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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. Analysis of lipids by gas-liquid chromatography and complementary methods in four strains of Aedes aegypti mosquitoes.

    PubMed

    Miller, S; Novak, R J

    1985-01-01

    Fatty acid composition of total lipids, neutral lipids and phospholipids of strains of Aedes aegypti were determined. The fatty acid composition of the strains differed quantitatively with regard to the relative percentage of commonly occurring fatty acids. Gas-liquid chromatography of fatty acid methyl esters showed 18:1 (oleic or elaidic) to be the predominant fatty acid. The fatty acid was identified as oleic by argentation thin-layer chromatography. A modified colorimetric method was used to determine tissue-free fatty acids. The lipids were predominantly triacylglycerol with lesser amounts of free fatty acids and decreasing amount of sterol ester, sterol, monoacylglycerol, diacylglycerol and hydrocarbons. The data show considerable lipid differences between the Caribbean strains (Les Cayes, Haiti, and San Juan, Puerto Rico) and the Jakarta (Indonesia) strain. The Shimba Hills (Kenya) strain was more similar to Jakarta than to the Caribbean strains. The results obtained with the different strains are discussed in relation to the established oral susceptibility to Dengue 1 and Dengue 2, yellow fever, and genetic analysis by isoenzyme studies. PMID:4017543

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

    PubMed

    1997-10-01

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

  5. 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

  6. 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... pressure. The device may include accessories such as columns, gases, column supports, and liquid...

  7. Modified extraction procedure for gas-liquid chromatography applied to the identification of anaerobic bacteria.

    PubMed Central

    Thomann, W R; Hill, G B

    1986-01-01

    Chloroform and ether commonly are used as solvents to extract metabolic organic acids for analysis by gas-liquid chromatography in the identification of anaerobic bacteria. Because these solvents are potentially hazardous to personnel, modified extraction procedures involving the use of a safer solvent, methyl tert-butyl ether were developed which remained both simple to perform and effective for organism identification. PMID:3700623

  8. 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

  9. 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.

  10. 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).

  11. 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.

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

    PubMed

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

    2011-01-01

    The method of determination of acrylamide in various food (milk powder, potato chips, instant coffee) by gas-liquid chromatography after pre-bromination was developed. Studies have shown the possibility of using bromination of acrylamide to give it the necessary properties for better extraction, purification and detection. Also revealed the possibility of qualitative and quantitative determine a acrylamide in food by gas-liquid chromatography with detection by electron capture detector. PMID:22232888

  13. Rapid presumptive identification of anaerobes in blood cultures by gas-liquid chromatography.

    PubMed Central

    Sondag, J E; Ali, M; Murray, P R

    1980-01-01

    Production of volatile and nonvolatile metabolic acids in blood culture broths by aerobic, facultative anaerobic, and obligate anaerobic bacteria was analyzed by gas-liquid chromatography. Anaerobic blood culture isolates were presumptively identified by the qualitative analysis of volatile fatty acids. Isolates, with a characteristic Gram stain reaction and cellular morphology, were identified by the following acid patterns: Bacteriodes fragilis group with acetic and propionic acids; Fusobacterium with acetic, butyric, and usually propionic acids; Veillonella with acetic and propionic acids; gram-positive cocci with acetic and butyric acids; and Clostridium with acetic and butyric acids. PMID:7381002

  14. Use of prototype automated blood culture system and gas-liquid chromatography for the analysis of continuous ambulatory peritoneal dialysis associated infection.

    PubMed Central

    Catchpole, C R; Macrae, F; Brown, J D; Palmer, M; Healing, D E; Richards, N T; Elliott, T S

    1997-01-01

    AIMS: (1) To compare the recovery of organisms from continuous ambulatory peritoneal dialysis (CAPD) effluent fluid obtained from patients with clinical evidence of peritonitis, with an automated system (AS) and the Septichek blood culture system; (2) to evaluate the times to detection of organisms with the two systems; (3) to identify anaerobes from CAPD samples by extended anaerobic culture and gas-liquid chromatography (GLC). METHODS: 168 CAPD effluent fluid samples were studied, representing 157 episodes of peritonitis in 97 patients. CAPD samples were inoculated into two AS bottles-one anaerobic, one aerobic-and a Septichek bottle; samples were also examined for cell count, Gram stain, and direct culture. Culture bottles were then subcultured onto various media, and any organisms isolated were identified. After routine culture, GLC was performed on culture fluid in the anaerobic AS and Septichek bottles. When volatile fatty acids were detected, the broths were cultured anaerobically on specialised medium for a further five days. RESULTS: 147 organisms were isolated from the 168 samples: 96 (57%) yielded growth of significant organisms by direct culture, as compared to 129 (76.8%) by both AS and Septichek. There was no significant difference in isolation rates between AS and Septichek, but time to detection was more rapid with the AS system (p < 0.002). GLC showed volatile fatty acid in 15 specimens; of these, 14 subsequently grew anaerobic organisms. CONCLUSIONS: AS was comparable to Septichek for numbers of isolations. Speed to detection was faster with the AS, which may be an advantage in management of patients with CAPD peritonitis. GLC showed anaerobes in several cases which would not have been detected without prolonged anaerobic culture; thus anaerobic cultures are recommended for patients who are unresponsive to antimicrobials or who have evidence of bowel perforation. PMID:9155676

  15. Preparation of fatty acid methyl esters for gas-liquid chromatography[S

    PubMed Central

    Ichihara, Ken'ichi; Fukubayashi, Yumeto

    2010-01-01

    A convenient method using commercial aqueous concentrated HCl (conc. HCl; 35%, w/w) as an acid catalyst was developed for preparation of fatty acid methyl esters (FAMEs) from sterol esters, triacylglycerols, phospholipids, and FFAs for gas-liquid chromatography (GC). An 8% (w/v) solution of HCl in methanol/water (85:15, v/v) was prepared by diluting 9.7 ml of conc. HCl with 41.5 ml of methanol. Toluene (0.2 ml), methanol (1.5 ml), and the 8% HCl solution (0.3 ml) were added sequentially to the lipid sample. The final HCl concentration was 1.2% (w/v). This solution (2 ml) was incubated at 45°C overnight or heated at 100°C for 1–1.5 h. The amount of FFA formed in the presence of water derived from conc. HCl was estimated to be <1.4%. The yields of FAMEs were >96% for the above lipid classes and were the same as or better than those obtained by saponification/methylation or by acid-catalyzed methanolysis/methylation using commercial anhydrous HCl/methanol. The method developed here could be successfully applied to fatty acid analysis of various lipid samples, including fish oils, vegetable oils, and blood lipids by GC. PMID:19759389

  16. 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)

  17. Estimation of chlorpyriphos and cypermethrin residues in chilli (Capsicum annuum L.) by gas-liquid chromatography.

    PubMed

    Jyot, Gagan; Mandal, Kousik; Battu, R S; Singh, Balwinder

    2013-07-01

    Dissipation of chlorpyriphos and cypermethrin in chilli was studied following three applications of a combination formulation of Nurelle-D 505 (chlorpyriphos 50% + cypermethrin 5%) at 1 and 2 L ha(-1) at an interval of 15 days. Residues of chlorpyriphos and cypermethrin in chilli were estimated by gas-liquid chromatography and confirmed by gas chromatography-mass spectrometry. Half-life periods for chlorpyriphos were found to be 4.43 and 2.01 days, whereas for cypermethrin these values were observed to be 2.51 and 2.64 days at single and double the application rates, respectively. Residues of chlorpyriphos dissipated to more than 80% after 10 days at both the dosages. However, residues of cypermethrin dissipated to the extent of more than 70% in 7 days. Soil samples collected after 15 days of the last application did not show the presence of chlorpyriphos and cypermethrin at their respective determination limit of 0.01 mg kg(-1). The use of chlorpyriphos and cypermethrin mixture at the recommended dosage does not seem to pose any hazards to the consumers, and a waiting period of 1 day is suggested to reduce the risk before consumption of green chilli. PMID:23114920

  18. Preparation of sphingolipid fatty acid methyl esters for determination by gas-liquid chromatography.

    PubMed

    MacGee, J; Williams, M G

    1981-01-30

    Sphingolipid fatty acids are first converted to a mixture of free acids and their n-butyl esters by heating the specimen at 85 degree C in aqueous butanolic hydrogen chloride; the butyl esters are then saponified with methanolic potassium hydroxide. After acidification and extraction into hexane, the fatty acids are extracted into a very small volume of aqueous trimethyl(m-trifluorotolyl)ammonium hydroxide (TMTFTH), injection of an aliquot of the TMTFTH extract into the gas chromatograph yields the fatty acid methyl esters by pyrolytic methylation of the quaternary ammonium salts of the fatty acids. The preparation of a specimen ready for the gas--liquid chromatographic (GLC) analysis with quantitative recovery of the sphingolipid fatty acids can be accomplished in less than 2 h. By comparison, none of a number of well-accepted techniques for the release of sphingomyelin fatty acids by hydrolysis or methanolysis released the fatty acids quantitatively in less than 3 h, and all required additional manipulations before GLC analysis. PMID:7217267

  19. Identification of Neisseria by electron capture gas-liquid chromatography of metabolites in a chemically defined growth medium.

    PubMed Central

    Morse, C D; Brooks, J B; Kellogg, D S

    1977-01-01

    A dual-purpose study was carried out in an attempt to develop a rapid, sensitive method to identify Neisseria species by gas chromatography and to learn more about the metabolism of these organisms. Sixty-nine isolates of Neisseria were grown in a chemically defined fluid medium; the spent medium was extracted sequentially at pH 2 with diethyl ether and at pH 10 with chloroform. The pH 10 extracts were derivatized with heptafluorobutyric anhydride and analyzed by electron capture gas-liquid chromatography. The resulting spent culture medium electron capture gas-liquid chromatography profiles showed several qualitative and significant quantitative differences among the Neisseria species potentially useful in separating and identifying these organisms. Putrescine and cadaverine which were present in the spent culture medium of some Neisseria, including N. gonorrhoeae, were tentatively identified. Substituting carbohydrates for the chemically defined medium containing glucose in the base medium produced altered profiles with increased quantitative and qualitative differences. PMID:21889

  20. 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.

  1. Rapid determination of dipicolinic acid in the spores of Clostridium species by gas-liquid chromatography.

    PubMed Central

    Tabor, M W; MacGee, J; Holland, J W

    1976-01-01

    A gas-liquid chromatographic procedure has been developed to quantitate dipicolinic acid in bacterial spores. The culture, washed from a plate, was hydrolyzed with acid containing the internal standard, pyridine-2,4-dicarboxylate, and then extracted into methyl isobutyl ketone. The internal standard and dipicolinic acid were then extracted into a small volume of trimethylphenylammonium hydroxide. Injection of the resultant quaternary ammonium salts into a gas chromatograph yielded, via thermal decomposition, the methyl ester derivatives of the dipicolinic acid and the internal standard. The amount of dipicolinic acid in the sample was determined from a standard curve. The method was sensitive to 100 ng of dipicolinic acid per sample and was 1,000 to 5,000 times more sensitive than the commonly used methods. Preparation of the sample required less than 1.5 h and less than 15 min of the analyst's time. PMID:942206

  2. Direct estimation of carbaryl by gas liquid chromatography with nitrogen phosphorus detection.

    PubMed

    Battu, Raminderjit Singh; Mandal, Kousik; Urvashi; Pandher, Suneet; Takkar, Reenu; Singh, Balwinder

    2012-07-01

    A simple and efficient analytical method was standardized for the estimation of residues of carbaryl in various substrates comprising grape berries, kinnow pulps, kinnow rind and soil. The samples were refluxed using mixture of methanol: 0.5 N HCl (1:1 v/v); diluted with brine solution, partitioned into chloroform and dried over anhydrous sodium sulfate. Further the samples were treated with anhydrous magnesium sulfate and primary secondary amine. Final clear extracts were concentrated under vacuum and reconstituted the volume into acetone. The residues were estimated directly on gas liquid chromatograph equipped with nitrogen phosphorus detection system equipped with a capillary column packed with 5 % diphenyl 95 % dimethyl polysiloxane non-polar phase. A consistent recovery from 82 % to 97 % for carbaryl was observed when samples were spiked at levels ranging from 0.05 to 1.00 mg kg(-1). The limit of quantification of the method was worked out to be 0.05 mg kg(-1) for grape berries, kinnow pulp, kinnow rind and soil. PMID:22487961

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

    EPA Science Inventory

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

  4. The determination of methionine in proteins by gas-liquid chromatography.

    PubMed Central

    Ellinger, G M; Duncan, A

    1976-01-01

    Intact methionine residues in proteins were rapidly and precisely determined by measuring methyl thiocyanate released during the reaction with CNBr and separated by g.l.c. Conditions for the reaction and for chromatography on columns of Porapak P-S are described. The recovery of methyl thiocyanate from several methionine derivatives and analogues were examined. Carbamoylmethionine was adopted as a stable primary standard and ethyl thiocyanate as internal standard. The measured methionine content of several isolated proteins was close to the theoretical value indicated by previous work and the results for these and a range of food proteins agreed well with results obtained by ion-exchange chromatography after performic acid oxidation. Since CNBr does not react with methionine sulphoxide and a preliminary hydrolysis is not required, the method discriminates between methionine and any methionine sulphoxide that may be present. It could be useful in studies on the nutritional availability of methionine in processed foods. PMID:949322

  5. 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

  6. Gas chromatography-mass spectrometry in the investigation of on-column dehydration of steroid hormones during gas-liquid chromatography.

    PubMed

    Trafford, D J; Coldwell, R D; Makin, H L

    1991-01-01

    Some underivatized steroids when injected onto conventional packed columns for gas-liquid chromatography underwent varying degrees of dehydration. This problem was traced to the presence of small pieces of broken glass on the top of the column at the point of injection. This observation provoked an examination of the effect of pre-column dehydration on a number of different types of steroids. Powdered aluminium was placed in the injection liner of a Hewlett-Packard gas chromatograph fitted with an HP1 capillary column connected to a mass selective detector, and injections were made using a new high temperature septumless injection system at temperatures between 200 and 400 degrees C. 5 alpha-androstan-3 alpha-ol, a simple monofunctional C19 steroid chosen as a model to establish optimum conditions, underwent dehydration at injection temperatures greater than 250 degrees C and the product reached a maximum at 400 degrees C when no unchanged steroid was present. Monohydroxylated androgens and oestrogens underwent dehydration at 400 degrees C producing products whose mass spectra indicated they were monenes, although the position of the double bond could not be assigned. Polyfunctional androgens and oestrogens and corticosteroids underwent complex changes producing a number of products some of whose structures could not be determined. The dehydration products had the advantage that they had relatively intense high mass ions and for suitable steroids this might provide enhanced sensitivity of detection during mass fragmentography. In such cases dehydration was reproducible and straight line standard curves were obtained. C27 and C28 secosteroids (vitamins D2 and D3) and some of their metabolites (e.g. 25-hydroxyvitamin D) underwent efficient dehydration, again producing products with intense molecular ions. In the case of 24,25-dihydroxyvitamin D3 and 25,26-dihydroxyvitamin D3, dehydration produced different products which were easily resolved in the chromatographic

  7. 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

  8. 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

  9. Determination by gas-liquid chromatography of trace amounts of soft polyvinyl chloride plastic additives in aqueous solutions. I. Epoxidized vegetable oils.

    PubMed

    Smistad, G; Waaler, T; Roksvaag, P O

    1989-01-01

    A gas-liquid chromatographic method for the determination of epoxidized vegetable oils (EVO), such as epoxidized soybean oil and epoxidized linseed oil, in aqueous solutions is described. The EVOs are extracted with n-hexane and transesterified to the methyl esters by sodium methoxide in methanol. 3% OV-210 is used as the stationary phase. The weakest standard solution corresponds to 5 micrograms/l (5 ppb) of EVO in an aqueous sample. The reproducibility of a single analysis is 5%. The method is used for the determination of EVO in intravenous fluids stored in flexible polyvinyl chloride bags. PMID:2597333

  10. Efficiency of buffered aqueous carboxylic acid solutions and organic solvents to absorb SO/sub 2/ from industrial flue gas; solubility data from gas-liquid chromatography

    SciTech Connect

    Sanza, G.J.

    1982-01-01

    Nine adsorbents were examined. These potential candidates for flue gas desulfurization included 1-methyl-2-pyrrolidinone, tri-n-butyl phosphate (TBP), both 0.5 M and 1.0 M solutions of citric acid and glycolic acid, buffered to pH's of 4.5 and 3.8, and pure water. Infinite dilution activity coefficients of SO/sub 2/ were obtained by gas-liquid chromatography in a trial solvent of Nitrobenzene, and then in systems of 1-methyl-2-pyrrolidinone and TBP, independently. The solubility data of SO/sub 2/ was derived and found to be comparable to data obtained from a classical bubble-sparger apparatus. Solubility data was then programmed into an absorber-stripper computer simulator in order to calculate the various concentration and temperature profiles that would exist, the degree of desulfurization, and the steam consumption for all nine systems. Concentrated solutions of citric acid buffered to a low pH exhibited the most favorable conditions for application in direct steam regeneration processes. 1-methyl-2-pyrrolidinone yielded better performance than TBP did with high-pressure indirect steam used for stripping. Comparison between the aqueous solution systems which employed direct steam, and the organic systems which used indirect steam was inconclusive.

  11. 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.

  12. 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.

  13. 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

  14. 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

  15. 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.

  16. Assay of glyceryl trinitrate, isosorbide dinitrate, and their metabolites in plasma by large-bore capillary column gas-liquid chromatography.

    PubMed

    Booth, B P; Bennett, B M; Brien, J F; Elliott, D A; Marks, G S; McCans, J L; Nakatsu, K

    1990-11-01

    Two large-bore capillary columns, one with dimethyl polysiloxane (HP-1) as the stationary phase and the other with phenyl (50 per cent) methyl (50 per cent) polysiloxane (DB-17), were used to develop gas-liquid chromatographic (GLC) assays for measuring isosorbide dinitrate (ISDN), glyceryl trinitrate (GTN), and their metabolites. ISDN, isosorbide-2-mononitrate (2-ISMN), and isosorbide-5-mononitrate (5-ISMN) in plasma, ranging in concentration from 1 to 300 nM, and GTN, glyceryl-1,2-dinitrate (1,2-GDN), and glyceryl-1,3-dinitrate (1,3-GDN), ranging in concentration from 3 to 60 nM in plasma, were analysed on both columns. GLC analysis yielded baseline resolution of the analytes. The method using the dimethyl polysiloxane column gave a lower limit of detectability for GTN of 0.75 nM (signal/noise (s/n) = 2), and the procedure using the phenyl-methyl column provided a lower limit of detectability for ISDN of 81 pM (s/n = 2). The large-bore column GLC procedures exhibited shorter retention times for both ISDN and GTN than those previously reported for capillary-column assays. The chromatographic resolution of analytes and column efficiency of the large-bore capillary columns were comparable to the results previously found using capillary-column GC. The assays for ISDN and GTN have been shown to be appropriate for pharmacokinetic studies in volunteers and patients. We determined that the HP-1 column is appropriate for the analysis of GTN and metabolites, and the DB-17 column is suitable for analysis of ISDN and its metabolites. We conclude that the use of large-bore capillary columns provides rapid and reliable GLC assays for organic nitrates. PMID:2125512

  17. 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

  18. Characterization by gas-liquid chromatography-mass spectrometry and proton-magnetic-resonance spectroscopy of pertrimethylsilyl methyl glycosides obtained in the methanolysis of glycoproteins and glycopeptides.

    PubMed

    Kamerling, J P; Gerwig, G J; Vliegenthart, J F; Clamp, J R

    1975-12-01

    The quantitative analysis by gas chromatography of monosaccharides present in glycoproteins and glycopeptides using methanolysis, followed by re-N-acetylation and trimethylsilylation, gives rise to several peaks for each monosaccharide. The identity of these peaks for xylose, fucose, mannose, galactose, glucose, N-acetylglucosamine, N-acetylgalactosamine and N-acetylneuraminic acid was established for alpha- and beta-methyl pyranosides and furanosides by combined g.l.c.-mass spectrometry and proton-magnetic-resonance spectroscopy. These data provide for the unambiguous interpretation of the gas chromatograms obtained in the application of this g.l.c. method, and supply basic information for the further application of mass spectrometry in this field. PMID:1218089

  19. Qualitative and quantitative evaluation of mono- and disaccharides in D-fructose, D-glucose and sucrose caramels by gas-liquid chromatography-mass spectrometry. Di-D-fructose dianhydrides as tracers of caramel authenticity.

    PubMed

    Ratsimba, V; García Fernández, J M; Defaye, J; Nigay, H; Voilley, A

    1999-06-01

    The monosaccharide (D-fructose, D-glucose, anhydrosugars), disaccharide (glucobioses) and pseudodisaccharide (di-D-fructose dianhydrides) content of D-fructose, D-glucose and sucrose caramels has been determined by gas-liquid chromatography-mass spectrometry (GLC-MS) of their trimethylsilyl (TMS) or TMS-oxime derivatives. The chromatographic profiles revealed significant differences in the disaccharide/pseudodisaccharide distribution depending on the caramel source: a D-fructose caramel contains prominent proportions of di-D-fructose dianhydrides, a D-glucose caramel mainly D-glucobioses, and a sucrose caramel similar proportions of both disaccharide/pseudodisaccharide series. It is noteworthy that di-D-fructose dianhydrides are found in all three types of caramels and might then be used as specific tracers of the authenticity of caramel, i.e., a product resulting from the controlled heat treatment of food-grade carbohydrates for use as food additives. PMID:10399331

  20. In vitro oxidation of i.v. lipid emulsions in different all-in-one admixture bags assessed by an iodometric assay and gas-liquid chromatography.

    PubMed

    Steger, P J; Mühlebach, S F

    1997-02-01

    Polyunsaturated fatty acids (FAs) of intravenous (IV) lipid emulsions can peroxidize to potentially harmful lipid hydroperoxides. In order to assess in vitro peroxidation of IV fat emulsions in all-in-one (AIO) admixture bags, an iodometric titration to determine lipid hydroperoxide content expressed by the peroxide value (PV) and a gas-liquid chromatographic (GLC) assay to determine changes of the FA pattern were established. A long-chain triglyceride (LCT) and medium-chain triglyceride-LCT emulsion were compared for the PV and the pH during storage at room temperature and daylight in AIO bags made of ethylvinylacetate (EVA) and polypropylene:polyamide 7:3 (V90). In contrast to storage in glass bottles, significant peroxidation was detected in both emulsions with 0.5-3.4 mmol peroxides/L after 28 d (150 times the control PV). A pH drop of at least 0.3 (EVA) and 1.2 (V90) units was measured. Initial PVs and peroxidation kinetics of the emulsions were different; V90 material showed better barrier properties against oxygen. PV was increased by higher temperature and light exposure. The FA pattern of an LCT emulsion with a PV > 6 (storage: 40 degrees C in a dark room for 28 d in AIO bags) assayed by GLC remained unchanged. The iodometric peroxide and the GLC assay were reproducible and easy to handle. Only the iodometric method was sensitive enough to detect peroxidation effects (detection limit: 0.02 mmol peroxides/L). IV fat emulsions can be checked for lipid hydroperoxide content with the rapid iodometric assay to guarantee optimal quality of IV lipids used for AIO admixtures. To prevent peroxidation, lipids in AIO bags should be stored light-protected in a refrigerator an oxygen-tight overwrap is mandatory for extended periods. PMID:9106791

  1. 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%.

  2. 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

  3. 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

  4. Determination of solute partition behavior with room-temperature ionic liquid based micellar gas-liquid chromatography stationary phases using the pseudophase model.

    PubMed

    Lantz, Andrew W; Pino, Verónica; Anderson, Jared L; Armstrong, Daniel W

    2006-05-19

    The use of micelles in ionic liquid based gas-chromatography stationary phases was evaluated using equations derived for a "three-phase" model. This model allows the determination of all three partition coefficients involved in the system, and elucidates the micellar contribution to retention and selectivity. Four types of micellar-ionic liquid columns were examined in this study: 1-butyl-3-methylimidazolium chloride with sodium dodecylsulfate or dioctyl sulfosuccinate, and 1-butyl-3-methylimidazolium hexafluorophosphate with polyoxyethylene-100-stearyl ether or polyoxyethylene-23-lauryl ether. The partition coefficients were measured for a wide range of probe molecules capable of a variety of types and magnitudes of interactions. In general, most probe molecules preferentially partitioned to the micellar pseudophase over the bulk ionic liquid component of the stationary phase. Therefore, addition of surfactant to the stationary phase usually resulted in greater solute retention. It is also shown that the selectivity of the stationary phase is significantly altered by the presence of micelles, either by enhancing or lessening the separation. The effects of surfactant on the interaction parameters of the stationary phase are determined using the Abraham solvation parameter model. The addition of sodium dodecylsulfate and dioctyl sulfosuccinate to 1-butyl-3-methylimidazolium chloride stationary phases generally increased the phase's hydrogen bond basicity and increased the level of dispersion interaction. Polyoxyethylene-100-stearyl ether and polyoxyethylene-23-lauryl ether surfactants, however, enhanced the pi-pi/n-pi, polarizability/dipolarity, and hydrogen bond basicity interactions of 1-butyl-3-methylimidazolium hexafluorophosphate to a greater degree than the ionic surfactants with 1-butyl-3-methylimidazolium chloride. However, these nonionic surfactants appeared to hinder the ability of the stationary phase to interact with solutes via dispersion forces

  5. Determination of Structure and Composition of Suberin from the Roots of Carrot, Parsnip, Rutabaga, Turnip, Red Beet, and Sweet Potato by Combined Gas-Liquid Chromatography and Mass Spectrometry 1

    PubMed Central

    Kolattukudy, P. E.; Kronman, Karen; Poulose, A. J.

    1975-01-01

    Suberin from the roots of carrots (Daucus carota), parsnip (Pastinaca sativa), rutabaga (Brassica napobrassica), turnip (Brassica rapa), red beet (Beta vulgaris), and sweet potato (Ipomoea batatas) was isolated by a combination of chemical and enzymatic techniques. Finely powdered suberin was depolymerized with 14% BF3 in methanol, and soluble monomers (20-50% of suberin) were fractionated into phenolic (<10%) and aliphatic (13-35%) fractions. The aliphatic fractions consisted mainly of ω-hydroxyacids (29-43%), dicarboxylic acids (16-27%), fatty acids (4-18%), and fatty alcohols (3-6%). Each fraction was subjected to combined gas-liquid chromatography and mass spectrometry. Among the fatty acids very long chain acids (>C20) were the dominant components in all six plants. In the alcohol fraction C18, C20, C22, and C24 saturated primary alcohols were the major components. C16 and C18 dicarboxylic acids were the major dicarboxylic acids of the suberin of all six plants and in all cases octadec-9-ene-1, 18-dioic acid was the major component except in rutabaga where hexadecane-1, 16-dioic acid was the major dicarboxylic acid. The composition of the ω-hydroxyacid fraction was quite similar to that of the dicarboxylic acids; 18-hydroxy-octadec-9-enoic acid was the major component in all plants except rutabaga, where equal quantities of 16-hydroxyhexadecanoic acid and 18-hydroxyoctadec-9-enoic acid (42% each) were found. Compounds which would be derived from 18-hydroxyoctadec-9-enoic acid and octadec-9-ene-1, 18-dioic acid by epoxidation, and epoxidation followed by hydration of the epoxide, were also detected in most of the suberin samples. The monomer composition of the six plants showed general similarities but quite clear taxonomic differences. PMID:16659124

  6. 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

  7. 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.

  8. 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

  9. 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

  10. 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...

  11. 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.

  12. 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

  13. 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)

  14. Effect of gas-liquid flow pattern and microbial diversity analysis of a pilot-scale biotrickling filter for anoxic biogas desulfurization.

    PubMed

    Almenglo, Fernando; Bezerra, Tercia; Lafuente, Javier; Gabriel, David; Ramírez, Martín; Cantero, Domingo

    2016-08-01

    Hydrogen sulfide removal from biogas was studied under anoxic conditions in a pilot-scale biotrickling filter operated under counter- and co-current gas-liquid flow patterns. The best performance was found under counter-current conditions (maximum elimination capacity of 140 gS m(-3) h(-1)). Nevertheless, switching conditions between co- and counter-current flow lead to a favorable redistribution of biomass and elemental sulfur along the bed height. Moreover, elemental sulfur was oxidized to sulfate when the feeding biogas was disconnected and the supply of nitrate (electron acceptor) was maintained. Removal of elemental sulfur was important to prevent clogging in the packed bed and, thereby, to increase the lifespan of the packed bed between maintenance episodes. The larger elemental sulfur removal rate during shutdowns was 59.1 gS m(-3) h(-1). Tag-encoded FLX amplicon pyrosequencing was used to study the diversity of bacteria under co-current flow pattern with liquid recirculation and counter-current mode with a single-pass flow of the liquid phase. The main desulfurizing bacteria were Sedimenticola while significant role of heterotrophic, opportunistic species was envisaged. Remarkable differences between communities were found when a single-pass flow of industrial water was fed to the biotrickling filter. PMID:27231880

  15. 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.

  16. [Gas-liquid chromatographic determination of etofenamate/ Determination, method and use in biological material (author's transl)].

    PubMed

    Dell, H D; Fiedler, J; Jacobi, H; Kolle, J

    1981-01-01

    Etofenamate in biological specimen can be determined by gas-liquid chromatography with etofenamate benzyl ether as internal standard. Determination in urine is done directly after extraction and concentration, whereas plasma and homogenates from organs have to be prepurified by thin-layer chromatography. Unchanged etofenamate is found in small amounts in human urine (0--4, 6--6, 6--8 h p. appl.). Inflamed rat paws after local application contain up to 75 microgram etofenamate/g in comparison to only 2 microgram flufenamic acid/g tissue. Both compounds are also found in non-inflamed paws, contents being only 3--4% as compared to the inflamed tissue. Elimination of etofenamate from the inflamed area occurs with a half-life of approx. 8.5 h. These results from gas-liquid chromatography correspond to results from t.l.c./fluorescence measurements. PMID:6971109

  17. Analysis assessment expert system for gas chromatography

    SciTech Connect

    Elling, J.W.; Roberts, R.S.; Lahiri, S.

    1995-12-01

    An artificial intelligence based analysis assessment system is presented to automate gas chromatography instrument troubleshooting. This system is capable of recognizing symptoms of common problems with GC analysis, reasoning with the symptoms to make a problem diagnosis, and suggest appropriate solutions. In this system, signal processing techniques are used to search for symptoms of problems in the time-series data. For example, peak shapes are analyzed for fronting and tailing and the baseline is analyzed for drift and the presence of electronic spikes. A measurement of the severity of each symptom is then used by the expert system to diagnose potential problems with the analysis. This system will be integrated with the instrument control and laboratory automation that is necessary to effect the recommended solutions when possible. The result will be a more robust instrument capable of recognizing failures and error modes from the sample data and capable of correcting many of the common failures.

  18. 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.

  19. 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 ...

  20. Minimizing liquid contaminants in natural gas liquids

    SciTech Connect

    Brown, R.L.; Wines, T.H.; Williamson, K.M.

    1996-12-31

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

  1. 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.

  2. Precursors in gas-liquid mixtures

    NASA Astrophysics Data System (ADS)

    Gasenko, V. G.; Gorelik, R. S.; Nakoryakov, V. E.; Timkin, L. S.

    2013-10-01

    Two types of precursors propagating at the speed of sound in a pure liquid have been revealed in the experiments on the evolution of pressure pulses in a gas-liquid mixture; at the same time, the main pressure pulse propagates at a low equilibrium speed of sound and its evolution is described by the Burgers-Korteweg-de Vries equation. The first high-frequency precursor is a complete analog of a classical Sommerfeld precursor, because the resonance dispersion equation for a bubble mixture coincides with that for insulators in the Lorentz model, and oscillates at a frequency close to the "plasma frequency." The second low-frequency precursor has been revealed in this work. The frequency of the low-frequency precursor is close to the resonance frequency of pulsations of bubbles, which is almost an order of magnitude lower than the frequency of the high-frequency precursor. The low-frequency precursor has a much larger amplitude of pulsations and smaller damping and is not described within the homogeneous model of the gas-liquid mixture. The observed phenomenon of low-frequency precursors has been explained within a simple heterogeneous model of a bubble liquid.

  3. 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

  4. Chromatography

    MedlinePlus

    ... a way of separating two or more chemical compounds. Chemical compounds are chemicals that are bonded together. For example, ... and hydrogen. Proteins are another type of chemical compound. There are different kinds of chromatography. These include ...

  5. 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.

  6. 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.

  7. Gas-Liquid Flow in Pipelines

    SciTech Connect

    Thomas J. Hanratty

    2005-02-25

    A research program was carried out at the University of Illinois in which develops a scientific approach to gas-liquid flows that explains their macroscopic behavior in terms of small scale interactions. For simplicity, fully-developed flows in horizontal and near-horizontal pipes. The difficulty in dealing with these flows is that the phases can assume a variety of configurations. The specific goal was to develop a scientific understanding of transitions from one flow regime to another and a quantitative understanding of how the phases distribute for a give regime. These basic understandings are used to predict macroscopic quantities of interest, such as frictional pressure drop, liquid hold-up, entrainment in annular flow and frequency of slugging in slug flows. A number of scientific issues are addressed. Examples are the rate of atomization of a liquid film, the rate of deposition of drops, the behavior of particles in a turbulent field, the generation and growth of interfacial waves. The use of drag-reducing polymers that change macroscopic behavior by changing small scale interactions was explored.

  8. 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.

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

    USGS Publications Warehouse

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

    1974-01-01

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

  10. 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.

  11. 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…

  12. 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/...

  13. 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...

  14. 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)

  15. /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%.

  16. Multiple-injection high-throughput gas chromatography analysis.

    PubMed

    Schafer, Wes; Wang, Heather; Welch, Christopher J

    2016-08-01

    Multiple-injection techniques have been shown to be a simple way to perform high-throughput analysis where the entire experiment resides in a single chromatogram, simplifying the data analysis and interpretation. In this study, multiple-injection techniques are applied to gas chromatography with flame ionization detection and mass detection to significantly increase sample throughput. The unique issues of implementing a traditional "Fast" injection mode of multiple-injection techniques with gas chromatography and mass spectrometry are discussed. Stacked injections are also discussed as means to increase the throughput of longer methods where mass detection is unable to distinguish between analytes of the same mass and longer retentions are required to resolve components of interest. Multiple-injection techniques are shown to increase instrument throughput by up to 70% and to simplify data analysis, allowing hits in multiple parallel experiments to be identified easily. PMID:27292909

  17. 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.'

  18. Injector design guidelines for gas/liquid propellant systems

    NASA Technical Reports Server (NTRS)

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

    1973-01-01

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

  19. Phase diagram and universality of the Lennard-Jones gas-liquid system.

    PubMed

    Watanabe, Hiroshi; Ito, Nobuyasu; Hu, Chin-Kun

    2012-05-28

    The gas-liquid phase transition of the three-dimensional Lennard-Jones particles system is studied by molecular dynamics simulations. The gas and liquid densities in the coexisting state are determined with high accuracy. The critical point is determined by the block density analysis of the Binder parameter with the aid of the law of rectilinear diameter. From the critical behavior of the gas-liquid coexisting density, the critical exponent of the order parameter is estimated to be β = 0.3285(7). Surface tension is estimated from interface broadening behavior due to capillary waves. From the critical behavior of the surface tension, the critical exponent of the correlation length is estimated to be ν = 0.63(4). The obtained values of β and ν are consistent with those of the Ising universality class. PMID:22667535

  20. 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

  1. 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.

  2. 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.

  3. Kinetic analysis of drug-protein interactions by affinity chromatography.

    PubMed

    Bi, Cong; Beeram, Sandya; Li, Zhao; Zheng, Xiwei; Hage, David S

    2015-10-01

    Information on the kinetics of drug-protein interactions is of crucial importance in drug discovery and development. Several methods based on affinity chromatography have been developed in recent years to examine the association and dissociation rates of these processes. These techniques include band-broadening measurements, the peak decay method, peak fitting methods, the split-peak method, and free fraction analysis. This review will examine the general principles and applications of these approaches and discuss their use in the characterization, screening and analysis of drug-protein interactions in the body. PMID:26724332

  4. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    PubMed

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-01

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. PMID:25200530

  5. 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.

  6. 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.

  7. 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…

  8. 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.

  9. 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.

  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. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Field gas chromatography-mass spectrometry for fast analysis.

    PubMed

    Makas, Alexei L; Troshkov, Mikhail L

    2004-02-01

    The objective of this presentation is to demonstrate the original device and procedure for fast gas chromatography-mass spectrometry (GC-MS) analysis of gaseous and liquid samples and to discuss its features and capabilities. The concept was developed in order to expand the range of compounds suitable for GC separation and to reduce the time of analysis. Field GC-MS, consisting of original "concentrator-thermodesorber" (CTD) unit, multiple module GC system and compact magnetic mass spectrometer with powerful two-stage vacuum system and multicollector ion detector, is represented. The whole weight of the device is 90 kg. Power consumption is 250 W. The device and analytical procedures allow high speed screening of toxic substances in air and extracts within 100 s per sample. The examples of applications are described, including fast screening of tributyl phosphate (TBP) in air at low ppt level at the rate 1 sample/min. PMID:14698236

  17. 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.

  18. 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

  19. Bubbling behaviors induced by gas-liquid mixture permeating through a porous medium

    NASA Astrophysics Data System (ADS)

    Hu, Liang; Li, Mingbo; Chen, Wenyu; Xie, Haibo; Fu, Xin

    2016-08-01

    This paper investigates the bubbling behaviors induced by gas-liquid mixture permeating through porous medium (PM), which was observed in developing immersion lithography system and was found having great differences with traditional bubbling behaviors injected with only gas phase through the PM. An experimental setup was built up to investigate the bubbling characteristics affected by the mixed liquid phase. Both the flow regimes of gas-liquid mixture in micro-channel (upstream of the PM) and the bubbling flow regimes in water tank (downstream of the PM) were recorded synchronously by high-speed camera. The transitions between the flow regimes are governed by gas and liquid Weber numbers. Based on the image analysis, the characteristic parameters of bubbling region, including the diameter of bubbling area on PM surface, gas-phase volume flux, and dispersion angle of bubbles in suspending liquid, were studied under different proportions of gas and liquid flow rate. Corresponding empirical correlations were developed to describe and predict these parameters. Then, the pertinent bubble characteristics in different bubbling flow regimes were systematically investigated. Specifically, the bubble size distribution and the Sauter mean diameter affected by increasing liquid flow rate were studied, and the corresponding analysis was given based on the hydrodynamics of bubble-bubble and bubble-liquid interactions. According to dimensionless analysis, the general prediction equation of Sauter mean diameter under different operating conditions was proposed and confirmed by experimental data. The study of this paper is helpful to improve the collection performance of immersion lithography and aims to reveal the differences between the bubbling behaviors on PM caused by only gas flow and gas-liquid mixture flow, respectively, for the researches of fluid flow.

  20. 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.

  1. RNA footprinting analysis using ion pair reverse phase liquid chromatography.

    PubMed Central

    Dickman, Mark J; Conroy, Matthew J; Grasby, Jane A; Hornby, David P

    2002-01-01

    Hydroxyl radical footprinting is a powerful technique often employed in characterization of the tertiary interactions between proteins and nucleic acids. Following the generation of a nucleic acid "ladder" either by chemical or enzymatic reactions, the radiolabeled products are traditionally separated by denaturing gel electrophoresis and further quantified by phosphorimaging techniques. Here we report the use of ion pair reverse phase liquid chromatography to analyze the products of an RNA footprinting reaction using fluorescently labeled RNA molecules. This technique offers several advantages over existing procedures, including rapid analysis, automation, and direct quantification of the cleavage products without the need to employ radiolabeling. To illustrate the resolving power of this technique, we have analyzed the products of base hydrolysis, generated from a fluorescently labeled RNA molecule and have subsequently used this method to define the solvent accessibility of the substrate strand as it docks with the hairpin ribozyme. PMID:11911369

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

    PubMed

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

    2016-07-01

    An ultrasensitive method for the simultaneous analysis of pesticides residues in tobacco was developed with online size exclusion chromatography with gas chromatography and tandem mass spectrometry. Tobacco samples were extracted with the solvent mixture of cyclohexane and acetone (7:3, v/v) and centrifuged. Then, the supernatant liquors were injected directly into the online size exclusion chromatography with gas chromatography and tandem mass spectrometry without any other purification procedures after being filtered with a 0.22 μm organic phase filter. The matrix interferences were effectively removed and recoveries of most pesticides were in the range of 72-121%. Especially, for chlorothalonil, the analysis efficiency of this method was much more favorable than that of the general method, in which dispersive solid-phase extraction was used as an additional purified procedure. In addition, the limits of quantitation of this method were from 1 to 50 μg/kg. Therefore, a rapid, cost-effective, labor-saving method was proposed in the present work, which was suitable for the analysis of 41 pesticide residues in tobacco. PMID:27197809

  3. 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

  4. 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

  5. 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...

  6. 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

  7. 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.

  8. 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.

  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

    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.

  11. Energy transfer at gas-liquid interface: Towards energetic materials

    NASA Astrophysics Data System (ADS)

    Szabo, Tamas

    Physicochemical surface processes have great importance in the different fields of everyday life and science. Computational characterization of collisional energy transfer at a gas-liquid interface is a helpful tool to interpret recent experimental studies and to yield insight into the energy feedback mechanism of multiphase combustion problems. As a first step, a simple Lennard-Jones system was used to investigate the dependence of the collisional energy transfer and the gas atom trapping probabilities on the temperature of the bulk liquid, on the gas/liquid particle mass ratios, on the incident angle of the impinging projectile, and on the gas-liquid interaction strength. We find in accord with the experimental results that the kinematic effects dominate the energy transfer dynamics, but the importance of the role of surface roughening as the temperature of the liquid increases is also seen. The second system, nitromethane was chosen to extend the range of simulations. It is a molecular model system, representing nitramine-type energetic materials. Having had a good potential description for the nitromethane molecule including all internal degrees of freedom, we generated simplified molecular systems based on the original nitromethane model to isolate particular features of the dynamics. We have investigated the effect of the initial incident energy, of the inclusion of the internal degrees of freedom, of the initial incident kinetic energy and of the gas-surface interaction strength. The incorporation of internal degrees of freedom enhanced the collisional energy transfer. These calculations also point to the importance of simple kinematics as it predicts the increase of the ratio of energy transferred with increased initial incident energy of the gas particle.

  12. Gas-liquid chromatographic determination of morphine, heroin, and cocaine.

    PubMed

    Prager, M J; Harrington, S M; Governo, T F

    1979-03-01

    Morphine, heroin, and cocaine are quantitatively determined with the same gas-liquid chromatographic system. The compounds are separated on a 6 ft X 2 mm id glass column packed with a 1:1 mixture of 5% SE-30 on 80--100 mesh Chromosorb W and 3% OV-17 on 80--100 mesh Varaport 30. The column is temperature-programmed. Flame ionization detector responses are measured with a computer-based data system. Heroin and cocaine are chromatographed directly; morphine is derivatized first. The procedure was evaluated with previously analyzed commercial and forensic samples. Accuracy and precision were 5 and 3%, respectively. PMID:447602

  13. About the statistical description of gas-liquid flows

    SciTech Connect

    Sanz, D.; Guido-Lavalle, G.; Carrica, P.

    1995-09-01

    Elements of the probabilistic geometry are used to derive the bubble coalescence term of the statistical description of gas liquid flows. It is shown that the Boltzmann`s hypothesis, that leads to the kinetic theory of dilute gases, is not appropriate for this kind of flows. The resulting integro-differential transport equation is numerically integrated to study the flow development in slender bubble columns. The solution remarkably predicts the transition from bubbly to slug flow pattern. Moreover, a bubbly bimodal size distribution is predicted, which has already been observed experimentally.

  14. 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.

  15. Analysis of methaqualone in biological matrices by micellar electrokinetic capillary chromatography. Comparison with gas chromatography-mass spectrometry.

    PubMed

    Plaut, O; Girod, C; Staub, C

    1998-04-01

    The analysis of methaqualone (MTQ) in biological matrices by capillary electrophoresis (CE) is described. This methods uses liquid-liquid extraction and micellar electrokinetic capillary chromatography (MECC), an operation mode of CE. Separations are made using a 25 cm long capillary and a borate/phosphate buffer at pH 8.2. Using gas chromatography with mass spectrometry detection (GC-MS) as reference method, MTQ has been analyzed in urine, blood, gastric content and hair. For hair analysis, supercritical fluid extraction was compared with liquid-liquid extraction. Linearity was established in urine and blood between 0.25 and 10.0 micrograms/ml. MTQ recovery from blood was estimated at 60%. The limit of detection of this method in urine is about 0.10 microgram/ml. Drawbacks and advantages of MECC over GC-MS are discussed. PMID:9627981

  16. 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.

  17. 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.

  18. Spatio-temporal evolution of interfacial instabilities in vertical gas-liquid flows

    NASA Astrophysics Data System (ADS)

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

    2014-11-01

    Vertical gas-liquid flows are characteristic for process engineering and widely employed in various technical applications. However, the dynamic behaviour of the liquid interface in such flows is still not fully understood. We focus in our work on characterising the interfacial instability as well as associated interfacial waves in vertical laminar-laminar gas-liquid flows over a wide range of parameters covering different flow regimes, i.e. counter-current, zero-interface velocity (loading) and partial-to-full liquid flow reversal (flooding). High-resolution direct numerical simulations using the TPLS flow solver (http://sourceforge.net/projects/tpls/) reveal the existence of weakly nonlinear interfacial waves, which are in good agreement with Stuart-Landau theory. These waves travel down- or upstream, depending on the flow regime. Furthermore, spatio-temporal linear stability analysis indicates the occurrence of absolute instability within the investigated parameter range. DNS is used to analyse this feature in more detail whereby agreement with linear theory has been established.

  19. Experimental study on gas-liquid flow characteristics of submerged air jets

    NASA Astrophysics Data System (ADS)

    Qin, S. J.; Liu, J. T.; Miao, T. C.; Wu, D. Z.

    2016-05-01

    The gas-liquid flow structure and interfacial behavior of submerged air jets were investigated experimentally using high speed digital video camera and image processing techniques. The jet pressure ratio varied from 1.8 to 4.8 in the experiment. And results from different jet nozzles were processed and compared. Statistical characteristics of the jet diameters along the axial distance were obtained and analyzed. Time series analysis was implemented to study the interface unsteadiness by calculating the gas-liquid interface deviation. The results showed that the jet diameters increase first linearly then nonlinearly and its growth rate decreases along the axial distance. The reason for the divergence between the result of this experiment and those done by other researchers was analyzed. Comparing the results of different pressure ratios and nozzle diameters, we found that larger jet pressure ratios have larger jet diameters and nozzle diameters nearly have no bearing on the distribution of dimensionless jet diameters. The interface unsteadiness in low and high pressure ratios exhibited totally distinct properties. And a minimum unsteady value was found along the axis of the air jets.

  20. The use of microemulsion electrokinetic chromatography in pharmaceutical analysis.

    PubMed

    Miola, M F; Snowden, M J; Altria, K D

    1998-12-01

    The use of a single set of microemulsion electrokinetic chromatography (MEEKC) separation conditions has been assessed for its applicability in the analysis of a range of pharmaceutical compounds. Particular emphasis was placed on neutral or very hydrophobic compounds, which can be difficult to analyse by conventional capillary electrophoresis. The microemulsion employed for the majority of separations consisted of 0.81% w/w octane, 6.61% w/w 1-butanol, 3.31% w/w sodium dodecyl sulphate and 89.27% w/w 10 mM sodium tetraborate buffer. Good separations of methyl, ethyl, butyl and propyl hydroxybenzoates, and a range of ionic and neutral water soluble and insoluble compounds was achieved using a single set of separation conditions. A number of novel applications of MEEKC were developed included the simultaneous determination of the active components and preservatives in liquid formulation and determination of drug related impurities. Improved performance was obtained through use of internal standards and preparation of the samples dissolved in the microemulsion solution. Validation aspects such as linearity, repeatability, accuracy, injection precision and sensitivity were successfully assessed. PMID:9919981

  1. 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 Haz

  2. 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

  3. Alkaloids analysis using off-line two-dimensional supercritical fluid chromatography × ultra-high performance liquid chromatography.

    PubMed

    Li, Kuiyong; Fu, Qing; Xin, Huaxia; Ke, Yanxiong; Jin, Yu; Liang, Xinmiao

    2014-07-21

    In this study, an off-line two-dimensional (2-D) supercritical fluid chromatography (SFC) × ultra-high performance liquid chromatography (UHPLC) method with high orthogonality was developed for the analysis of the practical amide alkaloids fraction from P. longum L. The effects of SFC parameters such as column type, organic modifier, temperature and back-pressure on separation were systematically evaluated. Different selectivity was observed for different columns (BEH, BEH 2-EP, XAmide and CSH FP). An investigation was then carried out of the orthogonality of different columns and systems following a geometric approach with a set of amide alkaloid samples. The orthogonality between a CSH FP column and a BEH column reached 50.79%, which was much higher than that for the other columns. While the orthogonality between SFC and UHPLC based on an XAmide column and an HSS T3 column reached 69.84%, which was the highest of all the combinations. At last, the practical amide alkaloids fraction was analyzed with an off-line 2-D chromatography SFC × UHPLC system. In total, at least 340 peaks were detected by this method. Rapid separation in these two dimensions and easy post treatment of SFC facilitated this 2-D system for the separation of complex samples. PMID:24828698

  4. 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.

  5. 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...

  6. 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)

  7. 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...

  8. 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...

  9. 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

  10. 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

  11. Simulating Gas-Liquid-Water Partitioning and Fluid Properties of Petroleum under Pressure: Implications for Deep-Sea Blowouts.

    PubMed

    Gros, Jonas; Reddy, Christopher M; Nelson, Robert K; Socolofsky, Scott A; Arey, J Samuel

    2016-07-19

    With the expansion of offshore petroleum extraction, validated models are needed to simulate the behaviors of petroleum compounds released in deep (>100 m) waters. We present a thermodynamic model of the densities, viscosities, and gas-liquid-water partitioning of petroleum mixtures with varying pressure, temperature, and composition based on the Peng-Robinson equation-of-state and the modified Henry's law (Krychevsky-Kasarnovsky equation). The model is applied to Macondo reservoir fluid released during the Deepwater Horizon disaster, represented with 279-280 pseudocomponents, including 131-132 individual compounds. We define >n-C8 pseudocomponents based on comprehensive two-dimensional gas chromatography (GC × GC) measurements, which enable the modeling of aqueous partitioning for n-C8 to n-C26 fractions not quantified individually. Thermodynamic model predictions are tested against available laboratory data on petroleum liquid densities, gas/liquid volume fractions, and liquid viscosities. We find that the emitted petroleum mixture was ∼29-44% gas and ∼56-71% liquid, after cooling to local conditions near the broken Macondo riser stub (∼153 atm and 4.3 °C). High pressure conditions dramatically favor the aqueous dissolution of C1-C4 hydrocarbons and also influence the buoyancies of bubbles and droplets. Additionally, the simulated densities of emitted petroleum fluids affect previous estimates of the volumetric flow rate of dead oil from the emission source. PMID:27117673

  12. 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...

  13. 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.

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

    NASA Astrophysics Data System (ADS)

    Devi, T. T.; Kumar, Bimlesh

    2015-01-01

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

  15. [Mechanism of the organic pollutant degradation in water by hybrid gas-liquid electrical discharge].

    PubMed

    Zhu, Li-nan; Ma, Jun; Yang, Shi-dong

    2007-09-01

    The method of hybrid gas-liquid electrical discharge was investigated for the removal of phenol. The results indicate that this new method can remove phenol in water effectively. The removal rate increases with increasing voltage and air aeration. The production quantity of H2O2 and O3 is measured respectively in the discharge region and the production quantity increases with increasing of voltage and air aeration. The energy consumption analysis indicates that with increasing the voltage, the increase extent of the phenol removal rate is smaller than the energy's, so the increase of energy efficiency is very small. Air aeration increases the energy consumption. At the same time, a considerable part of energy in the overall input energy makes the temperature of the solution increase, and more energy is transformed into heat, which leads to the waste of energy. PMID:17990549

  16. 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

  17. Trace level perchlorate analysis by ion chromatography-mass spectrometry.

    PubMed

    Mathew, Johnson; Gandhi, Jay; Hedrick, Joe

    2005-08-26

    Perchlorate is commonly used as an oxidant in solid fuel propellant for rockets and missiles. Recently perchlorate contamination was found in many aquifers associated with Colorado River and other sites. Perchlorate was also found at elevated level in crops that use contaminated water for irrigation. Ion chromatography with conductivity detection could be used to measure perchlorate levels in drinking and wastewaters as per United States Environmental Protection Agency method 314, but at lower levels and with complexity of the matrix there could be false positive and/or false negative. This study was done to demonstrate the detection of perchlorate with lower detection limit with high ionic matrix by ion chromatography-mass spectrometry. PMID:16106848

  18. [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

  19. Dynamic Modeling Strategy for Flow Regime Transition in Gas-Liquid Two-Phase Flows

    SciTech Connect

    Xia Wang; Xiaodong Sun; Benjamin Doup; Haihua Zhao

    2012-12-01

    In modeling gas-liquid two-phase flows, the concept of flow regimes has been widely 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 flow regime dependent. Current nuclear reactor safety analysis codes, such as RELAP5, classify flow regimes using flow regime maps or transition criteria that were developed for steady-state, fully-developed flows. As twophase flows are dynamic in nature, it is important to model the flow regime transitions dynamically to more accurately predict the two-phase flows. The present work aims to develop a dynamic modeling strategy to determine flow regimes in gas-liquid two-phase flows through 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 of the interfacial area, fluid particle (bubble or liquid droplet) disintegration, boiling and evaporation, and the destruction of the interfacial area, fluid particle coalescence and condensation. For 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 shapes, namely group-1 and group-2 bubbles. A preliminary approach to dynamically identify the flow regimes is discussed, in which discriminator s are based on the predicted information, such as the void fraction and interfacial area concentration. The flow regime predicted with this method shows good agreement with the experimental observations.

  20. Study of interfacial behavior in cocurrent gas-liquid flows

    SciTech Connect

    McCready, M.J.

    1990-01-01

    We have examined the mechanism of formation of solitary waves on gas-liquid flows and found, that these form from existing periodic waves which have sufficiently large ({approximately}1.5 to 2 depending upon fluid properties) amplitude to liquid layer-thickness ratios. The exact process for the wave shape change is not understood but it does not seem to be related to the wave steepness (amplitude/wavelength) or to separation of gas flow over the waves. The observed confinement of solitary waves to low liquid Reynolds numbers results because the necessary large precursor waves do not form if the wave speed dispersion is too large or if the wavelength of the dominant waves is too short, as occurs for higher Re{sub L}. Measurements of interface tracings and calculations of power spectra and bispectra as a function of flow distance for conditions close to neutral stability reveal that the initially, linearly unstable mode is stabilized by formation of overtones which are linearly stable and can dissipate energy. As a result, a stable wave field can occur. Mode equations, which include quadratic nonlinearities, can model this process to the extent of producing some degree of quantitative predictions for the amplitudes of the wave modes. However, a complete picture of the wave field must include sidebands as well because these are observed for some flow conditions. 34 refs., 12 figs., 2 tabs.

  1. 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.

  2. Semiphenomenological model for gas-liquid phase transitions.

    PubMed

    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 T(s) depending on the gas density. It is further shown that, even if T is only marginally lower than T(s), 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 T(s) being the temperature of saturated vapor and the high-density clusters representing liquid droplets. PMID:27078333

  3. 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.

  4. 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...

  5. 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

    ... 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...

  6. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 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...

  7. 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

    ... 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...

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

    PubMed

    Lesellier, E

    2001-11-30

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

  9. High pH reversed-phase chromatography with fraction concatenation as an alternative to strong-cation exchange chromatography for two-dimensional proteomic analysis

    PubMed Central

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

    2012-01-01

    Summary Orthogonal high-resolution separations are critical for attaining improved analytical dynamic range and protein coverage in proteomic measurements. High pH reversed-phase liquid chromatography (RPLC) followed by fraction concatenation affords better peptide analysis than conventional strong-cation exchange (SCX) chromatography applied for the two-dimensional proteomic analysis. For example, concatenated high pH reversed-phase liquid chromatography increased identification for peptides (1.8-fold) and proteins (1.6-fold) in shotgun proteomics analyses of a digested human protein sample. Additional advantages of high pH RPLC with fraction concatenation include improved protein sequence coverage, simplified sample processing, and reduced sample losses, making this an attractive alternative to SCX chromatography in conjunction with the second dimension low pH RPLC for two-dimensional proteomics analyses. PMID:22462785

  10. 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.

  11. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... mixture. Each of the constituents in a vaporized mixture of compounds is separated according to its vapor pressure. The device may include accessories such as columns, gases, column supports, and liquid...

  12. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... mixture. Each of the constituents in a vaporized mixture of compounds is separated according to its vapor pressure. The device may include accessories such as columns, gases, column supports, and liquid...

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

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... mixture. Each of the constituents in a vaporized mixture of compounds is separated according to its vapor pressure. The device may include accessories such as columns, gases, column supports, and liquid...

  14. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... mixture. Each of the constituents in a vaporized mixture of compounds is separated according to its vapor pressure. The device may include accessories such as columns, gases, column supports, and liquid...

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

    NASA Technical Reports Server (NTRS)

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

    1975-01-01

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

  16. Acoustic Probe for Solid-Gas-Liquid Suspension

    SciTech Connect

    Tavlarides, L.L.; Sangani, Ashok

    2003-09-14

    /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.

  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. 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.

  1. Accelerated gas-liquid visible light photoredox catalysis with continuous-flow photochemical microreactors.

    PubMed

    Straathof, Natan J W; Su, Yuanhai; Hessel, Volker; Noël, Timothy

    2016-01-01

    In this protocol, we describe the construction and use of an operationally simple photochemical microreactor for gas-liquid photoredox catalysis using visible light. The general procedure includes details on how to set up the microreactor appropriately with inlets for gaseous reagents and organic starting materials, and it includes examples of how to use it to achieve continuous-flow preparation of disulfides or trifluoromethylated heterocycles and thiols. The reported photomicroreactors are modular, inexpensive and can be prepared rapidly from commercially available parts within 1 h even by nonspecialists. Interestingly, typical reaction times of gas-liquid visible light photocatalytic reactions performed in microflow are lower (in the minute range) than comparable reactions performed as a batch process (in the hour range). This can be attributed to the improved irradiation efficiency of the reaction mixture and the enhanced gas-liquid mass transfer in the segmented gas-liquid flow regime. PMID:26633128

  2. Analysis of Polyamines in Higher Plants by High Performance Liquid Chromatography 1

    PubMed Central

    Flores, Hector E.; Galston, Arthur W.

    1982-01-01

    A sensitive (0.01-1 nmol) method has been developed for the analysis of polyamines in higher plant extracts based on high performance liquid chromatography (HPLC) of their benzoyl derivatives (Redmond, Tseng 1979 J Chromatogr 170: 479-481). Putrescine, cadaverine, agmatine, spermidine, spermine, and the less common polyamines nor-spermidine and homospermidine can be completely resolved by reverse phase HPLC, isocratic elution with methanol:water (64%, v/v) through a 5-μm C18 column, and detection at 254 nm. The method can be directly applied to crude plant extracts, and it is not subject to interference by carbohydrates and phenolics. A good quantitative correlation was found between HPLC analysis of benzoylpolyamines and thin layer chromatography of their dansyl derivatives. With the HPLC method, polyamine titers have been reproducibly estimated for various organs of amaranth, Lemna, oat, pea, Pharbitis, and potato. The analyses correlate well with results of thin layer chromatography determinations. Images PMID:16662279

  3. Hydrophilic interaction chromatography for the analysis of aminoglycosides.

    PubMed

    Kumar, Praveen; Rubies, Antoni; Companyó, Ramon; Centrich, Francesc

    2012-02-01

    The effect of mobile-phase constituents (pH and ionic strength) and chromatographic behaviour of ten aminoglycosides (streptomycin, dihydrostreptomycin, spectinomycin, apramycin, paramomycin, kanamycin A, gentamycin C1, gentamycin C2/C2a, gentamycin C1a and neomycin) in the bare silica, amino, amide and zwitterionic phases of hydrophilic interaction chromatography (HILIC) were studied systematically. Among the stationary phases studied, the zwitterionic phase provided the best separation of aminoglycosides. The effect of pH, ionic concentration and column temperature on retention time, peak shape and sensitivity was studied using a central composite design. pH affected sensitivity of the detection of analytes but not the retention time. High ionic strength in the mobile phase was necessary to control the ionic interactions between ionised aminoglycosides and the hydrophilic phase, thereby influencing peak shape and retention time. Column temperature affected sensitivity of the detection but not the retention time. During method development, crosstalk between the MS/MS channels of the analytes was observed and resolved. PMID:22282410

  4. Qualitative analysis of mycotoxins using micellar electrokinetic capillary chromatography

    SciTech Connect

    Holland, R.D.; Sepaniak, M.J. )

    1993-05-01

    Naturally occurring mycotoxins are separated using micellar electrokinetic capillary chromatography. Trends in the retention of these toxins, resulting from changes in mobile-phase composition and pH, are reported and presented as a means of alleviating coelution problems. Two sets of mobile-phase conditions are determined that provide unique separation selectivity. The facile manner by which mobile-phase conditions can be altered, without changes in instrumental configuration, allowed the acquisition of two distinctive, fully resolved chromatograms of 10 mycotoxins in a period of approximately 45 min. By adjusting retention times, using indigenous or added components in mycotoxin samples as normalization standards, it is possible to obtain coefficients of variation in retention time that average less than 1%. The qualitative capabilities of this methodology are evaluated by separating randomly generated mycotoxin-interferent mixtures. In this study, the utilization of normalized retention times applied to separations obtained with two sets of mobile-phase conditions permitted the identification of all the mycotoxins in five unknown samples without any misidentifications. 24 refs., 3 figs., 2 tabs.

  5. Quantitative analysis of terbutaline by gas chromatography-mass spectrometry.

    PubMed

    Leferink, J G; Baillie, T A; Lindberg, C

    1984-01-01

    Over the past 6 years, several gas chromatography-mass spectrometry (GC-MS) methods for terbutaline have been developed, each with certain advantages and disadvantages. They all involve monitoring of an ion selected from the mass spectrum of a suitable terbutaline derivative. This technique, often referred to as mass fragmentography or selected ion monitoring, reduces the interference from other drugs and endogenous compounds. Different ionization techniques have been employed to obtain high sensitivity, viz. electron impact and chemical ionization. Typically, the methods can be used to measure terbutaline concentrations down to 0.1-0.3 ng/mL in plasma or serum. Isolation of terbutaline from biological materials is complicated by the low partition of the drug from water to organic solvents. Extraction with a large volume of ethyl acetate, ion pair extraction, or isolation on a cation exchange column have been used. These methods are time consuming, and attempts have therefore been made to modify them. Rapid extraction can be achieved on a disposable reversed-phase octadecylsilyl column with unimpaired sensitivity and selectivity. Preliminary results indicate that negative ion chemical ionization of a fluorine-containing derivative can further increase the sensitivity of the terbutaline assays. PMID:6586484

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

    PubMed

    Rodríguez, R; Picó, Y; Font, G; Mañes, J

    2001-07-27

    A method based on solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC) was developed for the simultaneous determination of carbendazim, imazalil, methylthiophanate, O-phenylphenol, prochloraz, procimidone, thiabendazole and triadimefon residues in grape, lettuce, orange and tomato. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the type and concentration of surfactant and the methanol content in the mobile phase. A buffer consisting of 4 mM borate with 75 mM sodium cholate (pH 9.2) gave the best results. The recoveries of the fungicides in spiked fruit and vegetable samples ranged from 30 to 105%, and the limits of detection were between 0.1 and 1 mg kg(-1). The reproducibility and repeatability of the combination of SPE pretreatment and MEKC were good for all the compounds, except for imazalil and O-phenylphenol in oranges, due to some matrix compounds interfering with the separation. The method was applied to post harvest treated samples, and the fungicides were sometimes detected at concentration levels lower than maximum residue limits (MRLs). PMID:11521888

  7. 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...

  8. 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...

  9. 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...

  10. 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…

  11. 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...

  12. 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.

  13. 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...

  14. New trends in fast liquid chromatography for food and environmental analysis.

    PubMed

    Núñez, Oscar; Gallart-Ayala, Héctor; Martins, Claudia P B; Lucci, Paolo

    2012-03-01

    There is an increasing need for applications in food and environmental areas able to cope with a large number of analytes in very complex matrices. The new analytical procedures demand sensitivity, robustness and high resolution within an acceptable analysis time. The purpose of this review is to describe new trends based on fast liquid chromatography applied to the food and environmental analysis. It includes different column technologies, such as monolithic, sub-2 μm, porous shell, as well as different stationary phases such as reversed phase (C8 and C18), hydrophilic interaction liquid chromatography (HILIC) and fluorinated columns. Additionally, recent sample extraction and clean-up methodologies applied to reduce sample manipulation and total analysis time in food and environmental analysis--QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), on line solid phase extraction coupled to ultrahigh pressure liquid chromatography (on line SPE-UHPLC), turbulent flow chromatography (TFC) and molecularly imprinted polymers (MIPs), were also addressed. The advantages and drawbacks of these methodologies applied to the fast and sensitive analyses of food and environmental samples are going to be discussed. PMID:22153282

  15. Identification of amino acid thiohydantoins directly by thin-layer chromatography and indirectly by gas-liquid chromatography after hydrolysis.

    PubMed Central

    Rangarajan, M; Darbre, A

    1975-01-01

    A method is described for the identification of amino acid thiohydantoins by two-dimensional t.l.c. An indirect method for the determination of amino acid thiohydantoins is described which, after hydrolysis, the corresponding amino acids are determined by g.l.c. PMID:1167153

  16. Analysis of carbohydrates by anion exchange chromatography and mass spectrometry.

    PubMed

    Bruggink, Cees; Maurer, Rolf; Herrmann, Heiko; Cavalli, Silvano; Hoefler, Frank

    2005-08-26

    A versatile liquid chromatographic platform has been developed for analysing underivatized carbohydrates using high performance anion exchange chromatography (HPAEC) followed by an inert PEEK splitter that splits the effluent to the integrated pulsed amperometric detector (IPAD) and to an on-line single quadrupole mass spectrometer (MS). Common eluents for HPAEC such as sodium hydroxide and sodium acetate are beneficial for the amperometric detection but not compatible with electrospray ionisation (ESI). Therefore a membrane-desalting device was installed after the splitter and prior to the ESI interface converting sodium hydroxide into water and sodium acetate into acetic acid. To enhance the sensitivity for the MS detection, 0.5 mmol/l lithium chloride was added after the membrane desalter to form lithium adducts of the carbohydrates. To compare sensitivity of IPAD and MS detection glucose, fructose, and sucrose were used as analytes. A calibration with external standards from 2.5 to 1000 pmole was performed showing a linear range over three orders of magnitude. Minimum detection limits (MDL) with IPAD were determined at 5 pmole levels for glucose to be 0.12 pmole, fructose 0.22 pmole and sucrose 0.11 pmole. With MS detection in the selected ion mode (SIM) the lithium adducts of the carbohydrates were detected obtaining MDL's for glucose of 1.49 pmole, fructose 1.19 pmole, and sucrose 0.36 pmole showing that under these conditions IPAD is 3-10 times more sensitive for those carbohydrates. The applicability of the method was demonstrated analysing carbohydrates in real world samples such as chicory inulin where polyfructans up to a molecular mass of 7000 g/mol were detected as quadrupoly charged lithium adducts. Furthermore mono-, di-, tri-, and oligosaccharides were detected in chicory coffee, honey and beer samples. PMID:16106855

  17. Analysis of glycylsarcosine transport by lobster intestine using gas chromatography.

    PubMed

    Peterson, Maria L; Lane, Amy L; Ahearn, Gregory A

    2015-01-01

    Gas chromatography was used to measure transepithelial transport of glycylsarcosine (Gly-Sar) by perfused lobster (Homarus americanus) intestine. Unidirectional and net fluxes of dipeptide across the tissue and luminal factors affecting their magnitude and direction were characterized by perfusing the lumen with the dipeptide and measuring its appearance in saline on the serosal side of the organ. Transmural transport of 10 mM Gly-Sar resulted in serosal accumulation of only the dipeptide; no appearance of corresponding monomeric amino acids glycine or sarcosine was observed. Carrier-mediated and diffusional transmural intestinal transport of Gly-Sar was estimated at 1-15 mM luminal concentrations and followed a curvilinear equation providing a K m = 0.44 ± 0.17 mM, a J max = 1.27 ± 0.12 nmol cm(-2) min(-1), and a diffusional coefficient = 0.026 ± 0.008 nmol cm(-2) min(-1) mM(-1). Unidirectional mucosal to serosal and serosal to mucosal fluxes of 10 mM Gly-Sar provided a significant (p < 0.05) net absorptive flux toward the serosa of 3.54 ± 0.77 nmol cm(-2) min(-1), further supporting carrier-mediated dipeptide transport across the gut. Alkaline (pH 8.5) luminal pH more than doubled transmural Gly-Sar transport as compared to acidic (pH 5.5) luminal pH, while luminal amino acid-metal chelates (e.g., Leu-Zn-Leu), and high concentrations of amino acids alone significantly (p < 0.001) reduced intestinal Gly-Sar transfer by inhibiting carrier transport of the dipeptide. Proposed mechanisms accounting for intestinal dipeptide transport and luminal factors affecting this process are discussed. PMID:25260349

  18. Effect of liquid viscosity on wave behavior in gas-liquid two-phase flow

    SciTech Connect

    Kondo, Yoshiyuki; Mori, Koji; Yagishita, Takuya; Nakabo, Akinobu

    1999-07-01

    Measurements of time-spatial distributions of liquid holdups for the vertical upward gas-liquid two-phase flow were carried out by using the supermultiple cross-sectional mean liquid holdup probes (S-CHOP) and the semi-supermultiple point-electrode probes (SS-PEP) in the wide range of superficial gas and liquid velocity, j{sub g} and j{sub {ell}}, and the liquid kinematic viscosities were {nu}{sub {ell}} = 1 x 10{sup {minus}6}, 10 x 10{sup {minus}6} and 20 x 10{sup {minus}6} m{sup 1}/s. The time-spatial maps of wave behavior and the interfacial profiles were presented. Close inspection of these results reveals that there also exist huge waves and disturbance waves in the higher liquid viscosity conditions. To clarify the characteristics of these waves, the wave-vein analysis and the cluster analysis by K-mean algorithm were applied. These methods distinguished huge wave and disturbance wave objectively. The appearance regions of liquid slug, huge wave, and disturbance wave for each liquid viscosity condition were presented and the effects of liquid viscosity on them were discussed. Furthermore, velocity, width and height of these waves were determined, and the effects of liquid viscosity on them were clarified.

  19. 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

  20. 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.

  1. 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.

  2. 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

  3. TRACE ANALYSIS OF FLUORESCEIN-DERIVATIZED PHENOXY ACID HERBICIDES BY MICELLAR ELECTROKINETIC CHROMATOGRAPHY WITH LASER-INDUCTED FLUORESCENCE DETECTION

    EPA Science Inventory

    Micellar electrokinetic chromatography (MEKC) with laser-induced fluorescence (LIF) detection was used for the trace analysis of phenoxy acid herbicides. Capillary electrophoresis (CE) with LIF detection, which has not previously been used for pesticide analysis, overcomes the po...

  4. 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.

  5. Direct numerical simulation of interfacial wave generation in turbulent gas-liquid flows in horizontal channels

    NASA Astrophysics Data System (ADS)

    Campbell, Bryce; Hendrickson, Kelli; Liu, Yuming; Subramani, Hariprasad

    2014-11-01

    For gas-liquid flows through pipes and channels, a flow regime (referred to as slug flow) may occur when waves form at the interface of a stratified flow and grow until they bridge the pipe diameter trapping large elongated gas bubbles within the liquid. Slug formation is often accompanied by strong nonlinear wave-wave interactions, wave breaking, and gas entrainment. This work numerically investigates the fully nonlinear interfacial evolution of a two-phase density/viscosity stratified flow through a horizontal channel. A Navier-Stokes flow solver coupled with a conservative volume-of-fluid algorithm is use to carry out high resolution three-dimensional simulations of a turbulent gas flowing over laminar (or turbulent) liquid layers. The analysis of such flows over a range of gas and liquid Reynolds numbers permits the characterization of the interfacial stresses and turbulent flow statistics allowing for the development of physics-based models that approximate the coupled interfacial-turbulent interactions and supplement the heuristic models built into existing industrial slug simulators.

  6. 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.

  7. 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.

  8. High-throughput simultaneous analysis of pesticides by supercritical fluid chromatography/tandem mass spectrometry.

    PubMed

    Ishibashi, Megumi; Ando, Takashi; Sakai, Miho; Matsubara, Atsuki; Uchikata, Takato; Fukusaki, Eiichiro; Bamba, Takeshi

    2012-11-30

    Combination techniques such as gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS) are commonly used for pesticide residue analysis, but there is no reported method for the simultaneous analysis of multiple pesticides in a sample using a single instrument. Supercritical fluid chromatography (SFC) offers high resolution at high flow rates and various separation modes and hence may aid the rapid simultaneous analysis of pesticide. We developed an SFC/MS/MS method and analyzed 17 pesticides with a wide range of polarities (logP(ow)=-4.6 to 7.05) and molecular weights (112.1-888.6) within 11min using a polar-embedded reversed-phase column. To the best of our knowledge, there is no previous report on the SFC analysis of a wide variety of compounds, including highly hydrophilic ones. By SFC, diquat dibromide (logP(ow)=-4.6), together with cypermethrin (logP(ow)=6.6) and tralomethrin (logP(ow)=5.05), could be detected in the presence of various other pesticides using a single mobile phase. SFC/MS allows for the rapid and simultaneous analysis of low concentrations (ng/L levels) of pesticides that typically need to be analyzed by GC/MS and LC/MS separately. PMID:23102524

  9. [An analysis of maicaodi by high performance liquid chromatography].

    PubMed

    Yang, H; Chen, R; Jiang, M

    1997-05-01

    Maicaodi has recently been developed and produced by the pesticide plant of Nanjing Agricultural University. The quantitative analysis of the effective components--tribenuron methyl and R (-)napropamide in wettable powder of Maicaode, by a high performance liquid chromatographic method was carried out with a Lichrosorb Si-60 20cm x 0.46cm i.d. column, mobile phase of petroleum ether/isopropanol/methanol/acetonitrile/chloroform mixture solvent (80:5:5:5:5) and internal standard of diisooctyl phthalate. The sample was detected by ultraviolet absorption at 254 nm. The retention times of tribenuron methyl and R (-)napropamide were 10-11min and 6-7min respectively. The coefficient of variation of this analysis was 0.34% with a recovery of 99.51%-100.32%. The coefficient of linear correlation was 0.9999. PMID:15739379

  10. 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.

  11. 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

  12. The chemical interpretation and practice of linear solvation energy relationships in chromatography.

    PubMed

    Vitha, Mark; Carr, Peter W

    2006-09-01

    This review focuses on the use of linear solvation energy relationships (LSERs) to understand the types and relative strength of the chemical interactions that control retention and selectivity in the various modes of chromatography ranging from gas chromatography to reversed phase and micellar electrokinetic capillary chromatography. The most recent, widely accepted symbolic representation of the LSER model, as proposed by Abraham, is given by the equation: SP=c + eE + sS + aA + bB + vV, in which, SP can be any free energy related property. In chromatography, SP is most often taken as logk' where k' is the retention factor. The letters E, S, A, B, and V denote solute dependent input parameters that come from scales related to a solute's polarizability, dipolarity (with some contribution from polarizability), hydrogen bond donating ability, hydrogen bond accepting ability, and molecular size, respectively. The e-, s-, a-, b-, and v-coefficients and the constant, c, are determined via multiparameter linear least squares regression analysis of a data set comprised of solutes with known E, S, A, B, and V values and which span a reasonably wide range in interaction abilities. Thus, LSERs are designed to probe the type and relative importance of the interactions that govern solute retention. In this review, we include a synopsis of the various solvent and solute scales in common use in chromatography. More importantly, we emphasize the development and physico-chemical basis of - and thus meaning of - the solute parameters. After establishing the meaning of the parameters, we discuss their use in LSERs as applied to understanding the intermolecular interactions governing various gas-liquid and liquid-liquid phase equilibria. The gas-liquid partition process is modeled as the sum of an endoergic cavity formation/solvent reorganization process and exoergic solute-solvent attractive forces, whereas the partitioning of a solute between two solvents is thermodynamically

  13. 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

  14. [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

  15. 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.

  16. 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.

  17. Characterization of annular two-phase gas-liquid flows in microgravity

    NASA Technical Reports Server (NTRS)

    Bousman, W. Scott; Mcquillen, John B.

    1994-01-01

    A series of two-phase gas-liquid flow experiments were developed to study annular flows in microgravity using the NASA Lewis Learjet. A test section was built to measure the liquid film thickness around the perimeter of the tube permitting the three dimensional nature of the gas-liquid interface to be observed. A second test section was used to measure the film thickness, pressure drop and wall shear stress in annular microgravity two-phase flows. Three liquids were studied to determine the effects of liquid viscosity and surface tension. The result of this study provide insight into the wave characteristics, pressure drop and droplet entrainment in microgravity annular flows.

  18. Gas chromatography analysis of cellular fatty acids and neutral monosaccharides in the identification of lactobacilli.

    PubMed Central

    Rizzo, A F; Korkeala, H; Mononen, I

    1987-01-01

    Cellular fatty acids and monosaccharides in a group of 14 lactobacilli were analyzed by gas chromatography and the identity of the components was confirmed by gas chromatography-mass spectrometry. From the same bacterial sample, both monosaccharides and fatty acids were liberated by methanolysis, and in certain experiments, fatty acids alone were released by basic hydrolysis. The results indicate that basic hydrolysis gave more comprehensive information about the fatty acids, but the analysis of monosaccharides was found to be much more useful in distinguishing between different species of lactobacilli. The method described allowed differentiation of 11 of 14 Lactobacillus species, and even single colonies isolated from agar plates could be used for analysis without subculturing. PMID:3435147

  19. 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

  20. Venus lower atmospheric composition: analysis by gas chromatography.

    PubMed

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

    1979-02-23

    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 parts per million (ppm)], argon (18.6 ppm), neon (4.31 ppm), and sulfuir 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 clould tops to their bottoms, as implied by Earth-based observations and these resuilts, 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. PMID:17833004

  1. 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

  2. Fast gas chromatography for pesticide residues analysis using analyte protectants.

    PubMed

    Kirchner, Michal; Húsková, Renáta; Matisová, Eva; Mocák, Ján

    2008-04-01

    Fast GC-MS with narrow-bore columns combined with effective sample preparation technique (QuEChERS method) was used for evaluation of various calibration approaches in pesticide residues analysis. In order to compare the performance of analyte protectants (APs) with matrix-matched standards calibration curves of selected pesticides were searched in terms of linearity of responses, repeatability of measurements and reached limit of quantifications utilizing the following calibration standards in the concentration range 1-500 ng mL(-1)(the equivalent sample concentration 1-500 microg kg(-1)): in neat solvent (acetonitrile) with/without addition of APs, matrix-matched standards with/without addition of APs. For APs results are in a good agreement with matrix-matched standards. To evaluate errors of determination of concentration synthetic samples at concentration level of pesticides 50 ng mL(-1) (50 microg kg(-1)) were analyzed and quantified using the above given standards. For less troublesome pesticides very good estimation of concentration was obtained utilizing APs, while for more troublesome pesticides such as methidathion, malathion, phosalone and deltamethrin significant overestimation reaching up to 80% occurred. According to presented results APs can be advantegously used for "easy" pesticides determination. For "difficult" pesticides an alternative calibration approach is required for samples potentially violating MRLs. An example of real sample measurement is shown. In this paper also the use of internal standards (triphenylphosphate (TPP) and heptachlor (HEPT)) for peak areas normalization is discussed in terms of repeatability of measurements and quantitative data obtained. TPP normalization provided slightly better results than the use of absolute peak areas measurements on the contrary to HEPT. PMID:17920613

  3. 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

  4. 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.

  5. 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)

  6. 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...

  7. 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 ...

  8. 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

  9. 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

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

    NASA Astrophysics Data System (ADS)

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

    2010-03-01

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

  11. Effect of a falling gas-liquid absorption film temperature on entropy generation

    NASA Astrophysics Data System (ADS)

    Chermiti, Imen; Hidouri, Nejib; Brahim, Ammar Ben

    2013-08-01

    In this paper, an analytical study about the effect of a falling gas-liquid absorption film temperature on entropy generation is carried out. Entropy generation formulations due to viscous effects and mass transfer are derived. Results in terms of viscous, mass transfer and total irreversibilities are graphically presented and discussed.

  12. 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.

  13. On the possibility of shear-driven chromatography: a theoretical performance analysis.

    PubMed

    Desmet, G; Baron, G V

    1999-09-01

    The use of shear forces for the generation of the mobile phase flow in chromatographic separations is proposed. This novel chromatographic operating principle, referred to as shear-driven chromatography (SDC), completely circumvents the pressure-drop limitation of conventional pressure-driven GC and LC without affecting the operational flexibility (choice of mobile and stationary phases, possibility of solvent and/or temperature programming, etc.). In the present paper, the expression for the height equivalent to a theoretical plate in SDC in a channel with a flat rectangular cross-section is established and is used to demonstrate the large gain in analysis speed under LC, GC and supercritical fluid chromatography conditions. PMID:10514973

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

    PubMed

    Rao, Ramisetti Nageswara

    2014-08-01

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

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

    USGS Publications Warehouse

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

    1989-01-01

    A mixture of closely related streptomyces fermentation products, antimycin A, Is separated, and the components are identified by using reversed-phase high-performance liquid chromatography with directly linked 400-MHz proton nuclear magnetic resonance detection. Analyses of mixtures of three amino acids, alanine, glycine, and valine, are used to determine optimal measurement conditions. Sensitivity increases of as much as a factor of 3 are achieved, at the expense of some loss in chromatographic resolution, by use of an 80-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. A Size-Exclusion Chromatography Method for Analysis of Clostridium difficile Vaccine Toxins.

    PubMed

    Lancaster, Catherine; Rustandi, Richard R; Pannizzo, Paola; Ha, Sha

    2016-01-01

    High-performance size-exclusion chromatography (HPSEC or SEC) is a method that can be applied to measure size distribution of proteins, including aggregates, monomers, and fragments. In the biopharmaceutical industry the quantitation of aggregates contained in biotherapeutics and protein-based vaccines is critical given the potential impact on safety, immunogenicity, and efficacy. Hence, aggregation analysis of therapeutic proteins or protein-based vaccine products is almost always a requirement of regulatory agencies. SEC, also referred to as gel-filtration chromatography, separates molecules by size through a porous resin stationary phase. Under isocratic flow small molecules are retained on the column longer than large molecules. Here we describe the use of this SEC technique to characterize aggregation levels for four different protein antigens for a Clostridium difficile vaccine. PMID:27507349

  17. Confirmational analysis of beta-agonists by cryotrapping gas chromatography-Fourier transform infrared spectrometry.

    PubMed

    Visser, T; Vredenbregt, M J; de Jong, A P; van Rossum, H J; Stephany, R W; van Ginkel, L A

    1994-12-01

    Cryotrapping gas chromatography-Fourier transform infrared spectrometry has been used for confirmation analysis of the beta-agonists clenbuterol, salbutamol, mabuterol, bromobuterol, cimaterol, cimbuterol and mapenterol in urine and liver samples of veal calves, subsequent to selected ion detection gas chromatography-mass spectrometry. Samples have been analysed as their trimethylsilyl and methylboronate derivatives. Methylboronate derivatives yielded strongly diminished chemical background and interference levels in the infrared chromatograms of standards and samples. The limit of identification for methylboronate derivatives was at the low ppb level in incurred samples. The similarity of analyte and reference spectra, together with the retention time, was found to be a useful criterion for confirmation of unknown compounds. PMID:7879875

  18. Structural analysis of commercial ceramides by gas chromatography-mass spectrometry.

    PubMed

    Bleton, J; Gaudin, K; Chaminade, P; Goursaud, S; Baillet, A; Tchapla, A

    2001-05-11

    A simple method using gas chromatography-mass spectrometry was applied to analyse structures of ceramides. Identification of trimethylsilylated ceramides were obtained in short analysis times (derivatization of ceramides in 30 min at room temperature and 20 min gas chromatography mass spectrometry run) even for complex mixtures. For example in ceramide Type III, 18 peaks were observed which represent 27 various structures. The coeluted compounds were ceramides containing the same functional groups and the same carbon number but with a different distribution on the two alkyl chains of the molecule. They were accurately differentiated by mass spectrometry. Therefore, 83 structures of trimethylsilylated ceramides were identified in 11 different commercial mixtures. For 52 structures of these, mass spectral data were not described in the literature, neither full mass spectra nor characteristic fragments. PMID:11403477

  19. 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.

  20. 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

  1. [Microchip-based reversed-phase liquid chromatography-tandem mass spectrometry platform for protein analysis].

    PubMed

    Liang, Yu; Wu, Ci; Dai, Zhongpeng; Liang, Zuocheng; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

    2011-06-01

    Due to the high throughput and high sensitivity, the hyphenation of microchip-based high performance liquid chromatography with tandem mass spectrometry has been paid much attention. In our recent work, with poly (lauryl methacrylate-co-trimethylolpropane trimethacrylate) monolithic materials prepared in microchannels as trap and separation columns, conventional micro-liquid chromatography pumps and valves for fluidic control, and a small-bore open-tube capillary attached to the outlet channel as chip-mass spectrometer (MS) interface, the microchip-based reversed-phase liquid chromatography-tandem mass spectrometry (RPLC-MS/MS) platform was established, and applied for the identification of proteins. By such platform, 100 ng digest of bovine serum albumin (BSA) was successfully analyzed with the sequence coverages as 39.37%, 37.89% and 34.10% (with the relative standard deviation (RSD) of 7.3%) in three runs, separately. To evaluate the chip-to-chip reproducibility, BSA was identified by such platform with the microchips from different batches containing trap column, separation column and chip-MS interface. The obtained sequence coverage and the number of peptides identified were comparable. All these results showed high sensitivity and good reproducibility of such platform, demonstrating the great potential for rapid protein analysis. PMID:22032155

  2. Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry.

    PubMed

    Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E

    2015-09-01

    An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. PMID:26354690

  3. Evaluation of vermicompost maturity using scanning electron microscopy and paper chromatography analysis.

    PubMed

    Senthil Kumar, D; Satheesh Kumar, P; Rajendran, N M; Uthaya Kumar, V; Anbuganapathi, G

    2014-04-01

    Vermicompost was produced from flower waste inoculated with biofertilizers using the earthworm Eisenia fetida. Principal component analysis (PCA) and cluster analysis (CA) were carried out on the basis of physicochemical parameters of vermicomposted samples. From the results of the PCA and CA, it was possible to classify two different groups of vermicompost samples in the following categories: E2 and E5; and E1, E3, E4, and control. Scanning electron microscopy and biodynamic circular paper chromatography analysis were used to investigate the changes in surface morphology and functional groups in the control and vermicompost products. SEM analysis of E1-E5 shows more fragment and pores than the control. Chromatographic analysis of vermicompost indicated the mature condition of the compost materials. PMID:24634991

  4. Liquid chromatography mass spectrometric analysis of ouabainlike factor in biological fluid.

    PubMed

    Komiyama, Y; Nishimura, N; Dong, X H; Hirose, S; Kosaka, C; Masaki, H; Masuda, M; Takahashi, H

    2000-09-01

    Ouabainlike factor (OLF), assayed as ouabainlike immunoreactivity (OLI), is a probable endogenous digitalislike factor (EDLF). Liquid chromatography/mass spectrometry (LC/MS) is one of the most highly sensitive tools for obtaining structural information regarding low-molecular weight materials in a target compound, and to measure the concentrations of these materials. We have previously reported that OLI can be isolated from the culture supernatant of the rat pheochromocytoma cell line, PC12, by several reverse-phase chromatography and LC/MS techniques. The present study was performed to characterize OLF from biological fluids such as plasma and culture supernatant of PC12 cells by LC/MS. The previous applications of LC/MS to OLI in plasma have been limited to structural identification at the final stages of isolation, in which the starting volume of plasma has been over 10 I. In the present study, we tried to minimize the volume of plasma, and to develop a new preclearing step to gain adequate LC/MS characterization using MS/MS analysis. The plasma was acidified, and OLI was purified by ODS column chromatography. OLI in chromatographic fractions from plasma was assayed by a sensitive enzyme-linked immunosorbent assay for ouabain. After Sep-Pak treatment and two rounds of ODS column chromatography, OLI was identified from 80 ml of plasma. The structure of the purified OLI was identical to authentic ouabain and digoxin, as assessed by LC/MS. In conclusion, we identified the chemically or structurally clarified ouabain and digoxin as the circulating form in plasma by LC/MS. PMID:11016815

  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. 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

  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. Rapid chemical profiling of saponins in the flower buds of Panax notoginseng by integrating MCI gel column chromatography and liquid chromatography/mass spectrometry analysis.

    PubMed

    Yang, Wen-Zhi; Bo, Tao; Ji, Shuai; Qiao, Xue; Guo, De-An; Ye, Min

    2013-08-15

    The flower buds of Panax notoginseng (Notoginseng flower, FBP) are used as the traditional Chinese medicine San-Qi-Hua. In this study, we conducted column chromatography fractionation and liquid chromatography/mass spectrometry (LC/MS) analysis to comprehensively profile bioactive notoginseng saponins (ginsenosides) in FBP. MCI gel column chromatography allowed separation and enrichment of minor saponins. Electrospray ionization tandem mass spectrometry of [M-H](-) and [M+Na](+) precursor ions of the saponins provided reliable structural information for the sapogenin, and sequence of sugar chains. Confirmed by high-accuracy Q-TOF analysis, 170 notoginseng saponins were characterized from FBP, and 91 of them were reported from Panax species for the first time. The new ginsenosides contain acyl groups on α-chain, malonyl group at 20-OH, or di-malonyl groups. This study also indicated that the flower buds of P. notoginseng contained more protopanaxadiol-type but less protopanaxatriol-type ginsenosides than the roots. PMID:23561171

  9. 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

  10. 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

  11. 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

  12. 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

  13. 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

  14. High-throughput multiclass method for antibiotic residue analysis by liquid chromatography-tandem mass spectrometry.

    PubMed

    Chico, J; Rúbies, A; Centrich, F; Companyó, R; Prat, M D; Granados, M

    2008-12-12

    A simple and rapid method has been developed for the residue analysis of 39 antibiotics (tetracyclines, quinolones, penicillins, sulfonamides and macrolides) in foodstuffs of animal origin. The method combines an effective extraction technique, which uses water-methanol as extracting solvent, with ultra-high-pressure liquid chromatography-tandem mass spectrometry, allowing both confirmation and quantification in a single chromatographic run. The multiresidue method has been validated in chicken muscle matrix according to European Union Decision 2002/657/EC. It has been implemented as a routine method in a Public Health Laboratory, instead of the five plates test and LC methods previously used. PMID:18992888

  15. 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.

  16. Gas chromatography-mass spectrometry analysis of tert. -butyldimethylsilyl derivatives of 2-acetylaminofluorene and metabolites in isolated rat hepatocytes

    SciTech Connect

    Diez Ibanez, M.A.; Chessebeuf-Padieu, M.; Nordmann, P.; Padieu, P.

    1987-09-01

    A new technique for the conversion of 2-acetylaminofluorene and several ring-hydroxylated metabolites to mono- and di-tert.-butyldimethylsilyl derivatives was developed to permit their analysis by gas chromatography-mass spectrometry in order to quantify the metabolism of 2-acetylaminofluorene incubated in freshly isolated rat hepatocytes. This new gas chromatography-mass spectrometry method allowed the separation, identification and quantitation of seven known metabolites comprising five arylhydroxylated compounds, 2-aminofluorene and N-hydroxy-2-acetylaminofluorene.

  17. 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)

  18. 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

  19. BIOINTERACTION ANALYSIS BY HIGH-PERFORMANCE AFFINITY CHROMATOGRAPHY: KINETIC STUDIES OF IMMOBILIZED ANTIBODIES

    PubMed Central

    Nelson, Mary Anne; Moser, Annette; Hage, David S.

    2009-01-01

    A system based on high-performance affinity chromatography was developed for characterizing the binding, elution and regeneration kinetics of immobilized antibodies and immunoaffinity supports. This information was provided by using a combination of frontal analysis, split-peak analysis and peak decay analysis to determine the rate constants for antibody-antigen interactions under typical sample application and elution conditions. This technique was tested using immunoaffinity supports that contained monoclonal antibodies for 2,4-dichlorophenoxyacetic acid (2,4-D). Association equilibrium constants measured by frontal analysis for 2,4-D and related compounds with the immobilized antibodies were 1.7–12 × 106 M−1 at pH 7.0 and 25°C. Split-peak analysis gave association rate constants of 1.4–12 × 105 M−1s−1 and calculated dissociation rate constants of 0.01–0.4 s−1 under the application conditions. Elution at pH 2.5 for the analytes from the antibodies was examined by peak decay analysis and gave dissociation rate constants of 0.056–0.17 s−1. A comparison of frontal analysis results after various periods of column regeneration allowed the rate of antibody regeneration to be examined, with the results giving a first-order regeneration rate constant of 2.4 × 10−4 s−1. This combined approach and the information it provides should be useful in the design and optimization of immunoaffinity chromatography and other analytical methods that employ immobilized antibodies. The methods described are not limited to the particular analytes and antibodies employed in this study but should be useful in characterizing other targets, ligands and supports. PMID:19394281

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

    PubMed

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

    2014-10-01

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

  1. 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

  2. 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.

  3. 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

  4. 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.

  5. Effect of surface condition on the flow in segmented gas-liquid microreactors

    NASA Astrophysics Data System (ADS)

    Pouya, Shahram; Koochesfahani, Manoochehr

    2010-11-01

    The mixing process within segmented gas-liquid microreactors is of significance importance in design and optimization of devices for high throughput material synthesis. In a typical slug flow regime the liquid slugs are connected through a thin liquid film that plays an important role in hydrodynamics of the microreactor flow. Among the parameters that can influence the thin film layer, and the overall flow, is the surface condition of microchannel walls. We present preliminary results of this influence in the segmented gas-liquid flow of Ethanol/Nitrogen within PDMS microreactors. The results are presented specifically for microreactors with different level of roughness on the channel walls. The range of stable slug flow regime and behavior of liquid film are studied as a function of surface roughness.

  6. 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.

  7. 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

  8. Linked Gas Chromatography/Fourier Transform Infrared Spectrometry/Fourier Transform Mass Spectrometry For Mixture Analysis

    NASA Astrophysics Data System (ADS)

    Laude, David A., Jr.; Johlman, Carolyn; Wilkins, Charles L.

    1985-12-01

    During the past few years it has been demonstrated that linkage of multiple spectrometry systems with gas chromatography (GC) offers significant advantages for structural analysis of mixture components as they are sepa-rated. In the work to be described, a Fourier transform mass spectrometer (FTMS) has been linked in parallel with a Fourier transform infrared (FTIR) spectrometer for concurrent analysis of GC eluants from a fused silica capillary column. This system provides FTIR, electron impact, and chemical ionization mass spectral analysis of each mixture component as it emerges from the GC. Furthermore, mass measurement accuracy in the low ppm range in the absence of calibrant is made possible by the FTMS. Effective use of the com-plementary information obtained is shown to produce more reliable analytical performance than for any individual measurement.

  9. 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

  10. Slug frequency in horizontal gas-liquid flow

    SciTech Connect

    Wallis, G.B. )

    1990-02-01

    This report responds to American Gas Association's(AGA's) objective of initiating and planning means to create a reliable, mechanistic method of slug frequency prediction. Specific objectives were to: update the prior review of existing knowledge; identify one or more alternative modelling approaches; and recommend additional work if required. Examination of empirical correlations for slug frequency shows that they have uncertainties which are large compared with experimental data. A mechanistic approach is sought. Previous mechanistic models have been either incomplete or numerically unstable. Several improvements were made to the Taitel-Dukler model for this process and a new calculation procedure developed using the method of characteristics. It is demonstrated here that this approach alone cannot lead to cyclic slug formation. The processes of wave growth continually wash out downstream without causing new slugs to form upstream. This has led to concentration on the mechanism of slug formation near the inlet to a pipe segment. A new mechanism for cyclic slug formation, dependent on inlet boundary conditions, is proposed and a preliminary analysis developed. It is hypothesized that the formation of each slug transmits pressure fluctuations to the inlet and initiates perturbations there which eventually grow to form a new slug. Given the importance of the inlet conditions in determining slug frequency, lack of detailed knowledge of the boundary conditions for existing slug frequency data precludes meaningful comparisons with those data. It is proposed to develop this theory further and compare it with detailed observations in a small scale air-water test facility where the inlet boundary conditions are well characterized and well controlled in a systematic manner. When the theory is mature, its results will be correlated in a form suitable for practical use. 14 refs., 14 figs.

  11. Some spectral and pulsation characteristics of a horizontal gas-liquid stream

    NASA Astrophysics Data System (ADS)

    Krokovnyi, P. M.

    1980-07-01

    In the experiments described, the turbulence characteristics of a two-phase gas-liquid pipe flow were studied, using a 6 m long, 19-mm-diam tube. The inlet temperature of the suspension was maintained at 25 C. The friction energy spectra and the relative intensity of the friction pulsations were measured. The spectral and pulsation characteristics were obtained by an electrodiffusion technique which provided reliable data on the pulsations of the wall shear stress.

  12. Some spectral and pulsation characteristics of the horizontal flow of a gas-liquid suspension

    NASA Astrophysics Data System (ADS)

    Krokovnyi, P. M.

    1980-02-01

    In the experiments described, the turbulence characteristics of a two-phase gas-liquid pipe flow were studied, using a 6 m long, 19-mm-diam tube. The inlet temperature of the suspension was maintained at 25 C. The friction energy spectra and the relative intensity of the friction pulsations were measured. The spectral and pulsation characteristics were obtained by an electrodiffusion technique which provided reliable data on the pulsations of the wall shear stress.

  13. 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

  14. 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

  15. Capillary Liquid Chromatography Mass Spectrometry Analysis of Intact Monolayer-Protected Gold Clusters in Complex Mixtures.

    PubMed

    Black, David M; Bach, Stephan B H; Whetten, Robert L

    2016-06-01

    In some respects, large noble-metal clusters protected by thiolate ligands behave as giant molecules of definite composition and structure; however, their rigorous analysis continues to be quite challenging. Analysis of complex mixtures of intact monolayer-protected clusters (MPCs) by liquid chromatography mass spectrometry (LC-MS) could provide quantitative identification of the various components present. This advance is critical for biomedical and toxicological research, as well as in fundamental studies that rely on the identification of selected compositions. This work expands upon the separate LC and MS results previously achieved, by interfacing the capillary liquid chromatograph directly to the electrospray source of the mass spectrometer, in order to provide an extremely sensitive, quantitative, and rapid means to characterize MPCs and their derivatives far beyond that of earlier reports. Here, we show that nonaqueous reversed-phase chromatography can be coupled to mass-spectrometry detection to resolve complex mixtures in minute (∼100 ng) samples of gold MPCs, of molecular masses up to ∼40 kDa, and with single-species sensitivity easily demonstrated for components on the level of sub-10 ng or picomole (1 pmol). PMID:27216373

  16. 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

  17. Quantitative analysis of benzodiazepines in vitreous humor by high-performance liquid chromatography

    PubMed Central

    Bazmi, Elham; Behnoush, Behnam; Akhgari, Maryam; Bahmanabadi, Leila

    2016-01-01

    Objective: Benzodiazepines are frequently screened drugs in emergency toxicology, drugs of abuse testing, and in forensic cases. As the variations of benzodiazepines concentrations in biological samples during bleeding, postmortem changes, and redistribution could be biasing forensic medicine examinations, hence selecting a suitable sample and a validated accurate method is essential for the quantitative analysis of these main drug categories. The aim of this study was to develop a valid method for the determination of four benzodiazepines (flurazepam, lorazepam, alprazolam, and diazepam) in vitreous humor using liquid–liquid extraction and high-performance liquid chromatography. Methods: Sample preparation was carried out using liquid–liquid extraction with n-hexane: ethyl acetate and subsequent detection by high-performance liquid chromatography method coupled to diode array detector. This method was applied to quantify benzodiazepines in 21 authentic vitreous humor samples. Linear curve for each drug was obtained within the range of 30–3000 ng/mL with coefficient of correlation higher than 0.99. Results: The limit of detection and quantitation were 30 and 100 ng/mL respectively for four drugs. The method showed an appropriate intra- and inter-day precision (coefficient of variation < 10%). Benzodiazepines recoveries were estimated to be over 80%. The method showed high selectivity; no additional peak due to interfering substances in samples was observed. Conclusion: The present method was selective, sensitive, accurate, and precise for the quantitative analysis of benzodiazepines in vitreous humor samples in forensic toxicology laboratory.

  18. Reaction flow chromatography for rapid post column derivatisations: the analysis of antioxidants in natural products.

    PubMed

    Camenzuli, M; Ritchie, H J; Dennis, G R; Shalliker, R A

    2013-08-16

    The analysis of antioxidants from complex samples is conveniently achieved using liquid chromatography, which provides sample fraction, coupled with an on-line antioxidant assay, which provides detection. One particularly useful on-line antioxidant assay that has routinely been coupled with HPLC involves the diphenylpicrylhydrazyl radical (DPPH), which provides a positive test for phenolic antioxidants through a decolorisation of the DPPH reagent. A limitation of this assay, however, is the need to employ a reaction coil, which is often large with respect to the peak volume, consequently adding substantial band broadening to the separation. In this study we introduce a new concept that can be employed for systems requiring post column derivatisations, such as the DPPH assay. We have termed this 'reaction flow' chromatography, whereby, the derivatisation reagent can be added directly into one of the outlet ports of a parallel segmented flow column. Subsequently, the mixing between the derivatising reagent and the solute is very efficient removing the need to employ reaction coils. The concept is tested here using the DPPH assay for the analysis of antioxidants in samples derived from natural origin. PMID:23849586

  19. 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.

  20. 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.

  1. Influence of two-phase gas-liquid interaction on aerosol deposition in airways.

    PubMed

    Kim, C S; Abraham, W M; Chapman, G A; Sackner, M A

    1985-04-01

    Many patients with chronic simple bronchitis, viz., chronic productive cough without major airway obstruction, frequently show enhanced aerosol deposition in the airways. We hypothesized that this phenomenon might relate in part to wave motion of an accumulated layer of mucus caused by dynamic, two-phase gas-liquid interactions. In the present investigation, two-phase gas-liquid interaction was demonstrated in vivo by observing wave motion during tidal breathing of radiopaque-labeled viscous and viscoelastic fluids that had been added to distal tracheas of conscious sheep. Total aerosol deposition in the lung and mean pulmonary resistance (RL) were measured after addition of 4 to 10 ml of viscoelastic or viscous fluids to the distal main bronchi of conscious sheep. Change in aerosol deposition over baseline after fluid addition was compared with change in RL. In 21 experiments, 5 for each of 3 viscoelastic fluids with varying characteristics and 6 for a viscous fluid, aerosol deposition was significantly enhanced in every experiment, irrespective of the type of fluid added. This increase in aerosol deposition ranged from 13 to 66% above baseline. The RL increased in 5 of the 6 experiments with viscous fluid and in 4 of the 15 experiments with viscoelastic fluids. There was less wavelike motion with viscous than with viscoelastic fluids. These results suggest that two-phase gas-liquid interaction in the airways can account for increased aerosol deposition with little alteration in airway resistance. PMID:3994158

  2. 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.

  3. Low-frequency sound transmission through a gas-liquid interface.

    PubMed

    Godin, Oleg A

    2008-04-01

    Typically, sound speed in gases is smaller and mass density is much smaller than in liquids, resulting in a very strong acoustic impedance contrast at a gas-liquid interface. Sound transmission through a boundary with a strong impedance contrast is normally very weak. This paper studies the power output of localized sound sources and acoustic power fluxes through a plane gas-liquid interface in a layered medium. It is shown that, for low-frequency sound, a phenomenon of anomalous transparency can occur where most of the acoustic power generated by a source in a liquid half-space can be radiated into a gas half-space. The main physical mechanism responsible for anomalous transparency is found to be an acoustic power transfer by inhomogeneous (evanescent) waves in the plane-wave decomposition of the acoustic field in the liquid. The effects of a liquid's stratification and of guided sound propagation in the liquid on the anomalous transparency of the gas-liquid interface are considered. Geophysical and biological implications of anomalous transparency of water-air interface to infrasound are indicated. PMID:18396996

  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. Calculations of Gas-liquid Equilibrium in Wellbore with High Carbon dioxide Flow

    NASA Astrophysics Data System (ADS)

    Zhang, Jiaming; Wu, Xiaodong; Wang, Bo; Liu, Kai; Gao, Yue

    2014-05-01

    Carbon dioxide injection not only enhances the oil recovery dramatically, but also it will reduce the greenhouse effect, therefore, Carbon dioxide injection technique is applied extensively. During the process of carbon dioxide displacement, when carbon dioxide breaks though into oil production wells, carbon dioxide content will impacts the phase state and physical properties of the mixed liquor in the wellbore, as a result, it will affect the calculation of temperature and pressure in oil production wells. Applying the conventional black-oil model to calculate the phase state of the miscible fluids is unacceptable. To tackle the problem, this paper uses the gas-liquid flash theory and component model to program software, so that the phase state (gas, liquid or gas-liquid) and physical properties of the mixed liquor (including hydrogen sulfide, carbon dioxide and hydrocarbon) under initial conditions is calculated, moreover, the impact of carbon dioxide content on the physical properties(mainly including density, viscosity, specific heat at const pressure, surface tension, etc) of mixed liquor in oil production wells is analyzed in this paper. The comparison of the results shows that this model can meet the engineering needs with high accuracy.

  6. MIGRATION OF GAS-LIQUID INCLUSIONS IN KCl AND NaCl SINGLE CRYSTALS

    SciTech Connect

    Olander, Donald R.; Machiels, Albert J.; Muchowski, Eugen

    1980-08-01

    Natural salt deposits contain small brine inclusions which can be set into motion by a temperature gradient arising from storage of nuclear wastes in the salt. Inclusions totally filled with liquid move up the temperature gradient, but cavities which are filled partly with liquid and partly by an insoluble gas move in the opposite direction. The velocities of these gas-liquid inclusions are calculated from a model which includes: heat transport in the gas/liquid/solid composite medium; vapor transport of water in the gas bubble as the principal mechanism causing cavity motion; and the effect of molecular and thermal diffusion on transport of salt in the liquid phase. An analytical expression for the inclusion velocity is obtainable with certain simplifications, which include: approximating the cubical cavity in the solid as a spherical hole containing a central gas bubble and an annular shell of liquid; neglecting interface kinetics (i.e., slow dissolution and crystallization steps) and assuming the process to be diffusion-controlled and disregarding fluid motion generated by surface tension gradients at the gas/liquid interface. The theory predicts a change in the migration direction at a critical volume fraction gas in the cavity. For gas fractions greater than this critical value, the theory gives the velocities of migration down the temperature gradient which are in satisfactory agreement with available experimental data.

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

    PubMed

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

    2014-09-01

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

  8. Analysis of Estrogens and Androgens in Postmenopausal Serum and Plasma by Liquid Chromatography-Mass Spectrometry

    PubMed Central

    Wang, Qingqing; Bottalico, Lisa; Mesaros, Clementina; Blair, Ian A.

    2014-01-01

    Liquid chromatography-selected reaction monitoring/mass spectrometry-based methodology has evolved to the point where accurate analyses of trace levels of estrogens and androgens in postmenopausal serum and plasma can be accomplished with high precision and accuracy. A suite of derivatization procedures has been developed, which together with modern mass spectrometry instrumentation provide investigators with robust and sensitive methodology. Preionized derivatives are proving to be useful as they are not subject to suppression of the electrospray signal. Postmenopausal women with elevated plasma or serum estrogens are thought to be at increased risk for breast and endometrial cancer. Therefore, significant advances in risk assessment should be possible now that reliable methodology is available. It is also possible to conduct analyses of multiple estrogens in plasma or serum. Laboratories that are currently employing liquid chromatography/mass spectrometry methodology can now readily implement this strategy. This will help conserve important plasma and serum samples available in Biobanks, as it will be possible to conduct high sensitivity analyses using low initial sample volumes. Reported levels of both conjugated and non-conjugated estrogen metabolites are close to the limits of sensitivity of many assays to date, urging caution in the interpretation of these low values. The analysis of serum androgen precursors in postmenopausal women has not been conducted routinely in the past using liquid chromatography/mass spectrometry methodology. Integration of serum androgen levels into the panel of metabolites analyzed could provide additional information for assessing cancer risk and should be included in the future. PMID:25150018

  9. 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

  10. 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

  11. Phytochemical analysis of Hibiscus caesius using high performance liquid chromatography coupled with mass spectrometry.

    PubMed

    Ain, Quratul; Naveed, Muhammad Na; Mumtaz, Abdul Samad; Farman, Muhammad; Ahmed, Iftikhar; Khalid, Nauman

    2015-09-01

    Various species in genus Hibiscus are traditionally known for their therapeutic attributes. The present study focused on the phytochemical analysis of a rather unexplored species Hibiscus caesius (H. caesius), using high-pressure liquid chromatography coupled with mass spectrometry (HPLC-MS). The analysis revealed five major compounds in the aqueous extract, viz. vanillic acid, protocatechoic acid, quercetin, quercetin glucoside and apigenin, being reported for the first time in H. caesius. Literature suggests that these compounds have important pharmacological traits such as anti-cancer, anti-inflammatory, anti-bacterial and hepatoprotective etc. however, this requires further pharmacological investigations at in vitro and in vivo scale. The above study concluded the medicinal potential of H. caesius. PMID:26408882

  12. [Analysis of amines in water samples by high performance liquid chromatography-laser induced fluorescence detection].

    PubMed

    Liu, Fan; Gao, Fangyuan; Tang, Tao; Sun, Yuanshe; Li, Tong; Zhang, Weibing

    2013-11-01

    A sensitive high performance liquid chromatography (HPLC)-laser induced fluorescence detection (LIFD) method was developed for the determination of amines. The derivatization and separation conditions were investigated. Under the optimized conditions, spermidine, putrescine and histamine were analyzed. The limits of detection (LODs) of the three biogenic amines (S/N = 3) were as low as 10(-10) mol/L. This method showed excellent stability. The RSDs of retention times and peak areas of the three biogenic amines were lower than 0.3% and 3%, respectively. This method was applied in biogenic amine analysis in water samples, and the average recoveries were in the range of 94.99%-104.7%. Furthermore, the amines in seven tea samples were analyzed by this method, and satisfactory results were achieved. The developed assay is of excellent sensitivity and good reproducibility, which can be used in the analysis of the amines in water samples. PMID:24558849

  13. Analysis of fatty oil in Semen Ziziphi Spinosae by capillary gas chromatography.

    PubMed

    Yu-Juan, Li; Kai-Shun, Bi; Xin-Miao, Liang; Hong-Bin, Xiao

    2003-01-01

    A simple and fast capillary gas chromatographic (CGC) method with flame ionization detection is developed for the analysis of fatty oil in Semen Ziziphi Spinosae. After methyl-esterification, eight components are identified by gas chromatography-mass spectrometry. The derivatization condition is investigated in order to validate this method. Palmitic acid and stearic acid are quantitated simultaneously. The limits of detection are 5.024 microg/mL for palmitic acid and 6.957 microg/mL for stearic acid, respectively. The limits of quantitation are 16.76 microg/mL for palmitic acid and 23.19 microg/mL for stearic acid, respectively. The percent recoveries of palmitic and stearic acid are 97.4% and 96.6%. CGC is shown to be a quick and informative tool for the analysis of fatty oil in Semen Ziziphi Spinosae. PMID:12597596

  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. 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

  16. 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

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

    PubMed

    Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

    2015-11-01

    Bioactive botanicals contain natural compounds with specific biological activity, such as antibacterial, antioxidant, immune stimulating, and taste improving. A full characterization of the chemical composition of these botanicals is frequently necessary. A study of small carbohydrates from the plant materials of 18 bioactive botanicals is further described. The study presents the identification of the carbohydrate using a gas chromatographic-mass spectrometric analysis that allows detection of molecules as large as maltotetraose, after changing them into trimethylsilyl derivatives. A number of carbohydrates in the plant (fructose, glucose, mannose, sucrose, maltose, xylose, sorbitol, and myo-, chiro-, and scyllo-inositols) were quantitated using a novel liquid chromatography with tandem mass spectrometric technique. Both techniques involved new method developments. The gas chromatography with mass spectrometric analysis involved derivatization and separation on a Rxi(®)-5Sil MS column with H2 as a carrier gas. The liquid chromatographic separation was obtained using a hydrophilic interaction type column, YMC-PAC Polyamine II. The tandem mass spectrometer used an electrospray ionization source in multiple reaction monitoring positive ion mode with the detection of the adducts of the carbohydrates with Cs(+) ions. The validated quantitative procedure showed excellent precision and accuracy allowing the analysis in a wide range of concentrations of the analytes. PMID:26315495

  18. 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...

  19. 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

  20. Complementary fragmentation pattern analysis by gas chromatography-mass spectrometry and liquid chromatography tandem mass spectrometry confirmed the precious lignan content of Cirsium weeds.

    PubMed

    Boldizsár, I; Kraszni, M; Tóth, F; Noszál, B; Molnár-Perl, I

    2010-10-01

    In this paper, as novelties to the field, it is confirmed at first, that the fruits of Cirsium species, regarded as injurious weeds, do contain lignans, two, different butyrolactone-type glycoside/aglycone pairs: the well known arctiin/arctigenin and the particularly rare tracheloside/trachelogenin species. These experiences were supported by gas chromatography-mass spectrometry (GC-MS), by liquid chromatography tandem mass spectrometry (LC-MS/(MS)) and by nuclear magnetic resonance (NMR) spectroscopy. The study reflects the powerful impact of the complementary chromatographic mass fragmentation evidences resulting in the identification and quantification, the extremely rare, with on line technique not yet identified and described, tracheloside/trachelogenin pair lignans, without authentic standard compounds. Fragmentation pattern analysis of the trimethylsilyl (TMS) derivative of trachelogenin, based on GC-MS, via two different fragmentation pathways confirmed the detailed structure of the trachelogenin molecule. The complementary chromatographic evidences have been unambiguously confirmed, by (1)H and (13)C NMR analysis of trachelogenin, isolated by preparative chromatography. Identification and quantification of the fruit extracts of four Cirsium (C.) species (C. arvense, C. canum, C. oleraceum, and C. palustre), revealed that (i) all four species do accumulate the tracheloside/trachelogenin or the arctiin/arctigenin butyrolactone-type glycoside/aglycone pairs, (ii) the overwhelming part of lignans are present as glycosides (tracheloside 9.1-14.5 mg/g, arctiin 28.6-39.3 mg/g, expressed on dry fruit basis), (iii) their acidic and enzymatic hydrolyses to the corresponding aglycones, to trachelogenin and arctigenin are fast and quantitative and (iv) the many-sided beneficial trachelogenin and arctigenin can be prepared separately, without impurities, excellent for medicinal purposes. PMID:20813375

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

    SciTech Connect

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

    1982-10-01

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

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

    PubMed

    Ovando-Martínez, 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

  3. [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

  4. [Analysis of pigments from Rhodotorula glutinis by Raman spectroscopy and thin layer chromatography].

    PubMed

    Yuan, Yu-feng; Tao, Zhan-hua; Wang, Xue; Li, Yong-qing; Liu, Jun-xian

    2012-03-01

    The pigments from Rhodotorula glutinis were separated by using thin layer chromatography, and the result showed that Rhodotorula glutinis cells could synthesize at least three kinds of pigments, which were beta-carotene, torulene, and torularhodin. The Raman spectra based on the three pigments were acquired, and original spectra were preprocessed by background elimination, baseline correction, and three-point-smoothing, then the averaged spectra from different pigments were investigated, and the result indicated that Raman shift which represents C-C bond was different, and the wave number of beta-carotene demonstrated the largest deviation, finally torulene and torularhodin in Rhodotorula glutinis had more content than beta-carotene. Quantitative analysis of Raman peak height ratio revealed that peak height ratio of pigments showed little difference, which could be used as parameters for further research on living cells, providing reference content of pigments. The above results suggest that Raman spectroscopy combined with thin layer chromatography can be applied to analyze pigments from Rhodotorula glutinis, provides abundant information about pigments, and serves as an effective method to study pigments. PMID:22582635

  5. Routine application using single quadrupole liquid chromatography-mass spectrometry to pesticides analysis in citrus fruits.

    PubMed

    Soler, Carla; Mañes, Jordi; Picó, Yolanda

    2005-09-23

    A rapid and sensitive liquid chromatography-electrospray ionization-mass spectrometry method has been developed for the routine analysis of buprofezin, bupirimate, hexaflumuron, tebufenpyrad, fluvalinate and pyriproxyfen in citrus fruits. Extracts were obtained by matrix solid-phase dispersion (MSPD) using C18 as dispersant and dichloromethane-methanol (80:20, v/v) as eluent. Matrix effects were tested for all matrices by addition of standard to sample blank extracts (samples containing no detectable residues). Mean recoveries obtained at fortification levels between 0.01 and 5 mg kg(-1) were 57-97% with relative standard deviations (RSDs) from 5 to 19%. The limits of quantification (LOQ) were in the range of 0.01-0.2 mg kg(-1) and lower than maximum residue limits (MRLs) established by the Spanish legislation. The MSPD was compared with conventional ethyl acetate extraction, showing equivalent recoveries and precision. Although the sample is more concentrated (5-fold) by solid-liquid extraction (SLE) with ethyl acetate than by MSPD, LOQs obtained by both techniques, were almost equal, because MSPD reduces matrix effects, baseline noise, and interfering peaks from the matrix. The proposed method has been applied to the determination of selected pesticides in real samples. Liquid chromatography-tandem mass spectrometry (LC-MS-MS) with quadrupole ion trap (QIT) and triple quadrupole (TQ) have been used as confirmatory tool for positive samples according to a recent No. SANCO/10476/2003 European Union Guideline. PMID:16130755

  6. Analysis of aristolochic acids, aristololactams and their analogues using liquid chromatography tandem mass spectrometry.

    PubMed

    Yu, Jie; Ma, Chao-Mei; Wang, Xuan; Shang, Ming-Ying; Hattori, Masao; Xu, Feng; Jing, Yu; Dong, Shi-Wen; Xu, Yu-Qiong; Zhang, Cui-Ying; Cai, Shao-Qing

    2016-08-01

    More than 80 aristolochic acids (AAs) and aristololactams (ALs) have been found in plants of the Aristolochiaceae family, but relatively few have been fully studied. The present study aimed at developing and validating a liquid chromatography tandem mass spectrometry (LC/MS(n)) for the analysis of these compounds. We characterized the fragmentation behaviors of 31 AAs, ALs, and their analogues via high performance liquid chromatography coupled with electrospray ionization mass spectrometry. We summarized their fragmentation rules and used these rules to identify the constituents contained in Aristolochia contorta, Ar. debilis, Ar. manshurensis, Ar. fangchi, Ar. cinnabarina, and Ar. mollissima. The AAs and ALs showed very different MS behaviors. In MS(1) of AAs, the characteristic pseudomolecular ions were [M + NH4](+), [M + H](+), and [M + H - H2O](+). However, only [M + H](+) was found in the MS(1) of ALs, which was simpler than that of AAs. Distinct MS(n)fragmentation patterns were found for AAs and ALs, showing the same skeleton among the different substituent groups. The distribution of the 31 constituents in the 6 species of Aristolochia genus was reported for the first time. 25 Analogues of AAs and ALs were detected in this genus. A hierarchical schemes and a calculating formula of the molecular formula of these nitrophenanthrene carboxylic acids and their lactams were proposed. In conclusion, this method could be applied to identification of similar unknown constituents in other plants. PMID:27608953

  7. 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

  8. 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

  9. 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

  10. Liquid chromatography combined with mass spectrometry for 13C isotopic analysis in life science research.

    PubMed

    Godin, Jean-Philippe; Fay, Laurent-Bernard; Hopfgartner, Gérard

    2007-01-01

    Among the different disciplines covered by mass spectrometry, measurement of (13)C/(12)C isotopic ratio crosses a large section of disciplines from a tool revealing the origin of compounds to more recent approaches such as metabolomics and proteomics. Isotope ratio mass spectrometry (IRMS) and molecular mass spectrometry (MS) are the two most mature techniques for (13)C isotopic analysis of compounds, respectively, for high and low-isotopic precision. For the sample introduction, the coupling of gas chromatography (GC) to either IRMS or MS is state of the art technique for targeted isotopic analysis of volatile analytes. However, liquid chromatography (LC) also needs to be considered as a tool for the sample introduction into IRMS or MS for (13)C isotopic analyses of non-volatile analytes at natural abundance as well as for (13)C-labeled compounds. This review presents the past and the current processes used to perform (13)C isotopic analysis in combination with LC. It gives particular attention to the combination of LC with IRMS which started in the 1990's with the moving wire transport, then subsequently moved to the chemical reaction interface (CRI) and was made commercially available in 2004 with the wet chemical oxidation interface (LC-IRMS). The LC-IRMS method development is also discussed in this review, including the possible approaches for increasing selectivity and efficiency, for example, using a 100% aqueous mobile phase for the LC separation. In addition, applications for measuring (13)C isotopic enrichments using atmospheric pressure LC-MS instruments with a quadrupole, a time-of-flight, and an ion trap analyzer are also discussed as well as a LC-ICPMS using a prototype instrument with two quadrupoles. PMID:17853432

  11. 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.

  12. [Analysis of major components in water based stamp pad inks and their imprints by ultra high performance liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry].

    PubMed

    Zhang, Qing; Zou, Jixin; Shi, Gaojun; Zhang, Lijuan

    2010-12-01

    Ultra high performance liquid chromatography-mass spectrometry (UHPLC-MS) technology and gas chromatography-mass spectrometry (GC-MS) technology were used to qualitatively analyze the major components in water based stamp pad inks including major colorants and volatile components. After the samples were supersonically extracted and then centrifuged, UHPLC-MS was used to separate and identify the major colorants. A ZORBAX Eclipse Plus Phenyl-Hexyl (50 mm x 4.6 mm, 1.8 microm) column and 15 mmol/L ammonium acetate-acetonitrile were utilized for the separation and negative selected ion monitoring mode (SIM) was set for the MS analysis. An HP-INNOWAX (30 m x 0.25 mm, 0.25 microm) column was employed in the GC-MS analysis with the full-scan mode to determine the volatiles. This study demonstrated that the major colorants in the inks and their imprints were Acid Red R, Eosin Y and Pigment Red 112; and the major volatiles were glycerol, 1,2-propanediol, etc. The method is rapid and accurate. It also demonstrates that the method can meet the requirements for imprint determination in material evidence identification. The work provides a reliable tool for the categorization research in the forensic sciences. PMID:21438364

  13. 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

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

    PubMed

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

    1991-12-01

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

  15. 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

  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. Application of micellar electrokinetic capillary chromatography to the analysis of uncharged pesticides of environmental impact.

    PubMed

    Segura Carretero, Antonio; Cruces-Blanco, Carmen; Cortacero Ramírez, Sonia; Carrasco Pancorbo, Alegría; Fernández Gutiérrez, Alberto

    2004-09-22

    A test mixture of five pesticides and metabolites (naphthalene acetamide, carbaryl, 1-naphthol, thiabendazole, and carbendazime) has been investigated by capillary electrophoresis with an ultraviolet diode array detector. These compounds were separated in <10 min by micellar electrokinetic capillary chromatography (MEKC). MEKC was performed in 30 mM ammonium chloride/ammonia buffer (pH 9.0) containing 15 mM sodium dodecyl sulfate. The lowest detection limit was obtained for the insecticide carbaryl (0.22 microg mL(-)(1)) and the highest for its metabolite 1-naphthol (1.13 microg mL(-)(1)). This method was applied to the analysis of the pesticides in cultivated vegetables such as cucumbers, which were extracted with a liquid-liquid extraction procedure, obtaining recovery percentages ranging from 90.1 to 110.2%. PMID:15366822

  18. Headspace analysis of engine oil by gas chromatography/mass spectrometry.

    PubMed

    Levermore, D M; Josowicz, M; Rees, W S; Janata, J

    2001-03-15

    This study establishes the rationale necessary for determining the time to change engine oil. This is based on identifying gaseous components in new and used automobile lubricants. Key compounds, so-called "signature", are separated and identified qualitatively by coupled gas chromatography/mass spectrometry. Volatile antioxidants at zero miles and fuel contaminants at low mileage are observed in the headspace of engine oil. Several oxidative degradation components have been positively identified in the used oil, which include the following: acetaldehyde, acetone, butanal, 2-propanol, acetic acid, 2-hexanol, benzoic acid, benzaldehyde, and 1-pentanol. This study strongly suggests that the status of lubricating oil can be determined by the analysis of the gas phase above the oil. Most importantly, it opens the possibility of performing conditional maintenance of the combustion engine based on information obtained from gas sensors. PMID:11305675

  19. Quantitative analysis of oxytetracycline and related substances by high-performance liquid chromatography.

    PubMed

    Khan, N H; Roets, E; Hoogmartens, J; Vanderhaeghe, H

    1987-09-18

    Isocratic high-performance liquid chromatography on PLRP-S 8-microns poly(styrene-divinylbenzene) copolymer allows complete separation of oxytetracycline, 4-epioxytetracycline, tetracycline, anhydrooxytetracycline, alpha- and beta-apooxytetracycline. The mobile phase was tert.-butanol-0.2 M phosphate buffer pH 8.0-0.02 M tetrabutylammonium sulphate pH 8-0.0001 M sodium ethylenediaminetetraacetate pH 8.0-water (5.9:10:5:10:78.1, m/v/v/v/v). With this isocratic method, 2-acetyl-2-decarboxamidooxytetracycline is only partly resolved from oxytetracycline. The separation and the detection limits can be improved by the use of gradient elution. Gradient elution was used for the comparison of official standards and for the analysis of a number of commercial samples, and to monitor the stability of oxytetracycline hydrochloride during storage in the solid state for about 6 years at various temperatures. PMID:3693465

  20. Indirect hydrogen analysis by gas chromatography coupled to mass spectrometry (GC-MS).

    PubMed

    Varlet, V; Smith, F; Augsburger, M

    2013-08-01

    Gas chromatography (GC) is an analytical tool very useful to investigate the composition of gaseous mixtures. The different gases are separated by specific columns but, if hydrogen (H2 ) is present in the sample, its detection can be performed by a thermal conductivity detector or a helium ionization detector. Indeed, coupled to GC, no other detector can perform this detection except the expensive atomic emission detector. Based on the detection and analysis of H2 isotopes by low-pressure chemical ionization mass spectrometry (MS), a new method for H2 detection by GC coupled to MS with an electron ionization ion source and a quadrupole analyser is presented. The presence of H2 in a gaseous mixture could easily be put in evidence by the monitoring of the molecular ion of the protonated carrier gas. PMID:23893637

  1. 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

  2. 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…

  3. 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

  4. 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

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

    PubMed

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

    2012-11-30

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

  6. Derivatization of azaspiracid biotoxins for analysis by liquid chromatography with fluorescence detection.

    PubMed

    McCarron, Pearse; Giddings, Sabrina D; Miles, Christopher O; Quilliam, Michael A

    2011-11-01

    Azaspiracids (AZAs) are an important group of regulated lipophilic biotoxins that cause shellfish poisoning. Currently, the only widely available analytical method for quantitation of AZAs is liquid chromatography-mass spectrometry (LC-MS). Alternative methods for AZA analysis are needed for detailed characterization work required in the preparation of certified reference materials (CRMs) and by laboratories not equipped with LC-MS. Chemical derivatization of the amine and carboxyl groups on AZAs was investigated for the purpose of facilitating analysis by LC with fluorescence detection (FLD). Experiments towards chemical modification of AZA1 at the amine achieved only limited success. Derivatization of the carboxyl group, on the other hand, proved successful using the 9-anthryldiazomethane (ADAM) method previously applied to the okadaic acid (OA) group toxins. Extraction and clean-up methods were investigated for shellfish tissue samples and a post-reaction solid phase extraction procedure was developed for the AZA ADAM derivatives. Chromatographic separations were developed for the LC-FLD analysis of derivatized AZAs alone or in the presence of other derivatized toxins. This new analytical method for analysis of AZAs enabled verification of AZA1-3 concentrations in recently certified reference materials. The method demonstrated good linearity, repeatability and accuracy showing its potential as an alternative to LC-MS for measurement of AZAs. PMID:21968345

  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. 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.

  9. 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.

  10. 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.

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

    PubMed Central

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

    2014-01-01

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

  12. 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.

  13. Rapid Decomposition of Cellulose Dissolved in Ionic Liquid Using Gas-Liquid Interface Discharge

    NASA Astrophysics Data System (ADS)

    Furukawa, Shoichiro; Inoue, Nobuhiro; Ishioka, Toshio; Furuya, Kenji; Harata, Akira

    2012-07-01

    Cellulose was dissolved at 3 wt % in 15 mL of 1-allyl-3-methylimidazolium chloride ([Amim]Cl) together with 2 wt % water, and then gas-liquid interface discharge was carried out at 20 W for 200 s. As a result, 7.6% of initially dissolved cellulose decomposed and 3.9% of initially dissolved cellulose changed into reducing sugar. Adding a small amount of water to the solution was essential for the decomposition of cellulose. [Amim]Cl was stable against the discharge, as determined from the NMR signals measured before and after the discharge.

  14. 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.

  15. On the Motion of an Annular Film in Microgravity Gas-Liquid Flow

    NASA Technical Reports Server (NTRS)

    McQuillen, John B.

    2002-01-01

    Three flow regimes have been identified for gas-liquid flow in a microgravity environment: Bubble, Slug, and Annular. For the slug and annular flow regimes, the behavior observed in vertical upflow in normal gravity is similar to microgravity flow with a thin, symmetrical annular film wetting the tube wall. However, the motion and behavior of this film is significantly different between the normal and low gravity cases. Specifically, the liquid film will slow and come to a stop during low frequency wave motion or slugging. In normal gravity vertical upflow, the film has been observed to slow, stop, and actually reverse direction until it meets the next slug or wave.

  16. 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.

  17. 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 ...

  18. 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...

  19. 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...

  20. 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…

  1. 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)

  2. 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...

  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. Size distribution analysis of influenza virus particles using size exclusion chromatography.

    PubMed

    Vajda, Judith; Weber, Dennis; Brekel, Dominik; Hundt, Boris; Müller, Egbert

    2016-09-23

    Size exclusion chromatography is a standard method in quality control of biopharmaceutical proteins. In contrast, vaccine analysis is often based on activity assays. The hemagglutination assay is a widely accepted influenza quantification method, providing no insight in the size distribution of virus particles. Capabilities of size exclusion chromatography to complement the hemagglutination assay are investigated. The presented method is comparatively robust regarding different buffer systems, ionic strength and additive concentrations. Addition of 200mM arginine or sodium chloride is necessary to obtain complete virus particle recovery. 0.5 and 1.0M arginine increase the hydrodynamic radius of the whole virus particles by 5nm. Sodium citrate induces virus particle aggregation. Results are confirmed by dynamic light scattering. Retention of a H1N1v strain correlates with DNA contents between 5ng/mL and 670ng/mL. Quantitative elution of the virus preparations is verified on basis of hemagglutination activity. Elution of hemagglutination inducing compounds starts at a flow channel diameter of 7000nm. The universal applicability is demonstrated with three different influenza virus samples, including an industrially produced, pandemic vaccine strain. Size distribution of the pandemic H1N1v 5258, H1N1 PR/8/34, and H3N2 Aichi/2/68 preparations spreads across inter- and intra-particle volume and extends to the secondary interaction dominated range. Thus, virus particle debris seems to induce hemagglutination. Fragments generated by 0.5% Triton™ X-100 treatment increase overall hemagglutination activity. PMID:27578410

  5. Liquid chromatography – high resolution mass spectrometry analysis of fatty acid metabolism

    PubMed Central

    Kamphorst, Jurre J.; Fan, Jing; Lu, Wenyun; White, Eileen; Rabinowitz, Joshua D.

    2011-01-01

    We present a liquid chromatography – mass spectrometry (LC-MS) method for long-chain and very-long-chain fatty acid analysis, and its application to 13C-tracer studies of fatty acid metabolism. Fatty acids containing 14 to 36 carbon atoms are separated by C8 reversed-phase chromatography using a water-methanol gradient with tributylamine as ion pairing agent, ionized by electrospray, and analyzed by a stand-alone orbitrap mass spectrometer. The median limit of detection is 5 ng/ml with a linear dynamic range of 100-fold. Ratios of unlabeled to 13C-labeled species are quantitated precisely and accurately (average relative standard deviation 3.2% and deviation from expectation 2.3%). In samples consisting of fatty acids saponified from cultured mammalian cells, 45 species are quantified, with average intraday relative standard deviations for independent biological replicates of 11%. The method enables quantitation of molecular ion peaks for all labeled forms of each fatty acid. Different degrees of 13C-labeling from glucose and glutamine correspond to fatty acid uptake from media, de novo synthesis, and elongation. To exemplify the utility of the method, we examined isogenic cell lines with and without activated Ras oncogene expression. Ras increases the abundance and alters the labeling patterns of saturated and monounsaturated very-long-chain fatty acids, with the observed pattern consistent with Ras leading to enhanced activity of ELOVL4 or an enzyme with similar catalytic activity. This LC-MS method and associated isotope tracer techniques should be broadly applicable to investigating fatty acid metabolism. PMID:22004349

  6. Fast derivatization of fatty acids in different meat samples for gas chromatography analysis.

    PubMed

    Figueiredo, Ingrid Lima; Claus, Thiago; Oliveira Santos Júnior, Oscar; Almeida, Vitor Cinque; Magon, Thiago; Visentainer, Jesuí Vergilio

    2016-07-22

    In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R(2)=0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2-30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures. PMID:27320376

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

    PubMed

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

    2009-10-01

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

  8. 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

  9. 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.

  10. 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

  11. A simple ion chromatography method for inorganic anion analysis in edible seaweeds.

    PubMed

    Gómez-Ordóñez, Eva; Alonso, Esther; Rupérez, Pilar

    2010-09-15

    A new, simple, fast and sensitive ion chromatography (IC) method, for the simultaneous analysis of fluoride, chloride, nitrite, bromide, nitrate, phosphate and sulphate in edible seaweeds was developed and reported for the first time. The validation of the analytical method was studied in terms of linearity, sensitivity, precision and accuracy. All standard calibration curves showed very good correlation between anion peak area and concentration (r>0.999). Limits of detection and quantitation ranged between 0.002-0.05 mg/L and 0.01-0.1mg/L, respectively and indicated the high sensitivity of the method. Relative standard deviation values of repeatability and inter-day precision for standard anions with the same sample were less than 2%. Anion recoveries ranged from 97 to 113% for chloride and from 87 to 105% for sulphate, respectively and showed the fairly good accuracy of the method. The method was applied to the analysis of inorganic anions in brown and red edible seaweeds. Brown seaweeds were characterized by higher chloride content up to 33.7-36.9%, while red seaweeds were characterized by higher sulphate content (45-57%). Sulphate content in seaweeds is related to the presence of sulphated polysaccharides of biological importance. The method developed was well applicable to mineral anion analysis in edible seaweeds and shows suitability and reliability of use in other food samples of nutritional importance. PMID:20801334

  12. 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

  13. Multiresidue Analysis of Pesticides in Straw Roughage by Liquid Chromatography-Tandem Mass Spectrometry.

    PubMed

    Zhang, Zihao; Feng, Mengyuan; Zhu, Kechen; Han, Lijun; Sapozhnikova, Yelena; Lehotay, Steven J

    2016-08-10

    A multiresidue analytical method using a modification of the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) sample preparation approach combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis was established and validated for the rapid determination of 69 pesticides at different levels (1-100 ng/g) in wheat and rice straws. In the quantitative analysis, the recoveries ranged from 70 to 120%, and consistent RSDs ≤ 20% were achieved for most of the target analytes (53 pesticides in wheat straw and 58 in rice straw). Almost all of the analytes achieved good linearity with R(2) > 0.98, and the limit of validation levels (LVLs) for diverse pesticides ranged from 1 to 10 ng/g. Different extraction and cleanup conditions were evaluated in both types of straw, leading to different options. The use of 0.1% formic acid or not in extraction with acetonitrile yielded similar final outcomes, but led to the use of a different sorbent in dispersive solid-phase extraction. Both options are efficient and useful for the multiresidue analysis of targeted pesticides in wheat and rice straw samples. PMID:26881844

  14. 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

  15. 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

  16. 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.

  17. 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)

  18. 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...

  19. Determination of the specific radioactivity of fatty acids separated as their methyl esters by gas-liquid chromatography.

    PubMed

    Bishop, C; Glascock, R F; Newell, E M; Welch, V A

    1971-11-01

    Free or combined (3)H-labeled fatty acids are converted to their methyl-(14)C esters or, if labeled with (14)C, to their methyl-(3)H esters. For a given specific radioactivity of the methyl group, the nuclide ratio in the esters separated by GLC is a direct measure of the specific radioactivity of the fatty acids, and quantitative collection is unnecessary. Methods of methylation with minimum quantities of labeled methanol, and of deriving nuclide ratios from channel ratios in a scintillation spectrometer, are given. PMID:5124543

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

    NASA Technical Reports Server (NTRS)

    Falk, A. Y.

    1972-01-01

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

  1. 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

  2. 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.

  3. A Novel Charged Medium Consisting of Gas-Liquid Interfacial Plasmas

    NASA Astrophysics Data System (ADS)

    Kaneko, Toshiro; Hatakeyama, Rikizo

    2009-11-01

    Due to the unique properties of ionic liquids such as their extremely low vapor pressure and high heat capacity, we succeed in creating the reactive gas (plasmas)—liquid (ionic liquids) interfacial field under a low gas pressure condition, where the plasma ion behavior can be controlled. The effects of the plasma ion irradiation on the liquid medium are quantitatively revealed for the first time. In connection with the plasma ion irradiation, the potential structure and optical emission properties of the gas-liquid interfacial plasma are investigated by changing a polarity of the electrode in the liquid to evaluate the plasma-liquid interactions. These results would contribute to synthesizing the metal nanoparticles with carbon nanotubes as a template in the ionic liquid. It is found that the high density, mono-dispersed, and isolated metal nanoparticles are synthesized between or inside the carbon nanotubes by controlling the gas-liquid interfacial plasmas. Furthermore, we can form novel nano-bio composite materials, such as DNA encapsulated carbon nanotubes using the plasma ion irradiation method in an electrolyte plasma with DNA, and demonstrate modifications of the electrical properties of the carbon nanotubes depending on the kinds of encapsulated DNA for the first time.

  4. A Novel Charged Medium Consisting of Gas-Liquid Interfacial Plasmas

    SciTech Connect

    Kaneko, Toshiro; Hatakeyama, Rikizo

    2009-11-10

    Due to the unique properties of ionic liquids such as their extremely low vapor pressure and high heat capacity, we succeed in creating the reactive gas (plasmas)--liquid (ionic liquids) interfacial field under a low gas pressure condition, where the plasma ion behavior can be controlled. The effects of the plasma ion irradiation on the liquid medium are quantitatively revealed for the first time. In connection with the plasma ion irradiation, the potential structure and optical emission properties of the gas-liquid interfacial plasma are investigated by changing a polarity of the electrode in the liquid to evaluate the plasma-liquid interactions. These results would contribute to synthesizing the metal nanoparticles with carbon nanotubes as a template in the ionic liquid. It is found that the high density, mono-dispersed, and isolated metal nanoparticles are synthesized between or inside the carbon nanotubes by controlling the gas-liquid interfacial plasmas. Furthermore, we can form novel nano-bio composite materials, such as DNA encapsulated carbon nanotubes using the plasma ion irradiation method in an electrolyte plasma with DNA, and demonstrate modifications of the electrical properties of the carbon nanotubes depending on the kinds of encapsulated DNA for the first time.

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

    NASA Astrophysics Data System (ADS)

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

    2013-11-01

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

  6. Quantitative and fingerprinting analysis of Atractylodes rhizome based on gas chromatography with flame ionization detection combined with chemometrics.

    PubMed

    Liu, Qiutao; Kong, Dandan; Luo, Jiaoyang; Kong, Weijun; Guo, Weiying; Yang, Meihua

    2016-07-01

    This study assessed the feasibility of gas chromatography with flame ionization detection fingerprinting combined with chemometrics for quality analysis of Atractylodes rhizome. We extracted essential oils from 20 Atractylodes lancea and Atractylodes koreana samples by hydrodistillation. The variation in extraction yields (1.33-4.06%) suggested that contents of the essential oils differed between species. The volatile components (atractylon, atractydin, and atractylenolide I, II, and III) were quantified by gas chromatography with flame ionization detection and confirmed by gas chromatography with mass spectrometry, and the results demonstrated that the number and content of volatile components differed between A. lancea and A. koreana. We then calculated the relative peak areas of common components and similarities of samples by comparing the chromatograms of A. lancea and A. koreana extracts. Also, we employed several chemometric techniques, including similarity analysis, hierarchical clustering analysis, principal component analysis, and partial least-squares discriminate analysis, to analyze the samples. Results were consistent across analytical methods and showed that samples could be separated according to species. Five volatile components in the essential oils were quantified to further validate the results of the multivariate statistical analysis. The method is simple, stable, accurate, and reproducible. Our results provide a foundation for quality control analysis of A. lancea and A. koreana. PMID:27133960

  7. 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

  8. Post-column labeling techniques in amino acid analysis by liquid chromatography.

    PubMed

    Rigas, Pantelis G

    2013-10-01

    Amino acid analysis (AAA) has always presented an analytical challenge in terms of sample preparation, separation, and detection. Because of the vast number of amino acids, various separation methods have been applied taking into consideration the large differences in their chemical structures, which span from nonpolar to highly polar side chains. Numerous separation methods have been developed in the past 60 years, and impressive achievements have been made in the fields of separation, derivatization, and detection of amino acids (AAs). Among the separation methods, liquid chromatography (LC) prevailed in the AAA field using either pre-column or post-column labeling techniques in order to improve either separation of AAs or selectivity and sensitivity of AAA. Of the two approaches, the post-column technique is a more rugged and reproducible method and provides excellent AAs separation relatively free from interferences. This review considers current separations combined with post-column labeling techniques for AAA, comparison with the pre-column methods, and the strategies used to develop effective post-column methodology. The focus of the article is on LC methods coupled with post-column labeling techniques and studying the reactions to achieve optimum post-column derivatization (PCD) conditions in order to increase sensitivity and selectivity using various types of detectors (UV-Vis, fluorescence, electrochemical etc.) and illustrating the versatility of the PCD methods for practical analysis. PMID:24013667

  9. Analysis of antithyroid drugs in surface water by using liquid chromatography-tandem mass spectrometry.

    PubMed

    Pérez-Fernández, Virginia; Marchese, Stefano; Gentili, Alessandra; García, María Ángeles; Curini, Roberta; Caretti, Fulvia; Perret, Daniela

    2014-11-01

    This paper describes development and validation of a new method for the simultaneous determination of six antithyroid drugs (ATDs) in surface waters by using liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Target compounds include two ATD classes: thiouracil derivatives (thiouracil (TU), methyl-thiouracil (MTU), propyl-thiouracil (PTU), phenyl-thiouracil (PhTU)) and imidazole derivatives (tapazole (TAP), and mercaptobenzimidazole (MBI)). Sensitivity and selectivity of the LC-multiple reaction monitoring (MRM) analysis allowed applying a simple pre-concentration procedure and "shooting" the concentrated sample into the LC-MS/MS system without any other treatment. Recoveries were higher than 75% for all analytes. Intra-day precision and inter-day precision, calculated as relative standard deviation (RSD), were below 19 and 22%, respectively. Limits of detection (LODs) ranged from 0.05 to 0.25 μg/L; limits of quantitation (LOQs) varied between 0.15 and 0.75 μg/L. The validated method was successfully applied to the analysis of ATD residues in surface water samples collected from the Tiber River basin and three lakes of Lazio (central Italy). The analytes were quantified based on matrix-matched calibration curves with mercaptobenzimidazole-d4 (MBI-d4) as the internal standard (IS). The most widespread compound was TAP, one of the most common ATDs used in human medicine, but also TU and MBI were often detected in the analysed samples. PMID:25287266

  10. 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

  11. Analysis of creams. IV. Application of high performance liquid chromatography. Part I.

    PubMed

    Lake, O A; Hulshoff, A; Van De Vaart, F J; Indemans, A W

    1983-02-25

    The possibilities of applying reversed-phase high performance liquid chromatography to the analysis of o/w emulsion type creams without preceding sample clean-up were investigated. The chromatographic behaviour of cream base components and active compounds in reversed phase systems consisting of methanol-water mixtures as the mobile phase and a chemically bonded octadecyl stationary phase, was studied. A number of active compounds and the preservative (sorbic acid) could be determined--often in one chromatographic run--without complications, by simply dissolving the sample in a suitable solvent mixture and injecting an aliquot of the solution into the chromatograph. Separation was achieved by the proper choice of methanol content, pH and ionic strength of the eluent. The compounds were detected by UV absorption. Some of the lipophilic cream base components could easily be determined in the same manner, with methanol as the eluent and with refraction index detection. The developed procedure was applied to the analysis of a number of creams. Some of the results are presented as examples, demonstrating the suitability of the method for quality control purposes. PMID:6844121

  12. Microscale analysis of amino acids using gas chromatography-mass spectrometry after methyl chloroformate derivatization.

    PubMed

    Chen, Wen-Ping; Yang, Xiao-Yuan; Hegeman, Adrian D; Gray, William M; Cohen, Jerry D

    2010-08-15

    To conduct studies of stable isotope incorporation and dilution in growing plants, a rapid microscale method for determination of amino acid profiles from minute amounts of plant samples was developed. The method involves solid-phase ion exchange followed by derivatization and analysis by gas chromatography-mass spectrometry (GC-MS). The procedure allowed the eluent to be derivatized directly with methyl chloroformate without sample lyophilization or other evaporation procedures. Sample extraction and derivatization required only ca. 30min and quantification of the 19 amino acids eluted from the cation exchange solid-phase extraction step from a single cotyledon (0.4mg fresh weight) or three etiolated 7-day-old Arabidopsis seedlings (0.1mg fresh weight) was easily accomplished in the selected ion monitoring mode. This method was especially useful for monitoring mass isotopic distribution of amino acids as illustrated by Arabidopsis seedlings that had been labeled with deuterium oxide and (15)N salts. Sample preparation was facile, rapid, economical, and the method is easily modified for integration into robotic systems for analysis with large numbers of samples. PMID:20663719

  13. 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.

  14. 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, γ-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

  15. 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.

  16. Ultra performance liquid chromatography tandem mass spectrometry performance evaluation for analysis of antibiotics in natural waters.

    PubMed

    Tamtam, Fatima; Mercier, Fabien; Eurin, Joëlle; Chevreuil, Marc; Le Bot, Barbara

    2009-03-01

    An ultra performance liquid chromatography electrospray tandem mass spectrometry (UPLC/MS/MS) method was developed and validated for the determination of 17 antibiotics in natural waters in one single extraction and chromatographic procedure. Gradient separation conditions were optimised for 17 compounds belonging to five different antibiotic groups: quinolones (oxolinic acid, nalidixic acid, pipemidic acid, flumequine), fluoroquinolones (enoxacin, ciprofloxacin, norfloxacin, ofloxacin, enrofloxacin, sarafloxacin, danofloxacin, difloxacin, lomefloxacin), sulphonamides (sulphamethoxazole, sulphamethazine), nitro-imidazole (ornidazole) and diaminopyrimidine (trimethoprim). The separation of all compounds, obtained using a 1.7 microm particle size column (100 mm x 2.1 mm), was achieved within 10 min time. Water samples were adjusted to pH 7 and extracted using Oasis hydrophilic-lipophilic balance (HLB) solid phase extraction cartridges. After elution with methanol and concentration, extracts were injected in a C18 column (Acquity UPLC BEH C18) and detected by tandem mass spectrometry. Average recovery from 100 ng L(-1) fortified samples was higher than 70% for most of the compounds, with relative standard deviations below 20%. Performances of the method (recoveries, detection limit, quantification limit and relative standard deviation) and matrix effects were studied, and results obtained showed that method was suitable for routine analysis of antibiotics in surface water. Samples analysis from Seine River (France) confirmed the interest of antibiotic contamination evaluation in that area. PMID:19148627

  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. 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

  19. Elution-Extrusion Countercurrent Chromatography: Theory and Concepts in Metabolic Analysis

    PubMed Central

    Berthod, Alain; Friesen, J. Brent; Inui, Taichi; Pauli, Guido F.

    2008-01-01

    Elution-extrusion countercurrent chromatography (EECCC) takes full advantage of the liquid nature of the stationary phase in CCC by combining regular chromatographic elution with stationary phase extrusion. EECCC is shown to be a three-stage process consisting of classical elution (I), sweeping elution (II), and extrusion (III). After only two column volumes of solvent, it rapidly yields a high-resolution chromatogram that covers an extended polarity range of solutes. As hydrophilicity/lipophilicity balance is a crucial discriminatory property of analytes in highly complex mixtures such as metabolomic samples, the precise determination of CCC distribution constants (KD) is vital to the analysis of metabolomes and other complex biological matrices. This work builds the EECCC concept by performing a full theoretical treatment and providing equations for retention volumes, peak widths, resolution factors, and distribution constants. Experimental validation utilizes natural products standards that resemble the zero to infinity range of the polarity continuum. EECCC extends the “sweet spot” of high-resolution in CCC, and provides access to the otherwise practically unapproachable high-KD portion of the high-resolution chromatograms in CCC. Its improved capabilities of KD-targeting make EECCC a promising tool for the specific analysis of “small” molecules in complex samples such as in metabolomic fingerprinting and footprinting. PMID:17408244

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

    PubMed

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

    2013-01-10

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

  1. Analysis of Amadori compounds by high-performance cation exchange chromatography coupled to tandem mass spectrometry.

    PubMed

    Davidek, Tomas; Kraehenbuehl, Karin; Devaud, Stéphanie; Robert, Fabien; Blank, Imre

    2005-01-01

    High-performance cation exchange chromatography coupled to tandem mass spectrometry or electrochemical detection was found to be an efficient tool for analyzing Amadori compounds derived from hexose and pentose sugars. The method allows rapid separation and identification of Amadori compounds, while benefiting from the well-known advantages of mass spectrometry, such as specificity and sensitivity. Glucose- and xylose-derived Amadori compounds of several amino acids, such as glycine, alanine, valine, leucine/isoleucine, methionine, proline, phenylalanine, and glutamic acid, were separated or discriminated using this new method. The method is suitable for the analysis of both model reaction mixtures and food products. Fructosylglutamate was found to be the major Amadori compound in dried tomatoes (approximately 1.5 g/100 g) and fructosylproline in dried apricots (approximately 0.2 g/100 g). Reaction of xylose and glycine at 90 degrees C (pH 6) for 2 h showed rapid formation of xylulosylglycine (approximately 12 mol %, 15 min) followed by slow decrease over time. Analysis of pentose-derived Amadori compounds is shown for the first time, which represents a major breakthrough in studying occurrence, formation, and decomposition of these labile Maillard intermediates. PMID:15623289

  2. 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 2-100 μg/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 0.1-1.0 μg/kg, 0.1-4.0 μg/kg and 1.2-3.0 μg/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

  3. Analysis of selected carbonyl oxidation products in wine by liquid chromatography with diode array detection.

    PubMed

    Elias, Ryan J; Laurie, V Felipe; Ebeler, Susan E; Wong, Jon W; Waterhouse, Andrew L

    2008-09-19

    A high performance liquid chromatography (HPLC) method for the detection and quantitation of acetaldehyde, glyceraldehyde, pyruvic acid, 2-ketoglutaric acid, and formaldehyde in wine, based on the formation of the 2,4-dinitrophenylhydrazones, is presented. These carbonyl compounds often result from the chemical oxidation of major wine components, and are known to affect flavor and color stability. Their analysis in wine is complicated due to their instability and their tendency to react reversibly with bisulfite to form alpha-hydroxysulfonates. Published methods that break down the sulfonates for the quantitation of total carbonyls in wine involve alkaline hydrolysis of sulfite-bound carbonyls, but we show, for the first time, that this alkaline treatment step significantly increases the concentration of carbonyls during analysis. A solution based on oxygen exclusion is described. The technique offers good specificity, reproducibility (%RSD 0.45-10.6), and limits of detection (1.29-7.53microgL(-1)). The method was successfully used to monitor concentration changes of these compounds in both white and red wines. PMID:18761127

  4. 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.

  5. Analysis of fifteen estrogen metabolites using packed column supercritical fluid chromatography-mass spectrometry.

    PubMed

    Xu, Xia; Roman, John M; Veenstra, Timothy D; Van Anda, Jennifer; Ziegler, Regina G; Issaq, Haleem J

    2006-03-01

    Packed column supercritical fluid chromatography with tandem mass spectrometry was used for the separation of estrone, estradiol, estriol, 16-epiestriol, 17-epiestriol, 16-ketoestradiol, 16alpha-hydroxyestrone, 2-methoxyestrone, 4-methoxyestrone, 2-hydroxyestrone-3-methyl ether, 2-methoxyestradiol, 4-methoxyestradiol, 2-hydroxyestrone, 4-hydroxyestrone, and 2-hydroxyestradiol. A gradient of methanol in carbon dioxide (0-30% methanol in 15 min, 2% change/min) at a flow rate of 2 mL/min and cyanopropyl silica column connected in series with a diol column, both 2.1 mm i.d. x 150 mm long, packed with 5-mum spherical silica-based particles, resulted in the separation and quantification of all 15 estrogens in less than 10 min. The limit of detection (LOD) and limit of quantitation (LOQ) of this pSFC MS/MS method was determined to be 0.5 (S/N = 3), and 5 pg, respectively. Compared with RP-HPLC MS analysis of the same mixture in terms of speed of analysis and sensitivity, pSFC MS is much faster, 10 versus 70 min, with comparable LOD and LOQ. PMID:16503607

  6. 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

  7. ANALYSIS OF DRUG INTERACTIONS WITH HIGH DENSITY LIPOPROTEIN BY HIGH-PERFORMANCE AFFINITY CHROMATOGRAPHY

    PubMed Central

    Chen, Sike; Sobansky, Matthew R.; Hage, David S.

    2009-01-01

    Columns containing immobilized lipoproteins were prepared for the analysis of drug interactions with these particles by high-performance affinity chromatography. This approach was evaluated by using it to examine the binding of high density lipoprotein (HDL) to the drugs propranolol or verapamil. HDL was immobilized by the Schiff base method onto silica and gave HPLC columns with reproducible binding to propranolol over four to five days of continuous operation at pH 7.4. Frontal analysis experiments indicated that two types of interactions were occurring between R/S-propranolol and HDL at 37°C: saturable binding with an association equilibrium constant (Ka) of 1.1–1.9 × 105 M−1, and non-saturable binding with an overall affinity constant (n Ka) of 3.7–4.1 × 104 M−1. Similar results were found at 4 and 27°C. Verapamil also gave similar behavior, with a Ka of 6.0 × 104 M−1 at 37°C for the saturable sites and a n Ka value for the non-saturable sites of 2.5 × 104 M−1. These measured affinities gave good agreement with solution-phase values. The results indicated HPAC can be used to study drug interactions with HDL, providing information that should be valuable in obtaining a better description of how drugs are transported within the body. PMID:19833090

  8. 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.

  9. A variational approach to multi-phase motion of gas, liquid and solid based on the level set method

    NASA Astrophysics Data System (ADS)

    Yokoi, Kensuke

    2009-07-01

    We propose a simple and robust numerical algorithm to deal with multi-phase motion of gas, liquid and solid based on the level set method [S. Osher, J.A. Sethian, Front propagating with curvature-dependent speed: Algorithms based on Hamilton-Jacobi formulation, J. Comput. Phys. 79 (1988) 12; M. Sussman, P. Smereka, S. Osher, A level set approach for capturing solution to incompressible two-phase flow, J. Comput. Phys. 114 (1994) 146; J.A. Sethian, Level Set Methods and Fast Marching Methods, Cambridge University Press, 1999; S. Osher, R. Fedkiw, Level Set Methods and Dynamics Implicit Surface, Applied Mathematical Sciences, vol. 153, Springer, 2003]. In Eulerian framework, to simulate interaction between a moving solid object and an interfacial flow, we need to define at least two functions (level set functions) to distinguish three materials. In such simulations, in general two functions overlap and/or disagree due to numerical errors such as numerical diffusion. In this paper, we resolved the problem using the idea of the active contour model [M. Kass, A. Witkin, D. Terzopoulos, Snakes: active contour models, International Journal of Computer Vision 1 (1988) 321; V. Caselles, R. Kimmel, G. Sapiro, Geodesic active contours, International Journal of Computer Vision 22 (1997) 61; G. Sapiro, Geometric Partial Differential Equations and Image Analysis, Cambridge University Press, 2001; R. Kimmel, Numerical Geometry of Images: Theory, Algorithms, and Applications, Springer-Verlag, 2003] introduced in the field of image processing.

  10. Acoustic tuning of gas liquid scheme injectors for acoustic damping in a combustion chamber of a liquid rocket engine

    NASA Astrophysics Data System (ADS)

    Sohn, Chae Hoon; Park, I.-Sun; Kim, Seong-Ku; Jip Kim, Hong

    2007-07-01

    In a combustion chamber of a liquid rocket engine, acoustic fine-tuning of gas-liquid scheme injectors is studied numerically for acoustic stability by adopting a linear acoustic analysis. Injector length and blockage ratio at gas inlet are adjusted for fine-tuning. First, acoustic behavior in the combustor with a single injector is investigated and acoustic-damping effect of the injector is evaluated for cold condition by the quantitative parameter of damping factor as a function of injector length. From the numerical results, it is found that the injector can play a significant role in acoustic damping when it is tuned finely. The optimum tuning-length of the injector to maximize the damping capacity corresponds to half of a full wavelength of the first longitudinal overtone mode traveling in the injector with the acoustic frequency intended for damping in the chamber. In baffled chamber, the optimum lengths of the injector are calculated as a function of baffle length for both cold and hot conditions. Next, in the combustor with numerous resonators, peculiar acoustic coupling between a combustion chamber and injectors is observed. As the injector length approaches a half-wavelength, the new injector-coupled acoustic mode shows up and thereby, the acoustic-damping effect of the tuned injectors is appreciably degraded. And, damping factor maintains a near-constant value with blockage ratio and then, decreases rapidly. Blockage ratio affects also acoustic damping and should be considered for acoustic tuning.

  11. 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

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

    PubMed

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

    2014-02-21

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

  13. 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

  14. Supervised pattern recognition procedures for discrimination of whiskeys from gas chromatography/mass spectrometry congener analysis.

    PubMed

    González-Arjona, Domingo; López-Pérez, Germán; González-Gallero, Víctor; González, A Gustavo

    2006-03-22

    The volatile congener analysis of 52 commercialized whiskeys (24 samples of single malt Scotch whiskey, 18 samples of bourbon whiskey, and 10 samples of Irish whiskey) was carried out by gas chromatography/mass spectrometry after liquid-liquid extraction with dichloromethane. Pattern recognition procedures were applied for discrimination of different whiskey categories. Multivariate data analysis includes linear discriminant analysis (LDA), k nearest neighbors (KNN), soft independent modeling of class analogy (SIMCA), procrustes discriminant analysis (PDA), and artificial neural networks techniques involving multilayer perceptrons (MLP) and probabilistic neural networks (PNN). Classification rules were validated by considering the number of false positives (FPs) and false negatives (FNs) of each class associated to the prediction set. Artificial neural networks led to the best results because of their intrinsic nonlinear features. Both techniques, MLP and PNN, gave zero FPs and zero FNs for all of the categories. KNN is a nonparametric method that also provides zero FPs and FNs for every class but only when selecting K = 3 neighbors. PDA produced good results also (zero FPs and FNs always) but only by selecting nine principal components for class modeling. LDA shows a lesser classification performance, because of the building of linear frontiers between classes that does not apply in many real situations. LDA led to one FP for bourbons and one FN for scotches. The worse results were obtained with SIMCA, which gave a higher number of FPs (five for both scotches and bourbons) and FNs (six for scotchs and two for bourbons). The possible cause of these findings is the strong influence of class inhomogeneities on the SIMCA performance. It is remarkable that in any case, all of the methodologies lead to zero FPs and FNs for the Irish whiskeys. PMID:16536565

  15. 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

  16. 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.

  17. Analysis of anthocyanins in commercial fruit juices by using nano-liquid chromatography-electrospray-mass spectrometry and high-performance liquid chromatography with UV-vis detector.

    PubMed

    Fanali, Chiara; Dugo, Laura; D'Orazio, Giovanni; Lirangi, Melania; Dachà, Marina; Dugo, Paola; Mondello, Luigi

    2011-01-01

    Nano-LC and conventional HPLC techniques were applied for the analysis of anthocyanins present in commercial fruit juices using a capillary column of 100 μm id and a 2.1 mm id narrow-bore C(18) column. Analytes were detected by UV-Vis at 518 nm and ESI-ion trap MS with HPLC and nano-LC, respectively. Commercial blueberry juice (14 anthocyanins detected) was used to optimize chromatographic separation of analytes and other analysis parameters. Qualitative identification of anthocyanins was performed by comparing the recorded mass spectral data with those of published papers. The use of the same mobile phase composition in both techniques revealed that the miniaturized method exhibited shorter analysis time and higher sensitivity than narrow-bore chromatography. Good intra-day and day-to-day precision of retention time was obtained in both methods with values of RSD less than 3.4 and 0.8% for nano-LC and HPLC, respectively. Quantitative analysis was performed by external standard curve calibration of cyanidin-3-O-glucoside standard. Calibration curves were linear in the concentration ranges studied, 0.1-50 and 6-50 μg/mL for HPLC-UV/Vis and nano-LC-MS, respectively. LOD and LOQ values were good for both methods. In addition to commercial blueberry juice, qualitative and quantitative analysis of other juices (e.g. raspberry, sweet cherry and pomegranate) was performed. The optimized nano-LC-MS method allowed an easy and selective identification and quantification of anthocyanins in commercial fruit juices; it offered good results, shorter analysis time and reduced mobile phase volume with respect to narrow-bore HPLC. PMID:21246720

  18. 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

  19. Advances on the compositional analysis of glycosphingolipids combining thin-layer chromatography with mass spectrometry.

    PubMed

    Müthing, Johannes; Distler, Ute

    2010-01-01

    Glycosphingolipids (GSLs), composed of a hydrophilic carbohydrate chain and a lipophilic ceramide anchor, play pivotal roles in countless biological processes, including infectious diseases and the development of cancer. Knowledge of the number and sequence of monosaccharides and their anomeric configuration and linkage type, which make up the principal items of the glyco code of biologically active carbohydrate chains, is essential for exploring the function of GSLs. As part of the investigation of the vertebrate glycome, GSL analysis is undergoing rapid expansion owing to the application of novel biochemical and biophysical technologies. Mass spectrometry (MS) takes part in the network of collaborations to further unravel structural and functional aspects within the fascinating world of GSLs with the ultimate aim to better define their role in human health and disease. However, a single-method analytical MS technique without supporting tools is limited yielding only partial structural information. Because of its superior resolving power, robustness, and easy handling, high-performance thin-layer chromatography (TLC) is widely used as an invaluable tool in GSL analysis. The intention of this review is to give an insight into current advances obtained by coupling supplementary techniques such as TLC and mass spectrometry. A retrospective view of the development of this concept and the recent improvements by merging (1) TLC separation of GSLs, (2) their detection with oligosaccharide-specific proteins, and (3) in situ MS analysis of protein-detected GSLs directly on the TLC plate, are provided. The procedure works on a nanogram scale and was successfully applied to the identification of cancer-associated GSLs in several types of human tumors. The combination of these two supplementary techniques opens new doors by delivering specific structural information of trace quantities of GSLs with only limited investment in sample preparation. PMID:19609886

  20. 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

  1. Metabolomic Analysis of Gingival Crevicular Fluid Using Gas Chromatography/Mass Spectrometry

    PubMed Central

    Ozeki, Miho; Nozaki, Takenori; Aoki, Jun; Bamba, Takeshi; Jensen, Kirk R.; Murakami, Shinya; Toyoda, Michisato

    2016-01-01

    Periodontitis is one of the most prevalent threats to oral health as the most common cause of tooth loss. In order to perform effective treatment, a clinical test that detect sites where disease activity is high and predicts periodontal tissue destruction is strongly desired, however, it is still difficult to prognose the periodontal tissue breakdown on the basis of conventional methods. The aim of this study is to examine the usefulness of gas chromatography/mass spectrometry (GC/MS), which could eventually be used for on-site analysis of metabolites in gingival crevicular fluid (GCF) in order to objectively diagnose periodontitis at a molecular level. GCF samples were collected from two diseased sites (one site with a moderate pocket and another site with a deep pocket) from each patient and from clinically healthy sites of volunteers. Nineteen metabolites were identified using GC/MS. Total ion current chromatograms showed broad differences in metabolite peak patterns between GCF samples obtained from healthy sites, moderate-pocket sites, and deep-pocket sites. The intensity difference of some metabolites was significant at sites with deep pockets compared to healthy sites. Additionally, metabolite intensities at moderate-pocket sites showed an intermediate profile between the severely diseased sites and healthy sites, which suggested that periodontitis progression could be observed with a changing metabolite profile. Principal component analysis confirmed these observations by clearly delineating healthy sites and sites with deep pockets. These results suggest that metabolomic analysis of GCF could be useful for prediction and diagnosis of periodontal disease in a single visit from a patient and provides the groundwork for establishing a new, on-site diagnostic method for periodontitis. PMID:27446770

  2. Metabolomic Analysis of Gingival Crevicular Fluid Using Gas Chromatography/Mass Spectrometry.

    PubMed

    Ozeki, Miho; Nozaki, Takenori; Aoki, Jun; Bamba, Takeshi; Jensen, Kirk R; Murakami, Shinya; Toyoda, Michisato

    2016-01-01

    Periodontitis is one of the most prevalent threats to oral health as the most common cause of tooth loss. In order to perform effective treatment, a clinical test that detect sites where disease activity is high and predicts periodontal tissue destruction is strongly desired, however, it is still difficult to prognose the periodontal tissue breakdown on the basis of conventional methods. The aim of this study is to examine the usefulness of gas chromatography/mass spectrometry (GC/MS), which could eventually be used for on-site analysis of metabolites in gingival crevicular fluid (GCF) in order to objectively diagnose periodontitis at a molecular level. GCF samples were collected from two diseased sites (one site with a moderate pocket and another site with a deep pocket) from each patient and from clinically healthy sites of volunteers. Nineteen metabolites were identified using GC/MS. Total ion current chromatograms showed broad differences in metabolite peak patterns between GCF samples obtained from healthy sites, moderate-pocket sites, and deep-pocket sites. The intensity difference of some metabolites was significant at sites with deep pockets compared to healthy sites. Additionally, metabolite intensities at moderate-pocket sites showed an intermediate profile between the severely diseased sites and healthy sites, which suggested that periodontitis progression could be observed with a changing metabolite profile. Principal component analysis confirmed these observations by clearly delineating healthy sites and sites with deep pockets. These results suggest that metabolomic analysis of GCF could be useful for prediction and diagnosis of periodontal disease in a single visit from a patient and provides the groundwork for establishing a new, on-site diagnostic method for periodontitis. PMID:27446770

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

    PubMed

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

    2013-12-01

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

  4. 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 ...

  5. 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

  6. 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

  7. Determination of urinary glucose by a flow injection analysis amperometric biosensor and ion-exchange chromatography.

    PubMed

    Male, K B; Luong, J H

    1992-12-01

    A practical biosensor system has been developed for the determination of urinary glucose using a flow-injection analysis (FIA) amperometric detector and ion-exchange chromatography. Glucose oxidase was immobilized onto porous aminopropyl glass beads via glutaraldehyde activation to form an immobilized enzyme column. On the basis of its negative charge at pH 5.5, endogenous urate in urine samples was effectively retained by an upstream anion-exchange resin column. The biosensor system possessed a sensitivity of 160 +/- 2.4 RU microM-1 (RU or relative unit is defined as 2.86 microV at the detection output) for glucose with a minimum detection level of 10 microM. When applied for the determination of urinary glucose, the result obtained compared very well with that of the widely accepted hexokinase assay. The immobilized glucose oxidase could be reused for more than 1000 repeated analyses without losing its original activity. The reuse of the acetate anion-exchange column before replacement would be about 25-30 analyses. Acetaminophen and ascorbic acid were also effectively adsorbed by the acetate anion exchanger. The introduction of this type of anion exchanger thus greatly improved the selectivity of the FIA biosensor system and fostered its applicability for the determination of glucose in urine samples. PMID:1303063

  8. 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.

  9. 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

  10. Lipid analysis by thin-layer chromatography--a review of the current state.

    PubMed

    Fuchs, Beate; Süss, Rosmarie; Teuber, Kristin; Eibisch, Mandy; Schiller, Jürgen

    2011-05-13

    High-performance thin-layer chromatography (HPTLC) is a widely used, fast and relatively inexpensive method of separating complex mixtures. It is particularly useful for smaller, apolar compounds and offers some advantages over HPLC. This review gives an overview about the special features as well as the problems that have to be considered upon the HPTLC analysis of lipids. The term "lipids" is used here in a broad sense and comprises fatty acids and their derivatives as well as substances related biosynthetically or functionally to these compounds. After a short introduction regarding the stationary phases and the methods how lipids can be visualized on an HPTLC plate, the individual lipid classes will be discussed and the most suitable solvent systems for their separation indicated. The focus will be on lipids that are most abundant in biological systems, i.e. cholesterol and its derivates, glycerides, sphingo- and glycolipids as well as phospholipids. Finally, a nowadays very important topic, the combination between HPTLC and mass spectrometric (MS) detection methods will be discussed. It will be shown that this is a very powerful method to investigate the identities of the HPTLC spots in more detail than by the use of common staining methods. Future aspects of HPTLC in the lipid field will be also discussed. PMID:21167493

  11. Analysis of Nucleosides in Municipal Wastewater by Large-Volume Liquid Chromatography Tandem Mass Spectrometry

    PubMed Central

    Brewer, Alex J.; Lunte, Craig

    2015-01-01

    Nucleosides are components of both DNA and RNA, and contain either a ribose (RNA) or 2deoxyribose (DNA) sugar and a purine or pyrimidine base. In addition to DNA and RNA turnover, modified nucleosides found in urine have been correlated to a diminished health status associated with AIDS, cancers, oxidative stress and age. Nucleosides found in municipal wastewater influent are potentially useful markers of community health status, and as of now, remain uninvestigated. A method was developed to quantify nucleosides in municipal wastewater using large-volume injection, liquid chromatography, and mass spectrometry. Method accuracy ranged from 92 to 139% when quantified by using isotopically labeled internal standards. Precision ranged from 6.1 to 19% of the relative standard deviation. The method’s utility was demonstrated by the analysis of twenty-four hour composite wastewater influent samples that were collected over a week to investigate community nucleoside excretion. Nucleosides originating from RNA were more abundant that DNA over the study period, with total loads of nucleosides ranging from 2 to 25 kg/day. Given this relatively high amount of nucleosides found over the study period they present an attractive analyte for the investigation of community health. PMID:26322136

  12. Ultra-performance convergence chromatography (UPC²) method for the analysis of biogenic amines in fermented foods.

    PubMed

    Gong, Xiao; Qi, Ningli; Wang, Xiaoxi; Lin, Lijing; Li, Jihua

    2014-11-01

    A rapid ultra-performance convergence chromatography (UPC(2)) method for the determination of eight biogenic amines (spermine, spermidine, putrescine, cadaverine, tryptamine, phenylethylamine, histamine and tyramine) in fermented foods was developed. The amines were pre-column derivatized with dansyl chloride and separated on UPC(2) system with a HSS C18 SB column (3.0 × 100 mm, 1.8 μm) using gradient elution with a binary system of CO2 and n-hexane:isopropanol:ammonium hydroxide (70:30:0.15, v/v/v), back pressure of 2,000 psi, flow rate of 2.0 ml/min and DAD detection at 254 nm. The result showed excellent linearity (r=0.9995-1.0000). Limits of detection (LOD) and limits of quantification (LOQ) were 21-67 ng/L and 72-224 ng/L, respectively. Relative standard deviations (RSD) for repeatability and reproducibility were 0.21-0.87% and 1.98-4.02%, respectively. Furthermore, this method was successfully applied to analysis of biogenic amines in Yulu and Sufu samples. PMID:24874373

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

    PubMed

    Cretu, Georgiana C; Morlock, Gertrud E

    2014-03-01

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

  14. 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

  15. 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

  16. 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

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

    PubMed

    Cajka, Tomas; Fiehn, Oliver

    2014-10-01

    Liquid chromatography-mass spectrometry (LC-MS)-based lipidomics has been a subject of dramatic developments over the past decade. This review focuses on state of the art in LC-MS-based lipidomics, covering all the steps of global lipidomic profiling. On the basis of review of 185 original papers and application notes, we can conclude that typical LC-MS-based lipidomics methods involve: (1) extraction using chloroform/MeOH or MTBE/MeOH protocols, both with addition of internal standards covering each lipid class; (2) separation of lipids using short microbore columns with sub-2-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

  18. A validated method for analysis of Swerchirin in Swertia longifolia Boiss. by high performance liquid chromatography

    PubMed Central

    Shekarchi, M.; Hajimehdipoor, H.; Khanavi, M.; Adib, N.; Bozorgi, M.; Akbari-Adergani, B.

    2010-01-01

    Swertia spp. (Gentianaceae) grow widely in the eastern and southern Asian countries and are used as traditional medicine for gastrointestinal disorders. Swerchirin, one of the xanthones in Swertia spp., has many pharmacological properties, such as, antimalarial, antihepatotoxic, and hypoglycemic effects. Because of the pharmacological importance of Swerchirin in this investigation, it was purified from Swertia longifolia Boiss. as one of the main components and quantified by means of a validated high performance liquid chromatography (HPLC) technique. Aerial parts of the plant were extracted with acetone 80%. Phenolic and non-phenolic constituents of the extract were separated from each other during several processes. The phenolic fraction was injected into the semi-preparative HPLC system, which consisted of a C18 column and a gradient methanol: 0.1% formic acid mode. Using this method, we were able to purify six xanthones from the plant, in order to use them as standard materials. The analytical method was validated for Swerchirin as one of the most important components of the plant, with more pharmacological activities according to the validation parameters, such as, selectivity, linearity (r2 > 0.9998), precision (≤3.3), and accuracy, which were measured by the determination of recovery (98-107%). The limits of detection and quantization were found to be 2.1 and 6.3 μg/mL, respectively. On account of the speed and accuracy, the UV-HPLC method may be used for quantitative analysis of Swerchirin. PMID:20548931

  19. Analysis of acrylamide in coffee and cocoa by isotope dilution liquid chromatography-tandem mass spectrometry.

    PubMed

    Aguas, Patricia C; Fitzhenry, Matthew J; Giannikopoulos, Georgina; Varelis, Peter

    2006-08-01

    An accurate and precise method for the quantification of acrylamide using stable isotope dilution liquid chromatography-tandem mass spectrometry was developed and used to measure acrylamide in coffee and cocoa samples. The sample preparation involved extraction of the analyte and its internal standard, 13C3-acrylamide, into water and subsequent defatting of the aqueous extract with dichloromethane. An aliquot of the resulting aqueous extract was then azeotropically dried under reduced pressure and subsequently purified using an aminopropyl-bonded silica cartridge. The purified extracts were then chromatographed on a 5-microm 2.1 x 150 mm Hypercarb column, the effluent of which was monitored for the analyte and its internal standard using positive-ion APCI-selected reaction monitoring. The intra-laboratory reproducibility of the method, expressed as a relative coefficient of variation (%, n=5), was determined at four levels of concentration (12.3, 42.3, 139.3 and 464.8 microg kg(-1)) and was found to vary between 0.6-2.5%. The accuracy of the method was assessed using a reference sample of coffee. The average result obtained using our method differed from the assigned value of the reference material by less than 1%. An analysis of a cocoa sample revealed that the method is capable of precisely estimating acrylamide in challenging matrices down to a level of at least 12.3 microg kg(-1). PMID:16819634

  20. Analysis of nerve agent metabolites from nail clippings by liquid chromatography tandem mass spectrometry.

    PubMed

    Appel, Amanda S; Logue, Brian A

    2016-09-15

    While several methods for the bioanalysis of nerve agents or their metabolites have been developed for the verification of nerve agent exposure, these methods are generally limited in the amount of time after an exposure that markers of exposure can be detected (due to rapid metabolism from biological matrices). In this study, a method for the analysis of nerve agent hydrolysis products from nail clippings was developed to allow evaluation of nails as a long-term repository of these markers. Pinacolyl methylphosphonic acid (PMPA) and isopropyl methylphosphonic acid (IMPA) were extracted from nail samples with N,N-dimethylformamide and subsequently analyzed by liquid chromatography-tandem mass spectrometry. Limits of detection for PMPA and IMPA were 0.3μg/kg and 7.5μg/kg and linear ranges were 0.75-300μg/kg and 30-1500μg/kg, respectively. Precision was within 10% and 8% for PMPA and IMPA, respectively, and accuracy was 100±12% for both analytes. The approach presented here is complementary to current methods for nerve agent exposure verification, and should allow for long-term determination of nerve agent poisoning. PMID:27474780

  1. 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

  2. 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.

  3. [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

  4. Liquid chromatography with ultraviolet absorbance detection for the analysis of tetracycline residues in honey.

    PubMed

    Viñas, Pilar; Balsalobre, Nuria; López-Erroz, Carmen; Hernández-Córdoba, Manuel

    2004-01-01

    The separation of tetracyclines (TCs) using reversed-phase liquid chromatography (LC) is proposed. The use of an amide-based stationary phase prevents the interaction of tetracyclines with the residual silanol groups and thus avoids the appearance of tailed peaks. Detection was based on using an UV spectrophotometer and gradient elution with acetonitrile-oxalic acid as mobile phase permitted good separation of all the peaks. Specificity was demonstrated by the retention characteristics, UV spectra and peak purity index. Linearity, precision, recovery and sensitivity were satisfactory. The procedure was applied to the analysis of tetracycline residues (tetracycline, oxytetracycline (OTC), chlortetracycline (CTC), doxycycline (DC), minocycline (MINO) and methacycline (MTC)) in honey of different types. Extraction involved using a mild acidic solvent containing EDTA to release protein-bound or sugar-bound tetracyclines. For the clean-up step, solid phase extraction using phenyl cartridges was applied. Detection limits in the honey using the proposed procedure are between 15 and 30 ng g(-1), depending on the tetracycline. PMID:14753778

  5. 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.

  6. 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.

  7. DETECTION OF HETEROGENEOUS DRUG-PROTEIN BINDING BY FRONTAL ANALYSIS AND HIGH-PERFORMANCE AFFINITY CHROMATOGRAPHY

    PubMed Central

    Tong, Zenghan; Joseph, K.S.; Hage, David S.

    2011-01-01

    This study examined the use of frontal analysis and high-performance affinity chromatography for detecting heterogeneous binding in biomolecular interactions, using the binding of acetohexamide with human serum albumin (HSA) as a model. It was found through the use of this model system and chromatographic theory that double-reciprocal plots could be used more easily than traditional isotherms for the initial detection of binding site heterogeneity. The deviations from linearity that were seen in double-reciprocal plots as a result of heterogeneity were a function of the analyte concentration, the relative affinities of the binding sites in the system and the amount of each type of site that was present. The size of these deviations was determined and compared under various conditions. Plots were also generated to show what experimental conditions would be needed to observe these deviations for general heterogeneous systems or for cases in which some preliminary information was available on the extent of binding heterogeneity. The methods developed in this work for the detection of binding heterogeneity are not limited to drug interactions with HSA but could be applied to other types of drug-protein binding or to additional biological systems with heterogeneous binding. PMID:21612784

  8. Analysis of Drug Interactions with Lipoproteins by High-Performance Affinity Chromatography

    PubMed Central

    Sobansky, Matthew R.; Hage, David S.

    2013-01-01

    Lipoproteins such as high-density lipoprotein (HDL) and low-density lipoprotein (LDL) are known to interact with drugs and other solutes in blood. These interactions have been examined in the past by methods such as equilibrium dialysis and capillary electrophoresis. This chapter describes an alternative approach that has recently been developed for examining these interactions by using high-performance affinity chromatography. In this method, lipoproteins are covalently immobilized to a solid support and used within a column as a stationary phase for binding studies. This approach allows the same lipoprotein preparation to be used for a large number of binding studies, leading to precise estimates of binding parameters. This chapter will discuss how this technique can be applied to the identification of interaction models and be used to differentiate between systems that have interactions based on partitioning, adsorption or mixed-mode interactions. It is also shown how this approach can then be used for the measurement of binding parameters for HDL and LDL with drugs. Examples of these studies are provided, with particular attention being given to the use of frontal analysis to examine the interactions of R- and S-propranolol with HDL and LDL. The advantages and possible limitations of this method are described. The extension of this approach to other types of drug-lipoprotein interactions is also considered. PMID:25392741

  9. Supercritical fluid chromatography as a method of analysis for the determination of 4-hydroxybenzylglucosinolate degradation products.

    PubMed

    Buskov, S; Hasselstrøm, J; Olsen, C E; Sørensen, H; Sørensen, J C; Sørensen, S

    2000-07-01

    In the present study analytical and preparative supercritical fluid chromatography (SFC) were used for investigation of myrosinase catalysed degradation of 4-hydroxybenzylglucosinolate (sinalbin). Sinalbin occurs as a major glucosinolate in seeds of Sinapis alba L., in various mustards and other food products. The degradation products were identified and quantified by analysis based on a developed SFC method using a bare silica column. Determinations comprised transformation products of sinalbin, produced both during degradation of isolated sinalbin, and during autolysis of meal from S. alba seeds. The conditions in the developed SFC method were used as basis for the preparative SFC procedure applied for isolation of the components prior to their identification by nuclear magnetic resonance (NMR) spectroscopy. Myrosinase catalysed sinalbin hydrolysis resulted in the reactive 4-hydroxybenzyl isothiocyanate as an initial product at pH values from 3.5 to 7.5 whereas 4-hydroxybenzyl cyanide was one of the major products at low pH values. 4-Hydroxybenzyl isothiocyanate was found to disappear from the aqueous reaction mixtures in a few hours, as it reacted easily with available nucleophilic reagents. 4-Hydroxybenzyl alcohol was found as the product from reaction with water, and with ascorbic acid, 4-hydroxybenzylascorbigen was produced. PMID:10869674

  10. Qualitative and quantitative analysis of four species of Curcuma rhizomes using twice development thin layer chromatography.

    PubMed

    Zhang, J S; Guan, J; Yang, F Q; Liu, H G; Cheng, X J; Li, S P

    2008-11-01

    The rhizomes of Curcuma phaeocaulis, Curcuma kwangsiensis, Curcuma wenyujin and Curcuma longa are used as Ezhu or Jianghuang in traditional Chinese medicine for a long time. Due to their similar morphological characters, it is difficult to distinguish their origins of raw materials used in clinic. In this study, a simple, rapid and reliable twice development TLC method was developed for qualitative and quantitative analysis of the four species of Curcuma rhizomes. The chromatography was performed on silica gel 60F(254) plate with chloroform-methanol-formic acid (80:4:0.8, v/v/v) and petroleum ether-ethyl acetate (90:10, v/v) as mobile phase for twice development. The TLC markers were colorized with 1% vanillin-H(2)SO(4) solution. The four species of Curcuma were easily discriminated based on their characteristic TLC profiles, and simultaneous quantification of eight compounds, including bisdemethoxycurcumin, demethoxycurcumin, curcumine, curcumenol, curcumol, curdione, furanodienone and curzerene, in Curcuma were also performed densitometrically at lambda(scan)=518nm and lambda(reference)=800 nm. The investigated compounds had good linearity (r(2)>0.9905) within test ranges. Therefore, the developed TLC method can be used for quality control of Curcuma rhizomes. PMID:18722068

  11. Multiclass analysis of antibiotic residues in honey by ultraperformance liquid chromatography-tandem mass spectrometry.

    PubMed

    Vidal, Jose Luis Martínez; Aguilera-Luiz, María Del Mar; Romero-González, Roberto; Frenich, Antonia Garrido

    2009-03-11

    A method has been developed and validated for the simultaneous analysis of different veterinary drug residues (macrolides, tetracyclines, quinolones, and sulfonamides) in honey. Honey samples were dissolved with Na(2)EDTA, and veterinary residues were extracted from the supernatant by solid-phase extraction (SPE), using OASIS HLB cartridges. The separation and determination was carried out by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS), using an electrospay ionization source (ESI) in positive mode. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring (MRM) of two ion transitions per compound to provide a high degree of sensitivity and specificity. The method was validated, and mean recoveries were evaluated at three concentration levels (10, 50, and 100 microg/kg), ranging from 70 to 120% except for doxycycline, erythromycin, and tylmicosin with recovery higher than 50% at the three levels assayed. Relative standard deviations (RSDs) of the recoveries were less than 20% within the intraday precision and less than 25% within the interday precision. The limits of quantification (LOQs) were always lower than 4 microg/kg. The developed procedure was applied to 16 honey samples, and erythromycin, sarafloxacin, and tylosin were found in a few samples. PMID:19195999

  12. Multi-mycotoxin analysis in dairy products by liquid chromatography coupled to quadrupole orbitrap mass spectrometry.

    PubMed

    Jia, Wei; Chu, Xiaogang; Ling, Yun; Huang, Junrong; Chang, James

    2014-06-01

    A new analytical method was developed and validated for simultaneous analysis of 58 mycotoxins in dairy products. Response surface methodology was employed to optimize a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method. Ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap) was used for the separation and detection of all the analytes. The method was validated by taking into consideration the guidelines specified in Commission Decision 2002/657/EC and 401/2006/EC. The extraction recoveries were in a range of 86.6-113.7%, with coefficient of variation <6.2%. The 58 compounds could be detected in the 0.001-100 μg kg(-1) concentration range, with correlation coefficient >0.99. The limits of detection for the analytes are in the range 0.001-0.92 μg kg(-1). The repeatability was lower than 6.4%. This method has been successfully applied on screening of mycotoxins in commercial dairy product samples, and it is very useful for fast screening of different food contaminants. PMID:24794937

  13. Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

    PubMed

    Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

    2008-02-15

    With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we

  14. 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...

  15. 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 ...

  16. ENVIRONMENTAL ANALYSIS BY AB INITIO QUANTUM MECHANICAL COMPUTATION AND GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY.

    EPA Science Inventory

    Computational chemistry, in conjunction with gas chromatography/mass spectrometry/Fourier transform infrared spectrometry (GC/MS/FT-IR), was used to tentatively identify seven tetrachlorobutadiene (TCBD) isomers detected in an environmental sample. Computation of the TCBD infrare...

  17. 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...

  18. Parallelization of Catalytic Packed-Bed Microchannels with Pressure-Drop Microstructures for Gas-Liquid Multiphase Reactions

    NASA Astrophysics Data System (ADS)

    Murakami, Sunao; Ohtaki, Kenichiro; Matsumoto, Sohei; Inoue, Tomoya

    2012-06-01

    High-throughput and stable treatments are required to achieve the practical production of chemicals with microreactors. However, the flow maldistribution to the paralleled microchannels has been a critical problem in achieving the productive use of multichannel microreactors for multiphase flow conditions. In this study, we newly designed and fabricated a glass four-channel catalytic packed-bed microreactor for the scale-up of gas-liquid multiphase chemical reactions. We embedded microstructures generating high pressure losses at the upstream side of each packed bed, and experimentally confirmed the efficacy of the microstructures in decreasing the maldistribution of the gas-liquid flow to the parallel microchannels.

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

    SciTech Connect

    Johnson, S.

    1999-02-12

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

  20. Comprehensive analysis of pharmaceutical products using simultaneous mixed-mode (ion-exchange/reversed-phase) and hydrophilic interaction liquid chromatography.

    PubMed

    Kazarian, Artaches A; Nesterenko, Pavel N; Soisungnoen, Phimpha; Burakham, Rodjana; Srijaranai, Supalax; Paull, Brett

    2014-08-01

    Liquid chromatographic assays were developed using a mixed-mode column coupled in sequence with a hydrophilic interaction liquid chromatography column to allow the simultaneous comprehensive analysis of inorganic/organic anions and cations, active pharmaceutical ingredients, and excipients (carbohydrates). The approach utilized dual sample injection and valve-mediated column switching and was based upon a single high-performance liquid chromatography gradient pump. The separation consisted of three distinct sequential separation mechanisms, namely, (i) ion-exchange, (ii) mixed-mode interactions under an applied dual gradient (reversed-phase/ion-exchange), and (iii) hydrophilic interaction chromatography. Upon first injection, the Scherzo SS C18 column (Imtakt) provided resolution of inorganic anions and cations under isocratic conditions, followed by a dual organic/salt gradient to elute active pharmaceutical ingredients and their respective organic counterions and potential degradants. At the top of the mixed-mode gradient (high acetonitrile content), the mobile phase flow was switched to a preconditioned hydrophilic interaction liquid chromatography column, and the standard/sample was reinjected for the separation of hydrophilic carbohydrates, some of which are commonly known excipients in drug formulations. The approach afforded reproducible separation and resolution of up to 23 chemically diverse solutes in a single run. The method was applied to investigate the composition of commercial cough syrups (Robitussin®), allowing resolution and determination of inorganic ions, active pharmaceutical ingredients, excipients, and numerous well-resolved unknown peaks. PMID:24890905

  1. Enantioselective simultaneous analysis of selected pharmaceuticals in environmental samples by ultrahigh performance supercritical fluid based chromatography tandem mass spectrometry.

    PubMed

    Camacho-Muñoz, Dolores; Kasprzyk-Hordern, Barbara; Thomas, Kevin V

    2016-08-31

    In order to assess the true impact of each single enantiomer of pharmacologically active compounds (PACs) in the environment, highly efficient, fast and sensitive analytical methods are needed. For the first time this paper focuses on the use of ultrahigh performance supercritical fluid based chromatography coupled to a triple quadrupole mass spectrometer to develop multi-residue enantioselective methods for chiral PACs in environmental matrices. This technique exploits the advantages of supercritical fluid chromatography, ultrahigh performance liquid chromatography and mass spectrometry. Two coated modified 2.5 μm-polysaccharide-based chiral stationary phases were investigated: an amylose tris-3,5-dimethylphenylcarbamate column and a cellulose tris-3-chloro-4-methylphenylcarbamate column. The effect of different chromatographic variables on chiral recognition is highlighted. This novel approach resulted in the baseline resolution of 13 enantiomers PACs (aminorex, carprofen, chloramphenicol, 3-N-dechloroethylifosfamide, flurbiprofen, 2-hydroxyibuprofen, ifosfamide, imazalil, naproxen, ofloxacin, omeprazole, praziquantel and tetramisole) and partial resolution of 2 enantiomers PACs (ibuprofen and indoprofen) under fast-gradient conditions (<10 min analysis time). The overall performance of the methods was satisfactory. The applicability of the methods was tested on influent and effluent wastewater samples. To the best of our knowledge, this is the first feasibility study on the simultaneous separation of chemically diverse chiral PACs in environmental matrices using ultrahigh performance supercritical fluid based chromatography coupled with tandem mass spectrometry. PMID:27506366

  2. 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.

  3. Study of Co-Current and Counter-Current Gas-Liquid Two-Phase Flow Through Packed Bed in Microgravity

    NASA Astrophysics Data System (ADS)

    Revankar, Shripad T.

    2002-11-01

    The main goal of the project is to obtain new experimental data and development of models on the co-current and counter-current gas-liquid two-phase flow through a packed bed in microgravity and characterize the flow regime transition, pressure drop, void and interfacial area distribution, and liquid hold up. Experimental data will be obtained for earth gravity and microgravity conditions. Models will be developed for the prediction of flow regime transition, void fraction distribution and interfacial area concentration, which are key parameters to characterize the packed bed performance. Thus the specific objectives of the proposed research are to: (1) Develop experiments for the study of the gas liquid two-phase flow through the packed bed with three different flow combinations: co-current down flow, co-current upflow and counter current flow. (2) Develop pore scale and bed scale two-phase instrumentation for measurement of flow regime transition, void distribution and gas-liquid interfacial area concentration in the packed bed. (3) Obtain database on flow regime transition, pressure drop, void distribution, interfacial area concentration and liquid hold up as a function of bed characteristics such as bed particle size, porosity, and liquid properties such as viscosity and surface tension. (4) Develop mathematical model for flow regime transition, void fraction distribution and interfacial area concentration for co-current gas-liquid flow through the porous bed in gravity and micro gravity conditions.(4) Develop mathematical model for the flooding phenomena in counter-current gas-liquid flow through the porous bed in gravity and micro gravity conditions. The present proposal addresses the most important topic of HEDS-specific microgravity fluid physics research identified by NASA 's one of the strategic enterprises, OBPR Enterprise. The proposed project is well defined and makes efficient use of the ground-based parabolic flight research aircraft facility. The

  4. 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

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

    PubMed Central

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

    2009-01-01

    Smokeless tobacco contains 28 known carcinogens and causes precancerous oral lesions and oral and pancreatic cancer. A recent study conducted by our research team identified 8 different polycyclic aromatic hydrocarbons (PAH) in U.S. moist snuff, encouraging further investigations of this group of toxicants and carcinogens in smokeless tobacco products. In this study, we developed a gas chromatography-mass spectrometry method that allows simultaneous analysis of 23 various PAH in smokeless tobacco after a simple two-step extraction and purification procedure. The method produced coefficients of variation under 10% for most PAH. The limits of quantitation for different PAH varied between 0.3 ng/g tobacco and 11 ng/g tobacco, starting with a 300-mg sample. The recovery of the stable isotope-labeled internal standards averaged 87%. The method was applied to analysis of 23 moist snuff samples that include various flavors of the most popular U.S. moist snuff brands, as well as 17 samples representing the currently marketed brands of spit-free tobacco pouches, a relatively new type of smokeless tobacco. The sum of all detected PAH in conventional moist snuff averaged 11.6 (± 3.7) µg/g dry weight, 20% of this amount being comprised by carcinogenic PAH. The levels of PAH in new spit-free tobacco products were much lower than those in moist snuff, the sum of all detected PAH averaging 1.3 (±0.28) µg/g dry weight. Our findings render PAH one of the most prevalent groups of carcinogens in smokeless tobacco, along with tobacco-specific nitrosamines. Urgent measures are required from the U.S. tobacco industry to modify manufacturing processes so that the levels of these toxicants and carcinogens in the U.S. moist snuff are greatly reduced. PMID:19860436

  6. 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.

  7. Lagrangian approach to modeling unsteady gas-liquid flow in a well

    NASA Astrophysics Data System (ADS)

    Liapidevskii, V. Yu; Tikhonov, V.

    2016-06-01

    The purpose of this paper is to develop a numerical method of solving the problem of evolution of the finite gas volume that entered in a liquid flow at a set flow rate. The drift- flux model is used as gas-liquid mixture equations. The velocities of both phases, mixture and gas, are related by the Zuber-Findlay equation which coefficients depend on flow regime and gas void fraction. Lagrangian coordinates are used to simplify the initial equations. The numerical solution scheme is proposed. The numerical solution of the Riemann problem is verified by comparison with the exact self-similar solution. The model and numerical method efficiency is illustrated by examples of gas kick calculations in a vertical well.

  8. 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

  9. Microjets and coated wheels: versatile tools for exploring collisions and reactions at gas-liquid interfaces.

    PubMed

    Faust, Jennifer A; Nathanson, Gilbert M

    2016-07-01

    This tutorial review describes experimental aspects of two techniques for investigating collisions and reactions at the surfaces of liquids in vacuum. These gas-liquid scattering experiments provide insights into the dynamics of interfacial processes while minimizing interference from vapor-phase collisions. We begin with a historical survey and then compare attributes of the microjet and coated-wheel techniques, developed by Manfred Faubel and John Fenn, respectively, for studies of high- and low-vapor pressure liquids in vacuum. Our objective is to highlight the strengths and shortcomings of each technique and summarize lessons we have learned in using them for scattering and evaporation experiments. We conclude by describing recent microjet studies of energy transfer between O2 and liquid hydrocarbons, HCl dissociation in salty water, and super-Maxwellian helium evaporation. PMID:27126211

  10. 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.

  11. 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.

  12. Controllable gas/liquid/liquid double emulsions in a dual-coaxial microfluidic device.

    PubMed

    Xu, Jian-Hong; Chen, Ran; Wang, Yun-Dong; Luo, Guang-Sheng

    2012-05-01

    This article presents a simple and novel approach to prepare monodispersed gas-in-oil-in-water (G/O/W) and gas-in-water-in-oil (G/W/O) double-emulsions in the same dual-coaxial microfluidic device. The effects of three phase flow rates on the sizes of microbubbles and droplets and the number of the encapsulated microbubbles were systematically studied. We successfully synthesized two different types of gas/liquid/liquid (G/L/L) double emulsions with different inner structures in the same geometry by adjusting the flow rates sequentially. Mathematical models were developed to predict the size and structures of the double emulsions. This simple approach gives a new idea for preparing hollow and porous microspheres with microbubbles as the direct core/pores templates. PMID:22508390

  13. Hydrodynamics of two-phase flow in gas-liquid cylindrical cyclone separators

    SciTech Connect

    Arpandi, I.; Joshi, A.R.; Shoham, O.

    1995-12-31

    This paper presents new experimental data and an improved mechanistic model for the Gas-Liquid Cylindrical Cyclone (GLCC) separator. The data were acquired utilizing a 3 inch ID laboratory-scale GLCC, and are presented along with a limited number of field data. The data include measurements of several parameters of the flow behavior and the operational envelope of the GLCC. The operational envelope defines the conditions for which there will be no liquid carry-over or gas carry-under. The developed model enables the prediction of the hydrodynamic flow behavior in the GLCC, including the operational envelope, equilibrium liquid level, vortex shape, velocity and holdup distributions and pressure drop across the GLCC. The predictions of the model are compared with the experimental data. These provide the state-of-the-art for the design of GLCC`s for the industry.

  14. Performance improvement of gas liquid cylindrical cyclone separators using passive control system

    SciTech Connect

    Wang, S.; Mohan, R.; Shoham, O.; Kouba, G.

    1998-12-31

    The performance of Gas Liquid Cylindrical Cyclone (GLCC) separators can be improved by reducing or eliminating liquid carry-over into the gas stream or gas carry-under through liquid stream, utilizing suitable liquid level control. In this study, a new passive control system has been developed for the GLCC, in which the control is achieved by utilizing only the liquid flow energy. Passive control system is highly desirable for remote, unmanned location operated with no external power source. Salient features of this design are presented here. Detailed experimental and modeling studies have been conducted to evaluate the improvement in the GLCC operational envelope for liquid carry-over with the passive control system. The results demonstrate that a passive control system is feasible for operation in normal slug flow conditions. The result of this study could also form the basis for future development of active control systems using classical control approach.

  15. State of the art of gas/liquid cylindrical-cyclone compact-separator technology

    SciTech Connect

    Shoham, O.; Kouba, G.E.

    1998-07-01

    The petroleum industry has relied mainly on conventional, vessel-type separators to process wellhead production of oil/water/gas flow. However, economic and operational pressures continue to force the industry to seek less expensive and more efficient separation alternatives in the form of compact separators, especially for offshore applications. Compared with vessel-type separators, compact separators, such as the gas/liquid cylindrical cyclone (GLCC), are simple, low-cost, low-weight separators that require little maintenance and are easy to install and operate. However, the inability to predict GLCC performance adequately has inhibited its wide-spread deployment. Current R and D is aimed at creating the necessary performance-prediction tools for proper design and operation of GLCC separators. This paper presents the status of the development of the GLCC, the state of the art with respect to its simulation and design, and current successful and potential applications.

  16. 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

  17. 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

  18. 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

  19. A macroscopic model for countercurrent gas-liquid flow in packed columns

    SciTech Connect

    Dankworth, D.C.; Sundaresan, S. )

    1989-08-01

    A macroscopic model based on the volume-averaged equations of motion is presented for countercurrent gas-liquid flow in a packed bed. The model yields a column-limited flooding point as the loss of existence of uniform states. It correctly predicts the existence of two uniform states below the flooding point. The lower branch corresponds to the trends commonly observed experimentally. It is shown that the upper branch is made unattainable by the gas distributor/support plate at the bottom of the column. The occurrence of premature flooding induced by the support plate is also explained. It is suggested that the occurrence of spontaneous liquid segregation, necessitating frequent liquid redistribution in columns with large dumped packings and porosities, is a consequence of the loss of stability of the uniform state in the lower branch.

  20. Gas-liquid type phase transition in semiivietals at low temperatures and high magnetic fields

    NASA Astrophysics Data System (ADS)

    Mase, Shoichi; Fukami, Takeshi; Mori, Masatoshi; Inoue, Tomnio

    1982-07-01

    Remarkable anomalies have been found in the temperature and frequency dependences of the attenuation coefficient of sound waves in bismuth, antimony and pyrolytic graphite at low temperatures and high magnetic fields. The result for bismuth in particular is app]arently similar to those observed in second-order phase transition phenomena. On the basis of the Nakajima-Yoshioka-Kuramoto theory of the gas-liquid type phase transition in the electron-hole system, these anomalies are fairly well explained in terms of the fluctuation effect above the phase transition temperature, provided that the electron-hole correlation interaction is assumed to be sensitively dependent on the state of the overlapping of the electron and hole Landau levels.

  1. Convergence rates to stationary solutions of a gas-liquid model with external forces

    NASA Astrophysics Data System (ADS)

    Fan, Long; Liu, Qingqing; Zhu, Changjiang

    2012-10-01

    In this paper, we study the asymptotic behaviour of solutions to a gas-liquid model with external forces. Under some suitable assumptions on the initial data, if γ > 1 and \\theta\\in(0,\\frac{\\gamma}{2}]\\cap(0,\\gamma-1]\\cap(0,1-\\alpha\\gamma] , we prove the weak solution (cQ (x, t), u(x, t)) behaviour asymptotically to the stationary one by adapting and modifying the technique of weighted estimates. In addition, if \\theta\\in(0,\\frac{\\gamma}{2}]\\cap(0,\\gamma-1)\\cap(0,1-\\alpha\\gamma] , following the same idea used in Zhang and Fang (2006 Arch. Ration. Mech. Anal. 182 223-53), we estimate the stabilization rate of the solution as time tends to infinity in the sense of L∞ norm.

  2. 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.

  3. 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

  4. 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

  5. A novel method for measuring hollow fiber membrane permeability in a gas-liquid system.

    PubMed

    Lund, L W; Federspiel, W J; Walters, F R; Hattler, B G

    1996-01-01

    Designing an effective intravenous membrane oxygenator requires selecting hollow fiber membranes (HFMs) that present minimal resistance to gas exchange over extended periods of time. Microporous fiber membranes, as used in extracorporeal oxygenators, offer a minimal exchange resistance, but one that diminishes with time because of fiber wetting and subsequent serum leakage. Potentially attractive alternatives are composite HFMs, which inhibit fiber wetting and serum leakage by incorporating a true membrane layer within their porous walls. To evaluate composite and other HFMs, the authors developed a simple apparatus and method for measuring HFM permeability in a gas-liquid system under conditions relevant to intravenous oxygenation. The system requires only a small volume of liquid that is mixed with a pitched blade impeller driven by a direct current motor at controlled rates. Mass flux is measured from the gas flow exiting the fibers, eliminating the necessity of measuring any liquid side conditions. The authors measured the CO2 exchange permeabilities of Mitsubishi MHF 200L composite HFMs, KPF 280E microporous HFMs, and KPF 190 microporous HFMs. The membrane permeabilities to CO2 were 9.3 x 10(-5) ml/cm2/sec/cmHg for the MHF 200L fiber, 4.7 x 10(-4) ml/cm2/sec/cmHg for the KPF 280E fiber, and 2.8 x 10(-4) ml/cm2/sec/cmHg for the KPF 190 fiber. From these results it is concluded that 1) because of liquid-fiber surface interactions, the permeabilities of the microporous fibers are several orders of magnitude less than would be measured for completely gas filled pores, emphasizing the importance of measuring microporous fiber permeability in a gas-liquid system; and 2) the liquid diffusional boundary layer adjacent to the fibers generated by the pitched blade impeller is unique to each fiber, resulting in different boundary layer characterizations. PMID:8944921

  6. Crude oil and natural gas pricing. Chapters 300 to 499: natural gas liquids, natural gas

    SciTech Connect

    Kelly, P.D.

    1980-01-01

    This text analyzes the federal statutes and regulations that affect the pricing and allocation of crude oil, natural gas, and natural gas liquids. It does not cover refined products or imported crude oil except where necessary to place major decisions in historical context. Chapter 300 concerns natural gas liquids. For historical rather than logical reasons, these are regulated as an offshoot of crude oil controls rather than as a by-product of natural gas production. In December 1979, the Economic Regulatory Administration (ERA) deregulated butane and natural gasoline. However, it did not amend 10 CFR 212.161-212.173, and it did not deregulate propane or propane mixtures. Decontrol will be covered in the first update to this book. Chapters 400 to 468 concern natural gas. Although a great deal of attention has been focused on the Natural Gas Policy Act (NGPA), there has been no satisfactory description of the extent to which the Natural Gas Act (NGA; passed in 1938 and amended by the Phillips decision in 1954) still applies. This is quite a problem, since the NGPA is written in vague terms that encourage producers to disregard the NGA. The problem is compounded by the Federal Power Commission's (FPC) approach to regulatory development, which has scattered crucial regulations throughout 18 CFR. All Federal Energy Regulatory Commission (FERC) natural gas production regulations should be repealed, arranged into a systematic grouping, and reissued in a consolidated subpart of 18 CFR. Shortly after the publication of this text, the author will petition the FERC to commence a rulemaking proceeding to that effect. Chapters 480 to 498 will cover the use of natural gas. These chapters will be issued in the first revision to this text as general summaries since the programs do not directly affect gas producers.

  7. 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

  8. 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.

  9. 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.

  10. 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…

  11. Analysis of therapeutic proteins and peptides using multiangle light scattering coupled to ultra high performance liquid chromatography.

    PubMed

    Espinosa-de la Garza, Carlos E; Miranda-Hernández, Mariana P; Acosta-Flores, Lilia; Pérez, Néstor O; Flores-Ortiz, Luis F; Medina-Rivero, Emilio

    2015-05-01

    Analysis of the physical properties of biotherapeutic proteins is crucial throughout all the stages of their lifecycle. Herein, we used size-exclusion ultra high performance liquid chromatography coupled to multiangle light scattering and refractive index detection systems to determine the molar mass, mass-average molar mass, molar-mass dispersity and hydrodynamic radius of two monoclonal antibodies (rituximab and trastuzumab), a fusion protein (etanercept), and a synthetic copolymer (glatiramer acetate) employed as models. A customized instrument configuration was set to diminish band-broadening effects and enhance sensitivity throughout detectors. The customized configuration showed a performance improvement with respect to the high-performance liquid chromatography standard configuration, as observed by a 3 h column conditioning and a higher resolution analysis in 20 min. Analysis of the two monoclonal antibodies showed averaged values of 148.0 kDa for mass-average molar mass and 5.4 nm for hydrodynamic radius, whereas for etanercept these values were 124.2 kDa and 6.9 nm, respectively. Molar-mass dispersity was 1.000 on average for these proteins. Regarding glatiramer acetate, a molar mass range from 3 to 45 kDa and a molar-mass dispersity of 1.304 were consistent with its intrinsic peptide diversity, and its mass-average molar mass was 10.4 kDa. Overall, this method demonstrated an accurate determination of molar mass, overcoming the difficulties of size-exclusion chromatography. PMID:25727056

  12. Trend analysis of performance parameters of pre-packed columns for protein chromatography over a time span of ten years.

    PubMed

    Scharl, Theresa; Jungreuthmayer, Christian; Dürauer, Astrid; Schweiger, Susanne; Schröder, Tim; Jungbauer, Alois

    2016-09-23

    Pre-packed small scale chromatography columns are increasingly used for process development, for determination of design space in bioprocess development, and for post-licence process verifications. The packing quality of 30,000 pre-packed columns delivered to customers over a period 10 years has been analyzed by advanced statistical tools. First, the data were extracted and checked for inconsistencies, and then were tabulated and made ready for statistical processing using the programming language Perl (https://www.perl.org/) and the statistical computing environment R (https://www.r-project.org/). Reduced HETP and asymmetry were plotted over time to obtain a trend of packing quality over 10 years. The obtained data were used as a visualized coefficient of variation analysis (VCVA), a process that has often been applied in other industries such as semiconductor manufacturing. A typical fluctuation of reduced HETP was seen. A Tsunami effect in manufacturing, the effect of propagation of manufacturing deviations leading to out-of-specification products, was not observed with these pre-packed columns. Principal component analysis (PCA) showed that all packing materials cluster. Our data analysis showed that the current commercially available chromatography media used for biopharmaceutical manufacturing can be reproducibly and uniformly packed in polymer-based chromatography columns, which are designed for ready-to-use purposes. Although the number of packed columns has quadrupled over one decade the packing quality has remained stable. PMID:27575920

  13. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.

    1989-01-01

    -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.

  14. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres.

    PubMed

    Valentin, J R

    1989-03-01

    -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. PMID:11539794

  15. Counter-current chromatography for oil analysis: retention features and kinetic effects.

    PubMed

    Maryutina, Tatyana A; Soin, Alexander V; Katasonova, Olesya N

    2009-05-01

    Application of counter-current chromatography (CCC) for oil analysis has been suggested for the first time. CCC looks very promising as a tool for pre-concentration and isolation of trace elements from oil. Features of stationary phase retention of two-phase liquid systems (oil or oil products-aqueous nitric acid solutions) in CCC have been investigated. The influence of physicochemical properties of crude oil and oil products used as a mobile phase on the volume of stationary phase (acidic aqueous solutions) retained in CCC was studied. Chromatographic behavior of several oil samples was studied. It has been shown that physicochemical properties of test oil influence its chromatographic behavior. Optimal values of density and viscosity (rho<0.85g/cm(3), n<7cSt) of crude oil and oil products that could be analyzed using CCC were estimated. The influence of the column rotational speed and flow rate of mobile phase on the stationary phase retention was also investigated. It is known that kinetic aspects (mass transfer of elements between phases) can play a very important role in selecting an optimal composition of stationary phase for the pre-concentration of elements from oil. The influence of nitric acid concentration in the stationary phase on mass transfer was studied. Kinetic characteristic for trace element recovery has been investigated for the optimization of pre-concentration conditions of trace elements from crude oil and oil products. The extraction recoveries of Zn, Mn, Fe, Ni, V, Cu, Cd, Pb and Ba by CCC in dynamic mode are in the range of 75-95% while they are lower than 35% under batch conditions. PMID:19232415

  16. Analysis of Almond-Violet Oil by Gas Chromatography (A Traditional Formula)

    PubMed Central

    Feyzabadi, Zohre; Pasalar, Mehdi

    2016-01-01

    Background: Viola odorata L. belongs to Violaceae family and is native to Iran. It is used in the form of Almond-Violet oil in traditional Persian medicine (TPM) since ancient times. Almond-Violet oil was used for the treatment of insomnia, headache, cough, and fever based on TPM textbooks. There are two methods for the preparation of Almond-Violet oil. The first is macerating voila flowers in sweet almond oil for several days under the sunlight. The second method is cold pressing of violet flowers and sweet almond. Methods: In this study, after mixing the violet flowers with sweet almonds in 1:2 proportions, Almond-Violet oil was obtained under pressure. Fatty acid ingredients of Almond-Violet oil were analyzed by gas chromatography (GC) technique. Results: Analysis of Almond-Violet oil by GC method showed some major components such as oleic acid (70.54%), linoleic acid (Omega-6 fatty acids) (18.22%), palmitic acid (8.51%), stearic acid (1.58%), and palmitoleic acid (0.69%). Monounsaturated fat consumption has been considered to decrease low-density lipoprotein (LDL) cholesterol. Linoleic acid lipid radicals can also be used to act as an antioxidant agent in natural phenols. On the other hand, oleic acid may be responsible for the hypotensive (blood pressure reducing) effects. Palmitoleic acid is a beneficial fatty acid not only to increase insulin sensitivity by suppressing inflammation, but also to inhibit the destruction of insulin-secreting pancreatic beta cells. Conclusion: In some aspects, the result of the present study does not fully match with the standards of the Europe Pharmacopoeia. This could be due to differences associated with the environment and cultivation of the plants. Such differences should be considered whilst studying native plants. PMID:26722138

  17. 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

  18. Quantitative analysis of antibiotics in aquifer sediments by liquid chromatography coupled to high resolution mass spectrometry.

    PubMed

    Tong, Lei; Liu, Hui; Xie, Cong; Li, Minjing

    2016-06-24

    A highly effective analytical method for multi-residue determination of antibiotics in aquifer sediments was first established in this study. Microwave-assisted solvent extraction (MASE) and solid-phase extraction were used for sample pre-concentration and purification, ultra-high performance liquid chromatography coupled to hybrid quadrupole-high resolution Orbitrap mass spectrometry (UHPLC-Q-Orbitrap) was applied for detection. For high resolution mass spectrometry (HRMS), the target compounds were tentatively identified by retention time and accurate mass which was measured with precursor ions in Target-SIM scan, and then confirmed by the monitoring of daughter ion fragments which were generated in dd-MS(2) scan. The results provided good mass accuracy with mass deviations below 2ppm (except norfloxacin with -2.3ppm) for quantitative analysis of the compounds by HRMS. Reasonable recoveries of all analytes were obtained more than 60% (except doxytetracycline) in fortification samples at concentrations higher than 10μgkg(-1). Relative standard deviations of repeatability and inter-day precision were below 21% and 11%. Limits of detection (LOD) ranged from 0.1 to 3.8μgkg(-1), whereas limits of quantification (LOQ) were established between 0.3-9.0μgkg(-1). The method was applied to analyze real aquifer sediment samples in different aquifer depth of 4.0, 7.5, 13.0 and 18.0m. Chlorotetracycline and ofloxacin were observed at relative high concentrations of 53 and 19μgkg(-1) respectively in 18.0m deepness. The exposure to low doses of these compounds in subsurface environment increases concerns on long-term ecological security of underground system. PMID:27215464

  19. Quantitative analysis of glycerol levels in human urine by liquid chromatography-tandem mass spectrometry.

    PubMed

    Dong, Ying; Ma, Yanhua; Yan, Kuan; Shen, Li; Wang, Xiaobing; Xu, Youxuan; He, Genye; Wu, Yun; Lu, Jianghai; Yang, Zhiyong; Feng, Feifei

    2014-04-15

    Glycerol has the latent capacity to act as a plasma volume expander and disguise blood doping practices. Therefore, it has been prohibited in sports as a masking agent by the World Anti-Doping Agency (WADA) since January 2010 and a urinary threshold (1mg/mL) was recommended recently [1]. The purpose of this study was to establish and validate a novel quantitative method for the determination of urinary glycerol concentrations using a liquid chromatography-tandem mass spectrometry approach. This simple yet highly specific method made use of the derivatization of glycerol by benzoyl chloride in aqueous solution at 40°C followed by analysis via LC-ESI-MS/MS without sample pre-concentration or cleanup. The assay was linear over the concentration range of 1.0-1000μg/mL for glycerol in human urine. The lower limit of detection (LLOD) and lower limit of quantitation (LLOQ) were 0.3μg/mL and 1.0μg/mL, respectively. The intra- and inter-day precision of the method at three concentration levels (3, 500 and 900μg/mL) was less than 12.2%. The method also afforded satisfactory results in terms of accuracy, derivatization yield, extraction recovery, matrix effect and specificity. The method has been successfully applied to the detection of glycerol in "Quality Assurance Program" samples provided by the World Association of Anti-Doping Scientists (WAADS) and routine doping-control samples in our laboratory. PMID:24657408

  20. Analysis of daphnane orthoesters in poisonous Australian pimelea species by liquid chromatography-tandem mass spectrometry.

    PubMed

    Chow, Sharon; Fletcher, Mary T; McKenzie, Ross A

    2010-06-23

    Cattle grazing in arid rangelands of Australia suffer periodic extensive and serious poisoning by the plant species Pimelea trichostachya, P. simplex, and P. elongata. Pimelea poisoning (also known as St. George disease and Marree disease) has been attributed to the presence of the diterpenoid orthoester simplexin in these species. However, literature relating to previous studies is complicated by taxonomic revisions, and the presence of simplexin has not previously been verified in all currently recognized taxa capable of inducing pimelea poisoning syndrome, with no previous chemical studies of P. trichostachya (as currently classified) or P. simplex subsp. continua. We report here the isolation of simplexin from P. trichostachya and the development of a liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) method to measure simplexin concentrations in pimelea plant material. Simplexin was quantified by positive-ion atmospheric pressure chemical ionization (APCI) LC-MS/MS with selected reaction monitoring (SRM) of the m/z 533.3 > 253.3 transition. LC-MS/MS analysis of the four poisonous taxa P. trichostachya, P. elongata, P. simplex subsp. continua, and P. simplex subsp. simplex showed similar profiles with simplexin as the major diterpenoid ester component in all four taxa accompanied by varying amounts of related orthoesters. Similar analyses of P. decora, P. haematostachya, and P. microcephala also demonstrated the presence of simplexin in these species but at far lower concentrations, consistent with the limited reports of stock poisoning associated with these species. The less common, shrubby species P. penicillaris contained simplexin at up to 55 mg/kg dry weight and would be expected to cause poisoning if animals consumed sufficient plant material. PMID:20507137

  1. Multiresidue analysis of pesticides with hydrolyzable functionality in cooked vegetables by liquid chromatography tandem mass spectrometry.

    PubMed

    Lee, Sung Joong; Park, Semin; Choi, Jin Young; Shim, Jae-Han; Shin, Eun-Ho; Choi, Jeong-Heui; Kim, Soo Taek; Abd El-Aty, A M; Jin, Jong Sung; Bae, Dong Won; Shin, Sung Chul

    2009-07-01

    It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean-up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB-C(18) column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100gamma(ij) (%). A high matrix effect (<-30%) was detected for the seven polar pesticides, namely thiamethoxam, clothianidin, acetamiprid, aldicarb, thiacloprid, pirimicarb and methabenzthiazuron. The limits of detection were in the range of 0.1-8.1 microg/kg, indicating a good sensitivity. Most of the recoveries ranged from 70 to 131% with RSDs

  2. 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.

  3. Study and modeling of the evolution of gas-liquid partitioning of hydrogen sulfide in model solutions simulating winemaking fermentations.

    PubMed

    Mouret, Jean-Roch; Sablayrolles, Jean-Marie; Farines, Vincent

    2015-04-01

    The knowledge of gas-liquid partitioning of aroma compounds during winemaking fermentation could allow optimization of fermentation management, maximizing concentrations of positive markers of aroma and minimizing formation of molecules, such as hydrogen sulfide (H2S), responsible for defects. In this study, the effect of the main fermentation parameters on the gas-liquid partition coefficients (Ki) of H2S was assessed. The Ki for this highly volatile sulfur compound was measured in water by an original semistatic method developed in this work for the determination of gas-liquid partitioning. This novel method was validated and then used to determine the Ki of H2S in synthetic media simulating must, fermenting musts at various steps of the fermentation process, and wine. Ki values were found to be mainly dependent on the temperature but also varied with the composition of the medium, especially with the glucose concentration. Finally, a model was developed to quantify the gas-liquid partitioning of H2S in synthetic media simulating must to wine. This model allowed a very accurate prediction of the partition coefficient of H2S: the difference between observed and predicted values never exceeded 4%. PMID:25763810

  4. 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.

  5. Analysis of benzyldimethyldodecylammonium bromide in chemical disinfectants by liquid chromatography and capillary electrophoresis.

    PubMed

    Ding, Xiaojing; Mou, Shifen; Zhao, Shan

    2004-06-11

    Two novel analytical methodologies using capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) were developed and compared for the determination of benzyldimethyldodecylammonium bromide (BAB) in commercial compound chemical disinfectants. The LC analysis was performed with a Kromasil C18 (200 mm x 4.6 mm, 5 microm) column and a mobile phase of A:B = 80:20 (A: acetonitrile, B: 4 mmol/L octanesulfonic sodium--0.02 mol/L acetic sodium, adjusted with acetic acid to pH 5.2) at a flow rate of 1.0 mL/min. Detection was by ultraviolet absorption at 262 nm. The CE analysis was performed in a bare fused-silica capillary with 75 microm i.d. and total length of 46.4 cm with a buffer solution of 50% acetonitrile -50 mmol/L NaH2PO4, pH 2.24. The applied voltage was 20 kV. Detection was by ultraviolet absorption at 214 nm. Under optimized conditions, the HPLC retention time and CE migration time for BAB was 9.18 and 5.08 min, respectively. Calibration curves of peak area versus concentration gave correlation coefficients of 0.9996 for HPLC and 0.9994 for CE. The detection limits for HPLC and CE were 1.6 mg/L and 0.2 mg/L, respectively. Average recoveries at three concentration levels (50, 100, 200 mg/L for HPLC: 20, 40, 100 mg/L for CE) were 99.94 +/- 1.5, 99.64 +/- 1.3 and 99.61 +/- 0.4% for HPLC and 120.47 +/- 2.6, 102.06 +/- 8.7 and 103.05 +/- 3.0% for CE, respectively. Although both methods were shown to be suitable for the determination of BAB in commercial disinfectant compounds, CE provided analysis with less solvent purchase/disposal and better column efficiency, whereas HPLC provided superior precision. PMID:15250425

  6. 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

  7. 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

  8. 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.

  9. 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

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

    PubMed

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

    2011-10-15

    Chlorine isotope analysis of chlorinated hydrocarbons like trichloroethylene (TCE) is of emerging demand because these species are important environmental pollutants. Continuous flow analysis of noncombusted TCE molecules, either by gas chromatography/isotope ratio mass spectrometry (GC/IRMS) or by GC/quadrupole mass spectrometry (GC/qMS), was recently brought forward as innovative analytical solution. Despite early implementations, a benchmark for routine applications has been missing. This study systematically compared the performance of GC/qMS versus GC/IRMS in six laboratories involving eight different instruments (GC/IRMS, Isoprime and Thermo MAT-253; GC/qMS, Agilent 5973N, two Agilent 5975C, two Thermo DSQII, and one Thermo DSQI). Calibrations of (37)Cl/(35)Cl instrument data against the international SMOC scale (Standard Mean Ocean Chloride) deviated between instruments and over time. Therefore, at least two calibration standards are required to obtain true differences between samples. Amount dependency of δ(37)Cl was pronounced for some instruments, but could be eliminated by corrections, or by adjusting amplitudes of standards and samples. Precision decreased in the order GC/IRMS (1σ ≈ 0.1‰), to GC/qMS (1σ ≈ 0.2-0.5‰ for Agilent GC/qMS and 1σ ≈ 0.2-0.9‰ for Thermo GC/qMS). Nonetheless, δ(37)Cl values between laboratories showed good agreement when the same external standards were used. These results lend confidence to the methods and may serve as a benchmark for future applications. PMID:21851081

  11. 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

  12. 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

  13. Measurements of liquid-phase turbulence in gas-liquid two-phase flows using particle image velocimetry

    NASA Astrophysics Data System (ADS)

    Zhou, Xinquan; Doup, Benjamin; Sun, Xiaodong

    2013-12-01

    Liquid-phase turbulence measurements were performed in an air-water two-phase flow loop with a circular test section of 50 mm inner diameter using a particle image velocimetry (PIV) system. An optical phase separation method--planar laser-induced fluorescence (PLIF) technique—which uses fluorescent particles and an optical filtration technique, was employed to separate the signals of the fluorescent seeding particles from those due to bubbles and other noises. An image pre-processing scheme was applied to the raw PIV images to remove the noise residuals that are not removed by the PLIF technique. In addition, four-sensor conductivity probes were adopted to measure the radial distribution of the void fraction. Two benchmark tests were performed: the first was a comparison of the PIV measurement results with those of similar flow conditions using thermal anemometry from previous studies; the second quantitatively compared the superficial liquid velocities calculated from the local liquid velocity and void fraction measurements with the global liquid flow rate measurements. The differences of the superficial liquid velocity obtained from the two measurements were bounded within ±7% for single-phase flows and two-phase bubbly flows with the area-average void fraction up to 18%. Furthermore, a preliminary uncertainty analysis was conducted to investigate the accuracy of the two-phase PIV measurements. The systematic uncertainties due to the circular pipe curvature effects, bubble surface reflection effects and other potential uncertainty sources of the PIV measurements were discussed. The purpose of this work is to facilitate the development of a measurement technique (PIV-PLIF) combined with image pre-processing for the liquid-phase turbulence in gas-liquid two-phase flows of relatively high void fractions. The high-resolution data set can be used to more thoroughly understand two-phase flow behavior, develop liquid-phase turbulence models, and assess high

  14. [Research on diagnosis of gas-liquid detonation exhaust based on double optical path absortion spectroscopy technique].

    PubMed

    Lü, Xiao-Jing; Li, Ning; Weng, Chun-Sheng

    2014-03-01

    The effect detection of detonation exhaust can provide measurement data for exploring the formation mechanism of detonation, the promotion of detonation efficiency and the reduction of fuel waste. Based on tunable diode laser absorption spectroscopy technique combined with double optical path cross-correlation algorithm, the article raises the diagnosis method to realize the on-line testing of detonation exhaust velocity, temperature and H2O gas concentration. The double optical path testing system is designed and set up for the valveless pulse detonation engine with the diameter of 80 mm. By scanning H2O absorption lines of 1343nm with a high frequency of 50 kHz, the on-line detection of gas-liquid pulse detonation exhaust is realized. The results show that the optical testing system based on tunable diode laser absorption spectroscopy technique can capture the detailed characteristics of pulse detonation exhaust in the transient process of detonation. The duration of single detonation is 85 ms under laboratory conditions, among which supersonic injection time is 5.7 ms and subsonic injection time is 19.3 ms. The valveless pulse detonation engine used can work under frequency of 11 Hz. The velocity of detonation overflowing the detonation tube is 1,172 m x s(-1), the maximum temperature of detonation exhaust near the nozzle is 2 412 K. There is a transitory platform in the velocity curve as well as the temperature curve. H2O gas concentration changes between 0-7% during detonation under experimental conditions. The research can provide measurement data for the detonation process diagnosis and analysis, which is of significance to advance the detonation mechanism research and promote the research of pulse detonation engine control technology. PMID:25208369

  15. 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

  16. Rapid, quantitative analysis of americium, curium and plutonium isotopes in Hanford samples using extraction chromatography and precipitation plating

    SciTech Connect

    Kaye, J.H.; Strebin, R.S.; Orr, R.D.

    1994-04-01

    Recently developed methods for the rapid, quantitative analysis of americium (Am), curium (Cm), and plutonium (Pu) isotopes in Hanford soil, sludge, and waste-tank samples are described. After dissolution, dilutions are made as necessary based on alpha-energy analysis of a small aliquot of the original solution. isotopic tracers are then added and Am-Cm and Pu are separated by extraction chromatography, coprecipitated with neodymium fluoride, and counted. Examples of alpha spectra are given, and results obtained for Hanford sludge samples are presented.

  17. (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...

  18. 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)

  19. 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…

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

    EPA Science Inventory

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

  1. 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…

  2. 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...

  3. 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

  4. Flow chemistry: intelligent processing of gas-liquid transformations using a tube-in-tube reactor.

    PubMed

    Brzozowski, Martin; O'Brien, Matthew; Ley, Steven V; Polyzos, Anastasios

    2015-02-17

    CONSPECTUS: The previous decade has witnessed the expeditious uptake of flow chemistry techniques in modern synthesis laboratories, and flow-based chemistry is poised to significantly impact our approach to chemical preparation. The advantages of moving from classical batch synthesis to flow mode, in order to address the limitations of traditional approaches, particularly within the context of organic synthesis are now well established. Flow chemistry methodology has led to measurable improvements in safety and reduced energy consumption and has enabled the expansion of available reaction conditions. Contributions from our own laboratories have focused on the establishment of flow chemistry methods to address challenges associated with the assembly of complex targets through the development of multistep methods employing supported reagents and in-line monitoring of reaction intermediates to ensure the delivery of high quality target compounds. Recently, flow chemistry approaches have addressed the challenges associated with reactions utilizing reactive gases in classical batch synthesis. The small volumes of microreactors ameliorate the hazards of high-pressure gas reactions and enable improved mixing with the liquid phase. Established strategies for gas-liquid reactions in flow have relied on plug-flow (or segmented flow) regimes in which the gas plugs are introduced to a liquid stream and dissolution of gas relies on interfacial contact of the gas bubble with the liquid phase. This approach confers limited control over gas concentration within the liquid phase and is unsuitable for multistep methods requiring heterogeneous catalysis or solid supported reagents. We have identified the use of a gas-permeable fluoropolymer, Teflon AF-2400, as a simple method of achieving efficient gas-liquid contact to afford homogeneous solutions of reactive gases in flow. The membrane permits the transport of a wide range of gases with significant control of the stoichiometry of

  5. Modeling 3H-3He Gas-Liquid Phase Transport for Interpretation of Groundwater Age

    NASA Astrophysics Data System (ADS)

    Carle, S. F.; Esser, B.; Moran, J. E.

    2009-12-01

    California’s Groundwater Ambient Monitoring and Assessment (GAMA) Program has measured many hundreds of tritium (3H) and helium-3 (3He) concentrations in well water samples to derive estimates of groundwater age at production and monitoring wells in California basins. However, a 3H-3He age differs from an ideal groundwater age tracer in several respects: (1) the radioactive decay of 3H results in the accumulation of 3He being first-order with respect to 3H activity (versus a zero-order age-mass accumulation process for an ideal tracer), (2) surface concentrations of 3H as measured in precipitation over the last several decades have not been uniform, and (3) the 3H-3He “clock” begins at the water table and not at the ground surface where 3H source measurements are made. To better understand how these non-idealities affect interpretation of 3H-3He apparent groundwater age, we are modeling coupled gas-liquid phase flow and 3H-3He transport including processes of radiogenic decay, phase equilibrium, and molecular diffusion for water, air, 3H, and 3He components continuously through the vadose zone and saturated zone. Assessment of coupled liquid-gas phase processes enables consideration of 3H-3He residence time and dispersion within the vadose zone, including partitioning of tritiogenic 3He to the gas phase and subsequent diffusion into the atmosphere. The coupled gas-liquid phase modeling framework provides direct means to compare apparent 3H-3He age to ideal mean or advective groundwater ages for the same groundwater flow conditions. Examples are given for common groundwater flow systems involving areal recharge, discharge to streams or long-screened wells, and aquifer system heterogeneity. The Groundwater Ambient Monitoring and Assessment program is sponsored by the California State Water Resources Control Board and carried out in cooperation with the U.S. Geological Survey. This work was performed under the auspices of the U.S. Department of Energy by

  6. 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

  7. 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)

  8. 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

  9. 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

  10. Generating singlet oxygen bubbles: a new mechanism for gas-liquid oxidations in water.

    PubMed

    Bartusik, Dorota; Aebisher, David; Ghafari, BiBi; Lyons, Alan M; Greer, Alexander

    2012-02-01

    Laser-coupled microphotoreactors were developed to bubble singlet oxygen [(1)O(2) ((1)Δ(g))] into an aqueous solution containing an oxidizable compound. The reactors consisted of custom-modified SMA fiberoptic receptacles loaded with 150 μm silicon phthalocyanine glass sensitizer particles, where the particles were isolated from direct contact with water by a membrane adhesively bonded to the bottom of each device. A tube fed O(2) gas to the reactor chambers. In the presence of O(2), singlet oxygen was generated by illuminating the sensitizer particles with 669 nm light from an optical fiber coupled to the top of the reactor. The generated (1)O(2) was transported through the membrane by the O(2) stream and formed bubbles in solution. In solution, singlet oxygen reacted with probe compounds (9,10-anthracene dipropionate dianion, trans-2-methyl-2-pentanoate anion, N-benzoyl-D,L-methionine, or N-acetyl-D,L-methionine) to give oxidized products in two stages. The early stage was rapid and showed that (1)O(2) transfer occurred via bubbles mainly in the bulk water solution. The later stage was slow; it arose only from (1)O(2)-probe molecule contact at the gas/liquid interface. A mechanism is proposed that involves (1)O(2) mass transfer and solvation, where smaller bubbles provide better penetration of (1)O(2) into the flowing stream due to higher surface-to-volume contact between the probe molecules and (1)O(2). PMID:22260325

  11. Estimation of Liquid Wall and Interfacial Shear Stress in Horizontal Stratified Gas-liquid Pipe Flow

    NASA Astrophysics Data System (ADS)

    Liu, Yiping; Zhang, Hua; Wang, Jing

    2007-06-01

    A modified two-phase shear stress calculation method for pipe flow problems is explored. A force balance has been set up on the control volume of liquid phase to determine the interfacial friction factor by employing both the measured pressure gradient and liquid height. The gradient of height of liquid layer has been taken into account, which is suitable for the case where the interface may be smooth, rippled or wavy. The correlation of model indicates that the careful estimation for liquid-wall shear stress is necessary, and the assumption of a stationary liquid element is not applicable for the case of higher gas flow rates. The interfacial friction factor evaluated indirectly from experimental liquid height and pressure loss measurements, which are obtained in 50mm ID pipeline for air and water in cocurrent stratified flow, is used to achieve its correlation with the combination of characteristic parameters. The evaluation of new correlation has been conducted by the comparison of the predicted pressure drop with the experimental data. The performance of correlation depends on the form of the gas-liquid interface.

  12. Gas-liquid Phase Distribution and Void Fraction Measurements Using the MRI

    NASA Technical Reports Server (NTRS)

    Daidzic, N. E.; Schmidt, E.; Hasan, M. M.; Altobelli, S.

    2004-01-01

    We used a permanent-magnet MRI system to estimate the integral and spatially- and/or temporally-resolved void-fraction distributions and flow patterns in gas-liquid two-phase flows. Air was introduced at the bottom of the stagnant liquid column using an accurate and programmable syringe pump. Air flow rates were varied between 1 and 200 ml/min. The cylindrical non-conducting test tube in which two-phase flow was measured was placed in a 2.67 kGauss MRI with MRT spectrometer/imager. Roughly linear relationship has been obtained for the integral void-fraction, obtained by volume-averaging of the spatially-resolved signals, and the air flow rate in upward direction. The time-averaged spatially-resolved void fraction has also been obtained for the quasi-steady flow of air in a stagnant liquid column. No great accuracy is claimed as this was an exploratory proof-of-concept type of experiment. Preliminary results show that MRI a non-invasive and non-intrusive experimental technique can indeed provide a wealth of different qualitative and quantitative data and is especially well suited for averaged transport processes in adiabatic and diabatic multi-phase and/or multi-component flows.

  13. Design and Development of Gas-Liquid Cylindrical Cyclone Compact Separators for Three-Phase Flow

    SciTech Connect

    Mohan, Ram S.; Shoham, Ovadia

    1999-10-28

    The objective of this five-year project (October, 1997--September, 2002) is to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project will be executed in two phases. Phase I (1997--2000) will focus on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC) Separator. The activities of this phase will include the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000--2002), the developed GLCC separator will be tested under high pressure and real crudes conditions. This is crucial for validating the GLCC design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP.

  14. Design and Development of Gas-Liquid Cylindrical Cyclone Compact Separators for Three-Phase Flow

    SciTech Connect

    Mohan, R.S.; Shoham, O.

    2001-01-18

    The objective of this five-year project (October 1997 - September 2002) was to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project was executed in two phases. Phase I (1997 - 2000) focused on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC) Separator. The activities of this phase included the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000 - 2002), the developed GLCC separator will be tested under high pressure and real crude conditions. This is crucial for validating the GLCC design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP.

  15. Treatment of Dye Wastewater by Using a Hybrid Gas/Liquid Pulsed Discharge Plasma Reactor

    NASA Astrophysics Data System (ADS)

    Lu, Na; Li, Jie; Wu, Yan; Masayuki, Sato

    2012-02-01

    A hybrid gas/liquid pulsed discharge plasma reactor using a porous ceramic tube is proposed for dye wastewater treatment. High voltage pulsed discharge plasma was generated in the gas phase and simultaneously the plasma channel was permeated through the tiny holes of the ceramic tube into the water phase accompanied by gas bubbles. The porous ceramic tube not only separated the gas phase and liquid phase but also offered an effective plasma spreading channel. The effects of the peak pulse voltage, additive gas varieties, gas bubbling rate, solution conductivity and TiO2 addition were investigated. The results showed that this reactor was effective for dye wastewater treatment. The decoloration efficiency of Acid Orange II was enhanced with an increase in the power supplied. Under the studied conditions, 97% of Acid Orange II in aqueous solution was effectively decolored with additive oxygen gas, which was 51% higher than that with argon gas, and the increasing O2 bubbling rate also benefited the decoloration of dye wastewater. Water conductivity had a small effect on the level of decoloration. Catalysis of TiO2 could be induced by the pulsed discharge plasma and addition of TiO2 aided the decoloration of Acid Orange II.

  16. Design and Development of Gas-Liquid Cylindrical Cyclone Compact Separators for Three-Phase Flow

    SciTech Connect

    Mohan, R.S.; Shoham, O.

    2001-01-10

    The objective of this five-year project (October 1997--September 2002) was to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project was executed in two phases. Phase I (1997--2000) focused on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC) Separator. The activities of this phase included the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000--2002), the developed GLCC separator will be tested under high pressure and real crude conditions. This is crucial for validating the GLCC design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP.

  17. Computer modelling of the surface tension of the gas-liquid and liquid-liquid interface.

    PubMed

    Ghoufi, Aziz; Malfreyt, Patrice; Tildesley, Dominic J

    2016-03-01

    This review presents the state of the art in molecular simulations of interfacial systems and of the calculation of the surface tension from the underlying intermolecular potential. We provide a short account of different methodological factors (size-effects, truncation procedures, long-range corrections and potential models) that can affect the results of the simulations. Accurate calculations are presented for the calculation of the surface tension as a function of the temperature, pressure and composition by considering the planar gas-liquid interface of a range of molecular fluids. In particular, we consider the challenging problems of reproducing the interfacial tension of salt solutions as a function of the salt molality; the simulations of spherical interfaces including the calculation of the sign and size of the Tolman length for a spherical droplet; the use of coarse-grained models in the calculation of the interfacial tension of liquid-liquid surfaces and the mesoscopic simulations of oil-water-surfactant interfacial systems. PMID:26744846

  18. Two parametric flow measurement in gas-liquid two-phase flow

    NASA Astrophysics Data System (ADS)

    Chen, Z.; Chen, C.; Xu, Y.; Zhao, Z.

    The importance and current development of two parametric measurement during two-phase flow are briefly reviewed in this paper. Gas-liquid two-phase two parametric metering experiments were conducted by using an oval gear meter and a sharp edged orifice mounted in series in a horizontal pipe. Compressed air and water were used as gas and liquid phases respectively. The correlations, which can be used to predict the total flow rate and volumetric quality of two-phase flow or volumetric flow rate of each phase, have also been proposed in this paper. Comparison of the calculated values of flow rate of each phase from the correlations with the test data showed that the root mean square fractional deviation for gas flow rate is 2.9 percent and for liquid flow rate 4.4 percent. The method proposed in this paper can be used to measure the gas and liquid flow rate in two-phase flow region without having to separate the phases.

  19. The gas-liquid chromatograph and the electron capture detection in equine drug testing.

    PubMed Central

    Blake, J. W.; Tobin, T.

    1976-01-01

    Three gas-liquid chromatographic (G.L.C.) procedures discussed have been designed around the four "esses" of detection tests--speed, sensitivity, simplicity, and specificity. These techniques are admirably applicable to the very low plasma drug levels encountered in blood testing under pre-race conditions. The methods are equally applicable to post-race testing procedures, where both blood and urine samples are tested. Drugs can only rarely be detected by the electron capture detector (E.C.D.) without a prior derivatization step, which conveys to the drug(s) high electron affinity. Because of broad applicability, two derivatizing agents, heptafluorobutyric (HFBA) and pentafluorpropionic (PFPA) anhydrides are employed. The three techniques, allowing broad coverage of various drug classes are: 1) direct derivatization of drugs to form strongly electron capturing amides and esters. 2) reductive fragmentation of drugs with lithium aluminum hydride to form alcohols, with conversion to ester derivatives. 3) oxidative fragmentation of drugs with potassium dichromate to form derivatizable groups, followed by direct derivatization. PMID:1000157

  20. Continuous Liquid Lifting Experiment for the Gas Well with High Gas-liquid Ratio

    NASA Astrophysics Data System (ADS)

    Wei, N.; Meng, Y. F.; Li, Y. Q.; Chen, X. Y.; Li, Y. J.; Wan, L. P.; Liu, W. B.

    2011-09-01

    The feasible allocation of the gas well with high gas-liquid ratio (GLR> 1 370) depends on the liquid lifting ability of well and reservoir condition. Nowadays, liquid carrying droplet physical model for gas well is represented by sphere and ellipsoid. Since the two models are different from the stress in the gas flow, the critical conditions calculated by two mathematic models derived from those physical models are different in 2.46 times. The visual experimental rack has a lucite tube with the height of 16 m and a diameter of 40 mm. Taking the compressed air and water as the experimental media, we simulated continuous liquid carrying under different gas well conditions, and captured that the actual droplet shape was ellipsoid in the stream by high-speed video camera. In addition, we also tested the wellhead pressure, temperature, and gas production. The experiment result calculated by sphere model has 10% error and that by ellipsoid model has 58.3% error. This paper analyzes the ellipsoid stress state and experimental data, then derives a new ellipsoid mathematic model. We took 7 wells as examples and found that the calculated results were coincided with field production according to the new derived ellipsoid model.