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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. 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)

  3. Simulating retention in gas-liquid chromatography

    SciTech Connect

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

    1999-12-16

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

  4. Multicomponent analysis of bile acids in faeces by anion exchange and capillary column gas-liquid chromatography: application in oxytetracycline treated subjects.

    PubMed

    Korpela, J T; Fotsis, T; Adlercreutz, H

    1986-08-01

    A method is described for the multicomponent analysis of bile acids in faeces. Following homogenization and extraction, bile acids are separated into several groups according to their mode of conjugation by anion exchange chromatography on DEAE-Sephadex A-25 in the acetate form. The different conjugate groups are then processed separately and quantified using capillary column gas-liquid chromatography (GC), the identity of the individual bile acid components being established by gas chromatography-mass spectrometry (GC-MS). The method permits the quantitative determination, with good precision, of unconjugated bile acids, their saponifiable derivatives, and their glycine-, taurine- and sulfated conjugates. In five healthy men the mean daily excretion of bile acids was 472 +/- 21.8 mumol (SEM) and the mean faecal concentration 7.74 +/- 1.07 mumol (SEM)/g dry weight. Free bile acids constituted 74.8% +/- 5.8% (SEM), saponifiable conjugates 23.5% +/- 5.8% (SEM) glycine-conjugates 0.7% +/- 0.2% (SEM), taurine-conjugates 0.2% +/- 0.07% (SEM), and their sulfated conjugates 0.8% +/- 0.1% (SEM) of total faecal bile acids. In addition to a detailed description of the methodology the effect of antibiotics on faecal bile acid profiles is presented. Oxytetracycline consistently decreased faecal concentrations of saponifiable derivatives of bile acids while increasing the taurine- and sulfated conjugates. The concentrations of the primary bile acids, cholic- and chenodeoxycholic acid, were higher during the course of oxytetracycline. PMID:3747527

  5. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  6. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  7. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  8. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

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

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

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  10. Evaluation of gas-liquid chromatography for the rapid diagnosis of Clostridium difficile associated disease.

    PubMed Central

    Gianfrilli, P; Pantosti, A; Luzzi, I

    1985-01-01

    Direct gas-liquid chromatography of faecal specimens with isocaproic acid as a marker was used for the rapid diagnosis of Clostridium difficile associated diarrhoeal diseases. Ninety stools were examined and results were compared with conventional culture on selective medium and cytotoxin assay in tissue culture. Using a combined analysis of isocaproic acid and butyric acid peak heights we defined three categories: positive, negative, and indeterminate. When the indeterminate group was excluded, the positive and negative predictive values of gas-liquid chromatography analysis were 86.9% and 85% respectively compared with culture and 71.4% and 95% respectively compared with cytotoxin assay. PMID:4008667

  11. Gas-liquid chromatography of fecal neutral steriods.

    PubMed

    Gerhardt, K O; Gehrke, C W; Rogers, I T; Flynn, M A; Hentges, D J

    1977-05-21

    A method is described for the analysis of fecal neutral steriods with a dual-column gas-liquid chromatography (GLC) system. After saponification of the fecal slurry, the neutral steroids were extracted with hexane. The GLC separation of the compounds and quantitation were achieved by simultaneous injection of the derivatized and derivatized aliquots of the extract onto dual colmuns under identical conditions. The neutral steroids of interest were than identified by matching the retention times with those of known standards, and identification was confirmed by use of an interfaced GLC high-resolution mass spectrometry system. The detection limit was 0.003 mg of steroid/g of fecal slurry. The pricision of the method is illustrated by a relative standard diviation of 2-10% and a recovery of neutral steroids from 73-96%. The method was applied to the determination of fecal neutral steroids in a "High protein diet in colon cancer study". A considerably larger level of coprostanone than of coprostanol was observed. Data on neutral steroids in fecal samples from subjects on different diets are the subject of a separate publication. PMID:326802

  12. An uncooked vegan diet shifts the profile of human fecal microflora: computerized analysis of direct stool sample gas-liquid chromatography profiles of bacterial cellular fatty acids.

    PubMed Central

    Peltonen, R; Ling, W H; Hänninen, O; Eerola, E

    1992-01-01

    The effect of an uncooked extreme vegan diet on fecal microflora was studied by direct stool sample gas-liquid chromatography (GLC) of bacterial cellular fatty acids and by quantitative bacterial culture by using classical microbiological techniques of isolation, identification, and enumeration of different bacterial species. Eighteen volunteers were divided randomly into two groups. The test group received an uncooked vegan diet for 1 month and a conventional diet of mixed Western type for the other month of the study. The control group consumed a conventional diet throughout the study period. Stool samples were collected. Bacterial cellular fatty acids were extracted directly from the stool samples and measured by GLC. Computerized analysis of the resulting fatty acid profiles was performed. Such a profile represents all bacterial cellular fatty acids in a sample and thus reflects its microflora and can be used to detect changes, differences, or similarities of bacterial flora between individual samples or sample groups. GLC profiles changed significantly in the test group after the induction and discontinuation of the vegan diet but not in the control group at any time, whereas quantitative bacterial culture did not detect any significant change in fecal bacteriology in either of the groups. The results suggest that an uncooked extreme vegan diet alters the fecal bacterial flora significantly when it is measured by direct stool sample GLC of bacterial fatty acids. PMID:1482187

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

    USGS Publications Warehouse

    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.

  14. Combining NMR Spectroscopy and Gas-Liquid Chromatography for Analysis of the Fatty Acid Composition of Fenugreek Seed Oil (Trigonella foenum graecum L.)

    NASA Astrophysics Data System (ADS)

    Skakovskii, E. D.; Tychinskaya, L. Yu.; Mauchanava, V. A.; Karankevich, E. G.; Lamotkin, S. A.; Ahabalayeva, A. D.; Reshetnikov, V. N.

    2013-11-01

    1H and 13C NMR spectroscopy established that fenugreek seed oil consists mainly of triacylglycerides. Oleic and linoleic acids are found preferentially in the 2 position and α-linolenic acid is found preferentially in the 1,3 positions of the glycerol backbone. By combining NMR and gas-liquid chromatography, we have shown that fenugreek seeds contain 5.5 %-6.8 % oil, consisting mainly of unsaturated fatty acids (68.2 %-82.1 %): linoleic (31.3 %-46.8 %), α-linolenic (15.1 %-36.6 %), and oleic (11.6 %-21.3 %). The highest unsaturated fatty acid content is found in the cultivars D-19, Ovary Gold, Blidet, Ovary 4 and the lowest fatty acid content is found in the Metha cultivar. The percentage of polyunsaturated fatty acids is higher in oils of fenugreek cultivars from northern regions (Belarus, Hungary, France).

  15. 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

  16. 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.

  17. Capillary gas-liquid chromatography of 6-hydroxylated bile acids.

    PubMed

    Batta, A K; Aggarwal, S K; Tint, G S; Batta, M; Salen, G

    1995-06-01

    Gas-liquid chromatographic separation of several bile acids with a hydroxyl group at C-6 is described on two capillary columns, CP-Sil-19 CB and CP-Sil-5 CB. The gas-liquid chromatographic retention indices of bile acids with 6 alpha- and 6 beta-hydroxyl groups are compared with those of bile acids without the C-6 hydroxyl group and the effect of the C-6 hydroxyl group on the retention indices of bile acids is determined. Both 6 alpha- and 6 beta-hydroxyl groups increase the retention index of a bile acid. The retention indices of 6 alpha- or 6 beta-hydroxyl derivatives of chenodeoxycholic acid were found to be higher than those of the corresponding 6-hydroxy derivatives of cholic acid on the CP-Sil-19 CB column but lower on the CP-Sil-5 CB column. Although all 6-hydroxylated derivatives of lithocholic, chenodeoxycholic and cholic acids were not completely resolved on either column alone, combining the two columns resulted in the complete separation of all these compounds. PMID:7599745

  18. 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)

  19. DETERMINATION OF PENTACHLOROPHENOL IN MARINE BIOTA AND SEA WATER BY GAS-LIQUID CHROMATOGRAPHY AND HIGH-PRESSURE LIQUID CHROMATOGRAPHY

    EPA Science Inventory

    A method is described for measuring pentachlorophenol (PCP) in samples from the estuarine environment. Gas-liquid chromatography (GLC) is used to determine PCP residues in tissues as low as 0.01 ppm by formation of the ethyl diazohydrocarbon derivative, followed by Florisil clean...

  20. Assay of ambroxol in biological fluids by capillary gas-liquid chromatography.

    PubMed

    Schmid, J

    1987-02-20

    A sensitive and rapid method for the determination of ambroxol in biological fluids is described. It comprises a single extraction step, derivatization and selective determination with capillary gas-liquid chromatography (in split-mode) and electron-capture detection. The limit of quantification in plasma is ca. 3 ng/ml. The method is applied to the pharmacokinetics of ambroxol in humans. PMID:3571392

  1. Rapid differentiation of enterotoxigenic Escherichia coli that produce heat-stable and heat-labile toxins by frequency-pulsed electron capture gas-liquid chromatography analysis of diarrheal stool specimens.

    PubMed

    Brooks, J B; Basta, M T; el Kholy, A M; Moss, C W

    1984-12-01

    Thirty-three stool specimens from infants in the village of Tamooh near Cairo, Egypt, were studied by frequency-pulsed electron capture gas-liquid chromatography (FPEC-GLC). In 13 of the diarrheal cases, the suspected causative agent isolated was Escherichia coli which produced heat-stable toxin (ST), and in 10 other cases E. coli that produced heat-labile toxin (LT) were isolated. Ten control stool samples, collected from infants from whom no pathogenic organisms were isolated, were analyzed at the same time. Comparisons also were made against healthy control stools from individuals in the United States who had been previously analyzed by FPEC-GLC (Brooks et al., J. Clin. Microbiol. 20:549-560, 1984). The stools were suspended in water and centrifuged, and the supernatant was extracted with organic solvents and derivatized to form electron-capturing derivatives of carboxylic acids, hydroxy acids, alcohols, and amines. Results from the study showed distinct differences among the FPEC-GLC profiles of E. coli ST-positive stools, of E. coli LT-positive stools, and of the control stool samples. An unidentified compound appearing in the ether-soluble hydroxy acid fraction from E. coli ST-positive stools was tentatively identified by mass spectrometry as 6-methoxy-2-hydroxyhexanoic acid. 6-Methoxy-2-hydroxyhexanoic acid was found in all stools that contained E. coli ST but was not present either in stools from which E. coli LT was isolated or in control samples. 6-Methoxy-2-hydroxyhexanoic acid may prove to be an important marker for use in the identification of E. coli ST. In addition to 6-methoxy-2-hydroxyhexanoic acid, the carboxylic acid, alcohol, and amine FPEC-GLC profiles obtained from stools were very different between these two organisms. The data indicate that FPEC-GLC analysis of diarrheal stool specimens might be a rapid way to distinguish diarrhea caused by E. coli ST, E. coli LT, Clostridium difficile, and rotavirus. PMID:6394617

  2. Effect of different growth conditions on the discrimination of three bacteria by pyrolysis gas-liquid chromatography.

    PubMed Central

    Gutteridge, C S; Norris, J R

    1980-01-01

    High-resolution pyrolysis gas-liquid chromatography was applied to three bacteria (Escherichia coli NCTC 9001, Pseudomonas putida (NCIB 9494, and Staphylococcus aureus NCTC 8532) grown under a variety of conditions. Changing the culture medium drastically altered the quantitative aspects of the pyrograms of all three organisms, but the effects of culture time and incubation temperature were less severe. Mathematical analysis of the relative peak heights showed that four peaks could be used to discriminate the three bacteria however they were cultured. PMID:6999989

  3. Lipid Patterns of Selected Microorganisms as Determined by Gas-Liquid Chromatography1

    PubMed Central

    Steinhauer, John E.; Flentge, Robert L.; Lechowich, Richard V.

    1967-01-01

    The cellular lipid patterns of seven strains of microorganisms were examined by gas-liquid chromatography in this preliminary study. The chloroform methanol-soluble lipids were extracted by the Soxhlet method from dried cultures which had been grown at 25 ± 2 C for 18 hr with mechanical shaking. The cellular extract was methylated by use of a low temperature sulfuric acid method, and the resulting methyl esters were chromatographed. Considerable differences in the lipid patterns among the seven microorganisms tested indicated that this method might be useful for the identification of closely related microbial genera, and possibly for species differentiation. PMID:4860530

  4. Application of gas-liquid chromatography to the routine identification of nonfermenting gram-negative bacteria in clinical specimens.

    PubMed Central

    Veys, A; Callewaert, W; Waelkens, E; Van den Abbeele, K

    1989-01-01

    A total of 430 strains of glucose-nonfermenting gram-negative bacteria representing 35 species were analyzed for their cellular fatty acid composition by gas-liquid chromatography (GLC). On the basis of qualitative differences in their cellular fatty acid composition, these bacteria could be divided into 19 distinct chromatographic groups. Eight Pseudomonas species, Achromobacter xylosoxidans, group Vd, and Agrobacterium radiobacter were identified from their fatty acid compositions alone. The other glucose-nonfermenting gram-negative bacterial species studied here, classified within nine distinct GLC groups, were easily recognized by using the GLC fatty acid analysis supplemented with a limited number of conventional biochemical tests. The results support the hypothesis that bacterial fatty acid composition is rather specific and that qualitative GLC fatty acid analysis can be adapted in the clinical laboratory either to provide additional criteria for differentiation of closely related groups or to serve as a rapid and highly reproducible method for their routine identification. PMID:2768442

  5. 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

  6. Therapeutic drug assays with gas-liquid chromatography and optical detection.

    PubMed

    Karmen, A; Pritchett, T; Lam, S

    1981-11-01

    Clofibric acid (p-chlorophenoxyisobutyric acid), the major metabolite of Clofibrate, a drug used in the treatment of hyperlipemia, was assayed in blood serum using an ultraviolet absorbance monitor as a gas-liquid chromatographic detector. As in other gas-liquid chromatographic assays for this compound, an internal standard, p-chlorophenoxyacetic acid, was added, and the serum was acidified and extracted with organic solvent. The solvent was then evaporated and the acids converted into their methyl esters for analysis. The organic compounds in the effluent were scrubbed into a stream of 2-propanol, at a flow-rate of 0.5 ml/min. This was then "debubbled" and a portion drawn through the 20-microliters UV detector flow cell. With small-volume scubber and associated components, peak-broadening was minimal. Because of their moderately high extinction coefficients at 280 nm, the Clofibrate and the internal standard were detected in the submicrogram range without interference from long-chain fatty acid esters, which have similar retention times on the column used. PMID:7320112

  7. 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

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

    PubMed

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

    1983-02-01

    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

  9. Scaling analysis of gas-liquid two-phase flow pattern in microgravity

    NASA Technical Reports Server (NTRS)

    Lee, Jinho

    1993-01-01

    A scaling analysis of gas-liquid two-phase flow pattern in microgravity, based on the dominant physical mechanism, was carried out with the goal of predicting the gas-liquid two-phase flow regime in a pipe under conditions of microgravity. The results demonstrated the effect of inlet geometry on the flow regime transition. A comparison of the predictions with existing experimental data showed good agreement.

  10. Pyrolysis-gas-liquid chromatography with atomic emission detection for the identification of Corynebacterium species.

    PubMed

    Voisin, S; Renaud, F N; Freney, J; de Montclos, M; Boulieu, R; Deruaz, D

    1999-11-26

    We report here the application of pyrolysis-gas chromatography followed by atomic emission detection (AED) for the characterisation of microorganisms. AED measured the quantity of carbon, sulfur and nitrogen in the molecules separated chromatographically. Twenty-three strains, representing eight Corynebacterium species, were tested in this preliminary study. Co-ordinate principal analysis grouped 11 strains in their respective species group. Most of the other strains appear randomly distributed, perhaps because these strains require additional nutrients. These preliminary results show that the method could be used as a tool for the taxonomic and perhaps the epidemiologic characterisation of bacteria. PMID:10593504

  11. Analysis of Developing Gas/liquid Two-Phase Flows

    SciTech Connect

    Elena A. Tselishcheva; Michael Z. Podowski; Steven P. Antal; Donna Post Guillen; Matthias Beyer; Dirk Lucas

    2010-06-01

    The goal of this work is to develop a mechanistically based CFD model that can be used to simulate process equipment operating in the churn-turbulent regime. The simulations were performed using a state-of-the-art computational multiphase fluid dynamics code, NPHASE–CMFD [Antal et al,2000]. A complete four-field model, including the continuous liquid field and three dispersed gas fields representing bubbles of different sizes, was first carefully tested for numerical convergence and accuracy, and then used to reproduce the experimental results from the TOPFLOW test facility at Forschungszentrum Dresden-Rossendorf e.V. Institute of Safety Research [Prasser et al,2007]. Good progress has been made in simulating the churn-turbulent flows and comparison the NPHASE-CMFD simulations with TOPFLOW experimental data. The main objective of the paper is to demonstrate capability to predict the evolution of adiabatic churn-turbulent gas/liquid flows. The proposed modelling concept uses transport equations for the continuous liquid field and for dispersed bubble fields [Tselishcheva et al, 2009]. Along with closure laws based on interaction between bubbles and continuous liquid, the effect of height on air density has been included in the model. The figure below presents the developing flow results of the study, namely total void fraction at different axial locations along the TOPFLOW facility test section. The complete model description, as well as results of simulations and validation will be presented in the full paper.

  12. Data evaluation in chromatography by principal component analysis.

    PubMed

    Cserháti, T

    2010-01-01

    The newest achievements in the employment of principal component analysis, a multivariate mathematical statistical method, in the evaluation of chromatographic retention data are compiled. The results obtained by various chromatographic technologies such as gas-liquid chromatography, thin-layer chromatography, high-performance liquid chromatography and electrically driven systems are compiled and briefly discussed. PMID:19629960

  13. Determination of altosid insect growth regulator in waters, soils, plants, and animals by gas-liquid chromatography.

    PubMed

    Miller, W W; Wilkins, J S; Dunham, L L

    1975-01-01

    Residues of isopropyl (2E,4E)-11-methoxy-3,7,11-trimethyl-2,4-dodecadienoate (Altosid) insect growth regulator are determined in waters, soils, plants, milk, eggs, fish, shellfish, poultry and cattle tissues, blood, urine, and feces. Acetonitrile is the primary extraction solvent for all samples. Residues are extracted by high-speed blending followed by vacuum filtration. Fatty extracts are subjected to cold-temperature precipitation and filtration. Samples are cleaned up by petroleum ether partitioning and Florisil and neutral alumina chromatography. The concentrated eluants are analyzed by gas-liquid chromatography (GLC) on columns of differing polarity, using hydrogen flame ionization detectors. The identity of suspected residues is confirmed by additional GLC and by mass fragmentography. The lower limits of detection were: water samples, 0.0004-0.001 ppm; soils, blood, and urine, 0.001 ppm; forage grasses, forage legumes, and rice foliage, 0.005 ppm; and milk, eggs, fish, shellfish, poultry and cattle tissues, and feces, 0.010 ppm. PMID:1141142

  14. 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.

  15. Use of gas-liquid chromatography as a screening test for toxigenic Clostridium difficile in diarrhoeal stools.

    PubMed Central

    Pepersack, F; Labbe, M; Nonhoff, C; Schoutens, E

    1983-01-01

    In order to determine if gas-liquid chromatography (GLC) on concentrated stool extracts could be substituted to cell culture assay for cytotoxicity, we prospectively studied 154 diarrhoeal stools submitted for detection of Clostridium difficile toxin. Isocaproic-positive samples were cultured on egg yolk agar supplemented with cycloserine, cefoxitin and fructose for isolation of C difficile, and on egg yolk agar plus kanamycin for isolation of other clostridium species. Of the 154 samples, 129 were GLC-negative (height of the isocaproic peak less than 1.2 cm) and were toxin-negative. Twenty-five stools yielded isocaproic acid; C difficile isolated from 13 of them, six of which were also toxin-positive. Four other isocaproic-positive samples yielded C bifermentans and C sordellii; all were toxin-negative. These results indicate that a negative GLC is an excellent screening test for excluding C difficile infection; positive results must be checked by toxin testing and culture since they are not necessarily associated with the presence of C difficile or its toxin. PMID:6630574

  16. Evaluation and Quantitation of Intact Wax Esters of Human Meibum by Gas-Liquid Chromatography-Ion Trap Mass Spectrometry

    PubMed Central

    Butovich, Igor A.; Arciniega, Juan C.; Lu, Hua; Molai, Mike

    2012-01-01

    Purpose. Wax esters (WE) of human meibum are one of the largest group of meibomian lipids. Their complete characterization on the level of individual intact lipid species has not been completed yet. We obtained detailed structural information on previously uncharacterized meibomian WE. Methods. Intact WE were separated and analyzed by means of high-temperature capillary gas-liquid chromatography (GLC) in combination with low voltage (30 eV) electron ionization ion trap mass spectrometry (ITMS). 3D (mass-to-charge ratio [m/z] versus lipid sample weight versus signal intensity) calibration plots were used for quantitation of WE. Results. We demonstrated that GLC-ITMS was suitable for analyzing unpooled/underivatized WE collected from 14 individual donors. More than 100 of saturated and unsaturated WE (SWE and UWE, respectively) were detected. On average, UWE represented about 82% of the total WE pool. About 90% of UWE were based on oleic acid, while less than 10% were based on palmitoleic acid. The amounts of poly-UWE were <3% of their mono-UWA counterparts. SWE were based primarily on C16–C18 fatty acids (FA) in overall molar ratios of 22:65:13. A pool of C16:0-FA was comprised of a 20:80 (mol/mol) mixture of straight chain and iso-branched isomers, while the corresponding ratio for C18:0-FA was 43:57. Interestingly, C17:0-FA was almost exclusively branched, with anteiso- and iso-isomers found in a ratio of 93:7. Conclusions. GLC-ITMS can be used successfully to analyze more than 100 individual species of meibomian WE, which were shown to comprise 41 ± 8% (wt/wt) of meibum, which made them the largest group of lipids in meibum. PMID:22531701

  17. Differentiation of Peptococcus and Peptostreptococcus by gas-liquid chromatography of cellular fatty acids and metabolic products.

    PubMed Central

    Lambert, M A; Armfield, A Y

    1979-01-01

    Gas-liquid chromatographic (GLC) profiles of cellular fatty acids and metabolic products were useful in identifying strains of Peptococcus saccharolyticus, Peptococcus asaccharolyticus, Peptostreptococcus anaerobius, Peptostreptococcus micros, and Streptococcus intermedius. The GLC results supported the recent taxonomic decision to transfer aerotolerant Peptostreptococcus species to the genus Streptococcus. Because inconsistencies in the results prevented our differentiating Peptococcus prevotii. Peptococcus magnus, and Peptococcus variabilis by GLC, additional strains will have to been examined. These GLC techniques are amenable to routine use; however, for interlaboratory results to be meaningful, the classification and nomenclature of the anaerobic gram-positive cocci should be standardized. PMID:528680

  18. Rapid diagnosis of beta-haemolytic streptococcus group B endocarditis by buffy-coat examination and gas-liquid chromatography.

    PubMed Central

    Maliwan, N; Reid, R; Katzen, R

    1979-01-01

    A semicomatose 34-year-old man had fever, heart murmur, and multiple gangrenous lesions. Several blood cultures were negative. Cultures of the heart valve grew beta-haemolytic streptococcus group B. The organism was seen in buffy-coat examination of the venous blood. The gas-liquid chromatogram of the serum was different from those of normal controls and of patients with invasive candida infection; it closely mimicked the one obtained from the organism itself. These studies promise to be valuable diagnostic adjuncts. Images Fig. 1 PMID:92481

  19. Comparison of dieldrin, lindane, and DDT extractions from serum, and gas-liquid chromatography using glass capillary columns.

    PubMed

    Franken, J J; Luyten, B J

    1976-11-01

    Rats were given an oral dose of 14C-labeled chlorinated pesticides to obtain serum containing p,p'-DDT, dieldrin, or lindane. Simple hexane and formic acid-hexane extraction methods, involving pretreatment of the serum with formic acid, were compared by radiometric and by paper chromatographic and gas chromatographic analysis. In vivo binding of chlorinated pesticides to constituents of the serum does not necessarily prohibit their isolation by simple hexane extractions, provided that the extraction is very vigorous and at least 5 min long. Stable emulsions were broken by cooling in liquid nitrogen or Dry Ice-acetone. The hexane extraction method described yields quantitative recovery of the pesticides studied, whereas the formic acid-hexane method is quantitative for p,p'-DDT, 93% for dieldrin, and 89% for lindane. Gas chromatographic comparison of both methods, using human serum, shows that the hexane method extracts 16% more beta-BHC, 7% more dieldrin and HCB, and 4% more p,p'-DDE from serum than does the formic acid-hexane method. The difference for p,p'-DDT is not significant. Gas chromatography with glass capillary columns and an all-glass solids injection system yielded detection limits as low as 15 fg. Data show that the use of an internal standard considerably improves the precision of quantitation. PMID:62748

  20. Gas-liquid chromatography of polychlorinated biphenyl congeners between a nematic liquid crystal phase and a nonpolar phase

    SciTech Connect

    Zielinski, W.L. Jr.; Miller, M.M.; Ulma, G.; Wasik, S.P.

    1986-11-01

    The gas-liquid chromatographic retention behavior of 54 polychlorinated biphenyl (PCB) congeners containing one to ten chlorine atoms was evaluated on a nematic liquid crystal (N,N'-bis(p-methoxybenzylidene)-..cap alpha..,..cap alpha..'-bi-p-toluidine, BMBT). To a first approximation, as anticipated, retention on the liquid crystal appeared to be enhanced with an increasing molecular length-to-breadth ratio for congeners containing the same number of chlorine atoms. The retention behavior of 38 of the PCB's also was examined on a nonselective, nonpolar stationary phase (Apolane-87) in which retention is controlled more by solute vapor pressure differences than by solute-stationary phase free energy effects. The difference in the free energy of mixing of PCB solute pairs between the two phases was found to be predominantly greater in the liquid crystal phase, demonstrating an enhanced selectivity for PCB isomer separations over nonpolar phases. The retention data suggest that the separation of many of the congeners might be improved by using a liquid crystal stationary phase.

  1. [The study of vapor-liquid equilibria for polymer/solvents by using gas-liquid chromatography].

    PubMed

    Xie, J

    1999-05-01

    The infinite dilution weight fraction activity coefficient, omega 1 infinity, and Flory-Huggins interaction parameter, chi, have been determined for systems of polydimethylsiloxane (PDMS)/solvents and polymethyl-methacrylate (PMMA)/solvents by using gas chromatography from 58 degrees C to 180 degrees C. The solvents include styrene, acetone, ethyl ether, methanol, ethanol, acetic acid, trichloromethane, tetrahydrofuran and ethyl acetate in PDMS/solvent systems and n-hexane, n-heptane, cyclohexane, benzene, toluene, ethyl benzene, styrene, acetone, ethyl ether, methanol, ethanol, methyl methacrylate(MMA), trichloromethane, tetrahydrofuran and ethyl acetate in the PMMA/solvent systems. The results showed that omega 1 infinity and chi were decreased with the increase of temperature in the range from 58 degrees C to 180 degrees C. The study showed that UNIFAC and UNIFAC-FV models could not all be used to estimate omega 1 infinity of the solvents in PMMA/solvent systems. Therefore, UNIFAC and UNIFAC-FV models must be corrected or other models must be used. PMID:12549114

  2. Gas/liquid chromatographic analysis of pemoline in biological fluids using electron capture detection.

    PubMed

    Igwe, O J; Blake, J W

    1981-12-01

    An analytical gas/liquid chromatographic (GLC) protocol is described for the quantitation of pemoline in biological fluids of the horse. Plasma samples containing known quantities of pemoline and its analog as an internal standard (IS) were deproteinized with 5-sulfosalicylic acid, heated at 80 degree C, and centrifuged. 5-Phenyl-2,4-oxazolidinedione, the hydrolytic product of pemoline in acid medium, was extracted with dichloromethane (DCM). The organic layer was in turn re-extracted with 1% NaHCO3. The aqueous layer was acidified with HCI, and re-extracted with DCM, which was evaporated to dryness. The resulting residue was methylated with ethereal diazomethane. The methylated dione was dissolved in benzene, and analyzed with a gas/liquid chromatograph equipped with a tritiated scandium foil (Sc3H) electron capture detector (ECD). Urine samples to which pemoline was added were hydrolyzed with hydrochloric acid and carried through the analytical procedure in a manner similar to the plasma, except that the urine was further washed with lead acetate solution prior to the sodium bicarbonate extraction. The lower limits of detection were found to be 0.05 microgram/ml for plasma and 0.1 microgram/ml for urine when 1.0 ml of sample was used. This procedure can be used for pemoline detection control in international sporting events. PMID:7328158

  3. Lagrangian coherent structures analysis of gas-liquid flow in a bubble column

    NASA Astrophysics Data System (ADS)

    Wu, Qin; Wang, GuoYu; Huang, Biao; Bai, ZeYu

    2014-06-01

    The objective of this paper is to apply a new identifying method to investigating the gas-liquid two-phase flow behaviors in a bubble column with air injected into water. In the numerical simulations, the standard k- ɛ turbulence model is employed to describe the turbulence phenomenon occurring in the continuous fluid. The Finite-Time Lyapunov Exponent (FTLE) and Lagrangian Coherent Structures (LCS) are applied to analyze the vortex structures in multiphase flow. Reasonable agreements are obtained between the numerical and experimental data. The numerical results show that the evolution of gas-liquid in the column includes initial and periodical developing stages. During the initial stage, the bubble hose is forming and extending along the vertical direction with the vortex structures formed symmetrically. During the periodical developing stage, the bubble hose starts to oscillate periodically, and the vortexes move along the bubble hose to the bottom of column alternately. Compared to the Euler-system-based identification criterion of a vortex, the FTLE field presents the boundary of a vortex without any threshold defined and the LCS represents the divergence extent of infinite neighboring particles. During the initial stage, the interfaces between the forward and backward flows are highlighted by the LCS. As for the periodical developing stage, the LCS curls near the vortex centers, providing a method of analyzing a flow field from a dynamical system perspective.

  4. 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

    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.

  5. Estimation and Validation of Propanil Residues in Rice and Soil Samples by Gas Liquid Chromatography with Electron Capture Detector.

    PubMed

    Sandhu, Amanpal Kaur; Mandal, Kousik; Singh, Balwinder

    2015-09-01

    The purpose of this analysis was to develop an efficient analysis for the estimation of residues of propanil in rice grain, husk, straw and soil samples. A liquid-liquid partitioning method was used for the extraction of propanil residues from the rice grains and its contents. For this, representative 10 g samples of blended rice grain, husk, straw and soil were soaked in acetone for 24 h, and the contents then partitioned two times into 100 and 50 mL dichloromethane and one time with 100 mL hexane. The combined organic layers were collected and were concentrated to 10 mL acetone using a rotary vacuum evaporator at 40°C. The extract was then subjected to cleanup by dispersive solid phase extraction. The final extract was injected onto a GLC column, where the propanil residues were determined by electron capture detector. The percentage recoveries were ranged from 84.9 % to 98.3 % when samples were spiked at the levels of 0.05, 0.25 and 0.50 mg/kg. The limits of quantification and detection were 0.05 and 0.017 mg/kg, respectively. PMID:26232197

  6. Theoretical and experimental analysis of a multiphase screw pump, handling gas-liquid mixtures with very high gas volume fractions

    SciTech Connect

    Raebiger, K.; Maksoud, T.M.A.; Ward, J.; Hausmann, G.

    2008-09-15

    In the investigation of the pumping behaviour of multiphase screw pumps, handling gas-liquid mixtures with very high gas volume fractions, theoretical and experimental analyses were performed. A new theoretical screw pump model was developed, which calculates the time-dependent conditions inside the several chambers of a screw pump as well as the exchange of mass and energy between these chambers. By means of the performed experimental analysis, the screw pump model was verified, especially at very high gas volume fractions from 90% to 99%. The experiments, which were conducted with the reference fluids water and air, can be divided mainly into the determination of the steady state pumping behaviour on the one hand and into the analysis of selected transient operating conditions on the other hand, whereas the visualisation of the leakage flows through the circumferential gaps was rounded off the experimental analysis. (author)

  7. Determination of endotoxin by the measurement of the acetylated methyl glycoside derivative of Kdo with gas-liquid chromatography-mass spectrometry.

    PubMed

    Rybka, J; Gamian, A

    2006-02-01

    A gas-liquid chromatographic-mass spectrometric (GLC-MS) method was applied to the detection of 3-deoxy-d-manno-2-octulosonic acid (Kdo), a constituent of bacterial lipopolysaccharide (LPS, endotoxin). Samples containing LPS were dried, methanolyzed with 2 M HCl in methanol at 60 degrees C for 1 h and acetylated with acetic anhydride and pyridine (1:1, v/v) solution at 100 degrees C for 30 min, then the products were analyzed by GLC-MS or GLC-MSMS. Four acetylated methylglycoside methyl ester derivatives of Kdo are formed in these conditions, namely one with pyranose ring (Kdo1), two derivatives in the furanose form (Kdo2 and 3) and one derivative of anhydro Kdo (Kdo4), as results from their mass fragmentation patterns. Synthetic Kdo produced mainly Kdo4 derivative, whereas Kdo1 of pyranose ring shape was the predominating derivative formed from LPS. The ion fragment of m/z 375 was selected for the specific detection of this Kdo1 derivative, which might be applied for the endotoxin determination. That approach was used for the analysis of preparations of bacteria, bacteriophages and samples of animal sera. In order to ensure the removal of phosphate substitutions from Kdo, methanolyzed samples can be treated with alkaline phosphatase (2.6 U, pH 9.2, 37 degrees C, 15 min), what was elaborated on Vibrio LPS preparation. PMID:15932775

  8. Exergy destruction analysis of a vortices generator in a gas liquid finned tube heat exchanger: an experimental study

    NASA Astrophysics Data System (ADS)

    Ghazikhani, M.; Khazaee, I.; Monazzam, S. M. S.; Takdehghan, H.

    2016-01-01

    In the present work, the effect of using different shapes of vortices generator (VG) on a gas liquid finned heat exchanger is investigated experimentally with irreversibility analysis. In this project the ambient air with mass flow rates of 0.047-0.072 kg/s is forced across the finned tube heat exchanger. Hot water with constant flow rate of 240 L/h is circulated inside heat exchanger tubes with inlet temperature range of 45-73 °C. The tests are carried out on the flat finned heat exchanger and then repeated on the VG finned heat exchanger. The results show that using the vortex generator can decrease the ratio of air side irreversibility to heat transfer (ASIHR) of the heat exchanger. Also the results show that the IASIHR is >1.05 for all air mass flow rates, which means that ASIHR for the initial heat exchanger is higher than 5 % greater than that of improved heat exchanger.

  9. Modal Wavelets Analysis to Gas-Liquid Two Phase Flow PIV Images

    SciTech Connect

    Masahiro Takei; Hassan, Yassin A.; Ortiz-Villafuerte, J.; Tomomasa Uemura

    2006-07-01

    A modal wavelet transform, which overcomes the intrinsic data number limitation of power of two to conventional wavelet transform, has been applied to analysis of pseudo and real bubbly flow PIV images. The modal wavelet transform is compared with the discrete wavelet transform in order to select the best base function among Neumann, Dirichlet and Green function types base functions. Consequently, it is verified that Neumann type base function is the best because the correlation of Neumann type base function is the highest. From the result of wavelet analysis of the real bubbly flow PIV image, as the relative velocity is higher, the dominant eddy scale becomes smaller. The extraction modal wavelet level depends on the base function. (authors)

  10. Determination of partition coefficients of refrigerants by gas liquid chromatographic headspace analysis.

    PubMed

    Abraham, Michael H; Gil-Lostes, Javier; Corr, Stuart; Acree, William E

    2012-11-23

    Gas-water partition coefficients, K(w), and gas-solvent partition coefficients, K(s), have been determined for chlorodifluoromethane and for 1,1,1,3,3,3-hexafluoropropane by headspace analysis, using a very simple experimental procedure. These partition coefficients then yield water-solvent partition coefficients, P(s). Where comparisons can be made there is excellent agreement with literature values for K(w) and P(s). The obtained values of K(s) and P(s) can be used to obtain physicochemical properties, or descriptors, for the refrigerants. Combination of these descriptors with previous equations we have developed enables partition coefficients to be obtained for a host of systems. PMID:23089519

  11. Transfer processes in gas-liquid systems

    NASA Astrophysics Data System (ADS)

    Fedorovskii, Aleksandr D.; Nikiforovich, Evgenii I.; Prikhod'Ko, Nikolai A.

    Hydrodynamic processes occurring near gas-liquid interfaces and in gas-liquid flow are examined with reference to the results of recent theoretical and experimental studies. In particular, attention is given to the dynamics of stratified media without internal heat sources; asymptotic analysis of the Navier-Stokes equation in problems of the dynamics of stratified media with internal heat sources; a mathematical model of the temperature skin layer; and methods for visualizing hydrodynamic processes. The discussion also covers remote optical methods for studying the temperature fields on a water surface; dynamics and heat transfer of a single gas bubble in a liquid; and approximate methods for calculating gas-liquid bubble flows.

  12. 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%.

  13. Gas-liquid chromatography-tandem mass spectrometry methodology for the quantitation of estrogenic contaminants in bile of fish exposed to wastewater treatment works effluents and from wild populations.

    PubMed

    Fenlon, Kate A; Johnson, Andrew C; Tyler, Charles R; Hill, Elizabeth M

    2010-01-01

    Fish can be exposed to a complex mixture of chemical contaminants arising from the exposure to wastewater treatment works (WwTWs) effluents. Some of these contaminants are estrogenic and have been associated with feminisation of male fish and the presence of populations containing intersex individuals. However the detection of trace levels (ng/L) of estrogenic chemicals surface waters can be difficult and does not give information on the exposure of aquatic organisms to these contaminants. In this study we assessed whether the analysis of estrogenic substances that bioconcentrate in fish bile can be used to detect the exposure of fish to feminising contaminants in receiving waters and effluents, and thus facilitate their monitoring of these substances in aquatic environments. Estrogenic metabolites in bile were deconjugated using enzymatic hydrolysis and partially purified by solid phase extraction. Steroidal and xenoestrogens were derivatized to their trimethylsilyl ethers and quantified by gas-liquid chromatography-mass spectrometry (GC-MS/MS) using multiple reaction monitoring. The method was validated using spiked bile samples from immature female rainbow trout (Oncorhynchus mykiss) as well as bile from sexually mature roach (Rutilus rutilus) that had been exposed to either tap water or an undiluted estrogenic effluent for 10 days or captured from a river site downstream of a WwTWs effluent discharge. The mean recovery of target analytes from spiked bile was between 86 and 99% and the limit of detection was between 0.1 and 0.7ng/mL bile for bisphenol A (BPA), 17beta-estradiol (E2), estrone (E1) and 17alpha-ethinylestradiol (EE2), and 11, 60 and 327ng/mL bile for branched nonyl chain isomeric mixtures of 4-nonylphenolethoxylate (NP1EO), 4-nonylphenol (NP) and 4-nonylphenoldiethoxylate (NP2EO), respectively. All target analytes were detected in bile from roach exposed directly to a WwTWs effluent, with concentrations between 6-13microg/mL bile for NP, 18-21microg/mL for NP1EO, 75-135microg/mL for NP2EO, 0.7-2.5microg/mL for BPA, E2 and E1 and 17-29ng/mL for EE2. With the exception of NP2EO, all analytes were detected in at least 2 out of the 5 fish sampled from the River Thames. BPA and NP1EO were detected in all three reference fish held in tap water indicating possible contamination from laboratory plastics. The work shows that analysis of 20-100microL quantities of bile could be a useful approach in detecting exposure to mixtures of estrogenic contaminants taken up by fish from WwTW effluents and has the potential for monitoring the efficacy of remediation strategies that may be adopted for reduction of these endocrine disrupting chemicals in the aquatic environment. PMID:19932485

  14. Differentiation of Corynebacterium amycolatum, C. minutissimum, C. striatum and related species by pyrolysis-gas-liquid chromatography with atomic emission detection.

    PubMed

    Voisin, Sébastien; Deruaz, Daniel; Freney, Jean; Renaud, François N R

    2002-06-01

    We report here the application of pyrolysis-gas chromatography followed by atomic emission detection (AED) for the characterisation of Corynebacterium amycolatum and related species (i.e., C. striatum, C. minutissimum, C. xerosis and the recently described C. freneyi). This phenotypic method, which analyses the whole chemical composition of bacteria, clearly separates C. amycolatum from other species. Moreover, this C. amycolatum group is subdivided into two distinct subgroups. We cannot differentiate the C. minutissimum strains from those of C. striatum. On the other hand, C. freneyi and C. xerosis are clearly distinct from the other species. PMID:12160322

  15. A method for the confirmation and identification of drugs of misuse in urine using solid phase extraction and gas-liquid chromatography with mass spectrometry.

    PubMed Central

    Galloway, J H; Ashford, M; Marsh, I D; Holden, M; Forrest, A R

    1998-01-01

    A method is described for the confirmation/identification of a range of commonly misused drugs in urine samples. The method has been used for two years without problems for a range of purposes including hospital/clinic drugs of misuse screening and for toxicology in coroner's cases. Urine samples which have given a positive result on immunochemical screening for a particular drug group or groups (for example, opiates) can be processed with identification of the drugs present using a single procedure. Bond ElutCertify columns are used for the extraction of drugs from the samples followed by propionylation and gas chromatography with mass selective detection. PMID:9659249

  16. Gas-Liquid Chromatographic Isolation of Cytokinins from Natural Sources

    PubMed Central

    Upper, C. D.; Helgeson, John P.; Kemp, John D.; Schmidt, C. J.

    1970-01-01

    Gas-liquid chromatographic retention times for 20 purines or purine nucleosides, 14 of which are highly active cytokinins, are reported. With one exception, all of the naturally occurring cytokinins are separated. Ethyl acetate extraction of yeast transfer RNA hydrolysates and of culture filtrates of Agrobacterium tumefaciens gave sufficient concentration of the naturally occurring cytokinins for immediate gas-liquid chromatography. This procedure permitted the detection of 6-(3-methyl-2-butenylamino)-9-β, d-ribofuranosylpurine in yeast transfer RNA extracts. An active cytokinin was isolated from A. tumefaciens culture filtrates and was tentatively identified as 6-(3-methyl-2-butenylamino)purine. PMID:16657339

  17. Gas-liquid chromatographic determination of 3-trifluoromethyl-4-nitrophenol in natural waters.

    PubMed

    Coburn, J A; Chau, A S

    1976-07-01

    A procedure for the analysis of 3-trifluoromethyl-4-nitrophenol (TFM) in natural waters is described. The lampricide is extracted from acidified water samples on the macroreticular resin XAD-7 and eluted from the column with ethyl ether. The ether extract is dried, concentrated, and partitioned with potassium carbonate. TFM is acetylated in the aqueous alkaline solution and the acetate derivative is extracted into benzene for analysis by electron capture gas-liquid chromatography. Recoveries of TFM from natural waters exceeded 90% and as little as 0.01 mug TFM can be quantitated in a 1 L sample. PMID:939751

  18. Gas-liquid flows -- 1993

    SciTech Connect

    Rohatgi, U.S. ); Kim, J.H. ); O'Hern, T. ); Sharma, M.P. ); Shoukri, M. )

    1993-01-01

    This symposium was sponsored by the Multiphase Flow Committee of the ASME Fluids Engineering Division. The objective of the symposium was to bring together researchers, and practicing engineers in the area of gas-liquid flows, to share their knowledge and discuss the state of the art. Gas-liquid flows appear in a multitude of settings, some natural and some designed to achieve desired functions. Examples of the latter type of two-phase flows are: spray, drying, atomization, boiling which occurs in scrubbers, fountains, boilers, etc. However, two-phase flow can also appear in systems which are in accident conditions such as inadvertent depressurization or heat up in nuclear reactors. The gas-liquid flows offer a challenge to our understanding, due to the complex and stochastic nature of the interface. the flow regime determination is crucial for estimating the interfacial transfer processes. The modeling of two-phase flow requires many empirical correlations such as interfacial area density or coefficients of transfer processes at the interface or at the wall. The scaling of two-phase flow provides another challenge as there are many length and time scales in every flow regime. Papers cover modeling, theory and experiments. The papers are arranged in six sessions. The first two sessions deal with the experiments and the remaining four describe the analytical effort. All papers were processed separately for inclusion on the data base.

  19. 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.

  20. Analysis of energetic materials by ion chromatography

    SciTech Connect

    Hershey, M.K.

    1985-01-01

    Ion chromatography is a rapid, sensitive, and selective method for ion analysis in a variety of matrices. Ion chromatography was used to determine levels on chloride and chlorate in potassium perchlorate. Comparisons were made with the specific ion electrons method presently being used for these analyses. Also to be discussed are ion chromatographic methods for determining ammonium in boron potassium nitrate, and chloride and ammonium in CP.

  1. Rapid differentiation of rocky mountain spotted fever from chickenpox, measles, and enterovirus infections and bacterial meningitis by frequency-pulsed electron capture gas-liquid chromatographic analysis of sera.

    PubMed Central

    Brooks, J B; McDade, J E; Alley, C C

    1981-01-01

    Normal sera and sera from patients with Rocky Mountain spotted fever, chickenpox, enterovirus infections, measles, and Neisseria meningitidis infections were extracted with organic solvents under acidic and basic conditions and then derivatized with trichloroethanol or heptafluorobutyric anhydride-ethanol to form electron-capturing derivatives of organic acids, alcohols, and amines. The derivatives were analyzed by frequency-pulsed electron capture gas-liquid chromatography (FPEC-GLC). There were unique differences in the FPEC-GLC profiles of sera obtained from patients with these respective diseases. With Rocky Mountain spotted fever patients, typical profiles were detected as early as 1 day after onset of disease and before antibody could be detected in the serum. Rapid diagnosis of Rocky Mountain spotted fever by FPEC-GLC could permit early and effective therapy, thus preventing many deaths from this disease. PMID:7276147

  2. Microfluidic study of fast gas-liquid reactions.

    PubMed

    Li, Wei; Liu, Kun; Simms, Ryan; Greener, Jesse; Jagadeesan, Dinesh; Pinto, Sascha; Gnther, Axel; Kumacheva, Eugenia

    2012-02-15

    We present a new concept for studies of the kinetics of fast gas-liquid reactions. The strategy relies on the microfluidic generation of highly monodisperse gas bubbles in the liquid reaction medium and subsequent analysis of time-dependent changes in bubble dimensions. Using reactions of CO(2) with secondary amines as an exemplary system, we demonstrate that the method enables rapid determination of reaction rate constant and conversion, and comparison of various binding agents. The proposed approach addresses two challenges in studies of gas-liquid reactions: a mass-transfer limitation and a poorly defined gas-liquid interface. The proposed strategy offers new possibilities in studies of the fundamental aspects of rapid multiphase reactions, and can be combined with throughput optimization of reaction conditions. PMID:22176612

  3. APPLICATION OF GAS CHROMATOGRAPHY IN FOOD ANALYSIS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Gas chromatography (GC) is used widely in applications involving food analysis. Typical applications pertain to the quantitative and/or qualitative analysis of food composition, natural products, food additives, flavor and aroma components, a variety of transformation products, and contaminants suc...

  4. Paper Chromatography as an Adjunct in the Identification of Anaerobic Bacteria

    PubMed Central

    Slifkin, M.; Hercher, H. J.

    1974-01-01

    Modified paper chromatography procedures for the analysis of fatty acids produced by anaerobic bacteria are described. Both ethylamine and hydroxylamine derivatives of fatty acids were prepared from inoculated anaerobic culture broth. The derivatives were spotted on chromatography paper and developed with appropriate solvents. Paper chromatography is a valuable alternative to gas liquid chromatography as an ancillary procedure in the identification of anaerobic bacteria in the clinical bacteriology laboratory. PMID:4596386

  5. Chromatography in authenticity and traceability tests of vegetable oils and dairy products: a review.

    PubMed

    Cserháti, Tibor; Forgács, Esther; Deyl, Zdenek; Miksik, Ivan

    2005-04-01

    The new applications of various chromatographic techniques such as gas-liquid chromatography, high-performance liquid chromatography and electrophoretic methods employed for the analysis in macro- and micro-components in vegetable oils and dairy products are compiled and critically evaluated. The employment of these methods for authenticity tests and traceability is discussed. PMID:15803455

  6. Gas/liquid separation device

    SciTech Connect

    Takeyama, Masaki; Igashira, Toshihiko; Yoshinaga, Toru; Takigawa, Masahiro.

    1993-08-31

    A gas/liquid separation apparatus is described comprising: first passage means for passing there through a gas carrying a liquid component; swirl generator means, disposed on an upstream side said first passage means, for separating said liquid component from said gas with a swirl flow of said gas, thereby generating a vacuum pressure; first liquid accumulation means, disposed on said first passage means and on a downstream side of said swirl generator means, for trapping and accumulating said separated liquid component, said first liquid accumulation means having an annular groove surrounding said first passage means which traps and accumulates said separated liquid component, such that said liquid component does not pass through said first liquid accumulation means; second liquid accumulation means for drawing in and accumulating said separated liquid component accumulated in said annular groove of said first liquid accumulation means based on a difference in said vacuum pressure between said first liquid accumulation means and said second liquid accumulation means; second passage means, connecting said annular groove to said second liquid accumulation means, for passing there through said accumulated separated liquid component; and third passage means, connecting said second liquid accumulation means to a center portion of said swirl flow for communicating there through said vacuum pressure.

  7. Advances in gas-liquid flows 1990

    SciTech Connect

    Kim, J.M. . Nuclear Reactor Lab.); Rohatgi, U.S. ); Hashemi, A. )

    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.

  8. Simultaneous separation of chlorinated/brominated dioxins, polychlorinated biphenyls, polybrominated diphenyl ethers and their methoxylated derivatives from hydroxylated analogues on molecularly imprinted polymers prior to gas/liquid chromatography and mass spectrometry.

    PubMed

    Roszko, Marek; Szymczyk, Krystyna; Jędrzejczak, Renata

    2015-11-01

    Polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are important contaminants in the environment. In recent years also polybrominated dibenzo-p-dioxins/dibenzofurans (PBDD/Fs) have been reported as emerging environmental stressors. It has been suggested that hydroxylated polybrominated biphenyl ethers (OH-BDEs) are important - may be even the most important - precursors of brominated dioxins/furans. The aim of this study was to develop a robust, time-saving analytical procedure to collectively separate in animal tissues such compounds prior to determination of individual substances with a gas/liquid chromatograph coupled to an ion trap/time-of-flight mass spectrometer (GC/IT-MS or UPLC/TOF-MS). Two OH-CB/BDE separation methods including alkaline extraction and molecularly imprinted polymers (MIP) were compared. Performance of both methods was validated: absolute recovery values were in the 47-90% range depending on the compound, while recovery relative standard deviation was below 20% in most cases. Levels of the studied compounds have been assessed in some real life samples. PMID:26452807

  9. 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)

  10. Gas-liquid and gas-liquid-solid catalysis in a mesh microreactor.

    PubMed

    Abdallah, Radwan; Meille, Valérie; Shaw, John; Wenn, David; de Bellefon, Claude

    2004-02-21

    A microstructured mesh contactor that can offer residence time of more than minutes is used for gas-liquid-solid hydrogenations and gas-liquid asymmetric hydrogenations. Applications for catalyst/chiral inductor screening and for kinetic data acquisition are demonstrated. PMID:14765214

  11. Nonlinear longitudinal oscillations of fuel in rockets feed lines with gas-liquid damper

    NASA Astrophysics Data System (ADS)

    Avramov, K. V.; Filipkovsky, S.; Tonkonogenko, A. M.; Klimenko, D. V.

    2016-03-01

    The mathematical model of the fuel oscillations in the rockets feed lines with gas-liquid dampers is derived. The nonlinear model of the gas-liquid damper is suggested. The vibrations of fuel in the feed lines with the gas-liquid dampers are considered nonlinear. The weighted residual method is applied to obtain the finite degrees of freedom nonlinear model of the fuel oscillations. Shaw-Pierre nonlinear normal modes are applied to analyze free vibrations. The forced oscillations of the fuel at the principle resonances are analyzed. The stability of the forced oscillations is investigated. The results of the forced vibrations analysis are shown on the frequency responses.

  12. Gas-liquid contacting in mixing vessels

    SciTech Connect

    Mann, R.

    1983-01-01

    This report by Dr. R. Mann of UMIST presents a critical survey of literature on the contacting of gases with liquids in stirred vessels. Research undertaken in the last fifteen years in analysed, and promising areas for future research are identified. The report deals with physical contacting, mass transfer between the gas and liquid phases and the utilisation of the stirred vessel as a gas-liquid reactor. Three sections are given on gas-liquid contacting: physical aspects; interphase mass transfer; and chemical reactions. It also discusses recent new approaches and includes a summary of conclusions, nomenclature and references.

  13. Ion Chromatography Analysis of Dibutyl Phosphoric Acid

    SciTech Connect

    Ray, R.J.

    1998-12-04

    Analysis of dibutyl phosphate (DBP), a degradation product of tributyl phosphate (TBP), has long been a problem analysis by Ion Chromatography at the Savannah River Site. Due to the presence of UO{sub 2}{sup +2} and high NO{sub 3}{sup {minus}1} concentrations, inadequate recovery and separation of DBP on the chromatographic column had rendered the analysis undependable and very inconsistent, thus causing high uncertainties in the data. The method presented here by the Savannah River Technology Center (SRTC)/Analytical Development Section (ADS) addresses the sample preparation problems encountered when analyzing for DBP in the presence of uranium and nitrate. The data presented reflects the improvements made to decrease data uncertainty and increase data accuracy and precision.

  14. Chromatography

    MedlinePlus

    Chromatography is a way of separating two or more chemical compounds. Chemical compounds are chemicals that are ... of chemical compound. There are different kinds of chromatography. These include gas, high pressure liquid, or ion ...

  15. 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...

  16. 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

  17. Identification of the botanical origin of commercial pine nuts responsible for dysgeusia by gas-liquid chromatography analysis of Fatty Acid profile.

    PubMed

    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

  18. 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.

  19. Chromatography of amino acids and short peptides. New advances.

    PubMed

    Cserháti, T

    2007-08-01

    The newest results in the application of various chromatographic methods (gas-liquid chromatography, liquid chromatographic techniques, electrically driven systems) for the separation and quantitative determination of amino acids and short peptides in pure state and in complicated matrices are compiled. The results are concisely described and critically evaluated. The future trends of the chromatographic analysis of amino acids and short peptides are briefly discussed. PMID:17549676

  20. 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.

  1. Analysis of cephalosporins by hydrophilic interaction chromatography.

    PubMed

    Liu, Qiaoxia; Xu, Lingyan; Ke, Yanxiong; Jin, Yu; Zhang, Feifang; Liang, Xinmiao

    2011-02-20

    A simple hydrophilic interaction chromatography (HILIC) method was developed to analyze seven cephalosporins. These seven cephalosporins could be separated well on the Click β-CD column and Atlantis HILIC Silica column. The effects of buffer concentration and pH on the retention under HILIC mode were studied. Except cefepime hydrochloride (4), the retention of other six cephalosporins increased with increasing buffer concentration, while decreased with increasing pH. Different separation selectivities could be observed on the Click β-CD column and Atlantis HILIC Silica column, and changing pH also resulted in the changing of separation selectivity. The separations of cephalosporins by HILIC and reversed-phase high performance liquid chromatography (RP-HPLC) were compared, and the two separation modes had good orthogonality. In addition, cefotaxime sodium (1) and its degradation were separated well on the Click β-CD column, which indicated that the Click β-CD column by HILIC can be used for studying the stability of cephalosporins. PMID:21035295

  2. Short-Term Outlook for Hydrocarbon Gas Liquids

    EIA Publications

    2016-01-01

    U.S. liquid fuels production increased from 7.43 million barrels per day (b/d) in 2008 to 13.75 million b/d in 2015. However, the Short-Term Energy Outlook (STEO) expects liquid fuels production to decline to 12.99 million b/d in 2017, mainly as a result of prolonged low oil prices. The liquid fuels production forecast reflects a 1.24 million b/d decline in crude oil production by 2017 that is partially offset by a 450,000 b/d increase in the production of hydrocarbon gas liquids (HGL)—a group of products including ethane, propane, butane (normal and isobutane), natural gasoline, and refinery olefins. This analysis will discuss the outlook for each of these four HGL streams and related infrastructure projects through 2017.

  3. Characterization of Horizontal Gas-Liquid Two-Phase Flow Using Markov Model-Based Complex Network

    NASA Astrophysics Data System (ADS)

    Hu, Li-Dan; Jin, Ning-De; Gao, Zhong-Ke

    2013-05-01

    Horizontal gas-liquid two-phase flow widely exists in many physical systems and chemical engineering processes. Compared with vertical upward gas-liquid two-phase flow, investigations on dynamic behavior underlying horizontal gas-liquid flows are quite limited. Complex network provides a powerful framework for time series analysis of complex dynamical systems. We use a network generation method based on Markov transition probability to infer directed weighted complex networks from signals measured from horizontal gas-liquid two-phase flow experiment and find that the networks corresponding to different flow patterns exhibit different network structure. To investigate the dynamic characteristics of horizontal gas-liquid flows, we construct a number of complex networks under different flow conditions, and explore the network indices for each constructed network. In addition, we investigate the sample entropy of different flow patterns. Our results suggest that the network statistic can well represent the complexity in the transition among different flow patterns and further allows characterizing the interface fluctuation behavior in horizontal gas-liquid two-phase flow.

  4. CHEMICAL ANALYSIS OF WET SCRUBBERS UTILIZING ION CHROMATOGRAPHY

    EPA Science Inventory

    The report describes the key elements required to develop a sampling and analysis program for a wet scrubber using ion chromatography as the main analytical technique. The first part of the report describes a sampling program for two different types of wet scrubbers: the venturi/...

  5. IMPROVED FAST GAS CHROMATOGRAPHY FOR FAME ANALYSIS OF BACTERIA

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Bacteria are frequently identified by fatty acid analysis. We previously reported on methods to speed up sample preparation and gas chromatography, resulting in greatly improved speed and throughput (Buyer, 2002). In this paper we demonstrate that further reductions in chromatographic retention time...

  6. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    ERIC Educational Resources Information Center

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-01-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal

  7. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    ERIC Educational Resources Information Center

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-01-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal…

  8. Gas-liquid separator and method of operation

    DOEpatents

    Soloveichik, Grigorii Lev; Whitt, David Brandon

    2009-07-14

    A system for gas-liquid separation in electrolysis processes is provided. The system includes a first compartment having a liquid carrier including a first gas therein and a second compartment having the liquid carrier including a second gas therein. The system also includes a gas-liquid separator fluidically coupled to the first and second compartments for separating the liquid carrier from the first and second gases.

  9. Separation and IR Analysis of a Mixture of Organic Compounds.

    ERIC Educational Resources Information Center

    Thompson, Evan M.; Almy, John

    1982-01-01

    Presents an experiment which includes fractional distillation with gas-liquid chromatography (GLC) and infrared analysis. Objectives are to introduce students to fractional distillation and analysis of each fraction by GLC, to induce them to decide if each fraction is sufficient for infrared analysis, and to identify unknowns. (Author/JN)

  10. Pharmaceutical analysis using micellar electrokinetic capillary chromatography.

    PubMed

    Swaile, D F; Burton, D E; Balchunas, A T; Sepaniak, M J

    1988-08-01

    The potential utility in pharmaceutical analysis of a capillary electrokinetic separation technique that employs a micellar "pseudo-stationary phase" is discussed and illustrated. Chromatograms of separations of vitamin metabolites and derivatized amino acids are presented to illustrate the high efficiency of the technique and the ability to simultaneously separate the charged and neutral components of pharmaceutical samples. The analytical characteristics of the technique and the importance of optimizing experimental parameters, such as surfactant concentration and capillary column diameter, are discussed and demonstrated with the aid of chromatograms. PMID:3215989

  11. Gas-liquid chromatographic studies of reactions and structural relationships of steroids. V. Concurrent substitution in the pregnane side-chain and position II.

    PubMed

    Vandenheuvel, F A

    1977-03-11

    Qualitative and quantitative effects of classical reactions on steroids observed by gas-liquid chromatography (GLC) under standardized conditions, including the double internal standard technique, are reported. Simple procedures applicable to nanogram amounts of reactants are described. Reactions studied include the conversion of keto groups to hydroxyl groups by NaBH4, and the removal of the pregnane side-chain with NaBiO3. GLC chromatograms readily provide information on effects on functional groups at positions 3, 11, 17, 20, and 21 and the retention times of many steroids unavailable from commercial sources. GLC data analysis provides relationships between steroid structure and retention time from which methods for the computation of retention times and steroid identification are designed. The accuracy of these methods is demonstrated. PMID:838790

  12. /sup 57/Co-soap assay for plasma total non-esterified fatty acids compared with a gas-liquid chromatographic method

    SciTech Connect

    Turnell, D.C.; Price, C.P.; France, M.M.

    1980-12-01

    A relatively rapid radiochemical assay for determining plasma non-esterified fatty acids is described. Results correlated well with those by gas-liquid chromatography. The between-batch CV for 1.12 mmol of non-esterified fatty acids per liter was 7%.

  13. 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

  14. Size-exclusion chromatography system for macromolecular interaction analysis

    DOEpatents

    Stevens, Fred J.

    1988-01-01

    A low pressure, microcomputer controlled system employing high performance liquid chromatography (HPLC) allows for precise analysis of the interaction of two reversibly associating macromolecules such as proteins. Since a macromolecular complex migrates faster than its components during size-exclusion chromatography, the difference between the elution profile of a mixture of two macromolecules and the summation of the elution profiles of the two components provides a quantifiable indication of the degree of molecular interaction. This delta profile is used to qualitatively reveal the presence or absence of significant interaction or to rank the relative degree of interaction in comparing samples and, in combination with a computer simulation, is further used to quantify the magnitude of the interaction in an arrangement wherein a microcomputer is coupled to analytical instrumentation in a novel manner.

  15. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-07-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal for instructional use, especially to illustrate HS analysis or as an alternative to solid-phase microextraction (SPME) to which it is very similar. The basic principles and practice of HS-GC using SDME are described, including a complete review of the literature. Some possible experiments are suggested using water and N -methylpyrrolidone (NMP) as solvents.

  16. Acoustic probe for solid-gas-liquid suspensions. 1998 annual progress report

    SciTech Connect

    Tavlarides, L.L.; Sangani, A.S.; Greenwood, M.S.

    1998-06-01

    'The proposed research will develop an acoustic probe for monitoring particle size and volume fraction in slurries in the absence and presence of gas. The goals are to commission and verify the probe components and system operation, develop theory for the forward and inverse problems for acoustic wave propagation through a three phase medium, and experimentally verify the theoretical analysis. The acoustic probe will permit measurement of solid content in gas-liquid-solid waste slurries in tanks across the DOE complex.'

  17. DEVELOPMENT AND VALIDATION OF A MULTIFIELD MODEL OF CHURN-TURBULENT GAS/LIQUID FLOWS

    SciTech Connect

    Elena A. Tselishcheva; Steven P. Antal; Michael Z. Podowski; Donna Post Guillen

    2009-07-01

    The accuracy of numerical predictions for gas/liquid two-phase flows using Computational Multiphase Fluid Dynamics (CMFD) methods strongly depends on the formulation of models governing the interaction between the continuous liquid field and bubbles of different sizes. The purpose of this paper is to develop, test and validate a multifield model of adiabatic gas/liquid flows at intermediate gas concentrations (e.g., churn-turbulent flow regime), in which multiple-size bubbles are divided into a specified number of groups, each representing a prescribed range of sizes. The proposed modeling concept uses transport equations for the continuous liquid field and for each bubble field. The overall model has been implemented in the NPHASE-CMFD computer code. The results of NPHASE-CMFD simulations have been validated against the experimental data from the TOPFLOW test facility. Also, a parametric analysis on the effect of various modeling assumptions has been performed.

  18. Targeted analysis of glycomics liquid chromatography/mass spectrometry data

    PubMed Central

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

    2012-01-01

    Hydrophilic interaction chromatography (HILIC) liquid chromatography/mass spectrometry (LC/MS) is appropriate for all native and reductively aminated glycan classes. HILIC carries the advantage that retention times (RTs) vary predictably according to oligosaccharide composition. Chromatographic conditions are compatible with sensitive and reproducible glycomics analysis of large numbers of samples. The data are extremely useful for quantitative profiling of glycans expressed in biological tissues. With these analytical developments, the rate limiting factor for widespread use of HILIC LC/MS in glycomics is the analysis of the data. In order to eliminate this problem, a Java-based open source software tool, Manatee, was developed for targeted analysis of HILIC LC/MS glycan data sets. This tool uses user-defined lists of compositions that specify the glycan chemical space in a given biological context. The program accepts high resolution LC/MS data using the public mzXML format and is capable of processing a large data file in a few minutes on a standard desktop computer. The program allows mining of HILIC LC/MS data with an output compatible with multivariate statistical analysis. It is envisaged that the Manatee tool will complement more computationally intensive LC/MS processing tools based on deconvolution and deisotoping of LC/MS data. The capabilities of the tool were demonstrated using a set of HILIC LC/MS data on organ-specific heparan sulfates. PMID:20953780

  19. Group type analysis of asphalt by column liquid chromatography

    SciTech Connect

    Zhang, C.; Yang, J.; Xue, Y.; Li, Y.

    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.

  20. Gas-liquid chromatographic studies of reactions and structural relationships of steroids. IV. Substitution in the pregnane side-chain.

    PubMed

    Vandenheuvel, F A

    1975-12-10

    Qualitative and quantitative effects of classical reactions on steroids observed by gas-liquid chromatography (GLC) under standardized conditions, including the double internal standard technique are reported. Simple procedures applicable to nanogram amounts of reactants are described. Reactions studied include the conversion of keto groups to hydroxyl groups by NaBH4, and to dioxolone derivatives by 1,2-diethanol; 17 alpha-hydroxylation of C20-ketosteroids; the conversion of hydroxyl groups to trimethylsilyl (TMS) ethers by hexamethyldisilazane; the hydrolysis of dioxolone and TMS derivatives by H+. Effects of Wolff-Kishner reagents, and CrO3 were also studied. GLC chromatograms of reaction mixtures of single- and multistep reactions readily provide information on effects on functional groups at positions 3, 17, 20, and 21 in the pregnane series, and the retention times of many steroids unavailable from commercial and other sources. GLC data analysis provides relationships between steroid structure and retention time from which methods for the computation of retention times and for steroid identification are designed. The accuracy of the computation methods is demonstrated. PMID:1202059

  1. 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-ɛ model, RNG k-ɛ model, SST model and k-ω 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.

  2. A Lab Experiment to Introduce Gas/Liquid Solubility

    ERIC Educational Resources Information Center

    Fonsecaa, I. M. A.; Almeida, J. P. B.; Fachada, H. C.

    2008-01-01

    A simplified version of a volumetric apparatus for gas/liquid solubility measurements is proposed. The procedure familiarizes undergraduate students with the experimental study of the solubility of a gas in a liquid and contributes to the understanding of this important phase equilibrium concept. The experimental results report the determination…

  3. A Lab Experiment to Introduce Gas/Liquid Solubility

    ERIC Educational Resources Information Center

    Fonsecaa, I. M. A.; Almeida, J. P. B.; Fachada, H. C.

    2008-01-01

    A simplified version of a volumetric apparatus for gas/liquid solubility measurements is proposed. The procedure familiarizes undergraduate students with the experimental study of the solubility of a gas in a liquid and contributes to the understanding of this important phase equilibrium concept. The experimental results report the determination

  4. Parallel magnetic resonance imaging of gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Mueller, Christoph; Penn, Alexander; Pruessmann, Klaas P.

    2015-03-01

    Gas-liquids flows are commonly encountered in nature and industry. Experimental measurements of gas-liquid flows are challenging since such systems can be visually opaque and highly dynamic. Here we report the implementation of advanced magnetic resonance imaging (MRI) strategies allowing us to probe the dynamics (voidage and velocity measurements) of gas-liquid flows with ultra-fast acquisition speeds. Specifically, parallel MRI which exploits the spatial encoding capabilities of multiple receiver coils was implemented. To this end a tailored, 16 channels MR receive array was constructed and employed in the MR acquisition. A magnetic susceptibility matched gas-liquid system was set-up and used to probe the motion, splitting and coalescence of bubbles. The temporal and spatial resolution of our acquired data was 5 ms and 3.5 mm x 3.5 mm, respectively. The total field of view was 200 mm x 200 mm. We will conclude with an outlook of further possible advances in MRI that have the potential to reduce substantially the acquisition time, providing flexible gains in temporal and spatial resolution.

  5. Supercritical fluid chromatography-mass spectrometry for chemical analysis.

    PubMed

    Li, Fangbiao; Hsieh, Yunsheng

    2008-05-01

    Chromatography with a supercritical fluid as the mobile phase was suggested more than four decades ago (Klesper, E., Corwin, A. H., Turner, D. A., J. Org. Chem. 1962, 27, 700-701). Supercritical fluid chromatography (SFC) is basically a hybrid of GC and LC that eases the resolution of a mixture of compounds not conveniently resolved by either GC or LC. The mobile phases for SFC have low viscosities and high diffusion coefficients compared to those for HPLC and allow for high efficiency separations. SFC uses supercritical fluid as the mobile phase, polar organic solvents as the modifiers in conjunction with acidic/basic compounds as additives to run the chromatographic process like in HPLC. In many applications, SFC-based methods are advantageous over HPLC-based methods as a separation tool in terms of efficiency and economical impact perspectives. Today, the availability of commercial hardware and API interfaces with a mass spectrometer makes SFC even more widely applicable for chemical analysis in many research fields. This review summarizes a variety of novel SFC-MS methods for chemical analysis that have been reported in the peer-reviewed publications. PMID:18366029

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

    DOEpatents

    Davidson, J. Courtney; Balch, Joseph W.

    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.

  7. Prediction of gas-liquid two-phase flow regime in microgravity

    NASA Technical Reports Server (NTRS)

    Lee, Jinho; Platt, Jonathan A.

    1993-01-01

    An attempt is made to predict gas-liquid two-phase flow regime in a pipe in a microgravity environment through scaling analysis based on dominant physical mechanisms. Simple inlet geometry is adopted in the analysis to see the effect of inlet configuration on flow regime transitions. Comparison of the prediction with the existing experimental data shows good agreement, though more work is required to better define some physical parameters. The analysis clarifies much of the physics involved in this problem and can be applied to other configurations.

  8. Protein Mobility Shifts Contribute to Gel Electrophoresis Liquid Chromatography Analysis

    PubMed Central

    Carruthers, Nicholas J.; Parker, Graham C.; Gratsch, Theresa; Caruso, Joseph A.

    2015-01-01

    Profiling of cellular and subcellular proteomes by liquid chromatography with tandem mass spectrometry (MS) after fractionation by SDS-PAGE is referred to as GeLC (gel electrophoresis liquid chromatography)-MS. The GeLC approach decreases complexity within individual MS analyses by size fractionation with SDS-PAGE. SDS-PAGE is considered an excellent fractionation technique for intact proteins because of good resolution for proteins of all sizes, isoelectric points, and hydrophobicities. Additional information derived from the mobility of the intact proteins is available after an SDS-PAGE fractionation, but that information is usually not incorporated into the proteomic analysis. Any chemical or proteolytic modification of a protein that changes the mobility of that protein in the gel can be detected. The ability of SDS-PAGE to resolve proteins with chemical modifications has not been widely utilized within profiling experiments. In this work, we examined the ability of the GeLC-MS approach to help identify proteins that were modified after a small hairpin RNA-dependent knockdown in an experiment using stable isotope labeling by amino acids in cell culture-based quantitation. PMID:26229520

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

    PubMed

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

    2015-04-01

    The analysis of complex mixtures of permanent gases consisting of low molecular weight hydrocarbons, inert gases, and toxic species plays an increasingly important role in today's economy. A new gas chromatography detector based on vacuum ultraviolet (VUV) spectroscopy (GC-VUV), which simultaneously collects full scan (115-240 nm) VUV and UV absorption of eluting analytes, was applied to analyze mixtures of permanent gases. Sample mixtures ranged from off-gassing of decomposing Li-ion and Li-metal batteries to natural gas samples and water samples taken from private wells in close proximity to unconventional natural gas extraction. Gas chromatography separations were performed with a porous layer open tubular column. Components such as C1-C5 linear and branched hydrocarbons, water, oxygen, and nitrogen were separated and detected in natural gas and the headspace of natural gas-contaminated water samples. Of interest for the transport of lithium batteries were the detection of flammable and toxic gases, such as methane, ethylene, chloromethane, dimethyl ether, 1,3-butadiene, CS2, and methylproprionate, among others. Featured is the capability for deconvolution of co-eluting signals from different analytes. PMID:25724098

  10. Gas-liquid chromatographic determination of kepone in field-collected avian tissues and eggs

    USGS Publications Warehouse

    Stafford, C.J.; Reichel, W.L.; Swineford, D.M.; Prouty, R.M.; Gay, M.L.

    1978-01-01

    A procedure is described for determining Kepone (decachlorooctahydro-1,3,4-metheno-2H-cyclobuta [cd] pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2SO4-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography (GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry.

  11. Experimental determination and prediction of the gas-liquid n-hexadecane partition coefficients.

    PubMed

    Mutelet, F; Rogalski, M

    2001-07-20

    Experimental methods based on gas-phase chromatography were tested with a view to determine the gas-liquid n-hexadecane partition coefficients, log L16 of non-volatile compounds at 298.2 K. It was demonstrated that reliable values of log L16 of compounds more volatile than n-docosane can be obtained using either capillary, or packed columns. The main limitation of both methods is the column stability at high temperatures. Here we propose a new method based on the temperature gradient mode, to obtain log L16 of high-boiling compounds. A group contribution model is also presented in view to predicting log L16 values of non-volatile compounds. PMID:11510537

  12. 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.

  13. 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.

  14. Chemical analysis of outgassing contaminants on spacecraft surfaces

    NASA Technical Reports Server (NTRS)

    Mcnutt, R. C.

    1973-01-01

    Methods for analyzing and characterizing outgassing contaminants from such materials as RTV 501 potting compound and S 13 G paint are presented. Fractional distillation of a gross distillate from RTV 501 rubber was carried out and the distilled fractions examined as to their ultraviolet and infrared spectra by gas liquid chromatography. A sensitive technique for structural analysis and molecular identification was found to consist of a gas chromatography-mass spectroscopy system, which was determined to be economically unfeasible at present.

  15. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2002-06-01

    A new project was initiated this quarter to develop gas/liquid membranes for natural gas upgrading. Efforts have concentrated on legal agreements, including alternative field sites. Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project.

  16. 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.

  17. 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...

  18. Microemulsion electrokinetic chromatography for analysis of phthalates in soft drinks.

    PubMed

    Hsieh, Sung-Yu; Wang, Chun-Chi; Wu, Shou-Mei

    2013-12-15

    Microemulsion electrokinetic chromatography (MEEKC) is proposed for analysis of di-n-butyl phthalate (DBP) and di-(2-ethylhexyl) phthalate (DEHP) in soft drinks. However, the instability of microemulsion is a critical issue. In this research, a novel material, Pluronic® F-127, which has the properties of polymer and surfactant, was added for stabilizing the microemulsion in the MEEKC system. Our data demonstrate that the presence of Pluronic® F-127 (0.05-0.30%) also helps enhance resolution of highly hydrophobic compounds, DBP and DEHP. The electrokinetic injection of sodium dodecyl sulphate (SDS) including sample (-10 kV, 20 s) was introduced in this MEEKC system and this yielded about 25-fold sensitivity enhancement compared with hydrodynamic injection (1 psi, 10 s). During method validation, calibration curves were linear (r≥0.99), within a range of 75-500 ng/mL for DBP and 150-1000 ng/mL for DEHP. As the precision and accuracy assays, absolute values of relative standard deviation (RSD) and relative error (RE) in intraday (n=3) and interday (n=5) observations were less than 4.93%. This method was further applied for analyzing six commercial soft drinks and one was found containing 453.67 ng/mL of DEHP. This method is considered feasible for serving as a tool for analysis of highly hydrophobic molecules. PMID:23993511

  19. Analysis of rhubarb anthraquinones and bianthrones by microemulsion electrokinetic chromatography.

    PubMed

    Sun, Shao-Wen; Yeh, Pei-Chen

    2005-01-01

    In this work a method of microemulsion electrokinetic chromatography (MEEKC) has been developed for the analysis of nine anthraquinones and bianthrones in rhubarb. This study employed di-n-butyl tartrate as oil substance to make up the microemulsion. The composition of the microemulsion was 0.5% (w/w) di-n-butyl tartrate, 0.6% (w/w) SDS, 1.2% (w/w) 1-butanol and 97.7% (w/w) 10 mM sodium borate buffer, pH of the buffer being 9.2. Acetonitrile was added to the emulsion to improve the separation. The volume ratio between the emulsion solution and acetonitrile of an optimized separation was 70:30. With the optimized conditions all of the nine analytes were baseline-separated in peaks of good shapes within 20 min. After validation the method was used to analyze the components in a rhubarb sample. A solid-phase extraction procedure was employed. Five anthraquinones and two bianthrones had been detected in the sample and their amounts were determined. The method should be able to be used for the quantitative analysis of the main active components of rhubarb crude drugs. PMID:15620525

  20. The Use of Gas Chromatography for Biogas Analysis

    NASA Astrophysics Data System (ADS)

    Andersen, Amanda; Seeley, John; Aurandt, Jennifer

    2010-04-01

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

  1. Acoustic probe for solid-gas-liquid suspensions. 1997 annual progress report

    SciTech Connect

    Tavlarides, L.L.; Sangani, A.S.

    1997-01-01

    'Acoustic probes have shown promise to be quite effective in determining the solid content in solid-liquid suspensions. However, the presence of small amounts of gas in the waste slurries stored in tanks across the DOE complex prevents straightforward application for characterization of these slurries. The proposed research will develop an acoustic probe for monitoring particle size and volume fraction in slurries in the absence and the presence of gas bubbles. Theoretical Analysis Accomplished: Attenuation of sound waves depends on the size distribution of the solids and the volume fraction of solids. These can in principle be calculated from attenuation measured over a range of frequencies. However, small amounts of bubbles distort the measured attenuation. A typical result from theoretical analysis for the attenuation of solid- gas-liquid systems is given in Figure 1. The total attenuation of a sound wave v(o) equals the sum of contributions by a large number of ''bins'' of particle sizes. This notion yields the following equation for the (hitherto) unknown number density of solid particles as a function of particle radius N(a): j k(o,a)N(a)da = v(o), where the kernel k(o,a) is obtained from analysis. If N(a) is given, the above equation is used to calculate the attenuation v(o). This is referred to as solving the ''forward problem''. Solving for N(a) with v(o) given is the ''inverse problem''. A complication that one faces when trying to solve the inverse problem is that the stated problem is mathematically ill-posed, i.e., small fluctuations in v(o) cause large fluctuations in the result for the number density. Therefore the problem needs to be ''regularized'', i.e., the stated problem needs to be changed slightly such as to make it well-posed. This has been done by others for gas-liquid systems in the past. This approach is currently being applied in the present project to solid-liquid systems. As is shown in Figure 2, it successfully recovers the number density that has been used in the forward problem to generate attenuation data. Having this solution technique giving reliable results for the inverse problems of both gas-liquid and solid-liquid systems, the authors shall apply this method in the near future to solid-gas-liquid systems.'

  2. Use and practice of achiral and chiral supercritical fluid chromatography in pharmaceutical analysis and purification.

    PubMed

    Lemasson, Elise; Bertin, Sophie; West, Caroline

    2016-01-01

    The interest of pharmaceutical companies for complementary high-performance chromatographic tools to assess a product's purity or enhance this purity is on the rise. The high-throughput capability and economic benefits of supercritical fluid chromatography, but also the "green" aspect of CO2 as the principal solvent, render supercritical fluid chromatography very attractive for a wide range of pharmaceutical applications. The recent reintroduction of new robust instruments dedicated to supercritical fluid chromatography and the progress in stationary phase technology have also greatly benefited supercritical fluid chromatography. Additionally, it was shown several times that supercritical fluid chromatography could be orthogonal to reversed-phase high-performance liquid chromatography and could efficiently compete with it. Supercritical fluid chromatography is an adequate tool for small molecules of pharmaceutical interest: synthetic intermediates, active pharmaceutical ingredients, impurities, or degradation products. In this review, we first discuss about general chromatographic conditions for supercritical fluid chromatography analysis to better suit compounds of pharmaceutical interest. We also discuss about the use of achiral and chiral supercritical fluid chromatography for analytical purposes and the recent applications in these areas. The use of preparative supercritical fluid chromatography by pharmaceutical companies is also covered. PMID:26643850

  3. 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.

  4. Analysis of anions in beer using ion chromatography

    PubMed Central

    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

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

    PubMed

    Maksić, Jelena; Jovanović, Marko; Rakić, Tijana; Popović, Igor; Ivanović, Darko; Jančić-Stojanović, 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

  6. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2002-06-30

    Efforts this quarter have concentrated on legal agreements, including alternative field sites. Preliminary design of the bench-scale equipment continues. Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50--70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project.

  7. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2002-10-01

    Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. KPS and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project. Efforts this quarter have concentrated on legal agreements, including alternative field sites. Preliminary design of the bench-scale equipment continues.

  8. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2003-04-01

    Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. KPS and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project. Efforts this quarter have concentrated on field site selection. ChevronTexaco has nominated their Headlee Gas Plant in Odessa, TX for a commercial-scale dehydration test. Potting and module materials testing were initiated. Preliminary design of the bench-scale equipment continues.

  9. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2002-06-01

    Efforts this quarter have concentrated on legal agreements, including alternative field sites. Preliminary design of the bench-scale equipment has been initiated. Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50--70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project.

  10. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2003-01-01

    Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project. Efforts this quarter have concentrated on legal agreements, including alternative field sites. Preliminary design of the bench-scale equipment continues.

  11. Achiral and chiral analysis of camazepam and metabolites by packed-column supercritical fluid chromatography.

    PubMed

    Wang, M Z; Klee, M S; Yang, S K

    1995-03-10

    Supercritical fluid chromatography, using carbon dioxide as the mobile phase and ethanol as a modifier, has been applied to the analysis of products formed in rat liver microsomal metabolism of racemic camazepam, a hypnotic/anxiolytic drug in clinical use. An achiral (amino) column and a chiral (Chiralcel OD-H) column were used. The results suggest that achiral and chiral packed-column supercritical fluid chromatography gives a shorter analysis time and higher selectivity and efficiency than achiral and chiral stationary-phase high-performance liquid chromatography in the analysis of camazepam and its derivatives. PMID:7795784

  12. Two-phase, gas-liquid flows in static mixers

    SciTech Connect

    Shah, N.F.; Kale, D.D. )

    1992-02-01

    This paper reports that static mixers are used for many gas-liquid two-phase operations. some of the typical applications are processing of natural gas to remove hydrogen sulfide or carbon dioxide, waste water treatment, dissolution of gases, hydrogenation, chlorination, and so on. They have experimentally studied the pressure drop for oxygen-water system in a bubble column packed with Sulzer-Koch-type mixing elements. They observed that the ratio of pressure drop through the packed bubble column to that through the unpacked one was slightly greater than one. The suitability of static mixers to mix fluids of very widely different viscosities has been demonstrated. Two-phase operations in polymer industry involve very viscous fluids. Due to the high viscosity of these fluids, the flow will be predominantly in laminar region for both fluids. There are no data on gas-liquid two-phase systems incorporating viscous Newtonian and non-Newtonian fluids where flows are predominantly in laminar region.

  13. Strings of liquid beads for gas-liquid contact operations

    SciTech Connect

    Hattori, Kenji; Ishikawa, Mitsukuni; Mori, Y.H. . Dept. of Mechanical Engineering)

    1994-12-01

    Energy recovery from hot gases exhausted from power plants, garbage incineration facilities, and many industrial processes has been growing due to demands for saving the primary-energy consumption. A novel device for gas-liquid contact operations is proposed to feed a liquid onto wires (or threads) hanging down in a gas stream is proposed. The liquid disintegrates into beads strung on each wire at regular intervals; if the wire is moderately wettable, a thin film forms to sheathe the wire, thereby interconnecting the beads. Since the beads fall down slowly, which possibly renews the film flowing down even more slowly, a sufficient gas-liquid contact time is available even in a contactor with considerably limited height. An approximate calculation method is developed for predicting the variation in the temperature effectiveness for the liquid (the fractional approach of the liquid exit temperature to the gas inlet temperature) with the falling distance, assuming an applicability of strings-of-beads contactors to thermal energy recovery from hot gas streams.

  14. Vibration-Induced Gas-Liquid Interface Breakup

    NASA Astrophysics Data System (ADS)

    O'Hern, Timothy; Torczynski, John; Romero, Ed; Shelden, Bion

    2010-11-01

    Gas-liquid interfaces can be forced to break up when subjected to vibrations within critical ranges of frequency and amplitude. This breakup mechanism was examined experimentally using deep layers of silicone oils over a range of viscosity and sinusoidal, primarily axial vibration conditions that can produce dramatic disturbances at the gas-liquid free surface. Although small-amplitude vibrations produce standing Faraday waves, large-amplitude vibrations produce liquid jets into the gas, droplets pinching off from the jets, gas cavities in the liquid from droplet impact, and bubble transport below the interface. Experiments used several different silicone oils over a range of pressures and vibration conditions. Computational simulations exhibiting similar behavior will be included in the presentation. Applications include liquid fuel rockets, inertial sensing devices, moving vehicles, mixing processes, and acoustic excitation. Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

  15. 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...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  17. Qualitative Analysis of Analgesic Tablets: An Experiment Employing High Pressure Liquid Chromatography.

    ERIC Educational Resources Information Center

    Beaver, Rodney W.; And Others

    1983-01-01

    Describes an experiment on the qualitative analysis of several over-the-counter analgesic tablets. Background information, procedures used (including high pressure liquid chromatography), and typical student results are included. (JN)

  18. APPLICATION OF CAPILLARY SUPERCRITICAL FLUID CHROMATOGRAPHY TO THE ANALYSIS OF A MIDDLE DISTILLATE FUEL

    EPA Science Inventory

    The paper describes the application of capillary supercritical fluid chromatography (SFC) to the analysis of a middle distillate fuel. Small diameter (50 micrometer i.d.) fused silica capillary columns coated with crosslinked 50% phenyl polymethylsiloxane provided high separation...

  19. AN EPA MANUAL FOR ORGANICS ANALYSIS USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    This procedural manual defines the areas of applicability of gas chromatography-mass spectrometry in environmental analysis. The manual includes sample preparation methods specifically adapted to this measurement technique, data processing and interpretation methods, quality cont...

  20. ANALYSIS OF ELECTROLESS NICKEL SOLUTIONS BY ANION CHROMATOGRAPHY

    EPA Science Inventory

    The principal appeal of ion chromatography (IC) as analytical technique lies in the ability to rapidly analyze a mixture of ions of widely varying concentrations and properties in a single elution. It is therefore not surprising that IC has been hampered by the similar ion exchan...

  1. Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

    PubMed

    Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

    2016-02-01

    A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. PMID:26653484

  2. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2003-10-01

    Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project. Efforts this quarter have concentrated on field site selection. ChevronTexaco has nominated their Headlee Gas Plant in Odessa, TX for a commercial-scale dehydration test. Design and cost estimation for this new site are underway. A HazOp review was conducted. Potting and module materials testing continued. Preliminary design of the bench-scale equipment continues. A status meeting was held in Morgantown, WV with the DOE Project Manager.

  3. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2003-07-01

    Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project. Efforts this quarter have concentrated on field site selection. ChevronTexaco has nominated their Headlee Gas Plant in Odessa, TX for a commercial-scale dehydration test. Design and cost estimation for this new site are underway. Potting and module materials testing continued. Preliminary design of the bench-scale equipment continues.

  4. Drag reduction in two-phase gas-liquid flows

    SciTech Connect

    Kale, D.D.

    1987-02-01

    A considerable amount of drag reduction is observed in various flow regimes for two-phase gas-liquid flow of drag reducing fluids. Various attempts have been made to correlate the amount of drag reduction, but comparison with single phase flow of drag reducing fluids has not been done in a satisfactory manner. It is well known that single phase flow of drag reducing fluids exhibits a diameter effect. In order to account for this, a plot of percent drag reduction versus friction velocity, ..mu../sup */, in the absence of a polymer additive gives a simple method of estimating the amount of drag reduction for a given flow rate and pipe diameter. For two-phase flow no such comparison has been made.

  5. Gas-liquid phase separation in charged colloidal systems

    NASA Astrophysics Data System (ADS)

    Reščič, Jurij; Linse, Per

    2001-06-01

    A model system of charged spherical macroions and oppositely charged point counterions with a macroion-charge to counterion-charge ratio Zr=10 was investigated by employing a temperature and density scaling Monte Carlo simulation method. This approach allowed for a determination of the relative free energies among arbitrary number of thermodynamic states over a substantial region of the state space. Here, relative free energies were determined for the macroion volume fraction interval 0.04<φM<0.24 at different values of the electrostatic coupling parameter ΓII≡ZI2LB/RM, where ZI denotes the counterion charge, LB the Bjerrum length, and RM the macroion radius. The binodal curve separating the one-phase system and a gas-liquid two-phase region was determined near the critical point which was determined to φMcr=0.15 and ΓIIcr=2.6.

  6. A Numerical Method for Gas-Liquid Flows

    NASA Astrophysics Data System (ADS)

    Hao, Y.; Prosperetti, A.

    2002-11-01

    The numerical simulation of two-phase flow processes with heat transfer and phase change requires an accurate representation of the flow and temperature fields near gas-liquid (or vapor-liquid) interfaces. This circumstance renders rather problematic the use of several existing methods in which the interface is smeared over a few cells. The present method avoids this shortcoming by maintaining the interface sharp by means of a suitably modified front-tracking approach. In addition, the compressibility of the gas or vapor field can be accounted for, and realistic density ratios can be used. For the time being, the method has been developed and tested for three-dimensional adiabatic calculations. It has been found to perform very well, and its extension to the energy equation is planned for the near future.

  7. Semiphenomenological model for gas-liquid phase transitions

    NASA Astrophysics Data System (ADS)

    Benilov, E. S.; Benilov, M. S.

    2016-03-01

    We examine a rarefied gas with inter-molecular attraction. It is argued that the attraction force amplifies random density fluctuations by pulling molecules from lower-density regions into high-density regions and thus may give rise to an instability. To describe this effect, we use a kinetic equation where the attraction force is taken into account in a way similar to how electromagnetic forces in plasma are treated in the Vlasov model. It is demonstrated that the instability occurs when the temperature T is lower than a certain threshold value Ts depending on the gas density. It is further shown that, even if T is only marginally lower than Ts, the instability generates clusters with density much higher than that of the gas. These results suggest that the instability should be interpreted as a gas-liquid phase transition, with Ts being the temperature of saturated vapor and the high-density clusters representing liquid droplets.

  8. Modeling gas-liquid head performance of electrical submersible pumps

    NASA Astrophysics Data System (ADS)

    Sun, Datong

    The objectives of this study are to develop a simple and accurate theoretical model and to implement the model into a computational tool to predict Electrical Submersible Pumps (ESP) head performance under two-phase flow conditions. A new two-phase model including a set of one-dimensional mass and momentum balance equations was developed. The derived gas-liquid momentum equations along pump channels has improved Sachdeva (1992, 1994)'s model in petroleum industry and generalized Minemura (1998)'s model in nuclear industry. The resulting pressure ODE for frictionless incompressible single-phase flow is consistent with the pump Euler equation. In the two-phase momentum equations, new models for wall frictional losses for each phase, through using gas-liquid stratified assumption and existing correlations for impeller rotating effect, channel curvature effect, and channel cross section effect, have been proposed. New equations for radius of curvature along ESP channels, used in the curvature effect calculation, have been derived. A new shock loss model incorporating rotational speeds has been developed. A new correlation for drag coefficient and interfacial characteristic length effects has been obtained through fitting the model results with experimental data. An algorithm to solve the model equations has been developed and implemented. The model predicts pressure and void fraction distributions along impellers and diffusers and can also be used to predict the pump head performance curve under different fluid properties, pump intake conditions, and rotational speeds. The new two-phase model is validated with air-water experimental data. Results show the model provides a very good prediction for pump head performance under different gas flow rates, liquid flow rates, and different intake pressures. The new model is capable of predicting surging and gas lock conditions.

  9. [Analysis of 5'-deoxyribonucleotides by high-effective liquid chromatography].

    PubMed

    Galkina, O V; Pupkova, V I

    1980-01-01

    The paper describes a method of analyzing 5'-deoxyribonucleotides by high-effective liquid chromatography on the strong-basic anion exchange resin Aminex A-27 in a nongradient phosphate borate buffer with ethanol addition. This method is useful for simultaneous separation of up to 6 UV-absorbing impurities--mononucleotides and nucleosides--with a sensitivity of 0.01 to 0.025 microgram. PMID:7384015

  10. 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.

  11. Gas-liquid chromatographic determination of nifursol in frozen turkey tissues to ten parts per billion.

    PubMed

    Frahm, L J; George, G M; McDonnell, J P

    1975-07-01

    Nifursol (3,5-dinitrosalicylic acid (5-nitrofurfurylidene) hydrazide) is extracted into ethyl acetate from 10 g tissue in the presence of sodium sulfate. Tissue interferences are removed from the tissue extract by washing with petroleum ether after the extract has been transferred into an aqueous solution by evaporation of ethyl acetate. The drug is hydrolyzed under acid conditions to form 5-nitro-2-furaldehyde (5NF). After partition of 5NF from the aqueous phase into benzene the extract is further cleaned up on a Florisil column. The 5NF is eluted from the Florisil column with benzeneethyl acetate. Electron capture gas-liquid chromatography of a 10 mul injection of the concentrated column eluate is the determinative step. Quantitation is accomplished by comparison of the peak height of the sample to the peak height of the standard which is carried through the method simultaneously. Studies of method performance on turkey muscle, liver, kidney, and skin tissues fortified to contain 10 ppb nifursol show a recovery range of 87.4-95.0% and a coefficent of variation range of 5.7-11.2%. PMID:1150608

  12. Gas-liquid chromatographic determination of total cholesterol in multicomponent foods.

    PubMed

    Punwar, J K

    1975-07-01

    A method is described for the determination of total cholesterol in multicomponent foods and also other products such as nonfat dry milk, dried whole egg solids, and certain candy bars. The lipid is extracted from the sample by a mixed solvent and saponified. The unsaponifiable fraction which contains the cholesterol and other sterols is extracted with benzene. An aliquot is evaporated to dryness and the residue is dissolved in dimethylformamide. The sterols are derivatized to form trimethylsilyl (TMS) ethers. The TMS-cholesterol derivative is quantitatively determined by gas-liquid chromatography, using 5alpha-cholestane as an internal standard. Nine laboratories participated in a collaborative study of the determination of total cholesterol in deviled ham sandwich spread, vegetable beef stew, corned beef hash, frozen chicken pot pie, pizza pepperoni, fish sticks, breaded shrimp, chocolate-covered candy bars, dried whole egg solids, and nonfat dry milk and the results are reported here. The coefficient of variation ranged from 5.64 to 23.2%, with an average coefficient of variation of 14.8%. PMID:1173811

  13. Classification of natural resins by liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry using chemometric analysis.

    PubMed

    Rhourrhi-Frih, B; West, C; Pasquier, L; Andr, P; Chaimbault, P; Lafosse, M

    2012-09-21

    Twenty-six resins from six botanical sources belonging to the class Magnoliopsida were compared based on gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry data. The extracts were analysed by GC after silylation and by reversed phase LC combined with atmospheric pressure photoionisation (APPI) mass spectrometry. The chromatograms were re-organized in data matrices, where each sample was represented by a single column comprising 2755 observations (intensity, time, m/z) in GC-MS and 360 observations in LC-MS. A simple comparison of resin fingerprints was attempted by organizing data according to a three dimensional bubble chart (retention time against m/z where each point was a bubble which size represented the ion intensity) where it is possible to easily superimpose the fingerprints. Thus the common and different species can be easily observed enabling to classify the resins. Hierarchical cluster analysis based on characteristics of GC-MS and LC-MS profiles affords a complete description of the classes of the resins and shows that 26 resins are divided into five main clusters Commiphora mukul, Daniella oliveri, Gardenia gummifera, Canarium madagascariensis, Boswellia dalzielii and Boswellia serrata, respectively. In conclusion, the proposed method has been applied to three other resinous samples from the Burseraceae family to evaluate their alteration state. PMID:22885042

  14. A high-power ultrasonic microreactor and its application in gas-liquid mass transfer intensification.

    PubMed

    Dong, Zhengya; Yao, Chaoqun; Zhang, Xiaoli; Xu, Jie; Chen, Guangwen; Zhao, Yuchao; Yuan, Quan

    2015-02-21

    The combination of ultrasound and microreactor is an emerging and promising area, but the report of designing high-power ultrasonic microreactor (USMR) is still limited. This work presents a robust, high-power and highly efficient USMR by directly coupling a microreactor plate with a Langevin-type transducer. The USMR is designed as a longitudinal half wavelength resonator, for which the antinode plane of the highest sound intensity is located at the microreactor. According to one dimension design theory, numerical simulation and impedance analysis, a USMR with a maximum power of 100 W and a resonance frequency of 20 kHz was built. The strong and uniform sound field in the USMR was then applied to intensify gas-liquid mass transfer of slug flow in a microfluidic channel. Non-inertial cavitation with multiple surface wave oscillation was excited on the slug bubbles, enhancing the overall mass transfer coefficient by 3.3-5.7 times. PMID:25537767

  15. 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.

  16. Digitally Enhanced Thin-Layer Chromatography: An Inexpensive, New Technique for Qualitative and Quantitative Analysis

    ERIC Educational Resources Information Center

    Hess, Amber Victoria Irish

    2007-01-01

    A study conducted shows that if digital photography is combined with regular thin-layer chromatography (TLC), it could perform highly improved qualitative analysis as well as make accurate quantitative analysis possible for a much lower cost than commercial equipment. The findings suggest that digitally enhanced TLC (DE-TLC) is low-cost and easy…

  17. Digitally Enhanced Thin-Layer Chromatography: An Inexpensive, New Technique for Qualitative and Quantitative Analysis

    ERIC Educational Resources Information Center

    Hess, Amber Victoria Irish

    2007-01-01

    A study conducted shows that if digital photography is combined with regular thin-layer chromatography (TLC), it could perform highly improved qualitative analysis as well as make accurate quantitative analysis possible for a much lower cost than commercial equipment. The findings suggest that digitally enhanced TLC (DE-TLC) is low-cost and easy

  18. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 1: method of analysis.

    PubMed

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition. PMID:22770383

  19. Structural analysis of amorphous phosphates using high performance liquid chromatography

    SciTech Connect

    Sales, B.C.; Boatner, L.A.; Chakoumakos, B.C.; McCallum, J.C.; Ramey, J.O.; Zuhr, R.A.

    1993-12-31

    Determining the atomic-scale structure of amorphous solids has proven to be a formidable scientific and technological problem for the past 100 years. The technique of high-performance liquid chromatography (HPLC) provides unique detailed information regarding the structure of partially disordered or amorphous phosphate solids. Applications of the experimental technique of HPLC to phosphate solids are reviewed, and examples of the type of information that can be obtained with HPLC are presented. Inorganic phosphates encompass a large class of important materials whose applications include: catalysts, ion-exchange media, solid electrolytes for batteries, linear and nonlinear optical components, chelating agents, synthetic replacements for bone and teeth, phosphors, detergents, and fertilizers. Phosphate ions also represent a unique link between living systems and the inorganic world.

  20. Temporal interfacial instability in vertical gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Schmidt, Patrick; Ó Náraigh, Lennon; Lucquiaud, Mathieu; Valluri, Prashant

    2015-11-01

    We consider onset and dynamics of interfacial instability in gas-liquid flows, using two-dimensional channel flow of a thin falling film sheared by counter-current gas as a model. Our methodology consists of linear stability theory together with DNS of the two-phase flow in the case of nonlinear disturbances. We study the influence of three main flow parameters (density contrast between liquid and gas, film thickness, pressure drop applied to drive the gas stream) on the interfacial dynamics. Energy budget analyses based on Orr-Sommerfeld theory reveal coexisting unstable modes (interfacial, shear, internal) in the case of high density contrast, resulting in mode coalescence and mode competition, but only one dynamically relevant unstable interfacial mode for low density contrast. DNS of this scenario shows that linear theory holds up remarkably well upon the onset of large-amplitude waves as well as the existence of weakly nonlinear waves. In comparison, although linear stability theory successfully determines the most-dominant features in the interfacial wave dynamics at early-to-intermediate times in a high-density-contrast case, short waves selected by linear theory undergo secondary instability and the wave train is no longer regular but rather exhibits chaotic.

  1. Gas-Liquid Supersonic Cleaning and Cleaning Verification Spray System

    NASA Technical Reports Server (NTRS)

    Parrish, Lewis M.

    2009-01-01

    NASA Kennedy Space Center (KSC) recently entered into a nonexclusive license agreement with Applied Cryogenic Solutions (ACS), Inc. (Galveston, TX) to commercialize its Gas-Liquid Supersonic Cleaning and Cleaning Verification Spray System technology. This technology, developed by KSC, is a critical component of processes being developed and commercialized by ACS to replace current mechanical and chemical cleaning and descaling methods used by numerous industries. Pilot trials on heat exchanger tubing components have shown that the ACS technology provides for: Superior cleaning in a much shorter period of time. Lower energy and labor requirements for cleaning and de-scaling uper.ninih. Significant reductions in waste volumes by not using water, acidic or basic solutions, organic solvents, or nonvolatile solid abrasives as components in the cleaning process. Improved energy efficiency in post-cleaning heat exchanger operations. The ACS process consists of a spray head containing supersonic converging/diverging nozzles, a source of liquid gas; a novel, proprietary pumping system that permits pumping liquid nitrogen, liquid air, or supercritical carbon dioxide to pressures in the range of 20,000 to 60,000 psi; and various hoses, fittings, valves, and gauges. The size and number of nozzles can be varied so the system can be built in configurations ranging from small hand-held spray heads to large multinozzle cleaners. The system also can be used to verify if a part has been adequately cleaned.

  2. Resolving gas-liquid interface geometry using light field imaging

    NASA Astrophysics Data System (ADS)

    Jafek, Alexander; Belden, Jesse; Truscott, Tadd

    2014-11-01

    We present a novel approach for reconstructing the geometry of a three-dimensional specular gas-liquid interface from an image captured by a light-field camera. Whereas the scanning of a diffuse surface can be accomplished with a simple projector-camera system, the local reconstruction of a specular surface is non-unique and requires a more constrained sampling method. In our set-up, a known array of laser points is reflected by the unknown specular surface onto the image plane of a light-field camera. For each illuminated pixel, possible surfaces are generated that are defined by a depth location and local surface normal vector. We show that when the aperture is sufficiently small we can find the exact location and orientation of the local surface. Further, we present an algorithm that allows us to reconstruct a reflective surface from images that are taken with wider apertures. The algorithm searches the possible surfaces for points and normal vectors that are most consistent with each other based on input parameters. We present our simulated results with experimental validation.

  3. 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

    ... and Natural Gas Liquids 1 2 MM Table MM-1 to Subpart MM of Part 98 Protection of Environment... Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric tons/bbl... Natural Gas Liquids Aviation Gasoline 0.1120 85.00 0.3490 Special Naphthas 0.1222 84.76 0.3798...

  4. Gas liquid chromatography for detection of bacteriuria: examination for volatile acidic and neutral compounds.

    PubMed Central

    Barrett, E; Lynam, G; Trustey, S

    1978-01-01

    Direct injection of clinically infected urines on porous-polymer columns was investigated to determine which microbial metabolites were consistently detectable, and whether their presence could be used as a reliable index of infection. Chromosorb 101 was found to be the most suitable porous polymer for the detection of microbial metabolites; greater sensitivity of detection was achieved by partial purification of the urine before injection. Acetic acid was the only compound found consistently and it enabled 10(6) microorganisms per ml to be detected in urine. However, as urinary tract infection is diagnosed by the presence of 10(5) organisms or more per ml, our method is insufficiently sensitive for the detection of bacteriuria. Escherichia coli, Enterobacter cloacae, Klebsiella spp, Proteus spp, Stapyhlococcus albus, and Streptocococcus faecalis were detectable by our method but Pseudomonas aeruginosa and Candida albicans were not. PMID:711917

  5. Gas-Liquid flow characterization in bubble columns with various gas-liquid using electrical resistance tomography

    NASA Astrophysics Data System (ADS)

    Jin, Haibo; Yuhuan, Han; Suohe, Yang

    2009-02-01

    Electrical resistance tomography (ERT) is an advanced and new detecting technique that can measure and monitor the parameters of two-phase flow on line, such as gas-liquid bubble column. It is fit for the industrial process where the conductible medium serves as the disperse phase to present the key bubble flow characteristics in multi-phase medium. Radial variation of the gas holdup and mean holdups are investigated in a 0.160 m i. d. bubble column using ERT with two axial locations (Plane 1 and Plane 2). In all the experiments, air was used as the gas phase, tap water as liquid phase, and a series of experiments were done by adding KCl, ethanol, oil sodium, and glycerol to change liquid conductivity, liquid surface tension and viscosity. The superficial gas velocity was varied from 0.02 to 0.2 m/s. The effect of conductivity, surface tension, viscosity on the mean holdups and radial gas holdup distribution is discussed. The results showed that the gas holdup decrease with the increase of surface tension and increase with the increase of viscosity. Meanwhile, the settings of initial liquid conductivity slightly influence the gas holdup values, and the experimental data increases with the increase of the initial setting values in the same conditions.

  6. Acoustic Probe for Solid-Gas-Liquid Suspension

    SciTech Connect

    Tavlarides, L.L.; Sangani, Ashok

    2003-09-14

    The primary objective of the research project during the first funding period was to develop an acoustic probe to measure volume percent solids in solid-liquid slurries in the presence of small amounts of gas bubbles. This problem was addressed because of the great need for a non-invasive, accurate and reliable method for solids monitoring in liquid slurries in the presence of radiolytically generated gases throughout the DOE complex. These measurements are necessary during mobilization of salts and sediments in tanks, transport of these slurries in transfer lines to processing facilities across a site, and, in some instances, during high level waste processing. Although acoustic probes have been commonly used for monitoring flows in single-phase fluids (McLeod, 1967), their application to monitor two-phase mixtures has not yet fully realized its potential. A number of investigators in recent years have therefore been involved in developing probes for measuring the volume fractions in liquid solid suspensions (Atkinson and Kytomaa, 1993; Greenwood et al., 1993; Martin et al., 1995) and in liquid-liquid suspensions (Bonnet and Tavlarides, 1987; Tavlarides and Bonnet, 1988, Yi and Tavlarides, 1990; Tsouris and Tavlarides, 1993, Tsouris et al., 1995). In particular, Atkinson and Kytomaa (1993) showed that the acoustic technique can be used to determine both the velocity and the volume fraction of solids while Martin et al. (1995) and Spelt et al. (1999) showed that the acoustic probe can also be used to obtain information on the size distribution of the particles. In a recent testing of in-line slurry monitors with radioactive slurries suspended with Pulsair Mixers (Hylton & Bayne, 1999), an acoustic probe did not compare well with other instruments most probably due to presence of entrained gases and improper acoustic frequency range of interrogation. The work of the investigators cited has established the potential of the acoustic probe for characterizing/monitoring two-phase flows in relatively ideal, well-characterized suspensions. Two major factors which we judge has prevented its wide-spread use in the processing industry, particularly for dilute suspensions, is careful selection of the frequency range for interrogation and quantification and removal of the noise introduced by bubbles from the acoustic signal obtained from the suspension. Our research during the first funding period to develop an acoustic probe for solid-gas liquid suspensions has resulted in a theory, supported by our experiments, to describe small amplitude dilute suspensions (Norato, 1999, Spelt et al., 1999, Spelt et al., 2001). The theory agrees well with experimental data of sound attenuation up to 45 {approx}01% suspensions of 0.11 and 77 micron radius polystyrene particles in water and 0.4 to 40 vol %, suspensions of 32 micron soda-lime glass particles in water. Also, analyses of our attenuation experiments for solid-gas liquid experiments suggest the theory can be applied to correct for signal interference due to the presence of bubbles over a selected frequency range to permit determination of the solid-liquid volume fraction. Further, we show experimentally that a reliable linear dependency of weight percent solids with attenuation is obtained for low weight fractions at high frequencies of interrogation where bubble interference is minimal. There was a collaborative effort during the first funding period with the Pacific Northwest National Laboratories in that Dr. Margaret Greenwood was a co-investigator on the project. Dr. Greenwood provided a high level of experimental knowledge and techniques on ultrasound propagation, measurement and data processing. During the second funding period the slurry test loop at Oak Ridge National Laboratories under the direction of Mr. Tom Hylton will be employed to demonstrate the measurement capabilities of the prototype acoustic monitor.

  7. 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.

  8. Comparison of microemulsion electrokinetic chromatography with high-performance liquid chromatography for fingerprint analysis of resina draconis.

    PubMed

    Cao, Yuhua; Gong, Wenjun; Li, Nan; Yin, Changna; Wang, Yun

    2008-11-01

    Microemulsion electrokinetic chromatography (MEEKC) has been developed for fingerprint analysis of resina draconis, a substitute for sanguis draconis in the Chinese market. The microemulsion as the running buffer was made up of 3.3% (w/v) sodium dodecyl sulfate (SDS), 6.6% (w/v) n-butanol, 0.8% (w/v) n-octane, and 10 mmol/L sodium tetraborate buffer (pH 9.2), which was also used as the solvent for ultrasonic extraction of both water- and fat-soluble compounds in the traditional Chinese medicine samples. Four batches of resina draconis obtained from different pharmaceutical factories located in different geographic regions were used to establish the electrophoretic fingerprint. MEEKC was performed using a Beckman PACE/MDQ system equipped with a diode-array detector and with monitoring at 280 nm. The fingerprint of resina draconis comprised 27 common peaks within 100 min. The relative standard deviations of the relative migration time of these common peaks were less than 2.1%. Through repetitive injection of the sample solution six times in 24 h, all relative standard deviations of the migration time and peak area of loureirin A and loureirin B were less than 2.5 and 3.8%, which demonstrated that the method had good stability and reproducibility. The relative peak areas of these common peaks in the electropherograms of four batches of resina draconis were processed with two mathematical methods, the correlation coefficient and the interangle cosine, to valuate the similarity. The values of the similarity degree of all samples were more than 0.91, which showed resina draconis samples from different origins were consistent. On the other hand, high-performance liquid chromatography (HPLC) coupled with photodiode-array detection was also applied to establish the fingerprint of resina draconis. The samples were separated with a LiChrospher C(18) column using acetonitrile (solvent A) and water containing 0.1% H(3)PO(4) (solvent B) as the mobile phase in linear gradient elution mode at a flow rate of 0.6 mL/min and detection was at 280 nm. There were only 20 common peaks in the HPLC fingerprint, and the values of the similarity degree of all samples were also more than 0.91. Though the similarity results of fingerprint analysis seemed to be the same, MEEKC resulted in more common peaks and higher separation efficiency for a variety of polarities of the components than HPLC. So, MEEKC was more suitable for development of the fingerprint of resina draconis. PMID:18758761

  9. 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...

  10. 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...

  11. 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.

  12. High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

    ERIC Educational Resources Information Center

    Haddad, Paul; And Others

    1983-01-01

    Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

  13. ANALYSIS OF CHLORINATED HERBICIDES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    A method that uses high performance liquid chromatography/mass spectrometry (HPLC/MS) for the analysis of chlorinated phenoxyacid herbicides is described. uring method development different techniques were used to increase both the sensitivity and the specificity of thermospray H...

  14. 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...

  15. Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

    EPA Science Inventory

    Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

  16. Short-Term Energy Outlook Model Documentation: Hydrocarbon Gas Liquids Supply and Demand

    EIA Publications

    2015-01-01

    The hydrocarbon gas liquids (ethane, propane, butanes, and natural gasoline) module of the Short-Term Energy Outlook (STEO) model is designed to provide forecasts of U.S. production, consumption, refinery inputs, net imports, and inventories.

  17. Strong Cation Exchange Chromatography in Analysis of Posttranslational Modifications: Innovations and Perspectives

    PubMed Central

    Edelmann, Mariola J.

    2011-01-01

    Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide. PMID:22174558

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

    NASA Technical Reports Server (NTRS)

    Bytella, Joseph

    1991-01-01

    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.

  19. High resolution gas chromatography analysis of rice bran oil

    NASA Astrophysics Data System (ADS)

    Yu, Fengxiang; Lin, Qinlu; Chen, Xu; Wei, Xiaojun

    To assess the nutritional value and safety quality of rice bran oil (RBO) ,fatty acids of RBO from 15 species rice come from Hunan Province were analyzed by high resolution gas chromatography (HRGC). Crude RBOs were extracted by hexane 3-times using a solvent-to-rice bran ratio of 3:1 (w/w) at 40°C and composition of RBOs was analyzed by HRGC. The result showed that main fatty acids of 15 kinds of RBO include myristic acid (C14:0), palmitic acid (C16:0), palmitoleic acid (C16:1), stearic acid (C18:0), oleic acid (C18:1), linoleic acid (C18:2), linolenic acid (C18:3), arachidic acid (C20:0), arachidonic acid (C20:1). It is strange that arachidonic acid (C20:1) is not listed in Chinese standard of RBO (GB11192-2003), and it exists in our samples of RBO. The average value of linolenic acid in RBOs is 1.6304% (range from 1.2425% to 2.131%), and it showed higher level comparing with Chinese standard that linolenic acid is less than 1.0%. The average value of USFA and SFA are 76.81% (range 75.96% to 82.06% ) and 20.15% (range 13.72% to 23.06%) respectively, and USFA content is close to olive oil (83.75%), peanut oil (81.75%) and soybean oil (85.86%). USFA in Jingyou 13 RBO is the highest content. The ratio of USFA to SFA content is 4:1 (range from 3.32 to 5.98:1). The ratio of SFA: MUFA: PUFA of 15 RBOs is 1: 2.2: 1.8, and ω6/ω3 ratio is 21.69 (range from16.54 to 27.28) and it is close to the 26:1 which is reported to be helpful to increase SOD activity. The oleic acid /linoleic acid ratio of 15 RBOs is 1.23:1 (rang from 1.04:1 to 1.42:1). Our data analyzed composition of RBOs from 15 species rice of China and will provide new evidence to revise RBO standard. It also helps us to assess nutritional value of RBOs and identify different RBOs from various species rice and places of origin.

  20. 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

  1. Recent Advance in Liquid Chromatography/Mass Spectrometry Techniques for Environmental Analysis in Japan

    PubMed Central

    Suzuki, Shigeru

    2014-01-01

    The techniques and measurement methods developed in the Environmental Survey and Monitoring of Chemicals by Japan’s Ministry of the Environment, as well as a large amount of knowledge archived in the survey, have led to the advancement of environmental analysis. Recently, technologies such as non-target liquid chromatography/high resolution mass spectrometry and liquid chromatography with micro bore column have further developed the field. Here, the general strategy of a method developed for the liquid chromatography/mass spectrometry (LC/MS) analysis of environmental chemicals with a brief description is presented. Also, a non-target analysis for the identification of environmental pollutants using a provisional fragment database and “MsMsFilter,” an elemental composition elucidation tool, is presented. This analytical method is shown to be highly effective in the identification of a model chemical, the pesticide Bendiocarb. Our improved micro-liquid chromatography injection system showed substantially enhanced sensitivity to perfluoroalkyl substances, with peak areas 32–71 times larger than those observed in conventional LC/MS. PMID:26819891

  2. [Quantitative analysis of five antiviral drugs by hydrophilic interaction liquid chromatography-charged aerosol detection].

    PubMed

    Long, Zhen; Jin, Yan; Liu, Xiaoda; Guo, Zhimou; Shen, Aijin; Hu, Xingjuan; Wu, Ningpeng

    2015-09-01

    Antiviral drugs are widely used for human and animals. However, the analysis of the mixture of antiviral drugs is a challenge for high performance liquid chromatography, since some of the antiviral drugs have weak UV absorbance and poor retention in reversed phase liq- uid chromatography. A method of hydrophilic interaction liquid chromatography-charged aerosol detection (HILIC-CAD) was optimized for the qualitative and quantitative analysis of five antiviral drugs. In this study, Click TE-Cys was used as the stationary phase and CAD was used as the detector. Various chromatographic conditions including the kind of detector, chromatographic mode, column and mobile phase composition were investigated. Compared to UV-Vis, more antiviral drugs could be detected by CAD, since it is a universal detector. HILIC mode is an alternative to reversed phase liquid chromatography mode. HILIC provides higher sensitivity and unique selectivity to target compounds. After the optimized parameters were obtained, the developed method was used for the quantitative analysis of the five antiviral drugs. As a result, the current method has good repeatability, a wide linear range (0.07-2.28 mg/mL) and good sensitivity (LOQ ? 0.04 mg/mL). The RSDs of intra-day and inter-day peak areas were less than 3. 06% and 5. 38% respectively. The above results demonstrated that the current method is sensitive, robust and effective for the separation and determination of these five antiviral drugs. PMID:26753280

  3. Analysis of anions in geological brines using ion chromatography

    SciTech Connect

    Merrill, R.M.

    1985-03-01

    Ion chromatographic procedures for the determination of the anions bromide, sulfate, nitrite, nitrate, phosphate, and iodide in brine samples have been developed and are described. The techniques have been applied to the analysis of natural brines, and geologic evaporites. Sample matrices varied over a range from 15,000 mg/L to 200,000 mg/L total halogens, nearly all of which is chloride. The analyzed anion concentrations ranged from less than 5 mg/L in the cases of nitrite, nitrate, and phosphate, to 20,000 mg/L in the case of sulfate. A technique for suppressing chloride and sulfate ions to facilitate the analysis of lower concentration anions is presented. Analysis times are typically less than 20 minutes for each procedure and the ion chromatographic results compare well with those obtained using more time consuming classical chemical analyses. 10 references, 14 figures.

  4. Analysis of chromatography by means of transfer functions

    SciTech Connect

    Kamiyanagi, K.; Furusaki, S.

    1985-04-01

    The transfer-function method of Ostergaard and Michelson is extended to obtain the gel-chromatographic parameters, namely, the intraparticle diffusion coefficient, the distribution coefficient, and the longitudinal diffusivity. The accuracy is comparable with that of the method of moments. Impulse-response curves calculated from these parameters by Fourier analysis agree closely with experimental data.

  5. INTERLABORATORY COMPARISON OF THERMOSPRAY AND PARTICLE BEAM LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY INTERFACES: EVALUATION OF A CHLORINATED PHENOXY ACID HERBICIDE LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY ANALYSIS METHOD

    EPA Science Inventory

    Seven laboratories participated in an interlaboratory evaluation of a liquid chromatography/mass spectrometry (LC/MS) method for the analysis of 10 chlorinated phenoxy acid herbicides. The focus of this evaluation was to test the intercomparability of LC/MS data obtained from two...

  6. Counter-current chromatography for high throughput analysis of natural products.

    PubMed

    Wu, Shihua; Liang, Junling

    2010-12-01

    Counter-current chromatography (CCC) is a unique support-free liquid-liquid partition chromatography winning wide applications in the separation of various components from natural or synthetic mixtures. It has been one of the prime methods for isolating compounds from Traditional Chinese Medicines (TCM) and other comprehensive natural products. Although early CCC models produced a long-standing false image that CCC is a time-consuming technique, rapid and high-performance CCC devices and methods for high-throughput analysis of natural mixtures have been advanced. For instances, multi-channel CCC, dual CCC, elution-extrusion CCC, and solvent simplification protocols can provide high-throughput CCC analysis and produce high purity of compounds or large natural product libraries for drug discovery. This review summarizes the recent advancements of CCC in the high-throughput analysis of natural product with an emphasis on the developments of instruments and methods. PMID:20883188

  7. [Thin-layer chromatography analysis of methamphetamine in urine samples].

    PubMed

    Klimes, J; Pilarov, P

    1996-11-01

    The paper investigated the chromatographic conditions for TLC analysis of metamphetamine on silica gel and the lipophilic stationary phase RP V 18 in order to qualitatively analyze the drug in urine samples. Attention was also paid to chemical detection. Five detection reagents were tested, out of which Fast Black K salt, yielding orange-red spots with a detection limit of 1 microgram, proved to be the best. In the analysis of metamphetamine in the samples of model urine, the best results were achieved on Kieselgel. Using the developing system ethyl acetate-ethanol-concentrated solution of ammonia (36:2:2), a complete separation of the metamphetamine spot from the spots of ballast from the biological matrix was achieved. PMID:8998609

  8. Features for non-targeted cross-sample analysis with comprehensive two-dimensional chromatography.

    PubMed

    Reichenbach, Stephen E; Tian, Xue; Cordero, Chiara; Tao, Qingping

    2012-02-24

    This review surveys different approaches for generating features from comprehensive two-dimensional chromatography for non-targeted cross-sample analysis. The goal of non-targeted cross-sample analysis is to discover relevant chemical characteristics (such as compositional similarities or differences) from multiple samples. In non-targeted analysis, the relevant characteristics are unknown, so individual features for all chemical constituents should be analyzed, not just those for targeted or selected analytes. Cross-sample analysis requires matching the corresponding features that characterize each constituent across multiple samples so that relevant characteristics or patterns can be recognized. Non-targeted, cross-sample analysis requires generating and matching all features across all samples. Applications of non-targeted cross-sample analysis include sample classification, chemical fingerprinting, monitoring, sample clustering, and chemical marker discovery. Comprehensive two-dimensional chromatography is a powerful technology for separating complex samples and so is well suited for non-targeted cross-sample analysis. However, two-dimensional chromatographic data is typically large and complex, so the computational tasks of extracting and matching features for pattern recognition are challenging. This review examines five general approaches that researchers have applied to these difficult problems: visual image comparisons, datapoint feature analysis, peak feature analysis, region feature analysis, and peak-region feature analysis. PMID:21855071

  9. Characterizing the correlations between local phase fractions of gas-liquid two-phase flow with wire-mesh sensor.

    PubMed

    Tan, C; Liu, W L; Dong, F

    2016-06-28

    Understanding of flow patterns and their transitions is significant to uncover the flow mechanics of two-phase flow. The local phase distribution and its fluctuations contain rich information regarding the flow structures. A wire-mesh sensor (WMS) was used to study the local phase fluctuations of horizontal gas-liquid two-phase flow, which was verified through comparing the reconstructed three-dimensional flow structure with photographs taken during the experiments. Each crossing point of the WMS is treated as a node, so the measurement on each node is the phase fraction in this local area. An undirected and unweighted flow pattern network was established based on connections that are formed by cross-correlating the time series of each node under different flow patterns. The structure of the flow pattern network reveals the relationship of the phase fluctuations at each node during flow pattern transition, which is then quantified by introducing the topological index of the complex network. The proposed analysis method using the WMS not only provides three-dimensional visualizations of the gas-liquid two-phase flow, but is also a thorough analysis for the structure of flow patterns and the characteristics of flow pattern transition.This article is part of the themed issue 'Supersensing through industrial process tomography'. PMID:27185959

  10. Venus lower atmospheric composition - Analysis by gas chromatography

    NASA Technical Reports Server (NTRS)

    Oyama, V. I.; Carle, G. C.; Woeller, F.; Pollack, J. B.

    1979-01-01

    The first gas chromatographic analysis of the lower atmosphere of Venus is reported. Three atmospheric samples were analyzed. The third of these samples showed carbon dioxide (96.4 percent), molecular nitrogen (3.41 percent), water vapor (0.135 percent), molecular oxygen (69.3 ppm), argon (18.6 ppm), neon (4.31 ppm), and sulfur dioxide (186 ppm). The amounts of water vapor and sulfur dioxide detected are roughly compatible with the requirements of greenhouse models of the high surface temperature of Venus. The large positive gradient of sulfur dioxide, molecular oxygen, and water vapor from the cloud tops to their bottoms, as implied by Earth-based observations and these results, gives added support for the presence of major quantities of aqueous sulfuric acid in the clouds. A comparison of the inventory of inert gases found in the atmospheres of Venus, Earth, and Mars suggests that these components are due to outgassing from the planetary interiors.

  11. [Chromatography analysis of tobacco smoke condensate in biology tissue].

    PubMed

    Zurabashvili, D Z; Chanturia, I R; Kapanadze, L R

    2010-01-01

    Specialized analytical instrumentation for detailed analysis of nicotine, benz(alpha)pyrene, pyridine and benzene in tooth enamel and pulp of inveterate tobacco smokers is created. A Waters PPY-24 liquid chromatograph is equipped with Model M660 solvent programmer and a Model U6K sample injector is used. A Model 440 dual-wavelength detector is used to obtain absorbance ratios on dual-pen recorder. Our data show that concentration of tobacco smoke components in tooth cavity of inveterate tobacco smokers is different. The chisel tooth pulp contained considerably more nicotine and pyridine as compared with molars. The level of benzene does not change analyzed structures. The assumption of linearity between calculation of predicted retention times and concentration has been shown to be valid up to about 8,0% for all studied compounds. PMID:20157203

  12. Thin layer chromatography coupled with electrospray ionization mass spectrometry for direct analysis of raw samples.

    PubMed

    Hu, Bin; Xin, Gui-zhong; So, Pui-Kin; Yao, Zhong-Ping

    2015-10-01

    Conventional mass spectrometric analysis of raw samples commonly requires sample pretreatment and chromatographic separation using high performance liquid chromatography or gas chromatography, which could be time-consuming and laborious. In this study, thin layer chromatography (TLC) coupled with electrospray ionization mass spectrometry (ESI-MS) was developed for direct analysis of raw samples. The sorbent material of the TLC plate was found to be able to retain the interfering compounds and allow interested analytes to be extracted, ionized and detected by ESI-MS with much reduced matrix interference. Our results showed that this method could be effectively applied in direct analysis of samples containing common interfering compounds, e.g., salts and detergents, and rapid detection and quantitation of target analytes in raw samples. Offline and online separation and detection of different components in mixture samples, e.g., plant extracts, using TLC-ESI-MS were also demonstrated. Overall, this study revealed that TLC-ESI-MS could be a simple, rapid and efficient method for analysis of raw samples. PMID:26362806

  13. [Recent advances in analysis of petroleum geological samples by comprehensive two-dimensional gas chromatography].

    PubMed

    Gao, Xuanbo; Chang, Zhenyang; Dai, Wei; Tong, Ting; Zhang, Wanfeng; He, Sheng; Zhu, Shukui

    2014-10-01

    Abundant geochemical information can be acquired by analyzing the chemical compositions of petroleum geological samples. The information obtained from the analysis provides scientifical evidences for petroleum exploration. However, these samples are complicated and can be easily influenced by physical (e. g. evaporation, emulsification, natural dispersion, dissolution and sorption), chemical (photodegradation) and biological (mainly microbial degradation) weathering processes. Therefore, it is very difficult to analyze the petroleum geological samples and they cannot be effectively separated by traditional gas chromatography/mass spectrometry. A newly developed separation technique, comprehensive two-dimensional gas chromatography (GC x GC), has unique advantages in complex sample analysis, and recently it has been applied to petroleum geological samples. This article mainly reviews the research progres- ses in the last five years, the main problems and the future research about GC x GC applied in the area of petroleum geology. PMID:25739266

  14. Chromatography and its hyphenation to mass spectrometry for extracellular vesicle analysis.

    PubMed

    Pocsfalvi, Gabriella; Stanly, Christopher; Fiume, Immacolata; Vékey, Károly

    2016-03-25

    Extracellular vesicles (EVs), such as exosomes, microvesicles and apoptotic bodies are released by cells, both under physiological and pathological conditions. EVs can participate in a novel type of intercellular communication and deliver cargo of nucleic acids, proteins and lipids near or to distant host cells. EV research is proceeding at a fast pace; now they start to appear as promising therapeutic targets, diagnostic tools and drug delivery systems. Isolation and analysis of EVs are prerequisites for understanding their biological roles and for their clinical exploitation. In this process chromatography and mass spectrometry (MS)-based strategies are rapidly gaining importance; and are reviewed in the present communication. Isolation and purification of EVs is mostly performed by ultracentrifugation at present. Chromatography-based strategies are gaining ground, among which affinity and size exclusion chromatography (SEC) are particularly strong contenders. Their major advantages are the relative simplicity, robustness and throughput. Affinity chromatography has the added advantage of separating EV subtypes based on molecular recognition of EV surface motifs. SEC has the advantage that isolated EVs may retain their biological activity. EVs are typically isolated in small amounts, therefore high sensitivity is required for their analysis. Study of the molecular content of EVs (all compounds beside nucleic acids) is predominantly based on liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis. The chromatographic separation is mostly performed by reverse phase, nanoscale, ultra high performance LC technique. The MS analysis relying typically on nano-electrospray ionization MS/MS provides high sensitivity, selectivity and resolution, so that thousand(s) of proteins can be detected/identified/quantified in a EV sample. Beside protein identification, quantitation and characterization of protein post-translational modifications (PTMs), like glycosylation and phosphorylation are becoming feasible and increasingly important. Along with conventional LC-MS/MS, other chromatographic approaches hyphenated to MS are gaining importance for EV characterization. Hydrophilic interaction LC is used to characterize PTMs; LC-inductively coupled plasma/MS to identify metal containing molecules; while gas chromatography-MS to analyze some lipids and metabolites. PMID:26830636

  15. Pesticide analysis in rose wines by micellar electrokinetic chromatography.

    PubMed

    Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Angel

    2007-12-01

    In this work, the determination of 11 pesticides (pirimicarb, metalaxyl, pyrimethanil, procymidone, nuarimol, azoxystrobin, tebufenozide, fenarimol, benalaxyl, penconazole, and tetradifon) in rose wines by micellar EKC (MEKC) using reversed electrode polarity stacking mode (REPSM) as online preconcentration strategy is described. The MEKC buffer consisted of 100 mM sodium tetraborate and 30 mM SDS at pH 8.5 with 6% v/v 1-propanol. A solid-phase microextraction (SPME) procedure using PDMS/divinylbenzene (PDMS/DVB) fibers was applied to extract the selected pesticides from the rose wine samples. The comparison between the calibration curves obtained from hydroalcoholic solutions (12% v/v ethanol) and from rose wines (matrix matched calibration) showed the existence of a strong matrix effect. Furthermore, a comparison with calibration curves obtained with white wine samples also showed significant differences for most of the analyzed pesticides. As a result, a matrix matched calibration was developed. Quantitative extraction from spiked wine samples was carried out in triplicate at two levels of concentration (range 0.18-6.00 mg/L). LODs between 0.040 and 0.929 mg/L were achieved, which are below the maximum residue limits (MRLs) established for wine grapes (except for pirimicarb) by the EU and Spain legislation as well as by the Codex Alimentarius. The established method - which is solvent free, cost effective, and fast - was also applied to the analysis of several homemade rose wine samples and a commercial one. Two of the selected pesticides were found in some of the analyzed samples. PMID:18027361

  16. The analysis of clingfilms by infrared spectroscopy and thermal desorption capillary gas chromatography.

    PubMed

    Gilburt, J; Ingram, J M; Scott, M P; Underhill, M

    1991-01-01

    An automated thermal desorption gas chromatography technique has been adapted to analyse traces of volatile compounds in proprietary food-wrapping films. Fourteen brands of polyvinylchloride film, seven brands of polyethylene film and one polyvinylidene chloride film were discriminated. Prior infrared analysis was used to identify the polymer type. The chromatograms showed minor changes in volatiles along the length of a roll of film and major changes in films exposed to daylight or in contact with cannabis resin. PMID:1744625

  17. 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

  18. Acetic acid improves the sensitivity of theophylline analysis by gas chromatography-mass spectrometry.

    PubMed

    Saka, Kanju; Uemura, Koichi; Shintani-Ishida, Kaori; Yoshida, Ken-Ichi

    2007-02-01

    In the analysis of theophylline by gas chromatography-mass spectrometry (GC-MS), we found that the addition of acetic acid to the solvent (ethyl acetate) decreased the adsorption of theophylline to the glass wool packed into the inlet liner. The addition of acetic acid to ethyl acetate improved the sensitivity for theophylline (optimum concentration of 3%). This simple and sensitive method without derivatization can be applied to the quantification of theophylline in serum samples in clinical and toxicological practice. PMID:17011247

  19. Novel detection schemes and automated image analysis algorithms for planar chromatography and gel electrophoresis

    SciTech Connect

    Koutney, L.B.

    1992-09-09

    After a discussion of charge coupled devices and personal computer capabilities, examples of their applications involving novel analytical techniques are presented: laser-based indirect fluorometric detection in thin-layer chromatography; on-line detection of DNA and proteins in gel electrophoresis by uv absorption; automated image analysis for distortion compensation in sequencing gel electrophoresis; and expert systems for data acquisition to achieve constant signal-to-noise, with application to DNA sequencing slab gels.

  20. Gas/liquid flow measurement using coriolis-based flow meters

    SciTech Connect

    Liu, K.T.; Nguyen, T.V.

    1991-07-09

    This patent describes a method of determining total mass flow rate and phase distribution of individual components in a flowing gas/liquid stream. It comprises flowing at least a first gas/liquid stream through a Coriolis-based flow meter, the first gas/liquid stream having a first known total mass flow rate and component phase distribution; obtaining a first apparent total mass flow rate output and a first apparent density output from the Coriolis- based mass flow meter; correlating the first known total mass flow rate and phase distribution with the first apparent mass flow rate output and the first apparent density output obtained from the Coriolis-based mass flow meter to determine a set of correlation equations; flowing a second gas/liquid stream through the Coriolis-based mass flow meter; obtaining a second apparent mass flow rate output and a second apparent density output from the Coriolis-based mass flow meter; calculating a total mass flow rate and a component phase distribution of the second gas/liquid stream based on the correlation equations and the second apparent mass flow rate output and the second apparent density output.

  1. Thin layer chromatography coupled to paper spray ionization mass spectrometry for cocaine and its adulterants analysis.

    PubMed

    De Carvalho, Thays C; Tosato, Flavia; Souza, Lindamara M; Santos, Heloa; Merlo, Bianca B; Ortiz, Rafael S; Rodrigues, Rayza R T; Filgueiras, Paulo R; França, Hildegardo S; Augusti, Rodinei; Romão, Wanderson; Vaz, Boniek G

    2016-05-01

    Thin layer chromatography (TLC) is a simple and inexpensive type of chromatography that is extensively used in forensic laboratories for drugs of abuse analysis. In this work, TLC is optimized to analyze cocaine and its adulterants (caffeine, benzocaine, lidocaine and phenacetin) in which the sensitivity (visual determination of LOD from 0.5 to 14mgmL(-1)) and the selectivity (from the study of three different eluents: CHCl3:CH3OH:HCOOHglacial (75:20:5v%), (C2H5)2O:CHCl3 (50:50v%) and CH3OH:NH4OH (100:1.5v%)) were evaluated. Aiming to improve these figures of merit, the TLC spots were identified and quantified (linearity with R(2)>0.98) by the paper spray ionization mass spectrometry (PS-MS), reaching now lower LOD values (>1.0μgmL(-1)). The method developed in this work open up perspective of enhancing the reliability of traditional and routine TLC analysis employed in the criminal expertise units. Higher sensitivity, selectivity and rapidity can be provided in forensic reports, besides the possibility of quantitative analysis. Due to the great simplicity, the PS(+)-MS technique can also be coupled directly to other separation techniques such as the paper chromatography and can still be used in analyses of LSD blotter, documents and synthetic drugs. PMID:26970868

  2. Analysis of volatile organic compounds in groundwater samples by gas chromatography-mass spectrometry

    SciTech Connect

    Bernhardt, J.

    1995-08-23

    The Savannah River Site contains approximately 1500 monitoring wells from which groundwater samples are collected. Many of these samples are sent off-site for various analyses, including the determination of trace volatile organic compounds (VOCs). This report describes accomplishments that have been made during the past year which will ultimately allow VOC analysis to be performed on-site using gas chromatography-mass spectrometry. Through the use of the on-site approach, it is expected that there will be a substantial cost savings. This approach will also provide split-sample analysis capability which can serve as a quality control measure for off-site analysis.

  3. [Gas-liquid mass transfer in three-phase inverse turbulent bed reactor].

    PubMed

    Jin, Ren-Cun; Zheng, Ping; Chen, Jian-Wei; Tu, Zhan

    2007-01-01

    The characteristics of gas-liquid mass transfer of three-phase system comprising air, tap water/wastewater, and hollow glass beads were studied in a laboratory-scale inverse turbulent bed reactor. The influence of operational factors and liquid property on volumetric liquid-phase mass transfer coefficient kLa was investigated under the conditions of superficial gas velocity (0.53mm xs(-1) - 10mx s(-1) solid hold-up (0 - 0.3), and superficial liquid velocity (0 - 0.2mm x s(-1)). The results showed that the coefficient value was 0.0456 - 1. 414min -, which increased with superficial gas velocity and liquid velocity. The coefficient attained the maximum value at solid hold-up of 0.05 - 0.08. Compared with the coefficient value in tap water, that in synthetic wastewater and industrial wastewater is decreased by 39.0% and 50.9%, respectively. These data have provided a basis for the process analysis and mathematical simulation of inverse turbulent bed reactor. PMID:17366900

  4. Comparison of electrical and optical characteristics in gas-phase and gas-liquid phase discharges

    SciTech Connect

    Qazi, H. I. A.; Li, He-Ping Zhang, Xiao-Fei; Bao, Cheng-Yu; Nie, Qiu-Yue

    2015-12-15

    This paper presents an AC-excited argon discharge generated using a gas-liquid (two-phase) hybrid plasma reactor, which mainly consists of a powered needle electrode enclosed in a conical quartz tube and grounded deionized water electrode. The discharges in the gas-phase, as well as in the two-phase, exhibit two discharge modes, i.e., the low current glow-like diffuse mode and the high current streamer-like constrict mode, with a mode transition, which exhibits a negative resistance of the discharges. The optical emission spectral analysis shows that the stronger diffusion of the water vapor into the discharge region in the two-phase discharges boosts up the generation of OH (A–X) radicals, and consequently, leads to a higher rotational temperature in the water-phase plasma plume than that of the gas-phase discharges. Both the increase of the power input and the decrease of the argon flow rate result in the increase of the rotational temperature in the plasma plume of the water-phase discharge. The stable two-phase discharges with a long plasma plume in the water-phase under a low power input and gas flow rate may show a promising prospect for the degradation of organic pollutants, e.g., printing and dyeing wastewater, in the field of environmental protection.

  5. Comparison of electrical and optical characteristics in gas-phase and gas-liquid phase discharges

    NASA Astrophysics Data System (ADS)

    Qazi, H. I. A.; Nie, Qiu-Yue; Li, He-Ping; Zhang, Xiao-Fei; Bao, Cheng-Yu

    2015-12-01

    This paper presents an AC-excited argon discharge generated using a gas-liquid (two-phase) hybrid plasma reactor, which mainly consists of a powered needle electrode enclosed in a conical quartz tube and grounded deionized water electrode. The discharges in the gas-phase, as well as in the two-phase, exhibit two discharge modes, i.e., the low current glow-like diffuse mode and the high current streamer-like constrict mode, with a mode transition, which exhibits a negative resistance of the discharges. The optical emission spectral analysis shows that the stronger diffusion of the water vapor into the discharge region in the two-phase discharges boosts up the generation of OH (A-X) radicals, and consequently, leads to a higher rotational temperature in the water-phase plasma plume than that of the gas-phase discharges. Both the increase of the power input and the decrease of the argon flow rate result in the increase of the rotational temperature in the plasma plume of the water-phase discharge. The stable two-phase discharges with a long plasma plume in the water-phase under a low power input and gas flow rate may show a promising prospect for the degradation of organic pollutants, e.g., printing and dyeing wastewater, in the field of environmental protection.

  6. Gas-liquid mass transfer in filamentous slurries in airlift bioreactors

    SciTech Connect

    Chisti, M.Y.; Moo-Young, M. )

    1988-01-01

    Biotechnology production processes are often critically dependent on oxygen transfer in gas-liquid-solid multiphase systems. Some of these biofluid slurries are composed of fibrous or filamentous, mycelial, solids suspended in a water-like medium. Examples are the broths of Aspergilli, Penicillia, Neurospora and Streptomyces, all of which are of commercial importance. This paper reports of the gas-liquid mass transfer behaviour of aqueous slurries of cellulose fibre solids (1-3 wt./vol. % solids in 0.15 kmol m/sup -3/ NaCl) which simulate the filamentous fermentation broths of interest. Fundamental investigations into the relationship between the mass transfer coefficient (k/sub L/) and bubble diameter (d/sub B/) are undertaken. The observations can be usefully employed for scale-up of bioreactors for gas-liquid mass transfer as demonstrated in the paper.

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

    SciTech Connect

    Tu, X.; Yu, L.; Yan, J. H.; Cen, K. F.; Cheron, B. G.

    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.

  8. Measurement of pressure fluctuation in gas-liquid two-phase vortex street

    NASA Astrophysics Data System (ADS)

    Sun, Zhiqiang; Sang, Wenhui; Zhang, Hongjian

    2009-02-01

    The pressure fluctuation in the wake is an important parameter to characterize the shedding process of gas-liquid two-phase Karman vortex street. This paper investigated such pressure fluctuations in a horizontal pipe using air and water as the tested fluid media. The dynamic signal representing the pressure fluctuation was acquired by the duct-wall differential pressure method. Results show that in the wake of the gas-liquid two-phase Karman vortex street, the frequency of the pressure fluctuation is linear with the Reynolds number when the volume void fraction is within the range of 18%. Moreover, the mean amplitude of the pressure fluctuation decreases with the volume void fraction, and the mean amplitude is larger at higher water flowrates under the same volume void fraction. These findings contribute to an in-depth understanding of the gas-liquid two-phase Karman vortex street.

  9. Carbon-based sorbents in chromatography. New achievements.

    PubMed

    Cserháti, T

    2009-02-01

    The newest results in the employment of carbon-based composites in various chromatographic techniques such as gas-liquid chromatography, high-performance liquid chromatography and electrically driven separation techniques for the separation, quantitative determination and identification of a wide variety of compounds in complicated matrices are compiled. The results are concisely described and critically evaluated. The future trends in the application of carbon-based compounds in the chromatographic separation methods are briefly discussed. PMID:19137510

  10. Multiresidue analysis of pesticides in traditional Chinese medicines using gas chromatography - negative chemical ionization tandem mass spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In this study, a residue analysis method for the simultaneous determination of 107 pesticides in the traditional Chinese medicines (TCMs), Angelica sinensis, Angelica dahurica, Leonurus heterophyllus Sweet, Pogostemon cablin, and Lonicera japonica Thunb, was developed using gas chromatography couple...

  11. EXTRACTION AND QUANTITATIVE ANALYSIS OF ELEMENTAL SULFUR FROM SULFIDE MINERAL SURFACES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY. (R826189)

    EPA Science Inventory

    A simple method for the quantitative determination of elemental sulfur on oxidized sulfide minerals is described. Extraction of elemental sulfur in perchloroethylene and subsequent analysis with high-performance liquid chromatography were used to ascertain the total elemental ...

  12. Ion Chromatography.

    ERIC Educational Resources Information Center

    Mulik, James D.; Sawicki, Eugene

    1979-01-01

    Accurate for the analysis of ions in solution, this form of analysis enables the analyst to directly assay many compounds that previously were difficult or impossible to analyze. The method is a combination of the methodologies of ion exchange, liquid chromatography, and conductimetric determination with eluant suppression. (Author/RE)

  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 μg/kg, respectively; recovery values ranged from 72.8-94.6%; precision was lower than 3%. For avocado, limit of detection values were ˂450 μg/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. High pH reversed-phase chromatography with fraction concatenation for 2D proteomic analysis

    SciTech Connect

    Yang, Feng; Shen, Yufeng; Camp, David G.; Smith, Richard D.

    2012-04-01

    Orthogonal high-resolution separations are critical for attaining improved analytical dynamic ranges of proteome measurements. Concatenated high pH reversed phase liquid chromatography affords better separations than the strong cation exchange conventionally applied for two-dimensional shotgun proteomic analysis. For example, concatenated high pH reversed phase liquid chromatography increased identification coverage for peptides (e.g., by 1.8-fold) and proteins (e.g., by 1.6-fold) in shotgun proteomics analyses of a digested human protein sample. Additional advantages of concatenated high pH RPLC include improved protein sequence coverage, simplified sample processing, and reduced sample losses, making this an attractive first dimension separation strategy for two-dimensional proteomics analyses.

  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-μL NMR cell, Instead of a smaller 14-μL 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. Identification of polar organic compounds in coal-gasification condensate water by gas chromatography-mass spectrometry analysis of high-performance liquid chromatography fractions

    SciTech Connect

    Mohr, D.H.; King, C.J.

    1985-10-01

    A novel combination of analytical techniques was employed to identify polar organic compounds, including the first report of hydantoins, in condensate waters from a slagging fixed-bed coal-gasification process. The analytical technique consists of high-performance liquid chromatography (HPLC) separation and gas chromatography-mass spectrometry (GC-MS) analysis of HPLC fractions. Entrainer distillation was used to concentrate the HPLC fractions and remove water before GC-MS analysis. Analyses of four samples accounted for 69-84% of the measured chemical oxygen demand (COD), including 1-6% of the COD as dimethylhydantoin. This compound is highly polar and difficult to remove by solvent extraction. Other identified compounds included phenols, di-hydroxybenzenes, methanol, acetone, and acetonitrile. Many of the unidentified compounds (16-31% of the COD) were difficult to extract, had low volatility relative to water, and contained organic nitrogen. Some chemical changes were observed during storage of condensate water samples.

  17. Gas-liquid coexistence in a system of dipolar soft spheres.

    PubMed

    Jia, Ran; Braun, Heiko; Hentschke, Reinhard

    2010-12-01

    The existence of gas-liquid coexistence in dipolar fluids with no other contribution to attractive interaction than dipole-dipole interaction is a basic and open question in the theory of fluids. Here we compute the gas-liquid critical point in a system of dipolar soft spheres subject to an external electric field using molecular dynamics computer simulation. Tracking the critical point as the field strength is approaching zero we find the following limiting values: T(c)=0.063 and ?(c)=0.0033 (dipole moment ?=1). These values are confirmed by independent simulation at zero field strength. PMID:21230693

  18. The effects of bubbles on the structure of upward gas-liquid flow

    NASA Astrophysics Data System (ADS)

    Gubaidulin, D. A.; Snigerev, B. A.

    2016-01-01

    The paper presents the results of study of the local structure of turbulent gas-liquid flow in vertical pipe. A mathematical model based on the use of Eulerian description for both phases taking into account the action of different forces of interfacial interaction. Special attention is paid to the development of approaches for the simulation of polydispersed bubbly flows taking into account processes of coagulation and fragmentation. Comparison of simulation results with experimental data showed that the developed approach allows to obtain detailed information about the structures of turbulent gas-liquid flows, the distribution of bubbles by size.

  19. Gas-liquid mass transfer in a three-phase fluidized bed containing low density particles

    SciTech Connect

    Tang, W.T. ); Fan, L.S. . Dept. of Chemical Engineering)

    1990-01-01

    Gas-liquid mass-transfer behavior in a three-phase fluidized bed containing particles with properties comparable to those of bioparticles used in biological processes was examined. The volumetric gas-liquid mass-transfer coefficients, k{sub L}a, decrease with increasing solid concentration and with increasing terminal velocity of particles. An increase in the liquid velocity significantly increases k{sub L}a, but only slightly increases the gas holdup, thus suggesting a significant liquid velocity effect on k{sub L}.

  20. MISER chiral supercritical fluid chromatography for high throughput analysis of enantiopurity.

    PubMed

    Zawatzky, Kerstin; Biba, Mirlinda; Regalado, Erik L; Welch, Christopher J

    2016-01-15

    MISER chromatographic analysis (Multiple Injections in a Single Experimental Run) using supercritical fluid chromatography (SFC) with pressurized carbon dioxide-based eluents is well suited to the high throughput analysis of enantiopurity. SFC is currently the preferred method for fast enantiopurity analysis, with analysis times of only a few seconds achievable in some cases. Injector programming using both the Agilent Infinity and Shimadzu Nexera UC instruments permitted MISER SFC experiments to be performed. Several case studies are presented, showcasing the power and versatility of the technique, with 'plate analysis times' (the time required for analysis of enantiopurity of 96 samples) of less than 33-34min achievable in the best cases. PMID:26747691

  1. Flavor characterization of ripened cod roe by gas chromatography, sensory analysis, and electronic nose.

    PubMed

    Jonsdottir, Rosa; Olafsdottir, Gudrun; Martinsdottir, Emilia; Stefansson, Gudmundur

    2004-10-01

    Characterization of the flavors of ripened roe products is of importance to establish a basis for a standardized product. Flavor profiles of commercially processed ripened roe from Iceland and Norway were studied by sensory analysis, gas chromatography-olfactometry (GC-O), gas chromatography-mass spectrometry (GC-MS), and an electronic nose to characterize the headspace of ripened roe. Sensory analysis showed that ripened roe odor and flavor in combination with caviar flavor and whey/caramel-like odor give the overall positive effect of the complex characteristic roe flavor. Analysis of volatiles by GC-MS and electronic nose confirmed the presence of aroma compounds contributing to the typical ripening and spoilage flavors detected by the sensory analysis. Methional, 1-octen-3-ol, and 2,6-nonadienal were the most important compounds contributing to ripened roe odor. Spoilage flavors were partly contributed by 3-methyl-1-butanol and 3-methylbutanal, which can be measured by the electronic nose and are suggested as quality indicators for objectively assessing the ripening of roe. Principal component analysis of the overall data showed that GC-O correlated well with sensory evaluation and the electronic nose measurements. PMID:15453695

  2. Multivariate data analysis to characterize gas chromatography columns for dioxin analysis.

    PubMed

    Do, Lan; Geladi, Paul; Haglund, Peter

    2014-06-20

    Principal component analysis (PCA) was applied for evaluating the selectivity of 22 GC columns for which complete retention data were available for the 136 tetra- to octa-chlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs). Because the hepta- and octa-homologues are easy to separate the PCA was focused on the 128 tetra- to hexa-CDD/Fs. The analysis showed that 21 of the 22 GC columns could be subdivided into four groups with different selectivity. Group I consists of columns with non-polar thermally stable phases (Restek 5Sil MS and Dioxin 2, SGE BPX-DXN, Supelco Equity-5, and Agilent DB-1, DB-5, DB-5ms, VF-5ms, VF-Xms and DB-XLB). Group II includes ionic liquid columns (Supelco SLB-IL61, SLB-IL111 and SLB-IL76) with very high polarity. Group III includes columns with high-percentage phenyl and cyanopropyl phases (Agilent DB-17 and DB-225, Quadrex CPS-1, Supelco SP-2331, and Agilent CP-Sil 88), and Group IV columns with shape selectivity (Dionex SB-Smectic and Restek LC-50, Supelco βDEXcst, Agilent VF-Xms and DB-XLB). Thus, two columns appeared in both Group I and IV (Agilent VF-Xms and DB-XLB). The selectivity of the other column, Agilent DB-210, differs from those of these four groups. Partial least squares (PLS) regression was used to correlate the retention times of the tetra- to hexa-CDD/Fs on the 22 stationary phases with a set of physicochemical and structural descriptors to identify parameters that significantly influence the solute-stationary phase interactions. The most influential physicochemical parameters for the interaction were associated with molecular size (as reflects in the total energy, electron energy, core-core repulsion and standard entropy), solubility (aqueous solubility and n-octanol/water partition coefficient), charge distribution (molecular polarizability and dipolar moment), and reactivity (relative Gibbs free energy); and the most influential structural descriptors were related to these parameters, in particular, size and dipolar moment. Finally, the PCA and PLS analyses were complemented with linear regression analysis to identify the most orthogonal column combinations, which could be used in comprehensive two-dimensional gas chromatography (GC×GC) to enhance PCDD/F separation and congener profiling. PMID:24813707

  3. Intact-protein trapping columns for proteomic analysis in capillary high-performance liquid chromatography.

    PubMed

    Guan, Xia; Yan, Guoquan; Gao, Mingxia; Hong, Guangfeng; Deng, Chunhui; Zhang, Xiangmin

    2010-10-29

    A new type of monolithic trapping columns with high mechanical strength was prepared by thin-layer sol-gel coating method and applied to trapping intact proteins for on-line capillary liquid chromatography. Monolithic trapping columns were fabricated by entrapping C8 reversed-phase particles into the capillary columns through a sol-gel network, which was formed by hydrolysis and polycondensation of methyltriethoxysilane. Hundreds times of trapping/untrapping for intact proteins were carried out. The trapping columns showed long-term stability up to 300 bar. Recovery, loading capacity and reproducibility of trapping columns were evaluated using four proteins. The recovery of four protein mixtures for the C8 monolithic trapping columns was 99.3% on average. The loading capacity of 5 mm × 320 μm i.d. C8 trapping columns for the protein mixtures was 30 μg. Day-to-day relative standard deviation (RSD) values for recoveries of protein mixtures on the same C8 trapping column ranged from 2.34 to 5.87%, column-to-column RSD values were from 3.01 to 6.81%. The C8 trapping columns were used to trap normal mouse liver intact proteins in a capillary liquid chromatography system. Results demonstrated high efficiency of the monolithic trapping columns for trapping intact proteins for proteomic analysis in on-line capillary liquid chromatography system. PMID:20870240

  4. Coupling Charge Reduction Mass Spectrometry to Liquid Chromatography for Complex Mixture Analysis.

    PubMed

    Stutzman, John R; Crowe, Matthew C; Alexander, James N; Bell, Bruce M; Dunkle, Melissa N

    2016-04-01

    Electrospray ionization (ESI) of solution mixtures often generates complex mass spectra, even following liquid chromatography (LC), due to analyte multiple charging. Multiple charge state distributions can lead to isobaric interferences, mass spectral congestion, and ambiguous ion identification. As a consequence, data interpretation increases in complexity. Several charge reduction mass spectrometry (MS) approaches have been previously developed to reduce the average charge state of gaseous ions; however, all of these techniques have been restricted to direct infusion MS. In this study, synthetic polyols and surfactants separated by liquid chromatography and ionized by positive mode ESI have been subjected to polonium-210 α-particle radiation to reduce the average charge state to singly charged cations prior to mass analysis. LC/MS analysis of 5000 molecular weight poly(ethylene glycol) (PEG5000) generated an average charge state of 5.88+; whereupon, liquid chromatography/electrospray ionization/charge reduction/mass spectrometry (LC/CR/MS) analysis of PEG 5000 generated an average charge state of 1.00+. The PEG5000 results demonstrated a decrease in spectral complexity and enabled facile interpretation. Other complex solution mixtures representing specific MS challenges (i.e., competitive ionization and isobaric ion overlap) were explored and analyzed with LC/CR/MS to demonstrate the benefits of coupling LC to CR/MS. For example, polyol information related to initiator, identity/relative amount of monomer, and estimated molecular weight was characterized in random and triblock ethylene oxide/propylene oxide polyols using LC/CR/MS. LC/CR/MS is a new analytical technique for the analysis of complex mixtures. PMID:26971559

  5. Reducing Dilution and Analysis Time in Online Comprehensive Two-Dimensional Liquid Chromatography by Active Modulation.

    PubMed

    Gargano, Andrea F G; Duffin, Mike; Navarro, Pablo; Schoenmakers, Peter J

    2016-02-01

    Online comprehensive two-dimensional liquid chromatography (LC × LC) offers ways to achieve high-performance separations in terms of peak capacity (exceeding 1000) and additional selectivity to realize applications that cannot be addressed with one-dimensional chromatography (1D-LC). However, the greater resolving power of LC × LC comes at the price of higher dilutions (thus, reduced sensitivity) and, often, long analysis times (>100 min). The need to preserve the separation attained in the first dimension ((1)D) causes greater dilution for LC × LC, in comparison with 1D-LC, and long analysis times to sample the (1)D with an adequate number of second dimension separations. A way to significantly reduce these downsides is to introduce a concentration step between the two chromatographic dimensions. In this work we present a possible active-modulation approach to concentrate the fractions of (1)D effluent. A typical LC × LC system is used with the addition of a dilution flow to decrease the strength of the (1)D effluent and a modulation unit that uses trap columns. The potential of this approach is demonstrated for the separation of tristyrylphenol ethoxylate phosphate surfactants, using a combination of hydrophilic interaction and reversed-phase liquid chromatography. The modified LC × LC system enabled us to halve the analysis time necessary to obtain a similar degree of separation efficiency with respect to UHPLC based LC × LC and of 5 times with respect to HPLC instrumentation (40 compared with 80 and 200 min, respectively), while at the same time reducing dilution (DF of 142, 299, and 1529, respectively) and solvent consumption per analysis (78, 120, and 800 mL, respectively). PMID:26709410

  6. 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.

  7. [Analysis of oxygenates from fischer-Tropsch synthesis oil using column liquid chromatography and gas chromatography-mass spectrography].

    PubMed

    Fan, Gaixian; Xu, Yuanyuan; Li, Ying; Li, Ying; Xiang, Hongwei; Li, Yongwang

    2007-11-01

    A liquid chromatographic column filled with silica gel of 100 - 200 mesh was used to separate cold trap oil from Fischer-Tropsch synthesis with dimethylsulfoxide (DMSO) as eluent. With this pretreatment method, the cold trap oil was separated into two major classes, namely, hydrocarbons and oxygenates. Minor components were also enriched and determined, and small peaks adjacent to big peaks and tailings were also well solved. The oxygenates were then analyzed with gas chromatography-mass spectrometry (GC-MS), and 139 components were identified. PMID:18257312

  8. In situ search for organics by gas chromatography analysis: new derivatization / thermochemolysis approach

    NASA Astrophysics Data System (ADS)

    Geffroy, Claude; Buch, Arnaud; David, Marc; Aissat, Lyes; El Mufleh, Amel; Papot, S.; Sternberg, Robert

    Many organic molecules are present in interstellar clouds and might be carried to the early Earth by comets and meteorites during the heavy bombardment phase in the first few hundred million years of the solar system. It has been suggested that extraterrestrial organic material may well represent an important part of the organic material available for the origin of life. Until samples, brought by future space missions, are available on Earth, in situ measurements are one of the way to get unaltered and non-contaminated samples for analysis. The analytical technique has to be robust, sensitive and non-specific due to the large scope of targets molecules. The only currently flight qualified technique of analysis of organic molecules in space is gas chromatography (Viking, Cassini-Huygens, SAM-MSL, COSAC-Rosetta). The main objective of this work is to present a new approach with multi step analysis using derivatisation and thermochemolysis reagents for a one pot in situ analysis of volatile and refractory organics in surface or sub-surface samples (Mars, comets).Indeed, no single technology enables to identify all organic compounds because naturally occurring molecules have different polarities, molecular weights, being extractible or recalcitrant, bonded trapped or adsorbed on minerals. Thus, we propose to wider the scope of chemical reagent already validated for in situ wet chemistry such as MTBSTFA (Rodier et al. 2001, 2002), DMF-DMA (Rodier et al. 2002), or TMAH (Rodier et al, 2005, Geffroy-Rodier et al; 2009) to analyze enantiomers of amino acids, carbohydrates and lipids in a one pot several steps sub system using a multi reagent and multi step approach. Thus using a new derivatizing agent, we successfully identified twenty one amino acids including twelve of the twenty proteinic amino acids without inhibiting following multi step thermochemolysis. *Geffroy-Rodier C, Grasset L, Sternberg R. Buch A. Amblès A. (2009) Thermochemolysis in search for organics in extraterrestrial environments, Journal of Applied Pyrolysis 85: 454-459. *Rodier C, Sternberg R, Raulin F, Vidal-Madjar C (2001). In situ detection of organic molecules in extraterrestrial environment by gas chromatography / mass spectrometry. Journal of Chromatography A 915: 199-207. *Rodier C, Laurent C, Szopa C. Sternberg R, Raulin F (2002) Chirality and the origin of life: in situ enantiomeric separation for future space missions, Chirality 14: 527-532. *Rodier C. Sternberg R, Szopa C, Buch A, Cabane M and Raulin F (2005) Search for organics in extraterrestrial environments by in situ gas chromatography analysis. Advances in Space Research 36: 195-200. This work has been funded by CNES

  9. 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

  10. Chiral recognition ability of alpha-cyclodextrin with regard to some monoterpenoids under gas-liquid chromatographic conditions.

    PubMed

    Asztemborska, Monika; Sybilska, Danuta; Nowakowski, Robert; Perez, Giorgio

    2003-08-29

    Gas-liquid chromatography was applied to investigate the mechanism of alpha-cyclodextrin (alpha-CD) complexation processes with some chiral monoterpenoids differing from each other in chemical properties and structure. They were chosen from hydrocarbons, alcohols, aldehydes and ketones of acyclic, monocyclic and bicyclic structure. The relationships between the retention factor, k, of a guest solute (G) and alpha-CD concentration were studied. The obtained data enabled the stoichiometry, the stability of individual complexes and the separation factor of enantiomers to be determined. It was found that almost all the investigated monoterpenoids, apart from the acyclic ones, form inclusion complexes with alpha-CD. Straight-line relations (r vs. [alpha-CD]) were observed for monocyclic alcohols and pulegone, without any trace of enantioselectivity. This behaviour indicates that the 1:1 stoichiometry of the G-CD complexes does not lead to chiral recognition. Parabolic relations arising from 1:2 stoichiometry were found for limonene, alpha-phellandrene, some monocycylic ketones and all the investigated bicyclic terpenoids. It appeared that only the second step of complexation displayed marked enantioselectivity. However, a loss of efficiency resulting from slower equilibration is then noticeable. Attempts are made to rationalize the chromatographic results with respect to the structure of the investigated compounds. PMID:12974293

  11. Gas/liquid sensing via chemotaxis of Euglena cells confined in an isolated micro-aquarium.

    PubMed

    Ozasa, Kazunari; Lee, Jeesoo; Song, Simon; Hara, Masahiko; Maeda, Mizuo

    2013-10-21

    We demonstrate on-chip gas/liquid sensing by using the chemotaxis of live bacteria (Euglena gracilis) confined in an isolated micro-aquarium, and gas/liquid permeation through porous polydimethylsiloxane (PDMS). The sensing chip consisted of one closed micro-aquarium and two separated bypass microchannels along the perimeter of the micro-aquarium. Test gas/liquid and reference samples were introduced into the two individual microchannels separately, and the gas/liquid permeated through the PDMS walls and dissolved in the micro-aquarium water, resulting in a chemical concentration gradient in the micro-aquarium. By employing the closed micro-aquarium isolated from sample flows, we succeeded in measuring the chemotaxis of Euglena for a gas substance quantitatively, which cannot be achieved with the conventional flow-type or hydro-gel-type microfluidic devices. We found positive (negative) chemotaxis for CO2 concentrations below (above) 15%, with 64 ppm as the minimum concentration affecting the cells. We also observed chemotaxis for ethanol and H2O2. By supplying culture medium via the microchannels, the Euglena culture remained alive for more than 2 months. The sensing chip is thus useful for culturing cells and using them for environmental toxicity/nutrition studies by monitoring their motion. PMID:23934095

  12. Discrimination of honeys using colorimetric sensor arrays, sensory analysis and gas chromatography techniques.

    PubMed

    Tahir, Haroon Elrasheid; Xiaobo, Zou; Xiaowei, Huang; Jiyong, Shi; Mariod, Abdalbasit Adam

    2016-09-01

    Aroma profiles of six honey varieties of different botanical origins were investigated using colorimetric sensor array, gas chromatography-mass spectrometry (GC-MS) and descriptive sensory analysis. Fifty-eight aroma compounds were identified, including 2 norisoprenoids, 5 hydrocarbons, 4 terpenes, 6 phenols, 7 ketones, 9 acids, 12 aldehydes and 13 alcohols. Twenty abundant or active compounds were chosen as key compounds to characterize honey aroma. Discrimination of the honeys was subsequently implemented using multivariate analysis, including hierarchical clustering analysis (HCA) and principal component analysis (PCA). Honeys of the same botanical origin were grouped together in the PCA score plot and HCA dendrogram. SPME-GC/MS and colorimetric sensor array were able to discriminate the honeys effectively with the advantages of being rapid, simple and low-cost. Moreover, partial least squares regression (PLSR) was applied to indicate the relationship between sensory descriptors and aroma compounds. PMID:27041295

  13. Supercritical fluid chromatography for GMP analysis in support of pharmaceutical development and manufacturing activities.

    PubMed

    Hicks, Michael B; Regalado, Erik L; Tan, Feng; Gong, Xiaoyi; Welch, Christopher J

    2016-01-01

    Supercritical fluid chromatography (SFC) has long been a preferred method for enantiopurity analysis in support of pharmaceutical discovery and development, but implementation of the technique in regulated GMP laboratories has been somewhat slow, owing to limitations in instrument sensitivity, reproducibility, accuracy and robustness. In recent years, commercialization of next generation analytical SFC instrumentation has addressed previous shortcomings, making the technique better suited for GMP analysis. In this study we investigate the use of modern SFC for enantiopurity analysis of several pharmaceutical intermediates and compare the results with the conventional HPLC approaches historically used for analysis in a GMP setting. The findings clearly illustrate that modern SFC now exhibits improved precision, reproducibility, accuracy and robustness; also providing superior resolution and peak capacity compared to HPLC. Based on these findings, the use of modern chiral SFC is recommended for GMP studies of stereochemistry in pharmaceutical development and manufacturing. PMID:26412720

  14. 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)

  15. Study on the gas-liquid interface and polymer melt front in gas-assisted injection molding

    SciTech Connect

    Shen, Y.K.

    1997-03-01

    The algorithms are developed to predict the gas-liquid interface in gas-assisted injection molding. The simulation of two-dimensional, transient, non-isothermal and high viscous flow between two parallel plates with the generalized Newtonian fluid is presented in detail. The model takes into account the effects of the gas-liquid interface and polymer melt front.

  16. Approach to hydrophilic interaction chromatography column selection: application to neurotransmitters analysis.

    PubMed

    Chirita, Raluca-Ioana; West, Caroline; Finaru, Adriana-Luminita; Elfakir, Claire

    2010-04-30

    This paper presents the comparison between 12 hydrophilic interaction liquid chromatography columns that are commercially available. The main factors influencing the retention and selectivity toward 12 neurotransmitters for these different HILIC systems have been studied. For additional information, the retention data have been analyzed statistically by factor analysis. Principal component analyses (PCA) were calculated to evidence different separation behaviour between the stationary phases, based on the retention data measured for three compound classes: anionic acidic compounds, cationic basic compounds and zwitterionic amino acids. Finally, a generic procedure is suggested for optimization of HILIC analyses, depending on the ionization state of the analytes. PMID:20338567

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

    USGS Publications Warehouse

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

    1988-01-01

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

  18. Analysis of limonoid glucosides from citrus by electrospray ionization liquid chromatography-mass spectrometry.

    PubMed

    Schoch, T K; Manners, G D; Hasegawa, S

    2001-03-01

    An electrospray ionization liquid chromatography-mass spectrometry (ESI-LC-MS) method for the detection and quantitation of limonoid glucosides has been developed. Negative ions [M - H(+)](-) characteristic of six limonoid glucosides can be detected and quantified from selected ion monitoring chromatograms using carminic acid as an internal standard. The described method has been applied to the analysis of limonoid glucoside content in various liquid and solid Citrus spp. samples as well as complex mixtures of partially purified limonoid glucosides. Rapid and sensitive qualitative screening of samples for limonoid glucosides can also be accomplished with slight modifications of the method. PMID:11312819

  19. Issues pertaining to the analysis of buprenorphine and its metabolites by gas chromatography-mass spectrometry.

    PubMed

    Wang, Yu-Shan; Lin, Dong-Liang; Yang, Shu-Ching; Wu, Meng-Yan; Liu, Ray H; Su, Lien-Wen; Cheng, Pai-Sheng; Liu, Chiareiy; Fuh, Ming-Ren

    2010-03-01

    "Substitution therapy" and the use of buprenorphine (B) as an agent for treating heroin addiction continue to gain acceptance and have recently been implemented in Taiwan. Mature and widely utilized gas chromatography-mass spectrometry (GC-MS) technology can complement the low cost and highly sensitive immunoassay (IA) approach to facilitate the implementation of analytical tasks supporting compliance monitoring and pharmacokinetic/pharmacogenetic studies. Issues critical to GC-MS analysis of B and norbuprenorphine (NB) (free and as glucuronides), including extraction, hydrolysis, derivatization, and quantitation approaches were studied, followed by comparing the resulting data against those derived from IA and two types of liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods. Commercial solid-phase extraction devices, highly effective for recovering all metabolites, may not be suitable for the analysis of free B and NB; acetyl-derivatization products exhibit the most favorable chromatographic, ion intensity, and cross-contribution characteristics for GC-MS analysis. Evaluation of IA, GC-MS, and LC-MS/MS data obtained in three laboratories has proven the 2-aliquot GC-MS protocol effective for the determination of free B and NB and their glucuronides. PMID:20122691

  20. Metabolome analysis via comprehensive two-dimensional liquid chromatography: identification of modified nucleosides from RNA metabolism.

    PubMed

    Willmann, Lucas; Erbes, Thalia; Krieger, Sonja; Trafkowski, Jens; Rodamer, Michael; Kammerer, Bernd

    2015-05-01

    Modified nucleosides derived from the RNA metabolism constitute an important chemical class, which are discussed as potential biomarkers in the detection of mammalian breast cancer. Not only the variability of modifications, but also the complexity of biological matrices such as urinary samples poses challenges in the analysis of modified nucleosides. In the present work, a comprehensive two-dimensional liquid chromatography mass spectrometry (2D-LC-MS) approach for the analysis of modified nucleosides in biological samples was established. For prepurification of urinary samples and cell culture supernatants, we performed a cis-diol specific affinity chromatography using boronate-derivatized polyacrylamide gel. In order to establish a 2D-LC method, we tested numerous column combinations and chromatographic conditions. In order to determine the target compounds, we coupled the 2D-LC setup to a triple quadrupole mass spectrometer performing full scans, neutral loss scans, and multiple reaction monitoring (MRM). The combination of a Zorbax Eclipse Plus C18 column with a Zorbax Bonus-RP column was found to deliver a high degree of orthogonality and adequate separation. By application of 2D-LC-MS approaches, we were able to detect 28 target compounds from RNA metabolism and crosslinked pathways in urinary samples and 26 target compounds in cell culture supernatants, respectively. This is the first demonstration of the applicability and benefit of 2D-LC-MS for the targeted metabolome analysis of modified nucleosides and compounds from crosslinked pathways in different biological matrices. PMID:25736241

  1. Study of gas-liquid flow in model porous media for heterogeneous catalysis

    NASA Astrophysics Data System (ADS)

    Francois, Marie; Bodiguel, Hugues; Guillot, Pierre; Laboratory of the Future Team

    2015-11-01

    Heterogeneous catalysis of chemical reactions involving a gas and a liquid phase is usually achieved in fixed bed reactors. Four hydrodynamic regimes have been observed. They depend on the total flow rate and the ratio between liquid and gas flow rate. Flow properties in these regimes influence transfer rates. Rather few attempts to access local characterization have been proposed yet, though these seem to be necessary to better describe the physical mechanisms involved. In this work, we propose to mimic slices of reactor by using two-dimensional porous media. We have developed a two-dimensional system that is transparent to allow the direct observation of the flow and the phase distribution. While varying the total flow rate and the gas/liquid flow rate ratio, we observe two hydrodynamic regimes: at low flow rate, the gaseous phase is continuous (trickle flow), while it is discontinuous at higher flow rate (pulsed flow). Thanks to some image analysis techniques, we are able to quantify the local apparent liquid saturation in the system. Its fluctuations in time are characteristic of the transition between the two regimes: at low liquid flow rates, they are negligible since the liquid/gas interface is fixed, whereas at higher flow rates we observe an alternation between liquid and gas. This transition between trickle to pulsed flow is in relative good agreement with the existing state of art. However, we report in the pulsed regime important flow heterogeneities at the scale of a few pores. These heterogeneities are likely to have a strong influence on mass transfers. We acknowledge the support of Solvay.

  2. Comprehensive two-dimensional gas chromatography applied to illicit drug analysis.

    PubMed

    Mitrevski, Blagoj; Wynne, Paul; Marriott, Philip J

    2011-11-01

    Multidimensional gas chromatography (MDGC), and especially its latest incarnation--comprehensive two-dimensional gas chromatography (GC × GC)--have proved advantageous over and above classic one-dimensional gas chromatography (1D GC) in many areas of analysis by offering improved peak capacity, often enhanced sensitivity and, especially in the case of GC × GC, the unique feature of 'structured' chromatograms. This article reviews recent advances in MDGC and GC × GC in drug analysis with special focus on ecstasy, heroin and cocaine profiling. Although 1D GC is still the method of choice for drug profiling in most laboratories because of its simplicity and instrument availability, GC × GC is a tempting proposition for this purpose because of its ability to generate a higher net information content. Effluent refocusing due to the modulation (compression) process, combined with the separation on two 'orthogonal' columns, results in more components being well resolved and therefore being analytically and statistically useful to the profile. The spread of the components in the two-dimensional plots is strongly dependent on the extent of retention 'orthogonality' (i.e. the extent to which the two phases possess different or independent retention mechanisms towards sample constituents) between the two columns. The benefits of 'information-driven' drug profiling, where more points of reference are usually required for sample differentiation, are discussed. In addition, several limitations in application of MDGC in drug profiling, including data acquisition rate, column temperature limit, column phase orthogonality and chiral separation, are considered and discussed. Although the review focuses on the articles published in the last decade, a brief chronological preview of the profiling methods used throughout the last three decades is given. PMID:21769552

  3. Analysis and purification of nucleic acids by ion-pair reversed-phase high-performance liquid chromatography.

    PubMed

    Hecker, K H; Green, S M; Kobayashi, K

    2000-11-20

    Sizing of DNA fragments is a routine analysis traditionally performed on agarose or polyacrylamide gels. Electrophoretic analysis is labor-intensive with only limited potential for automation. Recovery of DNA fragments from gels is cumbersome. We present data on automated, size-based separation of DNA fragments by ion-pair reversed-phase high performance liquid chromatography (IP RP HPLC) - DNA chromatography - on the WAVE DNA Fragment Analysis System with the DNASep cartridge. This system is suitable for accurate and rapid sizing of double-stranded (ds) DNA fragments from 50 to ca. 2000 base pairs (bp). Fluorescently labeled DNA fragments are compatible with the technology. Length-dependent separation of dsDNA fragments is sequence independent and retention times are highly reproducible. The resolving capabilities of DNA chromatography are illustrated by the analysis of multiple DNA size markers. Resolved dsDNA fragments are easily collected and are suitable for downstream applications such as sequencing and cloning. DNA chromatography under denaturing conditions with fluorescently labeled DNA fragments offers a means for the separation and purification of individual strands of dsDNA. Analysis of DNA fragments on the WAVE System is highly automated and requires minimal manual intervention. DNA chromatography offers a reliable and automated alternative to gel electrophoresis for the analysis of DNA fragments. PMID:11086196

  4. Trace analysis of estradiol in animal chow by electron-capture gas chromatography.

    PubMed

    Bowman, M C; Nony, C R

    1977-05-10

    A gas chromatographic method is described for trace analysis of the natural steroidal hormone estradiol in animal chow at levels as low as 3 ppb. Salient elements of the method include extraction of the estradiol with methanol, an initial clean-up on a column of Sepadex LH-20, liquid-liquid partitioning at pH 14 and 10.2, additional cleanup on a slilica gel column, conversion of the estradiol to the pentafluoropropionly (PFP) derivative and analysis by electron-capture gas chromatography on a column of OV-25. Samples containing less than ppb of estradiol are subjected to further clean-up on silica gel after derivatization and prior to analysis. PMID:863991

  5. Application of Pre-Column Labeling Liquid Chromatography for Canine Plasma-Free Amino Acid Analysis

    PubMed Central

    Azuma, Kazuo; Hirao, Yoshiko; Hayakawa, Yoshihiro; Murahata, Yusuke; Osaki, Tomohiro; Tsuka, Takeshi; Imagawa, Tomohiro; Okamoto, Yoshiharu; Ito, Norihiko

    2016-01-01

    Plasma-free amino acid (PFAA) levels are a useful metric for diagnosing cancer and providing a prognosis. However, the use of analysis of PFAA levels has been limited in the veterinary medicine field. We addressed the application of liquid chromatography (LC) using a pre-column labeling technique for analysis of canine PFAA levels. This method significantly shortened the analysis time relative to conventional methods. No diurnal fluctuations were detected at 9:00 AM in most PFAA levels, and food intake increased the levels of some PFAAs, including valine, leucine, tyrosine, phenylalanine, and proline. These results indicate that LC with pre-column labeling is useful for measuring canine PFAA levels, for which time of day and interval after food intake must be taken into consideration. PMID:26771650

  6. Application of Pre-Column Labeling Liquid Chromatography for Canine Plasma-Free Amino Acid Analysis.

    PubMed

    Azuma, Kazuo; Hirao, Yoshiko; Hayakawa, Yoshihiro; Murahata, Yusuke; Osaki, Tomohiro; Tsuka, Takeshi; Imagawa, Tomohiro; Okamoto, Yoshiharu; Ito, Norihiko

    2016-01-01

    Plasma-free amino acid (PFAA) levels are a useful metric for diagnosing cancer and providing a prognosis. However, the use of analysis of PFAA levels has been limited in the veterinary medicine field. We addressed the application of liquid chromatography (LC) using a pre-column labeling technique for analysis of canine PFAA levels. This method significantly shortened the analysis time relative to conventional methods. No diurnal fluctuations were detected at 9:00 AM in most PFAA levels, and food intake increased the levels of some PFAAs, including valine, leucine, tyrosine, phenylalanine, and proline. These results indicate that LC with pre-column labeling is useful for measuring canine PFAA levels, for which time of day and interval after food intake must be taken into consideration. PMID:26771650

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

    PubMed

    Bartsch, Jennifer; Uhde, Erik; Salthammer, Tunga

    2016-01-21

    Scented consumer products are being bought in increasing amounts and gaining more popularity. There is, however, relatively little information available about their ingredients, emissions and allergenic potential. Frequently, a mixture of different fragrance substances and not solely an individual substance contributes to the overall desired smell. The aim of this study was to investigate the odorous volatile organic compounds (OVOCs) in consumer products containing fragrances. Over 44 products were selected: various scented candles, printing products with different scent types and other products types particularly meant to be used indoors. Measurements were carried out in a desiccator. Air samples were collected on thermal desorption tubes to determine the released fragrance substances by means of gas chromatography-mass spectrometry (GC-MS). Moreover, gas chromatography-olfactometry (GC-O) was used to obtain sensory data and to ensure no important odorant was overlooked. Using both methods it was possible to distinguish between odour active and inactive compounds and subsequently to identify almost 300 different odorants across all scented products. Besides the advantage of differentiation, as the human nose is a very sensitive detector, GC-O was found to be a useful tool for detecting traces and chosen target compounds. One focus in this study lay on the 26 EU-regulated fragrance allergens to prove their relevance in scented consumer goods. In total, 18 of them were identified, with at least one substance being present in almost every product. Benzyl alcohol, cinnamaldehyde, citronellol, eugenol, linalool and limonene were the prevalently detected allergens. Particularly linalool and limonene were observed in over 50% of the products. In addition, eugenol appeared to be one of the most frequently detected compounds in trace-level concentrations in the candle emissions. PMID:26724768

  8. Multivariate analysis of progressive thermal desorption coupled gas chromatography-mass spectrometry.

    SciTech Connect

    Van Benthem, Mark Hilary; Mowry, Curtis Dale; Kotula, Paul Gabriel; Borek, Theodore Thaddeus, III

    2010-09-01

    Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that vary as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief that this multivariate analysis will enable superior differentiation capabilities. In addition, noise and system artifacts challenge the analysis of GC-MS data collected on lower cost equipment, ubiquitous in commercial laboratories. This research has the potential to affect many areas of analytical chemistry including materials analysis, medical testing, and environmental surveillance. It could also provide a method to measure adsorption parameters for chemical interactions on various surfaces by measuring desorption as a function of temperature for mixtures. We have presented results of a novel method for examining offgas products of a common PDMS material. Our method involves utilizing a stepped TD/GC-MS data acquisition scheme that may be almost totally automated, coupled with multivariate analysis schemes. This method of data generation and analysis can be applied to a number of materials aging and thermal degradation studies.

  9. Use of permeation devices in the analysis of sulfur gases by gas chromatography

    SciTech Connect

    Flowers, D.G. )

    1990-07-01

    This paper describes instrumental techniques currently available for the analysis of parts per million (PPM) concentrations of sulfur gas compounds. These techniques are based on numerous chemical principles including spectroscopy, chromatography, or chemical reaction with a specific reagent. In order to achieve accurate results with these instruments, reliable standards at suitable concentrations of the sulfur compound analyte are required for proper calibration. Progress in the development of polymeric materials coupled with advances in membrane technology has led to the innovation of permeation devices for use as gas calibration standards. The principle of these devices is the controlled release of a specified compound by permeation across a polymeric material. The G-Cal tube is a commercially available permeation device which possesses sufficient thermal stability to permit usage without thermostatic control. For the analysis of sulfur gas compounds by gas chromatography, permeation devices offer an economical alternative to compressed gas standards. The use of these devices offers a safety advantage in the handling of toxic sulfur gases while minimizing the chemical reactivity inherent in sulfide and mercaptan compounds.

  10. Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

    PubMed

    Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

    2016-03-01

    A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples. PMID:26471553

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

    PubMed

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

    2015-12-11

    Ion-exchange chromatography (IEC) is widely used for profiling the charge heterogeneity of proteins, including monoclonal antibodies (mAbs). Despite good resolving power and robustness, ionic strength-based ion-exchange separations are generally product specific and can be time consuming to develop. In addition, conventional analytical scale ion-exchange separations require tens of micrograms of mAbs for each injection, amounts that are often unavailable in sample-limited applications. We report the development of a capillary IEC (c-IEC) methodology for the analysis of nanogram amounts of mAb charge variants. Several key modifications were made to a commercially available liquid chromatography system to perform c-IEC for charge variant analysis of mAbs with nanogram sensitivity. We demonstrate the method for multiple monoclonal antibodies, including antibody fragments, on different columns from different manufacturers. Relative standard deviations of <10% were achieved for relative peak areas of main peak, acidic and basic regions, which are common regions of interest for quantifying monoclonal antibody charge variants using IEC. The results herein demonstrate the excellent sensitivity of this c-IEC characterization method, which can be used for analyzing charge variants in sample-limited applications, such as early-stage candidate screening and in vivo studies. PMID:26596872

  12. A New Void Fraction Measurement Method for Gas-Liquid Two-Phase Flow in Small Channels.

    PubMed

    Li, Huajun; Ji, Haifeng; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing; Wu, Guohua

    2016-01-01

    Based on a laser diode, a 12 6 photodiode array sensor, and machine learning techniques, a new void fraction measurement method for gas-liquid two-phase flow in small channels is proposed. To overcome the influence of flow pattern on the void fraction measurement, the flow pattern of the two-phase flow is firstly identified by Fisher Discriminant Analysis (FDA). Then, according to the identification result, a relevant void fraction measurement model which is developed by Support Vector Machine (SVM) is selected to implement the void fraction measurement. A void fraction measurement system for the two-phase flow is developed and experiments are carried out in four different small channels. Four typical flow patterns (including bubble flow, slug flow, stratified flow and annular flow) are investigated. The experimental results show that the development of the measurement system is successful. The proposed void fraction measurement method is effective and the void fraction measurement accuracy is satisfactory. Compared with the conventional laser measurement systems using standard laser sources, the developed measurement system has the advantages of low cost and simple structure. Compared with the conventional void fraction measurement methods, the proposed method overcomes the influence of flow pattern on the void fraction measurement. This work also provides a good example of using low-cost laser diode as a competent replacement of the expensive standard laser source and hence implementing the parameter measurement of gas-liquid two-phase flow. The research results can be a useful reference for other researchers' works. PMID:26828488

  13. A New Void Fraction Measurement Method for Gas-Liquid Two-Phase Flow in Small Channels

    PubMed Central

    Li, Huajun; Ji, Haifeng; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing; Wu, Guohua

    2016-01-01

    Based on a laser diode, a 12 × 6 photodiode array sensor, and machine learning techniques, a new void fraction measurement method for gas-liquid two-phase flow in small channels is proposed. To overcome the influence of flow pattern on the void fraction measurement, the flow pattern of the two-phase flow is firstly identified by Fisher Discriminant Analysis (FDA). Then, according to the identification result, a relevant void fraction measurement model which is developed by Support Vector Machine (SVM) is selected to implement the void fraction measurement. A void fraction measurement system for the two-phase flow is developed and experiments are carried out in four different small channels. Four typical flow patterns (including bubble flow, slug flow, stratified flow and annular flow) are investigated. The experimental results show that the development of the measurement system is successful. The proposed void fraction measurement method is effective and the void fraction measurement accuracy is satisfactory. Compared with the conventional laser measurement systems using standard laser sources, the developed measurement system has the advantages of low cost and simple structure. Compared with the conventional void fraction measurement methods, the proposed method overcomes the influence of flow pattern on the void fraction measurement. This work also provides a good example of using low-cost laser diode as a competent replacement of the expensive standard laser source and hence implementing the parameter measurement of gas-liquid two-phase flow. The research results can be a useful reference for other researchers’ works. PMID:26828488

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

    NASA Astrophysics Data System (ADS)

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

    1998-05-01

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

  15. Saffron authentication based on liquid chromatography high resolution tandem mass spectrometry and multivariate data analysis.

    PubMed

    Rubert, Josep; Lacina, Ondrej; Zachariasova, Milena; Hajslova, Jana

    2016-08-01

    Saffron is one of the oldest and most expensive spices, which is often target of fraudulent activities. In this research, a new strategy of saffron authentication based on metabolic fingerprinting was developed. In the first phase, a solid liquid extraction procedure was optimized, the main aim was to isolate as maximal representation of small molecules contained in saffron as possible. In the second step, a detection method based on liquid chromatography coupled with high-resolution mass spectrometry was developed. Initially, principal component analysis (PCA) revealed clear differences between saffron cultivated and packaged in Spain, protected designation of origin (PDO), and saffron packaged in Spain of unknown origin, labeled Spanish saffron. Afterwards, orthogonal partial least square discriminant analysis (OPLS-DA) was favorably used to discriminate between Spanish saffron. The tentative identification of markers showed glycerophospholipids and their oxidized lipids were significant markers according to their origin. PMID:26988494

  16. Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

    PubMed Central

    Preti, Raffaella

    2016-01-01

    The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis. PMID:27143972

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

    PubMed

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

    2015-05-01

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

  18. Analysis of 5-hydroxymethylfurfural in foods by gas chromatography-mass spectrometry.

    PubMed

    Teixidó, E; Santos, F J; Puignou, L; Galceran, M T

    2006-11-24

    A new, simple and selective method for the analysis of 5-hydroxymethylfurfural (HMF) in foods by gas chromatography coupled to mass spectrometry (GC-MS) is proposed. Several derivatising procedures based on the formation of an HMF silylated derivative using different reagents were studied. Among the derivatising reagents examined, N,O-bis-trimethylsilyltrifluoroacetamide (BSTFA) provided the best derivatisation yield. Sample clean-up was also optimised, using either liquid-liquid extraction with dichloromethane or solid-phase extraction (SPE) with several commercially available cartridges, and the best results were obtained using ENV+ cartridges. Quality parameters such as day-to-day and run-to-run precision (RSD<10%), linearity (between 25 and 700 ng g(-1)) and detection limit (6 ng g(-1)) were established. This method was successfully applied to the analysis of HMF content in several Spanish food samples from a local market, such as jam, honey, orange juice and bakery products. PMID:17010355

  19. Size-Exclusion Chromatography for the Analysis of Protein Biotherapeutics and their Aggregates

    PubMed Central

    Hong, Paula; Koza, Stephan; Bouvier, Edouard S. P.

    2012-01-01

    In recent years, the use and number of biotherapeutics has increased significantly. For these largely protein-based therapies, the quantitation of aggregates is of particular concern given their potential effect on efficacy and immunogenicity. This need has renewed interest in size-exclusion chromatography (SEC). In the following review we will outline the history and background of SEC for the analysis of proteins. We will also discuss the instrumentation for these analyses, including the use of different types of detectors. Method development for protein analysis by SEC will also be outlined, including the effect of mobile phase and column parameters (column length, pore size). We will also review some of the applications of this mode of separation that are of particular importance to protein biopharmaceutical development and highlight some considerations in their implementation. PMID:23378719

  20. Disaccharide Analysis of Glycosaminoglycans Using Hydrophilic Interaction Chromatography and Mass Spectrometry

    PubMed Central

    Gill, Vanessa Leah; Aich, Udayanath; Rao, Srinivasa; Pohl, Chris; Zaia, Joseph

    2013-01-01

    Heparan sulfate (HS) and chondroitin sulfate/dermatan sulfate (CS/DS) glycosaminoglycans (GAGs) participate in many important biological processes. Quantitative disaccharide analysis of HS and CS/DS is essential for the characterization of GAGs and enables modeling of the GAG domain structure. Methods involving enzymatic digestion and chemical depolymerization have been developed to determine the type and location of sulfation/acetylation modifications as well as uronic acid epimerization. Enzymatic digestion generates disaccharides with Δ-4,5-unsaturation at the non-reducing end. Chemical depolymerization with nitrous acid retains the uronic acid epimerization. This work shows the use of hydrophilic interaction liquid chromatography (HILIC)-MS for quantification of both enzyme-derived and nitrous acid depolymerization products for structural analysis of HS and CS/DS. This method enables biomedical researchers to determine complete disaccharide profiles on GAG samples using a single LC-MS platform. PMID:23234263

  1. Characterization of Extracellular Proteins in Tomato Fruit using Lectin Affinity Chromatography and LC-MALDI-MS/MS analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The large-scale isolation and analysis of glycoproteins by lectin affinity chromatography coupled with mass spectrometry has become a powerful tool to monitor changes in the “glycoproteome” of mammalian cells. Thus far, however, this approach has not been used extensively for the analysis of plant g...

  2. The application of the high-performance ion-exchange chromatography for the analysis of bovine milk proteins.

    PubMed

    Bican, P

    1985-07-15

    A high-performance ion-exchange chromatographic (HPIEC) method for the analysis of milk proteins is described. The technique provides an alternative to other separation methods. The resolution obtained for both the proteins of the casein group and bovine lactoserum is comparable with that of electrophoretic analysis on polyacrylamide gels and low-pressure chromatography. PMID:4007137

  3. Study on measures to improve gas-liquid phase mixing in a multiphase pump impeller under high gas void fraction

    NASA Astrophysics Data System (ADS)

    Zhang, J. Y.; Zhu, H. W.; Ding, K.; Qiang, R.

    2012-11-01

    Rotodynamic multiphase pump can transport crude gas-liquid mixture produced from oil well, and is regarded as the good choice of oil-gas multiphase transportation in offshore product system, for its advantages that compact structure, large flow rate, not sensitive to solid particles in the fluid. However, it is prone to bring about gas-liquid separation within the impeller under high gas void fraction. To solve the problem, this paper presents several measures to break gas packet and inhibit gas-liquid separation, such as, depositing the short blades, opening holes at the blades where gas packets gather, using T-shaped blades, etc. Then, CFD software was used to simulate the flow fields which were added measures to inhibit gas-liquid separation. The results show that streamlines in three new impellers distribute more evenly than in original impeller, the gas-liquid two phases mixed degree was improved, and the gas-liquid separation was inhibited to some extent. However, adding the short blades and using T-blade impeller failed to improve the differential pressure of impellers. So the placement and the geometrical parameters of the measures inhibiting gas-liquid separation should be further optimized.

  4. [Fast analysis of indole alkaloids from Evodiae fructus by supercritical fluid chromatography].

    PubMed

    Li, Zhenyu; Fu, Qing; Li, Kuiyong; Liang, Tu; Jin, Yu

    2014-05-01

    A fast chromatographic separation of indole alkaloids from Evodiae fructus was developed by supercritical fluid chromatography (SFC). The initial screening of four stationary phases was investigated with a standard mixture of evodiamine and rutaecarpine, and a complex sample of indole alkaloids prepared from Evodiae fructus as probes. Later, the effects of chromatographic parameters on separation were studied including injection volume, organic modifier, additive, temperature and back pressure. The injection volume had significant impact on the peak shape. With the additives in the mobile phase, slight changes in peak shape and retention time were observed in separation. Variation in organic modifier led to dramatic change in chromatographic behavior. Both decreased temperature and increased back pressure shortened the retention time. Finally, a fast analytical method using SFC, on a Waters ACQUITY UPC2 BEH column, methanol as modifier, under 35 degrees C and 2.07 x 10(7) Pa, was developed to separate a complex sample of indole alkaloids in less than 15 min. Another rapid approach for the separation of a complex sample of indole alkaloids was developed by using ultra-high performance liquid chromatography (UHPLC). As a result, SFC can be used in the separation of natural products, giving high performance, good resolution and fast analysis speed. The difference in selectivity with UHPLC can be used to the development of natural product separation. PMID:25185311

  5. Analysis of starch in food systems by high-performance size exclusion chromatography.

    PubMed

    Ovando-Martnez, Maribel; Whitney, Kristin; Simsek, Senay

    2013-02-01

    Starch has unique physicochemical characteristics among food carbohydrates. Starch contributes to the physicochemical attributes of food products made from roots, legumes, cereals, and fruits. It occurs naturally as distinct particles, called granules. Most starch granules are a mixture of 2 sugar polymers: a highly branched polysaccharide named amylopectin and a basically linear polysaccharide named amylose. The starch contained in food products undergoes changes during processing, which causes changes in the starch molecular weight and amylose to amylopectin ratio. The objective of this study was to develop a new, simple, 1-step, and accurate method for simultaneous determination of amylose and amylopectin ratio as well as weight-averaged molecular weights of starch in food products. Starch from bread flour, canned peas, corn flake cereal, snack crackers, canned kidney beans, pasta, potato chips, and white bread was extracted by dissolving in KOH, urea, and precipitation with ethanol. Starch samples were solubilized and analyzed on a high-performance size exclusion chromatography (HPSEC) system. To verify the identity of the peaks, fractions were collected and soluble starch and beta-glucan assays were performed additional to gas chromatography analysis. We found that all the fractions contain only glucose and soluble starch assay is correlated to the HPSEC fractionation. This new method can be used to determine amylose amylopectin ratio and weight-averaged molecular weight of starch from various food products using as low as 25 mg dry samples. PMID:23330715

  6. Analysis of pendimethalin residues in fruit, nuts, vegetables, grass, and mint by gas chromatography.

    PubMed

    Engebretson, J; Hall, G; Hengel, M; Shibamoto, T

    2001-05-01

    Pendimethalin [N-(1-ethylpropyl)-3,4-dimethyl-2,6-dinitrobenzenamine], in the formulation of Prowl (a commercial herbicide), was applied to various crops. Analysis of pendimethalin and its metabolite [4(1-ethylpropyl)amino-2-methyl-3,5-dinitrobenzyl alcohol] was accomplished by utilizing liquid-liquid partitioning, gel permeation chromatography (GPC) for nuts and mint, solid-phase extraction (SPE) cleanup, and gas chromatography (GC) with a nitrogen--phosphorus detector (NPD). Method validation recoveries for fruits, nuts, vegetables, grass, and mint are given for both compounds. Pendimethalin average recoveries ranged from 71% to 126% over two levels of fortification. Pendimethalin metabolite average recoveries ranged from 69% to 123% over two levels of fortification. The quantitation limit for all crops except mint was 0.050 ppm. The quantitation limit for mint and mint oil was 0.10 ppm. Residues greater than the limit of quantitation were found for pendimethalin in apple pomace, fresh and dry fig, grass screenings, mint oil, almond hulls, green onion, and tomato pomace (wet and dry). Residues greater than the limit of quantitation were found for pendimethalin metabolite in grass screenings, grass straw, and almond hulls. All other crop analyses for pendimethalin and its metabolite were below the limit of quantitation. PMID:11368577

  7. Online coupling of hydrophilic interaction/strong cation exchange/reversed-phase liquid chromatography with porous graphitic carbon liquid chromatography for simultaneous proteomics and N-glycomics analysis.

    PubMed

    Zhao, Yun; Law, Henry C H; Zhang, Zaijun; Lam, Herman C; Quan, Quan; Li, Guohui; Chu, Ivan K

    2015-10-01

    In this study we developed a fully automated three-dimensional (3D) liquid chromatography methodology-comprising hydrophilic interaction separation as the first dimension, strong cation exchange fractionation as the second dimension, and low-pH reversed-phase (RP) separation as the third dimension-in conjunction downstream with additional complementary porous graphitic carbon separation, to capture non-retained hydrophilic analytes, for both shotgun proteomics and N-glycomics analyses. The performance of the 3D system alone was benchmarked through the analysis of the total lysate of Saccharomyces cerevisiae, leading to improved hydrophilic peptide coverage, from which we identified 19% and 24% more proteins and peptides, respectively, relative to those identified from a two-dimensional hydrophilic interaction liquid chromatography and low-pH RP chromatography (HILIC-RP) system over the same mass spectrometric acquisition time; consequently, the 3D platform also provided enhanced proteome and protein coverage. When we applied the integrated technology to analyses of the total lysate of primary cerebellar granule neurons, we characterized a total of 2201 proteins and 16,937 unique peptides for this primary cell line, providing one of its most comprehensive datasets. Our new integrated technology also exhibited excellent performance in the first N-glycomics analysis of cynomolgus monkey plasma; we successfully identified 122 proposed N-glycans and 135 N-glycosylation sites from 122 N-glycoproteins, and confirmed the presence of 38 N-glycolylneuraminic acid-containing N-glycans, a rare occurrence in human plasma, through tandem mass spectrometry for the first time. PMID:26362810

  8. Advances in liquid chromatography-high-resolution mass spectrometry for quantitative and qualitative environmental analysis.

    PubMed

    Aceña, Jaume; Stampachiacchiere, Serena; Pérez, Sandra; Barceló, Damià

    2015-08-01

    This review summarizes the advances in environmental analysis by liquid chromatography-high-resolution mass spectrometry (LC-HRMS) during the last decade and discusses different aspects of their application. LC-HRMS has become a powerful tool for simultaneous quantitative and qualitative analysis of organic pollutants, enabling their quantitation and the search for metabolites and transformation products or the detection of unknown compounds. LC-HRMS provides more information than low-resolution (LR) MS for each sample because it can accurately determine the mass of the molecular ion and its fragment ions if it can be used for MS-MS. Another advantage is that the data can be processed using either target analysis, suspect screening, retrospective analysis, or non-target screening. With the growing popularity and acceptance of HRMS analysis, current guidelines for compound confirmation need to be revised for quantitative and qualitative purposes. Furthermore, new commercial software and user-built libraries are required to mine data in an efficient and comprehensive way. The scope of this critical review is not to provide a comprehensive overview of the many studies performed with LC-HRMS in the field of environmental analysis, but to reveal its advantages and limitations using different workflows. PMID:26138893

  9. A study on measurement of gas-liquid interfacial area in a dispersed gas injection system

    NASA Astrophysics Data System (ADS)

    Park, H. K.; Yoon, J. K.

    1990-08-01

    The gas-liquid interfacial area in a dispersed gas injection system was estimated by a chemical method and measured directly by an electroresistivity probe method. In the chemical method, the gas-liquid interfacial area was obtained by plotting CO2 absorption rate in 0.1 mol/L KOH solution based on the gas absorption theory. In the electroresistivity probe method, local gas holdup, bubble rising velocity, and local bubble diameter were measured in the same solution into which air was injected upwardly. Overall mean values of gas holdup and bubble diameter in the vessel were obtained by means of statistical treatments. The specific interfacial area was calculated from these data. Measurements were done in a cylindrical water vessel under different conditions of gas flow rate and nozzle diameter. The measured values of the specific interfacial area by the electroresistivity probe method were compared with those by the chemical method and showed good agreement.

  10. 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.

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

    PubMed

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

    2015-08-01

    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

  12. Hollow fiber gas-liquid membrane contactors for acid gas capture: a review.

    PubMed

    Mansourizadeh, A; Ismail, A F

    2009-11-15

    Membrane contactors using microporous membranes for acid gas removal have been extensively reviewed and discussed. The microporous membrane acts as a fixed interface between the gas and the liquid phase without dispersing one phase into another that offers a flexible modular and energy efficient device. The gas absorption process can offer a high selectivity and a high driving force for transport even at low concentrations. Using hollow fiber gas-liquid membrane contactors is a promising alternative to conventional gas absorption systems for acid gas capture from gas streams. Important aspects of membrane contactor as an efficient energy devise for acid gas removal including liquid absorbents, membrane characteristics, combination of membrane and absorbent, mass transfer, membrane modules, model development, advantages and disadvantages were critically discussed. In addition, current status and future potential in research and development of gas-liquid membrane contactors for acid gas removal were also briefly discussed. PMID:19616376

  13. 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.

  14. The effect of surfactant on stratified and stratifying gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Heiles, Baptiste; Zadrazil, Ivan; Matar, Omar

    2013-11-01

    We consider the dynamics of a stratified/stratifying gas-liquid flow in horizontal tubes. This flow regime is characterised by the thin liquid films that drain under gravity along the pipe interior, forming a pool at the bottom of the tube, and the formation of large-amplitude waves at the gas-liquid interface. This regime is also accompanied by the detachment of droplets from the interface and their entrainment into the gas phase. We carry out an experimental study involving axial- and radial-view photography of the flow, in the presence and absence of surfactant. We show that the effect of surfactant is to reduce significantly the average diameter of the entrained droplets, through a tip-streaming mechanism. We also highlight the influence of surfactant on the characteristics of the interfacial waves, and the pressure gradient that drives the flow. EPSRC Programme Grant EP/K003976/1.

  15. 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

  16. Rapid and sensitive PCR-dipstick DNA chromatography for multiplex analysis of the oral microbiota.

    PubMed

    Tian, Lingyang; Sato, Takuichi; 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

  17. Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    SciTech Connect

    Owens, J; Hok, S; Alcaraz, A; Koester, C

    2008-11-13

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  18. Analysis and assessment of four commercial products of Asian ginseng by ultra-performance liquid chromatography and chemometric analysis.

    PubMed

    Zhang, Cuiying; Chen, Shilin; Dong, Liang

    2015-05-01

    Ginseng Radix et Rhizoma (GRR, also named as white ginseng), Ginseng Radix et Rhizoma Rubra (GRR Rubra. also named as red ginseng), Ginseng Folium (GF) and Ginseng Rootlet (GR) products from Asian ginseng, one of the well-known Chinese traditional medicine for thousands of years, are now widely used around the world. Thus the comprehensive quality control is of paramount concern basing on the contents of the bioactive ginsenosides. A rapid, sensitive and reliable method of ultra-performance liquid chromatography coupled with a photodiode array detection (UPLC-PAD) was developed for the quantitative analysis of the 12 ginsenosides in the four commercial ginseng products of Asian ginseng. The chromatography was performed on an ACQUITY UPLC™ BEH C18 column using a gradient elution with acetonitrile/water as the mobile phases. Method validation including calibration curves, accuracies, precisions, repeatabilities and recoveries was investigated. The contents of the 12 ginsenosides were determined in 20 GRR, 4 GF, 4 GR and 11 GRR Rubra samples. To evaluate the sample quality. chenometric methods including hierarchical cluster analysis (HCA) and principal components analysis (PCA) were engaged in evaluating the GRR, GRR Rubra, GF and GR products from Asian ginseng. The results showed that HCA and PCA can be considered as the attractive chemometric techniques in situations where high sample throughput and multiple analytes are required. PMID:26387210

  19. 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.

  20. Impact of Gas-liquid Two-phase Flow on Fluid Borne Noise

    NASA Astrophysics Data System (ADS)

    Taniwaki, Mitsuhiro; Shimomura, Nobuo

    In pipe lines such as those found in refrigeration cycle, a gas-liquid two-phase flow may occur because of a pressure change in the pipe. This flow causes noise. A vapor phase ratio in a fluid and the behavior of bubbles are related to the outbreak of noise. This experimental study investigated the fluid borne noise caused by gas-liquid two-phase flow passing through a contracted section in horizontal pipe. In the experiment, sound pressure was measured for two purposes: to see the influence of the air-water ratio on sound pressure and to see the change in sound pressure when a single bubble passed through a contracted section in horizontal pipe. The experiment showed that the fluid borne noise of gas-liquid two-phase flow grew louder than that of a liquid single-phase flow. As for the frequency distribution of the fluid borne noise, the sound pressure level was higher in the high frequency band. Furthermore, the fluid borne noise grew louder with increasing bubble diameter.

  1. 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.

  2. Ultrasound in gas-liquid systems: effects on solubility and mass transfer.

    PubMed

    Laugier, F; Andriantsiferana, C; Wilhelm, A M; Delmas, H

    2008-09-01

    The effect of ultrasound on the pseudo-solubility of nitrogen in water and on gas-liquid mass transfer kinetics has been investigated in an autoclave reactor equipped with a gas induced impeller. In order to use organic liquids and to investigate the effect of pressure, gas-liquid mass transfer coefficient was calculated from the evolution of autoclave pressure during gas absorption to avoid any side-effects of ultrasound on the concentrations measurements. Ultrasound effect on the apparent solubility is very low (below 12%). Conversely ultrasound greatly improves gas-liquid mass transfer, especially below gas induction speed, this improvement being boosted by pressure. In typical conditions of organic synthesis: 323 K, 1100 rpm, 10 bar, k(L).a is multiplied by 11 with ultrasound (20 kHz/62.6 W). The impact of sonication is much higher on gassing out than on gassing in. In the same conditions, this enhancement is at least five times higher for degassing. PMID:18468473

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

    SciTech Connect

    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.

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

    SciTech Connect

    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.

  5. Annual report of the origin of natural gas liquids production form EIA-64A

    SciTech Connect

    1995-12-31

    The collection of basic, verifiable information on the Nation`s reserves and production of natural gas liquids (NGL) is mandated by the Federal Energy Administration Act of 1974 (FEAA) (Public Law 93-275) and the Department of Energy Organization Act of 1977 (Public Law 95-91). Gas shrinkage volumes reported on Form EIA-64A by natural gas processing plant operators are used with natural gas data collected on a {open_quotes}wet after lease separation{close_quotes} basis on Form EIA-23, Annual Survey of Domestic Oil and Gas Reserves, to estimate {open_quotes}dry{close_quotes} natural gas reserves and production volumes regionally and nationally. The shrinkage data are also used, along with the plant liquids production data reported on Form EIA-64A, and lease condensate data reported on Form EIA-23, to estimate regional and national gas liquids reserves and production volumes. This information is the only comprehensive source of credible natural gas liquids data, and is required by DOE to assist in the formulation of national energy policies.

  6. High Throughput Quantitative Analysis of Serum Proteins Using Glycopeptide Capture and Liquid Chromatography Mass Spectrometry

    SciTech Connect

    Zhang, Hui; Yi, Eugene C.; Li, Xiao-jun; Mallick, Parag; Kelly-Spratt, Karen S.; Masselon, Christophe D.; Camp, David G.; Smith, Richard D.; Kemp, Christopher J.; Aebersold, Reudi

    2005-02-01

    It is expected that the composition of the serum proteome can provide valuable information about the state of the human body in health and disease and that this information can be extracted via quantitative proteomic measurements. Suitable proteomic techniques need to be sensitive, reproducible, and robust to detect potential biomarkers below the level of highly expressed proteins, generate data sets that are comparable between experiments and laboratories, and have high throughput to support statistical studies. Here we report a method for high throughput quantitative analysis of serum proteins. It consists of the selective isolation of peptides that are N-linked glycosylated in the intact protein, the analysis of these now deglycosylated peptides by liquid chromatography electrospray ionization mass spectrometry, and the comparative analysis of the resulting patterns. By focusing selectively on a few formerly N-linked glycopeptides per serum protein, the complexity of the analyte sample is significantly reduced and the sensitivity and throughput of serum proteome analysis are increased compared with the analysis of total tryptic peptides from unfractionated samples. We provide data that document the performance of the method and show that sera from untreated normal mice and genetically identical mice with carcinogen-induced skin cancer can be unambiguously discriminated using unsupervised clustering of the resulting peptide patterns. We further identify, by tandem mass spectrometry, some of the peptides that were consistently elevated in cancer mice compared with their control littermates.

  7. Ultra-performance liquid chromatography-tandem mass spectrometry: a novel challenge in multiresidue pesticide analysis in food.

    PubMed

    Kovalczuk, Tomás; Jech, Martin; Poustka, Jan; Hajslová, Jana

    2006-09-01

    Potential of ultra-performance liquid chromatography (UPLC) separation strategy coupled with tandem (in space) mass spectrometric detection (MS/MS) in multiresidue pesticide analysis was critically assessed. Performance parameters such as number of theoretical plates, height of theoretical plate, peak symmetry and peak capacity were measured/calculated on the basis of data generated by analysis of apple extracts containing 17 (semi)polar pesticides representing various classes of active ingredients of widely used crop protective preparations. Ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) procedure provided improved chromatographic parameters resulting in significantly increased sample throughput including lower solvent consumption and lower limits of quantitation (LOQs) for most of target analytes compared to common method employing conventional high-performance liquid chromatography (HPLC) separation. PMID:17723647

  8. Multivariate approach for the enantioselective analysis in micellar electrokinetic chromatography-mass spectrometry

    PubMed Central

    He, Jun; Shamsi, Shahab A.

    2009-01-01

    A mixture of two molecular micelles polysodium N-undecenoxy carbonyl-l-leucinate, (poly-l-SUCL) and polysodium N-undecanoyl leucylvalinate, (poly-l-SULV) was utilized in micellar electrokinetic chromatography-electrospray ionization-mass spectrometry (MEKC-ESI-MS) to simultaneously separate and detect enantiomers of binaphthyl derivatives. Separation parameters such as background buffer composition, voltage, temperature, and nebulizer pressure were optimized using a multivariate central composite design (CCD).Baseline enantioseparation for both analytes was achieved. The CCD was also used in the optimization of sheath liquid and spray chamber parameters to achieve optimum ESI-MS response. The results demonstrate that CCD is a powerful tool for the optimization of MEKC-MS parameters and the response surface model analysis can provide in-depth statistical understandings of the significant factors required to achieve maximum enantioresolution and ESI-MS sensitivity. PMID:19110258

  9. Integrating Paper Chromatography with Electrochemical Detection for the Trace Analysis of TNT in Soil.

    PubMed

    Ryan, Patrick; Zabetakis, Daniel; Stenger, David A; Trammell, Scott A

    2015-01-01

    We report on the development of an electrochemical probe for the trace analysis of 2,4,6-trinitrotoluene (TNT) in soil samples. The probe is a combination of graphite electrodes, filter paper, with ethylene glycol and choline chloride as the solvent/electrolyte. Square wave chromatovoltammograms show the probes have a sensitivity for TNT of 0.75 nA/ng and a limit of detection of 100 ng. In addition, by taking advantage of the inherent paper chromatography step, TNT can be separated in both time and cathodic peak potential from 4-amino-dinitrotolene co-spotted on the probe or in soil samples with the presence of methyl parathion as a possible interferent. PMID:26184223

  10. Analysis of radioactive waste samples by ion chromatography-ICP/MS

    SciTech Connect

    Farmer, O.T. III; Reeves, J.H.; Wyse, E.J.; Clemeston, C.J.; Barinaga, C.J.; Smith, M.R.; Koppenaal, D.W.

    1994-10-01

    A comprehensive ion chromatography (IC) with beta-counting (beta) and inductively coupled plasma mass spectrometry (ICP/MS) detection approach has been developed to separate and detect 20 radionuclides in a Hanford waste tank sample. The IC separation was performed using a multi-functional group (anion/cation) resin and eluents of oxalic acid, diglycolic acid, and hydrochloric acid. Shorter-lived radionuclides were detected by a solid-state beta scintillation counter on-line with the IC separation. Mass spectrometry detection using an efficient and robust plasma ionization source provides isotopic discernability for both stable isotopes and long-lived radioactive species. Effective separation of over 47 elements and 160 isotopes was obtained from a single-elution scheme lasting 70 min. Automated IC separations provide the potential for rapid isotopic and radionuclide analysis of complex radioactive waste, using minimal sample and reagent volumes and reducing personnel exposures.

  11. Integrating Paper Chromatography with Electrochemical Detection for the Trace Analysis of TNT in Soil

    PubMed Central

    Ryan, Patrick; Zabetakis, Daniel; Stenger, David A.; Trammell, Scott A.

    2015-01-01

    We report on the development of an electrochemical probe for the trace analysis of 2,4,6-trinitrotoluene (TNT) in soil samples. The probe is a combination of graphite electrodes, filter paper, with ethylene glycol and choline chloride as the solvent/electrolyte. Square wave chromatovoltammograms show the probes have a sensitivity for TNT of 0.75 nA/ng and a limit of detection of 100 ng. In addition, by taking advantage of the inherent paper chromatography step, TNT can be separated in both time and cathodic peak potential from 4-amino-dinitrotolene co-spotted on the probe or in soil samples with the presence of methyl parathion as a possible interferent. PMID:26184223

  12. Forensic analysis of ignitable liquids in fire debris by comprehensive two-dimensional gas chromatography.

    PubMed

    Frysinger, Glenn S; Gaines, Richard B

    2002-05-01

    The application of comprehensive two-dimensional gas chromatography (GC x GC) for the forensic analysis of ignitable liquids in fire debris is reported. GC x GC is a high resolution, multidimensional gas chromatographic method in which each component of a complex mixture is subjected to two independent chromatographic separations. The high resolving power of GC x GC can separate hundreds of chemical components from a complex fire debris extract. The GC x GC chromatogram is a multicolor plot of two-dimensional retention time and detector signal intensity that is well suited for rapid identification and fingerprinting of ignitable liquids. GC x GC chromatograms were used to identify and classify ignitable liquids, detect minor differences between similar ignitable liquids, track the chemical changes associated with weathering, characterize the chemical composition of fire debris pyrolysates, and detect weathered ignitable liquids against a background of fire debris pyrolysates. PMID:12051325

  13. Analysis of betamethasone, dexamethasone and related compounds by liquid chromatography/electrospray mass spectrometry.

    PubMed

    Arthur, Kathryn E; Wolff, Jean-Claude; Carrier, Dan J

    2004-01-01

    A reversed-phase high-performance liquid chromatography/electrospray ionisation mass spectrometry (HPLC/ESI-MS) method has been developed to conclusively differentiate the epimers betamethasone and dexamethasone and various esterification products (betamethasone and dexamethasone 21-acetate, betamethasone and dexamethasone 21-phosphate, betamethasone 17-valerate, betamethasone 21-valerate and betamethasone 17,21-dipropionate) in counterfeit drugs. Good separation with baseline resolution of all epimers or isomers was obtained on a Zorbax Eclipse XDB or Luna C8 column, using a step gradient with mobile phases of 0.05 M ammonium acetate and acetonitrile. Betamethasones can also be distinguished by the relative abundance of their m/z 279 ion in the positive electrospray tandem mass spectra. The LC/MS or LC/MS/MS method developed was successfully applied to the analysis of drug product samples, i.e. creams and tablets. PMID:15052579

  14. One-step cleanup for PAH residue analysis in plant matrices using size-exclusion chromatography.

    TOXLINE Toxicology Bibliographic Information

    Hubert A; Popp P; Wenzel KD; Engewald W; Schüürmann G

    2003-05-01

    A new one-step cleanup procedure, based on size-exclusion chromatography (SEC), usable for the extracts from accelerated solvent extraction (ASE), Soxhlet extraction, or ultrasonic extraction (USE), is described. The method is suitable for the determination of polycyclic aromatic hydrocarbons (PAHs), especially from very complicated plant matrices (e.g. pine needles, deciduous leaves, mosses). The main improvement compared with previous conventional procedures is that analyte peaks barely overlap with matrix peaks in the chromatograms and that it is a very rapid and simple one-step procedure with clearly improved analytical performance. Essential advantages of this SEC procedure are the sharper GC-MS chromatograms for the PAH fraction at retention times between 9.2 and 12.0 min, distinctly separated substance peaks resulting in better analysis, shorter running times, and lower solvent consumption.

  15. Analysis of the surface energy of pharmaceutical powders by inverse gas chromatography.

    PubMed

    Grimsey, Ian M; Feeley, Jane C; York, Peter

    2002-02-01

    The behavior of pharmaceutical solids, during either processing or use, can be noticeably affected by the surface energetics of the constituent particles. Several techniques exist to measure the surface energy, for example, sessile drop, and dynamic contact angle measurements. Inverse gas chromatography (IGC) is an alternative technique where the powder surface is characterized by the retention behavior of minute quantities of well-characterized vapors that are injected into a column containing the material of interest. Recently published articles using IGC on pharmaceutical powders have ranged from linking surface energetic data with triboelectric charging to studying the effect of surface moisture on surface energetics. Molecular modelling has also recently been used to explore the links between IGC data and the structural and chemical factors that influence surface properties, thereby achieving predictive knowledge regarding powder behavior during processing. In this minireview, the reported applications of IGC in the analysis of pharmaceutical powders are summarized and the major findings highlighted. PMID:11835214

  16. H2S Analysis in Biological Samples Using Gas Chromatography with Sulfur Chemiluminescence Detection

    PubMed Central

    Vitvitsky, Victor; Banerjee, Ruma

    2015-01-01

    Hydrogen sulfide (H2S) is a metabolite and signaling molecule in biological tissues that regulates many physiological processes. Reliable and sensitive methods for H2S analysis are necessary for a better understanding of H2S biology and for the pharmacological modulation of H2S levels in vivo. In this chapter, we describe the use of gas chromatography coupled to sulfur chemiluminescence detection to measure the rates of H2S production and degradation by tissue homogenates at physiologically relevant concentrations of substrates. This method allows separation of H2S from other sulfur compounds and provides sensitivity of detection to ~15 pg (or 0.5 pmol) of H2S per injected sample. PMID:25725519

  17. High-speed, low-pressure gas chromatography-mass spectrometry for essential oil analysis.

    PubMed

    Poynter, Samuel D H; Shellie, Robert A

    2008-07-18

    Analysis of parsley and fennel essential oils was performed by using low-pressure gas chromatography-mass spectrometry (GC-MS). The low-pressure instrument configuration was achieved by fitting a GC-MS instrument with a 530microm I.D. capillary column and an appropriate capillary restrictor at the inlet of the column. Comparison of the performance of the low-pressure GC-MS setup was made with fast GC-MS using a narrow-bore capillary column. By comparing the two approaches side-by-side the benefits of low-pressure GC-MS for characterisation of moderately complex essential oils comprising less than 50 detectable components can be fully appreciated. Although efficiency is sacrificed, the improved sample capacity of the 530microm I.D. column leads to higher peak intensities and in-turn better mass spectral library matching thus providing highly satisfactory results. PMID:18406412

  18. 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

  19. 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…

  20. 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

  1. Anion exchange SPE and liquid chromatography-tandem mass spectrometry in GHB analysis.

    PubMed

    Elian, Albert A; Hackett, Jeffery

    2011-12-01

    In this study, the extraction of γ-hydroxybutyrate (GHB) from urine using solid-phase extraction (SPE) is described. SPE was performed on anion exchange columns after samples of urine had been diluted with de-ionized water. After application of the diluted samples containing GHB-d(6) as an internal standard, the sorbent was washed with deionized water and methanol and dried. The GHB was eluted from the SPE column with a solvent consisting of methanol containing 6% glacial acetic acid. The eluent was collected, evaporated to dryness, and dissolved in mobile phase (100 μL) for analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative multiple reaction monitoring (MRM) mode. Liquid chromatography was performed in gradient mode employing a biphenyl column and a mobile phase consisting of acetontitrile (containing 0.1% formic acid) and 0.1% aqueous formic acid. The total run time for each analysis was less than 5 min. The limits of detection/quantification for this method were determined to be 50 and 100 ng/mL, respectively. The method was found to be linear from 500 ng/mL to 10,000 ng/mL (r(2)>0.995). The recovery of GHB was found to be greater than 75%. In this report, results of authentic urine samples analyzed for GHB by this method are presented. GHB concentrations in these samples were found to be range from less than 500 ng/mL to 5110 ng/mL. PMID:22055831

  2. Analysis of phenolic acids as chloroformate derivatives using solid phase microextraction-gas chromatography.

    PubMed

    Citová, Ivana; Sladkovský, Radek; Solich, Petr

    2006-07-28

    In the presented study, a simple and original procedure of phenolic acids derivatization treated by ethyl and methyl chloroformate performed in an aqueous media consisting of acetonitrile, water, methanol/ethanol and pyridine has been modified and optimized. Seven phenolic acid standards-caffeic, ferulic, gallic, p-coumaric, protocatechuic, syringic and vanillic were derivatized into corresponding methyl/ethyl esters and subsequently determined by the means of gas chromatography connected to the flame-ionisation detector (FID). Some selected validation parameters as linearity, detection and quantitation limits and peak area repeatability were valued. The total time of gas chromatography (GC) analysis was 24 min for methyl chloroformate and 30 min for ethyl chloroformate derivatization. The more suitable methyl chloroformate derivatization was used for further experiments on the possibility of multiple pre-concentration by the direct solid phase microextraction technique (SPME). For this purpose, polyacrylate (PA), polydimethylsiloxane (PDMS), carboxen/polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibres were tested and the extraction conditions concerning time of extraction, temperature and time of desorption were optimized. The most polar PA fibre gave the best results under optimal extraction conditions (50 min extraction time, 25 degrees C extraction temperature and 10 min desorption time). As a result, the total time of SPME-GC analysis was 74 min and an increase in method sensitivity was reached. The limits of quantitation (LOQ) of p-coumaric, ferulic, syringic and vanillic acid esters after SPME pre-concentration were 0.02, 0.17, 0.2 and 0.2 microg mL(-1), respectively, showing approximately 10 times higher sensitivity in comparison with the original GC method. PMID:17723529

  3. Improved separation and analysis of glycolipids by Iatroscan thin-layer chromatography-flame ionization detection.

    PubMed

    Gaparovi?, Blaenka; Kazazi?, Snjeana P; Cvitei?, Ana; Penezi?, Abra; Frka, Sanja

    2015-08-28

    We demonstrate improved power of Iatroscan thin layer chromatography/flame ionization detection (TLC-FID) technique for analysis of complex marine lipid mixture by developing protocol for the separation and analysis of glycolipids including sulfoquinovosyldiacylglycerols (SQDG), monogalactosyldiacylglycerols (MGDG) and digalactosyldiacylglycerols (DGDG). We have modified the common protocol used so far for the analysis of lipid classes by replacing the elution step which uses pure acetone for the elution of acetone mobile polar lipids, with the elution step containing chloroform-acetone (72:28, v:v) for separation of MGDG and DGDG. To separate SQDG from the complex lipid matrix we introduced solvent mixture acetone-chloroform-methanol-formic acid (33:33:33:0.6, v:v:v:v). Quantification of glycolipid classes was performed after calibration with glycolipid standards for the masses between 0.2 and 2.7-5.0?g. With this new protocol we have successfully separated three glycolipids from the complex particulate lipid mixture of the seawater samples. Such an approach extends the power of existing protocol for the analysis of lipids which altogether ensure detection and quantification of 18 lipid classes what was demonstrated on seawater samples. This enables to gain a very broad system overview of the particularly complex environments as are seas, oceans and freshwaters. PMID:26209191

  4. Linear and nonlinear instability in vertical counter-current laminar gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Schmidt, Patrick; Ó Náraigh, Lennon; Lucquiaud, Mathieu; Valluri, Prashant

    2016-04-01

    We consider the genesis and dynamics of interfacial instability in vertical gas-liquid flows, using as a model the two-dimensional channel flow of a thin falling film sheared by counter-current gas. The methodology is linear stability theory (Orr-Sommerfeld analysis) together with direct numerical simulation of the two-phase flow in the case of nonlinear disturbances. We investigate the influence of two main flow parameters on the interfacial dynamics, namely the film thickness and pressure drop applied to drive the gas stream. To make contact with existing studies in the literature, the effect of various density contrasts is also examined. Energy budget analyses based on the Orr-Sommerfeld theory reveal various coexisting unstable modes (interfacial, shear, internal) in the case of high density contrasts, which results in mode coalescence and mode competition, but only one dynamically relevant unstable interfacial mode for low density contrast. A study of absolute and convective instability for low density contrast shows that the system is absolutely unstable for all but two narrow regions of the investigated parameter space. Direct numerical simulations of the same system (low density contrast) show that linear theory holds up remarkably well upon the onset of large-amplitude waves as well as the existence of weakly nonlinear waves. For high density contrasts, corresponding more closely to an air-water-type system, linear stability theory is also successful at determining the most-dominant features in the interfacial wave dynamics at early-to-intermediate times. Nevertheless, the short waves selected by the linear theory undergo secondary instability and the wave train is no longer regular but rather exhibits chaotic motion. The same linear stability theory predicts when the direction of travel of the waves changes — from downwards to upwards. We outline the practical implications of this change in terms of loading and flooding. The change in direction of the wave propagation is represented graphically in terms of a flow map based on the liquid and gas flow rates and the prediction carries over to the nonlinear regime with only a small deviation.

  5. Comparison and analysis of organochlorine pesticides and hexabromobiphenyls in environmental samples by gas chromatography-electron capture detector and gas chromatography-mass spectrometry.

    PubMed

    Liu, Yu; Fu, Xiaofang; Tao, Shu; Liu, Liang; Li, Wei; Meng, Bingjun

    2015-02-01

    Two analytical methods, gas chromatography-electron capture detector (GC-ECD) and gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS), were evaluated and compared for the measurement of persistent organic pollutants, specifically for 26 organochlorine pesticides and two hexabromobiphenyls, in atmospheric particulate matter and soil samples. The hypothesis tested was that the coelution of non-target compounds may lead to false positives when analyzed by GC-ECD, and that the overestimation associated with these false positives can be eliminated using GC-NCI-MS. The study showed that both methods had satisfactory linearity and reproducibility for the target compounds. Although the sensitivities of GC-ECD for most of the compounds investigated were higher than those observed with the GC-NCI-MS method, the matrices interference was obvious with GC-ECD. There was indeed an apparently high false-positive rate or overestimate when GC-ECD was used for environmental samples, implying that the GC-ECD method has been used with care and that GC-NCI-MS is generally superior for the analysis of trace amounts of these compounds in environmental samples. Based on these results, the sample extraction and cleanup procedures of the GC-NCI-MS method were optimized for achieving acceptable recoveries and less matrices interference. PMID:24872522

  6. Extending the range of compounds amenable for gas chromatography-mass spectrometric analysis.

    PubMed

    Fialkov, Alexander B; Gordin, Alexander; Amirav, Aviv

    2003-04-01

    Gas chromatography-mass spectrometry (GC-MS) suffers from a major limitation in that an expanding number of thermally labile or low volatility compounds of interest are not amenable for analysis. We found that the elution temperatures of compounds from GC can be significantly lowered by reducing the column length, increasing the carrier gas flow rate, reducing the capillary column film thickness and lowering the temperature programming rate. Pyrene is eluted at 287 degrees C in standard GC-MS with a 30 m x 0.25 mm I.D. column with 1-microm DB5ms film and 1-ml/min He column flow rate. In contrast, pyrene is eluted at 79 degrees C in our "Supersonic GC-MS" system using a 1 m x 0.25 mm I.D. column with 0.1-microm DB5ms film and 100-ml/min He column flow rate. A simple model has been invoked to explain the significantly (up to 208 degrees C) lower elution temperatures observed. According to this model, every halving of the temperature programming rate, or number of separation plates (either through increased flow rate or due to reduced column length), results in approximately 20 degrees C lower elution temperature. These considerably lower elution temperatures enable the analysis of an extended range of thermally labile and low volatility compounds, that otherwise could not be analyzed by standard GC-MS. We demonstrate the analysis of large polycyclic aromatic hydrocarbons (PAHs) such as decacyclene with ten fused rings, well above the current GC limit of PAHs with six rings. Even a metalloporphirin such as magnesiumoctaethylporphin was easily analyzed with elution temperatures below 300 degrees C. Furthermore, a range of thermally labile compounds were analyzed including carbamates such as methomyl, aldicarb, aldicarbsulfone and oxamyl, explosives such as pentaerythritol tetranitrate, Tetryl and HMX, and drugs such as reserpine (608 a.m.u.). Supersonic GC-MS was used, based on the coupling of a supersonic molecular beam (SMB) inlet and ion sources with a bench-top Agilent 6890 GC plus 5972 MSD. The Supersonic GC-MS provides enhanced molecular ion without any ion source related peak tailing. Thus, the lower GC separation power involved in the analysis of thermally labile and low volatility compounds is compensated by increased separation power of the MS gained from the enhanced molecular ion. Several implications of these findings are discussed, including our conclusion that slower chromatography leads to better analysis of thermally labile compounds. PMID:12741601

  7. DETERMINATION OF VOLATILE ORGANIC COMPOUNDS IN SOILS USING EQUILIBRIUM HEADSPACE ANALYSIS AND CAPILLARY COLUMN GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    Existing methods for determination of volatile organic compounds (VOCs) in soil matrices using the purge and trap technique with gas chromatography/mass spectrometry (GC/MS) have several problems, which include preserving sample integrity from collection to analysis and efficient...

  8. Chemical Speciation Analysis of Sports Drinks by Acid-Base Titrimetry and Ion Chromatography: A Challenging Beverage Formulation Project

    ERIC Educational Resources Information Center

    Drossman, Howard

    2007-01-01

    Students have standardized a sodium hydroxide solution and analyzed commercially available sports drinks by titrimetric analysis of the triprotic citric acid, dihydrogen phosphate, and dihydrogen citrate and by ion chromatography for chloride, total phosphate and citrate. These experiments are interesting examples of analyzing real-world food and…

  9. A Laboratory Experiment in Pharmaceutical Analysis: Determination of Drugs of Abuse in Human Urine by Thin-Layer Chromatography.

    ERIC Educational Resources Information Center

    Bailey, Leonard C.

    1979-01-01

    An experiment is described that was developed for a course in Inorganic and Analytical Pharmaceutical Chemistry at Rutgers University to provide pharmacy students with practical experience in the thin-layer chromatography used for the analysis of urine to monitor patient compliance with drug abuse treatment programs. (JMD)

  10. 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...

  11. 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 ...

  12. 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...

  13. ANALYSIS OF TRACE-LEVEL ORGANIC COMBUSTION PROCESS EMISSIONS USING NOVEL MULTIDIMENSIONAL GAS CHROMATOGRAPHY-MASS SPECTROMETRY PROCEDURES

    EPA Science Inventory

    The paper discusses the analysis of trace-level organic combustion process emissions using novel multidimensional gas chromatography-mass spectrometry (MDGC-MS) procedures. It outlines the application of the technique through the analyses of various incinerator effluent and produ...

  14. ISOTOPE DILUTION ANALYSIS OF BROMATE IN DRINKING WATER MATRIXES BY ION CHROMATOGRAPHY WITH INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRIC DETECTION

    EPA Science Inventory

    Bromate is a disinfection byproduct in drinking water which is formed during the ozonation of source water containing bromide. This paper described the analysis of bromate via ion chromatography-inductively coupled plasma mass spectrometry. The separation of bromate from interfer...

  15. Chemical Speciation Analysis of Sports Drinks by Acid-Base Titrimetry and Ion Chromatography: A Challenging Beverage Formulation Project

    ERIC Educational Resources Information Center

    Drossman, Howard

    2007-01-01

    Students have standardized a sodium hydroxide solution and analyzed commercially available sports drinks by titrimetric analysis of the triprotic citric acid, dihydrogen phosphate, and dihydrogen citrate and by ion chromatography for chloride, total phosphate and citrate. These experiments are interesting examples of analyzing real-world food and

  16. Data analysis tool for comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.

    PubMed

    Castillo, Sandra; Mattila, Ismo; Miettinen, Jarkko; Orešič, Matej; Hyötyläinen, Tuulia

    2011-04-15

    Data processing and identification of unknown compounds in comprehensive two-dimensional gas chromatography combined with time-of-flight mass spectrometry (GC×GC/TOFMS) analysis is a major challenge, particularly when large sample sets are analyzed. Herein, we present a method for efficient treatment of large data sets produced by GC×GC/TOFMS implemented as a freely available open source software package, Guineu. To handle large data sets and to efficiently utilize all the features available in the vendor software (baseline correction, mass spectral deconvolution, peak picking, integration, library search, and signal-to-noise filtering), data preprocessed by instrument software are used as a starting point for further processing. Our software affords alignment of the data, normalization, data filtering, and utilization of retention indexes in the verification of identification as well as a novel tool for automated group-type identification of the compounds. Herein, different features of the software are studied in detail and the performance of the system is verified by the analysis of a large set of standard samples as well as of a large set of authentic biological samples, including the control samples. The quantitative features of our GC×GC/TOFMS methodology are also studied to further demonstrate the method performance and the experimental results confirm the reliability of the developed procedure. The methodology has already been successfully used for the analysis of several thousand samples in the field of metabolomics. PMID:21434611

  17. 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.

  18. Ultra-high performance liquid chromatography tandem mass spectrometry for comprehensive analysis of urinary acylcarnitines.

    PubMed

    Zuniga, Azeret; Li, Liang

    2011-03-01

    We report an enabling mass spectrometric method for the analysis of lipid metabolites in order to define better the lipid metabolome in terms of chemical diversity and generate fragment ion spectra of these metabolites as a potential resource for unknown metabolite identification. This work focuses on the analysis of one important class of lipid metabolites, the acylcarnitines. Current analytical methods have only detected and identified a limited number of these metabolites. The method described herein provides the most comprehensive acylcarnitine profile in urine of healthy individuals up to date. It involves an optimized solid phase extraction technique for selective analyte extraction using cartridges containing both lipophilic and cation-exchange properties. The captured analytes are then subjected to ultra-high performance liquid chromatography (UPLC) separation, followed by tandem mass spectrometry (MS/MS) analysis using information-dependent acquisitions and selected reaction monitoring (SRM). The urine of six healthy individuals was analyzed using this method. A total of 355 acylcarnitines were detected; only 43 of them have been previously reported in the urine of healthy individuals. Detection of this large number of acylcarnitines illustrates the great diversity of the lipid metabolome as well as the usefulness of the method for profiling acylcarnitines. Furthermore, the MS/MS spectra of the 355 acylcarnitines will be uploaded to a public human metabolome database as a mass spectrometric resource for unknown metabolite identification. PMID:21338760

  19. The use of a milli-whistle as a detector in gas analysis by gas chromatography.

    PubMed

    Lin, Cheng-Huang; He, Yi-San; Lin, Chien-Hung; Fan, Gang-Ting; Chen, Hsin-Kai

    2014-01-01

    This mini-review introduces a general understanding of the use of a milli-whistle as a gas chromatography (GC) detector in gas analysis, including our research on the methodology and theory associated with a number of different related applications. The milli-whistle is connected to the outlet of a GC capillary, and when the eluted gases and the GC carrier gas pass through it, a sound with a fundamental frequency is produced. The sound wave can be picked up by a microphone or an accelerometer, and after a fast Fourier transform, the online data obtained for frequency-change vs. retention time constitute a new method for detecting gases. The first part of this review discusses the fundamentals of the milli-whistle. Some modifications are also discussed, including various types of whistles and an attempt to maximize the sensitivity and stability of the method. The second part then focuses on several practical applications, including an analysis of hydrogen released from ammonia borane, inorganic gases produced from fireworks, the CO2/O2 ratio from expired human breath and a purity test for alcohols. These studies show that the GC-whistle method has great potential for use as a fast sampling ionization method, and for the direct analysis of biological and chemical samples at under ambient conditions. PMID:24420261

  20. Toward Sensitive and Accurate Analysis of Antibody Biotherapeutics by Liquid Chromatography Coupled with Mass Spectrometry

    PubMed Central

    An, Bo; Zhang, Ming

    2014-01-01

    Remarkable methodological advances in the past decade have expanded the application of liquid chromatography coupled with mass spectrometry (LC/MS) analysis of biotherapeutics. Currently, LC/MS represents a promising alternative or supplement to the traditional ligand binding assay (LBA) in the pharmacokinetic, pharmacodynamic, and toxicokinetic studies of protein drugs, owing to the rapid and cost-effective method development, high specificity and reproducibility, low sample consumption, the capacity of analyzing multiple targets in one analysis, and the fact that a validated method can be readily adapted across various matrices and species. While promising, technical challenges associated with sensitivity, sample preparation, method development, and quantitative accuracy need to be addressed to enable full utilization of LC/MS. This article introduces the rationale and technical challenges of LC/MS techniques in biotherapeutics analysis and summarizes recently developed strategies to alleviate these challenges. Applications of LC/MS techniques on quantification and characterization of antibody biotherapeutics are also discussed. We speculate that despite the highly attractive features of LC/MS, it will not fully replace traditional assays such as LBA in the foreseeable future; instead, the forthcoming trend is likely the conjunction of biochemical techniques with versatile LC/MS approaches to achieve accurate, sensitive, and unbiased characterization of biotherapeutics in highly complex pharmaceutical/biologic matrices. Such combinations will constitute powerful tools to tackle the challenges posed by the rapidly growing needs for biotherapeutics development. PMID:25185260

  1. Rapid direct analysis to discriminate geographic origin of extra virgin olive oils by flash gas chromatography electronic nose and chemometrics.

    PubMed

    Melucci, Dora; Bendini, Alessandra; Tesini, Federica; Barbieri, Sara; Zappi, Alessandro; Vichi, Stefania; Conte, Lanfranco; Gallina Toschi, Tullia

    2016-08-01

    At present, the geographical origin of extra virgin olive oils can be ensured by documented traceability, although chemical analysis may add information that is useful for possible confirmation. This preliminary study investigated the effectiveness of flash gas chromatography electronic nose and multivariate data analysis to perform rapid screening of commercial extra virgin olive oils characterized by a different geographical origin declared in the label. A comparison with solid phase micro extraction coupled to gas chromatography mass spectrometry was also performed. The new method is suitable to verify the geographic origin of extra virgin olive oils based on principal components analysis and discriminant analysis applied to the volatile profile of the headspace as a fingerprint. The selected variables were suitable in discriminating between "100% Italian" and "non-100% Italian" oils. Partial least squares discriminant analysis also allowed prediction of the degree of membership of unknown samples to the classes examined. PMID:26988501

  2. Rapid liquid chromatography for paralytic shellfish toxin analysis using superficially porous chromatography with AOAC Official Method 2005.06.

    PubMed

    Hatfield, Robert G; Turner, Andrew D

    2012-01-01

    The bioaccumulation of paralytic shellfish toxins in mussels, oysters, cockles, hard clams, razors, and king scallops is monitored in England, Scotland, and Wales by AOAC Official Method 2005.06 LC-with fluorescence detection (FLD). One of the commonly perceived disadvantages of using this method is the long turnaround time and low throughput in a busy laboratory environment. The chromatographic analysis of each sample typically utilizes a 15 min cycle time to achieve toxin oxidation product separation and column equilibration prior to subsequent analysis. A standard RP C18 analytical column, used successfully in recent years, achieves good separation with a long column lifetime. The analysis of a 40 sample qualitative screening batch takes approximately 18 h, including blanks, standards, and other QC samples. The availability of superficially porous column technology has offered the potential to reduce analysis time while retaining column performance on existing hardware. In this study, AOAC Official Method 2005.06 with LC-FLD was transferred to two different commercially available superficially porous columns, and the method performance characteristics were evaluated. Both columns separated all toxins adequately with cycle times less than half that of the existing method. Linearity for each toxin was acceptable up to two times the European maximum permitted limit of 800 microg di-HCl saxitoxin equivalent/kg flesh. LOD and LOQ values were substantially improved for the majority of toxins, with gonyautoxin 1&4 and neosaxitoxin showing up to a two- and fourfold improvement, respectively, depending on the column used. Quantification results obtained from parallel analysis of contaminated samples were acceptable on both columns. Comparative screen results gave a slight increase in the occurrence of contaminated samples, which was attributed to the improved detection limit for most toxins. Issues with rapidly increasing back pressure, however, were identified with both columns, with a limit of around 500 injections. This compares to the >3000 cycles routinely obtained with the standard RP-C18 HPLC columns currently in use. Overall, the gain achieved with these columns through shorter analysis time and improved analytical sensitivity is potentially of benefit in a high-throughput environment. For the routine high-throughput screening of shellfish samples, however, an improved column lifetime is desirable. PMID:22970577

  3. Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Qian, Michael C.

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

  4. 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...

  5. Formation of iron complexs from trifluoroacetic acid based liquid chromatography mobile phases as interference ions in liquid chromatography/electrospray ionization mass spectrometric analysis

    SciTech Connect

    Shukla, Anil K.; Zhang, Rui; Orton, Daniel J.; Zhao, Rui; Clauss, Therese RW; Moore, Ronald J.; Smith, Richard D.

    2011-05-30

    Two unexpected singly charged ions at m/z 1103 and 944 have been observed in mass spectra obtained from electrospray ionization-mass spectrometric analysis of liquid chromatography effluents with mobile phases containing trifluoroacetic acid. Accurate mass measurement and tandem mass spectrometry studies revealed that these two ions are not due to any contamination from solvents and chemicals used for mobile and stationary phases or from the laboratory atmospheric environment. Instead these ions are clusters of trifluoroacetic acid formed in association with acetonitrile, water and iron from the stainless steel union used to connect the column with the electrospray tip and to apply high voltage; the molecular formulae are Fe+((OH)(H2O)2)9(CF3COOH)5 and Fe+((OH)(H2O)2)6 (CF3COOH)5.

  6. Differentiation of betamethasone and dexamethasone using liquid chromatography/positive electrospray tandem mass spectrometry and multivariate statistical analysis.

    PubMed

    Antignac, Jean-Philippe; Le Bizec, Bruno; Monteau, Fabrice; Andre, François

    2002-01-01

    Betamethasone and dexamethasone are two corticosteroids differing in the stereoisomery of their C-16 methyl group. These two compounds are imperfectly separated by reversed-phase liquid chromatography and their mass spectra are very similar, leading to a difficult unambiguous identification according to European criteria. A method is proposed for differentiating betamethasone and dexamethasone using liquid chromatography/tandem mass spectrometry and multivariate statistical analysis. Multiple analysis of variance was used for the justification and the selection of diagnostic ions. Principal component analysis permitted the suitability of the approach to be tested on a large number of samples. Discriminant factorial analysis was finally performed to build a decisional model based on the six most significant ions. This novel utilization of mass spectrometric data appeared efficient for the unambiguous identification of the target analytes in urine samples. PMID:11813313

  7. Analysis of volatile components in Curcuma rhizome by microemulsion electrokinetic chromatography.

    PubMed

    Yang, Feng-Qing; Yang, Jing; Zhang, Xue-Mei; Xu, Pan; Xia, Zhi-Ning

    2013-02-01

    Volatile chemicals are a group of very important compounds in natural products. Curcuma rhizome, which contains many bioactive volatile compounds, is a traditional Chinese medicine that has long been used for the treatment of several diseases. In the present study, a microemulsion electrokinetic chromatography (MEEKC) method was developed for the analysis of four volatile components in Curcuma rhizome, including germacrone, furanodiene, curcumenol and curdione. Experimental parameters, including the pH, type and concentrations of background electrolyte, and microemulsion compositions (type and concentrations of surfactant, co-surfactant and oil phase) were intensively investigated. Finally, the primary compounds in the methanol extract of Curcuma rhizome were separated within 30 min using a running buffer composed of 2.31% w/v (80 mmol/L) sodium dodecyl sulfate (SDS), 0.91% w/v (80 mmol/L) 1-octane, 6.95% w/v (937.5 mmol/L) 1-butanol and 1.88% w/v (312.5 mmol/L) propanol in a 5-mM borate buffer (pH 8.1). The contents of the four investigated compounds were determined in the rhizome from C. phaeocaulis. The results showed that the developed MEEKC method provided an alternative tool for the analysis of volatile components, especially those of heat-sensitive compounds from natural products. PMID:22824329

  8. [Analysis of nine narcotics in urine by microemulsion electrokinetic chromatography-field samplified sample injection].

    PubMed

    Zhang, Yu; Li, Qin; Lu, Minghua; Zhang, Lan; Chen, Guonan; Cai, Zongwei

    2011-08-01

    A simple, sensitive and reproducible method using microemulsion electrokinetic chromatography (MEEKC)-field amplified sample injection (FASI) was developed for the analysis of nine narcotics (morphine, codeine, naloxone, heroin, thebaine, cocaine, pethidine, fentanyl and methadone) in urine. In the MEEKC method, sodium dodecyl sulfate (SDS), 1-butanol and ethyl acetate were used as surfactant, co-surfactant and organic solvent, respectively. The effects of the acidity and concentration of borate buffer, SDS, 1-butanol and ethyl acetate contents were investigated. The optimum concentrations (by mass fraction) of microemulsion system were 0.6% SDS, 1.2% 1-butanol, 0.6% ethyl acetate and 97.6% 10 mmol/L Na2B4O7 buffer (pH 9.5). The applied voltage was 25 kV. FASI was coupled with the MEEKC method to increase the sensitivity. Under the optimum conditions, the nine narcotics were baseline separated within 15 min and the detection limits (S/N = 3) were in the range of 0.3 - 8.0 microg/L. The spiked recoveries in urine samples were between 79.4% and 119.9% with the intraday relative standard deviations (RSDs) less than 5.5%. The developed method has been successfully applied to the analysis of methadone in the samples from in vitro metabolism study. PMID:22128745

  9. Application of microemulsion electrokinetic chromatography to the analysis of a wide range of pharmaceuticals and excipients.

    PubMed

    Altria, K D

    1999-06-01

    Microemulsion electrokinetic chromatography (MEEKC) is a capillary electrophoresis (CE) technique in which solutes partition with moving oil droplets present in a microemulsion buffer. Ionised species will also separate by electrophoresis. In this paper MEEKC is shown to give highly efficient and relatively rapid separations for a wide range of pharmaceuticals, vitamins and excipients. A single set of operating conditions was used to resolve both water-soluble and insoluble compounds. The method was also used to separate both ionic and neutral compounds. The method was especially useful in the analysis of water-insoluble neutral compounds such as steroids and lecithin, which are difficult to analyse by CE. The method was found to be both quantitative and highly repeatable. The quality of the separation was found to be dependent upon the sample diluent used if large injection volumes are employed. The use of MEEKC for the determination of complex mixtures such as multi-ingredient formulations and drug-related impurities was successfully demonstrated. MEEKC offers significant advantages over many forms of CE and capillary electrochromatography (CEC) and should be considered as an extremely useful option in pharmaceutical analysis. PMID:10636701

  10. Ultra Performance Liquid Chromatography and High Resolution Mass Spectrometry for the Analysis of Plant Lipids

    PubMed Central

    Hummel, Jan; Segu, Shruthi; Li, Yan; Irgang, Susann; Jueppner, Jessica; Giavalisco, Patrick

    2011-01-01

    Holistic analysis of lipids is becoming increasingly popular in the life sciences. Recently, several interesting, mass spectrometry-based studies have been conducted, especially in plant biology. However, while great advancements have been made we are still far from detecting all the lipids species in an organism. In this study we developed an ultra performance liquid chromatography-based method using a high resolution, accurate mass, mass spectrometer for the comprehensive profiling of more than 260 polar and non-polar Arabidopsis thaliana leaf lipids. The method is fully compatible to the commonly used lipid extraction protocols and provides a viable alternative to the commonly used direct infusion-based shotgun lipidomics approaches. The whole process is described in detail and compared to alternative lipidomic approaches. Next to the developed method we also introduce an in-house developed database search software (GoBioSpace), which allows one to perform targeted or un-targeted lipidomic and metabolomic analysis on mass spectrometric data of every kind. PMID:22629264

  11. Multiresidue analysis of environmental pollutants in edible vegetable oils by gas chromatography-tandem mass spectrometry.

    PubMed

    Zhou, Rui-Ze; Jiang, Jie; Mao, Ting; Zhao, Ya-Song; Lu, Yong

    2016-09-15

    A novel multiresidue determination of polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PAEs) and alkylphenols (APs) in edible vegetable oils was developed. The samples were extracted with hexane-saturated acetonitrile, and after concentration, the extract was directly qualitatively and quantitatively analyzed by gas chromatography-tandem mass spectrometry (GC-MS/MS) with multiple reaction monitoring (MRM) in positive ion mode. The calibration curve displayed good linearity in the range of 2-100μg/L, with correlation coefficients greater than 0.99. The mean recoveries were 70.0-110.8% by analysis of spiked oil, and the relative standard deviations (RSDs) were 2.1-10.2% (n=6), respectively. The limits of detection (LODs) for the 23 PAHs, 17 PAEs and 3 APs were 0.1-1.0μg/kg, 0.1-4.0μg/kg and 1.2-3.0μg/kg, respectively. The established method effectively avoided interference from large amounts of lipids and pigments. It was applied to real sample and shown to be a rapid and reliable alternative for determination and confirmation in routine analysis. PMID:27080878

  12. 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.

  13. Enantiomeric separation in comprehensive two-dimensional gas chromatography with accurate mass analysis.

    PubMed

    Chin, Sung-Tong; Nolvachai, Yada; Marriott, Philip J

    2014-11-01

    Chiral comprehensive two-dimensional gas chromatography (eGC×GC) coupled to quadrupole-accurate mass time-of-flight mass spectrometry (QTOFMS) was evaluated for its capability to report the chiral composition of several monoterpenes, namely, α-pinene, β-pinene, and limonene in cardamom oil. Enantiomers in a standard mixture were fully resolved by direct enantiomeric-GC analysis with a 2,3-di-O-methyl-6-t-butylsilyl derivatized β-cyclodextrin phase; however, the (+)-(R)-limonene enantiomer in cardamom oil was overlapped with other background components including cymene and cineole. Verification of (+)-(R)-limonene components based on characteristic ions at m/z 136, 121, and 107 acquired by chiral single-dimension GC-QTOFMS in the alternate MS/MSMS mode of operation was unsuccessful due to similar parent/daughter ions generated by interfering or co-eluting cymene and cineole. Column phases SUPELCOWAX, SLB-IL111, HP-88, and SLB-IL59, were incorporated as the second dimension column ((2)D) in chiral GC×GC analysis; the SLB-IL59 offered the best resolution for the tested monoterpene enantiomers from the matrix background. Enantiomeric ratios for α-pinene, β-pinene, and limonene were determined to be 1.325, 2.703, and 1.040, respectively, in the cardamom oil sample based on relative peak area data. PMID:24420979

  14. Analysis of meat samples for anabolic steroids residues by liquid chromatography/tandem mass spectrometry.

    PubMed

    Blasco, Cristina; Van Poucke, Christof; Van Peteghem, Carlos

    2007-06-22

    A rapid, specific and highly sensitive multi-residue method for the determination of anabolic steroid residues in bovine, pork and poultry muscle tissues was developed. The sample preparation involves enzymatic digestion followed by extraction with methanol. The crude extract was cleaned up by solid-phase extraction (SPE) combining C18 and NH2 columns. The detection was carried out by a highly sensitive liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method using both positive and negative ionization modes. Natural and synthetic steroids covering different polarities could be extracted, concentrated and purified using one single method. Mobile phase composition and additives were optimized to achieve the highest sensitivity. The linearity was not good enough for quantitative analysis but the method was well-suited for qualitative confirmation. The method was validated according to the European Commission Decision 2002/657/EC. Decision limits (CCalpha) and detection capabilities (CCbeta) were below 0.5 ng g(-1) for all the compounds in the three types of meat studied. The developed method is suitable for routine analysis in our laboratories. PMID:17459396

  15. Trace analysis of sulfamethazine in animal feed, human urine, and wastewater by electron capture gas chromatography

    SciTech Connect

    Holder, C.L.; Thompson, H.C. Jr.; Bowman, M.C.

    1981-12-01

    Sulfamethazine, a widely used antibacterial drug additive in feeds for swine, chickens, and cattle, was scheduled for toxicological evaluation because of potential human health hazards associated with its residues in edible animal tissues. Analytical chemical procedures that would ensure proper concentration, homogeneity, and stability of the drug in dosed feed and its safe usage during the animal studies were prerequisites for such toxicological tests. Electron capture gas chromatographic (EC/GC) methods were therefore devised for the analysis of sulfamethazine residues in animal feed, human urine, and wastewater at levels as low as 100, 10, and 10 ppb, respectively. Sample extracts were cleaned up by using liquid/liquid partitioning, and the extracts were subjected to two derivatizations followed by cleanup on a silica gel column. The derivatizations of sulfamethazine consisted of methylation followed by trifluoroacetylation of the primary amine function. Ancillary data concerning stability of the compound in animal feed, water, and as a dry residue on glass, extraction efficiencies, partition values with various solvents, and the analysis of residues in feed by high pressure liquid chromatography (HPLC) at levels as low as 1.0 ppm are presented.

  16. 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

  17. Morphological, spectral and chromatography analysis and forensic comparison of PET fibers.

    PubMed

    Farah, Shady; Tsach, Tsadok; Bentolila, Alfonso; Domb, Abraham J

    2014-06-01

    Poly(ethylene terephthalate) (PET) fiber analysis and comparison by spectral and polymer molecular weight determination was investigated. Plain fibers of PET, a common textile fiber and plastic material was chosen for this study. The fibers were analyzed for morphological (SEM and AFM), spectral (IR and NMR), thermal (DSC) and molecular weight (MS and GPC) differences. Molecular analysis of PET fibers by Gel Permeation Chromatography (GPC) allowed the comparison of fibers that could not be otherwise distinguished with high confidence. Plain PET fibers were dissolved in hexafluoroisopropanol (HFIP) and analyzed by GPC using hexafluoroisopropanol:chloroform 2:98 v/v as eluent. 14 PET fiber samples, collected from various commercial producers, were analyzed for polymer molecular weight by GPC. Distinct differences in the molecular weight of the different fiber samples were found which may have potential use in forensic fiber comparison. PET fibers with average molecular weights between about 20,000 and 70,000 g mol(-1) were determined using fiber concentrations in HFIP as low as 1 μg mL(-1). This GPC analytical method can be applied for exclusively distinguish between PET fibers using 1 μg of fiber. This method can be extended to forensic comparison of other synthetic fibers such as polyamides and acrylics. PMID:24725864

  18. 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.

  19. Molecular Ionization-Desorption Analysis Source (MIDAS) for Mass Spectrometry: Thin-Layer Chromatography

    NASA Astrophysics Data System (ADS)

    Winter, Gregory T.; Wilhide, Joshua A.; LaCourse, William R.

    2016-02-01

    Molecular ionization-desorption analysis source (MIDAS), which is a desorption atmospheric pressure chemical ionization (DAPCI) type source, for mass spectrometry has been developed as a multi-functional platform for the direct sampling of surfaces. In this article, its utility for the analysis of thin-layer chromatography (TLC) plates is highlighted. Amino acids, which are difficult to visualize without staining reagents or charring, were detected and identified directly from a TLC plate. To demonstrate the full potential of MIDAS, all active ingredients from an analgesic tablet, separated on a TLC plate, were successfully detected using both positive and negative ion modes. The identity of each of the compounds was confirmed from their mass spectra and compared against standards. Post separation, the chemical signal (blue permanent marker) as reference marks placed at the origin and solvent front were used to calculate retention factor (Rf) values from the resulting ion chromatogram. The quantitative capabilities of the device were exhibited by scanning caffeine spots on a TLC plate of increasing sample amount. A linear curve based on peak are, R2 = 0.994, was generated for seven spots ranging from 50 to 1000 ng of caffeine per spot.

  20. Molecular Ionization-Desorption Analysis Source (MIDAS) for Mass Spectrometry: Thin-Layer Chromatography.

    PubMed

    Winter, Gregory T; Wilhide, Joshua A; LaCourse, William R

    2016-02-01

    Molecular ionization-desorption analysis source (MIDAS), which is a desorption atmospheric pressure chemical ionization (DAPCI) type source, for mass spectrometry has been developed as a multi-functional platform for the direct sampling of surfaces. In this article, its utility for the analysis of thin-layer chromatography (TLC) plates is highlighted. Amino acids, which are difficult to visualize without staining reagents or charring, were detected and identified directly from a TLC plate. To demonstrate the full potential of MIDAS, all active ingredients from an analgesic tablet, separated on a TLC plate, were successfully detected using both positive and negative ion modes. The identity of each of the compounds was confirmed from their mass spectra and compared against standards. Post separation, the chemical signal (blue permanent marker) as reference marks placed at the origin and solvent front were used to calculate retention factor (Rf) values from the resulting ion chromatogram. The quantitative capabilities of the device were exhibited by scanning caffeine spots on a TLC plate of increasing sample amount. A linear curve based on peak are, R2 = 0.994, was generated for seven spots ranging from 50 to 1000 ng of caffeine per spot. PMID:26471042

  1. Hyphenation of optimized microfluidic sample preparation with nano liquid chromatography for faster and greener alkaloid analysis.

    PubMed

    Shen, Yao; van Beek, Teris A; Zuilhof, Han; Chen, Bo

    2013-10-01

    A glass liquid-liquid extraction (LLE) microchip with three parallel 3.5 cm long and 100 μm wide interconnecting channels was optimized in terms of more environmentally friendly (greener) solvents and extraction efficiency. In addition, the optimized chip was successfully hyphenated with nano-liquid chromatography with ultraviolet and mass spectrometric detection (nanoLC-UV-MS) for on-line analysis. In this system, sample pretreatment, separation and detection are integrated, which significantly shortens the analysis time, saves labor and drastically reduces solvent consumption. Strychnine was used as model analyte to determine the extraction efficiency of the optimized 3-phase chip. Influence of organic solvent, pH of feed phase, type of alkaloid, and flow rates were investigated. The results demonstrated that the 3-phase chip nanoLC-UV/MS hyphenation combines rapid (~25 s) and efficient (extraction efficiency >90%) sample prep, with automated alkaloid analyses. The method was applied to real samples including Strychnos nux-vomica seeds, Cephaelis ipecacuanha roots, Atropa belladonna leaves, and Vinca minor leaves. PMID:24050669

  2. Simultaneous analysis of multiple neurotransmitters by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry.

    PubMed

    Tufi, Sara; Lamoree, Marja; de Boer, Jacob; Leonards, Pim

    2015-05-22

    Neurotransmitters are endogenous metabolites that allow the signal transmission across neuronal synapses. Their biological role is crucial for many physiological functions and their levels can be changed by several diseases. Because of their high polarity, hydrophilic interaction liquid chromatography (HILIC) is a promising tool for neurotransmitter analysis. Due to the large number of HILIC stationary phases available, an evaluation of the column performances and retention behaviors has been performed on five different commercial HILIC packing materials (silica, amino, amide and two zwitterionic stationary phases). Several parameters like the linear correlation between retention and the distribution coefficient (logD), the separation factor k and the column resolution Rs have been investigated and the column performances have been visualized with a heat map and hierarchical clustering analysis. An optimized and validated HILIC-MS/MS method based on the ZIC-cHILIC column is proposed for the simultaneous detection and quantification of twenty compounds consisting of neurotransmitters, precursors and metabolites: 3-methoxytyramine (3-MT), 5-hydroxyindoleacetic acid (5-HIAA), 5-hydroxy-L-tripthophan, acetylcholine, choline, L-3,4-dihydroxyphenylalanine (L-DOPA), dopamine, epinephrine, ?-aminobutyric acid (GABA), glutamate, glutamine, histamine, histidine, L-tryptophan, L-tyrosine, norepinephrine, normetanephrine, phenylalanine, serotonin and tyramine. The method was applied to neuronal metabolite profiling of the central nervous system of the freshwater snail Lymnaea stagnalis. This method is suitable to explore neuronal metabolism and its alteration in different biological matrices. PMID:25869798

  3. 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)

  4. 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

  5. Determination of dietary fibre as non-starch polysaccharides with gas-liquid chromatographic, high-performance liquid chromatographic or spectrophotometric measurement of constituent sugars.

    PubMed

    Englyst, H N; Quigley, M E; Hudson, G J

    1994-07-01

    Methods for the measurement of dietary fibre as non-starch polysaccharides (NSP) are described. A common enzymic removal of starch and acid hydrolysis of the NSP to their constituent sugars are followed by one of three alternative techniques, gas-liquid chromatography, high-performance liquid chromatography or spectrophotometry, for measurement of the released sugars. The results obtained by the three methods are in good agreement for a wide range of raw and processed foods. NSP compose approximately 90% of the plant cell-wall material and are therefore a good index of this material. Values for NSP therefore provide a good marker for a diet rich in fruit, vegetables and high-extraction cereal products associated with health and recommended in dietary guidelines. Values for total, soluble and insoluble NSP may be obtained with any of the end-point techniques, and the detailed information obtained from the chromatographic methods is useful in studies of the relationship between the intakes of various types of NSP and health. The causes of some potential interferences in the spectrophotometric assay, especially from processed foods, have been identified and eliminated. The rapid spectrophotometric version is suitable for food labelling purposes and for quality control, and the changes described have made it more robust. PMID:7943740

  6. 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

  7. 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.

  8. Stable isotope labeling - Liquid chromatography/mass spectrometry for quantitative analysis of androgenic and progestagenic steroids.

    PubMed

    Guo, Ning; Liu, Ping; Ding, Jun; Zheng, Shu-Jian; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-01-28

    Steroid hormones play important roles in mammal at very low concentrations and are associated with numerous endocrinology and oncology diseases. Therefore, quantitative analysis of steroid hormones can provide crucial information for uncovering underlying mechanisms of steroid hormones related diseases. In the current study, we developed a sensitive method for the detection of steroid hormones (progesterone, dehydroepiandrosterone, testosterone, pregnenolone, 17-hydroxyprogesterone, androstenedione and 17α-hydroxypregnenolone) in body fluids by stable isotope labeling coupled with liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analysis. In this respect, a pair of isotopes labeling reagents, Girard reagent P (GP) and d5-Girard reagent P (d5-GP), were synthesized and utilized to label steroid hormones in follicular fluid samples and steroid hormone standards, respectively. The heavy labeled standards were used as internal standards for quantification to minimize quantitation deviation in MS analysis due to the matrix and ion suppression effects. The ionization efficiencies of steroid hormones were greatly improved by 4-504 folds through the introduction of a permanent charged moiety of quaternary ammonium from GP. Using the developed method, we successfully quantified steroid hormones in human follicular fluid. We found that the contents of testosterone and androstenedione exhibited significant increase while the content of pregnenolone had significant decrease in follicular fluid of polycystic ovarian syndrome (PCOS) patients compared with healthy controls, indicating that these steroid hormones with significant change may contribute to the pathogenesis of PCOS. Taken together, the developed stable isotope labeling coupled LC-ESI-MS/MS analysis demonstrated to be a promising method for the sensitive and accurate determination of steroid hormones, which may facilitate the in-depth investigation of steroid hormones related diseases. PMID:26755144

  9. Multidimensional chromatography: a powerful tool for the analysis of membrane proteins in mouse brain.

    PubMed

    Lohaus, Christiane; Nolte, Andreas; Blüggel, Martin; Scheer, Christian; Klose, Joachim; Gobom, Johan; Schüler, Andreas; Wiebringhaus, Thomas; Meyer, Helmut E; Marcus, Katrin

    2007-01-01

    Understanding the function of membrane proteins is of fundamental importance due to their crucial roles in many cellular processes and their direct association with human disorders. However, their analysis poses a special challenge, largely due to their highly amphipathic nature. Until recently, analyses of proteomic samples mainly were performed by two-dimensional polyacrylamide gel electrophoresis (2D-PAGE), due to the unprecedented separation power of the technique. However, in conventional 2D-PAGE membrane proteins are generally underrepresented due to their tendency to precipitate during isoelectric focusing and their inefficient transfer from the first to the second dimension. As a consequence, several other separation techniques, primarily based on liquid chromatography (LC), have been employed for analysis of this group of proteins. In the present study, different LC-based methods were compared for the analysis of crude protein extracts. One- and two-dimensional high-performance liquid chromatographic (1D- and 2D-HPLC) separations of brain protein tryptic digests with a predicted concentration range of up to 5 orders of magnitude were found to be insufficient, thus making a preceding fractionation step necessary. An additional protein separation step was introduced and a 3D-PAGE-HPLC analysis was performed. The results of these experiments are compared with results of 2D-PAGE/matrix-assisted laser desorption ionization mass spectrometric (MALDI MS) analyses of the same samples. Features, challenges, advantages, and disadvantages of the respective systems are discussed. The brain (mouse and human) was chosen as the analyzed tissue as it is of high interest in medical and pharmaceutical research into neurological diseases such as multiple sclerosis, stroke, Alzheimer's disease, and Parkinson's disease. The study is part of our ongoing research aimed at identifying new biomarkers for neurodegenerative diseases. PMID:17203954

  10. 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.

  11. The use of aviation gas-liquid heat exchangers employing heat pipes

    NASA Astrophysics Data System (ADS)

    Baranov, Iu. F.; Lokai, N. V.; Khananov, R. I.

    The possibility of using gas-liquid heat-pipe exchangers in different systems of aviation engines is examined, and methods for calculating the characteristics of such heat exchangers are discussed. A program developed for calculating the static and dynamic characteristics of heat-pipe exchangers is described. The program, which consists of 13 modules, uses the finite difference method. The program includes modules for calculating the gravitational characteristics of heat pipes with and without a capillary structure; the vapor parameters are calculated in the one-dimensional formulation for the viscous and inertial components with allowance for compressibility.

  12. Development of Numerical Simulation Method for Compressible Gas-Liquid Two-Phase Flows

    NASA Astrophysics Data System (ADS)

    Tamura, Y.

    2015-12-01

    A numerical simulation method of compressible gas-liquid two-phase flow is developed for analyses of a cavitation bubble. Thermodynamic state of both phases is described with stiffened gas equation of state. Interface of two phases is captured by Level-Set method. As internal energy jump between two phases is critical for the stability of computation, total energy equation is modified so that inviscid flux of energy is smoothly connected across the interface. Detail of governing equations as well as their discretization is described followed by the result of one-dimensional simple example computation.

  13. 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.

  14. Electrical impedance imaging in two-phase, gas-liquid flows: 1. Initial investigation

    NASA Technical Reports Server (NTRS)

    Lin, J. T.; Ovacik, L.; Jones, O. C.

    1991-01-01

    The determination of interfacial area density in two-phase, gas-liquid flows is one of the major elements impeding significant development of predictive tools based on the two-fluid model. Currently, these models require coupling of liquid and vapor at interfaces using constitutive equations which do not exist in any but the most rudimentary form. Work described herein represents the first step towards the development of Electrical Impedance Computed Tomography (EICT) for nonintrusive determination of interfacial structure and evolution in such flows.

  15. 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.

  16. Analysis of endocrine disrupters and related compounds in sediments and sewage sludge using on-line turbulent flow chromatography-liquid chromatography-tandem mass spectrometry.

    PubMed

    Gorga, Marina; Insa, Sara; Petrovic, Mira; Barceló, Damià

    2014-07-25

    A novel fully automated method based on dual column switching using turbulent flow chromatography followed by liquid chromatography coupled to tandem mass spectrometry (TFC-LC-MS/MS) was applied for the determination of endocrine disruptors (EDCs) and related compounds in sediment and sewage sludge samples. This method allows the unequivocal identification and quantification of the most relevant environmental EDCs such as natural and synthetic estrogens and their conjugates, antimicrobials, parabens, bisphenol A (BPA), alkylphenolic compounds, benzotriazoles, and organophosphorus flame retardants, minimizing time of analysis and alleviating matrix effects. Applying this technique, after the extraction of the target compounds by pressurized liquid extraction (PLE), sediment and sewage sludge extracts were directly injected to the chromatographic system and the analytes were concentrated into the clean-up loading column. Using six-port switching system, the analytes were transferred to the analytical column for subsequent detection by MS-MS (QqQ). In order to optimize this multiplexing system, a comparative study employing six types of TurboFlow™ columns, with different chemical modifications, was performed to achieve the maximum retention of analytes and best elimination of matrix components. Using the optimized protocol low limits of quantification (LOQs) were obtained ranging from 0.0083 to 1.6 ng/g for sediment samples and from 0.10 to 125 ng/g for sewage sludge samples (except for alkylphenol monoethoxylate). The method was used to evaluate the presence and fate of target EDCs in the Ebro River which is the most important river in Spain with intensive agricultural and industrial activities in the basin that contribute to deteriorating soil and water quality. PMID:24909438

  17. Identification of atmospheric organic sources using the carbon hollow tube-gas chromatography method and factor analysis

    SciTech Connect

    Cobb, G.P.; Braman, R.S.; Gilbert, R.A. )

    1989-04-15

    Atmospheric organics were sampled and analyzed by using the carbon hollow tube-gas chromatography method. Chromatograms from spice mixtures, cigarettes, and ambient air were analyzed. Principal factor analysis of row order chromatographic data produces factors which are eigenchromatograms of the components in the samples. Component sources are identified from the eigenchromatograms in all experiments and the individual eigenchromatogram corresponding to a particular source is determined in most cases. Organic sources in ambient air and in cigaretts are identified with 87% certainty. Analysis of clove cigarettes allows the determination of the relative amount of clove in different cigarettes. A new nondestructive quality control method using the hollow tube-gas chromatography analysis is discussed.

  18. Improvement of recovery and repeatability in liquid chromatography-mass spectrometry analysis of peptides.

    PubMed

    van Midwoud, Paul M; Rieux, Laurent; Bischoff, Rainer; Verpoorte, Elisabeth; Niederländer, Harm A G

    2007-02-01

    Poor repeatability of peak areas is a problem frequently encountered in peptide analysis with nanoLiquid Chromatography coupled on-line with Mass Spectrometry (nanoLC-MS). As a result, quantitative analysis will be seriously hampered unless the observed variability can be corrected in some way. Currently, labeling techniques or addition of internal standards are often applied for this purpose. However, these procedures are elaborate and error-prone and may render complex samples even more complex. Moreover, whenever poor repeatability results from variable recovery, not just quantification, but also sensitivity is affected. We have studied the parameters influencing the repeatability of chromatographic peak areas for a model set of proteolytic peptides (i.e., a cytochrome c tryptic digest) in nanoLC-MS analysis. It is demonstrated that repeatability issues are mainly due to poor recovery of peptides from the sample vial. Problems are largely resolved by addition of an organic modifier to the sample vial to improve solubility of the peptides, but care needs to be taken not to lose peptides due to reduced affinity for reversed-phase materials. Good results are obtained when applying dimethylsulfoxide (DMSO) for this purpose. When applying DMSO, repeatability increases, and the limit of detection (LOD) decreases. For the most hydrophobic peptides, a gain in LOD of at least an order of magnitude is obtained. In an aqueous sample containing 0.1% formic acid (FA), it is possible to detect 100-200 fmol of peptide, whereas +/-10 fmol can be detected in a sample containing 5% FA and 25% DMSO (10 microL injections). PMID:17269734

  19. Systematic analysis of glycerol: colourimetric screening and gas chromatography-mass spectrometric confirmation.

    PubMed

    Sardela, Vinícius F; Scalco, Fernanda B; Cavalcante, Karina M; Simoni, Ruth E; Silva, Deyvison R; Pereira, Henrique Marcelo G; de Oliveira, Maria Lúcia L Costa; Aquino Neto, Francisco R

    2015-10-01

    Glycerol is a naturally occurring polyol in the human body, essential for several metabolic processes. It is widely used in the food, pharmaceutical, and medical industries and in clinical practice as a plasma volume expander (PVE). Athletes, however, may use glycerol to mask the presence of forbidden substances or to enhance performance, inclusively through hyperhydration achieved by glycerol ingestion with added fluid. These practices are considered doping, and are prohibited by the World Anti-Doping Agency (WADA). Therefore, glycerol was introduced in the prohibited list. Doping through glycerol ingestion can readily be identified by detection of elevated glycerol concentrations in urine. In this paper, a protocol for the fast detection of glycerol in urine is proposed. It consists of a previous visual colourimetric screening, followed by a quantitative/qualitative confirmation analysis by mass spectrometry. The screening procedure involves a reaction in which polyhydric alcohols are oxidized by periodate to formic acid and formaldehyde, which is detected by the addition of a fuchsin solution. For the subsequent qualitative/quantitative confirmation analysis, a gas chromatography-mass spectrometry based approach with a non-deuterated internal standard and a drying step of only 10 min is proposed. The linear correlation was demonstrated within WADA´s threshold range. The calculated RSD were 2.1% for within-day precision and 2.8% for between-day precision. The uncertainty estimation was calculated, and a value of 2.7% was obtained. The procedure may also be used for the analysis of other polyols in urine, as for example the PVE mannitol. PMID:26112364

  20. Comparative analysis of steroidal saponins in four Dioscoreae herbs by high performance liquid chromatography coupled with mass spectrometry.

    PubMed

    Guo, Long; Zeng, Su-Ling; Zhang, Yu; Li, Ping; Liu, E-Hu

    2016-01-01

    Steroidal saponins, which exhibit multiple pharmacological effects, are the major bioactive constituents in herbal medicines from Dioscoreae species. In this study, a sensitive method based on high performance liquid chromatography-mass spectrometry (HPLC-MS) was established and validated for qualitative and quantitative analysis of steroidal saponins in four Dioscoreae herbs including Dioscoreae Nipponica Rhizome (DNR) and Dioscoreae Hypoglaucae Rhizome (DHR), Dioscoreae Spongiosae Rhizome (DSR) and Dioscoreae Rhizome (DR). A total of eleven steroidal saponins were identified by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF/MS). Furthermore, seven major steroidal saponins was simultaneous quantified using a high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ/MS). The qualitative and quantitative analysis results indicated that the chemical composition of DNR, DHR and DSR samples exhibited a high level of global similarity, while the ingredients in DR varied greatly from the other three herbs. Moreover, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were performed to compare and discriminate the Dioscoreae herbs based on the quantitative data. The results demonstrated the qualitative and quantitative analysis of steroidal saponins based on HPLC-MS is a feasible method for quality control of Dioscoreae herbs. PMID:26344383

  1. [Separation of tannins in Rhubarb and its analysis by high performance liquid chromatography-mass spectrometry].

    PubMed

    Ding, Mingyu; Ni, Weiwei

    2004-11-01

    In order to investigate the pharmaceutical actions of rhubarb, a method for extracting, separating and analyzing the tannin components in rhubarb was studied. At first, a procedure for the group separation of tannins from the water-ethanol extract of rhubarb was established based on the formation of tannins-caffein precipitation. Then, a high performance liquid chromatographic (HPLC) method for the analysis of tannins in rhubarb was developed. This HPLC method is based on a reversed-phase C18 column and polar mobile-phase such as water and methanol with gradient elution, and the tannins can be well separated. Finally, the identification of the tannin components in rhubarb was carried out by high performance liquid chromatography-mass spectrometry (HPLC-MS). The structures of the main tannin components (gallic acid, catechin, the dimer, trimer, tetramer and pentamer of catechin) in rhubarb are suggested. The fragmentation laws of the tannin components are summarized. In comparing with previous methods, it is simple and without the interference of co-existed compounds. PMID:15807111

  2. High-performance liquid chromatography (HPLC) analysis of eu- and pheomelanin in melanogenesis control.

    PubMed

    Ito, S

    1993-02-01

    Two types of melanogenesis, eumelanogenesis and pheomelanogenesis, can be switched from one type to another under certain physiologic or pathologic conditions. To study the regulation of melanogenesis, we developed a high-performance liquid chromatography method to analyze quantitatively the contents of eu- and pheomelanin in tissue samples without any isolation procedures. The rationale is that permanganate oxidation of eumelanin yields pyrrole-2,3,5-tricarboxylic acid, which may serve as a quantitatively significant indicator of eumelanin, whereas hydriodic acid hydrolysis of pheomelanin yields aminohydroxyphenylalanine as a specific indicator of pheomelanin. The method has been successfully applied to the analysis of eu- and pheomelanin not only in synthetic melanins, melanosomes, hair, feathers, and melanomas, but also in human epidermis and cultured melanocytes. These studies indicate that there exists an inverse relationship between the contents of eu- and pheomelanin. We propose that the switching between the two types of melanogenesis is mainly controlled by the level of tyrosinase activity: higher activity leads to eumelanogenesis and lower activity leads to pheomelanogenesis. When tyrosinase activity is low, dopaquinone, a reactive intermediate in melanogenesis, is quantitatively converted to glutathionyldopa, which gives rise exclusively to pheomelanin. When tyrosinase activity is high, an excess of dopaquinone is produced, which results in the inactivation of glutathione reductase and gamma-glutamyl transpeptidase, enzymes essential for pheomelanogenesis. These biochemical events eventually leads to eumelanogenesis. PMID:8433004

  3. Irreversible and reversible reactive chromatography: analytical solutions and moment analysis for rectangular pulse injections.

    PubMed

    Bibi, Sameena; Qamar, Shamsul; Seidel-Morgenstern, Andreas

    2015-03-13

    This work is concerned with the analysis of models for linear reactive chromatography describing irreversible A→B and reversible A↔B reactions. In contrast to previously published results rectangular reactant pulses are injected into initially empty or pre-equilibrated columns assuming both Dirichlet and Danckwerts boundary conditions. The models consist of two partial differential equations, accounting for convection, longitudinal dispersion and first order chemical reactions. Due to the effect of involved mechanisms on solute transport, analytical and numerical solutions of the models could be helpful to understand, design and optimize chromatographic reactors. The Laplace transformation is applied to solve the model equations analytically for linear adsorption isotherms. Statistical temporal moments are derived from solutions in the Laplace domain. Analytical results are compared with numerical predictions generated using a high-resolution finite volume scheme for two sets of boundary conditions. Several case studies are carried out to analyze reactive liquid chromatographic processes for a wide range of mass transfer and reaction kinetics. Good agreements in the results validate the correctness of the analytical solutions and accuracy of the proposed numerical algorithm. PMID:25670415

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

    PubMed Central

    2014-01-01

    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-μm or 2.6–2.8-μm (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

  5. Analysis of siloxanes in hydrocarbon mixtures using comprehensive two-dimensional gas chromatography.

    PubMed

    Ghosh, Abhijit; Seeley, Stacy K; Nartker, Steven R; Seeley, John V

    2014-09-19

    A comprehensive two-dimensional gas chromatography (GC×GC) method for separating siloxanes from hydrocarbons has been developed using a systematic process. First, the retention indices of a set of siloxanes and a set of hydrocarbons were determined on 6 different stationary phases. The retention indices were then used to model GC×GC separation on 15 different stationary phase pairs. The SPB-Octyl×DB-1 pair was predicted to provide the best separation of the siloxanes from the hydrocarbons. The efficacy of this stationary phase pair was experimentally tested by performing a GC×GC analysis of gasoline spiked with siloxanes and by analyzing biogas obtained from a local wastewater treatment facility. The model predictions agreed well with the experimental results. The SPB-Octyl×DB-1 stationary phase pair constrained the hydrocarbons to a narrow range of secondary retention times and fully isolated the siloxanes from the hydrocarbon band. The resulting GC×GC method allows siloxanes to be resolved from complex mixtures of hydrocarbons without requiring the use of a selective detector. PMID:25087744

  6. 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.

  7. Analysis of Parent Synthetic Cannabinoids in Blood and Urinary Metabolites by Liquid Chromatography Tandem Mass Spectrometry.

    PubMed

    Knittel, Jessica L; Holler, Justin M; Chmiel, Jeffrey D; Vorce, Shawn P; Magluilo, Joseph; Levine, Barry; Ramos, Gerardo; Bosy, Thomas Z

    2016-04-01

    Synthetic cannabinoids emerged on the designer drug market in recent years due to their ability to produce cannabis-like effects without the risk of detection by traditional drug testing techniques such as immunoassay and gas chromatography-mass spectrometry. As government agencies work to schedule existing synthetic cannabinoids, new, unregulated and structurally diverse compounds continue to be developed and sold. Synthetic cannabinoids undergo extensive metabolic conversion. Consequently, both blood and urine specimens may play an important role in the forensic analysis of synthetic cannabinoids. It has been observed that structurally similar synthetic cannabinoids follow common metabolic pathways, which often produce metabolites with similar metabolic transformations. Presented are two validated quantitative methods for extracting and identifying 15 parent synthetic cannabinoids in blood, 17 synthetic cannabinoid metabolites in urine and the qualitative identification of 2 additional parent compounds. The linear range for most synthetic cannabinoid compounds monitored was 0.1-10 ng/mL with the limit of detection between 0.01 and 0.5 ng/mL. Selectivity, specificity, accuracy, precision, recovery and matrix effect were also examined and determined to be acceptable for each compound. The validated methods were used to analyze a compilation of synthetic cannabinoid investigative cases where both blood and urine specimens were submitted. The study suggests a strong correlation between the metabolites detected in urine and the parent compounds found in blood. PMID:26792810

  8. Simultaneous analysis of serotonin, melatonin, piceid and resveratrol in fruits using liquid chromatography tandem mass spectrometry.

    PubMed

    Huang, Xin; Mazza, Giuseppe

    2011-06-24

    An analytical method was developed for the simultaneous quantification of serotonin, melatonin, trans- and cis-piceid, and trans- and cis-resveratrol using reversed-phase high performance liquid chromatography coupled to mass spectrometry (HPLC-MS) with electrospray ionization (ESI) in both positive and negative ionization modes. HPLC optimal analytical separation was achieved using a mixture of acetonitrile and water with 0.1% formic acid as the mobile phase in linear gradient elution. The mass spectrometry parameters were optimized for reliable quantification and the enhanced selectivity and sensitivity selected reaction monitoring mode (SRM) was applied. For extraction, the direct analysis of initial methanol extracts was compared with further ethyl acetate extraction. In order to demonstrate the applicability of this analytical method, serotonin, melatonin, trans- and cis-piceid, and trans- and cis-resveratrol from 24 kinds of commonly consumed fruits were quantified. The highest serotonin content was found in plantain, while orange bell peppers had the highest melatonin content. Grape samples possessed higher trans- and cis-piceid, and trans- and cis-resveratrol contents than the other fruits. The results indicate that the combination of HPLC-MS detection and simple sample preparation allows the rapid and accurate quantification of serotonin, melatonin, trans- and cis-piceid, and trans- and cis-resveratrol in fruits. PMID:21570690

  9. Analysis of monosaccharide composition of Cyclocarya paliurus polysaccharide with anion exchange chromatography.

    PubMed

    Xie, Jian-Hua; Shen, Ming-Yue; Nie, Shao-Ping; Liu, Xin; Zhang, Hui; Xie, Ming-Yong

    2013-10-15

    A simple, rapid and sensitive analytical method for the determination of monosaccharide composition in Cyclocarya paliurus polysaccharide was developed and validated. This method was based on hydrolysis of the polysaccharides followed by high-performance anion-exchange chromatography analysis. The effects of sodium hydroxide concentration and column temperature on retention and separation of the monosaccharide were investigated with Carbo PAC™ PA10 analytical column. The established method was validated and the results showed that this method had good linearity (R(2), 0.9987-0.9999), adequate accuracy (98.53-102.13% recovery), high precision (relative standard deviation <3.8%) and sensitive detection limits (2.57-7.86 nM), with a simple preparation of the samples (no need to derivatize the samples) and short run time (20 min). The results showed that the C. paliurus polysaccharide consisted of rhamnose, arabinose, galactose, glucose, mannose and xylose in the molar ratio of 1.00:1.85:3.26:3.12:0.85:0.29. PMID:23987436

  10. Mass Spectrometric Analysis of Intact Human Monoclonal Antibody Aggregates Fractionated by Size-Exclusion Chromatography

    PubMed Central

    Kükrer, Başak; Filipe, Vasco; van Duijn, Esther; Kasper, Piotr T.; Vreeken, Rob J.; Heck, Albert J. R.

    2010-01-01

    ABSTRACT Purpose The aim of this study was to develop a method to characterize intact soluble monoclonal IgG1 antibody (IgG) oligomers by mass spectrometry. Methods IgG aggregates (dimers, trimers, tetramers and high-molecular-weight oligomers) were created by subjecting an IgG formulation to several pH jumps. Protein oligomer fractions were isolated by high performance size exclusion chromatography (HP-SEC), dialyzed against ammonium acetate pH 6.0 (a mass spectrometry-compatible volatile buffer), and analyzed by native electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). Results Monomeric and aggregated IgG fractions in the stressed IgG formulation were successfully isolated by HP-SEC. ESI-TOF MS analysis enabled us to determine the molecular weight of the monomeric IgG as well as the aggregates, including dimers, trimers and tetramers. HP-SEC separation and sample preparation proved to be necessary for good quality signal in ESI-TOF MS. Both the HP-SEC protocol and the ESI-TOF mass spectrometric technique were shown to leave the IgG oligomers largely intact. Conclusions ESI-TOF MS is a useful tool complementary to HP-SEC to identify and characterize small oligomeric protein aggregates. PMID:20680668

  11. 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

  12. Liquid Chromatography-Tandem Mass Spectrometry for Analysis of Intestinal Permeability of Loperamide in Physiological Buffer

    PubMed Central

    Rubelt, Miriam S.; Amasheh, Salah; Grobosch, Thomas; Stein, Christoph

    2012-01-01

    Analysis of in vitro samples with high salt concentrations represents a major challenge for fast and specific quantification with liquid chromatography-tandem mass spectrometry (LC-MS/MS). To investigate the intestinal permeability of opioids in vitro employing the Ussing chamber technique, we developed and validated a fast, sensitive and selective method based on LC–MS/MS for the determination of loperamide in HEPES-buffered Ringer's solution. Chromatographic separation was achieved with an Atlantis dC18 column, 2.1 mm×20 mm, 3 µm particle size and a gradient consisting of methanol/0.1% formic acid and ammonium acetate. The flow rate was 0.7 ml/min, and the total run time was 3 min. For quantification, two mass transitions for loperamide and a deuterated internal standard (methadone-d3) were used. The lower limit of loperamide quantification was 0.2 ng/ml. This new LC-MS/MS method can be used for the detection of loperamide in any experimental setup using HEPES-buffered Ringer's solution as a matrix compound. PMID:23144895

  13. Holistic analysis of seven active ingredients by micellar electrokinetic chromatography from three medicinal herbs composing Shuanghuanglian.

    PubMed

    Zhou, Xian-Jing; Chen, Juan; Li, Ying-Dong; Jin, Ling; Shi, Yan-Ping

    2015-01-01

    A simple and reliable method has been developed with a new strategy named holistic analysis of multiple constituents to evaluate the quality of the well-known traditional Chinese medicine (TCM) Shuanghuanglian (SHL) oral liquid and soft capsule. Seven main constituents of the medicine, i.e., baicalein, baicalin, chlorogenic acid, wogonin, scutellarin, forsythin and hyperin, were selected as the evaluation markers and analyzed by micellar electrokinetic chromatography. The effects of buffer pH, concentration of electrolyte, organic modifier and applied voltage on migration behavior were studied systematically. The optimum conditions for the separation were achieved in a 12.5 mM borate-10 mM sodium dihydrogen phosphate-10 mM sodium dodecyl sulfate buffer at pH 9.1 containing 10% (v/v) acetonitrile under 15 kV. The analytes were identified by their relative time with regard to para-hydroxybenzoic acid migration time used as an internal standard. The method was validated in terms of linearity, limit of detection and quantification, precision, accuracy and recoveries. The correlation coefficient ranged from 0.9962 to 0.9992. The limits of detection (S/N = 3) were from 0.15 to 3.95 μg mL(-1). Recoveries of seven analytes in the SHL samples ranged from 89.00 to 103.04%. The proposed method was successfully applied for the quality control of complicated TCM SHL. PMID:26060213

  14. Systematic Optimization of Long Gradient Chromatography Mass Spectrometry for Deep Analysis of Brain Proteome

    SciTech Connect

    Wang, Hong; Yang, Yanling; Li, Yuxin; Bai, Bing; Wang, Xusheng; Tan, Haiyan; Liu, Tao; Beach, Thomas G.; Peng, Junmun; Wu, Zhiping

    2015-02-06

    Development of high resolution liquid chromatography (LC) is essential for improving the sensitivity and throughput of mass spectrometry (MS)-based proteomics. Here we present systematic optimization of a long gradient LC-MS/MS platform to enhance protein identification from a complex mixture. The platform employed an in-house fabricated, reverse phase column (100 μm x 150 cm) coupled with Q Exactive MS. The column was capable of achieving a peak capacity of approximately 700 in a 720 min gradient of 10-45% acetonitrile. The optimal loading level was about 6 micrograms of peptides, although the column allowed loading as many as 20 micrograms. Gas phase fractionation of peptide ions further increased the number of peptide identification by ~10%. Moreover, the combination of basic pH LC pre-fractionation with the long gradient LC-MS/MS platform enabled the identification of 96,127 peptides and 10,544 proteins at 1% protein false discovery rate in a postmortem brain sample of Alzheimer’s disease. As deep RNA sequencing of the same specimen suggested that ~16,000 genes were expressed, current analysis covered more than 60% of the expressed proteome. Further improvement strategies of the LC/LC-MS/MS platform were also discussed.

  15. Analysis of Amphetamine-Derived Designer Drugs by Gas Chromatography with Mass Spectrometry.

    PubMed

    Ondra, Peter; Válka, Ivo; Knob, Radim; Ginterová, Pavlína; Maier, Vítězslav

    2016-01-01

    The 22 amphetamine-derived synthetic drugs (ADSDs), mostly cathinones, were examined by gas chromatography with mass spectrometry using two different derivatization methods with (i) heptafluorobutyric anhydride (HFBA) and (ii) pentafluorobenzoyl chloride (PFBCl). Both developed derivatization approaches were evaluated and compared for urine and serum samples. Extraction procedures proved to give satisfactory results with regard to recoveries and extract purity, even though both derivatization methods reached acceptable sensitivity for the intended use. The derivatization with PFBCl showed better results with respect to retention and response stability, thus the PFBCl method was selected for validation. Calibration curves were linear over the tested concentration range of 20-1,000 ng/mL with the R(2) values ranging from 0.994 to 0.998. Intra- and interday precisions and accuracies were within 20% for all concentrations in the linear range. The limit of detection was determined to be lower than 2 ng/mL for all 22 analytes. The method proved to be a useful analytical tool in the course of systematic toxicological analysis. PMID:26446487

  16. A comprehensive quantitative analysis of methylated and ethylated DNA using high pressure liquid chromatography.

    PubMed

    Beranek, D T; Weis, C C; Swenson, D H

    1980-07-01

    Methods were developed for the efficient routine degradation and fractionation of ethylated and methylated DNA. Alkylated DNA was hydrolyzed by a neutral thermal method to yield 3- and 7- alkylpurines and O2-alkylcytosines. The partially apurinic DNA was separated from the bases by precipitation in 0.1 N HCl. Portions of the DNA precipitate were further hydrolyzed either by 0.1 N HCl to yield purine bases, or by enzymes to yield nucleosides and phosphotriesters. The chemical and enzymic digests were fractionated by a combination of high pressure liquid chromatography systems to yield quantitative estimates of the following products from methylated or ethylated DNA: 1-, 3-, and 7-alkyladenines, O2-alkylcytosines, 3-, O6-, and 7- alkylguanines and O2-, 3-, and O4-alkylthymines. N6-Alkyladenines, 1-alkylguanines and N2-alkylguanines were not detected and the 3- alkylcytosines were detected but not quantified. Phosphotriesters were estimated from the amounts of recovered alkyl phosphotriesters of thymidylyl (3'-5') thymidine. Using these methods, it was possible to account for 98, 81, 98, and 92% of the DNA bound alkyl groups obtained from DNA reacted with [14C]methyl methanesulfonate, [3H]ethyl methanesulfonate, N-[3H]-methyl-N-nitrosourea, and N-[14C]ethyl-N-nitrosourea, respectively. The methods described provide reproducible and quantitative methods of analysis for all the known methylated or ethylated products in a single DNA sample. PMID:11219835

  17. Enrichment of Integral Membrane Proteins for Proteomic Analysis Using Liquid Chromatography-Tandem Mass Spectrometry

    SciTech Connect

    Blonder, Josip; Goshe, Michael B.; Moore, Ronald J.; Pasa-Tolic, Liljiana; Masselon, Christophe D.; Lipton, Mary S.; Smith, Richard D.

    2002-04-01

    Currently, most proteomic studies rely on liquid chromatography-tandem mass spectrometry (LC-MS/MS) to detect and identify constituent peptides of enzymatically digested proteins obtained from various organisms and cell types. However, sample preparation methods for isolating membrane proteins typically involve the use of detergents, chaotropes, or reducing reagents that often interfere with electrospray ionization (ESI). To increase the identification of integral membrane proteins by LC-ESI-MS/MS, a sample preparation method combining carbonate extraction and surfactant-free organics solvent-assisted solubilization and proteolysis was developed and used to target the membrane subproteome of Deinococcus radiodurans. Out of 503 proteins identified, 135 were recognized as hydrophobic based on their positive grand average of hydropathicity values that covers 15% of the theoretical hydrophobic proteome. Using the PSORT algorithm, 268 identified proteins were recognized as integral membrane proteins covering 21% and 43% of the predicted integral cytoplasmic and outer membrane proteins, respectively. Of the integral cytoplasmic membrane proteins containing four or more predicted transmembrane domains (TMDs), 65% were identified by detecting at least one peptide spanning a TMD using LC-MS/MS. The extensive identification of highly hydrophobic proteins containing multiple TMDs confirms the efficacy of the described sample preparation protocol to isolate and solubilize integral membrane proteins and validates the method for large-scale analysis of bacterial membrane subproteomes using LC-ESI-MS/MS.

  18. Systematic Optimization of Long Gradient Chromatography Mass Spectrometry for Deep Analysis of Brain Proteome

    PubMed Central

    2015-01-01

    The development of high-resolution liquid chromatography (LC) is essential for improving the sensitivity and throughput of mass spectrometry (MS)-based proteomics. Here we present systematic optimization of a long gradient LC–MS/MS platform to enhance protein identification from a complex mixture. The platform employed an in-house fabricated, reverse-phase long column (100 μm × 150 cm, 5 μm C18 beads) coupled to Q Exactive MS. The column was capable of achieving a peak capacity of ∼700 in a 720 min gradient of 10–45% acetonitrile. The optimal loading level was ∼6 μg of peptides, although the column allowed loading as many as 20 μg. Gas-phase fractionation of peptide ions further increased the number of peptide identification by ∼10%. Moreover, the combination of basic pH LC prefractionation with the long gradient LC–MS/MS platform enabled the identification of 96 127 peptides and 10 544 proteins at 1% protein false discovery rate in a post-mortem brain sample of Alzheimer’s disease. Because deep RNA sequencing of the same specimen suggested that ∼16 000 genes were expressed, the current analysis covered more than 60% of the expressed proteome. Further improvement strategies of the LC/LC–MS/MS platform were also discussed. PMID:25455107

  19. Analysis of Dyes Extracted from Millimeter-Size Nylon Fibers by Micellar Electrokinetic Chromatography

    SciTech Connect

    Lewis, L.A.

    2001-07-30

    The Learning Objective is to present to the forensic community a potential qualitative/quantitative method for trace-fiber color comparisons using micellar electrokinetic chromatography (MEKC). Developing a means of analyzing extracted dye constituents from millimeter-size nylon fiber samples was the objective of this research initiative. Aside from ascertaining fiber type, color evaluation and source comparison of trace-fiber evidence plays a critical role in forensic-fiber examinations. Literally thousands of dyes exist to date, including both natural and synthetic compounds. Typically a three-color-dye combination is employed to affect a given color on fiber material. The result of this practice leads to a significant number of potential dye combinations capable of producing a similar color and shade. Since a typical forensic fiber sample is 2 mm or less in length, an ideal forensic dye analysis would qualitatively and quantitatively identify the extracted dye constituents from a sample size of 1 mm or smaller. The goal of this research was to develop an analytical method for comparing individual dye constituents from trace-fiber evidence with dyes extracted from a suspected source, while preserving as much of the original evidence as possible.

  20. 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 μg/mL with r2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 μg/mL and 1.28 μg/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).

  1. Human salivary glucose analysis by high-performance ion-exchange chromatography and pulsed amperometric detection.

    PubMed

    Gough, H; Luke, G A; Beeley, J A; Geddes, D A

    1996-02-01

    The aim of this project was to develop an analytical procedure with the required level of sensitivity for the determination of glucose concentrations in small volumes of unstimulated fasting whole saliva. The technique involves high-performance ion-exchange chromatography at high pH and pulsed amperometric detection. It has a high level of reproducibility, a sensitivity as low as 0.1 mumol/l and requires only 50 microliters samples (sensitivity = 0.002 pmol). Inhibition of glucose metabolism, by procedures such as collection into 0.1% (w/v) sodium fluoride, was shown to be essential if accurate results are to be obtained. Collection on to ice followed by storage at -20 degrees C was shown to be unsuitable and resulted in glucose loss by degradation. There were inter- and intraindividual variations in the glucose concentration in unstimulated mixed saliva (range; 0.02-0.4 mmol/l). The procedure can be used for the analysis of other salivary carbohydrates and for monitoring the clearance of dietary carbohydrates from the mouth. PMID:8712970

  2. 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

  3. Nano-liquid chromatography in nutraceutical analysis: determination of polyphenols in bee pollen.

    PubMed

    Fanali, Chiara; Dugo, Laura; Rocco, Anna

    2013-10-25

    In this study, a nano-liquid chromatography based method for the simultaneous separation of 16 polyphenols employing UV-vis detection has been developed. A 100 μm I.D. capillary column packed with C18 core-shell particles (2.6 μm particle size, 100 Å) for 10 cm was employed. The separation of analytes was performed with a step gradient in less than 20 min, using 0.5% formic acid aqueous solution and acetonitrile as eluents. The optimized analytical method was validated and the resulting RSD% for intra-day and inter-day repeatability, related to retention time, retention factor and peak area, were below 4.68 and 5.57%, respectively. LOD and LOQ values were as low as 0.78 and 3.12 μg/mL, while linearity, assessed in the concentration range of interest for all analytes, gave R(2)≥0.990. The method was finally applied to the analysis of polyphenols extracted from a collected bee pollen. Nine polyphenols, namely o-, p-coumaric acid, ferulic acid, myricetin, cinnamic acid, quercetin, naringenin, hesperitin and kaempferol, were identified. All analytes, with the exception of p-coumaric acid and myricetin, which partially co-eluted with other pollen components, were also quantified in the sample. PMID:23880468

  4. Determination of delta-aminolaevulinic acid in biological fluids by gas-liquid chromatography with electron-capture detection.

    PubMed Central

    Gorchein, A

    1984-01-01

    A derivative of delta-aminolaevulinic acid (AmLev), 2-methyl-3-acetyl-4-(3-propionic acid pentafluorobenzyl ester)pyrrole, with favourable properties for g.l.c. with electron-capture detection, was synthesized. Less than 1 pg could be detected on the column. 6-Amino-5-oxohexanoic acid formed the analogous derivative under similar conditions and was used as the internal standard in the development of a highly sensitive and specific assay for AmLev. The method has been applied to peripheral-venous and umbilical-cord plasma and to cerebrospinal fluid of normal and porphyric subjects. PMID:6547602

  5. 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 ...

  6. Reliable peak selection for multisample analysis with comprehensive two-dimensional chromatography

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Comprehensive two-dimensional chromatography is a powerful technology for analyzing the patterns of constituent compounds in complex samples, but matching chromatographic features across large sample sets is difficult. This paper describes a new, automated method for selecting chromatographic peaks ...

  7. 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...

  8. ANALYSIS OF HAZARDOUS WASTE AND ENVIRONMENTAL EXTRACTS BY CAPILLARY GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY AND CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    The relative sensitivities of fused-silica capillary column gas chromatography/Fourier transform infrared spectrometry (FSCC/GC/FT-IR) versus packed-column GC/FT-IR and FSCC/GC/FT-IR versus fused-silica capillary column gas chromatography/mass spectrometry (FSCC/GC/MS) were compa...

  9. 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.

  10. Direct Numerical Simulation of turbulent flows over superhydrophobic surfaces: capillary waves on gas-liquid interface

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

    Superhydrophobic surfaces under liquid flow can produce significant slip, and thus drag reduction, when they entrap gas bubbles within their roughness elements. Our work aims to explore the onset mechanism to the failure of drag reduction by superhydrophobic surfaces when they are exposed to turbulent boundary layers. We focus on the effect of finite surface tension to the dynamic response of deformable interfaces between overlying water flow and the gas pockets. To this end, we conduct direct numerical simulations of turbulent flows over superhydrophobic surfaces allowing deformable gas-liquid interface. DNS results show that spanwise-coherent, upstream-traveling waves develop on the gas-liquid interface as a result of its interactions with turbulence. We study the nature and scaling of the upstream-traveling waves through semi-analytical modeling. We will show that the traveling waves are well described by a Weber number based on the slip velocity at the interface. In higher Weber number, the stability of gas pocket decreases as the amplitude of interface deformation and the magnitude of pressure fluctuations are augmented. Supported by Office of Naval Research and the Kwanjeong Educational Scholarship Foundation.

  11. Shadow imaging in bubbly gas-liquid two-phase flow in porous structures

    NASA Astrophysics Data System (ADS)

    Altheimer, Marco; Häfeli, Richard; Wälchli, Carmen; Rudolf von Rohr, Philipp

    2015-09-01

    Shadow imaging is used for the investigation of bubbly gas-liquid two-phase flow in a porous structure. The porous structure is made of Somos WaterShed XC 11122, a clear epoxy resin used in rapid prototyping. Optical access is provided by using an aqueous solution of sodium iodide and zinc iodide having the same refractive index as the structure material (). Nitrogen is injected into the continuous phase at volumetric transport fractions in the range of resulting in a hold-up of . The obtained images of overlapping bubble shadows are processed to measure the bubble dimensions. Therefore, a new processing sequence is developed to determine bubble dimensions from overlapping bubble shadows by ellipse fitting. The accuracy of the bubble detection and sizing routine is assessed processing synthetic images. It is shown that the developed technique is suitable for volumetric two-phase flow measurements. Important global quantities such as gas hold-up and total interfacial area can be measured with only one camera. Operation parameters for gas-liquid two-phase flows are determined to improve mass and heat transfer between the phases.

  12. Kinetics of gas-liquid reaction between NO and Co(NH3)6(2+).

    PubMed

    Long, Xiang-li; Xiao, Wen-De; Yuan, Wei-kang

    2005-08-31

    Wet ammonia desulphurization process can be retrofitted for combined removal of SO2 and NO from the flue gas by adding soluble cobalt(II) salts into the aqueous ammonia solutions. The Co(NH3)6(2+) formed by ammonia binding with Co2+ is the active constituent of scrubbing NO from the flue gas streams. A stirred vessel with a plane gas-liquid interface was used to measure the chemical absorption rates of nitric oxide into the Co(NH3)6(2+) solution under anaerobic and aerobic conditions separately. The experiments manifest that the nitric oxide absorption reaction can be regarded as instantaneous when nitric oxide concentration levels are parts per million ranges. The gas-liquid reaction becomes gas film controlling as Co(NH3)6(2+) concentration exceeds 0.02 mol/l. The NO absorption rate is proportional to the nitric oxide inlet concentration. Oxygen in the gas phase is favorable to the absorption of nitric oxide. But it is of little significance to increase the oxygen concentration above 5.2%. The NO absorption rate decreases with temperature. The kinetic equation of NO absorption into the Co(NH3)6(2+) solution under aerobic condition can be written as. PMID:15869841

  13. Centrifugal scaling of isothermal gas-liquid flows in horizontal tubes

    NASA Astrophysics Data System (ADS)

    Geraets, Jacques Joseph Marie

    1986-05-01

    To test the similarity criteria of two-phase gas-liquid flows, arising from the governing equations and boundary conditions, the flow of air and a water-glycerine mixture in a 50 mm diameter horizontal tube is compared with a two-phase flow of helium and water in a 5 mm diameter tube rotating around a parallel vertical axis (the effective gravity is 113 g0). Results emphasize that in general only dimensionless correlations provide meaningful predictions. The homogeneous Dukler case 1 (1964b) correlation, which contains no two-phase information, provides the best fit (the standard deviation is 21%) with the measured pressure drops. For predicting flow pattern the most promising approach is that of Taitel and Dukler (1976). Examples of scaling down large diameter, high pressure pipelines are presented. With a scale factor of 1/30 equality of the Froude number, the gas-liquid density ratio, and either the Reynolds number or the Weber number can be realized. Compressibility and gas viscosity are not properly scaled.

  14. Deactivation of formate dehydrogenase (FDH) in solution and at gas-liquid interfaces.

    PubMed

    Bommarius, Andreas S; Karau, Andreas

    2005-01-01

    Enzymes, increasingly important in the synthesis of fine chemicals and pharmaceutical intermediates, are often insufficiently stable under reacting conditions. We have investigated the stability, in homogeneous aqueous solution and at gas-liquid interfaces, of formate dehydrogenase (FDH), important for cofactor regeneration, from Candida boidinii and overexpressed in E. coli. When exposed to mechanical stress, residual activity, [E](t)/[E](0), and residual protein were found to scale proportionally with gas-liquid surface area in the bubble column, verifying a surface-driven process, and with time and total throughput in a gear pump, but did not seem to be influenced much by shear in a Couette viscometer. All FDH variants are deactivated by chaotropes but not kosmotropes: the first-order deactivation constant k(d) correlates well with the Jones-Dole coefficient B but not well with the surface tension increment deltasigma of various concentrated ammonium salt solutions. This finding might provide guidance for focusing the search for quantitative theories of Hofmeister effects. PMID:16321049

  15. 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. Supported by the Office of Naval Research and the Kwanjeong Educational Scholarship Foundation.

  16. Observation of Gas-Liquid Flow Near the Exit Orifice of An Effervescent Atomizer

    NASA Astrophysics Data System (ADS)

    Sun, C. H.; Ning, Z.; Lü, M.; Fu, J.; Li, Y. X.

    For deepen the understanding of the mechanism of effervescent atomization: it is necessary to have a better observation on the gas-liquid flow near the exit orifice. Both image and acoustic ways were introduced to observe the gas-fluid flow by a transparent effervescent atomizer. The results show that: It can be clearly seen from images that internal flow regimes make great influence on the spray behavior. Spray acoustic observation is an effective way to grasp the gas-liquid two phases flow behavior when they ejecting from the exit orifice. The acoustic analyzing in time and frequency domain has the ability to obtain the discrete phenomenon existing in effervescent sprays, in thus way, acoustic features could give a new perspective on effervescent spray over time. What's more, the discrete phenomenon in dilute bubbly flow and slug flow can be easily captured from after acoustic analyzing. Uniform two-phase distribution of internal flow shows continues acoustic performance after observing the homogeneous bubbly flow and chum flow.

  17. 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.

  18. Thin-layer chromatography-pyrolysis-gas chromatography-mass spectrometry: a multidimensional approach to marine lipid class and molecular species analysis.

    PubMed

    Hudson, E D; Helleur, R J; Parrish, C C

    2001-04-01

    A new multidimensional chromatographic method is described in which material separated into lipid-class bands on silica-coated quartz thin-layer chromatography (TLC) rods (Chromarods) is desorbed using a pyrolysis unit interface and introduced directly into a gas chromatograph-mass spectrometer for molecular species analysis. Steryl esters, wax esters, hydrocarbons, ketones, and fatty-acid methyl esters (FAMEs) are thermally desorbed without pretreatment. In order to desorb free sterols, monoacylglycerols (MAGs), aliphatic alcohols, and free fatty acids, the esters are converted to trimethylsilyl derivatives on the rod. Triacylglycerols and phospholipids are converted to FAMEs by thermochemolysis with tetramethylammonium hydroxide. The method's utility is demonstrated with lipids from seawater particulate matter by first confirming the identity of lipid bands with the appropriate standards. The wax ester-steryl ester TLC band contained no more than 8% steryl esters. Wax esters of up to C42 are detected. In six individual acyl lipid classes, C14-C22 fatty acids are detected with C16 acids predominant in all but wax esters. C16-C22 MAGs are identified in the complex acetone-mobile polar lipid band. The method successfully extends the scope of latroscan TLC-flame-ionization detection on Chromarods, which is a widely used technique for lipid-class analysis. Modification of the pyrolysis probe to handle intact TLC rods is a future objective. PMID:11318066

  19. Ion chromatography applications

    SciTech Connect

    Smith, R.E.

    1988-01-01

    This book describes recent advances in ion chromatography and demonstrates how it is used to solve scientific and industrial problems. The basic principles of ion chromatography are explained, including gradient elution of ions and micromembrane suppressors. The various anion and cation exchange columns together with various detection methods and applications of ion chromatography in the environmental and life sciences and industry are reviewed. Over 100 chromatograms which illustrate parameters needed to perform analysis and data on gradient and mobile phase ion chromatography are included.

  20. Perceptual Characterization and Analysis of Aroma Mixtures Using Gas Chromatography Recomposition-Olfactometry

    PubMed Central

    Johnson, Arielle J.; Hirson, Gregory D.; Ebeler, Susan E.

    2012-01-01

    This paper describes the design of a new instrumental technique, Gas Chromatography Recomposition-Olfactometry (GC-R), that adapts the reconstitution technique used in flavor chemistry studies by extracting volatiles from a sample by headspace solid-phase microextraction (SPME), separating the extract on a capillary GC column, and recombining individual compounds selectively as they elute off of the column into a mixture for sensory analysis (Figure 1). Using the chromatogram of a mixture as a map, the GC-R instrument allows the operator to cut apart" and recombine the components of the mixture at will, selecting compounds, peaks, or sections based on retention time to include or exclude in a reconstitution for sensory analysis. Selective recombination is accomplished with the installation of a Deans Switch directly in-line with the column, which directs compounds either to waste or to a cryotrap at the operator's discretion. This enables the creation of, for example, aroma reconstitutions incorporating all of the volatiles in a sample, including instrumentally undetectable compounds as well those present at concentrations below sensory thresholds, thus correcting for the reconstitution discrepancy" sometimes noted in flavor chemistry studies. Using only flowering lavender (Lavandula angustifola Hidcote Blue) as a source for volatiles, we used the instrument to build mixtures of subsets of lavender volatiles in-instrument and characterized their aroma qualities with a sensory panel. We showed evidence of additive, masking, and synergistic effects in these mixtures and of lavender' aroma character as an emergent property of specific mixtures. This was accomplished without the need for chemical standards, reductive aroma models, or calculation of Odor Activity Values, and is broadly applicable to any aroma or flavor. PMID:22912722

  1. Analysis of polar urinary metabolites for metabolic phenotyping using supercritical fluid chromatography and mass spectrometry.

    PubMed

    Sen, Arundhuti; Knappy, Christopher; Lewis, Matthew R; Plumb, Robert S; Wilson, Ian D; Nicholson, Jeremy K; Smith, Norman W

    2016-06-01

    Supercritical fluid chromatography (SFC) is frequently used for the analysis and separation of non-polar metabolites, but remains relatively underutilised for the study of polar molecules, even those which pose difficulties with established reversed-phase (RP) or hydrophilic interaction liquid chromatographic (HILIC) methodologies. Here, we present a fast SFC-MS method for the analysis of medium and high-polarity (-7≤cLogP≤2) compounds, designed for implementation in a high-throughput metabonomics setting. Sixty polar analytes were first screened to identify those most suitable for inclusion in chromatographic test mixtures; then, a multi-dimensional method development study was conducted to determine the optimal choice of stationary phase, modifier additive and temperature for the separation of such analytes using SFC. The test mixtures were separated on a total of twelve different column chemistries at three different temperatures, using CO2-methanol-based mobile phases containing a variety of polar additives. Chromatographic performance was evaluated with a particular emphasis on peak capacity, overall resolution, peak distribution and repeatability. The results suggest that a new generation of stationary phases, specifically designed for improved robustness in mixed CO2-methanol mobile phases, can improve peak shape, peak capacity and resolution for all classes of polar analytes. A significant enhancement in chromatographic performance was observed for these urinary metabolites on the majority of the stationary phases when polar additives such as ammonium salts (formate, acetate and hydroxide) were included in the organic modifier, and the use of water or alkylamine additives was found to be beneficial for specific subsets of polar analytes. The utility of these findings was confirmed by the separation of a mixture of polar metabolites in human urine using an optimised 7min gradient SFC method, where the use of the recommended column and co-solvent combination resulted in a significant improvement in chromatographic performance. PMID:27143232

  2. Analysis of epinephrine, norepinephrine, and dopamine in urine samples of hospital patients by micellar liquid chromatography.

    PubMed

    García Ferrer, Daniel; García García, Aurelio; Peris-Vicente, Juan; Gimeno-Adelantado, José Vicente; Esteve-Romero, Josep

    2015-12-01

    An analytical method based on micellar liquid chromatography was developed to determine the concentration of three catecholamines (epinephrine, norepinephrine, and dopamine) in urine. The detection of these compounds in urine can be useful to diagnose several diseases, related to stress and sympathoadrenal system dysfunction, using a non-invasive collection procedure. The sample pretreatment was a simple dilution in a micellar solution, filtration, and direct injection, thus avoiding time-consuming and tedious extraction steps. Therefore, there is no need to use an internal standard. The three catecholamines were eluted using a C18 column and a mobile phase of 0.055 M sodium dodecyl sulfate-1.5% methanol buffered at pH 3.8 running at 1.5 mL/min under isocratic mode in less than 25 min. The detection was performed by amperometry applying a constant potential of +0.5 V. The procedure was validated following the guidelines of the European Medicines Agency in terms of the following: calibration range (0.09-5 μg/mL), linearity (r(2) > 0.9995), limit of detection (0.02 μg/mL), within- and between-run accuracy (-6.5 to +8.4%) and precision (<10.2%), dilution integrity, matrix effect, robustness (<8.4), and stability. The obtained values were below those required by the guide. The method was rapid, easy-to-handle, eco-friendly, and safe and provides reliable quantitative data, and is thus useful for routine analysis. The procedure was applied to the analysis of epinephrine, norepinephrine, and dopamine in urine samples from patients of a local hospital. PMID:26427500

  3. [Application of three-way data analysis (second-order tensor decomposition) algorithms in analysis of liquid chromatography].

    PubMed

    Zhang, Jin; Peng, Qianrong; Xu, Longquan; Yang, Min; Wu, Aijing; Ye, Shizhu

    2014-11-01

    Using dropline separation, tangent skimming, and triangulation to estimate the area of an overlapping chromatographic peak might contribute to a large deviation. It is easy, however, to eliminate these errors caused by geometric segmentation using three-way data analysis (second-order tensor decomposition) algorithms. This method of chromatographic analysis has many advantages: automation, anti-interference, high accuracy in the resolution of overlapping chrom- atographic peaks. It even makes the final goal of analytical chemistry achievable without the aid of complicated separation procedures. The core of this method is the process of utilizing useful information and building models through chemometric algorithms. Three-way chromatographic data set can be divided into trilinear dataset and nontrilinear dataset, correspondingly, three-way data analysis (second-order tensor decomposition) algorithms can be divided into trilinear algorithms and nontrilinear algorithms. In this paper, three-way calibration used in liquid chromatography for complex chemical systems in the last decade is reviewed, and focused on sample pretreatment, auxiliary algorithms, the combination and comparison of correction algorithms. PMID:25764649

  4. Measurement of bubble size distribution in a gas-liquid foam using pulsed-field gradient nuclear magnetic resonance.

    PubMed

    Stevenson, Paul; Sederman, Andrew J; Mantle, Mick D; Li, Xueliang; Gladden, Lynn F

    2010-12-01

    Pulsed-field gradient nuclear magnetic resonance, previously used for measuring droplet size distributions in emulsions, has been used to measure bubble size distributions in a non-overflowing pneumatic gas-liquid foam that has been created by sparging propane into an aqueous solution of 1.5g/l (5.20mM) SDS. The bubble size distributions measured were reproducible and approximated a Weibull distribution. However, the bubble size distributions did not materially change with position at which they were measured within the froth. An analysis of foam coarsening due to Ostwald ripening in a non-overflowing foam indicates that, for the experimental conditions employed, one would not expect this to be a significant effect. It is therefore apparent that the eventual collapse of the foam is due to bubble bursting (or surface coalescence) rather than Ostwald ripening. This surface coalescence occurs because of evaporation from the free surface of the foam. An analytical solution for the liquid fraction profile for a certain class of non-overflowing pneumatic foam is given, and a mean bubble size that is appropriate for drainage calculations is suggested. PMID:20832808

  5. High-Throughput Analysis of Sucrose Fatty Acid Esters by Supercritical Fluid Chromatography/Tandem Mass Spectrometry

    PubMed Central

    Hori, Katsuhito; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-01-01

    Supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry was applied to the profiling of sucrose fatty acid esters (SEs). The SFC conditions (column and modifier gradient) were optimized for the effective separation of SEs. In the column test, a silica gel reversed-phase column was selected. Then, the method was used for the detailed characterization of commercial SEs and the successful analysis of SEs containing different fatty acids. The present method allowed for fast and high-resolution separation of monoesters to tetra-esters within a shorter time (15 min) as compared to the conventional high-performance liquid chromatography. The applicability of our method for the analysis of SEs was thus demonstrated. PMID:26819875

  6. Evaluation of a commercial gas chromatography/matrix isolation-infrared spectrometer for quantitative analysis of priority pollutants

    SciTech Connect

    Schneider, J.F.; Schneider, K.R.; Spiro, S.E.

    1989-10-01

    Gas chromatography/matrix isolation-infrared spectrometry (GC/MI-IR) is being applied to many analyses normally done by gas chromatography/mass spectrometry. Qualitatively, the infrared spectra of matrix-isolated compounds contain much information about their structure. The information obtained from the infrared spectrum is complementary to the information obtained from mass spectrometry. The technique of GC/MI-IR should also be useful as a quantitative detector. In this study, the utility of a commercial GC/MI-IR for quantitative trace organic analysis was evaluated. Results indicate that the reproducibility of the commercial instrument is only suitable for semiquantitative analysis. The precision of the commercial instrument might be improved by redesign of its open-split interface. 12 refs., 39 figs., 9 tabs.

  7. Liquid chromatography-tandem mass spectrometry for the analysis of eicosanoids and related lipids in human biological matrices: a review.

    PubMed

    Kortz, Linda; Dorow, Juliane; Ceglarek, Uta

    2014-08-01

    Today, there is an increasing number of liquid chromatography tandem-mass spectrometric (LC-MS/MS) methods for the analysis of eicosanoids and related lipids in biological matrices. An overview of currently applied LC-MS/MS methods is given with attention to sample preparation strategies, chromatographic separation including ultra high performance liquid chromatography (UHPLC) and chiral separation, as well as to mass spectrometric detection using multiple reacting monitoring (MRM). Further, the application in recent clinical research is reviewed with focus on preanalytical aspects prior to LC-MS/MS analysis as well as applications in major diseases of Western civilization including respiratory diseases, diabetes, cancer, liver diseases, atherosclerosis, and neurovascular diseases. PMID:24583205

  8. Flow Injection Analysis and Liquid Chromatography for Multifunctional Chemical Analysis (MCA) Systems

    ERIC Educational Resources Information Center

    Mayo, Ana V.; Loegel, Thomas N.; Bretz, Stacey Lowery; Danielson, Neil D.

    2013-01-01

    The large class sizes of first-year chemistry labs makes it challenging to provide students with hands-on access to instrumentation because the number of students typically far exceeds the number of research-grade instruments available to collect data. Multifunctional chemical analysis (MCA) systems provide a viable alternative for large-scale

  9. Flow Injection Analysis and Liquid Chromatography for Multifunctional Chemical Analysis (MCA) Systems

    ERIC Educational Resources Information Center

    Mayo, Ana V.; Loegel, Thomas N.; Bretz, Stacey Lowery; Danielson, Neil D.

    2013-01-01

    The large class sizes of first-year chemistry labs makes it challenging to provide students with hands-on access to instrumentation because the number of students typically far exceeds the number of research-grade instruments available to collect data. Multifunctional chemical analysis (MCA) systems provide a viable alternative for large-scale…

  10. Advanced proteomic liquid chromatography

    SciTech Connect

    Xie, Fang; Smith, Richard D.; Shen, Yufeng

    2012-10-26

    Liquid chromatography coupled with mass spectrometry is the predominant platform used to analyze proteomics samples consisting of large numbers of proteins and their proteolytic products (e.g., truncated polypeptides) and spanning a wide range of relative concentrations. This review provides an overview of advanced capillary liquid chromatography techniques and methodologies that greatly improve separation resolving power and proteomics analysis coverage, sensitivity, and throughput.

  11. Search for organics in extraterrestrial environments by in situ gas chromatography analysis

    NASA Astrophysics Data System (ADS)

    Rodier, C.; Sternberg, R.; Szopa, C.; Buch, A.; Cabane, M.; Raulin, F.

    Many organic molecules are present in interstellar clouds and might be carried to the early Earth by comets and meteorites during the heavy bombardment period in the first few hundred million years of the solar system. It has been suggested that extraterrestrial organic material may well represent an important part of the organic material available for the origin of life. This assumption is significantly supported by the study of the Murchison meteorite that revealed more than 500 organic compounds, including several nucleic acid bases and 80 amino acids, 8 of them being proteinaceous. Investigation of extraterrestrial environments therefore appears of primary interest to determine the nature of the organic molecules (either endogenous or exogenous) which could be present on Earth when prebiotic chemistry occurred and life emerged. Until samples brought by future space missions are available on Earth, in situ measurements are the only way to get unaltered samples for analysis. The current most powerful technique for the analysis of organic molecules in extraterrestrial environments is gas chromatography (GC) coupled to mass spectrometry (MS).It was first used in the Viking landers, by the GC-MS experiments which looked for organics on the surface and subsurface of Mars. Viking failed to detect organics at the ppb levels for complex organics. Since the meteorites and interplanetary dust should carry organics to Mars, their absence in the samples analysed by Viking suggests that they are actively destroyed. It is however thought today that organics could be present on the surface at levels below the detection limit of the Viking GC-MS, or that the could be preserved in the Martian subsurface beneath the depth that Viking was able to access. This is why several surface missions are currently planned to investigate Mars to seek again for organics, and GC-MS should be the main experimental device used for this task. Besides Mars, Titan and the comet Churyumov-Gerasimenko will be the next targets for the search for organics by GCMS experiments on board atmospheric (Huygens) and landing probes (Philae of the Rosetta mission). The main objective of this work is to present the capabilities of GC based subsystems, developed in our laboratories for present and future space missions and including sample treatment and capillary column analysis, for the in situ analysis of volatile and refractory organics in atmospheric (Titan) and/or surface or sub-surface samples (Mars, comets).

  12. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.

    1989-01-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan-Cassini entry probe, which is being jointly planned by NASA and the European Space Agency (ESA), might be launched as early as 1994. As in the Pioneer mission, limited time--perhaps only 3-4 h--will be available for the completion of all analyses while the probe descends through the atmosphere. A conventional GC or GC-MS system would be able to analyze no more than two aerosol and two gas samples during the probe's descent. Conventional GC also is limited by the sensitivity of the detector and by the sample volume. For the Titan mission, the sensitivity problems will be worse because the atmospheric pressure at the time of instrument deployment is expected to be < 3 torr. Consequently, the sample volume might not be large enough to satisfy the detector sensitivity requirements. Because of such limitations, alternative GC analysis techniques have been investigated for future NASA missions. Multiplex gas chromatography has been investigated as a possible candidate for chemical analysis within a spacecraft or other restricted environment, and chemical modulators have been developed and used when needed with this technique to reduce the size and weight of the instrumentation. Also, several new multiplex techniques have been developed for use in specific applications.

  13. Chirospecific analysis of plant volatiles

    NASA Astrophysics Data System (ADS)

    Tkachev, A. V.

    2007-10-01

    Characteristic features of the analysis of plant volatiles by enantioselective gas (gas-liquid) chromatography and gas chromatography/mass spectrometry are discussed. The most recent advances in the design of enantioselective stationary phases are surveyed. Examples of the preparation of the most efficient phases based on modified cyclodextrins are given. Current knowledge on the successful analytical resolution of different types of plant volatiles (aliphatic and aromatic compounds and mono-, sesqui- and diterpene derivatives) into optical antipodes is systematically described. Chiral stationary phases used for these purposes, temperature conditions and enantiomer separation factors are summarised. Examples of the enantiomeric resolution of fragrance compounds and components of plant extracts, wines and essential oils are given.

  14. 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.

  15. Liquid chromatography-mass spectrometry analysis of five bisphosphonates in equine urine and plasma.

    PubMed

    Wong, April S Y; Ho, Emmie N M; Wan, Terence S M; Lam, Kenneth K H; Stewart, Brian D

    2015-08-15

    Bisphosphonates are used in the management of skeletal disorder in humans and horses, with tiludronic acid being the first licensed veterinary medicine in the treatment of lameness associated with degenerative joint disease. Bisphosphonates are prohibited in horseracing according to Article 6 of the International Agreement on Breeding, Racing and Wagering (published by the International Federation of Horseracing Authorities). In order to control the use of bisphosphonates in equine sports, an effective method to detect the use of bisphosphonates is required. Bisphosphonates are difficult-to-detect drugs due to their hydrophilic properties. The complexity of equine matrices also added to their extraction difficulties. This study describes a method for the simultaneous detection of five bisphosphonates, namely alendronic acid, clodronic acid, ibandronic acid, risedronic acid and tiludronic acid, in equine urine and plasma. Bisphosphonates were first isolated from the sample matrices by solid-phase extractions, followed by methylation with trimethylsilyldiazomethane prior to liquid chromatography - tandem mass spectrometry analysis using selective reaction monitoring in the positive electrospray ionization mode. The five bisphosphonates could be detected at low ppb levels in 0.5mL equine plasma or urine with acceptable precision, fast instrumental turnaround time, and negligible matrix interferences. The method has also been applied to the excretion study of tiludronic acid in plasma and urine collected from a horse having been administered a single dose of tiludronic acid. The applicability and effectiveness of the method was demonstrated by the successful detection and confirmation of the presence of tiludronic acid in an overseas equine urine sample. To our knowledge, this is the first reported method in the successful screening and confirmation of five amino- and non-amino bisphosphonates in equine biological samples. PMID:26143477

  16. Assessment of oil weathering by gas chromatography-mass spectrometry, time warping and principal component analysis.

    PubMed

    Malmquist, Linus M V; Olsen, Rasmus R; Hansen, Asger B; Andersen, Ole; Christensen, Jan H

    2007-09-14

    Detailed characterization and understanding of oil weathering at the molecular level is an essential part of tiered approaches for forensic oil spill identification, for risk assessment of terrestrial and marine oil spills, and for evaluating effects of bioremediation initiatives. Here, a chemometric-based method is applied to data from two in vitro experiments in order to distinguish the effects of evaporation and dissolution processes on oil composition. The potential of the method for obtaining detailed chemical information of the effects from evaporation and dissolution processes, to determine weathering state and to distinguish between various weathering processes is investigated and discussed. The method is based on comprehensive and objective chromatographic data processing followed by principal component analysis (PCA) of concatenated sections of gas chromatography-mass spectrometry chromatograms containing homologue series of n-alkanes (m/z 85) and alkyltoluenes (m/z 105). The PCA model based solely on in vitro samples and validated by samples from an authentic marine oil spill gives a detailed description of the temporal changes in n-alkane and alkyltoluene compositions. The PCA model is able to distinguish the two physical weathering processes both with respect to removal rate and relative changes. The model shows that evaporation has a large impact on both the alkyltoluenes and on the n-alkanes (e.g., nC-18 is completely removed after 192 days of in vitro evaporation). Dissolution, however, is shown to be a much slower process for weathering of heavy fuel oils with only limited impact on the alkyltoluenes, and no effects on the n-alkane distribution. PMID:17669412

  17. Comparison of different liquid chromatography conditions for the separation and analysis of organotin compounds in mussel and oyster tissue by liquid chromatography-inductively coupled plasma mass spectrometry.

    PubMed

    Wahlen, Raimund; Catterick, Tim

    2003-01-01

    In this paper, a new high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) methodology for the analysis of organotin compounds in complex matrices is described. Earlier studies had failed to show baseline resolution between dibutyltin (DBT) and triphenyltin (TPhT). The data presented in this paper show that, by using a different C-18 stationary phase material (Ace C-18) with decreased particle size, baseline resolution of DBT and TPhT can be achieved, with the resultant separation of a third interfering component. In addition, the Ace C-18 stationary phase yields a significant increase in the number of theoretical plates, and, combined with changes in the mobile phase composition, a reduction in run-time by approximately 25%. It is shown that the minor compounds detected are present in the sample and not artefacts of the analytical procedure. The accuracy and precision of the proposed HPLC-ICP-MS method was demonstrated for the determination of TBT in oyster tissue during the BCR "MULSPOT" international interlaboratory certification project. PMID:12450542

  18. Separation of polychlorobiphenyls from chlorinated pesticides in sediment and oyster samples for analysis by gas chromatography.

    PubMed

    Teichman, J; Bevenue, A; Hylin, J W

    1978-04-11

    Polychlorobiphenyls (PCBs) have been separated from DDT and its analogs and from the other common chlorinated pesticides by adsorption chromatography on columns of alumina and charcoal. Elution from alumina columns with increasing fractional amounts of hexane first isolates dieldrin and heptachlor epoxide from a mixture of chlorinated pesticides and PCBs. The remaining fraction, when added to a charcoal column, can be separated into two fractions, one containing the chlorinated pesticides, the other containing the PCBs, by eluting with acetone-diethyl ether (25:75) and benzene, respectively. The PCBs and the pesticides are then determined by gas chromatography on the separate column eluates without cross interference. The method is applicable to sample extracts prepared for gas chromatography. Recoveries of the PCBs (Aroclors) and the chlorinated pesticides are good and the method is applicable to sediment and marine biota samples. PMID:417089

  19. Impedance Analysis of Colloidal Gold Nanoparticles in Chromatography Paper for Quantitation of an Immunochromatographic Assay.

    PubMed

    Hori, Fumitaka; Harada, Yuji; Kuretake, Tatsumi; Uno, Shigeyasu

    2016-01-01

    A detection method of gold nanoparticles in chromatography paper has been developed for a simple, cost-effective and reliable quantitation of immunochromatographic strip test. The time courses of the solution resistance in chromatography paper with the gold nanoparticles solution are electrochemically measured by chrono-impedimetry. The dependence of the solution resistance on the concentration of gold nanoparticles has been successfully observed. The main factor to increase the solution resistance may be obstruction of the ion transport due to the presence of gold nanoparticles. The existence of gold nanoparticles with 1.92 × 10(9) particles/mL in an indistinctly-colored chromatography paper is also identified by a solution resistance measurement. This indicates that the solution resistance assay has the potential to lower the detection limit of the conventional qualitative assay. PMID:26960618

  20. Description and operating report on the world's first totally offshore NGL (natural gas liquids) facility in operation

    SciTech Connect

    Scheer, T.H.

    1980-01-01

    A description and operating report on the world's first totally offshore NGL (natural gas liquids) facility in operation, the Ardjuna plant operated by Atlantic Richfield Indonesia Inc. for Pertamina P.N., covers the $173.1 million investment cost; estimated $13 million 1979 operating cost; the four compressor stations which compress associated gas to 650 to 750 psig at a present feed rate of 90 million cu ft/day to give 5.7 gpm natural gas liquids recoveries with a propane extraction efficiency of 95%; operating problems of the central plant; the Ardjuna Sakt.

  1. APPLICATIONS OF INFORMATION THEORY AND PATTERN RECOGNITION TO GAS CHROMATOGRAPHY-MASS SPECTROMETRIC ANALYSIS OF TOXIC ORGANIC COMPOUNDS IN AMBIENT AIR

    EPA Science Inventory

    The number of information channels contained in the gas chromatographic, mass spectrometric, and combined gas chromatography-mass spectrometric analysis of 78 toxic organic compounds has been determined. The toxic compounds are those routinely monitored in ambient air samples usi...

  2. Analysis of four pentacyclic triterpenoid acids in several bioactive botanicals with gas and liquid chromatography and mass spectrometry detection.

    PubMed

    Moldoveanu, Serban C; Scott, Wayne A

    2016-01-01

    Several pentacyclic triterpenoid acids including betulinic, oleanolic, and ursolic acids were reported to have health beneficial properties such as antiviral and anti-inflammatory properties, as well as the capability to inhibit "in vitro" the development of various cancer cell types. For this reason betulinic, oleanolic, and ursolic acids are used as neutraceuticals. For the analysis of the pentacyclic triterpenoid acids in complex plant materials, an improved scheme was developed, involving a qualitative screening using silylation and gas chromatography with mass spectrometry analysis, followed by quantitation using a novel liquid chromatography with tandem mass spectrometry procedure. The use of the two methods provides more reliable information regarding the plant materials with unknown composition. Besides betulinic, oleanolic, and ursolic acids that were analyzed, by this procedure a fourth pentacyclic triterpenoid acid was identified and quantitated that was not previously reported to be present in plants. This acid has been identified as 3β-3-hydroxy-lupa-18,20(29)-dien-28-oic acid. The newly identified acid has a structure as a derivative of lupane, although lupane with a double bond in the 18-position was not previously reported as present in plants. The new liquid chromatography with tandem mass spectrometry procedure developed for this study offers a very low limit of quantitation, excellent precision, and robustness. Rosemary was found to contain the largest levels of pentacyclic triterpenoid acids among all the analyzed botanicals. PMID:26549610

  3. Separation of Berberine Hydrochloride and Tetrahydropalmatine and Their Quantitative Analysis with Thin Layer Chromatography Involved with Ionic Liquids

    PubMed Central

    Lu, Jing; Ma, Hong-yan; Zhang, Wei; Ma, Zhi-guo; Yao, Shun

    2015-01-01

    [BMIM]OH was used in mobile and stationary phase of thin layer chromatography (TLC) to analyze berberine hydrochloride and tetrahydropalmatine for the first time. Supported imidazole ionic liquid with hydroxide ion on silica gel (SiO2·Im+·OH−) was synthesized through simple procedure and characterized by Fourier transform infrared spectroscopy (FT-IR), elemental analysis, and scanning electron microscope (SEM). Moreover, on the plates prepared by SiO2·Im+·OH−, the contents of the above alkaloids in the Chinese patent medicine (CPM) of “Stomacheasy” capsule were successfully determined by TLC scanner. The key conditions and chromatographic behaviors were also investigated in detail. According to similar ways, ionic liquids (ILs) also can be used in other planar chromatographies in two modes. This study is expected to be helpful in expanding the application of IL and its bonded silica gel in TLC separation field. PMID:26609463

  4. Gas and liquid chromatography with inductively coupled plasma mass spectrometry detection for environmental speciation analysis — advances and limitations

    NASA Astrophysics Data System (ADS)

    Szpunar, Joanna; McSheehy, Shona; Połeć, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; Łobiński, Ryszard

    2000-07-01

    Recent advances in the coupling of gas chromatography (GC) and high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP MS) and their role in trace element speciation analysis of environmental materials are presented. The discussion is illustrated with three research examples concerning the following topics: (i) development and coupling of multicapillary microcolumn GC with ICP MS for speciation of organotin in sediment and biological tissue samples; (ii) speciation of arsenic in marine algae by size-exclusion-anion-exchange HPLC-ICP MS; and (iii) speciation of cadmium in plant cell cultures by size-exclusion HPLC-ICP MS. Particular attention is paid to the problem of signal identification in ICP MS chromatograms; the potential of electrospray MS/MS for this purpose is highlighted.

  5. Feasibility of thiocarbamate pesticide analysis in apples by supercritical fluid extraction and high-performance liquid chromatography.

    PubMed

    Howard, A L; Braue, C; Taylor, L T

    1993-08-01

    Supercritical fluid extraction produced comparable results with liquid-solid extraction for the analysis of several thiocarbamate pesticides from apples at the 2 ppm spike level. These results were achieved with a simple one-step extraction procedure. The use of diatomaceous earth (Celite, Supelco, Inc.; Bellefonte, PA) served to increase thiocarbamate recoveries by aiding in the immobilization of the aqueous component of the apple matrix. High-performance liquid chromatography coupled with ultraviolet absorbance detection (HPLC-UV) had the most viable means of quantitation when compared with micro-HPLC-sulfur chemiluminescence detection (SCD) and gas chromatography-flame-ionization detection (GC-FID). The small injection volumes used with the micro-HPLC-SCD system made thiocarbamate detection at a spiking level of 2 ppm impossible. SCD did provide, however, valuable qualitative information about the nature of the apple coextractants. PMID:8376544

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

    NASA Astrophysics Data System (ADS)

    Giebel, Brian M.

    2011-12-01

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

  7. Quantitative analysis of urinary glycerol levels for doping control purposes using gas chromatography-mass spectrometry.

    PubMed

    Thevis, Mario; Guddat, Sven; Flenker, Ulrich; Schänzer, Wilhelm

    2008-01-01

    The administration of glycerol to endurance athletes results in an increased fluid retention and improved performance, particularly under hot and humid conditions. Consequently, glycerol is considered relevant for sports drug testing and methods for its detection in urine specimens are required. A major issue in this regard is the natural occurrence of trace amounts of glycerol in human urine, which necessitates a quantitative analysis and the determination of normal urinary glycerol levels under various sporting conditions. A quantitative method was established using a gas chromatography/isotope-dilution mass spectrometry-based approach that was validated with regard to lower limit of detection (0.3 microg mL(-1)), lower limit of quantification (0.9 microg mL(-1)), specificity, linearity (1.0-98.0 microg mL(-1)), intraday and interday precision (<20% at 2.4, 24.1 and 48.2 microg mL(-1)) as well as accuracy (92-110%). Sample aliquots of 20 microL were enriched with five-fold deuterated glycerol, dried and derivatised using N-methyl-trimethylsilyltrifluoroacetamide (MSTFA) before analysis. The established method was applied to a total of 1039 doping control samples covering various sport disciplines (349 endurance samples, 286 strength sport samples, 325 game sport samples and 79 other samples) in- and out-of-competition, which provided quantitative information about the glycerol content commonly observed in elite athletes' urine samples. About 85% of all specimens yielded glycerol concentrations < 20.0 microg mL(-1) and few reached values up to 132.6 microg mL(-1). One further sample, however, was found to contain 2690 microg mL(-1), which might indicate the misuse of glycerol, but no threshold for urinary glycerol concentrations has been established yet due to the lack of substantial data. Based on the results obtained from the studied reference population, a threshold for glycerol levels in urine set at 200 microg mL(-1) is suggested, which provides a tool to doping control laboratories to test for the misuse of this agent in elite and amateur sport. PMID:18708691

  8. Computer code for gas-liquid two-phase vortex motions: GLVM

    NASA Technical Reports Server (NTRS)

    Yeh, T. T.

    1986-01-01

    A computer program aimed at the phase separation between gas and liquid at zero gravity, induced by vortex motion, is developed. It utilizes an explicit solution method for a set of equations describing rotating gas-liquid flows. The vortex motion is established by a tangential fluid injection. A Lax-Wendroff two-step (McCormack's) numerical scheme is used. The program can be used to study the fluid dynamical behavior of the rotational two-phase fluids in a cylindrical tank. It provides a quick/easy sensitivity test on various parameters and thus provides the guidance for the design and use of actual physical systems for handling two-phase fluids.

  9. Dispersed bubble reactor for enhanced gas-liquid-solids contact and mass transfer

    DOEpatents

    Vimalchand, Pannalal; Liu, Guohai; Peng, WanWang; Bonsu, Alexander

    2016-01-26

    An apparatus to promote gas-liquid contact and facilitate enhanced mass transfer. The dispersed bubble reactor (DBR) operates in the dispersed bubble flow regime to selectively absorb gas phase constituents into the liquid phase. The dispersion is achieved by shearing the large inlet gas bubbles into fine bubbles with circulating liquid and additional pumped liquid solvent when necessary. The DBR is capable of handling precipitates that may form during absorption or fine catalysts that may be necessary to promote liquid phase reactions. The DBR can be configured with multistage counter current flow sections by inserting concentric cylindrical sections into the riser to facilitate annular flow. While the DBR can absorb CO.sub.2 in liquid solvents that may lead to precipitates at high loadings, it is equally capable of handling many different types of chemical processes involving solids (precipitates/catalysts) along with gas and liquid phases.

  10. Studies of momentum and energy transfer across wavy gas-liquid interfaces

    NASA Astrophysics Data System (ADS)

    Dukler, A. E.

    1993-06-01

    Two phase gas-liquid flow and its associated interfaces exist in a wide variety of situations of importance to the Navy and this has prompted the study of the basic flow mechanics which underlie this complex process. The existence of wind-wave interactions over large bodies of water have long been recognized as a special case of two phase flow where the presence of the deformable interface plays a complex role in the generation of waves due to the action of the wind. Less well recognized, but of great importance, are situations of two phase flow which are found in component of power systems such as condensers, boiler refrigeration loops, and cryogen lines. Here the characteristics of two phase flow are critical to the reliable design and safe operation of such systems.

  11. Gas-liquid mass transfer characteristics in a bubble column with suspended sparingly soluble fine particles

    SciTech Connect

    Sada, E.; Fujiwara, N.; Kumazawa, M.; Lee, C.

    1985-04-01

    (To investigate the influence of suspended particles on mass transfer characteristics in a slurry bubble column, physical and chemical absorptions were performed into aqueous slurries of fine calcium hydroxide particles ca. 7 ..mu..m in average size. Such mass transfer parameters as volumetric liquid-side mass transfer coefficient, specific gas-liquid interfacial area, and hence liquid-side mass transfer coefficient were determined under various electrolyte concentrations, solid concentrations, and gas flow rates.) and K /SUB L/ /SUP o/ a could be correlated by the gas flow rate. (The volumetric gas-side mass transfer coefficient was determined and correlated by the gas flow rate. The enhancement factors during absorption of dilute carbon dioxide into aqueous calcium hydroxide slurries were compared with the theoretical predictions based on the film theoryincorporating a finite slurry concept.)

  12. Unit operations for gas-liquid mass transfer in reduced gravity environments

    NASA Technical Reports Server (NTRS)

    Pettit, Donald R.; Allen, David T.

    1992-01-01

    Basic scaling rules are derived for converting Earth-based designs of mass transfer equipment into designs for a reduced gravity environment. Three types of gas-liquid mass transfer operations are considered: bubble columns, spray towers, and packed columns. Application of the scaling rules reveals that the height of a bubble column in lunar- and Mars-based operations would be lower than terrestrial designs by factors of 0.64 and 0.79 respectively. The reduced gravity columns would have greater cross-sectional areas, however, by factors of 2.4 and 1.6 for lunar and Martian settings. Similar results were obtained for spray towers. In contract, packed column height was found to be nearly independent of gravity.

  13. Cell stimulus and lysis in a microfluidic device with segmented gas-liquid flow.

    PubMed

    El-Ali, Jamil; Gaudet, Suzanne; Günther, Axel; Sorger, Peter K; Jensen, Klavs F

    2005-06-01

    We describe a microfluidic device with rapid stimulus and lysis of mammalian cells for resolving fast transient responses in cell signaling networks. The device uses segmented gas-liquid flow to enhance mixing and has integrated thermoelectric heaters and coolers to control the temperature during cell stimulus and lysis. Potential negative effects of segmented flow on cell responses are investigated in three different cell types, with no morphological changes and no activation of the cell stress-sensitive mitogen activated protein kinases observed. Jurkat E6-1 cells are stimulated in the device using alpha-CD3, and the resulting activations of ERK and JNK are presented for different time points. Stimulation of cells performed on chip results in pathway activation identical to that of conventionally treated cells under the same conditions. PMID:15924398

  14. Thermal dispersion in vertical gas-liquid flows with foaming and non-foaming liquids

    SciTech Connect

    Pino, L.R.Z.; Saez, A.E.

    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.

  15. 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

  16. Rapid gas-liquid chromatographic method for determination of sulfathiazole in swine feed.

    PubMed

    Munns, R K; Roybal, J E

    1983-03-01

    A gas-liquid chromatographic (GLC) method for determining residues of sulfathiazole (STZ) in swine feed has been developed. Feed is extracted first with acetone and then with ammonia-acetone. STZ is isolated from other feed extractives on a Sephadex LH-20 column with methanol-toluene. The sulfa residues are methylated with diazomethane, and the eluate is evaporated to dryness. A solution containing an internal standard of methyl sulfasymazine is used to dilute the sample before injection onto an OV-25 GLC column. The precision of the method was determined by assaying 10 sets of feed spiked at 0.5, 1, 2, and 5 ppm STZ. The mean recoveries and coefficients of variation were 90.2 (5.90), 89.5 (4.67), 87.4 (5.62), and 87.7% (4.29), respectively. The critical steps of the method, including the stability of STZ, were also determined. PMID:6853414

  17. Rapid gas-liquid chromatographic method for determination of sulfamethazine in swine feed.

    PubMed

    Munns, R K; Roybal, J E

    1982-09-01

    A gas-liquid chromatographic method is described for the quantitative determination of trace amounts of sulfamethazine in swine feed. Sulfamethazine is extracted in ammoniated acetone and isolated from other extractants on a Sephadex LH-20 column. The eluate is methylated with diazomethane and evaporated to dryness. The residue is dissolved in a solvent containing an internal standard of methyl sulfasymazine before being injected onto an OV-25 GLC column. An estimation of precision was established by assaying 10 sets of swine feed fortified with 0.5, 1,2, and 5 ppm SMZ. Mean recoveries were 96.0, 94.3, 93.5, and 94.0%, respectively, with an average coefficient of variation of 3.07%. The critical steps and ruggedness of the method were also determined. PMID:7130074

  18. Gas-liquid phase-transfer catalysis; A new continuous-flow method in organic synthesis

    SciTech Connect

    Tundo, P. ); Moraglio, G.; Trotta, F. )

    1989-07-01

    A synthetic method, gas-liquid phase-transfer catalysis (GL-PTC0), is described. GL-PTC is a continuous-flow procedure where gaseous reagents flow through a molten phase-transfer (PT) catalyst supported on a solid; no solvent is used. Reactions may develop through new mechanistic pathways compared with those of classical conditions; moreover, the reactions often occur in very selective ways. Some typical syntheses carried out under GL-PTC conditions are described in detail. They include syntheses of 2-alkylmalonic acid esters from the corresponding malonic acid esters and primary alkyl halides from primary alkyl alcohols and the reactions of dimethyl carbonate, which give N-methylanilines from anilines, anisoles from phenols, and 2-arylpropionitriles from aryl-acetonitriles.

  19. Bubble size and gas-liquid interfacial area measurements using molten paraffin waxes in bubble columns

    SciTech Connect

    Bukur, D.B.; Patel, S.A.; Daly, J.G.; Raphael, M.L.

    1987-01-01

    Experiments were conducted in 0.05 m ID and 0.23 m ID by 3 m tall bubble columns with different types of molten waxes as the liquid medium and nitrogen as the gas, under processing conditions typical or Fischer-Tropsch synthesis over iron catalysts (i.e. gas velocities up to 0.15 m s, and temperatures between 200 and 270/sup 0/C) to estimate gas liquid interfacial area from measured values of average gas hold-up and Sauter mean bubble diameter. The gas hold-up was estimated from visual observations of the expanded and static liquid heights, and the Sauter was estimated from bubble size measurements obtained by photography and dynamic gas disengagement. The paraffin wax (FT-300) used in the authors' studies is non-coalescing and has a tendency to foam. The amount of foam is greater for runs conducted in the order of increasing gas velocities, than in runs with decreasing velocities. Thus, two values of hold-up are possible and the start-up procedure determines which one will be attained. At higher gas velocities (> 0.05 m/s) the foam disappears and a transition to the slug flow, churn-turbulent regime takes place. Reactor waxes are coalescing in nature and do not produce foam. Despite similar hold-ups for the different waxes at higher gas velocities, the Sauters are significantly different and this is reflected in the specific gas-liquid interfacial areas, with larger values obtained with the paraffin wax compared to values with reactor waxes.

  20. The inactivation of Chlorella spp. with dielectric barrier discharge in gas-liquid mixture

    NASA Astrophysics Data System (ADS)

    Song, Dan; Sun, Bing; Zhu, Xiaomei; Yan, Zhiyu; Liu, Hui; Liu, Yongjun

    2013-03-01

    The inactivation of Chlorella spp. with high voltage and frequency pulsed dielectric barrier discharge in hybrid gas-liquid reactor with a suspension electrode was studied experimentally. In the hybrid gas-liquid reactor, a steel plate was used as high voltage electrode while a quartz plate as a dielectric layer, another steel plate placing in the aqueous solution worked as a whole ground electrode. A suspension electrode is installed near the surface of solution between high voltage and ground electrode to make the dielectric barrier discharge uniform and stable, the discharge gap was between the quartz plate and the surface of the water. The effect of peak voltage, treatment time, the initial concentration of Chlorella spp. and conductivity of solution on the inactivation rate of Chlorella spp. was investigated, and the inactivation mechanism of Chlorella spp. preliminarily was studied. Utilizing this system inactivation of Chlorella spp., the inactivation rate increased with increasing of peak voltage, treatment time and electric conductivity. It was found that the inactivation rate of Chlorella spp. arrived at 100% when the initial concentration was 4 106 cells mL-1, and the optimum operation condition required a peak voltage of 20 kV, a treatment time of 10 min and a frequency of 7 kHz. Though the increasing of initial concentration of the Chlorella spp. contributed to the addition of interaction probability between the Chlorella spp. and O3, H2O2, high-energy electrons, UV radiation and other active substances, the total inactivation number raise, but the inactivation rate of the Chlorella spp. decreased.

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

    PubMed

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

    2013-06-14

    This study focused on an investigation into the experimental quantities inherent in the determination of partition coefficients from gas-liquid chromatographic measurements through the use of capillary columns. We prepared several squalane - (2,6,10,15,19,23-hexamethyltetracosane) - containing columns with very precisely known phase ratios and determined solute retention and hold-up times at 30, 40, 50 and 60°C. We calculated infinite dilution partition coefficients from the slopes of the linear regression of retention factors as a function of the reciprocal of the phase ratio by means of fundamental chromatographic equations. In order to minimize gas-solid and liquid-solid interface contributions to retention, the surface of the capillary inner wall was pretreated to guarantee a uniform coat of stationary phase. The validity of the proposed approach was first tested by estimating the partition coefficients of n-alkanes between n-pentane and n-nonane, for which compounds data from the literature were available. Then partition coefficients of sixteen aliphatic alcohols in squalane were determined at those four temperatures. We deliberately chose these highly challenging systems: alcohols in the reference paraffinic stationary phase. These solutes exhibited adsorption in the gas-liquid interface that contributed to retention. The corresponding adsorption constant values were estimated. We fully discuss here the uncertainties associated with each experimental measurement and how these fundamental determinations can be performed precisely by circumventing the main drawbacks. The proposed strategy is reliable and much simpler than the classical chromatographic method employing packed columns. PMID:23659974

  2. 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.

  3. Foam formation and mitigation in a three-phase gas-liquid-particulate system.

    PubMed

    Vijayaraghavan, Krishna; Nikolov, Alex; Wasan, Darsh

    2006-11-16

    Foaming is of great concern in a number of industrial processes involving three-phase gas-liquid-finely divided solid systems such as those encountered in the vitrification of highly radioactive nuclear waste slurries and sludges. Recent work has clearly shown that the surface properties of the particles such as hydrophilicity, hydrophobicity or biphilicity (i.e. partially wetted by water) are the cause of foamability and foam stability. The literature data on particles causing foaminess and foam stability in the absence of any surfactant are rather scarce. This paper presents experimental observations on aqueous foams with polyhedral structures containing over 90% air generated due to the presence of irregularly-shaped fine crystalline particles of sodium chloride which were modified into amphiphilic particles by physical adsorption of a cationic surfactant. Cross-polarized light microscopy was used to visualize the physical adsorption of the surfactant on the crystal surface. It is shown that these biphilic or amphiphilic particles attach to the air bubble surface and prevent the coalescence of bubbles, thereby extending the life of the foam. The foaming power of solid particles increases with an increase in the concentration of amphiphilic particles, and a maximum in foaminess is observed which is due to two competing effects. Amphiphilic particles promote foamability by attachment to the bubble surfaces as individual particles and foam inhibition due to the clustering or flocculation of particles in the bulk at high particle concentrations. We studied the adsorption of amphiphilic particles at a planar air-water surface and found that the degree of foamability correlates well with the particle coverage (i.e. adsorption density) at the air-liquid surface. An exploratory study was also conducted using an antifoam recently developed by IIT researchers to mitigate foaming in particle-laden gas-liquid systems. PMID:16997269

  4. Electrochemical detection coupled with high-performance liquid chromatography in pharmaceutical and biomedical analysis: a mini review.

    PubMed

    Wang, Chengyin; Xu, Jianyun; Zhou, Guiyou; Qu, Qishu; Yang, Gongjun; Hu, Xiaoya

    2007-08-01

    Recent advances in electrochemical detection techniques coupled with high-performance liquid chromatography (HPLC-ECD) in pharmaceutical and biomedical analysis are reviewed. ECD classification and modes including common amperometric, coulometric, conductimetric, and potentiometric detector, are outlined and the some typical examples of determinations in pharmaceutical and biomedical analysis are described. The electrochemical detection system can offer superior merits over other detectors commonly used with HPLC. These techniques have great potential owing to their prominent characteristics in high-throughput screening procedures of drugs in various matrices. Fundamental 67 references from last 5 years related with a field are cited in this review. PMID:17979637

  5. Ultraperformance ion-pairing liquid chromatography with on-line electrospray ion trap mass spectrometry for heparin disaccharide analysis

    PubMed Central

    Yang, Bo; Weyers, Amanda; Baik, Jong Youn; Sterner, Eric; Sharfstein, Susan; Mousa, Shaker A.; Zhang, Fuming; Dordick, Jonathan S.; Linhardt, Robert J.

    2011-01-01

    A high resolution method for the separation and analysis of disaccharides prepared from heparin and heparan sulfate (HS) using heparin lyases is described. Ultraperformance liquid chromatography in a reverse-phase, ion-pairing mode efficiently separates eight heparin/HS disaccharides. The disaccharides can then be detected and quantified using electrospray ionization mass spectrometry. This method is particularly useful in the analysis of small amounts of biological samples, including cells, tissues and biological fluids, as it provides high sensitivity without being subject to interference from proteins, peptides and other sample impurities. PMID:21530482

  6. Qualitative Analysis by Gas Chromatography: GC versus the Nose in Formulating Artificial Fruit Flavors.

    ERIC Educational Resources Information Center

    Rasmussen, P. W.

    1984-01-01

    Describes an undergraduate laboratory experiment used to illustrate the use of gas chromatography retention indices for the identification of unknown compounds, specifically for the identification of unknown compounds and for the identification of the volatile compounds responsible for the odor of the banana. Procedures, reference data, and sample…

  7. 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...

  8. 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)

  9. 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…

  10. (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...

  11. Qualitative Analysis by Gas Chromatography: GC versus the Nose in Formulating Artificial Fruit Flavors.

    ERIC Educational Resources Information Center

    Rasmussen, P. W.

    1984-01-01

    Describes an undergraduate laboratory experiment used to illustrate the use of gas chromatography retention indices for the identification of unknown compounds, specifically for the identification of unknown compounds and for the identification of the volatile compounds responsible for the odor of the banana. Procedures, reference data, and sample

  12. 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 ...

  13. 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

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

    PubMed

    Lísa, Miroslav; Holčapek, 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 μm 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

  15. Application of micellar electrokinetic capillary chromatography to forensic analysis of barbiturates in biological fluids.

    PubMed

    Ferslew, K E; Hagardorn, A N; McCormick, W F

    1995-03-01

    Micellar electrokinetic capillary chromatography (MECC) is a form of capillary zone electrophoresis. Addition of a surfactant produces micelles in an aqueous/organic buffer. Separation of drugs is obtained via differences in the electrophoretic mobilities of the analytes within the capillary, resulting from their electrophoretic velocity and the electroosmotic flow of the buffer in a given electric field. The migration order is determined by the differential partitioning of the drugs between the micelles and the aqueous/organic phase. Barbiturates were extracted from various biological fluids at pH 4.5 with TOXI-TUBES B. MECC analyses were performed using a Waters Quanta 4000 Capillary Electrophoretic System with a 745 Data Module with a 75 microns x 60 cm capillary and an aqueous/organic buffer of 85% 10 mM borate, 10 mM phosphate, 100 mM sodium dodecyl sulfate and 15% acetonitrile at a pH of 8.5 with a voltage of 20 kV using ultraviolet absorption detection at 214 nm. Migration times were: phenobarbital, 7.78 min.; butalbital, 8.01 min.; butabarbital, 8.23 min.; mephobarbital (internal standard), 8.88 min.; amobarbital, 9.41 min.; pentobarbital, 10.03 min. and secobarbital, 10.79 min. Correlation coefficients (r) between peak areas and concentration ranges of 3 to 60 micrograms/mL were from 0.964 to 0.999. Coefficients of variation (CV) ranged from 2.6 to 8.6% between days and 2.3 to 9.8% within day. Application of this methodology to four forensic cases of butalbital intoxication detected concentrations of 0.7 to 12.7 micrograms/mL in blood; 0.8 to 1.9 micrograms/mL in vitreous humor and 1.5 to 7.6 micrograms/mL in urine. MECC is applicable to forensic analysis of barbiturates extracted from biological fluids. PMID:7602286

  16. Benchmarking of candidate detectors for multiresidue analysis of pesticides by comprehensive two-dimensional gas chromatography.

    PubMed

    Engel, Erwan; Ratel, Jérémy; Blinet, Patrick; Chin, Sung-Tong; Rose, Gavin; Marriott, Philip J

    2013-10-11

    The present study discusses the relevance, performance and complementarities of flame photometric detector in phosphorus (FPD/P) and sulfur (FPD/S) modes, micro electron capture detector (μECD), nitrogen phosphorus detector (NPD), flame ionization detector (FID) and time-of-flight mass spectrometer (TOF/MS) for the comprehensive two-dimensional gas chromatography (GC×GC) analysis of pesticides. A mix of 41 pesticides including organophosphorus pesticides, synthetic pyrethroids and fungicides was investigated in order to benchmark GC×GC systems in terms of linearity (R(2)), limits of detection (LOD), and peak shape measures (widths and asymmetries). A mixture of pesticides which contained the heteroatoms phosphorus, sulfur, nitrogen and one or several halogens, was used to acquire a comparative data set to monitor relative detector performances. GC×GC datasets were systematically compared to their GC counterpart acquired with an optimized one-dimensional GC configuration. Compared with FID, considered the most appropriate detector in terms of suitability for GC×GC, the element-selective detector FPD/P and μECD best met the peak widths (0.13-0.27s for FPD/P; 0.22-0.26s for μECD) and tailing factors (0.99-1.66 for FPD/P; 1.32-1.52 for μECD); NPD exhibited similar peak widths (0.23-0.30s), but exceeded those of the above detectors for tailing factors (1.97-2.13). These three detectors had improved detection limits of 3-7 times and 4-20 times lower LODs in GC×GC mode compared with FID and TOF-MS, respectively. In contrast FPD/S had poor peak shape (tailing factor 3.36-5.12) and much lower sensitivity (10-20 fold lower compared to FPD/P). In general, element-selective detectors with favorable detection metrics can be considered viable alternatives for pesticide determination using GC×GC in complex matrices. The controversial issue of sensitivity enhancement in GC×GC was considered for optimized GC and GC×GC operation. For all detectors, we found no significant LOD enhancement in GC×GC. PMID:24011509

  17. Analysis of chemical profiles of insect adhesion secretions by gas chromatography-mass spectrometry.

    PubMed

    Reitz, Manuela; Gerhardt, Heike; Schmitt, Christian; Betz, Oliver; Albert, Klaus; Lämmerhofer, Michael

    2015-01-01

    This article reports on the chemical analysis of molecular profiles of tarsal secretions of the desert locust Schistocerca gregaria (Forsskål, 1775) by gas chromatography hyphenated with quadrupol mass spectrometry (GC-MS) as well as (1)H-nuclear magnetic resonance ((1)H NMR) spectroscopy. Special focus of this study was to elaborate on sampling methods which enable selective microscale extraction of insect secretions in a spatially controlled manner, in particular tarsal adhesive secretions and secretions located on cuticle surfaces at the tibia. Various solvent sampling procedures and contact solid-phase microextraction (SPME) methods were compared in terms of comprehensiveness and extraction efficiencies as measured by signal intensities in GC-MS. Solvent sampling with water as extraction solvent gave access to the elucidation of chemical profiles of polar compound classes such as amino acids and carbohydrates, but is extremely tedious. Contact SPME on the other hand can be regarded as a simplified and more elegant alternative, in particular for the lipophilic compound fraction. Many proteinogenic amino acids and ornithine as well as carbohydrate monomers arabinose, xylose, glucose, and galactose were detected in tarsal secretions after acid hydrolysis of aqueous extracts. Qualitatively similar but quantitatively significantly different molecular profiles were found for the lipid fraction which contained mainly n-alkanes and internally branched monomethyl-, dimethyl-, and trimethyl-alkanes in the C23-C49 range as well as long chain fatty acids and aldehydes. Especially, hydrocarbons with >C40 carbon numbers have previously been rarely reported for insect secretions. The results suggest that the investigated insect secretions are complex emulsions which allow the attachment of tarsi on various otherwise incompatible materials of smooth and rough surfaces. The solid consistence of the established alkanes at ambient temperatures might contribute to a semi-solid consistence of the adhesive, amalgamating partly opposing functions such as slip resistance, tarsal release, desiccation resistance, and mechanical compliance. The methods developed can be extended to other similar applications of studying compositions of insect secretions of other species. PMID:25479867

  18. 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 μm 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

  19. Classification of gas-liquid flow patterns by the norm entropy of wavelet decomposed pressure fluctuations across a bluff body

    NASA Astrophysics Data System (ADS)

    Sun, Zhiqiang; Chen, Yanping; Gong, Hui

    2012-12-01

    Identification of gas-liquid flow patterns remains one of the paramount needs in multiphase flow metering. It is hardly possible to realize accurate measurement and control of parameters in a gas-liquid flow system without a clear understanding of its flow pattern. Here we explore the characterization of gas-liquid flow patterns using the norm entropy extracted from the wavelet decomposed pressure fluctuations across a bluff body. Experiments on air-water two-phase flow at ambient temperature and atmospheric pressure are carried out in the bubble, plug, slug and annular flow patterns. On the basis of the experimental results, two original flow-pattern maps are constructed: one is coordinated with the average norm entropy versus the total mass flow rate, and the other is the average norm entropy versus the volumetric void fraction. Verification tests demonstrate that the overall identification rates of the flow-pattern maps developed exceed 95%. This approach provides an effective and simple solution to the classification of gas-liquid flow patterns.

  20. 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

    ... 40 Protection of Environment 22 2013-07-01 2013-07-01 false Default Factors for Petroleum Products and Natural Gas Liquids 1 2 MM Table MM-1 to Subpart MM of Part 98 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) MANDATORY GREENHOUSE GAS REPORTING Suppliers of Petroleum Products Pt. 98, Subpt....

  1. 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

    ... 40 Protection of Environment 22 2012-07-01 2012-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  2. Separation of Delta5- and Delta7-phytosterols by adsorption chromatography and semipreparative reversed phase high-performance liquid chromatography for quantitative analysis of phytosterols in foods.

    PubMed

    Zhang, Xin; Cambrai, Amandine; Miesch, Michel; Roussi, Stamatiki; Raul, Francis; Aoude-Werner, Dalal; Marchioni, Eric

    2006-02-22

    A method for the separation, isolation, and identification of phytosterols was developed. A commercial phytosterols mixture, Generol 95S, was fractionated first by adsorption silica gel column chromatography and then separated by means of a semipreparative reverse phase high-performance liquid chromatography fitted with a Polaris C8-A column (250 mm x 10 mm i.d., 5 microm) using isocratic acetonitrile:2-propanol:water (2:1:1, v/v/v) as the mobile phase. Milligram scales of six individual phytosterols, including citrostadienol, campesterol, beta-sitosterol, Delta7-avenasterol, Delta7-campesterol, and Delta7-sitosterol, were obtained. Purities of these isolated sterols were 85-98%. Relative response factors (RRF) of these phytosterols were calculated against cholestanol as an authentic commercial standard. These RRF values were used to quantify by gas chromatography-mass spectrometry (GC-MS) the phytosterols content in a reference material, oils, and chocolates. PMID:16478236

  3. 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

  4. Development of capillary size exclusion chromatography for the analysis of monoclonal antibody fragments extracted from human vitreous humor.

    PubMed

    Rea, Jennifer C; Lou, Yun; Cuzzi, Joel; Hu, Yuhua; de Jong, Isabella; Wang, Yajun Jennifer; Farnan, Dell

    2012-12-28

    Recombinant antigen-binding fragments (Fabs) are currently on the market and in development for the treatment of ophthalmologic indications. Recently, Quality by Design (QbD) initiatives have been implemented that emphasize understanding the relationship between quality attributes of the product and their impact on safety and efficacy. In particular, changes in product quality once the protein is administered to the patient are of particular interest. Knowledge of protein aggregation in vivo is of importance due to the possibility of antibody aggregates eliciting an immunogenic response in the patient. Presently, there are few analytical methods with adequate sensitivity to analyze Fab aggregates in human vitreous humor (HVH) because the Fab amount available for analysis is often quite low. Here, we report the development of a highly sensitive capillary size exclusion chromatography (SEC) methodology for Fab aggregate analysis in HVH. We demonstrate a process to perform capillary SEC to analyze Fabs with picogram sensitivity and an RSD of less than 8% for the relative peak area of high molecular weight species (HMWS). In addition, we have developed a Protein G affinity chromatography method to capture Fabs from HVH for capillary SEC analysis. Recovery efficiencies ranging from 86 to 99% were achieved using this recovery method with 300 μL HVH samples containing Fab1. Finally, we demonstrate the applicability of the methodology by quantifying Fab aggregates in HVH, which can potentially be used for aggregate analysis of clinically relevant samples. PMID:23177154

  5. High-performance liquid chromatography with fluorescence detection for the rapid analysis of pheophytins and pyropheophytins in virgin olive oil.

    PubMed

    Li, Xueqi; Woodman, Michael; Wang, Selina C

    2015-08-01

    Pheophytins and pyropheophytin are degradation products of chlorophyll pigments, and their ratios can be used as a sensitive indicator of stress during the manufacturing and storage of olive oil. They increase over time depending on the storage condition and if the oil is exposed to heat treatments during the refining process. The traditional analysis method includes solvent- and time-consuming steps of solid-phase extraction followed by analysis by high-performance liquid chromatography with ultraviolet detection. We developed an improved dilute/fluorescence method where multi-step sample preparation was replaced by a simple isopropanol dilution before the high-performance liquid chromatography injection. A quaternary solvent gradient method was used to include a fourth strong solvent wash on a quaternary gradient pump, which avoided the need to premix any solvents and greatly reduced the oil residues on the column from previous analysis. This new method not only reduces analysis cost and time but shows reliability, repeatability, and improved sensitivity, especially important for low-level samples. PMID:26047465

  6. Thin-layer chromatography and colorimetric analysis of multi-component explosive mixtures

    DOEpatents

    Pagoria, Philip F.; Mitchell, Alexander R.; Whipple, Richard E.; Carman, M. Leslie

    2014-08-26

    A thin-layer chromatography method for detection and identification of common military and peroxide explosives in samples includes the steps of provide a reverse-phase thin-layer chromatography plate; prepare the plate by marking spots on which to deposit the samples by touching the plate with a marker; spot one micro liter of a first standard onto one of the spots, spot one micro liter of a second standard onto another of the spots, and spot samples onto other of spots producing a spotted plate; add eluent to a developing chamber; add the spotted plate to the developing chamber; remove the spotted plate from the developing chamber producing a developed plate; place the developed plate in an ultraviolet light box; add a visualization agent to a dip tank; dip the developed plate in the dip tank and remove the developed plate quickly; and detect explosives by viewing said developed plate.

  7. Pyrolysis analysis of the herbicide paraquat on cannabis by coupled gas chromatography-infrared spectroscopy.

    PubMed

    Beutler, J A; Varano, A; DerMarderosian, A

    1979-10-01

    Pyrolysis gas chromatography coupled with infrared identification of eluted peaks confirms that paraquat is pyrolyzed into chloromethane and 4,4'-dipyridyl at smoking temperatures and above. This reaction occurs at 610 degrees C to completion in small amounts in an inert atmosphere. The toxicity of 4,4'-dipyridyl remains to be determined. Pyrolysis of contaminated marijuana also produces the same two products, although detection at low limits is difficult with this procedure. PMID:541644

  8. Signal analysis of NEMS sensors at the output of a chromatography column

    SciTech Connect

    Bertholon, François; Harant, Olivier; Bourlon, Bertrand; Gerfault, Laurent; Grangeat, Pierre; Jutten, Christian

    2015-01-13

    This article introduces a joined Bayesian estimation of gas samples issued from a gas chromatography column (GC) coupled with a NEMS sensor based on Giddings Eyring microscopic molecular stochastic model. The posterior distribution is sampled using a Monte Carlo Markov Chain and Gibbs sampling. Parameters are estimated using the posterior mean. This estimation scheme is finally applied on simulated and real datasets using this molecular stochastic forward model.

  9. Recent trends in the liquid chromatography-mass spectrometry analysis of organic contaminants in environmental samples.

    PubMed

    Petrovic, Mira; Farré, Marinella; de Alda, Miren Lopez; Perez, Sandra; Postigo, Cristina; Köck, Marianne; Radjenovic, Jelena; Gros, Merixell; Barcelo, Damia

    2010-06-18

    An overview of liquid chromatography-mass spectrometry methods used for the determination of trace organic contaminants in environmental samples is presented. Among the organic contaminants the focus is given on five groups of emerging contaminants that raised most concern as environmental contaminants and therefore attracted attention of a research community: pharmaceuticals, drugs of abuse, polar pesticides, perfluorinated compounds and nanoparticles. Various aspects of current LC-MS methodology, using tandem and hybrid MS instruments, including sample preparation, are discussed. PMID:20334864

  10. A simple, inexpensive thin-layer chromatography method for the analysis of theophylline tablets.

    PubMed Central

    Flinn, P. E.; Juhl, Y. H.; Layloff, T. P.

    1989-01-01

    A simple, low-cost thin-layer chromatography (TLC) procedure to estimate the quality of simple pharmaceuticals in tablet form is described together with easily built equipment to carry out the test in the field. The approach is demonstrated for theophylline, but can be used to assay the drug content of any tablet or to determine its dissolution or disintegration characteristics. The procedure can be used in the field without the need for any instrumentation. PMID:2611977

  11. 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

  12. Direct numerical simulation of the near-field dynamics of annular gas-liquid two-phase jets

    NASA Astrophysics Data System (ADS)

    Siamas, George A.; Jiang, Xi; Wrobel, Luiz C.

    2009-04-01

    Direct numerical simulation has been used to examine the near-field dynamics of annular gas-liquid two-phase jets. Based on an Eulerian approach with mixed fluid treatment, combined with an adapted volume of fluid method and a continuum surface force model, a mathematical formulation for the flow system is presented. The swirl introduced at the jet nozzle exit is based on analytical inflow conditions. Highly accurate numerical methods have been utilized for the solution of the compressible, unsteady, Navier-Stokes equations. Two computational cases of gas-liquid two-phase jets including swirling and nonswirling cases have been performed to investigate the effects of swirl on the flow field. In both cases the flow is more vortical at the downstream locations. The swirling motion enhances both the flow instability resulting in a larger liquid spatial dispersion and the mixing resulting in a more homogeneous flow field with more evenly distributed vorticity at the downstream locations. In the annular nonswirling case, a geometrical recirculation zone adjacent to the jet nozzle exit was observed. It was identified that the swirling motion is responsible for the development of a central recirculation zone, and the geometrical recirculation zone can be overwhelmed by the central recirculation zone leading to the presence of the central recirculation region only in the swirling gas-liquid case. Results from a swirling gas jet simulation were also included to examine the effect of the liquid sheet on the flow physics. The swirling gas jet developed a central recirculation region, but it did not develop a precessing vortex core as the swirling gas-liquid two-phase jet. The results indicate that a precessing vortex core can exist at relatively low swirl numbers in the gas-liquid two-phase flow. It was established that the liquid greatly affects the precession and the swirl number alone is an insufficient criterion for the development of a precessing vortex core.

  13. 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 (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  14. Simultaneous Analysis and Quantification of Markers of Manjisthadi Churna Using High Performance Thin Layer Chromatography

    PubMed Central

    Patel, V. R.; Patel, R. K.

    2013-01-01

    Manjisthadi churna has been traditionally used in the Ayurvedic system of medicine and by traditional medical practices of India to treat hyperlipidemia. A rapid, simple and accurate method with high performance thin layer chromatography has been developed to standardised Manjisthadi churna using rubiadin, sennoside and ellagic acid as markers. Methanol extract of Manjisthadi churna were used for high performance thin layer chromatography on silica gel plates. The Rf of rubiadin, sennoside-A and ellagic acid were found to 0.48, 0.23 and 0.72, respectively with densitometric scanning at 280 nm and the calibration plot were linear in the range of 100-600 ng of markers. The correlation coefficients were higher than 0.99 were indicative of good linear dependence of peaks area on concentration. The rubiadin, sennoside-A and ellagic acid contents in Manjisthadi churna were found to be 0.014, 0.038 and 0.534% w/w, respectively. This method permits reliable quantification of rubiadin, sennoside-A and ellagic acid with good resolution and separation of the same from other constitutes of the extract of Manjisthadi churna. Recovery value from 95.66-102.33% showed the reliability and reproducibility of the method. The proposed high performance thin layer chromatography method for simultaneous quantification of markers in Manjisthadi churna can be used for routine quality testing. PMID:23901170

  15. Affinity Chromatography.

    ERIC Educational Resources Information Center

    Gray, Gary R.

    1980-01-01

    Presents selected recent advances in immobilization chemistry which have important connections to affinity chromatography. Discusses ligand immobilization and support modification. Cites 51 references. (CS)

  16. Precolumn sample-enrichment device for analysis of ambient volatile organics by gas chromatography-mass spectrometry

    SciTech Connect

    Arnts, R.R.

    1985-01-01

    Gas chromatographic-mass spectrometric (GC/MS) identification of air pollutants generally requires a preconcentration step to provide sufficient sample for analysis. Cryogenic trapping is often used to enrich the sample since nitrogen and oxygen are not condensed. It does, however, concentrate enormous quantities of water and carbon dioxide - enough to plug high-resolution narrow-bore capillary columns needed for separation of complex environmental samples. Whole-air samples were collected in stainless steel containers or Tedlar bags for analysis by gas chromatography with flame ionization detection (GC/FID). In order to provide identification of unknown peaks and confirmation of tentatively named peaks, the system described herein was designed and built to enrich samples for GC/MS analysis of volatile organics. The preconcentration system consists of a solid sorbent trap and a cryogenic trap used in sequence to collect organic vapors and focus them for analysis by GC/MS.

  17. Quantum-state resolved reaction dynamics at the gas-liquid interface: Direct absorption detection of HF(v,J) product from F(2P)+squalane

    NASA Astrophysics Data System (ADS)

    Zolot, Alexander M.; Harper, Warren W.; Perkins, Bradford G.; Dagdigian, Paul J.; Nesbitt, David J.

    2006-07-01

    Exothermic reactive scattering of F atoms at the gas-liquid interface of a liquid hydrocarbon (squalane) surface has been studied under single collision conditions by shot noise limited high-resolution infrared absorption on the nascent HF (v,J) product. The nascent HF (v,J) vibrational distributions are inverted, indicating insufficient time for complete vibrational energy transfer into the surface liquid. The HF (v=2,J) rotational distributions are well fit with a two temperature Boltzmann analysis, with a near room temperature component (TTD≈290K) and a second much hotter scattering component (THDS≈1040K). These data provide quantum state level support for microscopic branching in the atom abstraction dynamics corresponding to escape of nascent HF from the liquid surface on time scales both slow and fast with respect to rotational relaxation.

  18. Diode-laser-based optical rotation detector for high-performance liquid chromatography and on-line polarimetric analysis

    SciTech Connect

    Lloyd, D.K.; Goodall, D.M.; Scrivener, H. )

    1989-06-01

    A simple polarimeter with microdegree sensitivity based on a near-infrared (820 nm) semiconductor diode laser is described, and signal to noise ratio analysis is discussed. With the use of small-volume flow cells (typically 8 {mu}L) its utility as a high-performance liquid chromatography (HPLC) detector in the gradient elution separation of carbohydrates is shown. Coupled with a UV detector, the HPLC enantiomeric purity determination of D-/L-tryptophan mixtures without chiral separation is demonstrated. On a laboratory-scale system an application from the sugar industry is reported, monitoring molasses flow streams which are opaque at visible wave-lengths.

  19. 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

  20. Chromatography, Absorption, and Fluorescence: A New Instrumental Analysis Experiment on the Measurement of Polycyclic Aromatic Hydrocarbons in Cigarette Smoke

    NASA Astrophysics Data System (ADS)

    Wingen, Lisa M.; Low, Jason C.; Finlayson-Pitts, Barbara J.

    1998-12-01

    The recent approval by the American Chemical Society of an undergraduate chemistry degree with an option in environmental chemistry requires the development of new experiments that teach fundamental chemistry in the context of environmental issues. We present an experiment suitable for an undergraduate junior/senior-level instrumental analysis laboratory which illustrates the principles of high-performance liquid chromatography (HPLC) and its application to the identification and measurement of polycyclic aromatic hydrocarbons (PAH) in tobacco smoke. Absorption and fluorescence detection methods for PAH, especially the differences in sensitivity and selectivity of these methods, are clearly demonstrated along with the basic principles of HPLC.

  1. 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.

  2. Qualitative drug analysis of hair extracts by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.

    PubMed

    Guthery, Bill; Bassindale, Tom; Bassindale, Alan; Pillinger, Colin T; Morgan, Geraint H

    2010-06-25

    A technique using comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GCxGC/TOFMS) is applied to a qualitative analysis of three sample extracts from hair suspected of containing various drug compounds. The samples were also subjected to a quantitative target analysis for codeine, morphine, 6-monoacetylmorphine (6-MAM), amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethylamphetamine (MDMA), methadone, and benzylpiperazine (BZP) by liquid chromatography-tandem mass spectrometry (LC-MS/MS). GCxGC/TOFMS provided a non-specific procedure that identified various drugs, metabolites, and impurities not included in the target analysis. They included cocaine, diazepam, and methaqualone (quaalude). Comprehensive GCxGC separation was achieved using twin-stage cryo-modulation to focus eluant from a DB-5 ms (5% phenyl) to a BPX50 (50% phenyl) GC column. The TOF mass spectrometer provided unit mass resolution in the mass range m/z 5-1000 and rapid spectral acquisition (< or = 500spectra/s). Clean mass spectra of the individual components were obtained using mass spectral deconvolution software. The 'unknown' components were identified by comparison with mass spectra stored in a library database. PMID:20471020

  3. Highly sensitive and selective analysis of widely targeted metabolomics using gas chromatography/triple-quadrupole mass spectrometry.

    PubMed

    Tsugawa, Hiroshi; Tsujimoto, Yuki; Sugitate, Kuniyo; Sakui, Norihiro; Nishiumi, Shin; Bamba, Takeshi; Fukusaki, Eiichiro

    2014-01-01

    In metabolomics studies, gas chromatography coupled with time-of-flight or quadrupole mass spectrometry has frequently been used for the non-targeted analysis of hydrophilic metabolites. However, because the analytical platform employs the deconvolution method to extract single-metabolite information from co-eluted peaks and background noise, the extracted peak is artificial product depending on the mathematical parameters and is not completely compatible with the pure component obtained by analyzing a standard compound. Moreover, it has insufficient ability for quantitative metabolomics. Therefore, highly sensitive and selective methods capable of pure peak extraction without any complicated mathematical techniques are needed. For this purpose, we have developed a novel analytical method using gas chromatography coupled with triple-quadrupole mass spectrometry (GC-QqQ/MS). We developed a selected reaction monitoring (SRM) method to analyze the trimethylsilyl derivatives of 110 metabolites, using electron ionization. This methodology enables us to utilize two complementary techniques-non-targeted and widely targeted metabolomics in the same sample preparation protocol, which would facilitate the formulation or verification of novel hypotheses in biological sciences. The GC-QqQ/MS analysis can accurately identify a metabolite using multichannel SRM transitions and intensity ratios in the analysis of living organisms. In addition, our methodology offers a wide dynamic range, high sensitivity, and highly reproducible metabolite profiles, which will contribute to the biomarker discoveries and quality evaluations in biology, medicine, and food sciences. PMID:23867096

  4. [Analysis of C4 fluoride compounds in alkylation materials by gas chromatography/flame ionization detection (GC/FID)].

    PubMed

    Han, Jianghua; Yang, Haiying

    2004-09-01

    A method for the analysis of C4 fluoride compounds in alkylation materials was developed by GC/FID. In order to confirm the presence of C4 fluoride compounds in alkylation materials, 1-fluorobutane, 2-fluorobutane and 2-fluoro-2-methylpropane were synthesized and analysed by GC/FID, gas chromatography/atomic emission detection (GC/AED) and gas chromatography/mass spectrometry (GC/MS). The results showed that only 2-fluoro-2-methylpropane existed in the alkylation materials. Based on the properties of element response on GC/AED, the calibration factors of C4 fluoride compounds on GC/FID were calculated. The analysis was performed on OV-225 (50 m x 0.25 mm i. d. x 0.25 microm) and SE-54 (44 m x 0.22 mm i. d. x 0.25 microm) columns, which were connected in series. FID was used as the detector. In quantitative analysis of the alkylation materials the methods of calibration normalization and indirect external standard were suggested. The calibration curves were linear (r = 0.992) in the concentration range of 156 - 700 microL/L. The minimum detection limit of 2-fluoro-2-methylpropane in real samples was 150 microL/L (S/N = 3). The method is simple, reproducible and easy to be applied. The other components in the alkylation materials can also be analyzed if the calibration normalization method is used. PMID:15706940

  5. Analysis of Whiskey by Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography/Mass Spectrometry: An Upper Division Analytical Chemistry Experiment Guided by Green Chemistry

    ERIC Educational Resources Information Center

    Owens, Janel E.; Zimmerman, Laura B.; Gardner, Michael A.; Lowe, Luis E.

    2016-01-01

    Analysis of whiskey samples prepared by a green microextraction technique, dispersive liquid-liquid microextraction (DLLME), before analysis by a qualitative gas chromatography-mass spectrometry (GC/MS) method, is described as a laboratory experiment for an upper division instrumental methods of analysis laboratory course. Here, aroma compounds in…

  6. Analysis of Whiskey by Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography/Mass Spectrometry: An Upper Division Analytical Chemistry Experiment Guided by Green Chemistry

    ERIC Educational Resources Information Center

    Owens, Janel E.; Zimmerman, Laura B.; Gardner, Michael A.; Lowe, Luis E.

    2016-01-01

    Analysis of whiskey samples prepared by a green microextraction technique, dispersive liquid-liquid microextraction (DLLME), before analysis by a qualitative gas chromatography-mass spectrometry (GC/MS) method, is described as a laboratory experiment for an upper division instrumental methods of analysis laboratory course. Here, aroma compounds in

  7. Gas Chromatography.

    ERIC Educational Resources Information Center

    Karasek, Francis W.; And Others

    1984-01-01

    This review covers fundamental developments in gas chromatography during 1982 and 1983. Literature is considered under these headings: columns; liguid phases; solid supports; sorption processes and solvents; open tubular column gas chromatography; instrumentation; high-resolution columns and applications; other techniques; qualitative and…

  8. 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.

  9. Developments in suppressor technology for inorganic ion analysis by ion chromatography using conductivity detection.

    PubMed

    Hadda, Paul R; Jackson, Peter E; Shaw, Matthew J

    2003-06-01

    A review is presented detailing the development and use of suppression devices for the conductimetric detection of inorganic ions by ion chromatography (IC). An overview of the general response equation for conductivity detection is also given. Topics of discussion include the role and function of suppressors, the development of early suppressors including packed column and membrane devices from 1975 to 1990 and the subsequent progression towards present day commercially available suppressors and recent innovations. Post-suppression devices for signal enhancement are also discussed. PMID:12877197

  10. Analysis of doxylamine in plasma by high-performance liquid chromatography.

    PubMed

    Kohlhof, K J; Stump, D; Zizzamia, J A

    1983-08-01

    A rapid and sensitive high-performance liquid chromatographic (HPLC) assay for the quantitative determination of doxylamine in plasma is described. The drug levels of doxylamine in plasma were monitored after the oral administration of a single 25-mg tablet of doxylamine succinate to each of 20 male volunteers. The compound was extracted from the plasma samples, concentrated under a nitrogen stream, and analyzed by HPLC using normal-phase chromatography with detection at 254 nm. The detection limit is approximately 5 ng/ml. PMID:6620159

  11. Direct transesterification of lipids in mammalian tissue for fatty acid analysis via dehydration with 2,2'-dimethoxypropane.

    PubMed

    Shimasaki, H; Phillips, F C; Privett, O S

    1977-07-01

    A method is described for the transesterification of lipids of mammalian tissues for fatty acid analysis by gas-liquid chromatography (GLC) that eliminates the extraction step of conventional procedures. The method involves the direct reaction of anhydrous HCl-methanol with the lipids in approximately 10 mg of tissue or 0.1 ml of serum after removal of water by reacting it with 2,2'-dimethoxypropane (DMP). Acetone and methanol produced from water in the sample, as well as the excess DMP, are evaporated prior to transesterification in order to eliminate the formation of artifacts from the solvents. The method was demonstrated with rat serum and brain tissue. PMID:894145

  12. Gas chromatography in space

    NASA Technical Reports Server (NTRS)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  13. Advanced proteomic liquid chromatography

    PubMed Central

    Xie, Fang; Smith, Richard D.; Shen, Yufeng

    2012-01-01

    Liquid chromatography coupled with mass spectrometry is the predominant platform used to analyze proteomics samples consisting of large numbers of proteins and their proteolytic products (e.g., truncated polypeptides) and spanning a wide range of relative concentrations. This review provides an overview of advanced capillary liquid chromatography techniques and methodologies that greatly improve separation resolving power and proteomics analysis coverage, sensitivity, and throughput. PMID:22840822

  14. Supercritical Fluid Chromatography as an Alternative Tool for the Qualitative and Quantitative Analysis of Metarhizium brunneum Metabolites from Culture Broth.

    PubMed

    Taibon, Judith; Sturm, Sonja; Seger, Christoph; Werth, Marion; Strasser, Hermann; Stuppner, Hermann

    2015-12-01

    A fast and selective ultrahigh-performance supercritical fluid chromatography photodiode array detector method was established for the qualitative and quantitative analysis of destruxins, cyclic hexadepsipeptides, from fungal culture broth samples. Prior to analysis, sample purification was carried out using an off-line solid-phase extraction protocol on a reversed-phase material in order to remove unwanted matrix constituents. For separation, detection, and identification, an ultrahigh-performance supercritical fluid chromatography photodiode array detector system hyphenated to a triple quadrupole mass spectrometer was utilized. Analyses were performed on an Acquity ethylene bridged hybrid 2-ethylpyridine sub 2 µm particle size column with CO2 and an acidified (0.02 % trifluor acetic acid) modifier mixture of methanol/acetonitrile (8/2 v/v) serving as mobile phase. For the optimal separation of destruxins, the amount of the modifier was increased in a 10 min linear gradient from 2 % to 20 %, and the column outlet pressure and temperature was set at 140 bars and 60 °C, respectively. Seventeen analytes were separated within an elution window of 4 minutes. Five destruxin congeners (destruxin A, destruxin B, destruxin D, destruxin E, and destruxin E-diol) were identified using reference material. Additionally, eight analytes were tentatively assigned as known destruxins by the evaluation of mass spectrometry data performed as multiple reaction monitoring experiments in the positive electrospray ionization mode. PMID:26366754

  15. 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

  16. 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

  17. Analysis of Essential Oil in Jerusalem Artichoke (Helianthus tuberosus L.) Leaves and Tubers by Gas Chromatography-Mass Spectrometry

    PubMed Central

    Helmi, Zead; Al Azzam, Khaldun Mohammad; Tsymbalista, Yuliya; Ghazleh, Refat Abo; Shaibah, Hassan; Aboul-Enein, Hassan

    2014-01-01

    Purpose: To investigate, for the first time, the chemical composition of essential oil of the tubers and leaves of Jerusalem artichoke (Helianthus tuberosus L.), a species of sunflower native to eastern North America, growing in Ukraine. Methods: A hydrodistillation apparatus was used for the extraction of volatile components and then it was analysed by gas chromatography equipped with a split-splitless injector (split ratio, 1:50) and flame ionization detector (FID). The oil was analyzed under linear temperature programming applied at 4°C/min from 50°C - 340°C. Temperatures of the injector and FID detector were maintained at 280°C and 300°C, respectively. The chemical analysis of the oil was carried out using gas chromatography coupled to mass spectrometry (GC-MS), to determine the chemical composition of the volatile fraction. Results: The essential oils content ranged from 0.00019 to 0.03486 and 0.00011 to 0.00205 (g/100g), in leaves and tubers, respectively. The qualitative and quantitative analysis led to the identification of 17 components in both species samples. The major component found in leaves and tubers was (-)-β-bisabolene with 70.7% and 63.1%, respectively. Conclusion: Essential oil profile of Jerusalem artichoke species showed significant differences between leaves and tubers species. Additionally, the leaves of Jerusalem artichoke are a promising source of natural β-bisabolene. PMID:25671184

  18. 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

  19. Direct analysis of oligomeric tackifying resins in rubber compounds by automatic thermal desorption gas chromatography/mass spectrometry

    PubMed

    Kim

    1999-01-01

    Two analytical methods, automatic thermal desorption gas chromatography/mass spectrometry (ATD-GC/MS) and pyrolysis gas chromatography/mass spectrometry (Py-GC/MS), were applied as direct methods for the analysis of oligomeric tackifying resins in a vulcanized rubber. The ATD-GC/MS method, based on discontinuous volatile extraction, was found to be an effective means for direct analysis of the oligomeric tackifying resins contained in a vulcanized rubber. The oligomeric tackifying resins, such as t-octylphenolformaldehyde (TOPF) resin, rosin-modified terpene resin, and cashew resin, could be directly analyzed in vulcanized rubber by ATD-GC/MS. Much simpler total ion chromatograms were obtained by ATD-GC/MS than by flash pyrolysis with a Curie-point pyrolyzer, permitting much easier interpretation. Ions at m/z 206, 135, and 107 were fingerprints in the characteristic mass spectra obtained by ATD-GC/MS for TOPF resin in the vulcanized rubber. 1H-Indene, styrene, and isolongifolene were observed as their characteristic mass spectra in the pyrolyzate of the rosin-modified terpene resin. From the cashew resin, phenol, 3-methylphenol, and 4-(1,1,3, 3-tetramethylbutyl)phenol were obtained as the characteristic pyrolyzates by discontinuous thermal extraction via ATD-GC/MS. Copyright 1999 John Wiley & Sons, Ltd. PMID:10589102

  20. Application of integrated comprehensive/multidimensional gas chromatography with mass spectrometry and olfactometry for aroma analysis in wine and coffee.

    PubMed

    Chin, Sung-Tong; Eyres, Graham T; Marriott, Philip J

    2015-10-15

    Component coelution in chromatographic analysis complicates identification and attribution of individual odour-active volatile molecules in complex multi-component samples. An integrated system incorporating comprehensive two-dimensional gas chromatography (GC × GC) and multidimensional gas chromatography (MDGC), with flame ionisation, olfactometry and mass spectrometry detection was developed to circumvent data correlation across different systems. Identification of potent odorants in Shiraz wine and the headspace of ground coffee are demonstrated as selected applications. Multiple solid-phase microextraction (SPME) sampling with GC-O located odour-active regions; GC × GC established the complexity of odour-active regions; MDGC provided high-resolution separation for each region; simultaneous 'O' and MS detection completed the analysis for target resolved peaks. Seven odour regions in Shiraz were analysed with MDGC-O/MS detection, revealing 11 odour volatiles through matching of mass spectrometry and retention indices from both separating dimensions, including acetic acid; octen-3-ol; ethyl octanoate; methyl-2-oxo-nonanoate; butanoic acid, 2-methylbutanoic acid, and 3-methylbutanoic acid; 3-(methylthio)-1-propanol; hexanoic acid; β-damascenone; and ethyl-3-phenylpropanoate. A capsicum odour in ground coffee was identified as 2-methoxy-3-isobutylpyrazine with a 5-fold increase in S/N of the odorant when acquired using a 6-time cumulative SPME sampling approach. PMID:25952879