r2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 ?g/mL and 1.28 ?g/mL, respectively. Solid phase extraction (SPE) method using octadecylsilane (C18) as a sorbent was used to clean-up and pre-concentrated of the urine sample prior to HPLC analysis. The average recoveries of fluconazole in spiked urine sample was 72.4% with RSD of 3.21% (n=3).

  9. ANALYSIS OF PERFLUORINATED CARBOXYLIC ACIDS IN SOILS II: OPTIMIZATION OF CHROMATOGRAPHY AND EXTRACTION

    EPA Science Inventory

    With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorinated octanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary p...

  10. Very fast analysis of impurities in immunoglobulin concentrates using conjoint liquid chromatography on short monolithic disks

    Microsoft Academic Search

    K Branovic; G Lattner; M Barut; A Strancar; Dj Josic; A Buchacher

    2002-01-01

    Transferrin and albumin are often present in immunoglobulin G (IgG) concentrates and are considered as impurities. Therefore, it is important to determine their concentration in order to obtain a well-characterized biological product. Here, we describe their determination based on conjoint liquid chromatography (CLC). The established method combines two different chromatographic modes in one step: affinity and ion-exchange chromatography (IEC) combined

  11. Fast separation liquid chromatography–tandem mass spectrometry for the confirmation and quantitative analysis of avermectin residues in food

    Microsoft Academic Search

    M. D. Hernando; J. M. Suárez-Barcena; M. J. M. Bueno; J. F. Garcia-Reyes; A. R. Fernández-Alba

    2007-01-01

    A new residue analytical method for the confirmation and quantification of avermectin residues in food is described in this article. This method allows a fast analysis for the determination of avermectin residues, abamectin (ABM), ivermectin (IVM), emamectin benzoate (EMA) and doramectin (DOR) by liquid chromatography–tandem mass spectrometry (LC–MS\\/MS). Separation was performed using a short column of 1.8?m particle size.The hybrid

  12. Analysis of aggregates of human immunoglobulin G using size-exclusion chromatography, static and dynamic light scattering

    Microsoft Academic Search

    K. Ahrer; A. Buchacher; G. Iberer; D. Josic; A. Jungbauer

    2003-01-01

    Large aggregates (Mr: 106–107 g\\/mol) of human immunoglobulins are present in extremely small concentrations in IgG preparations (<0.1%). Traces of large protein aggregates cannot be determined by conventional size-exclusion chromatography (SEC) using UV detection due to limitations in sensitivity. The conventional analysis of IgG by SEC is limited to dimers and oligomers. Using light scattering it is possible to determine

  13. Thermal Degradation Behavior of Waste Video Cards Using Thermogravimetric Analysis and Pyrolysis Gas Chromatography\\/Mass Spectrometry Techniques

    Microsoft Academic Search

    Huabo Duan; Jinhui Li; Jyh-Feng Hwang; Wang Chen; Elisabeth Gilmore; Peter Adams; Lester Lave; Weifeng Jia; Violeta Mugica; Sara Hernandez; Miguel Torres; Rocio García; Antton Melendez; Estibaliz García; Pedro Carnicer; Egoitz Pena; Miren Larrion; Juan Legarreta; Cristina Gutierrez-Canas; Parikhit Sinha; William Schew; Aniket Sawant; Kyle Kolwaite; Sarah Strode; Stephanie Weber; Jill Engel-Cox; Raymond Hoff; Ana Prados; Hai Zhang; Valerie Garcia; Kristen Foley; Edith Gego; David Holland; S. Rao; Sundar Christopher; Pawan Gupta; Chengwen Wang; Yujue Wang; Yanqi Zhang; Qi Zhao; Ran Wang; Christian Murray; Frederick Lipfert; Jung-Nan Hsu; Hsunling Bai; Shou-Nan Li; Chuen-Jinn Tsai

    2010-01-01

    The thermal degradation characteristics of a printed circuit board assembly (PCBA), specifically video cards from waste computers, was studied using pyrolysis-gas chromatography-mass spectrometry (Py-GC\\/MS) and thermogravimetric analysis (TGA). The video-card waste was dismantled into substrate, integrated circuits (ICs), and plastic slots for comparable investigation. The results by TGA revealed that the initial temperature at which degradation began was 300 °C

  14. Comprehensive multi-residue method for the target analysis of pesticides in crops using liquid chromatography–tandem mass spectrometry

    Microsoft Academic Search

    Maurice Hiemstra; André de Kok

    2007-01-01

    A liquid chromatography–tandem quadrupole mass spectrometry (LC–MS\\/MS) multi-residue method for the simultaneous target analysis of a wide range of pesticides and metabolites in fruit, vegetables and cereals has been developed. Gradient elution has been used in conjunction with positive mode electrospray ionization tandem mass spectrometry to detect up to 171 pesticides and\\/or metabolites in different crop matrices using a single

  15. Characterization of multicapillary gas chromatography–microwave-induced plasma atomic emission spectrometry for the expeditious analysis for organometallic compounds

    Microsoft Academic Search

    Isaac Rodriguez Pereiro; Andrzej Wasik; Ryszard ?obi?ski

    1998-01-01

    Multicapillary column gas chromatography (MC-GC)–microwave-induced plasma atomic emission spectrometry (MIP-AES) is evaluated for fast speciation analysis of organometallic compounds. In situ derivatized organomercury, organotin and organolead compounds are separated isothermally within several seconds instead of several minutes required by the conventional procedures. Neither the resolution nor the sample capacity are sacrificed compared with conventional capillary GC with oven temperature gradient

  16. Applications of liquid chromatography with electrochemical detection to the analysis of oil shale process waters and leachates

    Microsoft Academic Search

    Batley

    1984-01-01

    The application of high performance liquid chromatography with electrochemical detection to the analysis of resin-separated fractions of oil shale retort waters and leachates is described. For compounds such as phenols and amines, having oxidizable functional groups, enhanced selectivity and sensitivity are achievable over conventional u.v. spectrophotometric detection. Phenol, 2-, 3and 4- cresol, dimethylphenols, resorcinol and 2and 5- methylresorcinol, were detected

  17. In-capillary derivatization and laser-induced fluorescence detection for the analysis of organophosphorus pesticides by micellar electrokinetic chromatography

    Microsoft Academic Search

    Lei Zhou; Zhi Luo; Shumin Wang; Yang Hui; Zhide Hu; Xingguo Chen

    2007-01-01

    We developed a rapid and sensitive method using in-capillary derivatization and laser-induced fluorescence (LIF) detection for the fully automated analysis of organophosphorus pesticides (OPPs), including glufosinate, aminomethylphosphonic acid (AMPA) and glyphosate by micellar electrokinetic chromatography (MEKC). The potential of 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) as in-capillary derivatization reagent is described for the first time. The unique feature of this MEKC method is the

  18. A novel analysis method for diterpenoids in rat plasma by liquid chromatography–electrospray ionization mass spectrometry

    Microsoft Academic Search

    Yingfeng Du; Pengwei Liu; Xiaowei Shi; Yiran Jin; Qiao Wang; Xiaowei Zhang; Xiaona Sheng; Lantong Zhang

    2010-01-01

    A sensitive, specific, and rapid liquid chromatography–mass spectrometry (LC–MS) method was developed and validated for analysis of lasiodonin, oridonin, ponicidin, and rabdoternin A in rat plasma using sulfamethoxazole as an internal standard (IS). The plasma samples were pretreated and extracted by liquid–liquid extraction. Chromatographic separation was performed on a C18 column with linear gradient elution using water and methanol, both

  19. The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

    SciTech Connect

    Johnson, S.

    1999-02-12

    The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

  20. Analysis of 23 polycyclic aromatic hydrocarbons in smokeless tobacco by gas chromatography-mass spectrometry

    PubMed Central

    Stepanov, Irina; Villalta, Peter W.; Knezevich, Aleksandar; Jensen, Joni; Hatsukami, Dorothy; Hecht, Stephen S.

    2009-01-01

    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 tobacco after a simple two-step extraction and purification procedure. The method produced coefficients of variation under 10% for most PAH. The limits of quantitation for different PAH varied between 0.3 ng/g tobacco and 11 ng/g tobacco, starting with a 300-mg sample. The recovery of the stable isotope-labeled internal standards averaged 87%. The method was applied to analysis of 23 moist snuff samples that include various flavors of the most popular U.S. moist snuff brands, as well as 17 samples representing the currently marketed brands of spit-free tobacco pouches, a relatively new type of smokeless tobacco. The sum of all detected PAH in conventional moist snuff averaged 11.6 (± 3.7) µg/g dry weight, 20% of this amount being comprised by carcinogenic PAH. The levels of PAH in new spit-free tobacco products were much lower than those in moist snuff, the sum of all detected PAH averaging 1.3 (±0.28) µg/g dry weight. Our findings render PAH one of the most prevalent groups of carcinogens in smokeless tobacco, along with tobacco-specific nitrosamines. Urgent measures are required from the U.S. tobacco industry to modify manufacturing processes so that the levels of these toxicants and carcinogens in the U.S. moist snuff are greatly reduced. PMID:19860436

  1. Analysis of atmospheric aerosols by particle-induced X-ray emission, instrumental neutron activation analysis, and ion chromatography

    NASA Astrophysics Data System (ADS)

    Maenhaut, Willy; Raes, Nico; Wang, Wan

    2011-11-01

    Particle-induced X-ray emission (PIXE), ion chromatography (IC), and occasionally also instrumental neutron activation analysis (INAA) were used in combination for the analysis of atmospheric aerosol samples that were collected on Nuclepore polycarbonate filters. A comparison of the results enabled us to evaluate the matrix effects (i.e., particle size effects) of the PIXE analysis for the light elements and to assess the water-solubility and/or speciation of a number of elements (e.g., S, K, Ca). Results are presented from several measurement campaigns at urban and forested sites in Europe, whereby PM10 or PM2.5 filter samples were taken. From the PIXE and IC results for a 2003 summer campaign at the K-puszta site in Hungary, it was estimated that organosulphates could be responsible for 20% of the total sulphur concentration and 30% of the organic aerosol in PM10. The comparison of the IC and PIXE data for K and Ca from the various sites indicated that most of the Ca was water-soluble (the mineral dust Ca was presumably mostly present as calcite, and perhaps also in part as gypsum); in contrast, for K, only half of it was typically water-soluble, indicating that it was to a large extent associated with insoluble mineral dust. Exceptions, with almost fully water-soluble K, were found for samples that were substantially impacted by biomass burning.

  2. Contribution to complex gas-liquid flows: Development and validation of a mathematical model

    NASA Astrophysics Data System (ADS)

    Selma, Brahim

    This study describes the development and validation of Computational Fluid Dynamics (CFD) model for the simulation of dispersed two-phase flows taking in the account the population balance of particles size distribution. A two-fluid (Euler-Euler) methodology previously developed for complex flows is adapted to the present project. The continuous phase turbulence is represented using a two-equation k --- epsilon turbulence model which contains additional terms to account for the effects of the dispersed on the continuous phase turbulence and the effects of the gas-liquid interface. The inter-phase momentum transfer is determined from the instantaneous forces acting on the dispersed phase, comprising drag, lift, virtual mass and drift velocity. These forces are phase fraction dependent and in this work revised modelling is put forward in order to capture a good accuracy for gas hold-up, liquid velocity profiles and turbulence parameters. Furthermore, a correlation for the effect of the drift velocity on the turbulence behaviour is proposed. The revised modelling is based on an extensive survey of the existing literature. The conservation equations are discretised using the finite-volume method and solved in a solution procedure, which is loosely based on the PISO algorithm. Special techniques are employed to ensure the stability of the procedure when the phase fraction is high or changing rapidely [61]. Finally, assessment of the model is made with reference to experimental data for gas-liquid bubbly flow in a rectangular bubble column [133; 134; 135; 18], in a double-turbine stirred tank reactor [126; 127] and in an air-lift bioreacator [101]. Key words: mathematical modelling, complex flow gas-liquid, turbulence, population balance, computational fluids dynamics CFD, OpenFOAM, moments method, method of classes, QMOM, DQMOM.

  3. Volatile compounds of rehydrated French beans, bell peppers and leeks. Part II. Gas chromatography\\/sniffing port analysis and sensory evaluation

    Microsoft Academic Search

    Saskia M. Van Ruth; Jacques P. Roozen; Jan L. Cozijnsen; Maarten A. Posthumus

    1995-01-01

    The flavours of rehydrated diced French beans, red bell peppers and leeks were characterised by gas chromatography\\/sniffing port analysis (GC\\/SP) of volatile compounds released in a mouth model system, and by descriptive sensory analysis. Volatile compounds were identified by combined gas chromatography\\/mass spectrometry. In French beans, bell peppers and leeks, respectively, 10, 16 and 22 compounds possessed detectable odours. A

  4. Analysis of biomass sugars and galacturonic acid by gradient anion exchange chromatography and pulsed amperometric detection without post-column addition

    Microsoft Academic Search

    Wilbur Widmer

    2011-01-01

    While the most accurate method for analysis of sugars in biomass is based on gas chromatography of trimethylsilane or alditol\\u000a acetate derivatives of sugars, the derivation method is time consuming and laborious. In comparison, sample preparation for\\u000a sugar analysis of hydrolyzed biomass samples using liquid chromatography is a simple dilution procedure with water. A gradient\\u000a HPLC method using a anion-exchange

  5. Direct numerical simulation of turbulent flows over superhydrophobic surfaces: gas-liquid interface dynamics

    NASA Astrophysics Data System (ADS)

    Seo, Jongmin; García-Mayoral, Ricardo; Mani, Ali

    2013-11-01

    Superhydrophobic surfaces can induce large slip velocities for liquid flows, reducing the skin friction on walls, by entrapping gas pockets within the surface roughness. This work explores the onset mechanism leading to gas depletion through interface breakage under turbulent conditions. We conduct direct numerical simulations of flows over superhydrophobic walls. The superhydrophobic texture is conventionally modeled as a pattern of slip/no-slip boundary conditions for the wall-parallel velocities but, to take into account the dynamic deformation of the gas-liquid interface, we also introduce non-zero boundary conditions for the wall-normal velocity. These conditions are derived from the deformation of the interface in response to the overlying turbulent pressure fluctuations, following the Young-Laplace equation. Surface protrusions in the form of posts and streamwise-aligned ridges are studied, and results are presented as a function of the ``deformability'' of the gas-liquid interfaces, expressed as a Weber number. We will also discuss results for misaligned ridges. Superhydrophobic surfaces can induce large slip velocities for liquid flows, reducing the skin friction on walls, by entrapping gas pockets within the surface roughness. This work explores the onset mechanism leading to gas depletion through interface breakage under turbulent conditions. We conduct direct numerical simulations of flows over superhydrophobic walls. The superhydrophobic texture is conventionally modeled as a pattern of slip/no-slip boundary conditions for the wall-parallel velocities but, to take into account the dynamic deformation of the gas-liquid interface, we also introduce non-zero boundary conditions for the wall-normal velocity. These conditions are derived from the deformation of the interface in response to the overlying turbulent pressure fluctuations, following the Young-Laplace equation. Surface protrusions in the form of posts and streamwise-aligned ridges are studied, and results are presented as a function of the ``deformability'' of the gas-liquid interfaces, expressed as a Weber number. We will also discuss results for misaligned ridges. Supported by the Office of Naval Research and the Kwanjeong Educational Scholarship Foundation.

  6. Generalization of low pressure, gas-liquid, metastable sound speed to high pressures

    NASA Technical Reports Server (NTRS)

    Bursik, J. W.; Hall, R. M.

    1981-01-01

    A theory is developed for isentropic metastable sound propagation in high pressure gas-liquid mixtures. Without simplification, it also correctly predicts the minimum speed for low pressure air-water measurements where other authors are forced to postulate isothermal propagation. This is accomplished by a mixture heat capacity ratio which automatically adjusts from its single phase values to approximately the isothermal value of unity needed for the minimum speed. Computations are made for the pure components parahydrogen and nitrogen, with emphasis on the latter. With simplifying assumptions, the theory reduces to a well known approximate formula limited to low pressure.

  7. Probing the microscopic corrugation of liquid surfaces with gas-liquid collisions

    NASA Technical Reports Server (NTRS)

    King, Mackenzie E.; Nathanson, Gilbert M.; Hanning-Lee, Mark A.; Minton, Timothy K.

    1993-01-01

    We have measured the directions and velocities of Ne, Ar, and Xe atoms scattering from perfluorinated ether and hydrocarbon liquids to probe the relationship between the microscopic roughness of liquid surfaces and gas-liquid collision dynamics. Impulsive energy transfer is governed by the angle of deflection: head-on encounters deposit more energy than grazing collisions. Many atoms scatter in the forward direction, particularly at glancing incidence. These results imply that the incoming atoms recoil locally from protruding C-H and C-F groups in hard spherelike collisions.

  8. Numerical modeling of gas-liquid flows in mini- and microchannels

    NASA Astrophysics Data System (ADS)

    Guzei, D. V.; Minakov, A. V.; Pryazhnikov, M. I.; Dekterev, A. A.

    2015-01-01

    The paper presents the results of testing a methodology for calculating two-phase flows in mini- and microchannels. The numerical methodology is based on the known fluid-in-cell method (VOF method) and the CSF procedure to account for surface tension forces. Solutions of several test problems of two-phase flow in microchannels, including the water-oil emulsion flow and gas-liquid flow in microchannels of the T-type and the stationary slug flow in a circular minichannel, were considered with the aid of this technique. Comparisons of numerical results with experimental data were carried out. A good agreement between the results was obtained.

  9. Gas liquid flow at microgravity conditions - Flow patterns and their transitions

    NASA Technical Reports Server (NTRS)

    Dukler, A. E.; Fabre, J. A.; Mcquillen, J. B.; Vernon, R.

    1987-01-01

    The prediction of flow patterns during gas-liquid flow in conduits is central to the modern approach for modeling two phase flow and heat transfer. The mechanisms of transition are reasonably well understood for flow in pipes on earth where it has been shown that body forces largely control the behavior observed. This work explores the patterns which exist under conditions of microgravity when these body forces are suppressed. Data are presented which were obtained for air-water flow in tubes during drop tower experiments and Learjet trajectories. Preliminary models to explain the observed flow pattern map are evolved.

  10. Time-dependent gas-liquid interaction in molecular-sized nanopores.

    PubMed

    Sun, Yueting; Li, Penghui; Qiao, Yu; Li, Yibing

    2014-01-01

    Different from a bulk phase, a gas nanophase can have a significant effect on liquid motion. Herein we report a series of experimental results on molecular behaviors of water in a zeolite ? of molecular-sized nanopores. If sufficient time is provided, the confined water molecules can be "locked" inside a nanopore; otherwise, gas nanophase provides a driving force for water "outflow". This is due to the difficult molecular site exchanges and the relatively slow gas-liquid diffusion in the nanoenvironment. Depending on the loading rate, the zeolite ?/water system may exhibit either liquid-spring or energy-absorber characteristics. PMID:25293525

  11. Time-dependent Gas-liquid Interaction in Molecular-sized Nanopores

    PubMed Central

    Sun, Yueting; Li, Penghui; Qiao, Yu; Li, Yibing

    2014-01-01

    Different from a bulk phase, a gas nanophase can have a significant effect on liquid motion. Herein we report a series of experimental results on molecular behaviors of water in a zeolite ? of molecular-sized nanopores. If sufficient time is provided, the confined water molecules can be “locked” inside a nanopore; otherwise, gas nanophase provides a driving force for water “outflow”. This is due to the difficult molecular site exchanges and the relatively slow gas-liquid diffusion in the nanoenvironment. Depending on the loading rate, the zeolite ?/water system may exhibit either liquid-spring or energy-absorber characteristics. PMID:25293525

  12. Hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry for acidic herbicides and metabolites analysis in fresh water.

    PubMed

    Fauvelle, Vincent; Mazzella, Nicolas; Morin, Soizic; Moreira, Sylvia; Delest, Brigitte; Budzinski, Hélène

    2015-03-01

    Theoretical papers and environmental applications of hydrophilic interaction liquid chromatography (HILIC) have been published for a wide range of analytes, but to our knowledge, no study focused on acidic herbicides (e.g., triketones, phenoxy acids, sulfonylurea, and acidic metabolites of chloroacetanilides). Matrix effects are the main obstacle to natural sample analysis by liquid chromatography coupled with tandem mass spectrometry (MS) via an electrospray ionization (ESI) interface. Therefore, we paid particular attention on limiting interference by (i) adapting the emerging HILIC technique, which is generally considered more sensitive than conventional reversed phase liquid chromatography and (ii) optimizing the solid phase extraction (SPE) step using a design of experiment. A rapid and reliable off line SPE-HILIC-ESI-MS/MS method was thus developed for the quantification of acidic herbicides in fresh water, with limits of quantifications (LOQs) ranging from 5 to 22 ng L(-1). Then, the analysis of freshwater samples highlighted the robustness of the method, and the importance of the chloroacetanilides metabolites among the studied analytes. PMID:24859693

  13. Analysis of modified polyamide 6.6 using coupled liquid chromatography and MALDI-TOF-mass spectrometry

    NASA Astrophysics Data System (ADS)

    Weidner, Steffen M.; Just, Ulrich; Wittke, Wolfgang; Rittig, Frank; Gruber, Freddy; Friedrich, Joerg F.

    2004-11-01

    A new approach of analysis of polyamide 6.6 using the principle of coupling polymer liquid chromatography to matrix assisted laser desorption ionization-time of flight-mass spectrometry (MALDI-TOF-MS) is presented. In contrast to the known technique of two-dimensional chromatography, MALDI-TOF-MS was applied in the 2nd chromatographic dimension. According to the synthesis of polyamide 6.6 various species with different end groups are expected. Due to the capping of the end groups during the synthesis, either performed by the addition of mono-functional amines or acids, additional structures are formed and found. Although the resolution of chromatography applied for separation was poor in comparison to the broad variety of expected species, a complete identification of those components was achieved applying the MALDI-TOF-MS technique. The results were presented in a two-dimensional plot, which can be used as a fingerprint method for the analysis of polyamide 6.6.

  14. Analysis of acetylene in blood and urine using cryogenic gas chromatography-mass spectrometry.

    PubMed

    Kashiwagi, Masayuki; Hara, Kenji; Fujii, Hiroshi; Kageura, Mitsuyoshi; Takamoto, Mutsuo; Matsusue, Aya; Sugimura, Tomoko; Kubo, Shin-ichi

    2009-09-01

    A method for quantitative analysis of acetylene in blood and urine samples was investigated. Using cryogenic gas chromatography-mass spectrometry (GC-MS), acetylene was measured with isobutane as the internal standard in the headspace method, which revealed a linear response over the entire composite range with an excellent correlation coefficient, both in blood (R = 0.9968, range = 5.39-43.1 microg/ml) and urine (R = 0.9972, range = 2.16-10.8 microg/ml). The coefficients of variation (CV) for blood ranged from 2.62 to 11.6% for intra-day and 4.55 to 10.4% for inter-day. The CV for urine ranged from 2.38 to 3.10% for intra-day and 4.83 to 11.0% for inter-day. The recovery rate as an index of accuracy ranged from 83 to 111%. The present method showed good reliability, and is also simple and rapid. In actual samples from a charred cadaver due to acetylene explosion, the measured concentrations of acetylene by this method were 21.5 microg/ml for femoral vein blood, 17.9 microg/ml for right atrial blood, 25.5 microg/ml for left atrial blood and 7.49 microg/ml for urine. Quantification of acetylene provides important information, because the acetylene concentration is a vital reaction or sign. For example, when acetylene is filled in a closed space and then explodes, in antemortem explosion, the blood acetylene concentration of the cadaver might be significant. On the other hand, in postmortem explosion, acetylene is not detected in blood. Furthermore, when several victims are involved in one explosion, comparison of the sample concentrations can also provide useful information to establish the conditions at the accident scene; therefore, the present method is useful in forensics. PMID:19423404

  15. Linker-assisted immunoassay and liquid chromatography/mass spectrometry for the analysis of glyphosate

    USGS Publications Warehouse

    Lee, E.A.; Zimmerman, L.R.; Bhullar, B.S.; Thurman, E.M.

    2002-01-01

    A novel, sensitive, linker-assisted enzyme-linked immunosorbent assay (L'ELISA) was compared to on-line solidphase extraction (SPE) with high-performance liquid chromatography/mass spectrometry (HPLC/MS) for the analysis of glyphosate in surface water and groundwater samples. The L'ELISA used succinic anhydride to derivatize glyphosate, which mimics the epitotic attachment of glyphosate to horseradish peroxidase hapten. Thus, L'ELISA recognized the derivatized glyphosate more effectively (detection limit of 0.1 ??g/L) and with increased sensitivity (10-100 times) over conventional ELISA and showed the potential for other applications. The precision and accuracy of L'ELISA then was compared with on-line SPE/HPLC/MS, which detected glyphosate and its degradate derivatized with 9-fluorenylmethyl chloroformate using negative-ion electrospray (detection limit 0.1 ??g/L, relative standard deviation ??15%). Derivatization efficiency and matrix effects were minimized by adding an isotope-labeled glyphosate (2-13C15N). The accuracy of L'ELISA gave a false positive rate of 18% between 0.1 and 1.0 ??g/L and a false positive rate of only 1% above 1.0 ??g/L. The relative standard deviation was ??20%. The correlation of L'ELISA and HPLC/MS for 66 surface water and groundwater samples was 0.97 with a slope of 1.28, with many detections of glyphosate and its degradate in surface water but not in groundwater.

  16. Analyses of pecan, peanut, and other oils by gas-liquid chromatography and ultra-violet spectrophotometry

    Microsoft Academic Search

    R. B. French

    1962-01-01

    Comparative analyses of oils obtained from 12 varieties of pecans, 11 of peanuts, two of avocados and one each of citrus seed,\\u000a Wesson oil, corn, and of lard by GLC and UV procedures showed good agreement except for Wesson oil, corn oil, and lard. Iodine\\u000a values computed from GLC results checked Wijs values closely. Oleic acid ranged from 51 to

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

    PubMed

    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. PMID:15472953

  18. Radiochemical analysis of uranium isotopes in soil and sediment samples with extraction chromatography.

    PubMed

    Lee, M H; Lee, C W

    2001-03-30

    An accurate and simple analytical technique for uranium isotopes in highly contaminated soil samples was developed and validated by application to IAEA-Reference samples and environmental samples. For overcoming the demerits of the TBP extraction method, sample materials were decomposited with HNO(3) and HF and uranium isotopes were purified with an anion exchange resin and a TRU Spec resin. With the extraction chromatography method, hindrance elements were completely removed from the uranium fraction. The chemical yields with the extraction chromatography method were <10% higher than those with the TBP extraction method. The concentrations of uranium isotopes using the extraction chromatography method were consistent with the reference values reported by the IAEA. PMID:18968240

  19. Analysis of aliphatic biopolymers using thermochemolysis with tetramethylammonium hydroxide (TMAH) and gas chromatography- mass spectrometry

    Microsoft Academic Search

    PATRICK G. HATCHER

    1998-01-01

    Abstract—Selected aliphatic biopolyesters (cutins, cuticles and a suberin) isolated from diÄerent plants have,been,analyzed,using thermochemolysis,with,tetramethylammonium,hydroxide,(TMAH). This method consists of a high-temperature saponification\\/transesterification, and yields methyl esters of fatty acids and the methyl ethers of alcohols, which are subsequently analyzed by gas chromatography and,gas chromatography?mass spectrometry. The main,compounds,produced,from,the analyzed samples correspond to the methyl derivatives of long-chain fatty acids, hydroxy fatty acids

  20. Space Storable Propellant Performance Gas/Liquid Like-Doublet Injector Characterization

    NASA Technical Reports Server (NTRS)

    Falk, A. Y.

    1972-01-01

    A 30-month applied research program was conducted, encompassing an analytical, design, and experimental effort to relate injector design parameters to simultaneous attainment of high performance and component (injector/thrust chamber) compatibility for gas/liquid space-storable propellants. The gas/liquid propellant combination selected for study was FLOX (82.6% F2)/ambient temperature gaseous methane. The injector pattern characterized was the like-(self)-impinging doublet. Program effort was apportioned into four basic technical tasks: injector and thrust chamber design, injector and thrust chamber fabrication, performance evaluation testing, and data evaluation and reporting. Analytical parametric combustion analyses and cold flow distribution and atomization experiments were conducted with injector segment models to support design of injector/thrust chamber combinations for hot fire evaluation. Hot fire tests were conducted to: (1) optimize performance of the injector core elements, and (2) provide design criteria for the outer zone elements so that injector/thrust chamber compatibility could be achieved with only minimal performance losses.

  1. Enzyme transmission during crossflow filtration of yeast suspensions using gas/liquid two-phase flows.

    PubMed

    Mercier-Bonin, Muriel; Fonade, Christian

    2003-03-01

    The optimal conditions for recovery of an enzyme were determined using gas/liquid two-phase flows. When filtering the enzyme-only solution under single-phase flow conditions, severe fouling occurred. This fouling was manifest as a decline in flux to less than 2% of the initial water flux and a decline in protein concentration in the permeate to 30% of its initial value, during a five-hour filtration period. When yeast cells were added under the same experimental conditions, enzyme transmission was maintained at 100% for the five-hour period and the enzyme mass flux was twofold higher. During gas-sparged microfiltration of the enzyme/yeast mixture in a permeate-recycling mode at the same liquid flow rate, gas/liquid slug flow strongly decreased the transmission of the enzyme (70% decrease), even though the permeate flux was improved (140% improvement). As a result, the mass flux of the enzyme was significantly reduced. However, with a bubble flow pattern, the permeate flux was 1.5 times higher and the transmission was maintained at a high level. The enzyme mass flux was then 25% higher when compared to single-phase flow filtration conditions. During diafiltration experiments with a bubble flow pattern, a 13% higher enzyme recovery was achieved. PMID:12783839

  2. High-Throughput and Comprehensive Lipidomic Analysis Using Ultrahigh-Performance Supercritical Fluid Chromatography-Mass Spectrometry.

    PubMed

    Lísa, Miroslav; Hol?apek, Michal

    2015-07-21

    New analytical approach for high-throughput and comprehensive lipidomic analysis of biological samples using ultrahigh-performance supercritical fluid chromatography (UHPSFC) with electrospray ionization-mass spectrometry (ESI-MS) is presented in this work as an alternative approach to established shotgun MS or high-performance liquid chromatography-MS. The lipid class separation is performed by UHPSFC method based on 1.7 ?m particle-bridged ethylene hybrid silica column with a gradient of methanol-water-ammonium acetate mixture as a modifier. All parameters of UHPSFC conditions are carefully optimized and their influence on the chromatographic behavior of lipids is discussed. The final UHPSFC/ESI-MS method enables a fast separation of 30 nonpolar and polar lipid classes within 6 min analysis covering 6 main lipid categories including fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, and prenols. Individual lipid species within lipid classes are identified based on positive and negative-ion full-scan and tandem mass spectra measured with high mass accuracy and high resolving power. Developed UHPSFC/ESI-MS method is applied for the analysis of porcine brain extract as a complex lipidomic sample, where 24 lipid classes containing 436 lipid species are identified. The method is validated for the quantitative analysis of lipid species in biological tissues using internal standards for each lipid class. This high-throughput, comprehensive and accurate UHPSFC/ESI-MS method is suitable for the lipidomic analysis of large sample sets in the clinical research. PMID:26095628

  3. Analysis of Currently Available Analgesic Tablets by Modern Liquid Chromatography: An Undergraduate Laboratory Introduction to HPLC.

    ERIC Educational Resources Information Center

    Kagel, R. A.; Farwell, S. O.

    1983-01-01

    Background information, procedures, and results, are provided for an undergraduate experiment in which analgesic tablets are analyzed using liquid chromatography. The experiment, an improved, modified version of the Waters Associates Inc. experiment, is simple to prepare, requiring little glassware and minimal sample manipulation by students. (JN)

  4. Analysis of fatty acids by gas chromatography, and its relevance to research on health and nutrition

    Microsoft Academic Search

    T Seppänen-Laakso; I Laakso; R Hiltunen

    2002-01-01

    Gas chromatography (GC) has been an indispensable analytical technique ever since the first exciting steps in the application of fatty acid determinations in oilseed plant breeding, biosynthesis and human metabolism. Present-day GC methods with high-quality capillary columns allow sensitive and reproducible fatty acid analyses, as well as the characterization of complex mixtures of geometric isomers when combined with other chromatographic

  5. High-resolution gas chromatography/mass spectrometric analysis of tobacco and marijuana sterols.

    PubMed

    Novotny, M; Lee, M L; Low, C E; Maskarinec, M P

    1976-05-01

    Components of the sterol fraction of tobacco and marijauna were resolved as trimethylsilyl derivatives by gas chromatography with glass capillary columns. Ten phytosterols in tobacco and five in marijuana were identified by comparisons of their retention with authentic compounds on three different stationary phases and through mass-spectral data. PMID:941185

  6. APPLICATION OF GC/ITD (GAS CHROMATOGRAPHY/ION TRAP DETECTOR) TO ENVIRONMENTAL ANALYSIS (JOURNAL VERSION)

    EPA Science Inventory

    The choice of gas chromatography (GC) detectors has expanded rapidly. The necessity for mass spectrometric (MS) characterization of GC effluents stems from the complexity of the matrices associated with environmental samples. There are currently several MS types being used in con...

  7. Analysis of Peppermint Leaf and Spearmint Leaf Extracts by Thin-Layer Chromatography

    ERIC Educational Resources Information Center

    Pelter, Libbie S. W.; Amico, Andrea; Gordon, Natalie; Martin, Chylah; Sandifer, Dessalyn; Pelter, Michael W.

    2008-01-01

    In this inquiry-based activity, the usefulness of thin-layer chromatography (TLC) to visualize the difference between spearmint and peppermint is explored. The experiment may be used in any class where TLC is discussed from high school to college. We have used this activity with science majors in an organic chemistry laboratory, with non-science…

  8. Analysis of Quaternary Amine Compounds by Hydrophilic Interaction Chromatography\\/Mass Spectrometry (HILIC\\/MS)

    Microsoft Academic Search

    Yong Guo

    2005-01-01

    Hydrophilic interaction chromatography (HILIC) was explored for the separation of selected quaternary amine compounds of biological and environmental importance, including acetylcholine, choline, betaine, chlormequat, and mepiquat. The HILIC method was successful in separating the model quaternary amine compounds without the need for ion?pairing reagents. The present study indicates that the amide phase provides much stronger retention for the quaternary amine

  9. (PRESENT AT NCCU) ANALYSIS OF SELECTED PYRETHROID PESTICIDES USING REVERSE PHASE HIGH LIQUID CHROMATOGRAPHY

    EPA Science Inventory

    This research was conducted in cooperation with EPA Region 4 in Athens, GA to develop a method to analyze selected pyrethroid pesticides using Reverse Phase-High Pressure Liquid Chromatography (HPLC). This HPLC method will aid researchers in separating and identifying these pyre...

  10. ANALYSIS OF SELECTED PYRETHROID PESTICIDES USING REVERSE PHASE HIGH PRESSURE LIQUID CHROMATOGRAPHY/UV

    EPA Science Inventory

    This research was conducted in cooperation with EPA Region 4 in Athens, GA to develop a method to analyze selected pyrethroid pesticides using Reverse Phase-High Pressure Liquid Chromatography (HPLC). This HPLC method will aid researchers in separating and identifying these py...

  11. Reconsidering the quantitative analysis of organic carbon concentrations in size exclusion chromatography

    Microsoft Academic Search

    Ulrich Lankes; Margit B. Müller; Matthias Weber; Fritz H. Frimmel

    2009-01-01

    The evaluation of the molecular size distribution of natural organic matter (NOM) in aquatic environments via size exclusion chromatography (SEC) is important for the understanding of environmental processes such as nutrient cycling and pollutant transport as well as of technical water treatment processes. The use of organic carbon (OC) detectors has become popular in recent studies due to improved availability

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

    Microsoft Academic Search

    Markus Ganzera; Christoph Egger; Christian Zidorn; Hermann Stuppner

    2008-01-01

    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

  13. A liquid chromatography–mass spectrometry method for the quantitative analysis of urinary endogenous estrogen metabolites

    Microsoft Academic Search

    Xia Xu; Larry K Keefer; Regina G Ziegler; Timothy D Veenstra

    2007-01-01

    The ability to measure estrogen metabolites (EMs) quantitatively is important for investigating their individual roles in cancer screening, treatment and prevention, as well as in a host of other hormone-related disorders. In this protocol we describe a method that is capable of quantitating 15 distinct EMs in urine. Endogenous EMs are quantitatively measured using a liquid chromatography–tandem mass spectrometry method

  14. SURVEY ANALYSIS OF PHENOLIC COMPOUNDS IN INDUSTRIAL EFFLUENTS BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    Analyzing industrial effluents for phenolic compounds involves a number of problems both in the separation of these compounds from the aqueous medium and in the chromatography of the extracted compounds. Use of continuous liquid-liquid extractor improved the recovery of phenolic ...

  15. Simple and rapid analysis of methyldibromo glutaronitrile in cosmetic products by gas chromatography mass spectrometry

    Microsoft Academic Search

    Manuela Pellegrini; Elena Bossù; Maria Concetta Rotolo; Roberta Pacifici; Simona Pichini

    2011-01-01

    A simple and rapid gas chromatography (GC) method with mass spectrometry (MS) detection has been developed for the determination of methyldibromo glutaronitrile (MDBGN) in cosmetic products. The presence of this preservative in commercial cosmetic samples is prohibited since 2007 because of its allergenic properties. The analyzed products were opportunely diluted in methanol and MDBGN was separated by fused silica capillary

  16. Analysis of triacylglycerols on porous graphitic carbon by high temperature liquid chromatography

    Microsoft Academic Search

    Bérangère Merelli; Marine De Person; Patrick Favetta; Michel Lafosse

    2007-01-01

    The retention behaviour of several triacylglycerols (TAGs) and fats on Hypercarb®, a porous graphitic carbon column (PGC), was investigated in liquid chromatography (LC) under isocratic elution mode with an evaporative light scattering detector (ELSD). Mixtures of chloroform\\/isopropanol were selected as mobile phase for a suitable retention time to study the influence of temperature. The retention was different between PGC and

  17. Current trends in green liquid chromatography for the analysis of pharmaceutically active compounds in the environmental water compartments.

    PubMed

    Shaaban, Heba; Górecki, Tadeusz

    2015-01-01

    Green analytical chemistry is an aspect of green chemistry which introduced in the late nineties. The main objectives of green analytical chemistry are to obtain new analytical technologies or to modify an old method to incorporate procedures that use less hazardous chemicals. There are several approaches to achieve this goal such as using environmentally benign solvents and reagents, reducing the chromatographic separation times and miniaturization of analytical devices. Traditional methods used for the analysis of pharmaceutically active compounds require large volumes of organic solvents and generate large amounts of waste. Most of them are volatile and harmful to the environment. With the awareness about the environment, the development of green technologies has been receiving increasing attention aiming at eliminating or reducing the amount of organic solvents consumed everyday worldwide without loss in chromatographic performance. This review provides the state of the art of green analytical methodologies for environmental analysis of pharmaceutically active compounds in the aquatic environment with special emphasis on strategies for greening liquid chromatography (LC). The current trends of fast LC applied to environmental analysis, including elevated mobile phase temperature, as well as different column technologies such as monolithic columns, fully porous sub-2 ?m and superficially porous particles are presented. In addition, green aspects of gas chromatography (GC) and supercritical fluid chromatography (SFC) will be discussed. We pay special attention to new green approaches such as automation, miniaturization, direct analysis and the possibility of locating the chromatograph on-line or at-line as a step forward in reducing the environmental impact of chromatographic analyses. PMID:25476373

  18. Aggregation analysis of pharmaceutical human immunoglobulin preparations using size-exclusion chromatography and analytical ultracentrifugation sedimentation velocity.

    PubMed

    Krayukhina, Elena; Uchiyama, Susumu; Nojima, Kiyoko; Okada, Yoshiaki; Hamaguchi, Isao; Fukui, Kiichi

    2013-01-01

    In the pharmaceutical industry, analysis of soluble aggregates in pharmaceutical formulations is most commonly performed using size-exclusion chromatography (SEC). However, owing to concerns that aggregates can be overlooked by SEC analysis, it has been suggested that its results should be confirmed with orthogonal methods. One of the main alternative methods for SEC is analytical ultracentrifugation sedimentation velocity (AUC-SV), which has been indicated as an important tool for the measurement of protein aggregation. The present study aimed to show that AUC-SV can be effectively applied for the characterization of marketed immunoglobulin pharmaceutical preparations to support the results obtained by SEC. In addition, the present research aimed to assess the appropriateness of two integration approaches for the quantitative analysis of the SEC results. Thus, the aggregates were measured in seven different preparations of human immunoglobulins by AUC-SV and SEC, and the acquired chromatographic data were processed by using either the vertical drop method or the Gaussian skim approach, implemented in the Empower II chromatography data software (Waters, Tokyo, Japan). The results of aggregation measurements performed using AUC-SV were in good agreement with those obtained using SEC. As expected, the Gaussian skim integration approach inherently provided lower estimates of aggregation content than the results of the vertical drop method. The finding of this study confirmed the complementary nature of AUC-SV to SEC for aggregate composition analysis and underscored the important role that the different integration methods can play in the quantitative interpretation of chromatographic results. PMID:22925901

  19. Analysis of xanthohumol and isoxanthohumol in different hop products by liquid chromatography-diode array detection-electrospray ionization tandem mass spectrometry

    Microsoft Academic Search

    Paulo J. Magalhães; Luís F. Guido; José M. Cruz; Aquiles A. Barros

    2007-01-01

    An analytical methodology based on the sample extraction with methanol\\/formic acid by ultra-sonication and subsequent analysis by high-performance liquid chromatography with diode array detection is proposed for the determination of xanthohumol (XN) and isoxanthohumol (IXN) in different hop products. The identity of the compounds was confirmed by high-performance liquid chromatography\\/electrospray ionization tandem mass spectrometry in positive ion mode. The performance

  20. Gas-liquid coexistence for the boson square-well fluid and the He4 binodal anomaly

    NASA Astrophysics Data System (ADS)

    Fantoni, Riccardo

    2014-08-01

    The binodal of a boson square-well fluid is determined as a function of the particle mass through a quantum Gibbs ensemble Monte Carlo algorithm devised by R. Fantoni and S. Moroni [J. Chem. Phys. (to be published)]. In the infinite mass limit we recover the classical result. As the particle mass decreases, the gas-liquid critical point moves at lower temperatures. We explicitly study the case of a quantum delocalization de Boer parameter close to the one of He4. For comparison, we also determine the gas-liquid coexistence curve of He4 for which we are able to observe the binodal anomaly below the ?-transition temperature.

  1. Gas-liquid coexistence for the boson square-well fluid and the (4)He binodal anomaly.

    PubMed

    Fantoni, Riccardo

    2014-08-01

    The binodal of a boson square-well fluid is determined as a function of the particle mass through a quantum Gibbs ensemble Monte Carlo algorithm devised by R. Fantoni and S. Moroni [J. Chem. Phys. (to be published)]. In the infinite mass limit we recover the classical result. As the particle mass decreases, the gas-liquid critical point moves at lower temperatures. We explicitly study the case of a quantum delocalization de Boer parameter close to the one of (4)He. For comparison, we also determine the gas-liquid coexistence curve of (4)He for which we are able to observe the binodal anomaly below the ?-transition temperature. PMID:25215668

  2. Multiclass mycotoxin analysis in food, environmental and biological matrices with chromatography/mass spectrometry.

    PubMed

    Capriotti, Anna Laura; Caruso, Giuseppe; Cavaliere, Chiara; Foglia, Patrizia; Samperi, Roberto; Laganà, Aldo

    2012-01-01

    Mold metabolites that can elicit deleterious effects on other organisms are classified as mycotoxins. Human exposure to mycotoxins occurs mostly through the intake of contaminated agricultural products or residues due to carry over or metabolite products in foods of animal origin such as milk and eggs, but can also occur by dermal contact and inhalation. Mycotoxins contained in moldy foods, but also in damp interiors, can cause diseases in humans and animals. Nephropathy, various types of cancer, alimentary toxic aleukia, hepatic diseases, various hemorrhagic syndromes, and immune and neurological disorders are the most common diseases that can be related to mycotoxicosis. The absence or presence of mold infestation and its propagation are seldom correlated with mycotoxin presence. Mycotoxins must be determined directly, and suitable analytical methods are necessary. Hundreds of mycotoxins have been recognized, but only for a few of them, and in a restricted number of utilities, a maximum acceptable level has been regulated by law. However, mycotoxins seldom develop alone; more often various types and/or classes form in the same substrate. The co-occurrence might render the individual mycotoxin tolerance dose irrelevant, and therefore the mere presence of multiple mycotoxins should be considered a risk factor. The advantage of chromatography/mass spectrometry (MS) is that many compounds can be determined and confirmed in one analysis. This review illustrates the state-of-the-art of mycotoxin MS-based analytical methods for multiclass, multianalyte determination in all the matrices in which they appear. A chapter is devoted to the history of the long-standing coexistence and interaction among humans, domestic animals and mycotoxicosis, and the history of the discovery of mycotoxins. Quality assurance, although this topic relates to analytical chemistry in general, has been also examined for mycotoxin analysis as a preliminary to the systematic literature excursus. Sample handling is a crucial step to devise a multiclass analytical method; so when possible, it has been treated separately for a better comparison before tackling the instrumental part of the whole analytical method. This structure has resulted sometimes in unavoidable redundancies, because it was also important to underline the interconnection. Most reviews do not deal with all the possible mycotoxin sources, including the environmental ones. The focus of this review is the analytical methods based on MS for multimycotoxin class determination. Because the final purpose to devise multimycotoxin analysis should be the assessment of the danger to health of exposition to multitoxicants of natural origin (and possibly also the interaction with anthropogenic contaminants), therefore also the analytical methods for environmental relevant mycotoxins have been thoroughly reviewed. Finally, because the best way to shed light on actual risk assessment could be the individuation of exposure biomarkers, the review covers also the scarce literature on biological fluids. PMID:22065561

  3. Fast gas chromatography and negative-ion chemical ionization tandem mass spectrometry for forensic analysis of cannabinoids in whole blood

    Microsoft Academic Search

    Aurélien Thomas; Christèle Widmer; Gérard Hopfgartner; Christian Staub

    2007-01-01

    The present work describes a fast gas chromatography\\/negative-ion chemical ionization tandem mass spectrometric assay (Fast GC\\/NICI-MS\\/MS) for analysis of tetrahydrocannabinol (THC), 11-hydroxy-tetrahydrocannabinol (THC-OH) and 11-nor-9-carboxy-tetrahydrocannabinol (THC-COOH) in whole blood. The cannabinoids were extracted from 500?L of whole blood by a simple liquid–liquid extraction (LLE) and then derivatized by using trifluoroacetic anhydride (TFAA) and hexafluoro-2-propanol (HFIP) as fluorinated agents. Mass spectrometric

  4. Analysis of the scent gland secretions of Dumeril's ground boa (Acrantophis dumerili Jan) by gas chromatography-mass spectrometry

    E-print Network

    Simpson, John Thomas

    1989-01-01

    SIMPSON Approved to style and content by: Karl H. Dahm (Co-Chair of Committee) &9 Paul J. Weldon (Co-Chair of Committee) as . arp (Me er) Michael B. all (Head of Department) May 1989 ABSTRACT Analysis of the Scent Gland Secretions of Dumeri...Vs Ground Boa (Acranrophis dumerili Jan) by Gas Chromatography-Mass Spectrometry. (May 1989) John Thomas Simpson, B. S. , Louisiana State University Co-Chairs of Advisory Committee: Dr. Karl H. Dahm Dr. Paul J. Weldon When disturbed by predators, many...

  5. Comprehensive two-dimensional liquid chromatography with evaporative light-scattering detection for the analysis of triacylglycerols in Borago officinalis.

    PubMed

    Mondello, Luigi; Beccaria, Marco; Donato, Paola; Cacciola, Francesco; Dugo, Giovanni; Dugo, Paola

    2011-03-01

    An optimized 2-D liquid chromatography (LC×LC) set-up, based on the different selectivities of a silver ion (Ag) and a non-aqueous reversed phase (NARP), employed in the first (D1) and the second dimension (D2), respectively, in combination with evaporative light-scattering detection (ELSD), has been developed for the analysis of the triacylglycerol (TAG) fraction in a Borago officinalis oil. The 2-D set-up, thanks to the complementary separation selectivity provided by the two columns, allowed to distribute 78 TAGs throughout the 2-D LC retention plane otherwise unachievable by 1-D LC. PMID:21413146

  6. Column Chromatography

    NSDL National Science Digital Library

    Julie Yu

    2007-01-01

    In this activity, learners separate the components of Gatorade using a home-made affinity column. In doing so, learners model the basic principle of affinity chromatography, a technique used to purify chemicals as well as bio-pharmaceuticals and petroleum products. This resource contains information about affinity chromatography and polarity.

  7. Qualitative analysis of seized synthetic cannabinoids and synthetic cathinones by gas chromatography triple quadrupole tandem mass spectrometry.

    PubMed

    Gwak, Seongshin; Arroyo-Mora, Luis E; Almirall, José R

    2015-02-01

    Designer drugs are analogues or derivatives of illicit drugs with a modification of their chemical structure in order to circumvent current legislation for controlled substances. Designer drugs of abuse have increased dramatically in popularity all over the world for the past couple of years. Currently, the qualitative seized-drug analysis is mainly performed by gas chromatography-electron ionization-mass spectrometry (GC-EI-MS) in which most of these emerging designer drug derivatives are extensively fragmented not presenting a molecular ion in their mass spectra. The absence of molecular ion and/or similar fragmentation pattern among these derivatives may cause the equivocal identification of unknown seized-substances. In this study, the qualitative identification of 34 designer drugs, mainly synthetic cannabinoids and synthetic cathinones, were performed by gas chromatography-triple quadrupole-tandem mass spectrometry with two different ionization techniques, including electron ionization (EI) and chemical ionization (CI) only focusing on qualitative seized-drug analysis, not from the toxicological point of view. The implementation of CI source facilitates the determination of molecular mass and the identification of seized designer drugs. Developed multiple reaction monitoring (MRM) mode may increase sensitivity and selectivity in the analysis of seized designer drugs. In addition, CI mass spectra and MRM mass spectra of these designer drug derivatives can be used as a potential supplemental database along with EI mass spectral database. PMID:24827678

  8. Glycopeptide enrichment for MALDI-TOF mass spectrometry analysis by hydrophilic interaction liquid chromatography solid phase extraction (HILIC SPE).

    PubMed

    Jensen, Pia Hønnerup; Mysling, Simon; Højrup, Peter; Jensen, Ole Nørregaard

    2013-01-01

    Glycoproteins, and in particular glycopeptides, are highly hydrophilic and are often not retained by reversed phase (RP) chromatography. The separation principle of normal phase (NP) is based on hydrophilic interactions, which in many aspects is complementary to RP separations. Hydrophilic interaction liquid chromatography (HILIC) is a fairly new variation of the NP separations used in the 1970s, the major difference being the use of aqueous solvents. HILIC provides a versatile tool for enrichment of glycopeptides before mass spectrometric (MS) analysis, particularly when used for solid phase extraction (SPE), or in combination with other chromatographic resins or ion-pairing reagents. HILIC SPE can be used for glyco-profiling, i.e., for determining the glycan heterogeneity at one specific glycosylation site, for enrichment of glycopeptides from a complex mixture of peptides, as well as for pre-fractionation of complex samples at the protein or peptide level. In this chapter we present a straightforward HILIC SPE enrichment technique and then combine C18 RP and HILIC enrichment for analysis of glycopeptides. Finally, we demonstrate HILIC enrichment using trifluoroacetic acid as an ion-pairing reagent for the enrichment of glycopeptides prior to mass spectrometry analysis. PMID:23296529

  9. Isolation of naturally occurring aluminium ligands using immobilized metal affinity chromatography for analysis by ESI-MS.

    PubMed

    Baldwin, Carson; Cumming, Jonathan; Timperman, Aaron T

    2005-03-01

    Aluminium (iii) is one of the most abundant metal ions found in soil. Typically, Al(+3) is bound to minerals, but its bioavailability and toxicity toward vascular plants increases with increasing soil acidity. Ectomycorrhizal fungi, which live symbiotically on the roots of numerous woody plants, often confer Al(+3) resistance to host plants by reducing metal availability to the plant by unknown mechanisms. A potential mechanism of detoxification is binding of the Al(+3) by organic compounds that are exuded by the fungi into the surrounding soil and solution. A novel method has been developed to purify and characterize Al(+3) binding ligands from Pisolithus tinctorius exudate solutions using Al(+3) immobilized metal affinity chromatography (IMAC), reversed phase chromatography, and mass spectrometry. Fungal exudates produced by P. tinctorius exhibit a strong binding capacity for Al(+3), allowing their selective enrichment and collection using this IMAC method. Elution of the ligands requires the use of high pH. RP-HPLC separation and elemental analysis of the IMAC elutent indicates that the Al(+3) and the exudate ligands both elute from the column but are not bound in a complex. Thus, reversed phase HPLC at pH 10 is used for separation of the ligands and Al(+3) prior to MS analysis. The strongest binding IMAC fraction is analyzed by electrospray ionization mass spectrometry in positive and negative ion modes. This report provides new methods for the direct purification and analysis of naturally occurring ligands that bind hard metal ions. PMID:15724160

  10. Analysis of flavonoids from Cyclanthera pedata fruits by liquid chromatography/electrospray mass spectrometry.

    PubMed

    Carbone, Virginia; Montoro, Paola; de Tommasi, Nunziatina; Pizza, Cosimo

    2004-02-01

    A liquid chromatography/mass spectrometry (LC/MS) based method was developed for the characterization of fruits of Cyclanthera pedata Scrabs (Caigua), a Peruvian food and medicinal plant. This method is based on the separation of flavonoid glycosides present in the methanolic extracts from C. pedata fruits using high performance liquid chromatography (HPLC) followed by detection with electrospray ionization mass spectrometry (ESI/MS). Chromatographic separation of the analytes of interest was achieved on a Symmetry C-18 column with detection in positive ion mode. Calibration graphs were obtained by determining the area ratio between external standard of each major compound and the internal standard naringine. Due to the sensitivity and the repeatability of the assay, this method is suitable for industrial quality control of raw materials and final products. PMID:15013143

  11. Applied analysis of lacquer films based on pyrolysis-gas chromatography\\/mass spectrometry

    Microsoft Academic Search

    Rong Lu; Yukio Kamiya; Tetsuo Miyakoshi

    2006-01-01

    Ancient lacquer film, a Nanban lacquer film, an old lacquer-ware object imported from an Asian country, and the Baroque and Rococo lacquer films were analyzed by pyrolysis-gas chromatography\\/mass spectrometry. Compared with the results of the natural lacquer film, it was revealed that the ancient lacquer film and Nanban lacquer film were made from Rhus vernicifera, and the old lacquer-ware imported

  12. Analysis of ACE inhibitors in pharmaceutical dosage forms by derivative UV spectroscopy and liquid chromatography (HPLC)

    Microsoft Academic Search

    D Bonazzi; R Gotti; V Andrisano; V Cavrini

    1997-01-01

    Derivative UV spectroscopy and high performance liquid chromatography (HPLC) were applied to the determination of angiotensin-converting enzyme (ACE) inhibitors in their pharmaceutical dosage forms. For spectrophotometric determinations, the more appropriate derivative order was selected for each drug: ramipril (third-order), benazepril (second-order), enalapril maleate (second-order), lisinopril (first- and second-order) and quinapril (first-order). Reverse phase HPLC procedures (ODS column) were developed able

  13. Analysis of reduced monoclonal antibodies using size exclusion chromatography coupled with mass spectrometry

    Microsoft Academic Search

    Hongcheng Liu; Georgeen Gaza-Bulseco; Chris Chumsae

    2009-01-01

    Size-exclusion chromatography (SEC) has been widely used to detect antibody aggregates, monomer, and fragments. SEC coupled\\u000a to mass spectrometry has been reported to measure the molecular weights of antibody; antibody conjugates, and antibody light\\u000a chain and heavy chain. In this study, separation of antibody light chain and heavy chain by SEC and direct coupling to a mass\\u000a spectrometer was further

  14. Multiresidue analysis of pesticides in fruits and vegetables by gas chromatography-mass spectrometry

    Microsoft Academic Search

    M. Araoud; W. Douki; A. Rhim; M. F. Najjar; N. Gazzah

    2007-01-01

    A multiresidue method was assessed for the determination of several pesticides (organochlorine, organophosphorus, pyrethroids, triazole, amidine) using gas chromatography\\/mass spectrometry. The extraction of pesticides was carried out by liquid-liquid extraction (LLE) and solid-phase extraction (SPE) using two types of columns (CN and C18). The extracts were cleaned by the addition of florisil, the pesticides were separated by capillary column gas

  15. Hydrophilic interaction liquid chromatography–mass spectrometry for the analysis of paralytic shellfish poisoning (PSP) toxins

    Microsoft Academic Search

    Carmela Dell’Aversano; Philipp Hess; Michael A. Quilliam

    2005-01-01

    Hydrophilic interaction liquid chromatography (HILIC) was examined for the separation of paralytic shellfish poisoning (PSP) toxins using the stationary phase TSK-gel Amide-80®. The parameters tested included type of organic modifier and percentage in the mobile phase, buffer concentration, pH, flow rate and column temperature. Using mass spectrometric (MS) detection, the HILIC column allowed the determination of all the major PSP

  16. Analysis of abamectin residues in avocados by high-performance liquid chromatography with fluorescence detection

    Microsoft Academic Search

    Javier Hernández-Borges; Lidia M. Ravelo-Pérez; Estrella M. Hernández-Suárez; Aurelio Carnero; Miguel Ángel Rodríguez-Delgado

    2007-01-01

    In this work an analytical method for the determination of abamectin residues in avocados is developed using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection. A pre-column derivatization with trifluoroacetic anhydride (TFAA) and N-methylimidazole (NMIM) was carried out. The mobile phase consisted of water, methanol and acetonitrile (5:47.5:47.5v\\/v\\/v) and was pumped at a rate of 1mL\\/min (isocratic elution). The fluorescence

  17. Liquid chromatography–tandem mass spectrometry analysis of nitazoxanide and its major metabolites in goat

    Microsoft Academic Search

    Zhanzhong Zhao; Lifang Zhang; Feiqun Xue; Xiaoyang Wang; Wenli Zheng; Tao Zhang; Chenzhong Fei; Keyu Zhang; Minqi Qiu; Ruixiang Xin; Fengkun Yang

    2008-01-01

    A rapid, sensitive and specific liquid chromatography–electrospray ionization (ESI) tandem mass spectrometry (LC–MS–MS) method has been developed for the identification of nitazoxanide metabolites in goat plasma and urine. The purified samples was separated using an XTerra MS C8 column with the mobile phase consisted of acetonitrile and 10-mM ammonium acetate buffer (pH 2.5) followed a linear gradient elution, and detected

  18. Analysis of triterpenoids in Ganoderma lucidum using liquid chromatography coupled with electrospray ionization mass spectrometry

    Microsoft Academic Search

    Min Yang; Xiaoming Wang; Shuhong Guan; Jiameng Xia; Jianghao Sun; Hui Guo; De-an Guo

    2007-01-01

    Triterpenoids extracted from Ganoderma lucidum (Leyss. ex Fr.) Karst were separated and characterized using optimized reversed-phase liquid chromatography with diode array\\u000a detection and electrospray ion trap tandem mass spectrometry (HPLC-DAD-ESI-MSn). They could be classified into five types depending on the fragmentation behavior. All triterpenoids gave [M?H]? and [2M?H]? ions by electrospray ionization monitored in the negative ion mode; in addition,

  19. High-performance liquid chromatography analysis of plant saponins: An update 2005-2010

    PubMed Central

    Negi, Jagmohan S.; Singh, Pramod; Pant, Geeta Joshi Nee; Rawat, M. S. M.

    2011-01-01

    Saponins are widely distributed in plant kingdom. In view of their wide range of biological activities and occurrence as complex mixtures, saponins have been purified and separated by high-performance liquid chromatography using reverse-phase columns at lower wavelength. Mostly, saponins are not detected by ultraviolet detector due to lack of chromophores. Electrospray ionization mass spectrometry, diode array detector , evaporative light scattering detection, and charged aerosols have been used for overcoming the detection problem of saponins. PMID:22303089

  20. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    USGS Publications Warehouse

    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 (?g/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 ?g/kg dry weight.

  1. Analysis of cocaethylene, benzoylecgonine and cocaine in human urine by high-performance thin-layer chromatography with ultraviolet detection: a comparison with high-performance liquid chromatography

    Microsoft Academic Search

    Letizia Antonilli; Carmen Suriano; Maria Caterina Grassi; Paolo Nencini

    2001-01-01

    Cocaine and ethanol are frequently used at the same time, resulting in the formation of cocaethylene by transesterification. We studied the capability of high-performance thin-layer chromatography (HPTLC) to simultaneously detect cocaethylene, cocaine and benzoylecgonine in 16 urine specimens of drug addicts, previously tested as positive for benzoylecgonine at immunoenzymatic screening. Accuracy and precision, as well as detection and quantitation limits

  2. An effective device for gas-liquid oxygen removal in enclosed microalgae culture.

    PubMed

    Su, Zhenfeng; Kang, Ruijuan; Shi, Shaoyuan; Cong, Wei; Cai, Zhaoling

    2010-01-01

    A high-performance gas-liquid transmission device (HPTD) was described in this paper. To investigate the HPTD mass transfer characteristics, the overall volumetric mass transfer coefficients, K(A)(La,CO(2)) for the absorption of gaseous CO(2) and K(A)(La,O(2)) for the desorption of dissolved O(2) were determined, respectively, by titration and dissolved oxygen electrode. The mass transfer capability of carbon dioxide was compared with that of dissolved oxygen in the device, and the operating conditions were optimized to suit for the large-scale enclosed micro-algae cultivation. Based on the effectiveness evaluation of the HPTD applied in one enclosed flat plate Spirulina culture system, it was confirmed that the HPTD can satisfy the demand of the enclosed system for carbon supplement and excessive oxygen removal. PMID:18779934

  3. Thermal dispersion in vertical gas-liquid flows with foaming and non-foaming liquids

    SciTech Connect

    Pino, L.R.Z.; Saez, A.E. [Univ. Simmon Bolivar, Caracas (Venezuela). Dept. de Termodinamica y Fenomenos de Transferecia] [Univ. Simmon Bolivar, Caracas (Venezuela). Dept. de Termodinamica y Fenomenos de Transferecia

    1995-05-01

    Heat transfer experiments have been performed in gas-liquid upwards flow in a vertical column with non-foaming (water) and foaming (kerosene) liquids. The main purpose of the experiments has been to characterized the degree of thermal mixing in the system. For the range of conditions employed, the nonfoaming liquid exhibits complete mixing a low liquid superficial velocities. An increased in liquid velocity leads to incomplete mixing. In the latter case, the thermal dispersion coefficient at low gas superficial velocities is larger than what correlations in the literature predict. For the foaming liquid, when foaming and bubbling regions coexist in the bubble column, each region behaves as a completely-mixed subsystem.

  4. Effect of impeller geometry on gas-liquid mass transfer coefficients in filamentous suspensions.

    PubMed

    Dronawat, S N; Svihla, C K; Hanley, T R

    1997-01-01

    Volumetric gas-liquid mass transfer coefficients were measured in suspensions of cellulose fibers with concentrations ranging from 0 to 20 g/L. The mass transfer coefficients were measured using the dynamic method. Results are presented for three different combinations of impellers at a variety of gassing rates and agitation speeds. Rheological properties of the cellulose fibers were also measured using the impeller viscometer method. Tests were conducted in a 20 L stirred-tank fermentor and in 65 L tank with a height to diameter ratio of 3:1. Power consumption was measured in both vessels. At low agitation rates, two Rushton turbines gave 20% better performance than the Rushton and hydrofoil combination and 40% better performance than the Rushton and propeller combination for oxygen transfer. At higher agitation rates, the Rushton and hydrofoil combination gave 14 and 25% better performance for oxygen transfer than two Rushton turbines and the Rushton and hydrofoil combination, respectively. PMID:18576095

  5. Crude oil and natural gas pricing. Chapters 300 to 499: natural gas liquids, natural gas

    SciTech Connect

    Kelly, P.D.

    1980-01-01

    This text analyzes the federal statutes and regulations that affect the pricing and allocation of crude oil, natural gas, and natural gas liquids. It does not cover refined products or imported crude oil except where necessary to place major decisions in historical context. Chapter 300 concerns natural gas liquids. For historical rather than logical reasons, these are regulated as an offshoot of crude oil controls rather than as a by-product of natural gas production. In December 1979, the Economic Regulatory Administration (ERA) deregulated butane and natural gasoline. However, it did not amend 10 CFR 212.161-212.173, and it did not deregulate propane or propane mixtures. Decontrol will be covered in the first update to this book. Chapters 400 to 468 concern natural gas. Although a great deal of attention has been focused on the Natural Gas Policy Act (NGPA), there has been no satisfactory description of the extent to which the Natural Gas Act (NGA; passed in 1938 and amended by the Phillips decision in 1954) still applies. This is quite a problem, since the NGPA is written in vague terms that encourage producers to disregard the NGA. The problem is compounded by the Federal Power Commission's (FPC) approach to regulatory development, which has scattered crucial regulations throughout 18 CFR. All Federal Energy Regulatory Commission (FERC) natural gas production regulations should be repealed, arranged into a systematic grouping, and reissued in a consolidated subpart of 18 CFR. Shortly after the publication of this text, the author will petition the FERC to commence a rulemaking proceeding to that effect. Chapters 480 to 498 will cover the use of natural gas. These chapters will be issued in the first revision to this text as general summaries since the programs do not directly affect gas producers.

  6. DESIGN AND DEVELOPMENT OF GAS-LIQUID CYLINDRICAL CYCLONE COMPACT SEPARATORS FOR THREE-PHASE FLOW

    SciTech Connect

    Dr. Ram S. Mohan; Dr. Ovadia Shoham

    2003-06-25

    The U.S. Department of Energy (DOE) has awarded a five-year (1997-2002) grant (Mohan and Shoham, DE-FG26-97BC15024, 1997) to The University of Tulsa, to develop compact multiphase separation components for 3-phase flow. The research activities of this project have been conducted through cost sharing by the member companies of the Tulsa University Separation Technology Projects (TUSTP) research consortium and the Oklahoma Center for the Advancement of Science and Technology (OCAST). As part of this project, several individual compact separation components have been developed for onshore and offshore applications. These include gas-liquid cylindrical cyclones (GLCC{copyright}), liquid-liquid cylindrical cyclones (LLCC{copyright}), and the gas-liquid-liquid cylindrical cyclones (GLLCC{copyright}). A detailed study has also been completed for the liquid-liquid hydrocyclones (LLHC). Appropriate control strategies have been developed for proper operation of the GLCC{copyright} and LLCC{copyright}. Testing of GLCC{copyright} at high pressure and real crude conditions for field applications is also completed. Limited studies have been conducted on flow conditioning devices to be used upstream of the compact separators for performance improvement. This report presents a brief overview of the activities and tasks accomplished during the 5-year project period, October 1, 1997-March 31, 2003 (including the no-cost extended period of 6 months). An executive summary is presented initially followed by the tasks of the 5-year budget periods. Then, detailed description of the experimental and modeling investigations are presented. Subsequently, the technical and scientific results of the activities of this project period are presented with some discussions. The findings of this investigation are summarized in the ''Conclusions'' section, followed by relevant references. The publications resulting from this study in the form of MS Theses, Ph.D. Dissertation, Journal Papers and Conference Presentations are provided at the end of this report.

  7. An Ultra-Trace Analysis Technique for SF6 Using Gas Chromatography with Negative Ion Chemical Ionization Mass Spectrometry.

    PubMed

    Jong, Edmund C; Macek, Paul V; Perera, Inoka E; Luxbacher, Kray D; McNair, Harold M

    2015-07-01

    Sulfur hexafluoride (SF6) is widely used as a tracer gas because of its detectability at low concentrations. This attribute of SF6 allows the quantification of both small-scale flows, such as leakage, and large-scale flows, such as atmospheric currents. SF6's high detection sensitivity also facilitates greater usage efficiency and lower operating cost for tracer deployments by reducing quantity requirements. The detectability of SF6 is produced by its high molecular electronegativity. This property provides a high potential for negative ion formation through electron capture thus naturally translating to selective detection using negative ion chemical ionization mass spectrometry (NCI-MS). This paper investigates the potential of using gas chromatography (GC) with NCI-MS for the detection of SF6. The experimental parameters for an ultra-trace SF6 detection method utilizing minimal customizations of the analytical instrument are detailed. A method for the detection of parts per trillion (ppt) level concentrations of SF6 for the purpose of underground ventilation tracer gas analysis was successfully developed in this study. The method utilized a Shimadzu gas chromatography with negative ion chemical ionization mass spectrometry system equipped with an Agilent J&W HP-porous layer open tubular column coated with an alumina oxide (Al2O3) S column. The method detection limit (MDL) analysis as defined by the Environmental Protection Agency of the tracer data showed the method MDL to be 5.2 ppt. PMID:25452581

  8. Combining Hydrophilic Interaction Chromatography (HILIC) and Isotope Tagging for Off-Line LC-NMR Applications in Metabolite Analysis

    PubMed Central

    Appiah-Amponsah, Emmanuel; Owusu-Sarfo, Kwadwo; Gowda, G.A. Nagana; Ye, Tao; Raftery, Daniel

    2013-01-01

    The complementary use of liquid chromatography (LC) and nuclear magnetic resonance (NMR) has shown high utility in a variety of fields. While the significant benefit of spectral simplification can be achieved for the analysis of complex samples, other limitations remain. For example, 1H LC-NMR suffers from pH dependent chemical shift variations, especially during urine analysis, owing to the high physiological variation of urine pH. Additionally, large solvent signals from the mobile phase in LC can obscure lower intensity signals and severely limit the number of metabolites detected. These limitations, along with sample dilution, hinder the ability to make reliable chemical shift assignments. Recently, stable isotopic labeling has been used to detect quantitatively specific classes of metabolites of interest in biofluids. Here we present a strategy that explores the combined use of two-dimensional hydrophilic interaction chromatography (HILIC) and isotope tagged NMR for the unambiguous identification of carboxyl containing metabolites present in human urine. The ability to separate structurally related compounds chromatographically, in off-line mode, followed by detection using 1H-15N 2D HSQC (two-dimensional heteronuclear single quantum coherence) spectroscopy, resulted in the assignment of low concentration carboxyl-containing metabolites from a library of isotope labeled compounds. The quantitative nature of this strategy is also demonstrated. PMID:24860727

  9. High Sensitivity Quantitative Lipidomics Analysis of Fatty Acids in Biological Samples by Gas Chromatography-Mass Spectrometry

    PubMed Central

    Quehenberger, Oswald; Armando, Aaron M.; Dennis, Edward A.

    2011-01-01

    Historically considered to be simple membrane components serving as structural elements and energy storing entities, fatty acids are now increasingly recognized as potent signaling molecules involved in many metabolic processes. Quantitative determination of fatty acids and exploration of fatty acid profiles have become common place in lipid analysis. We present here a reliable and sensitive method for comprehensive analysis of free fatty acids and fatty acid composition of complex lipids in biological material. The separation and quantitation of fatty acids is achieved by capillary gas chromatography. The analytical method uses pentafluorobenzyl bromide derivatization and negative chemical ionization gas chromatography-mass spectrometry. The chromatographic procedure provides base line separation between saturated and unsaturated fatty acids of different chain lengths as well as between most positional isomers. Fatty acids are extracted in the presence of isotope-labeled internal standards for high quantitation accuracy. Mass spectrometer conditions are optimized for broad detection capacity and sensitivity capable of measuring trace amounts of fatty acids in complex biological samples. PMID:21787881

  10. Partition coefficients of organic compounds in new imidazolium based ionic liquids using inverse gas chromatography

    Microsoft Academic Search

    Anne-Laure Revelli; Fabrice Mutelet; Jean-Noël Jaubert

    2009-01-01

    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

  11. Effect of an external magnetic field on the gas-liquid transition in the Heisenberg spin fluid

    NASA Astrophysics Data System (ADS)

    Sokolovska, T. G.; Sokolovskii, R. O.

    1999-04-01

    We present the theoretical phase diagrams of the classical Heisenberg fluid in an external magnetic field. A consistent account of correlations is carried out by the integral equation method. A nonmonotonic effect of fields on the temperature of the gas-liquid critical point is found. Within the mean spherical approximation this nonmonotonic behavior disappears for short-range enough spin-spin interactions.

  12. Fast Model Based Approximation of the Closed-loop Performance Limits of Gas/Liquid Inline Separators for Accelerated Design

    E-print Network

    Van den Hof, Paul

    Fast Model Based Approximation of the Closed-loop Performance Limits of Gas/Liquid Inline Separators for Accelerated Design M. Leskens, A. Huesman, P.M.J. Van den Hof* S. Belfroid, E. Nennie** P called inline separators (ILS). Unlike their large conventional counterparts, the operation

  13. Working process study of a novel scroll type multiphase pump for the transportation of gas-liquid mixtures

    NASA Astrophysics Data System (ADS)

    Wang, J.; Zha, H. B.; Zhang, X. H.; Zhang, D. H.

    2012-11-01

    A novel scroll type multiphase pump was proposed to transport gas-liquid two-phase mixture. There is a pressure unloading gap from compression chambers to the discharge port by constructing scroll wrap profile with variational meshing clearance in this scroll multiphase pump. In the working process when the volume of working chamber decreases, the pressure of gas-liquid mixtures increases gradually, at the same time small amounts of gas-liquid mixture are pushed to the discharge port from compression chambers through the pressure unloading gap. Therefore, this multiphase pump has an advantage of unloading pressure method automatically, and the frequently problem of liquid impacting in volume multiphase pump is solved. The safety and reliability of volumetric multiphase pump are improved, and the scope of multiphase pump of the gas-liquid ratio is expanded. The working process and the performance characteristics of scroll multiphase pump were analyzed too, and the generation method of scroll wrap profile with variational meshing clearance was investigated. The equations of the profile were obtained, and the changing principle of the working volume and the meshing clearance were analyzed. The geometric theory of scroll multiphase pump was formed. All of that lay the theoretical foundation for engineering design of this novel scroll.

  14. Study and modeling of the evolution of gas-liquid partitioning of hydrogen sulfide in model solutions simulating winemaking fermentations.

    PubMed

    Mouret, Jean-Roch; Sablayrolles, Jean-Marie; Farines, Vincent

    2015-04-01

    The knowledge of gas-liquid partitioning of aroma compounds during winemaking fermentation could allow optimization of fermentation management, maximizing concentrations of positive markers of aroma and minimizing formation of molecules, such as hydrogen sulfide (H2S), responsible for defects. In this study, the effect of the main fermentation parameters on the gas-liquid partition coefficients (Ki) of H2S was assessed. The Ki for this highly volatile sulfur compound was measured in water by an original semistatic method developed in this work for the determination of gas-liquid partitioning. This novel method was validated and then used to determine the Ki of H2S in synthetic media simulating must, fermenting musts at various steps of the fermentation process, and wine. Ki values were found to be mainly dependent on the temperature but also varied with the composition of the medium, especially with the glucose concentration. Finally, a model was developed to quantify the gas-liquid partitioning of H2S in synthetic media simulating must to wine. This model allowed a very accurate prediction of the partition coefficient of H2S: the difference between observed and predicted values never exceeded 4%. PMID:25763810

  15. Analysis of biomass sugars and galacturonic acid by gradient anion exchange chromatography and pulsed amperometric detection without post-column addition

    Technology Transfer Automated Retrieval System (TEKTRAN)

    While the most accurate method for analysis of sugars in biomass is based on gas chromatography of trimethylsilane or alditol acetate derivatives of sugars, the derivation method is time consuming and laborious. In comparison, sample preparation for sugar analysis of hydrolyzed biomass samples using...

  16. Ultra-Trace Analysis of Nine Macrolides, including Tulathromycin A (Draxxin), in Edible Animal Tissues with Mini-Column Liquid Chromatography Tandem Mass Spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Analysis of 9 macrolides is presented, including tulathromycin A (Draxxin), in beef, poultry and pork muscle with a simple multi-residue extraction and analysis method using high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry. The extraction method inv...

  17. Chemical absorption process for degradation of VOC gas using heterogeneous gas-liquid photocatalytic oxidation: toluene degradation by photo-Fenton reaction.

    PubMed

    Tokumura, Masahiro; Nakajima, Rina; Znad, Hussein Tawfeek; Kawase, Yoshinori

    2008-10-01

    A novel process for degradation of toluene in the gas-phase using heterogeneous gas-liquid photocatalytic oxidation has been developed. The degradation of toluene gas by photo-Fenton reaction in the liquid-phase has experimentally examined. The photo-Fenton reaction in the liquid-phase could improve the overall toluene absorption rate by increasing the driving force for mass transfer and as a result enhance the removal of toluene in the exhaust gas. The toluene concentrations in the inlet gas were varied in the range from 0.0968 to 8.69 g m(-3) with initial hydrogen peroxide concentration of 400 mg l(-1) and Fe dose of 5.0 mg l(-1). It was found that toluene in the inlet gas was almost completely dissolved into water and degraded in the liquid-phase for the inlet toluene gas concentration of less than 0.42 g m(-3). The dynamic process of toluene gas degradation by the photo-Fenton reaction providing information for reaction kinetics and mass transfer rate was examined. Toluene removal kinetic analysis indicated that photo-Fenton degradation was significantly affected by H(2)O(2) concentration. The experimental results were satisfactorily described by the predictions simulated using the simplified tanks-in-series model combined with toluene removal kinetic analysis. The present results showed that the proposed chemical absorption process using the photo-Fenton heterogeneous gas-liquid photocatalytic oxidation is very effective for degradation of volatile organic gases. PMID:18653212

  18. Analysis of benzo(a)pyrene in airborne particulates by gas chromatography

    NASA Technical Reports Server (NTRS)

    Luedecke, E.

    1976-01-01

    A routine method was developed to measure benzo(a)pyrene in airborne particulates. Samples were collected on a filter and the organic portion was extracted with cyclohexane. The polynuclear hydrocarbon (PNHC) fraction was separated from the aliphatics by column chromatography. An internal standard was added to the extract and a portion of it was injected into a gas chromatograph. Although the gas chromatographic method has often been reported in the literature, satisfactory separation of benzo(a)pyrene and benzo(e)pyrene has not been achieved. With the introduction of a nematic liquid crystal as the stationary phase good separation is now possible.

  19. Analysis of isothiazolinones in environmental waters by gas chromatography–mass spectrometry

    Microsoft Academic Search

    Astrid Rafoth; Sabine Gabriel; Frank Sacher; Heinz-Jürgen Brauch

    2007-01-01

    This paper describes an analytical method for the determination of five biocides of isothiazolinone type (2-methyl-3-isothiazolinone (MI), 5-chloro-2-methyl-3-isothiazolinone (CMI), 1,2-benzisothiazolinone (BIT), 2-octyl-3-isothiazolinone (OI), 4,5-dichloro-2-octyl-3-isothiazolinone (DCOI)) in environmental waters. The method is based on pre-concentration of the analytes by solid-phase extraction onto a mixture of a polymeric material and RP-C18 material and subsequent determination by gas chromatography–mass spectrometry (GC–MS). One of

  20. Rapid analysis of ionic and nonionic surfactant homologs by high performance liquid chromatography

    Microsoft Academic Search

    K. Nakamura; Y. Morikawa; I. Matsumoto

    1981-01-01

    Several ionic and nonionic surfactants were separated into their homologs and their homologous distributions were determined\\u000a by high performance liquid chromatography on an octadecyl-silica (TSK Gel LS-410) column with a water-methanol-sodium chloride\\u000a mixture as a mobile phase. The recommended condition for the separation was as follows: column size, 4 mm id x 250 mm; mobile\\u000a phase, water\\/methanol (15\\/85, v\\/v) containing

  1. Ion Exchange Chromatography and Mass Spectrometric Methods for Analysis of Cadmium-Phytochelatin (II) Complexes

    PubMed Central

    Merlos Rodrigo, Miguel Angel; Cernei, Natalia; Kominkova, Marketa; Zitka, Ondrej; Beklova, Miroslava; Zehnalek, Josef; Kizek, Rene; Adam, Vojtech

    2013-01-01

    In this study, in vitro formed Cd-phytochelatin (PC2) complexes were characterized using ion exchange chromatography (IEC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. The ratio of both studied compounds as well as experimental conditions were optimized. The highest yield of the complex was observed under an applied concentration of 100 µg·mL?1 PC2 and 100 µg·mL?1 of CdCl2. The data obtained show that IEC in combination with MALDI-TOF is a reliable and fast method for the determination of these complexes. PMID:23538727

  2. Measurements of liquid-phase turbulence in gas-liquid two-phase flows using particle image velocimetry

    NASA Astrophysics Data System (ADS)

    Zhou, Xinquan; Doup, Benjamin; Sun, Xiaodong

    2013-12-01

    Liquid-phase turbulence measurements were performed in an air-water two-phase flow loop with a circular test section of 50 mm inner diameter using a particle image velocimetry (PIV) system. An optical phase separation method--planar laser-induced fluorescence (PLIF) technique—which uses fluorescent particles and an optical filtration technique, was employed to separate the signals of the fluorescent seeding particles from those due to bubbles and other noises. An image pre-processing scheme was applied to the raw PIV images to remove the noise residuals that are not removed by the PLIF technique. In addition, four-sensor conductivity probes were adopted to measure the radial distribution of the void fraction. Two benchmark tests were performed: the first was a comparison of the PIV measurement results with those of similar flow conditions using thermal anemometry from previous studies; the second quantitatively compared the superficial liquid velocities calculated from the local liquid velocity and void fraction measurements with the global liquid flow rate measurements. The differences of the superficial liquid velocity obtained from the two measurements were bounded within ±7% for single-phase flows and two-phase bubbly flows with the area-average void fraction up to 18%. Furthermore, a preliminary uncertainty analysis was conducted to investigate the accuracy of the two-phase PIV measurements. The systematic uncertainties due to the circular pipe curvature effects, bubble surface reflection effects and other potential uncertainty sources of the PIV measurements were discussed. The purpose of this work is to facilitate the development of a measurement technique (PIV-PLIF) combined with image pre-processing for the liquid-phase turbulence in gas-liquid two-phase flows of relatively high void fractions. The high-resolution data set can be used to more thoroughly understand two-phase flow behavior, develop liquid-phase turbulence models, and assess high-fidelity codes for multi-phase flows.

  3. Floral classification of honey using liquid chromatography-diode array detection-tandem mass spectrometry and chemometric analysis.

    PubMed

    Zhou, Jinhui; Yao, Lihu; Li, Yi; Chen, Lanzhen; Wu, Liming; Zhao, Jing

    2014-02-15

    A high performance liquid chromatography-diode array detection-tandem mass spectrometry (HPLC-DAD-MS/MS) method for the floral origin traceability of chaste honey and rape honey samples was firstly presented in this study. Kaempferol, morin and ferulic acid were used as floral markers to distinguish chaste honey from rape honey. Chromatographic fingerprinting at 270 nm and 360 nm could be used to characterise chaste honey and rape honey according to the analytical profiles. Principal component analysis (PCA), partial least squares (PLS), partial least squares-discrimination analysis (PLS-DA) and soft independent modeling of class analogy (SIMCA) were applied to classify the honey samples according to their floral origins. The results showed that chaste honey and rape honey could be successfully classified by their floral sources with the analytical methods developed through this study and could be considered encouraging and promising for the honey traceability from unifloral or multifloral nectariferous sources. PMID:24128567

  4. Affinity Chromatography

    NSDL National Science Digital Library

    Using exposition, graphics, and commercial videos, this module teaches the theory and application of affinity chromatography in the characterization of proteins, nucleic acids, and other biochemical/biomedical systems. Problems and application examples support the tutorial material.

  5. Fingerprint analysis of Hibiscus mutabilis L. leaves based on ultra performance liquid chromatography with photodiode array detector combined with similarity analysis and hierarchical clustering analysis methods

    PubMed Central

    Liang, Xianrui; Ma, Meiling; Su, Weike

    2013-01-01

    Background: A method for chemical fingerprint analysis of Hibiscus mutabilis L. leaves was developed based on ultra performance liquid chromatography with photodiode array detector (UPLC-PAD) combined with similarity analysis (SA) and hierarchical clustering analysis (HCA). Materials and Methods: 10 batches of Hibiscus mutabilis L. leaves samples were collected from different regions of China. UPLC-PAD was employed to collect chemical fingerprints of Hibiscus mutabilis L. leaves. Results: The relative standard deviations (RSDs) of the relative retention times (RRT) and relative peak areas (RPA) of 10 characteristic peaks (one of them was identified as rutin) in precision, repeatability and stability test were less than 3%, and the method of fingerprint analysis was validated to be suitable for the Hibiscus mutabilis L. leaves. Conclusions: The chromatographic fingerprints showed abundant diversity of chemical constituents qualitatively in the 10 batches of Hibiscus mutabilis L. leaves samples from different locations by similarity analysis on basis of calculating the correlation coefficients between each two fingerprints. Moreover, the HCA method clustered the samples into four classes, and the HCA dendrogram showed the close or distant relations among the 10 samples, which was consistent to the SA result to some extent. PMID:23930008

  6. Multiresidue analysis of pesticides in fruits and vegetables by gas chromatography-mass spectrometry.

    PubMed

    Araoud, M; Douki, W; Rhim, A; Najjar, M F; Gazzah, N

    2007-02-01

    A multiresidue method was assessed for the determination of several pesticides (organochlorine, organophosphorus, pyrethroids, triazole, amidine) using gas chromatography/mass spectrometry. The extraction of pesticides was carried out by liquid-liquid extraction (LLE) and solid-phase extraction (SPE) using two types of columns (CN and C18). The extracts were cleaned by the addition of florisil, the pesticides were separated by capillary column gas chromatography and detected by mass spectrometry in the electron impact mode. The extraction using C18 column provided the best results for most of the analyzed pesticides. The majority of pesticides recoveries from the four fruits and vegetables (apples, pears, tomatoes and pepper) were greater than 60%. Linearity and precision were satisfactory. The estimated limits of detection and limits of quantification ranged from 0.01 to 0.1 mg/kg and from 0.02 to 0.3 mg/kg, respectively. The proposed procedure was found to be useful for the multiresidue analyses of pesticides in agricultural products for routine monitoring programs. PMID:17365333

  7. Analysis of triacylglycerols on porous graphitic carbon by high temperature liquid chromatography.

    PubMed

    Merelli, Bérangère; De Person, Marine; Favetta, Patrick; Lafosse, Michel

    2007-07-20

    The retention behaviour of several triacylglycerols (TAGs) and fats on Hypercarb, a porous graphitic carbon column (PGC), was investigated in liquid chromatography (LC) under isocratic elution mode with an evaporative light scattering detector (ELSD). Mixtures of chloroform/isopropanol were selected as mobile phase for a suitable retention time to study the influence of temperature. The retention was different between PGC and non-aqueous reversed phase liquid chromatography (NARP-LC) on octadecyl phase. The retention of TAGs was investigated in the interval 30-70 degrees C. Retention was greatly affected by temperature: it decreases as the column temperature increases. Selectivity of TAGs was also slightly influenced by the temperature. Moreover, this chromatographic method is compatible with a mass spectrometer (MS) detector by using atmospheric pressure chemical ionisation (APCI): same fingerprints of cocoa butter and shea butter were obtained with LC-ELSD and LC-APCI-MS. These preliminary results showed that the PGC column could be suitable to separate quickly triacylglycerols in high temperature conditions coupled with ELSD or MS detector. PMID:17517419

  8. Gas chromatography analysis with olfactometric detection (GC-O) as a useful methodology for chemical characterization of odorous compounds.

    PubMed

    Brattoli, Magda; Cisternino, Ezia; Dambruoso, Paolo Rosario; de Gennaro, Gianluigi; Giungato, Pasquale; Mazzone, Antonio; Palmisani, Jolanda; Tutino, Maria

    2013-01-01

    The gas chromatography-olfactometry (GC-O) technique couples traditional gas chromatographic analysis with sensory detection in order to study complex mixtures of odorous substances and to identify odor active compounds. The GC-O technique is already widely used for the evaluation of food aromas and its application in environmental fields is increasing, thus moving the odor emission assessment from the solely olfactometric evaluations to the characterization of the volatile components responsible for odor nuisance. The aim of this paper is to describe the state of the art of gas chromatography-olfactometry methodology, considering the different approaches regarding the operational conditions and the different methods for evaluating the olfactometric detection of odor compounds. The potentials of GC-O are described highlighting the improvements in this methodology relative to other conventional approaches used for odor detection, such as sensoristic, sensorial and the traditional gas chromatographic methods. The paper also provides an examination of the different fields of application of the GC-O, principally related to fragrances and food aromas, odor nuisance produced by anthropic activities and odorous compounds emitted by materials and medical applications. PMID:24316571

  9. Gas Chromatography Analysis with Olfactometric Detection (GC-O) as a Useful Methodology for Chemical Characterization of Odorous Compounds

    PubMed Central

    Brattoli, Magda; Cisternino, Ezia; Dambruoso, Paolo Rosario; de Gennaro, Gianluigi; Giungato, Pasquale; Mazzone, Antonio; Palmisani, Jolanda; Tutino, Maria

    2013-01-01

    The gas chromatography-olfactometry (GC-O) technique couples traditional gas chromatographic analysis with sensory detection in order to study complex mixtures of odorous substances and to identify odor active compounds. The GC-O technique is already widely used for the evaluation of food aromas and its application in environmental fields is increasing, thus moving the odor emission assessment from the solely olfactometric evaluations to the characterization of the volatile components responsible for odor nuisance. The aim of this paper is to describe the state of the art of gas chromatography-olfactometry methodology, considering the different approaches regarding the operational conditions and the different methods for evaluating the olfactometric detection of odor compounds. The potentials of GC-O are described highlighting the improvements in this methodology relative to other conventional approaches used for odor detection, such as sensoristic, sensorial and the traditional gas chromatographic methods. The paper also provides an examination of the different fields of application of the GC-O, principally related to fragrances and food aromas, odor nuisance produced by anthropic activities and odorous compounds emitted by materials and medical applications. PMID:24316571

  10. Pesticide residues in chicken eggs - A sample preparation methodology for analysis by gas and liquid chromatography/tandem mass spectrometry.

    PubMed

    Hildmann, Fanny; Gottert, Christina; Frenzel, Thomas; Kempe, Guenther; Speer, Karl

    2015-07-17

    A sample preparation method was developed for the analysis of chicken eggs to determine 97 GC and 81 LC amenable residues, including organophosphates, organochlorines, pyrethroids, triazoles, carboxyl-containing compounds, and the indicator PCBs. Hereby, considerations were given to the recoveries of the analytes, the method's suitability for routine analysis, and the assessment of the clean-up effect, for which a simple thin layer chromatography was implemented to visualize the most important lipid classes. The procedure consisted of (I) the extraction by matrix solid phase dispersion, and the clean-up by means of (II) small-scale gel permeation chromatography (GPC) and (III) two different solid phase extractions (SPE) for GC and LC amenable analytes, as well as (IV) the quantification using GC-MS/MS and LC-MS/MS. Cyclohexane/ethyl acetate was chosen as extraction solvent due to its suitability for extracting strong non-polar but also more polar analytes. The classical GPC was scaled down to ensure a 50% lower solvent consumption. The comprehensive investigation of conventional and modern zirconium-oxide-coated SPE materials resulted in the selection of octadecyl-modified silica (C18) combined with primary secondary amine using acetonitrile as elution solvent for GC amenable analytes and pure C18 in combination with acidified methanol for LC amenable pesticides. Compared to the currently established EN 1528 method the sample preparation proposed offered a higher sample throughput and a lower solvent consumption. Furthermore, for the first time the clean-up effectiveness of the sample preparation steps was documented as shown by means of thin-layer chromatography. The validation of chicken eggs proved the fulfillment of the quality control criteria for 164 of the 178 analytes tested, mostly at the lowest validated level of 5?g/kg for pesticides and 0.5?g/kg for the single indicator PCBs. However, the analysis of strongly polar analytes was still problematic, which could be attributed to the extraction and the GPC step. Nevertheless, the successful investigation of EU proficiency test materials (EUPT AO 07-09) confirmed the comparability of the results with the currently established sample preparation procedures and demonstrated the potential of the applicability of the presented method to other matrices as exemplified for lean poultry meat and fatty liquid cream. PMID:26051081

  11. Flow chemistry: intelligent processing of gas-liquid transformations using a tube-in-tube reactor.

    PubMed

    Brzozowski, Martin; O'Brien, Matthew; Ley, Steven V; Polyzos, Anastasios

    2015-02-17

    CONSPECTUS: The previous decade has witnessed the expeditious uptake of flow chemistry techniques in modern synthesis laboratories, and flow-based chemistry is poised to significantly impact our approach to chemical preparation. The advantages of moving from classical batch synthesis to flow mode, in order to address the limitations of traditional approaches, particularly within the context of organic synthesis are now well established. Flow chemistry methodology has led to measurable improvements in safety and reduced energy consumption and has enabled the expansion of available reaction conditions. Contributions from our own laboratories have focused on the establishment of flow chemistry methods to address challenges associated with the assembly of complex targets through the development of multistep methods employing supported reagents and in-line monitoring of reaction intermediates to ensure the delivery of high quality target compounds. Recently, flow chemistry approaches have addressed the challenges associated with reactions utilizing reactive gases in classical batch synthesis. The small volumes of microreactors ameliorate the hazards of high-pressure gas reactions and enable improved mixing with the liquid phase. Established strategies for gas-liquid reactions in flow have relied on plug-flow (or segmented flow) regimes in which the gas plugs are introduced to a liquid stream and dissolution of gas relies on interfacial contact of the gas bubble with the liquid phase. This approach confers limited control over gas concentration within the liquid phase and is unsuitable for multistep methods requiring heterogeneous catalysis or solid supported reagents. We have identified the use of a gas-permeable fluoropolymer, Teflon AF-2400, as a simple method of achieving efficient gas-liquid contact to afford homogeneous solutions of reactive gases in flow. The membrane permits the transport of a wide range of gases with significant control of the stoichiometry of reactive gas in a given reaction mixture. We have developed a tube-in-tube reactor device consisting of a pair of concentric capillaries in which pressurized gas permeates through an inner Teflon AF-2400 tube and reacts with dissolved substrate within a liquid phase that flows within a second gas impermeable tube. This Account examines our efforts toward the development of a simple, unified methodology for the processing of gaseous reagents in flow by way of development of a tube-in-tube reactor device and applications to key C-C, C-N, and C-O bond forming and hydrogenation reactions. We further describe the application to multistep reactions using solid-supported reagents and extend the technology to processes utilizing multiple gas reagents. A key feature of our work is the development of computer-aided imaging techniques to allow automated in-line monitoring of gas concentration and stoichiometry in real time. We anticipate that this Account will illustrate the convenience and benefits of membrane tube-in-tube reactor technology to improve and concomitantly broaden the scope of gas/liquid/solid reactions in organic synthesis. PMID:25611216

  12. Drop tower experiment for performance evaluation of gas-liquid equilibrium thruster for small spacecraft

    NASA Astrophysics Data System (ADS)

    Motooka, Norizumi; Yamamoto, Takayuki; Mori, Osamu; Okano, Yoshinobu; Kishino, Yoshihiro; Kawaguchi, Junichiro

    JAXA/ISAS is developing the gas-liquid equilibrium thruster for a small spacecraft. In small spacecrafts, the thruster system must be simple and its weight must be light. This thruster system uses HFC-134a (1,1,1,2-tetrafluoroethane) , a kind of liquefied gas, as propellant because of its harmlessness and ease of handling. And this thruster stores propellant as liquid in the tank and ejects propellant as gas using the gas-liquid equilibrium pressure to produce thrust, so the propellant tank only needs to resist the vapor pressure of propellant. In this thruster system, the porous metal is also equipped in the tank for the following performance advantages: (1) liquid fuel retention: The porous metal reduces sloshing problems which cause bad effects on spacecraft attitude by retaining liquid propellant inside the porous metal: (2) vapor-liquid separation: The porous metal also helps propellant separate gas from liquid by advancing propellant vaporization on its large surface area and retaining liquid propellant using its surface tension. In last autumn, we carried out the experiment to evaluate these two advantages of porous metal under micro gravity condition using 50 meters drop tower in Hokkaido, Japan. The system of this experiment divides into two different systems. The first one evaluates liquid propellant retention performance by adding disturbance to liquid propellant absorbed in porous metal. The disturbance is centrifugal force and angular acceleration worked on the liquid propellant by rotating propellant tank controlled by motor. A high speed camera records the behavior of the liquid propellant. The other one evaluates the ability of gas-liquid separation on the case of propellant ejection. In this evaluation, the parameters are full filling porous metal or some ullage in the tank, nozzle diameters and the filling ratio of liquid propellant in the tank. As for (1) liquid fuel retention, in all conducted cases without propellant ejection, liquid propellant was retained in the porous metal. It is obvious that the porous metal is effective for decreasing of sloshing problems. We evaluated this effectiveness analytically based on head pressure worked on liquid propellant as centrifugal force and angular acceleration. As for (2)vapor-liquid separation, liquid propellant retained inside the porous metal started to boil right after propellant ejection occurred and propellant was ejected mixed with liquid. And after propellant ejection, it takes some time to recover tank pressure into saturated vapor pressure. To obtain stable thrust force, it is required to halt the propellant ejection just before the tank pressure reaches to the break point pressure and to take enough ejection intervals to recover the tank pressure. From these experiments, for practical use of this thruster system, that is, to avoid liquid propellant ejection, it is important to ensure adequate ullage volume of tank to achieve mission requirement.

  13. Improved analysis of vitamin D metabolites in plasma using liquid chromatography tandem mass spectrometry, and its application to cardiovascular research.

    PubMed

    Sandhu, Jatinderpal K; Auluck, Janica; Ng, Leong L; Jones, Donald J L

    2014-06-01

    The accurate and specific measurement of vitamin D is increasingly important for determining the role of vitamin D in the pathogenesis of disease. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS) has increasingly become the analytical modality of choice for the analysis of vitamin D. There are many advantages to using LC/MS/MS, such as high specificity and sensitivity to help distinguish the isomers of vitamin D. This rapid method, modified from a Waters Corporation application note, consists of minimal sample manipulation using liquid-liquid extraction and incorporates an internal standard. The supernatant is dried down and injected onto an ultra-high-performance liquid chromatography/electrospray ionization tandem mass spectrometer. The total analysis time is 10 min per injection, enabling high throughput of samples. This method also incorporates two commercial quality control standards to provide a robust system with acceptable coefficient of variation. The analysis of control and heart failure plasma samples showed significant differences in the levels of vitamin D3 between these two groups; however, in the control group, there were individuals who were vitamin D deficient. Overall, the vitamin D3 levels were higher in control samples than in heart failure individuals. As expected, vitamin D2 levels were not observed in many of the samples analysed. This modified method is quick and incorporates an internal standard to allow for any loss in the extraction procedure. The method also includes quality control samples to enable assay standardization. The assay involves inexpensive pre-sample clean-up, aiding high throughput, which is important in many laboratories. PMID:24861764

  14. Direct multicomponent analysis of beer samples constituents using micellar electrokinetic capillary chromatography.

    PubMed

    Cortacero-Ramírez, Sonia; Segura-Carretero, Antonio; Cruces-Blanco, Carmen; Hernáinz-Bermúdez de Castro, Miguel; Fernández-Gutiérrez, Alberto

    2004-06-01

    A capillary electrophoretic method was developed using micellar electrokinetic capillary chromatography (MEKC) with diode-array detection to analyze simultaneously 26 beer constituents in a single procedure, including alcohols, iso-alpha-acids, amino acids, flavonoids, isoflavonoids, a vitamin, purine and pyrimidine bases. After filtration, sample components were separated with an uncoated capillary and a 25 mM sodium borate and 110 mM SDS buffer at pH 10.5. Analyses were run at 14 kV and 8 s of hydrodynamic injection with UV detection at 210 nm and 270 nm. The proposed method was successfully applied to the direct determination of beer constituents without any sample cleanup procedures. PMID:15213986

  15. Quantitative Analysis and Fingerprint Profiles for Quality Control of Fructus Schisandrae by Gas Chromatography: Mass Spectrometry

    PubMed Central

    Xia, Yong-Gang; Yang, Bing-You; Liang, Jun; Yang, Qi; Wang, Di; Kuang, Hai-Xue

    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 by using GC-MS techniques. The relative retention times of these characteristic peaks in the GC-MS fingerprint were established as an important parameter for identification of Schisandra samples. Meanwhile, relative peak areas may be a feasible approach to discriminate the S. chinensis and S. sphenanthera. Finally, these pharmacologically active constituents in the titled plant, schisandrins A–C and schizandrols A and B, were quantitatively determined using a validated GC-MS method. PMID:24574919

  16. Analysis of lipophilic pigments from a phototrophic microbial mat community by high performance liquid chromatography

    NASA Technical Reports Server (NTRS)

    Palmisano, A. C.; Cronin, S. E.; Des Marais, D. J.

    1988-01-01

    As assay for lipophilic pigments in phototrophic microbial mat communities using reverse phase-high performance liquid chromatography was developed which allows the separation of 15 carotenoids and chloropigments in a single 30 min program. Lipophilic pigments in a laminated mat from a commercial salina near Laguna Guerrero Negro, Baja California Sur, Mexico reflected their source organisms. Myxoxanthophyll, echinenone, canthaxanthin, and zeaxanthin were derived from cyanobacteria; chlorophyll c, and fucoxanthin from diatoms; chlorophyll a from cyanobacteria and diatoms; bacteriochlorophylls a and c, bacteriophaeophytin a, and gamma-carotene from Chloroflexus spp.; and beta-carotene from a variety of phototrophs. Sensitivity of detection was 0.6-6.1 ng for carotenoids and 1.7-12 ng for most chloropigments. This assay represents a significant improvement over previous analyses of lipophilic pigments in microbial mats and promises to have a wider application to other types of phototrophic communities.

  17. [Analysis of cracking gas compressor fouling by pyrolysis gas chromatography-mass spectrometry].

    PubMed

    Hu, Yunfeng; Fang, Fei; Wei, Tao; Liu, Shuqing; Jiang, Guangshen; Cai, Jun

    2013-06-01

    The fouling from the different sections of the cracked gas compressor in Daqing Petrochemical Corporation was analyzed by pyrolysis gas chromatography-mass spectrometry (Py/GC-MS). All the samples were cracked in RJ-1 tube furnace cracker at the cracking temperature of 500 degrees C, and separated with a 60 m DB-1 capillary column. An electron impact ionization (EI) source was used with the ionizing voltage of 70 eV. The results showed the formation of fouling was closely related with cyclopentadiene which accounted for about 50% of the cracking products. Other components detected were 1-butylene, propylene, methane and n-butane. This Py/GC-MS method can be used as an effective approach to analyze the causes of fouling in the petrochemical plants. PMID:24063202

  18. A versatile cryo-focussing flow switching gas chromatography inlet for trace analysis of intractable compounds.

    PubMed

    Apps, Peter; Mmualefe, Lesego

    2012-09-28

    A wide variety of samples that can be analysed by gas chromatography do not lend themselves to the usual preparation of solvent extracts for split-splitless injections, and are best handled by purge and trap or equilibrium headspace sampling. A cryo-focussing, flow switching gas chromatography inlet system that handles different types of sample without the need for hardware changes has been prototyped. It provides excellent repeatability and linearity with liquid injections, purge and trap, and equilibrium headspace samples, in both split and splitless modes. The performance of the system was tested with sub-nanogram quantities of challenging analytes such as free carboxylic acids, alcohols, diols, phenols and aldehydes, and volatiles purged from contaminated soil, mammal faeces, a pesticide formulation, and a spice. Repeatability RSDs for peak areas were consistently below 11% and repeatabilities of retention times below 0.05%, independently of sample type (liquid or gas phase) and nature or quantity of compound. Regression coefficients of peak areas vs. quantity were typically ? 0.999 over two orders of magnitude ranges extending down to below 0.01 ng, also independently of sample and analyte. Limits of quantitation were robustly below 0.1-0.2 ng. Peak shapes and resolution are the same with use of the cryo-trap and flow switch as they are with conventional injections. Performance is robust to flow rate and, for most compounds, to trapping and desorption temperature. The cryo-trapping flow switching inlet's performance parameters match those of other sample introduction systems, and are achieved with sub-nanogram quantities of intractable analytes. PMID:22920301

  19. Ultrahigh performance liquid chromatography analysis of volatile carbonyl compounds in virgin olive oils.

    PubMed

    Zhu, Hanjiang; Li, Xueqi; Shoemaker, Charles F; Wang, Selina C

    2013-12-18

    The enzymatic and chemical oxidation reaction in olive oil produces many volatile carbonyl compounds that contribute to the complex flavor of olive oil. A novel ultrahigh performance liquid chromatography (UHPLC) method with dynamic headspace sampling and 2,4-dinitrophenylhydrazine (DNPH) derivatization were established to determine the volatile carbonyls in virgin olive oil. Quantification of nine characteristic carbonyls (acetone, hexanal, E-2-hexenal, octanal, E-2-octenal, nonanal, E-2-nonenal, E,E-2,4-nonadienal, and E,E-2,4-decadienal) was achieved using cyclopentanal as an internal standard. This method provides comparable linearity (R(2) = 0.9917-1.0000) and repeatability (less than 7.6% relative standard deviations) with solid phase microextraction gas chromatography (SPME-GC). The relative standard deviations (%RSD) of all applied carbonyl standards were lower than 7.6%. The limits of detection (LOD) and quantification (LOQ) were in the ranges of 1.6-150.1 and 4.8-906.1 ?g/kg. The recoveries obtained for olive oil samples were in the range of 81.0-115.3%. To show the potential of this method on the quantification of other volatile carbonyls that were not included in this study, GC-electron ionization mass spectrometry (GC-EI/MS) was employed to identify the derivatized carbonyls (carbonyl (2,4-DNPH) hydrazones) while peak assignments were made on the basis of elution sequences and peak areas. This method provided feasibility of using LC to determine volatile carbonyls in oil matrices, which can be applied to exam the degree of lipid oxidation and evaluate the sensory properties of VOO and other edible oils. PMID:24279346

  20. Analysis of plant galactolipids by reversed-phase high-performance liquid chromatography/mass spectrometry with accurate mass measurement.

    PubMed

    Zábranská, Marie; Vrkoslav, Vladimír; Sobotníková, Jana; Cva?ka, Josef

    2012-07-01

    The composition of plant membrane lipids was investigated by reversed-phase high performance liquid chromatography mass spectrometry with accurate mass measurement. The data dependent methods for the analysis of monogalactosyldiacylglycerols (MGDGs) and digalactosyldiacylglycerols (DGDGs) have been developed. The optimised chromatographic systems were based on a 2.0 mm i.d. Nucleosil C18 column with methanol/water (MGDGs) or acetonitrile/methanol/water (DGDGs) gradients. The galactolipids were ionised by electrospray operated in the positive ion mode and identified based on their MS/MS spectra. High resolution spectra with accurate masses were found to be essential for correct interpretation of the MS data. The elution order of non-oxidised MGDGs and DGDGs followed the equivalent carbon numbers. The methods were applied for detailed characterisation of the MGDGs and DGDGs in the leaves of Arabidopsis thaliana and Melissa officinalis. PMID:22465211

  1. Fourier transform-infrared spectroscopy and Gas chromatography-mass spectroscopy: Reliable techniques for analysis of Parthenium mediated vermicompost

    NASA Astrophysics Data System (ADS)

    Rajiv, P.; Rajeshwari, Sivaraj; Venckatesh, Rajendran

    2013-12-01

    Fourier transform infrared spectroscopy (FT-IR) and Gas chromatography-mass spectroscopy have been carried out to investigate the chemical composition of Parthenium mediated vermicompost. Four different concentrations of Parthenium and cow dung mixtures were vermicomposted using the earthworms (Eudrilus eugeniae). FT-IR spectra reveal the absence of Parthenin toxin (sesquiterpene lactone) and phenols in vermicompost which was obtained from high concentration of cow dung mixed treatments. GC-MS analysis shows no phenolic compounds and predominant level of intermediate metabolites such as 4,8,12,16-Tetramethylheptadecan-4-olide (7.61%), 2-Pentadecanone, 6,10,14-trimethyl- (5.29%) and Methyl 16-methyl-heptadecanoate (4.69%) during the vermicomposting process. Spectral results indicated that Parthenin toxin and phenols can be eradicated via vermicomposting if mixed with appropriate quantity of cow dung.

  2. Fourier transform-infrared spectroscopy and Gas chromatography-mass spectroscopy: reliable techniques for analysis of Parthenium mediated vermicompost.

    PubMed

    Rajiv, P; Rajeshwari, Sivaraj; Venckatesh, Rajendran

    2013-12-01

    Fourier transform infrared spectroscopy (FT-IR) and Gas chromatography-mass spectroscopy have been carried out to investigate the chemical composition of Parthenium mediated vermicompost. Four different concentrations of Parthenium and cow dung mixtures were vermicomposted using the earthworms (Eudrilus eugeniae). FT-IR spectra reveal the absence of Parthenin toxin (sesquiterpene lactone) and phenols in vermicompost which was obtained from high concentration of cow dung mixed treatments. GC-MS analysis shows no phenolic compounds and predominant level of intermediate metabolites such as 4,8,12,16-Tetramethylheptadecan-4-olide (7.61%), 2-Pentadecanone, 6,10,14-trimethyl- (5.29%) and Methyl 16-methyl-heptadecanoate (4.69%) during the vermicomposting process. Spectral results indicated that Parthenin toxin and phenols can be eradicated via vermicomposting if mixed with appropriate quantity of cow dung. PMID:23998948

  3. Headspace solid-phase microextraction gas chromatography-mass spectrometry analysis of Eupatorium odoratum extract as an oviposition repellent.

    PubMed

    Cui, Shufen; Tan, Shuo; Ouyang, Gangfeng; Jiang, Shihong; Pawliszyn, Janusz

    2009-07-01

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) analysis was used to study volatile and semi-volatile compounds emitted by the Eupatorium odoratum (E. odoratum) extract. Variables of HS-SPME such as the type of SPME fiber, extraction time and temperature, incubation time, desorption time and temperature have been optimized. Optimized conditions were obtained by the use of divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber, 5 min/20 min incubation/extraction time at 65 degrees C, 5 min desorption time at 260 degrees C. Using three different polar chromatographic columns to get retention index and mass spectrometry data, 99 volatile and semi-volatile compounds were tentatively identified in the E. odoratum extract. This study has identified the promising source of E. odoratum oviposition repellent. PMID:19501027

  4. A multidimensional gas chromatography method for the analysis of hydrogen sulfide in crude oil and crude oil headspace.

    PubMed

    Heshka, Nicole E; Hager, Darcy B

    2014-12-01

    Two-dimensional heart-cutting gas chromatography is used to analyze dissolved hydrogen sulfide in crude samples. Liquid samples are separated first on an HP-PONA column, and the light sulfur gases are heart-cut to a GasPro column, where hydrogen sulfide is separated from other light sulfur gases and detected with a sulfur chemiluminescence detector. Heart-cutting is accomplished with the use of a Deans switch. Backflushing the columns after hydrogen sulfide detection eliminates any problems caused by high-boiling hydrocarbons in the samples. Dissolved hydrogen sulfide is quantified in 14 crude oil samples, and the results are shown in this work. The method is also applicable to the analysis of headspace hydrogen sulfide over crude oil samples. Gas hydrogen sulfide measurements are compared to liquid hydrogen sulfide measurements for the same sample set. The chromatographic system design is discussed, and chromatograms of representative gas and liquid measurements are shown. PMID:25311312

  5. Screening for key odorants in Moroccan green olives by gas chromatography-olfactometry/aroma extract dilution analysis.

    PubMed

    Iraqi, Rafika; Vermeulen, Catherine; Benzekri, Amale; Bouseta, Amina; Collin, Sonia

    2005-02-23

    "Spanish style" Moroccan green table olives were screened for potent odorants by gas chromatography-olfactometry/aroma extraction dilution analysis of a representative Likens-Nickerson extract. (Z)-3-Hexenal [flavor dilution factor (FD) = 256], (E,E)-2,4-decadienal (FD = 128), and (E,Z)-2,4-decadienal (FD = 64) were revealed to confer green and coriander/paraffin oil odors to both fruit and oil extracts, whereas guaiacol (FD = 128) imparted a bad olive, phenolic note. Methional (3-methylthiopropionaldehyde, FD = 128) and several terpenes (FD

  6. Characterization of Benthic Microbial Community Structure by High-Resolution Gas Chromatography of Fatty Acid Methyl Esters

    PubMed Central

    Bobbie, Ronald J.; White, David C.

    1980-01-01

    Fatty acids are a widely studied group of lipids of sufficient taxonomic diversity to be useful in defining microbial community structure. The extraordinary resolution of glass capillary gas-liquid chromatography can be utilized to separate and tentatively identify large numbers of fatty acid methyl esters derived from the lipids of estuarine detritus and marine benthic microbiota without the bias of selective methods requiring culture or recovery of the microbes. The gas-liquid chromatographic analyses are both reproducible and highly sensitive, and the recovery of fatty acids is quantitative. The analyses can be automated, and the diagnostic technique of mass spectral fragmentation analysis can be readily applied. Splitless injection on glass capillary gas chromatographic columns detected by mass spectral selective ion monitoring provides an ultrasensitive and definitive monitoring system. Reciprocal mixtures of bacteria and fungi, when extracted and analyzed, showed progressive changes of distinctive fatty acid methyl esters derived from the lipids. By manipulating the environment of an estuarine detrital microbial community with antibiotics and culture conditions, it was possible to produce a community greatly enriched in eucaryotic fungi, as evidenced by scanning electron microscopic morphology. The fatty acid methyl esters from the lipids in the fungus-enriched detritus showed enrichment of the C18 dienoic and the C18 and C20 polyenoic esters. Manipulation of the detrital microbiota that increased the procaryotic population resulted in an absence of large structures typical of fungal mycelia or diatoms, as evidenced by scanning electron microscopy, and a significantly larger proportion of anteiso- and isobranched C15 fatty acid esters, C17 cyclopropane fatty acid esters, and the cis-vaccenic isomer of the C18 monoenoic fatty acid esters. As determined by these techniques, a marine settling community showed greater differences in bacterial as contrasted to microeucaryotic populations when compared with the microbial communities of benthic cores. Images PMID:16345583

  7. Quantitative analysis in gas chromatography\\/low power atmospheric-pressure helium microwave-induced plasma atomic emission interferometry and ion cyclotron resonance mass spectroscopy

    Microsoft Academic Search

    Loo

    1990-01-01

    The development of experimental and data analysis techniques for quantitative analysis in gas chromatography\\/low power atmospheric pressure helium microwave-induced plasma atomic emission interferometry (GC\\/HeMIPAEI) and ion cyclotron resonance mass spectroscopy (ICR\\/MS) is presented. A discussion of interferometric data analysis by discrete and fast Fourier transform (DFT and FFT, respectively) is given. Additionally, the use of two techniques (the maximum entropy

  8. Enzyme recovery during gas/liquid two-phase flow microfiltration of enzyme/yeast mixtures.

    PubMed

    Mercier-Bonin, Muriel; Fonade, Christian

    2002-12-20

    The effect of a gas/liquid two-phase flow on the recovery of an enzyme was evaluated and compared with standard crossflow operation when confronted with the microfiltration of a high-fouling yeast suspension. Ceramic tubular and flat sheet membranes were used. At constant feed concentration (permeate recycling) and transmembrane pressure, the results obtained with the tubular membrane were dependent on the two-phase flow pattern. In comparison with single-phase flow performances at the same liquid velocity, the enzyme transmission was maintained at a high level with a bubble flow pattern but it decreased by 70% with a slug flow, whatever the flow rate ratio. Identical results were obtained with flat sheet membranes: for the highest flow rate ratio, the enzyme transmission was reduced by 70% even though the permeate flux was improved by 240%. During diafiltration experiments with the tubular membrane, it was found that a bubble flow pattern led to a 13% higher enzyme recovery compared to single-phase flow conditions, whereas with a slug flow the enzyme recovery was strongly reduced. With bubble flow conditions, energy consumption was minimal, confirming that this flow pattern was the most suitable for enzyme recovery. PMID:12378602

  9. Gas-Liquid Two-Phase Flows Through Packed Bed Reactors in Microgravity

    NASA Technical Reports Server (NTRS)

    Motil, Brian J.; Balakotaiah, Vemuri

    2001-01-01

    The simultaneous flow of gas and liquid through a fixed bed of particles occurs in many unit operations of interest to the designers of space-based as well as terrestrial equipment. Examples include separation columns, gas-liquid reactors, humidification, drying, extraction, and leaching. These operations are critical to a wide variety of industries such as petroleum, pharmaceutical, mining, biological, and chemical. NASA recognizes that similar operations will need to be performed in space and on planetary bodies such as Mars if we are to achieve our goals of human exploration and the development of space. The goal of this research is to understand how to apply our current understanding of two-phase fluid flow through fixed-bed reactors to zero- or partial-gravity environments. Previous experiments by NASA have shown that reactors designed to work on Earth do not necessarily function in a similar manner in space. Two experiments, the Water Processor Assembly and the Volatile Removal Assembly have encountered difficulties in predicting and controlling the distribution of the phases (a crucial element in the operation of this type of reactor) as well as the overall pressure drop.

  10. Gravity-induced density and concentration profiles in binary mixtures near gas-liquid critical lines

    NASA Astrophysics Data System (ADS)

    Chang, R. F.; Sengers, J. M. H. Levelt; Doiron, T.; Jones, J.

    1983-09-01

    We have calculated gravity-induced density and concentration gradients using scaled equations of state fashioned after that of Leung and Griffiths for binary mixtures near gas-liquid critical lines. The mixtures considered here are those of helium-3 and helium-4 and of carbon dioxide and ethane. Our calculations show that the density profiles for both mixtures in any proportion of the components are similar to those of pure fluids. The concentration gradients in the helium mixture have the same appearance as the density gradients. In the carbon dioxide-ethane system, however, the form of the concentration profile varies greatly, depending on the overall composition. Moreover, the temperature at which a mixture separates into two phases is slightly different from that expected for the mixture in the absence of gravity. We have also examined the case where a mixture is subjected to a large gravitational field such as can be generated in a centrifuge and found that, although the density gradient in all the mixtures is like that in pure fluids, the concentration gradients in the mixtures of carbon dioxide and ethane have complex features related to the presence of critical azeotropy.

  11. Generating Singlet Oxygen Bubbles: A New Mechanism for Gas-Liquid Oxidations in Water

    PubMed Central

    Bartusik, Dorota; Aebisher, David; Ghafari, BiBi

    2012-01-01

    Laser-coupled microphotoreactors were developed to bubble singlet oxygen [1O2 (1?g)] into an aqueous solution containing an oxidizable compound. The reactors consisted of custom-modified SMA fiber-optic receptacles loaded with 150-?m silicon phthalocyanine glass sensitizer particles, where the particles were isolated from direct contact with water by a membrane adhesively bonded to the bottom of each device. A tube fed O2 gas to the reactor chambers. In the presence of O2, singlet oxygen was generated by illuminating the sensitizer particles with 669-nm light from an optical fiber coupled to the top of the reactor. The generated 1O2 was transported through the membrane by the O2 stream and formed bubbles in solution. In solution, singlet oxygen reacted with probe compounds (either 9,10-anthracene dipropionate dianion, trans-2-methyl-2-pentanoate anion, N-benzoyl-D,L-methionine, and N-acetyl-D,L-methionine) to give oxidized products in two stages. The early stage was rapid and showed that 1O2 transfer occurred via bubbles mainly in the bulk water solution. The later stage was slow, it arose only from 1O2-probe molecule contact at the gas/liquid interface. A mechanism is proposed that involves 1O2 mass transfer and solvation, where smaller bubbles provide better penetration of 1O2 into the flowing stream due to higher surface-to-volume contact between the probe molecules and 1O2. PMID:22260325

  12. Effect of impeller geometry on gas-liquid mass transfer coefficients in filamentous suspensions

    SciTech Connect

    Dronawat, S.N.; Svihla, C.K.; Hanley, T.R. [Univ. of Louisville, KY (United States)

    1997-12-31

    Volumetric gas-liquid mass transfer coefficients were measured in suspensions of cellulose fibers with concentrations ranging from 0 to 20 g/L. The mass transfer coefficients were measured using the dynamic method. Results are presented for three different combinations of impellers at a variety of gassing rates and agitation speeds. Rheological properties of the cellulose fibers were also measured using the impeller viscometer method. Tests were conducted in a 20 L stirred-tank fermentor and in 65 L tank with a height to diameter ratio of 3:1. Power consumption was measured in both vessels. At low agitation rates, two Rushton turbines gave 20% better performance than the Rushton and hydrofoil combination and 40% better performance than the Rushton and propeller combination for oxygen transfer. At higher agitation rates, the Rushton and hydrofoil combination gave 14 and 25% better performance for oxygen transfer than two Rushton turbines and the Rushton and hydrofoil combination, respectively. 8 refs., 11 figs., 1 tab.

  13. Analysis of Camellia sinensis green and black teas via ultra high performance liquid chromatography assisted by liquid-liquid partition and two-dimensional liquid chromatography (size exclusion × reversed phase).

    PubMed

    Scoparo, Camila T; de Souza, Lauro M; Dartora, Nessana; Sassaki, Guilherme L; Gorin, Philip A J; Iacomini, Marcello

    2012-01-27

    Green and black teas (Camellia sinensis) contain compounds ranging from simple phenolics to complex glycosides, many of which have well-recognized health benefits. Here, we describe two methodologies aiming to achieve a comprehensive analysis of hydro-alcoholic extracts of C. sinensis. In the first step, the extracts were partitioned in water, n-butanol, ethyl acetate and chloroform to separate the compounds according to their polarity, yielding less complex samples to be analyzed by ultra high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS). Additionally, a comprehensive two dimensional liquid chromatography (2D-LC) technique, employing size exclusion chromatography (SEC) × reversed phase (BEH-C18) was developed. The following compounds were identified on the basis of retention time, UV-spectra and MS fragmentation patterns: catechins, theaflavins and their gallate derivatives; kaempferol, quercetin and myricetin mono-, di-, tri- and tetraglycosides; esters of quinic acid and gallic or hydroxycinnamic acids; purine alkaloids, such as caffeine and theobromine and many lipids. Additionally, there were many novel compounds that were previously undescribed, such as saponin isomers and gallic acid esters of four glycosides of myricetin, quercetin and kaempferol. PMID:22204932

  14. ANALYSIS OF HOUSTON AEROSOL SAMPLES BY GC/MS (GAS CHROMATOGRAPHY-MASS SPECTROMETRY) METHODS

    EPA Science Inventory

    An analysis procedure developed to give a qualitative and quantitative analysis for organic compounds adsorbed on aerosols collected by Hi-Vol filters was adapted and applied to a similar analysis of aerosols collected by dichotomous filters. Analysis was conducted for five dicho...

  15. Chromatographic fingerprinting analysis of Zhizhu Wan preparation by high-performance liquid chromatography coupled with photodiode array detector

    PubMed Central

    Sun, Hui; Chen, Xi; Zhang, Aihua; Sakurai, Tetsuro; Jiang, Jinzhong; Wang, Xijun

    2014-01-01

    Background: Traditional Chinese medicine (TCM) formula has been used for over 1000 years and most of them contain complicate chemical constituents. Chromatographic fingerprinting has been widely accepted as a crucial method for qualitative and quantitative analyses for TCM. Zhi Zhu Wan (ZZW), a classical Chinese medical formula, has been commonly used for the treatment of gastrointestinal disease, which pose a serious challenge to its quality control. Materials and Methods: In this work, a sensitive and reliable method of high-performance liquid chromatography coupled with photodiode array detector (HPLC-PDA) was developed to control the quality of ZZW for chemical fingerprint analysis and quantitative analysis of four major bioactive constituents, including hesperidin, naringin, neohesperidin, and atractylenolide I. The chromatographic separation was performed on a Waters Symmetry C18 column (4.6 mm × 250 mm, 5 ?m particle size), with an aqueous 0.095% phosphate acid and acetonitrile mobile phase gradient. Results: Optimization of other experimental conditions was validated with satisfactory accuracy, precision, repeatability, and recovery. In quantitative analysis, the four components showed good regression (R > 0.9994) within test ranges, and the recovery method ranged from 99.32% to 100.630%. HPLC fingerprints of the ZZW samples were compared by performing similarity analysis. Conclusion: The results indicated that the newly developed HPLC-PDA fingerprint method would be suitable for quality control of ZZW. PMID:25422548

  16. Closed tube sample introduction for gas chromatography–ion mobility spectrometry analysis of water contaminated with a chemical warfare agent surrogate compound

    Microsoft Academic Search

    Richard P. Erickson; Ashish Tripathi; Waleed M. Maswadeh; A. Peter Snyder; Philip A. Smith

    2006-01-01

    Ion mobility spectrometry (IMS) is a proven technology for detection of vapor phase chemical warfare agents. The technology is suitable for field portable instrumentation due to its small size, high sensitivity, speed of analysis, and low power consumption. However, it suffers from a limited dynamic range and potential difficulties in identifying compounds in complex matrices. The use of gas chromatography

  17. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection of analysis of agrochemical residues and mycotoxines in food - challenges and applications

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence o...

  18. Asia Pacific food analysis network (APFAN) training exercise: the determination of niacin in cereals by alkaline extraction and high performance liquid chromatography

    Microsoft Academic Search

    Suzy M Juraja; V. Craige Trenerry; Roderick G Millar; Pieter Scheelings; Donald R Buick

    2003-01-01

    Analysts from 20 laboratories, mainly from developing countries in the Asia Pacific Food Analysis Network (APFAN), were invited to participate in a training exercise for the determination of niacin (vitamin B3) in cereals using alkaline extraction and high performance liquid chromatography (HPLC) as the determinative step. The purpose of the study was to assist these laboratories in adopting a robust

  19. Analysis of commercial beverage products by size exclusion chromatography coupled with UV–vis absorbance detection and dynamic surface tension detection

    Microsoft Academic Search

    Karisa M. Pierce; Emilia Bramanti; Massimo Onor; Roberto Spiniello; Alexandra Kangas; Kristen J. Skogerboe; Robert E. Synovec

    2010-01-01

    Multidimensional analysis of instant coffee and barley beverage samples using size exclusion chromatography (SEC) combined with a dynamic surface tension detector (DSTD) and a UV–vis absorbance detector (UV) is reported. A unique finding of this study was the action of the tetrabutylammonium (TBA) cation as a modifying agent (with bromide as the counter anion) that substantially increased the surface pressure

  20. A Rapid Modified Method for Compositional Carbohydrate Analysis of Lignocellulosics by High pH AnionExchange Chromatography with Pulsed Amperometric Detection (HPAEC\\/PAD)

    Microsoft Academic Search

    Mark W. Davis

    1998-01-01

    During the last decade, high pH anion exchange chromatography with pulsed amperometric detection (HPAEC\\/PAC) has gained increasing acceptance as the method of choice for analysis of neutral sugars commonly occurring in woods, pulps, and other lignocellulosics. This paper describes modified chromatographic conditions and discusses other critical factors that improve the precision and efficiency of this application. The method involves a

  1. Developments in the analysis of petroleum hydrocarbons in oils, petroleum products and oil-spill-related environmental samples by gas chromatography

    Microsoft Academic Search

    Zhendi Wang; Merv Fingas

    1997-01-01

    This review gives a brief survey and comparison of chemical fingerprinting techniques by gas chromatography that are currently used for the characterization of petroleum hydrocarbons, the identification of oil spills and in assessing environmental impacts. This review focuses on new trends and developments in oil analysis methods.

  2. A NEW SW-846 METHOD FOR THE ANALYSIS OF TOXAPHENE AND TOXAPHENE CONGENERS IN SOLID AND AQUEOUS SAMPLES USING GAS CHROMATOGRAPHY / NEGATIVE ION MASS SPECTROMETRY

    EPA Science Inventory

    US EPA SW-846 methods have typically relied on dual column gas chromatography coupled with electron capture detection (GC-ECD) for analysis of low concentrations of organochlorine pesticides, including toxaphene, in environmental samples. Toxaphene is one of the most widely appl...

  3. Analysis of intact tetraether lipids in archaeal cell material and sediments by high performance liquid chromatography\\/atmospheric pressure chemical ionization mass spectrometry

    Microsoft Academic Search

    J. S. Sinninghe Damsté; E. C. Hopmans; S. Schouten; R. D. Pancost; M. T. J. van der Meer

    2000-01-01

    A method combining normal phase high performance liquid chromatography (HPLC) with positive ion atmospheric pressure chemical ionization mass spectrometry (APCI-MS) was developed for the analysis of intact glycerol dialkyl glycerol tetraethers (GDGTs) in archaeal cell material and sediments. All GDGTs previously reported to occur in the thermophilic archaeon Sulfolobus solfataricus could be identified based on their mass spectra and retention

  4. AUTOMATED GEL-PERMEATION SYSTEM FOR REMOVAL OF LIPIDS IN GAS CHROMATOGRAPHY/MASS SPECTROMETRIC ANALYSIS OF FATTY TISSUES FOR XENOBIOTIC CHEMICALS

    EPA Science Inventory

    The interference of natural lipids in gas chromatography/mass spectrometric analysis of xenobiotic chemicals in fatty tissue can be substantially reduced using gel-permeation chromatographic removal of the lipids. This paper presents an inexpensive controller which can be used wi...

  5. Optimization of separation and detection conditions for comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) are among the most toxic compounds known. The current predominant method of analysis is too expensive and cumbersome, and comprehensive gas chromatography coupled to time-of-flight mass spect...

  6. Evaluation of low-pressure gas chromatography-tandem mass spectrometry method for analysis of greater than 140 pesticides in fish

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A multi-residue method for analysis of 143 pesticide residues in fish was developed and evaluated using fast, low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with ace...

  7. Extraction and preconcentration of ?-blockers in human urine for analysis with high performance liquid chromatography by means of carrier-mediated liquid phase microextraction

    Microsoft Academic Search

    Li Zhang; Xiaoli Su; Chenggong Zhang; Li Ouyang; Qingji Xie; Ming Ma; Shouzhuo Yao

    2010-01-01

    A novel method was developed for the analysis of four ?-blockers, namely sotalol, carteolol, bisoprolol, and propranolol, in human urine by coupling carrier-mediated liquid phase microextraction (CM-LPME) to high performance liquid chromatography (HPLC). By adding an appropriate carrier in organic phase, simultaneous extraction and enrichment of hydrophilic (sotalol, carteolol, and bisoprolol) and hydrophobic (propranolol) drugs were achieved. High enrichment factors

  8. Visualization and void fraction measurement of gas-liquid two-phase flow in plate heat exchanger.

    PubMed

    Asano, H; Takenaka, N; Fujii, T; Maeda, N

    2004-10-01

    Adiabatic and boiling gas-liquid two-phase flows in a simulated plate heat exchanger with a single-ribbed channel were visualized by a thermal neutron radiography method. In the experiments under adiabatic condition, the air-water two-phase flows in an aluminum test section were visualized. In the boiling two-phase flow experiments, chlorofluorocarbon R141b was used as the working fluid. Two-dimensional distributions of void fraction were measured from visualized images via some image processing techniques. As a result, it was shown that both the phases tended to flow straight in the ribbed channel, and mixing of gas and liquid phases was weak. Moreover, when working fluids flew into the test section as a gas-liquid mixture, the phase distributions were strongly affected by a liquid pool at the test section inlet. PMID:15246421

  9. Study on Flow Characteristics and Initial Pressure in Gas-Liquid Two Phase Slug Flow on Long Distance Conduit Transportation

    NASA Astrophysics Data System (ADS)

    Yamada, Yasumasa; Endo, Shigekatsu; Ochiai, Minoru

    Conduit transportation of two-phase and three-phase flow is applied as one of the transportation methods. Slug flow is generated when gas-liquid is mixed simultaneously in a conduit. This flow can transport the solid and material with high viscosity. The feature of this slug flow is that it generates a high-speed intermittent turbulent flow and it is a complex current with a pressure fluctuation affected by flow energy loss. Therefore, it is expected to have applications in many engineering fields like processing of colony algae, collection of methane hydrate in sea bottom and the sterilization of ballast water in tankers that use ozone gas. In this paper, we examined the fluidity characteristics of slug flow, acceleration loss due to the liquid film and prediction of initial pressure was investigated for gas-liquid slug flow generation which is being considered for future use in long distance horizontal pipe where the compressibility of the gas became remarkable.

  10. CFD Simulation of Single-Phase and Two-Phase Flow in Gas-Liquid Cylindrical Cyclone Separators

    Microsoft Academic Search

    Ferhat M. Erdal; Siamack A. Shirazi; Ovadia Shoham; Gene E. Kouba

    The petroleum industry has shown interest in utilizing the Gas-Liquid Cylindrical Cyclone (GLCC) separator as an alternative to the vessel-type separator. Thus, it is important to d e- velop predictive tools for design and to improve the technology of the GLCC. Previous studies have resulted in mechanistic models capable of predicting the operational envelope for liquid carry-over. However, these models

  11. Modelling of Mass Transfer in Gas-Liquid Stirred Tanks Agitated by Rushton Turbine and CD6 Impeller

    Microsoft Academic Search

    J. Gimbun; C. D. Rielly; Z. K. Nagy

    A combined computational fluid dynamics (CFD) and population balance model (PBM) approach has been applied to simulate gas-liquid stirred tanks agitated by (i) a Rushton turbine and (ii) a CD-6 impeller, operating at aeration numbers from 0.017 to 0.038. The multiphase simulations were realised via an Eulerian-Eulerian two-fluid model and the drag coefficient of spherical and distorted bubbles was modelled

  12. Enhancement of gas–liquid mass transfer during the unsteady-state catalytic decomposition of ozone in water

    Microsoft Academic Search

    R. Rosal; A. Rodríguez; M. Zerhouni

    2006-01-01

    Unsteady mass transfer and kinetic experiments were conducted in a gas–liquid reactor to study the catalytic and non-catalytic decomposition of ozone in water. In the absence of catalyst, first-order decomposition constants and volumetric mass transfer coefficients were determined at temperatures between 20°C and 30°C. Catalytic runs were performed on fumed colloidal TiO2, which primary particles had an average diameter of

  13. Gas—liquid mass transfer in external-loop airlift columns with newtonian and non-newtonian fluids

    Microsoft Academic Search

    Yoshinori Kawase; Nanae Hashiguchi

    1996-01-01

    Gas—liquid mass transfer in external-loop airlift columns has been examined. The measurements have been carried out in two external-loop airlift columns and a bubble column with newtonian and non-newtonian fluids. The experimental results indicate that the volumetric mass transfer coefficient kLa decreases with increasing downcomer-to-riser cross-sectional area ratio and its dependence increases with non-newtonian flow behaviour or shear thinning.A theoretical

  14. Experimental study on desulfurization efficiency and gas–liquid mass transfer in a new liquid-screen desulfurization system

    Microsoft Academic Search

    Zhongwei Sun; Shengwei Wang; Qulan Zhou; Shi’en Hui

    2010-01-01

    This paper presents a new liquid-screen gas–liquid two-phase flow pattern with discarded carbide slag as the liquid sorbent of sulfur dioxide (SO2) in a wet flue gas desulfurization (WFGD) system. On the basis of experimental data, the correlations of the desulfurization efficiency with flue gas flow rate, slurry flow rate, pH value of slurry and liquid–gas ratio were investigated. A

  15. Gas-liquid flow in dividing Tee-junctions with a horizontal inlet and different branch orientations and diameters

    Microsoft Academic Search

    J. Reimann; H. J. Brinkmann; R. Domanski

    1988-01-01

    A data base summarizing experiments on the phase redistribution and pressure differences for a gas-liquid mixture flowing through the horizontal inlet pipe (diameter D1 = 50 mm) of a Tee-junction is presented. Branch to inlet diameter ratios of D3\\/D1 = 1; 0.52; 0.2; and 0.08 were investigated. The branch orientation was horizontal, vertical upward, or vertical downward. Mostly air-water experiments

  16. Gas\\/solid and gas\\/liquid partitioning of organic compounds: Critical evaluation of the interpretation of equilibrium constants

    Microsoft Academic Search

    Kai-Uwe Goss; René P. Schwarzenbach

    1998-01-01

    Gas\\/solid and gas\\/liquid partition processes are pivotal for the transport and residence time of organic pollutants in the atmosphere. Commonly, experimentally determined partition constants (K) between air and condensed phases (i.e., aerosols, rain, fog, snow, soils, plants) of a series of compounds are evaluated as a function of their liquid saturation vapor pressure p{sub L}°. Frequently, a linear free energy

  17. Enantiomeric analysis of polycyclic musks in water by chiral gas chromatography-tandem mass spectrometry.

    PubMed

    Wang, Lili; McDonald, James A; Khan, Stuart J

    2013-08-16

    Galaxolide (HHCB), tonalide (AHTN), phantolide (AHDI), traseolide (ATII) and cashmeran (DPMI) are synthetic polycyclic musks (PCMs). They are all commonly used in fragrance industries as racemic mixtures. A sensitive and robust enantioselective analytical method was developed to facilitate measurement of these chemicals in wastewater and environmental samples. The method is based on gas chromatography with tandem mass spectrometry (GC-MS/MS). Enantioseparation was assessed using four commercially available chiral capillary columns. Optimised resolution was achieved using a dual-column configuration of a chiral heptakis(2,3- di-O-methyl-6-O-t-butyl dimethylsilyl)-?-cyclodextrin column combined with a (non-chiral) HP-5MS column. This configuration was demonstrated to be capable of effectively resolving all commercially manufactured enantiomers of these five PCMs. Method detection limits for single enantiomers in drinking water and surface water range between 1.01 and 2.39ngL(-1). Full validation of the application of this method in these aqueous matrices is provided. PMID:23866122

  18. [Analysis of the preservative chlorphenesin in cosmetics by high performance liquid chromatography].

    PubMed

    Zhu, Huijuan; Zhang, Weiqiang; Yang, Yanwei; Zhu, Ying

    2014-01-01

    An analytical method was developed for the determination of the preservative of chlorphenesin in cosmetics by high performance liquid chromatography (HPLC). A C18 column (250 mm x 4.6 mm, 5 microm) and a photodiode array detector were used. The mobile phase was methanol-water (55:45, v/v) with a flow rate of 1.0 mL/min. The detection wavelength was set at 280 nm and the column temperature was 25 degrees C. The limit of detection was 3 ng. A good linear relationship was obtained between the peak area and the mass concentration of chlorphenesin in the range of 1 - 500 mg/L and the correlation coefficient was 1.000 0. The recoveries of chlorphenesin at different spiked levels were 99.0% - 103% with the relative standard deviations (RSD) < or = 1.2%. Interference test and sample test were also applied meanwhile and validation experiments were performed by three laboratories. The method is simple, sensitive, accurate, stable and suitable for the determination of chlorphenesin in cosmetics. PMID:24783875

  19. On-line solid-phase extraction for liquid chromatography-mass spectrometry analysis of pesticides.

    PubMed

    Lucci, Paolo; Núñez, Oscar

    2014-10-01

    Public concern about pesticides in food and water has increased dramatically in the last two decades. In order to guarantee consumers' health and safety, analytical methods that could provide fast and reliable answers without compromising accuracy and precision are required. Sample treatment is probably the most tedious and time-consuming step in many analytical procedures and, despite the significant advances in chromatographic separations and mass spectrometry techniques, sample treatment is still one of the most important parts of the analytical process for achieving good analytical results. Therefore, over the last years, considerable efforts have been made to simplify the stage and to develop fast, accurate, and robust methods that allow the determination of a wide range of pesticides without compromising the integrity of the extraction process. This review article intends to give a short overview of recently developed on-line solid-phase extraction, preconcentration, and clean-up procedures for the determination of pesticides in complex matrices by liquid chromatography-mass spectrometry techniques. PMID:25103367

  20. Analysis of isothiazolinones in environmental waters by gas chromatography-mass spectrometry.

    PubMed

    Rafoth, Astrid; Gabriel, Sabine; Sacher, Frank; Brauch, Heinz-Jürgen

    2007-09-14

    This paper describes an analytical method for the determination of five biocides of isothiazolinone type (2-methyl-3-isothiazolinone (MI), 5-chloro-2-methyl-3-isothiazolinone (CMI), 1,2-benzisothiazolinone (BIT), 2-octyl-3-isothiazolinone (OI), 4,5-dichloro-2-octyl-3-isothiazolinone (DCOI)) in environmental waters. The method is based on pre-concentration of the analytes by solid-phase extraction onto a mixture of a polymeric material and RP-C18 material and subsequent determination by gas chromatography-mass spectrometry (GC-MS). One of the target compounds (BIT) is derivatised with diazomethane after pre-concentration to improve its chromatographic performance. The method was optimised with respect to pre-concentration conditions (liquid-liquid extraction versus solid-phase extraction, solid-phase material, elution solvent and volume) and extensively validated. Applying the method to surface waters, groundwaters, and drinking waters, limits of detection between 0.01 and 0.1 microg/l could be achieved and the repeatability was below 10% for all compounds except for MI. Additional investigations showed that the stability of the isothiazolinones in environmental waters is limited and sample storage at 4 degrees C is mandatory to preserve the target biocides. First investigations of influents and effluents of a wastewater treatment plant showed that conventional wastewater treatment exhibits a high efficiency for removal of the isothiazolinones. In river waters, the target isothiazolinones could not be detected. PMID:17681349

  1. Analysis of environmental samples for explosives and explosives degradation products by liquid chromatography-mass spectrometry

    SciTech Connect

    Gates, P.M.; Furlong, E.T.; Lindley, C.E.; Burkhardt, M.R. [Geological Survey, Arvada, CO (United States). National Water Quality Lab.

    1994-12-31

    Nitroaromatic explosives and their degradation products are regulated water-soluble contaminants that may pose a hazard to human health and could be important water contaminants. The reliable identification of most explosives, in particular, the identification of degradation products, is a major shortcoming in most analytical methods. As an improvement, high-performance liquid chromatography (HPLC) (coupled to Thermospray) mass spectrometry was used to determine compound molecular weights, and tandem-mass spectrometry was applied to confirm molecular structure. Compounds were separated isocratically using methanol-water with an octadecylsilane HPLC column. The identities of known nitroaromatic explosives were confirmed by combined ultraviolet absorbance and negative ion mass spectra. For optimal detection of known compounds, selected ion monitoring mass spectrometry was used. Calibration curves fit quadratic models, with correlation coefficients typically exceeding 0.995 over two orders of magnitude. Instrument detection limits ranged from 2.5 to 10 nanograms per injection, resulting in method-detection limits from about 100 to 400 nanograms per liter for a typical water sample. Unknown analytes (indicated by optical spectra) were identified by full scan and tandem mass spectrometry experiments on sample extracts or isolated extract fractions. This combined ultraviolet-diode array mass spectrometric approach is a superior method for analyzing soil or water samples where known explosives and unknown degradation products might be present.

  2. Rapid analysis of caffeine in "smart drugs" and "energy drinks" by microemulsion electrokinetic chromatography (MEEKC).

    PubMed

    Liotta, Eloisa; Gottardo, Rossella; Seri, Catia; Rimondo, Claudia; Miksik, Ivan; Serpelloni, Giovanni; Tagliaro, Franco

    2012-07-10

    A novel method based on microemulsion electrokinetic chromatography (MEEKC) with diode array detection (DAD) for rapid determination of caffeine in commercial and clandestine stimulants, known as "energy drinks" and "smart drugs", is described. Separations were carried out in 50 cm × 50 ?m (ID) uncoated fused silica capillaries. The optimized buffer electrolyte was composed of 8.85 mM sodium tetraborate pH 9.5, SDS 3.3% (w/v), n-hexane 1.5% (v/v) and 1-butanol 6.6% (v/v). Separations were performed at a voltage of 20 kV. Sample injection conditions were 0.5 psi, 3 s. Diprofilline was used as internal standard. The determination of the analytes was based on the UV signal recorded at 275 nm, corresponding to the maximum wavelength of absorbance of caffeine, whereas peak identification and purity check was performed on the basis of the acquisition of UV radiation between 200 and 400 nm wavelengths. Under the described conditions, the separation of the compounds was achieved in 6 min without any interference from the matrix. Linearity was assessed within a caffeine concentration range from 5 to 100 ?g/mL. The intra-day and inter-day precision values were below 0.37% for migration times and below 9.86% for peak areas. The present MEEKC method was successfully applied to the direct determination of caffeine in smart drugs and energy drinks. PMID:22497701

  3. Quantitative Metabolome Analysis Based on Chromatographic Peak Reconstruction in Chemical Isotope Labeling Liquid Chromatography Mass Spectrometry.

    PubMed

    Huan, Tao; Li, Liang

    2015-07-21

    Generating precise and accurate quantitative information on metabolomic changes in comparative samples is important for metabolomics research where technical variations in the metabolomic data should be minimized in order to reveal biological changes. We report a method and software program, IsoMS-Quant, for extracting quantitative information from a metabolomic data set generated by chemical isotope labeling (CIL) liquid chromatography mass spectrometry (LC-MS). Unlike previous work of relying on mass spectral peak ratio of the highest intensity peak pair to measure relative quantity difference of a differentially labeled metabolite, this new program reconstructs the chromatographic peaks of the light- and heavy-labeled metabolite pair and then calculates the ratio of their peak areas to represent the relative concentration difference in two comparative samples. Using chromatographic peaks to perform relative quantification is shown to be more precise and accurate. IsoMS-Quant is integrated with IsoMS for picking peak pairs and Zero-fill for retrieving missing peak pairs in the initial peak pairs table generated by IsoMS to form a complete tool for processing CIL LC-MS data. This program can be freely downloaded from the www.MyCompoundID.org web site for noncommercial use. PMID:26086729

  4. Analysis of fatty alcohol derivatives with comprehensive two-dimensional liquid chromatography coupled with mass spectrometry.

    PubMed

    Elsner, Victoria; Laun, Sabrina; Melchior, David; Köhler, Michael; Schmitz, Oliver J

    2012-12-14

    A simultaneous separation of anionic (fatty alcohol sulfates, fatty alcohol ether sulfates), non-ionic (alkyl polyglucosides, fatty alcohol ethoxylates) and amphoteric (cocamidopropyl betaines) surfactants was performed by comprehensive two-dimensional liquid chromatography (LCxLC) utilizing a ZIC(®)-HILIC column in the first dimension, a Reprosphere 100 C8-Aqua column in the second dimension and a 10-port two position valve as the interface. The volume of the two sample loops were 25 or 50 ?L and allow a one or two minute modulation at a 25 ?L/min flow rate. In the first dimension, a gradient of acetonitrile and an ammonium acetate buffer was used to separate polyethoxylated surfactants by their degree of ethoxylation (EO number) whereas in the second dimension, a separation by alkyl chain was performed using a methanol/ammonium acetate buffer gradient. A baseline separation of the above mentioned surfactants according to both EO number and alkyl chain was achieved. The best performance was used to compare two different LCxLC-QTOF MS systems, which demonstrate that a transfer of the method from one system to a totally different system is possible. However, because of the differences in delay volume and extra-column volume between these systems the separation power is changed. PMID:23116798

  5. Analysis of reduced monoclonal antibodies using size exclusion chromatography coupled with mass spectrometry

    NASA Astrophysics Data System (ADS)

    Liu, Hongcheng; Gaza-Bulseco, Georgeen; Chumsae, Chris

    2009-12-01

    Size-exclusion chromatography (SEC) has been widely used to detect antibody aggregates, monomer, and fragments. SEC coupled to mass spectrometry has been reported to measure the molecular weights of antibody; antibody conjugates, and antibody light chain and heavy chain. In this study, separation of antibody light chain and heavy chain by SEC and direct coupling to a mass spectrometer was further studied. It was determined that employing mobile phases containing acetonitrile, trifluoroacetic acid, and formic acid allowed the separation of antibody light chain and heavy chain after reduction by SEC. In addition, this mobile phase allowed the coupling of SEC to a mass spectrometer to obtain a direct molecular weight measurement. The application of the SEC-MS method was demonstrated by the separation of the light chain and the heavy chain of multiple recombinant monoclonal antibodies. In addition, separation of a thioether linked light chain and heavy chain from the free light chain and the free heavy chain of a recombinant monoclonal antibody after reduction was also achieved. This optimized method provided a separation of antibody light chain and heavy chain based on size and allowed a direct measurement of molecular weights by mass spectrometry. In addition, this method may help to identify peaks eluting from SEC column directly.

  6. Analysis of tomato glycoalkaloids by liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    PubMed

    Cataldi, Tommaso R I; Lelario, Filomena; Bufo, Sabino A

    2005-01-01

    Steroidal glycoalkaloids (SGAs) extracted from tomato leaves and berries (Lycopersicon esculentum Mill.) were separated and identified using optimized reversed-phase liquid chromatography with electrospray ionization (ESI) and ion trap mass spectrometry (ITMS). The ESI source polarity and chromatographic conditions were evaluated. The ESI spectra contain valuable information, which includes the mass of SGAs, the mass of the aglycones, and several characteristic fragment ions. Cleavage at the interglycosidic bonds proximal to the aglycones is the most prominent process in the ESI process. A protonated molecule, [M+H]+, accompanied by a mixed adduct ion, [M+H+Na]2+, was observed for alpha-tomatine (i.e., m/z 1034.7 and 528.9) and dehydrotomatine (i.e., m/z 1032.6 and 527.9) in positive ion mode spectra. The structures of these tomato glycoalkaloids were confirmed using tandem mass spectrometry. The identification of a new alpha-tomatine isomer glycoalkaloid, named filotomatine (MW 1033), which shares a common tetrasaccharide structure (i.e., lycotretraose) with alpha-tomatine and dehydrotomatine, and soladulcidine as an aglycone, is described for the first time. It occurs in significant amounts in the extracts of wild tomato foliage. Multistage mass spectrometry both of the protonated molecules and of the doubly charged ions was used for detailed structural elucidation of SGAs. Key fragmentations and regularities in fragmentation pathways are described and the fragmentation mechanisms involved are proposed. PMID:16200652

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

    PubMed

    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 = 4.4%), precision (inter-day sigma(rel) < or = 8.13%, intra-day sigma(rel) < or = 4.32%), accuracy (recovery rates from 96.8 to 102.4%), sensitivity (limit of detection (LOD) < or = 4.5 microg mL(-1)) and linearity (R(2) > 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. PMID:18420051

  8. Forensic analysis of hallucinogenic mushrooms and khat (Catha edulis Forsk) using cation-exchange liquid chromatography.

    PubMed

    Laussmann, Tim; Meier-Giebing, Sigrid

    2010-02-25

    Hallucinogenic mushrooms (e.g. Psilocybe and Panaeolus species) as well as leaves and young shoots of the khat tree (Catha edulis Forsk) are illicit drugs in many countries. The exact concentration of the hallucinogenic alkaloids psilocin and psilocybin in mushrooms and the sympathomimetic alkaloids cathinone and cathine in khat is usually essential for jurisdiction. Facing an increasing number of mushroom and khat seizures by German customs authorities, a convenient comprehensive quantitative HPLC method based on cation-exchange liquid chromatography for these rather "exotic" drugs has been developed which avoids time-consuming multi-step sample preparation or chemical derivatization procedures. Using this method a number of different hallucinogenic fungi species and products that are mainly distributed via the internet have been analysed (dried and fresh Psilocybe cubensis Singer as well as P. cubensis collected from "grow boxes", Panaeolus cyanescens Berkeley and Broome and so-called "philosopher stones" (sclerotia of Psilocybe species)). Highest total amounts of psilocin have been detected in dried P. cyanescens reaching up to 3.00+/-0.24 mg per 100 mg. The distribution of khat alkaloids in different parts of the khat shoots has been studied. High concentrations of cathinone have not only been detected in leaves but also in green parts and barks of stalks. Additionally, the sample treatment for fresh mushroom and khat samples has been optimised. Highest amounts of alkaloids were found when fresh material was freeze-dried. PMID:20047807

  9. Magnetic solid phase extraction and gas chromatography-mass spectrometrical analysis of sixteen polycyclic aromatic hydrocarbons.

    PubMed

    Cai, Ying; Yan, Zhihong; NguyenVan, Manh; Wang, Lijia; Cai, Qingyun

    2015-08-01

    Fluorenyl functionalized superparamagnetic core/shell magnetic nanoparticles (MNPs, Fe3O4@SiO2@Flu) were prepared and characterized by transmission electron microscope, X-ray diffraction and infrared spectroscopy. The MNPs having an average diameter of 200nm were then used as solid-phase extraction sorbent for the determination of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in water samples designated by United States Environmental Protection Agency (U.S. EPA). The main influencing parameters, including sorbent amount, desorption solvent, sample volume and extraction time were optimized. Analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels. Limit of detection ranging from 0.5 to 4.0ng/L were obtained. The repeatability was investigated by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) lower than 13.1%. Finally, the proposed method was successfully applied for the determination of PAHs in water samples with the recoveries in the range of 96.0-106.7%. PMID:26122856

  10. Paper Chromatography

    NSDL National Science Digital Library

    Reeves, James H.

    2011-05-19

    This is a site with experiments that provide a brief introduction to the idea of separation of components in a mixture and a set of instructions for students for separating colored compounds by paper chromatography (on coffee filters). The appropriate audience would be students in a high-school or introductory, non major college chemistry class.

  11. Organic analysis by ion chromatography. 1. Determination of aromatic amines and aromatic diisocyanates by cation-exchange chromatography with amperometric detection.

    PubMed

    Zhu, Yan; Wang, Muhua; Du, Huangyong; Wang, Fang; Mou, Shifen; Haddad, Paul R

    2002-05-17

    A method has been developed for the simultaneous determination of a range of aromatic amines using cation-exchange chromatography performed on a standard ion chromatography column using d.c. amperometric detection. The analytes separated were 2,4- and 2,6-toluenediamine (2,4- and 2,6-TDA), aniline, o-toluidine, benzidine, p-chloroaniline, 4,4'-diaminodiphenyl (4,4'-DDP), m-nitroaniline and 1-naphthylamine. A Dionex CS12 column was used with gradient elution from an initial eluent of 5% CH3CN+35 mM H2SO4 to 27% CH3CN+35 mM H2SO4 (at 35 min). Detection limits in the range 2.6-22.6 microg/l were observed for all analytes except m-nitroaniline, for which the detection limit was 201 microg/l. Linear calibrations and good precision were observed and the method was applied to the determination of benzidine, p-chloroaniline and 1-naphthylamine in wastewater samples. Further, the separation was also used (after some modification of the eluent conditions) for the determination of 2,4- and 2,6-toluene diisocyanate (2,4- and 2,6-TDI) and 4,4'-methylenediphenyl diisocyanate (4,4'-MDI) after their hydrolysis to 2,4-TDA, 2,6-TDA and 4,4'-DDP. Detection limits for 2,6- and 2,4-TDI and 4,4'-MDI were 3.8, 8.2, and 11.2 microg/l, respectively. The method was applied to the determination of diisocyanates in air. PMID:12108653

  12. [Rapid analysis of 28 primary aromatic amines in aqueous food simulants by high performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Xiao, Xiaofeng; Wang, Jianling; Yang, Juanjuan; Liu, Tingfei; Chen, Tong; He, Jun; Deng, Hongyi; Gao, Qiyan

    2013-01-01

    A novel method for rapid analysis of the migration amounts of 28 primary aromatic amines (PAAs) in aqueous food simulants (10% ethanol, 30 g/L acetic acid and 20% ethanol aqueous solution) was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After the migration test, the soaking solution was cooled down from 100 degrees C, vortexed, filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe, and then the filtrate was analyzed by HPLC-MS/MS. A Zorbax SB-Phenyl column (250 mm x 4.6 mm, 5 microm) was selected for chromatography. The mobile phase consisted of water and 0.1% formic acid-25% acetonitrile-methanol solution with gradient elution. The 28 PAAs in aqueous food simulants were detected by tandem mass spectrometer operated in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The limits of quantification for the 28 PAAs were between 0.002 microg/L and 10 microg/L. The linearity of the method was good with correlation coefficients (r2) greater than 0.995 over the concentration range from 5 microg/L or 10 microg/L to 100 microg/L. The average recoveries of the 28 PAAs were between 76.6% and 114% with the relative standard deviations between 1.53% and 8.97% at the levels of 10, 20, and 40 microg/L. The method shows rapid pretreatment, the lower limits of quantification, good recoveries and accuracies, and meets the requirement of European Union (EU) No 10/2011 regulation for the specific migration of PAAs. The method has been applied to analyze the 28 PAAs in different aqueous food simulants from the migration test of 30 batches of food contact material samples exported to EU. PMID:23667988

  13. Analysis of the class composition of some residual oils and asphalts by HPLC (high performance liquid chromatography)

    SciTech Connect

    Changming, Z.; Aiying, L.; Yongji, L.; Zengmin, S. (Institute of Coal Chemistry, Shanxi (China))

    1989-04-01

    Characterization of heavy oil residues and pitches from petroleum and coal processing has grown increasingly important because of the need to sufficiently use products. These heavy oil products often contain many polycyclic aromatic hydrocarbons, saturated hydrocarbons, polar substances, etc. The specificity of heavy oil residues and pitches are inherently dependent upon the class composition of hydrocarbons present. Some methods were proposed for class composition analysis by high performance liquid chromatography (HPLC), in which aromatic hydrocarbons were only separated into 1 to 3 ring aromatics. However, multi-ring aromatic hydrocarbons higher than 3 rings frequently exist in heavy oil residues. So it is needed to further improve the existing HPLC method for class composition analysis and especially to develop aromatic ring distribution (ARD) analysis, to meet the requirement for further utilization of these heavy oil products. In this paper, a new ARD determination method has been developed applying normal phase HPLC. The class compositions of some heavy oils in China have been determined by the method established in the present paper.

  14. Chemical fingerprint and quantitative analysis of Salvia plebeia R.Br. by high-performance liquid chromatography.

    PubMed

    Jin, Xiao-feng; Lu, Yan-hua; Wei, Dong-zhi; Wang, Zheng-tao

    2008-09-10

    To control the quality of Salvia plebeia R.Br., a simple and reliable method of high-performance liquid chromatography coupled with photodiode array detector (HPLC-DAD) was developed both for fingerprint analysis and quantitative determination of seven bioactive compounds, namely caffeic acid, luteolin-7-glucoside, nepetin-7-glucoside, homoplantaginin, luteolin, nepetin and hispidulin. In fingerprint analysis, twelve peaks were selected as characteristic peaks. In quantitative analysis, seven compounds showed good regression (R2>0.9995) within test ranges and the recovery of the method was in the range of 91.7-103.2%. The content ranges (mg/g) of seven compounds in the collected samples of S. plebeia were 0.80-1.67 (hispidulin), 2.18-5.75 (homoplantaginin), 0.52-1.22 (nepetin), 1.56-3.48 (nepetin-7-glucoside), 0.12-0.24 (luteolin), 0.97-2.22 (luteolin-7-glucoside) and 0.21-0.44 (caffeic acid), respectively. From the results obtained, the content of homoplantaginin was the highest. In addition, luteolin and luteolin-7-glucoside were isolated for the first time from S. plebeia. PMID:18678457

  15. An accurate and reliable analysis of trimethylamine using thermal desorption and gas chromatography-time of flight mass spectrometry.

    PubMed

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2013-05-30

    Trimethylamine (TMA) is well-known for manifesting the odor of rotting fish and urine. The analysis of TMA in environmental samples generally suffers from low reproducibility and poor sensitivity. In this study, a technique for the quantitative analysis of gas phase TMA was developed using thermal desorption (TD)-gas chromatography (GC)-time of flight mass spectrometry (TOF-MS). This new approach yielded good linearity (R(2)=0.9930), precision (RSE=1.59%), and high sensitivity with the method detection limit (MDL) of 51 pg, i.e., detection of 0.021 ppb of TMA at 1L sample (limit of detection (LOD): 5.32 pg (0.002 ppb). This method was tested against gas samples collected from two representative sources of TMA: (1) rotten thornback fish and (2) cat urine-soaked clay. The concentration of TMA in these samples, when analyzed after treatment at varying dilution ratios, averaged 293±29.7 ppm (RSE=3.82%) and 74.1±5.78 ppb (RSE=3.19%), respectively. The feasibility of this approach, when tested with TD-GC-Quadruple (Q) MS, showed a good compatibility with moderately reduced sensitivity. The results of this study demonstrated that one can achieve highly reliable and reproducible analysis of TMA from environmental samples when using thermal desorption (for pretreatment) and detection (by the TOF or Q-MS system). PMID:23680550

  16. Combining membrane extraction with mobile gas chromatography for the field analysis of volatile organic compounds in contaminated waters.

    PubMed

    Hauser, B; Popp, P

    2001-02-01

    A mobile gas chromatographic device (Airmobtx HC 1000 monitor manufactured by Airmotec, Germany), originally designed for the analysis of benzene, toluene, ethylbenzene and xylenes (BTEX) in air, was connected to a flow cell for dynamic membrane extraction. Volatile organic compounds (VOCs) diffuse out of a water stream through a hollow fibre, are enriched onto sorption tubes integrated in the mobile device, and are then thermally desorbed and analysed by gas chromatography-flame ionisation detection. Battery operation of the device enables continuous on-site analysis of VOCs. Influences of the water flow-rate on system response and memory effects were investigated. The linear range of the method depends on the flow-rate of the water sample and did not exceed two orders of magnitude. The detection limits for trichloroethene, chlorobenzene and the BTEX compounds were found to be between 0.1 and 1.0 microg/l using a water flow-rate of 30 ml/min. Dynamic membrane extraction combined with the mobile gas chromatographic device was used for the on-site analysis of contaminated waters in the area of Leipzig. PMID:11218139

  17. [Matrix effects in analysis of three beta-agonist residues in pig edible tissues using gas chromatography-mass spectrometry].

    PubMed

    Bian, Kui; Lin, Tao; Liu, Min; Yang, Jianwen; Wang, Zongnan; He, Limin

    2014-02-01

    A gas chromatography-mass spectrometry (GC-MS) method was established for the determination of the residues of three beta-agonists (clenbuterol, salbutamol and ractopamine) in pig edible tissues. The matrix effects (MEs) in the analysis of the three compounds with the developed method were determined. The influences of matrix state and its weight on MEs were evaluated statistically. The analytes in pig liver and muscle and their corresponding freeze-dried powders were derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide. Then the derivatives were determined in selected ion monitoring mode and the intensities of MEs of the three beta-agonists were obtained. Significant matrix enhancement was observed for the three analytes, and especially, the ME of ractopamine was more than 1000%. The results of analysis of variance (ANOVA) demonstrated that MEs were significantly different for the three analytes in two matrices among different matrix weights (P < 0.05), and MEs of the three analytes increased from 1 g to 5 g with the increase of matrix weight. MEs for the three analytes were not significantly different between fresh pig tissues and its freeze-dried powder matrices (P > 0.05), indicating that the freeze-dried powder matrices might be used to conveniently prepare the matrix-matched calibration solution, which could efficiently compensate the MEs of the beta-agonists in GC-MS analysis. PMID:24822451

  18. Semi-automated liquid chromatography–mass spectrometric imaging platform for enhanced detection and improved data analysis of complex peptides?

    PubMed Central

    Zhang, Zichuan; Jiang, Shan; Li, Lingjun

    2013-01-01

    A semi-automated analytical platform featuring the coupling of monolithic reversed-phase liquid chromatography (RPLC) to matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI MSI) has been developed and evaluated. This is the first time that LC separation is readily coupled to MS imaging detection for the analysis of complex peptide mixtures both qualitatively and quantitatively. Methacrylate-based monolithic column with C12 functional groups is fabricated for fast RPLC separation. The LC flow and matrix flow are collected on a commercially available MALDI plate which is mechanically controlled and analyzed with MALDI MSI subsequently. Both tryptic peptides digested from bovine serum albumin (BSA) and endogenous neuropeptides extracted from the blue crab Callinectes sapidus are analyzed with this novel LC–MSI platform. Compared with regular offline LC fractionation coupled with MALDI MS detection, LC–MSI exhibits significantly increased MS signal intensity due to retaining of temporal resolution from separation dimension via continuous sampling, which results in increased number of peptides detected and accurate quantitation. In addition, imaging signals enable improved data analysis based on either mass-to-charge ratio or retention time, which is extremely beneficial for the analysis of complex analytes. These findings have demonstrated the potential of employing LC–MSI platform for enhanced proteomics and peptidomics studies. PMID:23623366

  19. Semi-automated liquid chromatography-mass spectrometric imaging platform for enhanced detection and improved data analysis of complex peptides.

    PubMed

    Zhang, Zichuan; Jiang, Shan; Li, Lingjun

    2013-06-01

    A semi-automated analytical platform featuring the coupling of monolithic reversed-phase liquid chromatography (RPLC) to matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI MSI) has been developed and evaluated. This is the first time that LC separation is readily coupled to MS imaging detection for the analysis of complex peptide mixtures both qualitatively and quantitatively. Methacrylate-based monolithic column with C12 functional groups is fabricated for fast RPLC separation. The LC flow and matrix flow are collected on a commercially available MALDI plate which is mechanically controlled and analyzed with MALDI MSI subsequently. Both tryptic peptides digested from bovine serum albumin (BSA) and endogenous neuropeptides extracted from the blue crab Callinectes sapidus are analyzed with this novel LC-MSI platform. Compared with regular offline LC fractionation coupled with MALDI MS detection, LC-MSI exhibits significantly increased MS signal intensity due to retaining of temporal resolution from separation dimension via continuous sampling, which results in increased number of peptides detected and accurate quantitation. In addition, imaging signals enable improved data analysis based on either mass-to-charge ratio or retention time, which is extremely beneficial for the analysis of complex analytes. These findings have demonstrated the potential of employing LC-MSI platform for enhanced proteomics and peptidomics studies. PMID:23623366

  20. Minimization of carryover for high-throughput liquid chromatography with tandem mass spectrometry analysis of 14 mycotoxins in corn grits.

    PubMed

    Tamura, Masayoshi; Matsumoto, Keiko; Watanabe, Jun; Iida, Junko; Nagatomi, Yasushi; Mochizuki, Naoki

    2014-07-01

    A method for the simultaneous analysis of 14 mycotoxins with the minimization of carryover was developed. Our verification experiments suggested that the carryover occurred due to the chelation of fumonisins with the metal. To wash the fumonisins from the metal, the inner surface of the injection needle was rinsed with 10 mM trisodium citrate and 1% formic acid in water/methanol/acetonitrile/isopropanol after each injection, and the analysis was performed on a metal-free Mastro C18 column. This approach remarkably minimized the carryover of fumonisins. Fourteen mycotoxins in samples were extracted with 2% acetic acid in water/acetonitrile and a quick, easy, cheap, effective, rugged, and safe extraction kit, purified on a MultiSep 229 Ochra, and then quantified by liquid chromatography with tandem mass spectrometry. Determinations performed using this method produced a linearity greater than 0.99 and recoveries ranging from 72.6 to 117.4%, with good intraday precision from 4.0 to 12.4%, and interday precision from 6.5 to 17.0%. The limits of detection ranged from 0.01 to 0.71 ?g/kg, demonstrating that a highly sensitive method for the simultaneous analysis of mycotoxins over a wide range of concentrations was achieved with minimal carryover. When 12 samples of commercially available corn grits were analyzed with this method, deoxynivalenol, fumonisin B1, fumonisin B2, fumonisin B3, and zearalenone were present most frequently. PMID:24723378

  1. Chiral nano-liquid chromatography-mass spectrometry applied to amino acids analysis for orange juice profiling.

    PubMed

    D'Orazio, Giovanni; Cifuentes, Alejandro; Fanali, Salvatore

    2008-06-01

    Determination of amino acid enantiomers is a very important topic in food analysis, since the presence of d-isomers may indicate, e.g., adulteration, microbiological contamination, uncontrolled fermentation processes, etc. In fact, the d- and l-enantiomers contents can be a useful marker for several elements such as quality control, contamination detection, processing monitoring, etc. Here we studied the potentiality of nano-liquid chromatography (nano-LC) coupled with mass spectrometry for the enantiomeric separation of several d- and l-amino acids that can be found in food products. Analytes were derivatized with fluorescein isothiocyanate (FITC). The mixture was injected and compounds focused on a C18 cartridge, then nano-LC analysis was carried out in a capillary column (75?m i.d.) packed with vancomycin-modified silica-diol particles. The effect of some experimental parameters, such as pH and buffer concentration on enantioresolution and retention factors, was studied for method optimization. The chromatographic separation system was coupled with an ion-trap mass spectrometer through a nano spray interface. It provided a final evaluation on analytes detected in all investigated samples with LOD values as low as 8ng/mL. That method was applied to the comparative analysis of two different orange juice samples (fresh natural vs. commercial one). Obtained profiles confirmed expected high quality standards. In fact, they mainly contained l-amino acids forms and not their antipodes. PMID:26065779

  2. Direct and comprehensive analysis of ginsenosides and diterpene alkaloids in Shenfu injection by combinatory liquid chromatography-mass spectrometric techniques.

    PubMed

    Yang, Hua; Liu, Lei; Gao, Wen; Liu, Ke; Qi, Lian-Wen; Li, Ping

    2014-04-01

    Shenfu injection (SFI) is a widely used Chinese herbal formulation for cardiac diseases prepared from red ginseng and processed aconite root. Clinical observations and pharmacological effects on SFI have been well investigated. Chemical analysis and quality control studies of this formulation, however, are relatively limited, especially regarding toxic aconite alkaloids. In this work, a high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS) method was applied to comprehensive analysis of constituents in SFI. Highly sensitive MS allows direct analysis of injections without additional sample pretreatment required. Using diagnostic ions and fragmentation rules, we identified 23 trace diterpene alkaloids, nineteen ginseng saponins, one panaxytriol, and one 5-hydroxymethylfurfural in SFI. A LC-MS method with selected ion monitoring was then used to quantify 24 major alkaloids and ginsenosides. The method was validated in terms of linearity, accuracy and precision. Especially, the limits of quantification were low to 0.4-18ng/mL for diterpene alkaloids. The total concentrations of saponins and alkaloids were about 676-742?g/mL and 3-7?g/mL in five batches of SFI samples, respectively. Finally, cosine ratio and euclidean distance were introduced to evaluate the batch-to-batch reproducibility of SFI samples, and the results demonstrated high quality consistency. Global identification and quantification of complex constituents based on LC-MS promises wide applications in quality control and batch monitoring for herbal products. PMID:24469096

  3. LIQUID AND GAS CHROMATOGRAPHIC ANALYSIS OF DIETHYL PHTHALATE IN WATER AND SEDIMENT

    EPA Science Inventory

    Diethyl phthalate was determined in water and sediment by high performance liquid chromatography (HPLC) and in water by gas-liquid chromatography with electron capture detection (GLC-ECD). Water samples were extracted with hexane, using a high-speed homogenizer-ultrasonic apparat...

  4. Analysis of paralytic shellfish toxins using high-field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry.

    PubMed

    Beach, Daniel G; Melanson, Jeremy E; Purves, Randy W

    2015-03-01

    The analysis of paralytic shellfish toxins (PSTs) by liquid chromatography-mass spectrometry remains a challenge because of their high polarity, large number of analogues and the complex matrix in which they occur. Here we investigate the potential utility of high-field asymmetric waveform ion mobility spectrometry (FAIMS) as a gas-phase ion separation tool for analysis of PSTs by mass spectrometry. We investigate the separation of PSTs using FAIMS with two divergent goals: using FAIMS as a primary separation tool for rapid screening by electrospray ionization (ESI)-FAIMS-MS or combined with LC in a multidimensional LC-ESI-FAIMS-MS separation. First, a survey of the parameters that affect the sensitivity and selectivity of PST analysis by FAIMS was carried out using ESI-FAIMS-MS. In particular, the use of acetonitrile as a gas additive in the carrier gas flow offered good separation of all PST epimeric pairs. A second set of FAIMS conditions was also identified, which focussed PSTs to a relatively narrow CV range allowing development of an LC-ESI-FAIMS-MS method for analysis of PST toxins in complex mussel tissue extracts. The quantitative capabilities of this method were evaluated by analysing a PST containing mussel tissue matrix material. Results compared favourably with analysis by an established LC-post-column oxidation-fluorescence method with recoveries ranging from 70 to 106%, although sensitivity was somewhat reduced. The current work represents the first successful separation of PST isomers using ion mobility and shows the promise of FAIMS as a tool for analysis of algal biotoxins in complex samples and outlines some critical requirements for its future improvement. PMID:25619987

  5. Analysis of gibberellins as free acids by ultra performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Urbanová, Terezie; Tarkowská, Danuše; Novák, Ond?ej; Hedden, Peter; Strnad, Miroslav

    2013-08-15

    A robust, reliable and high-throughput method for extraction and purification of gibberellins (GAs), a group of tetracyclic diterpenoid carboxylic acids that include endogenous growth hormones, from plant material was developed. The procedure consists of two solid-phase extraction steps (Oasis(®) MCX-HLB and Oasis(®) MAX) and gives selective enrichment and efficient clean-up of these compounds from complex plant extracts. The method was tested with plant extracts of Brassica napus and Arabidopsis thaliana, from which total recovery of internal standards of about 72% was achieved. A rapid baseline chromatographic separation of 20 non-derivatised GAs by ultra performance liquid chromatography is also presented where a reversed-phase chromatographic column Acquity CSH(®) and a mobile phase consisting of methanol and aqueous 10mM-ammonium formate is used. This method enables sensitive and precise quantitation of GAs by MS/MS in multiple-reaction monitoring mode (MRM) by a standard isotope dilution method. Optimal conditions, including final flow rate, desolvation temperature, desolvation gas flow, capillary and cone voltage for effective ionisation in the electrospray ion source were found. All studied GAs were determined as free acids giving dominant quasi-molecular ions of [M-H](-) with limits of detection ranging between 0.08 and 10 fmol and linear ranges over four orders of magnitude. Taking advantage of highly effective chromatographic separation of 20 GAs and very sensitive mass spectrometric detection, the presented bioanalytical method serves as a useful tool for plant biologists studying the physiological roles of these hormones in plant development. PMID:23708542

  6. [Analysis of piperidinium ionic liquid cations by ion chromatography with direct conductivity detection].

    PubMed

    Zhang, Renqing; Yu, Hong; Liu, Yuzhen

    2012-07-01

    A method of ion chromatography with direct conductivity detection was established to determine three piperidinium ionic liquid cations, i. e. N-methyl, ethyl piperidinium cation ([MEPi]+), N-methyl, propyl piperidinium cation ([MPPi]+) and N-methyl, butyl piperidinium cation ([MBPi]+). The effects of eluent types, eluent concentration and column temperature on the retention of the cations were investigated with sulfonic acid base cation exchange column using ethylenediamine-citric acid-acetonitrile as eluent. The results indicated that, with the increase of column temperature, the retention times of piperidinium cations were reduced, so the retention process of piperidinium cations was exothermic. The retentions of piperidinium cation homologue accorded with carbon number rule. The successful separation of the three piperidinium cations within 7 min was achieved using the optimized eluent of 0.2 mmol/L ethylenediamine-0.3 mmol/L citric acid-3% acetonitrile (pH 4.4) at a flow rate of 1.0 mL/min and the column temperature of 30 degrees C. Under these conditions, the detection limits at a signal-to-noise ratio of 3 for [MEPi]+, [MPPi] and [MBPi]+ were 0.14, 0.20 and 0.56 mg/L, respec-tively. The relative standard deviations (n = 5) for peak areas were less than 1.2%. The method has been applied to the determination of piperidinium ionic liquids synthesized in chemical laboratory with the spiked recoveries of 97.6% to 105.1%. The method is accurate, reliable, rapid, and has better practicability. PMID:23189670

  7. Combined liquid chromatography-tandem mass spectrometry analysis of progesterone metabolites.

    PubMed

    Sinreih, Maša; Zukunft, Sven; Sosi?, Izidor; Cesar, Jožko; Gobec, Stanislav; Adamski, Jerzy; Lanišnik Rižner, Tea

    2015-01-01

    Progesterone has a number of important functions throughout the human body. While the roles of progesterone are well known, the possible actions and implications of progesterone metabolites in different tissues remain to be determined. There is a growing body of evidence that these metabolites are not inactive, but can have significant biological effects, as anesthetics, anxiolytics and anticonvulsants. Furthermore, they can facilitate synthesis of myelin components in the peripheral nervous system, have effects on human pregnancy and onset of labour, and have a neuroprotective role. For a better understanding of the functions of progesterone metabolites, improved analytical methods are essential. We have developed a combined liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for detection and quantification of progesterone and 16 progesterone metabolites that has femtomolar sensitivity and good reproducibility in a single chromatographic run. MS/MS analyses were performed in positive mode and under constant electrospray ionization conditions. To increase the sensitivity, all of the transitions were recorded using the Scheduled MRM algorithm. This LC-MS/MS method requires small sample volumes and minimal sample preparation, and there is no need for derivatization. Here, we show the application of this method for evaluation of progesterone metabolism in the HES endometrial cell line. In HES cells, the metabolism of progesterone proceeds mainly to (20S)-20-hydroxy-pregn-4-ene-3-one, (20S)-20-hydroxy-5?-pregnane-3-one and (20S)-5?-pregnane-3?,20-diol. The investigation of possible biological effects of these metabolites on the endometrium is currently undergoing. PMID:25680188

  8. Combined Liquid Chromatography–Tandem Mass Spectrometry Analysis of Progesterone Metabolites

    PubMed Central

    Sinreih, Maša; Zukunft, Sven; Sosi?, Izidor; Cesar, Jožko; Gobec, Stanislav; Adamski, Jerzy; Lanišnik Rižner, Tea

    2015-01-01

    Progesterone has a number of important functions throughout the human body. While the roles of progesterone are well known, the possible actions and implications of progesterone metabolites in different tissues remain to be determined. There is a growing body of evidence that these metabolites are not inactive, but can have significant biological effects, as anesthetics, anxiolytics and anticonvulsants. Furthermore, they can facilitate synthesis of myelin components in the peripheral nervous system, have effects on human pregnancy and onset of labour, and have a neuroprotective role. For a better understanding of the functions of progesterone metabolites, improved analytical methods are essential. We have developed a combined liquid chromatography—tandem mass spectrometry (LC-MS/MS) method for detection and quantification of progesterone and 16 progesterone metabolites that has femtomolar sensitivity and good reproducibility in a single chromatographic run. MS/MS analyses were performed in positive mode and under constant electrospray ionization conditions. To increase the sensitivity, all of the transitions were recorded using the Scheduled MRM algorithm. This LC-MS/MS method requires small sample volumes and minimal sample preparation, and there is no need for derivatization. Here, we show the application of this method for evaluation of progesterone metabolism in the HES endometrial cell line. In HES cells, the metabolism of progesterone proceeds mainly to (20S)-20-hydroxy-pregn-4-ene-3-one, (20S)-20-hydroxy-5?-pregnane-3-one and (20S)-5?-pregnane-3?,20-diol. The investigation of possible biological effects of these metabolites on the endometrium is currently undergoing. PMID:25680188

  9. The off-line combination of high performance liquid chromatography and comprehensive two-dimensional gas chromatography-mass spectrometry: a powerful approach for highly detailed essential oil analysis.

    PubMed

    Tranchida, Peter Q; Zoccali, Mariosimone; Bonaccorsi, Ivana; Dugo, Paola; Mondello, Luigi; Dugo, Giovanni

    2013-08-30

    The present contribution is focused on the off-line combination of high performance liquid chromatography (HPLC) and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GC×GC-quadMS), and its application to the detailed qualitative analysis of essential oils. Specifically, a silica column was exploited for the separation of the essential oil constituents in two groups, namely hydrocarbon and oxygenated compounds. After, each HPLC-fraction was reduced in volume, and then subjected to cryogenically modulated GC×GC-quadMS analysis. The volatiles were separated on a normal-phase GC×GC column set, and identified through database matching and linear retention index information. The concentrated HPLC fractions gave origin to unexpectably crowded chromatograms, due to two fundamental GC×GC characteristics, namely the enhanced separation power and sensitivity. The results attained were particularly stimulating with regards to the oxygenated compounds, namely those constituents which contribute most to the essential oil aroma, and are of more use for the evaluation of quality and genuineness. Two genuine Citrus essential oils, bergamot and sweet orange, were subjected to analysis, and compared to applications carried out with a GC-quadMS instrument. PMID:23890548

  10. Differentiating organically and conventionally grown oregano using ultraperformance liquid chromatography mass spectrometry (UPLC-MS), headspace gas chromatography with flame ionization detection (headspace-GC-FID), and flow injection mass spectrum (FIMS) fingerprints combined with multivariate data analysis.

    PubMed

    Gao, Boyan; Qin, Fang; Ding, Tingting; Chen, Yineng; Lu, Weiying; Yu, Liangli Lucy

    2014-08-13

    Ultraperformance liquid chromatography mass spectrometry (UPLC-MS), flow injection mass spectrometry (FIMS), and headspace gas chromatography (headspace-GC) combined with multivariate data analysis techniques were examined and compared in differentiating organically grown oregano from that grown conventionally. It is the first time that headspace-GC fingerprinting technology is reported in differentiating organically and conventionally grown spice samples. The results also indicated that UPLC-MS, FIMS, and headspace-GC-FID fingerprints with OPLS-DA were able to effectively distinguish oreganos under different growing conditions, whereas with PCA, only FIMS fingerprint could differentiate the organically and conventionally grown oregano samples. UPLC fingerprinting provided detailed information about the chemical composition of oregano with a longer analysis time, whereas FIMS finished a sample analysis within 1 min. On the other hand, headspace GC-FID fingerprinting required no sample pretreatment, suggesting its potential as a high-throughput method in distinguishing organically and conventionally grown oregano samples. In addition, chemical components in oregano were identified by their molecular weight using QTOF-MS and headspace-GC-MS. PMID:25050447

  11. Development and validation of a fast high pressure liquid chromatography method for the analysis of lignocellulosic biomass hydrolysis and fermentation products

    Microsoft Academic Search

    Christopher J. Scarlata; Deborah A. Hyman

    2010-01-01

    A simple, precise, and accurate 10-min high pressure liquid chromatography (HPLC) method was developed and validated for the analysis of organic acids, alcohols, and furans from processing biomass into renewable fuels. The method uses an H+ form cation-exchange resin stationary phase that has a five-fold shorter analysis time versus that in the traditional method. The new method was used for

  12. Analysis of video images used to study gas-liquid transfer

    E-print Network

    Ferreira, Márcia M. C.

    , this array can be analyzed using PCA (performed by first unfolding the three-way array) or PARAFAC in vertical bands mostly at the left-hand-side of the tank. dummy Component 1 describes the flux of CO2 from

  13. Green methodology based on dispersive liquid-liquid microextraction and micellar electrokinetic chromatography for 5-nitroimidazole analysis in water samples.

    PubMed

    Hernández-Mesa, Maykel; Cruces-Blanco, Carmen; García-Campaña, Ana M

    2013-09-01

    Dispersive liquid-liquid microextraction has been proposed as an extraction technique combined with micellar electrokinetic chromatography (MEKC) for the analysis of eight 5-nitroimidazole compounds, including some metabolites, in water samples. Determination has been carried out using a diode array detector, employing 20 mM sodium phosphate and 150 mM SDS as separation buffer. Separation has taken place under a voltage of 25 kV and a temperature of 20°C. Samples were prepared in a buffer without micelles and they were hydrodynamically injected at 50 mbar for 25 s, producing a sweeping effect on the analytes for increasing sensitivity. Different factors involved in the dispersive liquid-liquid microextraction procedure were optimized, such as sample pH, nature, and volume of extraction and dispersive solvents in the mixture, percentage of NaCl added to sample and shaking time after the injection of the extraction and dispersive solvents. The method was characterized for water samples, achieving detection limits lower than 2.4 ?g/L. Trueness was checked in river, tap, and bottled water. Dispersive liquid-liquid microextraction combined with MEKC constitutes an easy, cheap, and green alternative for 5-nitroimidazole analysis in environmental water samples. PMID:23857677

  14. Bottom-up low molecular weight heparin analysis using liquid chromatography-Fourier transform mass spectrometry for extensive characterization.

    PubMed

    Li, Guoyun; Steppich, Julia; Wang, Zhenyu; Sun, Yi; Xue, Changhu; Linhardt, Robert J; Li, Lingyun

    2014-07-01

    Low molecular weight heparins (LMWHs) are heterogeneous, polydisperse, and highly negatively charged mixtures of glycosaminoglycan chains prescribed as anticoagulants. The detailed characterization of LMWH is important for the drug quality assurance and for new drug research and development. In this study, online hydrophilic interaction chromatography (HILIC) Fourier transform mass spectrometry (FTMS) was applied to analyze the oligosaccharide fragments of LMWHs generated by heparin lyase II digestion. More than 40 oligosaccharide fragments of LMWH were quantified and used to compare LMWHs prepared by three different manufacturers. The quantified fragment structures included unsaturated disaccharides/oligosaccharides arising from the prominent repeating units of these LMWHs, 3-O-sulfo containing tetrasaccharides arising from their antithrombin III binding sites, 1,6-anhydro ring-containing oligosaccharides formed during their manufacture, saturated uronic acid oligosaccharides coming from some chain nonreducing ends, and oxidized linkage region oligosaccharides coming from some chain reducing ends. This bottom-up approach provides rich detailed structural analysis and quantitative information with high accuracy and reproducibility. When combined with the top-down approach, HILIC LC-FTMS based analysis should be suitable for the advanced quality control and quality assurance in LMWH production. PMID:24905078

  15. Highly sensitive analysis of flavonoids by zwitterionic microemulsion electrokinetic chromatography coupled with light-emitting diode-induced fluorescence detection.

    PubMed

    Cao, Wan; Hu, Shuai-Shuai; Li, Xing-Ying; Pang, Xiao-Qing; Cao, Jun; Ye, Li-Hong; Dai, Han-Bin; Liu, Xiao-Juan; Da, Jian-Hua; Chu, Chu

    2014-09-01

    A rapid zwitterionic microemulsion electrokinetic chromatography (ZI-MEEKC) approach coupled with light-emitting-diode-induced fluorescence (LED-IF, 480nm) detection was proposed for the analysis of flavonoids. In the optimization process, we systematically investigated the separation conditions, including the surfactants, cosurfactants, pH, buffers and fluorescence parameters. It was found that the baseline separation of the seven flavonoids was obtained in less than 5min with a running buffer consisting of 92.9% (v/v) 5mM sodium borate, 0.6% (w/v) ZI surfactant, 0.5% (w/v) ethyl acetate and 6.0% (w/v) 1-butanol. High sensitivity was obtained by the application of LED-IF detection. The limits of detection for seven flavonoids were in the range of 3.30×10(-8) to 2.15×10(-6)molL(-1) without derivatization. Ultimately, the detection method was successfully applied to the analysis of flavonoids in hawthorn plant and food products with satisfactory results. PMID:25047822

  16. A NEW METHOD OF PEAK DETECTION FOR ANALYSIS OF COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY MASS SPECTROMETRY DATA.

    PubMed

    Kim, Seongho; Ouyang, Ming; Jeong, Jaesik; Shen, Changyu; Zhang, Xiang

    2014-06-01

    We develop a novel peak detection algorithm for the analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) data using normal-exponential-Bernoulli (NEB) and mixture probability models. The algorithm first performs baseline correction and denoising simultaneously using the NEB model, which also defines peak regions. Peaks are then picked using a mixture of probability distribution to deal with the co-eluting peaks. Peak merging is further carried out based on the mass spectral similarities among the peaks within the same peak group. The algorithm is evaluated using experimental data to study the effect of different cut-offs of the conditional Bayes factors and the effect of different mixture models including Poisson, truncated Gaussian, Gaussian, Gamma, and exponentially modified Gaussian (EMG) distributions, and the optimal version is introduced using a trial-and-error approach. We then compare the new algorithm with two existing algorithms in terms of compound identification. Data analysis shows that the developed algorithm can detect the peaks with lower false discovery rates than the existing algorithms, and a less complicated peak picking model is a promising alternative to the more complicated and widely used EMG mixture models. PMID:25264474

  17. Improved high sensitivity analysis of polyphenols and their metabolites by nano-liquid chromatography-mass spectrometry.

    PubMed

    Wilson, Landon; Arabshahi, Ali; Simons, Brigitte; Prasain, Jeevan K; Barnes, Stephen

    2014-10-01

    This study was conducted to assess the value of a high resolution, high mass accuracy time-of-flight analyzer in combination with nanoliquid chromatography for the analysis of polyphenols and their metabolites. The goal was to create a method that utilizes small volumes of biological fluids and provides a significant improvement in sensitivity compared with existing methods. Accordingly, nanoLC-MS and nanoLC-pseudo-multiple reaction monitoring (MRM) methods were developed that had a lower limit of quantification of 0.5 nM for several polyphenols and were linear over 2-3 orders of magnitude (R(2)>0.999). Using urine samples, the ability to observe and quantify polyphenols in such a complex biological fluid depended on much narrower mass windows (0.050 amu or less) on a TOF analyzer than those used on a quadrupole analyzer (0.7 amu). Although a greater selectivity was possible with the low mass resolution of a triple quadrupole instrument using the MRM approach, for the daidzein metabolite O-DMA, a chromatographically resolvable second peak could only be substantially reduced by using a 0.01 amu mass window. The advantage of a TOF analyzer for product ion data is that the whole MSMS spectrum is collected at high mass accuracy and MRM experiments are conducted in silico after the analysis. PMID:24967696

  18. Fast volatile organic compound recovery from soil standards for analysis by thermal desorption gas chromatography.

    PubMed

    Meniconi, Maria de Fátima Guadalupe; Parris, R; Thomas, C L P

    2003-10-01

    The development of high-throughput environmental screening assays are needed to meet high-specification data quality objectives (DQOs) that require large numbers of samples to be taken and analysed rapidly. The acquisition and stabilisation of the sample is a key technical and operational challenge in analytical sequences associated with the determination of volatile organic compound (VOC) contamination of soils. Further the development of miniaturised and embedded analytical systems for environmental conditioning monitoring requires the development of new sampling techniques. A proof-of-concept study is described that shows how pressurised gas, in this case carbon dioxide, may be used to recover reversibly-bound VOCs from soil into an adsorbent sampler, and then analysed by thermal desorption-gas chromatography. The effects of the volume of the pressurised gas, the gas flow rate and the mass of the soil sample on the recovery efficiency and breakthrough from the adsorbent trap were investigated in a preliminary characterisation study. Two distinct approaches were identified. The first involved ventilation of the voids within the soil matrix to displace the soil-gas headspace, a rapid screening approach. The second involved a more prolonged purge of the matrix to strip reversibly bound species into the gas phase and hence pass them into the adsorbent trap, a purge and trap approach. The shortest possible sample processing time required to yield analytically useful responses was 5 s with the use of the headspace approach. In this case n-octane, benzene and toluene were recovered from conditioned spiked soil samples at concentrations in the range 42 to 1690 mg kg(-1). The limit of detection for the system was estimated to be no greater than 1.2 mg kg(-1). Using the purge and trap variant enabled recovery efficiencies greater than 93% to be achieved with liquid spikes of n-octane onto soil samples. These preliminary studies showed that a system based on this approach would need to balance recovery efficiency, time and analyte breakthrough from the adsorbent trap. PMID:14667158

  19. Recent advances in forensic drug analysis by DART-MS.

    PubMed

    Lesiak, Ashton D; Shepard, Jason Re

    2014-03-01

    Mass spectrometry methods play a major role in many forensic applications. While gas chromatography-mass spectrometry methods are commonly used in crime laboratories and enforcement agencies, a variety of advanced techniques are now available that can improve upon standard methods and address emerging issues in forensic science. New mass spectrometry technologies include more versatile ionization sources, allowing the next generation of instrumentation to be more multipurpose and adaptable to the needs of the discipline. Direct analysis in real-time mass spectrometry is an ambient ionization method that allows direct testing of gas, liquid and solid samples without the need for any preparation or extraction, based on thermal desorption and ionization directly from the sample surface. This Review will provide an in-depth description of direct analysis in real-time time-of-flight mass spectrometry as applied to samples relevant to forensic science, with a focus on analysis and characterization related to forensic drug chemistry. PMID:24702113

  20. Chromatography Lab

    NSDL National Science Digital Library

    2014-09-18

    To increase students' awareness of possible invisible pollutants in drinking water sources, students perform an exciting lab requiring them to think about how solutions and mixtures exist even in unsuspecting places such as ink. They use alcohol and chromatography paper to separate the components of black and colored marker ink. Students witness first-hand how components of a solution can be separated, even when those individual components are not visible in solution.

  1. [Analysis of toxaphene and its eight congeners in sediment and fish tissue by gas chromatography-negative ion mass spectrometry].

    PubMed

    Lao, Wenjian

    2013-07-01

    Toxaphene quantification incorporating gas chromatography/negative chemical ionization mass spectrometry (GC/NCI-MS) offers improved sensitivity and specificity. The U. S. Environmental Protection Agency (USEPA) recently released a GC/NCI-MS method (Method 8276) for the measurement of technical toxaphene and eight specific congeners (Hx-Sed, Hp-Sed, P26, P41, P40, P44, P50 and P62). However, there is still lack of a practical and complete analytical method including sample extraction, clean up, instrumental analysis, and data analysis. The goal of this work was to develop a ready-to-use method for the quantification of total toxaphene and the eight congeners. Sediment and salmon fish tissue were selected as sample matrices and extracted with methylene chloride using an accelerated solvent extraction system. The sample extracts were cleaned up with active copper powder or gel permeation chromatography, and finally silica/alumina combination column. Separation was performed on a DB-XLB column. GC/NCI-MS was operated under selected ion monitoring mode with an identical set of confirmation and quantitation ions for total toxaphene and the eight congeners. Oxygen reaction of polychlorinated biphenyls (PCB) was monitored by PCB204, an internal calibration standard, and the reaction level was kept below 1%. Average relative response factors were used in quantitation. Quantitation of total toxaphene employed the sum of all detectable (S/N > or = 3) 6-C1 to 10-Cl homolog peak areas, while the individual congeners were quantified followed the standard procedures for single analytes. Multi-point calibration solutions ranged from 0. 5 (5 for P62) to 500 microg/L for the individual congeners, and 50 to 500 microg/L for technical toxaphene, with the lowest calibration levels as lower limits of quantitation. Average congener recovery was (90.8 +/- 17.4)% (n =10) in spiked sediment with relative standard deviations of 5.4% - 12.8% (n =10), underscoring an excellently accurate and precise method. The method was applied to analyze sediment and fish tissue sample. PMID:24164036

  2. A chemometric-assisted method based on gas chromatography-mass spectrometry for metabolic profiling analysis.

    PubMed

    Yu, Yong-Jie; Fu, Hai-Yan; Zhang, Li; Wang, Xiao-Yu; Sun, Pei-Jian; Zhang, Xiao-Bing; Xie, Fu-Wei

    2015-06-19

    An automatic and efficient data analysis method for comprehensive metabolic profiling analysis is urgently required. In this study, a new chemometric-assisted method for metabolic profiling analysis (CAMMPA) was developed to discover potentially valuable metabolites automatically and efficiently. The proposed method mainly consists of three stages. First, automatic chromatographic peak detection is performed based on the total ion chromatograms of samples to extract chromatographic peaks that can be accurately quantified. Second, a novel peak-shift alignment technique based on peak detection results is implemented to resolve time-shift problems across samples. Consequently, aligned results, including aligned chromatograms, and peak area tables, among others, can be successfully obtained. Third, statistical analysis using results from unsupervised and supervised classification results, together with ANOVA and partial least square-discriminate analysis, is performed to extract potential metabolites. To demonstrate the proposed technique, a complex GC-MS metabolic profiling dataset was measured to identify potential metabolites in tobacco plants of different growth stages as well as different plant tissues after maturation. Results indicated that the efficiency of the routine metabolic profiling analysis procedure can be significantly improved and potential metabolites can be accurately identified with the aid of CAMMPA. PMID:25943833

  3. Systematic Comparison of Reverse Phase and Hydrophilic Interaction Liquid Chromatography Platforms for the Analysis of N-linked Glycans

    PubMed Central

    Walker, S. Hunter; Carlisle, Brandon C.; Muddiman, David C.

    2013-01-01

    Due to the hydrophilic nature of glycans, reverse phase chromatography has not been widely used as a glycomic separation technique coupled to mass spectrometry. Other approaches such as hydrophilic interaction chromatography and porous graphitized carbon chromatography are often employed, though these strategies frequently suffer from decreased chromatographic resolution, long equilibration times, indefinite retention, and column bleed. Herein, it is shown that through an efficient hydrazone formation derivatization of N-linked glycans (?4 hr of additional sample preparation time which is carried out in parallel), numerous experimental and practical advantages are gained when analyzing the glycans by online reverse phase chromatography. These benefits include an increased number of glycans detected, increased peak capacity of the separation, and the ability to analyze glycans on the identical liquid chromatography-mass spectrometry platform commonly used for proteomic analyses. The data presented show that separation of derivatized N-linked glycans by reverse phase chromatography significantly out-performs traditional separation of native or derivatized glycans by hydrophilic interaction chromatography. Furthermore, the movement to a more ubiquitous separation technique will afford numerous research groups the opportunity to analyze both proteomic and glycomic samples on the same platform with minimal time and physical change between experiments, increasing the efficiency of ‘multi-omic’ biological approaches. PMID:22954204

  4. High-speed counter-current chromatography coupled online to high performance liquid chromatography-diode array detector-mass spectrometry for purification, analysis and identification of target compounds from natural products.

    PubMed

    Liang, Xuejuan; Zhang, Yuping; Chen, Wei; Cai, Ping; Zhang, Shuihan; Chen, Xiaoqin; Shi, Shuyun

    2015-03-13

    A challenge in coupling high-speed counter-current chromatography (HSCCC) online with high performance liquid chromatography (HPLC) for purity analysis was their time incompatibility. Consequently, HSCCC-HPLC was conducted by either controlling HPLC analysis time and HSCCC flow rate or using stop-and-go scheme. For natural products containing compounds with a wide range of polarities, the former would optimize experimental conditions, while the latter required more time. Here, a novel HSCCC-HPLC-diode array detector-mass spectrometry (HSCCC-HPLC-DAD-MS) was developed for undisrupted purification, analysis and identification of multi-compounds from natural products. Two six-port injection valves and a six-port switching valve were used as interface for collecting key HSCCC effluents alternatively for HPLC-DAD-MS analysis and identification. The ethyl acetate extract of Malus doumeri was performed on the hyphenated system to verify its efficacy. Five main flavonoids, 3-hydroxyphloridzin (1), phloridzin (2), 4',6'-dihydroxyhydrochalcone-2'-O-?-D-glucopyranoside (3, first found in M. doumeri), phloretin (4), and chrysin (5), were purified with purities over 99% by extrusion elution and/or stepwise elution mode in two-step HSCCC, and 25mM ammonium acetate solution was selected instead of water to depress emulsification in the first HSCCC. The online system shortened manipulation time largely compared with off-line analysis procedure and stop-and-go scheme. The results indicated that the present method could serve as a simple, rapid and effective way to achieve target compounds with high purity from natural products. PMID:25678319

  5. Comprehensive multi-residue method for the target analysis of pesticides in crops using liquid chromatography-tandem mass spectrometry.

    PubMed

    Hiemstra, Maurice; de Kok, André

    2007-06-22

    A liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS) multi-residue method for the simultaneous target analysis of a wide range of pesticides and metabolites in fruit, vegetables and cereals has been developed. Gradient elution has been used in conjunction with positive mode electrospray ionization tandem mass spectrometry to detect up to 171 pesticides and/or metabolites in different crop matrices using a single chromatographic run. Pesticide residues were extracted/partitioned from the samples with acetone/dichloromethane/light petroleum. The analytical performance was demonstrated by the analysis of extracts from lettuce, orange, apple, cabbage, grape and wheat flour, spiked at three concentration levels ranging from 0.01 to 0.10 mg/kg for each pesticide and/or metabolite. In general, recoveries ranging from 70 to 110%, with relative standard deviations better than 15%, were obtained. The recovery and repeatability data are in good accordance with EU guidelines for pesticide residue analysis. The limit of quantification for all targeted pesticides and metabolites tested was 0.01 mg/kg. The selectivity and robustness of the LC-MS/MS method was demonstrated by a 1-year comparison of its analytical results with those obtained from our validated GC and LC multi-residue methods applied to more than 3500 routine samples. The validated LC-MS/MS method has been implemented in our analytical scheme since 2004, replacing four of the conventional detection methods, i.e. GC-flame-photometric detection (acephate, methamidophos, etc.), GC-nitrogen-phosphorus detection, LC-UV detection (carbendazim, thiabendazole, imazalil and prochloraz) and LC-fluorescence detection (N-methylcarbamate pesticides). During a 3-year period, the LC-MS/MS method has been applied to the analyses of more than 12,000 samples. PMID:17442324

  6. A novel methodological approach for ?(18)O analysis of sugars using gas chromatography-pyrolysis-isotope ratio mass spectrometry.

    PubMed

    Zech, Michael; Saurer, Matthias; Tuthorn, Mario; Rinne, Katja; Werner, Roland A; Siegwolf, Rolf; Glaser, Bruno; Juchelka, Dieter

    2013-01-01

    Although the instrumental coupling of gas chromatography-pyrolysis-isotope ratio mass spectrometry (GC-Py-IRMS) for compound-specific ?(18)O analysis has been commercially available for more than a decade, this method has been hardly applied so far. Here we present the first GC-Py-IRMS ?(18)O results for trimethylsilyl-derivatives of plant sap-relevant sugars and a polyalcohol (glucose, fructose, sucrose, raffinose and pinitol). Particularly, we focus on sucrose, which is assimilated in leaves and which is the most important transport sugar in plants and hence of utmost relevance in plant physiology and paleoclimate studies. Replication measurements of sucrose standards and concentration series indicate that the GC-Py-IRMS ?(18)O measurements are not stable over time and that they are amount (area) dependent. We, therefore, suggest running sample batch replication measurements in alternation with standard concentration series of reference material. This allows for carrying out (i) a drift correction, (ii) a calibration against reference material and (iii) an amount (area) correction. Tests with (18)O-enriched water do not provide any evidence for oxygen isotope exchange reactions affecting sucrose and raffinose. We present the first application of GC-Py-IRMS ?(18)O analysis for sucrose from needle extract (soluble carbohydrate) samples. The obtained ?(18)Osucrose/ Vienna Standard Mean Ocean Water (VSMOW) values are more positive and vary in a wider range (32.1-40.1 ‰) than the ?(18)Obulk/ VSMOW values (24.6-27.2 ‰). Furthermore, they are shown to depend on the climate parameters maximum day temperature, relative air humidity and cloud cover. These findings suggest that ?(18)Osucrose of the investigated needles very sensitively reflects the climatically controlled evaporative (18)O enrichment of leaf water and thus highlights the great potential of GC-Py-IRMS ?(18)Osucrose analysis for plant physiology and paleoclimate studies. PMID:24313371

  7. Development and Application of Pyrolysis Gas Chromatography/Mass Spectrometry for the Analysis of Bound Trinitrotoluene Residues in Soil

    USGS Publications Warehouse

    Weiss, J.M.; Mckay, A.J.; Derito, C.; Watanabe, C.; Thorn, K.A.; Madsen, E.L.

    2004-01-01

    TNT (trinitrotoluene) is a contaminant of global environmental significance, yet determining its environmental fate has posed longstanding challenges. To date, only differential extraction-based approaches have been able to determine the presence of covalently bound, reduced forms of TNT in field soils. Here, we employed thermal elution, pyrolysis, and gas chromatography/mass spectrometry (GC/MS) to distinguish between covalently bound and noncovalently bound reduced forms of TNT in soil. Model soil organic matter-based matrixes were used to develop an assay in which noncovalently bound (monomeric) aminodinitrotoluene (ADNT) and diaminonitrotoluene (DANT) were desorbed from the matrix and analyzed at a lower temperature than covalently bound forms of these same compounds. A thermal desorption technique, evolved gas analysis, was initially employed to differentiate between covalently bound and added 15N-labeled monomeric compounds. A refined thermal elution procedure, termed "double-shot analysis" (DSA), allowed a sample to be sequentially analyzed in two phases. In phase 1, all of an added 15N-labeled monomeric contaminant was eluted from the sample at relatively low temperature. In phase 2 during high-temperature pyrolysis, the remaining covalently bound contaminants were detected. DSA analysis of soil from the Louisiana Army Ammunition Plant (LAAP; ???5000 ppm TNT) revealed the presence of DANT, ADNT, and TNT. After scrutinizing the DSA data and comparing them to results from solvent-extracted and base/acid-hydrolyzed LAAP soil, we concluded that the TNT was a noncovalently bound "carryover" from phase 1. Thus, the pyrolysis-GC/MS technique successfully defined covalently bound pools of ADNT and DANT in the field soil sample.

  8. High-Pressure Liquid Chromatography: Quantitative Analysis of Chinese Herbal Medicine

    ERIC Educational Resources Information Center

    Chan, W. F.; Lin, C. W.

    2007-01-01

    An HPLC undergraduate experiment on the analysis of traditional Chinese medicine (TCM) has been developed. Two commonly used herbs ("glycyrrhizae radix" and "cinnamomi ramulus") are studied. Glycyrrhizin, cinnamic acid, and cinnamaldehyde are chosen as markers for the herbs. The dried herbs in their natural state and a TCM preparation in powder…

  9. Analysis of pesticide residues by fast gas chromatography in combination with negative chemical ionization mass spectrometry

    Microsoft Academic Search

    Renáta Húšková; Eva Matisová; Svetlana Hrouzková; ?ubomír Švorc

    2009-01-01

    A combination of fast GC with narrow-bore column and bench top quadrupole mass spectrometer (MS) detector in negative chemical ionization (NCI) mode (with methane as reagent gas) is set up and utilized for the ultratrace analysis of 25 selected pesticides. The observed pesticides, belonging to the endocrine disrupting chemicals (EDCs), were from different chemical classes. A comparative study with electron

  10. Integrated cation–anion\\/volatile fluid inclusion analysis by gas and ion chromatography; methodology and examples

    Microsoft Academic Search

    D. M. DeR Channer; C. J Bray; E. T. C Spooner

    1999-01-01

    Combined gas and ion chromatographic analysis of well characterized, small (?1 g) fluid inclusion-bearing samples is a powerful, but simple, means for obtaining integrated fluid concentrations of major and trace, volatile and ionic fluid constituents without using microthermometrically determined salinity for normalization. The methodology, which is described and assessed in detail, involves crushing a carefully cleaned sample at ?105°C in

  11. Column Chromatography Analysis of Brain Tissue: An Advanced Laboratory Exercise for Neuroscience Majors

    NSDL National Science Digital Library

    William H. Church (Trinity College; )

    2005-04-29

    This article describes an experiment done in a six session (4 hours each) component of a neuroscience research methods course. The experiment focuses on the neurochemical analysis of discrete brain structures in experimental animals, which provides important information on synthesis, release, and metabolism changes following behavioral or pharmacological experimental manipulations.

  12. Analysis of Fluorotelomer Alcohols in Soils: Optimization of Extraction and Chromatography

    EPA Science Inventory

    This article describes the development of an analytical method for the determination of fluorotelomer alcohols (FTOHs) in soil. The sensitive and selective determination of the telomer alcohols was performed by extraction with mthyl tert-butyl ether (MTBE) and analysis of the ext...

  13. RAPID AND SENSITIVE FAME ANALYSIS OF BACTERIA BY COLD TRAP INJECTION GAS CHROMATOGRAPHY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Fatty acid analysis is commonly used to identify bacteria. A cold trap is used to focus peaks at the head of the GC column. When combined with a rapid sample processing method that uses smaller volumes of solvents, it becomes possible to correctly identify bacteria from 1-2 mg of biomass....

  14. Analysis of primisulfuron and triasulfuron in water and soil samples by micellar electrokinetic capillary chromatography

    Microsoft Academic Search

    Kumar V Penmetsa; Ross B Leidy; Damian Shea

    1997-01-01

    A capillary electrophoresis (CE) method was developed to separate and determine residues of two sulfonylurea herbicides (primisulfuron and triasulfuron) in water and soil samples. Fortified water samples were extracted by solvent partitioning with methylene chloride and analysis by CE. Fortified soil samples were extracted by shaking in methanol–phosphate buffer (1:1) followed by partitioning of the residues into methylene chloride and

  15. Microemulsion mediated in situ derivatization-extraction and gas chromatography-mass spectrometric analysis of alkylphosphonic acids.

    PubMed

    Pardasani, Deepak; Palit, Meehir; Gupta, A K; Kanaujia, Pankaj K; Sekhar, K; Dubey, D K

    2006-03-10

    Detection and identification of environmental signatures of chemical warfare agents is an important aspect of verification program of Chemical Weapons Convention (CWC). Alkylphosphonic acids (APAs) are ultimate and persistent degradation products of nerve agents. Their identification in a sample submitted for off-site analysis infers possible indication of contamination with nerve agents. This paper describes the development of a new sample preparation method which involves 'in situ derivatization and extraction' (INDEX) of acids from water. Derivatization is performed by alkylation of APAs with alkylbromides in surfactant less microemulsion (SLME). The derivatized analytes were analyzed by gas chromatography coupled with mass spectrometry. The developed method involves simultaneous derivatization (alkylation) and extraction of acidic analytes mediated by surfactant less microemulsion. Various derivatization-extraction parameters such as solvent, reaction time and temperature, base and alkyl bromides were optimized. Pentyl bromide in the presence of potassium carbonate and diisopropylamine at 100 degrees C derivatized the selected acids efficiently. Kinetic data for alkylation of methylphosphonic acids and some carboxylic acids were obtained to assess their relative susceptibility for alkylation in microemulsion. Methylphosphonic acid and isopropyl methylphosphonic acid took 140-150 min to reach completion while carboxylic acids took 100 min to complete the reaction. INDEX could be successfully performed even in the presence of interfering Ca(2+) and Mg(2+) ions. PMID:16455095

  16. Complete Analysis of a Biologically Active Tetrapeptide: A Project Utilizing Thin-Layer Chromatography and Tandem Quadrupole Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Lefevre, Joseph W.; Dodsworth, David W.

    2000-04-01

    The biologically active tetrapeptide d-Ala-Gly-l-Phe-d-Leu ([des-Tyr1-d-Ala2-d-Leu5]enkephalin) was analyzed for its amino acid content and stereochemistry by normal and reversed-phase thin-layer chromatography (TLC), and its sequence was determined by tandem quadrupole mass spectrometry. The project involved sequential N-dansylation of a portion of the tetrapeptide, hydrolysis, isolation, and identification of the N-terminal amino acid as dansyl-alanine by comparison with standards using normal-phase TLC. A second portion of the tetrapeptide was hydrolyzed and the resulting four free amino acids were converted to their corresponding dansyl derivatives and purified by preparative normal-phase TLC. The three dansyl amino acids not identified previously were identified by TLC. The stereochemistry of each was determined by comparison with dansyl-dl-amino acid standards using reversed-phase TLC in the presence of ß-cyclodextrin, a chiral mobile phase additive. Finally, the correct amino acid sequence was determined by tandem quadrupole mass spectrometry. This project gives students valuable experience in microscale synthesis, both normal and reversed-phase TLC, stereochemical analysis, and mass spectrometry.

  17. Analysis of rocuronium in human plasma by liquid chromatography-tandem mass spectrometry with application in clinical pharmacokinetics.

    PubMed

    de Moraes, Natália Valadares; Lauretti, Gabriela Rocha; Filgueira, Gabriela Campos de Oliveira; Lopes, Bruno Carvalho Portes; Lanchote, Vera Lucia

    2014-03-01

    Rocuronium (ROC) is a neuromuscular blocking agent used in surgical procedures which is eliminated primarily by biliary excretion. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for analysis of ROC in human plasma. Separation of ROC and IS (verapamil) was performed using an endcapped C-18 column and a mixture of water:acetonitrile:trifluoracetic acid (50:50:0.1, v/v) as mobile phase. Aliquots of 100 ?L of human plasma were extracted at pH 3, using dichloromethane. The lower limit of quantification of 5 ng/mL shows the high sensitivity of this method. Intra- and inter-assay precision (as relative standard deviation) was all ?14.2% and accuracy (as relative standard error) did not exceed 10.1%. The validated method was successfully applied to quantify ROC concentrations in patients under surgical procedures up to 6h after the administration of the 0.4-0.9 mg/kg ROC. The pharmacokinetic parameter estimations of ROC showed AUC/dose of 563 ?g min/mL, total clearance of 2.5 mL/min/kg, volume of distribution at steady state of 190 mL/kg and mean residence time of 83 min. PMID:24370612

  18. Chemical and technical challenges in the analysis of central carbon metabolites by liquid-chromatography mass spectrometry.

    PubMed

    Siegel, David; Permentier, Hjalmar; Reijngoud, Dirk-Jan; Bischoff, Rainer

    2014-09-01

    This review deals with chemical and technical challenges in the analysis of small-molecule metabolites involved in central carbon and energy metabolism via liquid-chromatography mass-spectrometry (LC-MS). The covered analytes belong to the prominent pathways in biochemical carbon oxidation such as glycolysis or the tricarboxylic acid cycle and, for the most part, share unfavorable properties such as a high polarity, chemical instability or metal-affinity. The topic is introduced by selected examples on successful applications of metabolomics in the clinic. In the core part of the paper, the structural features of important analyte classes such as nucleotides, coenzyme A thioesters or carboxylic acids are linked to "problematic hotspots" along the analytical chain (sample preparation and-storage, separation and detection). We discuss these hotspots from a chemical point of view, covering issues such as analyte degradation or interactions with metals and other matrix components. Based on this understanding we propose solutions wherever available. A major notion derived from these considerations is that comprehensive carbon metabolomics inevitably requires multiple, complementary analytical approaches covering different chemical classes of metabolites. PMID:24326023

  19. Environmental analysis by on-line immunoextraction and reversed-phase liquid chromatography: optimization of the immunoextraction/RPLC interface.

    PubMed

    Nelson, Mary Anne; Papastavros, Efthimia; Dodlinger, Maud; Hage, David S

    2007-05-16

    The use of antibodies in HPLC columns for on-line immunoextraction combined with reversed-phase liquid chromatography (RPLC) is of growing interest in environmental and agricultural analysis. This technique is typically performed by using a small RPLC precolumn to capture and concentrate analytes as they elute from the immunoextraction column; however, there is little information on the conditions required for optimizing this interface. This study examined the behavior of this interface by using 2,4-dichlorophenoxyacetic acid (2,4-D) and related herbicides as model analytes. It was found that analyte dissociation from immunoextraction columns followed first-order decay and that the elution of these analytes through the immunoextraction/RPLC interface gave an exponentially modified Gaussian profile. Computer simulations were used to see how analyte elution through the interface changed with different dissociation and retention conditions. Several guidelines were developed from this work that could be used for developing and optimizing on-line immunoextraction/RPLC systems for other chemicals of environmental or agricultural interest. PMID:17455948

  20. High performance liquid chromatography coupled to mass spectrometry for profiling and quantitative analysis of folate monoglutamates in tomato.

    PubMed

    Tyagi, Kamal; Upadhyaya, Pallawi; Sarma, Supriya; Tamboli, Vajir; Sreelakshmi, Yellamaraju; Sharma, Rameshwar

    2015-07-15

    Folates are essential micronutrients for animals as they play a major role in one carbon metabolism. Animals are unable to synthesize folates and obtain them from plant derived food. In the present study, a high performance liquid chromatography coupled to mass spectrometric (HPLC-MS/MS) method was developed for the high throughput screening and quantitative analysis of folate monoglutamates in tomato fruits. For folate extraction, several parameters were optimized including extraction conditions, pH range, amount of tri-enzyme and boiling time. After processing the extract was purified using ultra-filtration with 10 kDa membrane filter. The ultra-filtered extract was chromatographed on a RP Luna C18 column using gradient elution program. The method was validated by determining linearity, sensitivity and recovery. This method was successfully applied to folate estimation in spinach, capsicum, and garden pea and demonstrated that this method offers a versatile approach for accurate and fast determination of different folate monoglutamates in vegetables. PMID:25722141

  1. NF2 mutation screening by denaturing high-performance liquid chromatography and high-resolution melting analysis.

    PubMed

    Sestini, Roberta; Provenzano, Aldesia; Bacci, Costanza; Orlando, Claudio; Genuardi, Maurizio; Papi, Laura

    2008-06-01

    Neurofibromatosis type 2 (NF2) is an autosomal-dominant disorder caused by mutations in the NF2 gene and predisposing to the development of nervous system. Identification of germline mutations is essential to provide appropriate genetic counseling in NF2 patients, but it represents an extremely challenging task because the vast majority of mutations are unique and spread over the entire coding sequence. Moreover, about 30% of de novo patients are indeed mosaic, and direct sequencing can undetect mutated alleles present in a minority of cells. As most screening techniques do not meet the requirements for efficient NF2 testing, we have developed a semi-automated denaturing high-performance liquid chromatography (DHPLC) method for point mutation detection combined with a multiplex ligation-dependent probe amplification approach to screen for gene rearrangements. In addition, we have evaluated high-resolution melting analysis (HRMA) as an exon scanning procedure to identify point mutations in the NF2 gene. The results obtained in 92 NF2 patients expand the NF2 mutational spectrum and indicate DHPLC and HRMA as good systems to screen for point mutations in diseases with a heterogeneous spectrum of alterations. PMID:18554169

  2. High-throughput simultaneous analysis of pesticides by supercritical fluid chromatography coupled with high-resolution mass spectrometry.

    PubMed

    Ishibashi, Megumi; Izumi, Yoshihiro; Sakai, Miho; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi

    2015-05-13

    Recently, a generally applicable screening method for multiresidue pesticide analysis, which is simple, quick, and accurate and has a reliable performance, is becoming increasingly important for food safety and international trade. This paper proposes a high-throughput screening methodology that enables the detection of multiresidue pesticides using supercritical fluid chromatography coupled to a high-performance benchtop quadrupole Orbitrap mass spectrometry (SFC/Q Exactive) and an automated library-based detection. A total of 444 chemicals covering a wide polarity range (logPow from -4.2 to 7.7) and a wide molecular weight range (from 99.0 to 872.5) were analyzed simultaneously through a combination of high mass resolution (a value of m/?m = 70000), high mass accuracy (<5 ppm) with positive/negative polarity switching, and highly efficient separation by SFC. A total of 373 pesticides were detected in QuEChERS spinach extracts without dispersive solid phase extraction at the 10 ?g kg(-1) level (provisional maximum residue limits in Japan). In conclusion, the developed analytical system is a potentially useful tool for practical multiresidue pesticide screening with high throughput (time for data acquisition, 72 samples per day; and time for data processing of 72 samples, approximately 45 min). PMID:25547162

  3. Improvement of sugar analysis sensitivity using anion-exchange chromatography-electrospray ionization mass spectrometry with sheath liquid interface.

    PubMed

    Xu, Xian-Bing; Liu, Ding-Bo; Guo, Xiao Ming; Yu, Shu-Juan; Yu, Pei

    2014-10-31

    A novel interface that enables high-performance anion-exchange chromatography (HPAEC) to be coupled with electrospray ionization (ESI) mass spectrometry (MS) is reported. A sheath liquid consisting of 50mM NH4Ac in isopropanol with 0.05% acetic acid, infused at a flow rate of 3?L/min at the tip of the electrospray probe, requires less ESI source cleaning and promotes efficient ionization of mono- and di-carbohydrates. The results suggest that use of a sheath liquid interface rather than a T-joint allows volatile ammonium salts to replace non-volatile metal salts as modifiers for improving sugar ESI signals. The efficient ionization of mono- and di-carbohydrates in the ESI source is affected by the sheath liquid properties such as buffer concentration and type of organic solvent. HPAEC-ESI-MS was used for the analysis of monocarbohydrates in pectins, particularly co-eluted sugars, and the performance was evaluated. Addition of a make-up solution through the sheath liquid interface proved to be an efficient tool for enhancing the intensities of sugars analyzed using HPAEC-ESI-MS. PMID:25246101

  4. Liquid Chromatography-Tandem Mass Spectrometry Analysis of Perfluorooctane Sulfonate and Perfluorooctanoic Acid in Fish Fillet Samples

    PubMed Central

    Paiano, Viviana; Fattore, Elena; Carrà, Andrea; Generoso, Caterina; Fanelli, Roberto; Bagnati, Renzo

    2012-01-01

    Perfluorooctane sulfonate (PFOS) and perfluorooctanoic (PFOA) acid are persistent contaminants which can be found in environmental and biological samples. A new and fast analytical method is described here for the analysis of these compounds in the edible part of fish samples. The method uses a simple liquid extraction by sonication, followed by a direct determination using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The linearity of the instrumental response was good, with average regression coefficients of 0.9971 and 0.9979 for PFOS and PFOA, respectively, and the coefficients of variation (CV) of the method ranged from 8% to 20%. Limits of detection (LOD) were 0.04?ng/g for both the analytes and recoveries were 90% for PFOS and 76% for PFOA. The method was applied to samples of homogenized fillets of wild and farmed fish from the Mediterranean Sea. Most of the samples showed little or no contamination by perfluorooctane sulfonate and perfluorooctanoic acid, and the highest concentrations detected among the fish species analyzed were, respectively, 5.96?ng/g and 1.89?ng/g. The developed analytical methodology can be used as a tool to monitor and to assess human exposure to perfluorinated compounds through sea food consumption. PMID:22567564

  5. Application of programmed-temperature split/splitless injection to the trace analysis of aliphatic hydrocarbons by gas chromatography.

    PubMed

    Miñones Vázquez, M; Vázquez Blanco, M E; Muniategui Lorenzo, S; López Mahía, P; Fernández Fernández, E; Prada Rodríguez, D

    2001-06-15

    The dependence of the programmed-temperature solvent split sampling technique using a PSS (programmed-split/splitless) injection mode on different variables affecting the introduction of large sample volumes for a mixture of alkanes in capillary GC was evaluated. Apart from the studies found in the literature on different factors such as speed of injection. presence of adsorbent in the liner, internal diameter of the liner, initial and final injector temperature, split flow-rate and initial split time, affecting the chromatographic signal of different compounds, others were studied whose influence has not been considered until now. They include length of the microsyringe needle, adsorbent distribution in the liner, injection volume on analyte discrimination, speed of injector heating, time which the column stays at the initial temperature and time that the injector stays at the final temperature. Once finalised, the study of the PSS injection mode was compared with the conventional mode of gas chromatography splitless injection, and found that the proposed method increases sensitivity in GC trace analysis. Finally, the application of both injection modes in the determination of aliphatic hydrocarbons was tested in an atmospheric particulate sample. PMID:11442043

  6. [Simultaneous analysis of trehalose, glucose and maltose in biotransformation samples by high performance anion exchange chromatography with pulsed ampere detection].

    PubMed

    Xu, Ying; Zang, Ying; Jiang, Ting; Zheng, Zhaojuan; Quyang, Jia

    2014-12-01

    An analytical method for the determination of trehalose, maltose, and glucose in biotransformation samples was developed by using high performance anion exchange chromatography coupled with pulsed ampere detection (HPAEC-PAD). The analysis was performed on a CarboPac™ 10 column (250 mm x 2 mm) with the gradient elution of NaOH-NaAc as the mobile phase. The column temperature was set at 30 °C, the flow rate was 0. 30 mL/min. The results showed that trehalose, maltose, and glucose in biotransformation system were completely separated and determined in 15 min. The linear ranges and the working curves were determined by using standard samples. The correlation coefficients of three kinds of carbohydrates were over 0. 9998 . The detection limits (LODs) were 0. 010 - 0. 100 mg/L. Under the optimized separation conditions, the recoveries of saccharides in the transformation system at three different spiked levels ranged from 89. 4% to 103. 2%. In biotransformation system, 50 IU trehalose synthase were added into 200 g/L maltose for reaction of 8 h at 37 °C, pH 8. 0. Under the above conditions, the concentration of trehalose in biotransformation sample was 101. 084 g/L, and the conversion rate of trehalose reached 50. 5%. The method can be applied to determine the composition in the transformation system with the advantages of simplicity and convenience. PMID:25902650

  7. Practical aspects in gas chromatography-mass spectrometry for the analysis of pesticide residues in exotic fruits.

    PubMed

    España Amórtegui, Julio César; Guerrero Dallos, Jairo Arturo

    2015-09-01

    The most relevant parameters of a multimode inlet were optimized to increase the injection volume up to 25 ?L using solvent vent mode in order to improve the sensitivity of the gas chromatography-mass spectrometry system. Consequently, the implementation of a concurrent backflushing was necessary to largely prevent the expected loss of performance derived from such matrix load out of a general-purpose extraction (EN-15622-QuEChERS). Additionally, four mixtures of compounds used as analyte protectants were tested using spiked physalis to enhance the quality of signals. The chosen mixture remarkably improved sensitivity and yield better peak shapes, significantly more than others also tested. The analysis of pesticide residues in exotic fruits using instruments of limited selectivity is challenging since these complex matrices usually give notably dirty extracts. This scheme included an instrumental optimization and the addition of selected compounds that enabled to selectively reach limits of quantitation of 0.01 mg kg(-1) for most analytes. PMID:25842302

  8. Fast analysis of triterpenoids in Ganoderma lucidum spores by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

    PubMed

    Yan, Zhou; Xia, Bing; Qiu, Ming Hua; Li Sheng, Ding; Xu, Hong Xi

    2013-11-01

    A rapid and reliable method was established for simultaneous determination of main triterpenoids in Ganoderma lucidum spores using ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-TQ-MS). The established method was validated in terms of linearity, sensitivity, precision, accuracy and stability, and was successfully applied to determine the contents of 10 main triterpenoids in different batches of G. lucidum spores. The analysis results showed that moderate levels of triterpenoids were found in G. lucidum spores. In addition, a MS full scan with a daughter ion scan experiment was performed to identify the potential derivatives of triterpenoids present in G. lucidum spores. As a result, a total of 22 triterpenoids from different G. lucidum spores were unequivocally or tentatively identified via comparisons with authentic standards and literatures. This method provides both qualitative and quantitative results without the need for repetitive UPLC-MS analyses, thereby increasing efficiency and productivity, making it suitable for high-throughput applications. PMID:23780736

  9. Analysis of organophosphate flame retardants and plasticisers in water by isotope dilution gas chromatography-electron ionisation tandem mass spectrometry.

    PubMed

    Teo, Tiffany L L; McDonald, James A; Coleman, Heather M; Khan, Stuart J

    2015-10-01

    The widespread use of organophosphate flame retardants (PFRs) in commercial products have led to their increased presence in the environment. In this study, a rapid and reliable analytical method was developed for the analysis of five PFRs in water using gas chromatography tandem mass spectrometry (GC-MS/MS) with electron ionisation (EI) and a run time of 13min. The PFRs investigated were tributyl phosphate (TBP), tris(2-chloroethyl) phosphate (TCEP), tris(1-chloro-2-propyl) phosphate (TCPP), tris(1,3-dichloro-2-propyl) phosphate (TDCP) and triphenyl phosphate (TPP). Solid phase extraction (SPE) was undertaken to extract and concentrate target analytes from aqueous matrices. All water samples were extracted from a volume of 500mL. Isotopically labelled compounds were used to account for analytical variability and for accurate quantification by isotope dilution. Method recoveries for all compounds were above 80% in all tested water samples. Method detection limits for all target analytes ranged from 0.3 to 24ng/L in ultrapure water, tap water, seawater, surface water, secondary effluent and swimming pool water. Validation of this method confirmed satisfactory method stability with less than 1% coefficients of variation, verifying that this approach produced good reproducibility. PMID:26078137

  10. Determination of disease biomarkers in Eucalyptus by comprehensive two-dimensional gas chromatography and multivariate data analysis.

    PubMed

    Hantao, Leandro Wang; Aleme, Helga Gabriela; Passador, Martha Maria; Furtado, Edson Luiz; Ribeiro, Fabiana Alves de Lima; Poppi, Ronei Jesus; Augusto, Fabio

    2013-03-01

    In this paper is reported the use of the chromatographic profiles of volatiles to determine disease markers in plants - in this case, leaves of Eucalyptus globulus contaminated by the necrotroph fungus Teratosphaeria nubilosa. The volatile fraction was isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography-fast quadrupole mass spectrometry (GC×GC-qMS). For the correlation between the metabolic profile described by the chromatograms and the presence of the infection, unfolded-partial least squares discriminant analysis (U-PLS-DA) with orthogonal signal correction (OSC) were employed. The proposed method was checked to be independent of factors such as the age of the harvested plants. The manipulation of the mathematical model obtained also resulted in graphic representations similar to real chromatograms, which allowed the tentative identification of more than 40 compounds potentially useful as disease biomarkers for this plant/pathogen pair. The proposed methodology can be considered as highly reliable, since the diagnosis is based on the whole chromatographic profile rather than in the detection of a single analyte. PMID:23394740

  11. Characterization of dissolved organic matter in municipal wastewater using fluorescence PARAFAC analysis and chromatography multi-excitation/emission scan: a comparative study.

    PubMed

    Li, Wen-Tao; Chen, Shi-Yu; Xu, Zi-Xiao; Li, Yan; Shuang, Chen-Dong; Li, Ai-Min

    2014-03-01

    Dissolved organic matter (DOM) in municipal wastewater was mainly characterized using high-performance liquid chromatography (HPLC) and size exclusion chromatography (HPSEC) with multi-excitation/emission fluorescence scan. Meanwhile, fluorescence excitation-emission-matrix combined with parallel factor analysis (EEM-PARAFAC) was also applied. Compared with chromatography fluorescence fingerprints, the EEM-PARAFAC model could not reflect the variety of DOM species with similar fluorescence but different physicochemical properties. The chromatography results showed that the protein-like species were variable among different municipal wastewater treatment plants, some of which are in combination with humic-like species; while there were two major humic-like species fractionated by hydrophilicity and molecular weight (MW), which are also the major contributors to UV absorbance at 254 nm. It was also identified that the relatively hydrophilic humic fractions were slightly larger than the relatively hydrophobic humic fractions. In all the investigated wastewater treatment plants, the relatively hydrophilic and larger MW humic fraction mainly contributed to the fluorescence intensity of humic-like EEM-PARAFAC components. As well as facilitating interpretations of EEM-PARAFAC components, the HPLC/HPSEC fluorescence fingerprints also contributed to a better understanding of fluorescent DOM species in municipal wastewater. PMID:24460470

  12. ANALYSIS OF FLAVONOIDS AND HYROXYCINNAMATES IN CITRUS PROCESSING BYPRODUCTS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY-ELECTROSPRAY IONIZATION-MASS SPECTROMETRY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Electrospray ionization-high performance liquid chromatography-mass spectrometry (ESI-HPLC-MS) greatly facilitates analyses of the complex phenolic constituents of citrus peel and associated citrus processing byproducts. The numerous flavonoid glycosides and polymethoxylated flavones (PMFs) in thes...

  13. An automated method for the analysis of urinary free catecholamines using ASTED and high-pressure liquid chromatography.

    PubMed

    Green, B; Cooper, J D; Turnell, D C

    1989-07-01

    A high-pressure liquid chromatography procedure for the measurement of free catecholamines in urine is described. 'On-line' sample preparation using a cartesian robot combined with the ASTED process ensures minimal operator intervention and reduced costs. PMID:2764490

  14. Analysis of tensides in complex samples with comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry.

    PubMed

    Hübner, Jane; Taheri, Rahil; Melchior, David; Kling, Hans-Willi; Gäb, Siegmar; Schmitz, Oliver J

    2007-08-01

    Multidimensional gas-chromatographical analysis of various tensides of natural or synthetic origin in cosmetic products is demonstrated. Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry allows the qualitative and quantitative determination of alkyl polyglucosides (AG), fatty alcohol ethoxylates (FAEO), fatty alcohol sulfates (FAS), fatty alcohol ether sulfates (FAES) and cocamidopropyl betaines (CAPB) in shower gel and cleaning agents. The samples were aliquoted in two parts. The first part was silylated, diluted and analysed; then, in order to detect anionic tensides (FAES, FAS) too, the second aliquot was hydrolysed before being silylated for analysis. Because of their amphoteric character, the betaines can only be analysed by gas chromatography after thermal decomposition in the injector, which leads to the corresponding amidoamines among other products. PMID:17581745

  15. N2O analysis in the atmosphere via electron capture-gas chromatography

    NASA Technical Reports Server (NTRS)

    Rasmussen, R. A.; Krasnec, J.; Pierotti, D.

    1976-01-01

    The potential of commercially available pulse-modulated electron capture detector (ECD)-equipped gas chromatographs for direct measurement of ambient levels of N2O is assessed. Since the sensitivity of ECD to N2O is directly proportional to the detector operating temperature and detector standing current, it is necessary to use a 'hot' ECD (250-350 C). The method is shown to be very precise with a standard error not exceeding 1% for automated analysis of ambient air samples. The technology is available to permit highly accurate routine direct analysis of N2O in the troposphere and stratosphere. Both captured air samples or direct real-time measurement from research vessels or airborne platforms are possible.

  16. Analysis of trihalomethanes in drinking water using headspace-SPME technique with gas chromatography

    Microsoft Academic Search

    Deok-Hee Cho; Sung-Ho Kong; Seong-Geun Oh

    2003-01-01

    In many drinking water treatment plants, the chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of trihalomethanes (THMs) such as chloroform, dichlorobromomethane, chlorodibromomethane and bromoform. In this study, headspace-solid-phase microextraction (HS-SPME, 85?m carboxen\\/polydimethylsiloxane fiber) technique was applied for the analysis of THMs in drinking water. The effects

  17. Carbohydrate analysis in hydrothermally degraded plant material by high-pressure liquid chromatography (HPLC)

    Microsoft Academic Search

    R. Niesner; W. Briiller; O. Bobleter

    1978-01-01

    Summary  A high-pressure liquid chromatograph is described. This equipment was used for the analysis of carbohydrate solutions obtained by hydrothermal degradation of cellulosic plant matter. With an anion-exchange column the pentoses of the hemicellulose fraction, and the hexoses of the cellulose fraction of wheat straw samples were analysed with acetonitrile: H2O ratios of 7525 and 8020 as elution media. Glucose and

  18. Analysis of Chloramphenicol Residues in Honey by Liquid Chromatography–Tandem Mass Spectrometry

    Microsoft Academic Search

    D. Ortelli; P. Edder; C. Corvi

    2004-01-01

    Antibiotics are often used in bee-keeping to control European and American foulbrood. The broad spectrum antibiotic chloramphenicol (CAP) was used for curative purposes in veterinary medicine, but is now forbidden in numerous countries, although still used in south-east Asia. A liquid-chromatographic method with tandem mass spectrometric detection (LC–MS–MS) has been developed for analysis of sub-µg kg -1 residues of chloramphenicol

  19. Nano-high-performance liquid chromatography–electron ionization mass spectrometry approach for environmental analysis

    Microsoft Academic Search

    Achille Cappiello; Giorgio Famiglini; Filippo Mangani; Pierangela Palma; Antonella Siviero

    2003-01-01

    We describe a method, based on a new nano-HPLC gradient generator coupled to a modified direct electron ionization (EI) LC–MS interface, for the analysis of several compounds of environmental interest. The gradient generator was installed on a conventional HPLC system and the nano-flow rate was achieved using a double splitter. Reproducible gradients of different shapes (i.e. linear, convex, concave) can

  20. Accurate mass tag retention time database for urine proteome analysis by chromatography-mass spectrometry

    Microsoft Academic Search

    I. A. Agron; D. M. Avtonomov; A. S. Kononikhin; I. A. Popov; S. A. Moshkovskii; E. N. Nikolaev

    2010-01-01

    Information about peptides and proteins in urine can be used to search for biomarkers of early stages of various diseases.\\u000a The main technology currently used for identification of peptides and proteins is tandem mass spectrometry, in which peptides\\u000a are identified by mass spectra of their fragmentation products. However, the presence of the fragmentation stage decreases\\u000a sensitivity of analysis and increases