Science.gov

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

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...2013-04-01 false Gas liquid chromatography system for clinical use. ...§ 862.2250 Gas liquid chromatography system for clinical use. ...Identification. A gas liquid chromatography system for clinical...

  3. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ...2014-04-01 false Gas liquid chromatography system for clinical use. ...§ 862.2250 Gas liquid chromatography system for clinical use. ...Identification. A gas liquid chromatography system for clinical...

  4. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...2012-04-01 false Gas liquid chromatography system for clinical use. ...§ 862.2250 Gas liquid chromatography system for clinical use. ...Identification. A gas liquid chromatography system for clinical...

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

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ...2011-04-01 false Gas liquid chromatography system for clinical use. ...§ 862.2250 Gas liquid chromatography system for clinical use. ...Identification. A gas liquid chromatography system for clinical...

  6. Metabolic analysis of serologically defined Neisseria meningitidis isolates by frequency-pulsed electron capture gas-liquid chromatography.

    PubMed Central

    Brooks, J B; Kellogg, D S; Shepherd, M E; Craven, D E

    1981-01-01

    Eight serogroups [A, B, C, D, X, Y, 29E [Z'], and W135] along with nongroupable and nontypable strains of Neisseria meningitidis were cultured in a defined liquid medium. The whole-culture spent medium was extracted, derivatized, and analyzed by frequency-pulsed electron capture gas-liquid chromatography. The frequency-pulsed electron capture gas-liquid chromatography profiles were then used to group the organisms on the basis of their metabolic profiles. First, two basic groups were formed which consisted of elevated spent-medium compounds and reduced spent-medium compounds. Then, these two basic groups were further subdivided on the basis of metabolites and cellular fatty acids detected in the spent medium to form a total of seven metabolic groups. The nongroupable strains (with the exception of two strains) fell within one of these metabolic groups. The elevated spent-medium compounds group contained all of the A, B, Y, and Z' strains, and the reduced spent-medium compounds group contained most of the C and all of the W135 and D strains. The potential usefulness of the metabolic group scheme is discussed. PMID:6787074

  7. 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

  8. 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.

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

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... false Gas liquid chromatography system for clinical use. 862.2250 Section 862.2250 Food...HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory...

  10. Differentiation and characterization of Klebsiella pneumoniae strains by pyrolysis-gas-liquid chromatography-mass spectrometry.

    PubMed Central

    Abbey, L E; Highsmith, A K; Moran, T F; Reiner, E J

    1981-01-01

    Nine coded duplicate strains of capsular nontypable Klebsiella pneumoniae were analyzed by pyrolysis-gas-liquid chromatography-mass spectrometry. All duplicate strains were correctly matched, and individual strains, including seven nontypable strains, were clearly distinguishable from one another. The addition of mass spectrometry to the analysis has aided the process of identification and has provided chemical structural information on K. pneumoniae strains. Application of this technique to the identification of some disease outbreaks or nosocomial problems could be of epidemiological importance, especially when conventional methods do not identify the epidemic strain. PMID:7009639

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

    EPA Science Inventory

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

  12. [Determination of unchanged clonazepam in plasma by gas-liquid chromatography].

    PubMed

    Marliac, Y; Barazi, S

    1989-01-01

    A gas-liquid chromatography method for unchanged clonazepam determination in plasma using a nitrogen-phosphorus detector is presented. The drug is extracted from buffered plasma at pH 9.0 with benzen. The proposed method is simple, rapid and permits to determine clonazepam with a good precision (delta = 3.10 p. cent) and reproductibility (CV = 3.04 p. cent). The method allows the determination of other benzodiazepins. Plasmatics levels of inchanged clonazepam had been determined on some clinical cases. PMID:2690682

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

    PubMed Central

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

    1989-01-01

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

  14. Simultaneous determination of some active ingredients in cough-cold syrups by gas-liquid chromatography.

    PubMed

    Lau, O W; Cheung, Y M

    1990-10-01

    A simple, efficient and accurate gas-liquid chromatography (GLC) method for the simultaneous determination of eight active ingredients in cough-cold syrups has been developed. The active ingredients under study were bromhexine, chlorpheniramine, codeine, dextromethorphan, diphenhydramine, ephedrine/pseudoephedrine, guaiphenesin and papaverine. Before injection, the active ingredients were first separated, from the excipients present in the cough-cold syrups, with chloroform, from alkaline medium. They were then separated by GLC on a glass column (5 ft x 2 mm i.d.) packed with 3% of OV-25 supported on Supelcoport (80-100 mesh). The column temperature was maintained at 170 degrees C for 1 min, then programmed to 265 degrees C at a rate of 10 degrees C min-1, and maintained at this temperature for 10 and 1 min, respectively, for samples with and without papaverine. The flow-rate of the nitrogen carrier gas was 30 ml min-1. A flame-ionisation detector was used for detection, and clomipramine hydrochloride was used as the internal standard. The recoveries of the drugs ranged from 96.0 to 99.7%, and the relative standard deviations for ten replicate determinations ranged from 0.49 to 4.7%. Results are reported for nine commercially available cough-cold syrups. PMID:2270875

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

    PubMed

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

    2012-12-28

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

  16. Data evaluation in chromatography by principal component analysis.

    PubMed

    Cserháti, T

    2010-01-01

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

  17. 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.

  18. 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

  19. 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.

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

    PubMed

    Xie, J

    1999-05-01

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

  1. 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

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

    NASA Astrophysics Data System (ADS)

    Ramskill, Nicholas P.; Wang, Mi

    2011-10-01

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

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

    PubMed

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

    2010-01-01

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

  4. 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%.

  5. 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...

  6. Christhin: Quantitative Analysis of Thin Layer Chromatography

    E-print Network

    Barchiesi, Maximiliano; Renaudo, Carlos; Rossi, Pablo; Pramparo, María de Carmen; Nepote, Valeria; Grosso, Nelson Ruben; Gayol, María Fernanda

    2012-01-01

    Manual for Christhin 0.1.36 Christhin (Chromatography Riser Thin) is software developed for the quantitative analysis of data obtained from thin-layer chromatographic techniques (TLC). Once installed on your computer, the program is very easy to use, and provides data quickly and accurately. This manual describes the program, and reading should be enough to use it properly.

  7. 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)

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

    PubMed

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

    2005-04-01

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

  9. AN ANALYSIS OF FRONT TRACKING FOR CHROMATOGRAPHY BURTON WENDROFF \\Lambda

    E-print Network

    AN ANALYSIS OF FRONT TRACKING FOR CHROMATOGRAPHY BURTON WENDROFF \\Lambda Abstract. We prove that front tracking has a convergent subsequence for the equations of chromatography for initial data. An example of a computation with the latter is presented. Key Words. Chromatography, hyperbolic, front

  10. Chromatography

    MedlinePLUS

    ... high pressure liquid, or ion exchange chromatography. In general, chromatography takes advantage of the differences in the chemicals you want to separate, such as their size, electric charge, or ability to stick to (bind) to ...

  11. Supercritical fluid chromatography in pharmaceutical analysis.

    PubMed

    Desfontaine, Vincent; Guillarme, Davy; Francotte, Eric; Nováková, Lucie

    2015-09-10

    In the last few years, there has been a resurgence of supercritical fluid chromatography (SFC), which has been stimulated by the introduction of a new generation of instruments and columns from the main providers of chromatographic instrumentation, that are strongly committed to advancing the technology. The known limitations of SFC, such as weak UV sensitivity, limited reliability and poor quantitative performance have been mostly tackled with these advanced instruments. In addition, due to the obvious benefits of SFC in terms of kinetic performance and its complementarity to LC, advanced packed-column SFC represents today an additional strategy in the toolbox of the analytical scientist, which may be particularly interesting in pharmaceutical analysis. In the present review, the instrumentation and experimental conditions (i.e. stationary phase chemistry and dimensions, mobile phase nature, pressure and temperature) to perform "advanced SFC" are discussed. The applicability of SFC in pharmaceutical analysis, including the determination of drugs in formulations and biofluids is critically discussed. PMID:25818887

  12. Human Plasma Proteome Analysis by Multidimensional Chromatography Prefractionation and Linear Ion Trap Mass

    E-print Network

    Tian, Weidong

    Human Plasma Proteome Analysis by Multidimensional Chromatography Prefractionation and Linear Ion chromatography has attracted extensive attention, but most published works have focused on the fractionation strong cation exchange chromatography and reversed-phase chromatography. The resulting 30 samples were

  13. 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.

  14. 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; J?drzejczak, 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

  15. 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.

  16. 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...

  17. 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/...

  18. FSU's natural gas liquids business needs investment

    SciTech Connect

    Plotnikov, V.S.; Berman, M.; Angerinos, G.F. )

    1995-03-13

    Production of natural gas liquids has fallen seriously behind its potential in the former Soviet Union (FSU). Restoration of the gas liquids business thus represents a rich investment opportunity. Capital, however, must come from international sources, which remain uncertain about the FSU's legal, commercial, and political systems. If these hurdles can be overcome, FSU output of liquid petroleum gas alone might double between 1990 and 2010. In the FSU, LPG is produced from associated and nonassociated natural gas, condensate, and refinery streams. It also comes from what is known in the FSU as ShFLU--a mixture of propane, butane, pentane, and hexane produced at gas processing plants in Western Siberia and fractionated elsewhere. The paper reviews FSU production of gas liquids focusing on West Siberia, gives a production outlook, and describes LPG use and business development.

  19. Waves and instabilities in inclined gas-liquid pipe flow

    SciTech Connect

    Grolman, E.; Fortuin, J.M.H.

    1996-12-31

    The Modified Apparent Rough Surface (MARS) model successfully predicts liquid holdup and pressure gradient for wavy gas-liquid pipe flow in slightly inclined pipes, up to the transition to slug (intermittent) flow. Additional equations are used to predict the transition from wavy-to-intermittent flow and for the velocity of waves on the gas-liquid interface. In this paper, Linear (stability) Theory is compared with the MARS model, on the basis of measurements in horizontal and slightly inclined (0{degree} {le} {beta} 6{degree}) pipes. Viscous terms in the linear analysis require estimates of shear stresses. Using the MARS model for the interfacial and liquid-to-wall friction factors, stability can be predicted to within reasonable degree of accuracy. Credible wave velocities are also obtained, provided the interfacial waves are not assumed to be marginally stable. Earlier semi-theoretical equations (MARS model) still provide better estimates of both stability and wave velocity and are much easier to handle than Linear Theory. However, the use of good friction factor equations, i.e. those capable of predicting liquid holdup and pressure gradient, has significantly improved the results obtained with Linear Theory. This opens the way to further studies into the mechanisms determining the velocity, growth and instability of waves in gas-liquid pipe flow.

  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. (Downers Grove, IL)

    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. Journal of Chromatography A, 1169 (2007) 7076 Purification of dinosterol for hydrogen isotopic analysis using

    E-print Network

    Gilli, Adrian

    2007-01-01

    Journal of Chromatography A, 1169 (2007) 70­76 Purification of dinosterol for hydrogen isotopic analysis using high-performance liquid chromatography­mass spectrometry Rienk H. Smittenberg, Julian P September 2007 Abstract A semi-preparative normal-phase high-performance liquid chromatography

  3. Differential Protein Expression Analysis via Liquid-Chromatography/Mass-Spectrometry Data Visualization

    E-print Network

    Linsen, Lars

    Differential Protein Expression Analysis via Liquid-Chromatography/Mass-Spectrometry Data, Germany (a) (b) Figure 1: Interactive visualization of liquid-chromatography/mass-spectrometry data: (a of liquid-chromatography/mass-spectrometry data in a 3D space, which allows for the understanding

  4. Recycling Size Exclusion Chromatography for the Analysis and Separation of Nanocrystalline Gold

    E-print Network

    Aazhang, Behnaam

    Recycling Size Exclusion Chromatography for the Analysis and Separation of Nanocrystalline Gold Ali University, MS-60 6100 Main Street, Houston, Texas 77025 Recycling size exclusion chromatography (RSEC defined sizes. This work aims to use size exclusion chromatography, or SEC, as a tool for evaluating

  5. Stability analysis of switching hyperbolic systems: the example of SMB chromatography

    E-print Network

    Bastin, Georges

    Stability analysis of switching hyperbolic systems: the example of SMB chromatography Georges chromatography, how exponential stability (in L2-norm) can be established when the switching mechanism through the specific example of SMB chromatography [16] and to show how exponential stability (in L2-norm

  6. Reliable Peak Selection for Multisample Analysis with Comprehensive Two-Dimensional Chromatography

    E-print Network

    Reichenbach, Stephen E.

    Reliable Peak Selection for Multisample Analysis with Comprehensive Two-Dimensional Chromatography with samples of complex bio-oils analyzed by comprehensive two-dimensional gas chromatography (GCxGC) coupled-dimensional gas chromatography (GCxGC) and comprehensive two-dimensional liquid chroma- tography (LCxLC), hold

  7. Research paper A novel extraction chromatography and MC-ICP-MS technique for rapid analysis of

    E-print Network

    Research paper A novel extraction chromatography and MC-ICP-MS technique for rapid analysis of REE extraction chromatography MC-ICP-MS Post-Archean Australian Shale (PAAS) A new analytical protocol TODGA extraction chromatography step. A dynamic multi-collector cup configuration was developed

  8. Stability analysis of switching hyperbolic systems: the example of SMB chromatography

    E-print Network

    Bastin, Georges

    Stability analysis of switching hyperbolic systems: the example of SMB chromatography Georges chromatography, how exponential stability (in L2-norm) can be established when the switching mechanism the specific example of SMB chromatography [16] and to show how exponential stability (in L2-norm) can

  9. 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.

  10. 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)

  11. 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.

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

    DOEpatents

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

    2001-01-01

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

  13. 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

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

    PubMed Central

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

    2015-01-01

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

  15. Analysis of desmethylmethsuximide using high-performance liquid chromatography.

    PubMed

    Streete, J M; Berry, D J; Clarke, L A; Newbery, J E

    1995-06-01

    Analysis of desmethylmethsuximide by high-performance liquid chromatography (HPLC) is described. After adding an internal standard (IS), 200 microliters of plasma was buffered to pH 4.5 and extracted with dichloroethane. The organic solvent was then evaporated to dryness and the residue reconstituted in 100 microliters of mobile phase prior to injecting a 20 microliters aliquot onto a Hypersil 5 MOS column, which was eluted with acetonitrile/acetate buffer (pH 5.5) 36:64 vol/vol. Constituents were separated in approximately 8 min. Using this method, down to 1.0 mg/L of desmethylmethsuximide in plasma can be accurately determined. The method is suitable for therapeutic monitoring of desmethylmethsuximide in patient samples. PMID:7624925

  16. 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.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  18. 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.

  19. 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

  20. The Use of Gas Chromatography for Biogas Analysis

    NASA Astrophysics Data System (ADS)

    Andersen, Amanda; Seeley, John; Aurandt, Jennifer

    2010-04-01

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

  1. Enzymatic isomerization and epimerization of D-erythrose 4-phosphate and its quantitative analysis by gas chromatography/mass spectrometry.

    PubMed

    Ohashi, K; Terada, T; Kohno, T; Hosomi, S; Mizoguchi, T; Uehara, K

    1984-07-16

    An enzyme preparation from beef liver catalyzed the isomerization and epimerization of D-erythrose 4-phosphate to D-erythrulose 4-phosphate and D-threose 4-phosphate. The presence of D-erythrulose 4-phosphate and D-threose 4-phosphate was demonstrated by several analytical methods. After dephosphorylation, the presence of D-erythrulose and D-threose was confirmed by thin-layer chromatography, gas-liquid chromatography and an enzymatic method depending upon D-erythrulose reductase. The enzymatic products were also identified and simultaneously quantitated by a new procedure using gas chromatography/mass spectrometry. Each of three tetroses was distinguished by the combination of the reduction with sodium borodeuteride and the determination of relative intensities of the ion pairs m/z 379 and 380 of sugar tetritol trifluoroacetate. By gas chromatography/mass spectrometry, we observed that D-threose 4-phosphate was also converted into D-erythrulose 4-phosphate and D-erythrose 4-phosphate. At the equilibrium, about 90% of the tetrose 4-phosphate existed in the form of D-erythrulose 4-phosphate. On the basis of gas chromatography/mass spectrometric evidence together with gas chromatographic and thin-layer chromatographic patterns, it is suggested that the single enzyme of the beef liver catalyzed both reactions of isomerization and epimerization of aldotetrose 4-phosphate. PMID:6547672

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

    PubMed

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

    2015-01-01

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

  3. Supercritical fluid chromatography hyphenated with twin comprehensive two-dimensional gas chromatography for ultimate analysis of middle distillates.

    PubMed

    Adam, Frédérick; Thiébaut, Didier; Bertoncini, Fabrice; Courtiade, Marion; Hennion, Marie-Claire

    2010-02-19

    This paper reports the conditions of online hyphenation of supercritical fluid chromatography (SFC) with twin comprehensive two-dimensional gas chromatography (twin-GCxGC) for detailed characterization of middle distillates; this is essential for a better understanding of reactions involved in refining processes. In this configuration, saturated and unsaturated compounds that have been fractionated by SFC are transferred on two different GC x GC columns sets (twin-GCxGC) placed in the same GC oven. Cryogenic focusing is used for transfer of fractions into the first dimension columns before simultaneous GCxGC analysis of both saturated and unsaturated fractions. The benefits of SFC-twin-GC x GC are demonstrated for the extended alkane, iso-alkane, alkene, naphthenes and aromatics analysis (so-called PIONA analysis) of diesel samples which can be achieved in one single injection. For that purpose, saturated and unsaturated compounds have been separated by SFC using a silver loaded silica column prior to GC x GC analysis. Alkenes and naphthenes are quantitatively recovered in the unsaturated and saturated fractions, respectively, allowing their identification in various diesel samples. Thus, resolution between each class of compounds is significantly improved compared to a single GCxGC run, and for the first time, an extended PIONA analysis of diesel samples is presented. PMID:20053407

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

    PubMed

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

    2012-10-01

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

  5. 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)

  6. Thin layer chromatography - flame ionization detection analysis of in-situ petroleum biodegradation 

    E-print Network

    Stephens, Frank Lanier

    2004-11-15

    . This technique uses thin layer chromatography coupled with flame ionization detection (TLC-FID) to characterize the saturate and aromatic (hydrocarbon) fractions and the resin and asphaltene (non-hydrocarbon, polar) fractions. Other analysis techniques...

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

    EPA Science Inventory

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

  9. 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...

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

    EPA Science Inventory

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

  11. Gas-liquid separator and method of operation

    DOEpatents

    Soloveichik, Grigorii Lev (Latham, NY); Whitt, David Brandon (Albany, NY)

    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.

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

    PubMed

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

    2016-02-01

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

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

    E-print Network

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

    2011-01-01

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

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

    E-print Network

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

    2011-01-28

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

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

    PubMed

    Löfvenberg, L; Backman, L

    2001-05-15

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-05-01

    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 ? = 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 ? = 0.63(4). The obtained values of ? and ? are consistent with those of the Ising universality class.

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

    SciTech Connect

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

    2009-07-01

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

  18. Third-Order Gas-Liquid Phase Transition and the Nature of Andrews Critical Point

    E-print Network

    Tian Ma; Shouhong Wang

    2010-07-13

    The main objective of this article is to study the nature of the Andrews critical point in the gas-liquid transition in a physical-vapor transport (PVT) system. A dynamical model, consistent with the van der Waals equation near the Andrews critical point, is derived. With this model, we deduce two physical parameters, which interact exactly at the Andrews critical point, and which dictate the dynamic transition behavior near the Andrews critical point. In particular, it is shown that 1) the Andrews critical point is a switching point where the phase transition changes from the first order to the third order, 2) the gas-liquid co-existence curve can be extended beyond the Andrews critical point, and 3) the liquid-gas phase transition going beyond Andrews point is of the third order. This clearly explains why it is hard to observe the gas-liquid phase transition beyond the Andrews critical point. Furthermore, the analysis leads naturally the introduction of a general asymmetry principle of fluctuations and the preferred transition mechanism for a thermodynamic system.

  19. 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.

  20. 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

  1. 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.

  2. A Lab Experiment to Introduce Gas/Liquid Solubility

    ERIC Educational Resources Information Center

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

    2008-01-01

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

  3. 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-?m 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

  4. 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...

  5. 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.

  6. CAPILLARY ELECTROPHORESIS AND LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY ANALYSIS OF BISPHENOL A (BPA) IN ENVIRONMENTAL

    E-print Network

    Gosselin, Louis A.

    CAPILLARY ELECTROPHORESIS AND LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY ANALYSIS OF BISPHENOL A (BPA, Augustana Campus April 2015 © Amna Farooq THOMPSON RIVERS UNIVERSITY (Kamloops) #12;ii Abstract Bisphenol is from rivers and streams. Presence of bisphenols in the environment is crucial and use of analytical

  7. Capillary Electrophoresis and Liquid Chromatography-Mass Spectrometry Analysis of Bisphenol A in Environmental Waters

    E-print Network

    Gosselin, Louis A.

    Capillary Electrophoresis and Liquid Chromatography-Mass Spectrometry Analysis of Bisphenol. Cheeptham Bisphenol A (BPA) and its structural analogues (BPF, BPS, BPP, BPZ, BADGE, BPAP, BPAF) are used water is from rivers and streams. Presence of bisphenols in the environment is crucial and use

  8. 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...

  9. 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...

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

    EPA Science Inventory

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

  12. ANALYSIS OF 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...

  13. 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...

  14. 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

  15. 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

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

    PubMed

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

    2014-10-01

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

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

    E-print Network

    Ferguson, Thomas S.

    A variational approach to motion of triple junction of gas, liquid and solid Kensuke Yokoia;b;c;1 a to deal with motion of triple junctions of gas, liquid (or two kinds of uid) and solid based on the level with triple junctions of gas, liquid and solid. Numerical simulations for free surface ows with moving

  18. 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...

  19. 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.

  20. Methods for analysis of conjugated linoleic acids and trans-18:1 isomers in dairy fats by using a combination of gas chromatography, silver-ion thin-layer chromatography/gas chromatography, and silver-ion liquid chromatography.

    PubMed

    Cruz-Hernandez, Cristina; Deng, Zeyuan; Zhou, Jianqiang; Hill, Arthur R; Yurawecz, Martin P; Delmonte, Pierluigi; Mossoba, Magdi M; Dugan, Michael E R; Kramer, John K G

    2004-01-01

    Conjugated linoleic acids (CLA) are octadecadienoic acids (18:2) that have a conjugated double-bond system. Interest in these compounds has expanded since CLA were found to be associated with a number of physiological and pathological responses such as cancer, metastases, atherosclerosis, diabetes, immunity, and body fat/protein composition. The main sources of these conjugated fatty acids are dairy fats. Rumen bacteria convert polyunsaturated fatty acids, especially linoleic and linolenic acids, to CLA and numerous trans- containing mono- and diunsaturated fatty acids. It has been established that an additional route of CLA synthesis in ruminants and monogastric animals, including humans, occurs via delta9 desaturation of the trans-18:1 isomers. To date, a total of 6 positional CLA isomers have been found in dairy fats, each occurring in 4 geometric forms (cis,trans; trans,cis; cis,cis; and trans,trans) for a total of 24. All of these CLA isomers can be resolved only by a combination of gas chromatography (GC), using 100 m highly polar capillary columns, and silver-ion liquid chromatography, using 3 of these 25 cm columns in series. Complete analysis of all the trans-18:1 isomers requires prior isolation of trans monoenes by silver-ion thin-layer chromatography (TLC), followed by GC analysis using the same 100 m capillary columns operated at low temperatures starting from 120 degrees C. These analytical techniques are required to assess the purity of commercial CLA preparations, because their purity will affect the interpretation of any physiological and/or biochemical response obtained. Prior assessment of CLA preparations by TLC is also recommended to determine the presence of any other impurities. The availability of pure CLA isomers will permit the evaluation and analysis of individual CLA isomers for their nutritional and biological activity in model systems, animals, and humans. These techniques are also essential to evaluate dairy fats for their content of specific CLA isomers and to help design experimental diets to increase the level of the desired CLA isomers in dairy fats. These improved techniques are further required to evaluate the CLA profile in monogastric animals fed commercial CLA preparations for CLA enrichment of animal products. This is particularly important because absorption and metabolism will alter the ingested-CLA profile in the animal fed. PMID:15164853

  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 ?6/?3 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. US crude oil, natural gas, and natural gas liquids reserves

    SciTech Connect

    Not Available

    1990-10-05

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

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

    EIA Publications

    2014-01-01

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

  4. 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.

  5. 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.

  6. Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

    SciTech Connect

    Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

    1994-08-01

    Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids.

  7. SUPERCRITICAL FLUID CHROMATOGRAPHY FOR HIGH MOLECULAR WEIGHT ORGANIC ANALYSIS

    EPA Science Inventory

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

  8. Gas-Liquid Coexistence in the Primitive Model for Water

    E-print Network

    F. Romano; P. Tartaglia; F. Sciortino

    2007-05-08

    We evaluate the location of the gas-liquid coexistence line and of the associated critical point for the primitive model for water (PMW), introduced by Kolafa and Nezbeda [J. Kolafa and I. Nezbeda, Mol. Phys. 61, 161 (1987)]. Besides being a simple model for a molecular network forming liquid, the PMW is representative of patchy proteins and novel colloidal particles interacting with localized directional short-range attractions. We show that the gas-liquid phase separation is metastable, i.e. it takes place in the region of the phase diagram where the crystal phase is thermodynamically favored, as in the case of articles interacting via short-range attractive spherical potentials. Differently from spherical potentials, we do not observe crystallization close to the critical point. The region of gas-liquid instability of this patchy model is significantly reduced as compared to equivalent models of spherically interacting particles, confirming the possibility of observing kinetic arrest in an homogeneous sample driven by bonding as opposed to packing.

  9. Analysis of polar metabolites by hydrophilic interaction chromatography--MS/MS.

    PubMed

    Jian, Wenying; Xu, Yaodong; Edom, Richard W; Weng, Naidong

    2011-04-01

    Increasing emphasis has been placed on quantitative characterization of drug metabolites during drug discovery and development. Due to the more polar nature of drug metabolites, quantitative analysis using traditional reversed-phase liquid chromatography tandem mass spectrometry (RPLC-MS/MS) can be quite challenging. As an alternative chromatographic mode, hydrophilic interaction chromatography (HILIC) offers unique advantages for analysis of polar metabolites, providing better retention/separation, higher sensitivity, higher efficiency and potential for ultra-fast analysis to improve throughput. In this article, selected case studies from the authors' own laboratory, and examples from current literature, will be discussed to demonstrate some practical considerations for method development of HILIC-MS/MS assays. The effectiveness of using HILIC-MS/MS for mitigating analytical challenges associated with quantitation of polar metabolites, including phase I and II metabolites of drugs, as well as endogenous metabolites, will be exhibited. PMID:21510763

  10. Analysis of anions in geological brines using ion chromatography

    SciTech Connect

    Merrill, R.M.

    1985-03-01

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

  11. 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)

  12. Solid phase microextraction coupled to liquid chromatography. Analysis of organosulphur compounds avoiding artifacts formation.

    PubMed

    Locatelli, Daniela A; Altamirano, Jorgelina C; Luco, Juan M; Norlin, Rikard; Camargo, Alejandra B

    2014-08-15

    This work proposes the novel application of a microextraction technique, solid phase microextraction (SPME), coupled to liquid chromatography with UV detection (HPLC-UV) for the analysis of organosulfur compounds (OSCs) in garlic samples. Additionally, a comparative study of OSCs profiles obtained by SPME coupled to HPLC-UV and gas chromatography with flame photometric detector (GC-FPD), respectively; was carried out. This study provided complementary evidence about OSCs's lability and "artifacts" formation during the analytical process. Raw, cooked and distilled garlic samples were considered. The target analytes were diallyl disulphide (DADS), diallyl sulphide (DAS), diallyl trisulphide (DATS), allicin, 3-vinyl-4H-1,3-dithiin (3-VD), 2-vinyl-4H-1,2-dithiin (2-VD) and (E)- and (Z)-ajoene, which are the most important OSCs with biological activities present in raw and processed garlic. The coupling of SPME and HPLC showed to be reliable, fast, sensible and selective methodology for OSCs analysis. PMID:24679771

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

    SciTech Connect

    X. Wang; X. Sun; H. Zhao

    2011-09-01

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

  14. 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

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

    SciTech Connect

    Koutney, L.B.

    1992-09-09

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

  16. 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.

  17. Gas Chromatography -Mass Spectrometry

    E-print Network

    Nizkorodov, Sergey

    GCMS - 1 Gas Chromatography - Mass Spectrometry GC-MS ANALYSIS OF ETHANOL AND BENZENE IN GASOLINE Last updated: June 17, 2014 #12;GCMS - 2 Gas Chromatography - Mass Spectrometry GC-MS ANALYSIS). The goal of this experiment is to separate the components in a sample of gasoline using Gas Chromatography

  18. Computerized rapid analysis of complex mixtures by gas chromatography

    SciTech Connect

    Demirgian, J.C.

    1984-04-01

    A computerized rapid analysis system and its application to two research problems are described. The system uses one central minicomputer to gather analog and digital data from several instruments. Various programs calibrate and convert the data into formatted reports. If desired, this computer sends the report to a more powerful mainframe computer for comparison of different reports and establishment of a data base. Data interpretation begins when a calibration program accesses an external standard file, identifies peaks, calculates response factors for each peak, and stores the results on disk. A master program produces a quantitative report based on retention times and two relative retention time index systems. This report is transferred by modem to a mainframe computer. Statistical programs on the mainframe computer compare runs and/or reprint the data in another format. Additional programming allows for the addition and correction of peak names. The entire procedure produces reports rapidly, allows for variable formats, and compares data from multiple runs. The applicability of the system in studying fluid degradation and solvent extraction efficiency is demonstrated. 13 references, 10 figures, 1 table.

  19. 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...

  20. 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 ...

  1. Quantitative analysis of analgoantipyretics in dosage form using planar chromatography.

    PubMed

    Franeta, J T; Agbaba, D D; Eric, S M; Pavkov, S P; Vladimirov, S D; Aleksic, M B

    2001-03-01

    In the therapy of pain of weaker genesis, frequently used drugs usually represent a mix of analgoantipyretics of different chemical structures, mostly derivatives of salicylic acid, pyrazolone and p-aminophenol as well as derivatives of propionic and acetylsalicylic acid. For the determination of these drugs, different chromatographic methods have been applied, mostly HPLC, due to the the lower polarity (pyrazolones derivatives) and thermolability, as well as nonvolatility of compounds investigated. TLC method, considering advantages which include simplicity, reasonable sensitivity, rapidity, excellent resolving power and low cost has been successfully explored for the determination of analgoantipyretic compounds. The aim of this work was to develop a simple and rapid HPTLC method for the determination of acetylsalicylic acid, paracetamol, caffeine and phenobarbitone in dosage form. The determination of analgoantipyretics were performed on pre-coated HPTLC silica gel plates (10 x 20 cm(2)) by development in the mobile phase dichlormethane-ethyl acetate-cyclohexane-isopropanol-0.1 M HCL-formic acid (9:8:3:1.5:0.2:0.2 v/v/v/v/v/v). Migration distances (68.6+0.2 mm, 54.1+0.1 mm, 36.4+0.14 mm and 85.9+0.11 mm for acetylsalicylic acid, paracetamol, caffeine and phenobarbitone, respectively) with low RSD values (0.13--0.39%) showed a satisfactory reproductivity of the chromatographic system. TLC scanner was used for direct evaluation of the chromatograms in the reflectance/absorbance mode. Established calibration curves (r>0.999), precision (0.3--1.02%) and detection limits, as well as recovery values (96.51--98.1%) were validated and found to be satisfactory. The method was found to be reproducible and convenient for the quantitative analysis of compounds investigated in their dosage forms. PMID:11248516

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  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 of the bench-scale equipment continues.

  7. Engineering aspects of gas-liquid catalytic reactions

    SciTech Connect

    Carra, S.; Santacesaria, E.

    1980-01-01

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

  8. 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.

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

    E-print Network

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

    1988-01-01

    Industrial Energy Technology Conference, Houston, TX, September 13-15, 1988 passes to the atmosphere. The heated liquid moves through a closed circuit to tubular exchangers where its heat is transferred to a working fluid. The liquid then recirculates to t... BY DIRECf CONTACf GAS-LIQUID HEAT EXCHANGE James R. Fair and Jose L. Bravo Separations Research Program The University o/Texas at Austin Austin, Texas ABSIRACf Energy from hot gas discharge streams can be recovered by transfer directly to a coolant...

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

    PubMed

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

    2015-04-01

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

  11. Gel permeation chromatography-high performance liquid chromatography combination as an automated clean-up technique for the multiresidue analysis of fats.

    PubMed

    Rimkus, G G; Rummler, M; Nausch, I

    1996-06-14

    The well-known and almost universally utilizable clean-up technique of gel permeation chromatography (GPC) and subsequent conventional silica-gel column chromatography was automated by an on-line solvent evaporation of the GPC fraction, followed by normal-phase HPLC separation. The ternary solvent system n-hexane-toluene-acetone (88:10:2, v/v/v) was used as the mobile phase which resulted in only one HPLC fraction for all relevant analytes. The HPLC column was cleaned automatically after each sample by backflushing with polar solvents. The recoveries and reproducibilities of 35 analytes (mainly organochlorine compounds) were in the range of 77-90% and 3-7%, respectively; the high efficiency of the HPLC separation provide very clean extracts for the GC analysis. This automated clean-up technique is routinely used for the multiresidue analysis of various fat-containing food and biota samples. PMID:8777464

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

    USGS Publications Warehouse

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

    1989-01-01

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

  13. 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.

  14. 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.

  15. 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

  16. Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography.

    PubMed

    Li, Wei; Wang, Jun; Yan, Zheng-Yu

    2015-10-10

    A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods. PMID:26103526

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

    PubMed

    Kostanyan, Artak E

    2015-08-01

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

  18. 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

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

    NASA Astrophysics Data System (ADS)

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

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

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

    PubMed

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

    2016-01-01

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

  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 HazOp review was conducted. Potting and module materials testing continued. Preliminary design of the bench-scale equipment continues. A status meeting was held in Morgantown, WV with the DOE Project Manager.

  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 and module materials testing continued. Preliminary design of the bench-scale equipment continues.

  3. Determination of Np-237 by radiochemical neutron activation analysis combined with extraction chromatography.

    PubMed

    Kalmykov, St N; Aliev, R A; Sapozhnikov, D Yu; Sapozhnikov, Yu A; Afinogenov, A M

    2004-01-01

    A procedure for determination of 237Np, 238Pu, 239,240Pu and 241Pu in environmental samples is described. Neptunium-237 is determined using radiochemical neutron activation analysis with pre- and post-irradiation chemistry based on solvent extraction and extraction chromatography. 238Pu, 239,240Pu is determined using alpha spectrometry and 241Pu by liquid scintillation spectrometry. The vertical profiles of 237Np, 238Pu, 239,240Pu in bottom sediments from the Black Sea are presented. PMID:14987710

  4. 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

  5. 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.

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

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 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...

  7. 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...

  8. 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...

  9. 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...

  10. 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...

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

    SciTech Connect

    Kale, D.D.

    1987-02-01

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

  12. An experimental study of gas-liquid slug flow

    NASA Astrophysics Data System (ADS)

    Mao, Zai-Sha; Dukler, A. E.

    1989-12-01

    Experimental measurements were carried out for upward gas-liquid slug flow in a 50.8 mm diameter pipe. Parallel conductance wires were used to distinguish the Taylor bubbles and liquid slugs and to determine translation velocities and lengths, an electrochemical probe provided the magnitude and direction of the wall shear stress and a radio-frequency local probe was used for the axial and radial distribution of voidage in the liquid slugs. Data are reported over wide range of flow conditions covering slug flow and into the churn flow pattern. Comparison with the Fernandes model predictions are presented. Numerical simulation of slug flow provided information on the structure of flow in a liquid slug and, in particular, on the process of mixing behind a Taylor bubble.

  13. 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

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

    NASA Astrophysics Data System (ADS)

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

    2012-01-01

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

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

    ERIC Educational Resources Information Center

    Bailey, Leonard

    1978-01-01

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

  16. Comparison of microemulsion electrokinetic chromatography and micellar electrokinetic chromatography as methods for the analysis of ten benzophenones.

    PubMed

    Huang, Hsi-Ya; Chiu, Chen-Wen; Chen, Yen-Chen; Yeh, Jui-Ming

    2005-02-01

    Microemulsion electrokinetic chromatography (MEEKC) and micellar electrokinetic chromatograpy (MEKC) were compared for their abilities to separate and detect ten similar benzophenones, which are commonly used as UV filters in various plastic and cosmetic products. Sodium dodecyl sulfate (SDS) concentration and column temperature rarely affected separation resolution for MEEKC, but separation of benzophenones could be improved by changing the SDS concentration and column temperature for MEKC. Buffer pH and ethanol (organic modifier) were found to markedly influence the separation selectivity for both MEEKC and MEKC systems. In addition, a higher electric voltage improved the separation efficiency without a noticeable reduction in separation resolution for MEEKC, whereas it caused a poor separation resolution for the MEKC system. PMID:15714549

  17. 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

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

    SciTech Connect

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

    2010-09-01

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

  19. Determination of partition coefficients from surface acoustic wave vapor sensor responses and correlation with gas-liquid chromatographic partition coefficients

    SciTech Connect

    Grate, J.W.; Snow, A.; Ballantine, D.S. Jr.; Wohltjen, H.; Abraham, M.H.; McGill, R.A.; Sasson, P.

    1988-05-01

    Surface acoustic wave (SAW) devices coated with a thin film of a stationary phase sense chemical vapors in the gas phase by detecting the mass of the vapor that distributes into the stationary phase. This distribution can be described by the partition coefficient. An equation is presented that allows partition coefficients to be calculated from SAW vapor sensor frequency shifts. The experimental responses of fluoropolyol-coated 158-MHz dual delay line SAW vapor sensors are converted to partition coefficients by this method, and these results are compared with partition coefficients determined by gas-liquid chromatography. These two methods rank the vapors in the same order of increasing sorption, but individual partition coefficient values are not always in precise agreement. The influence of temperature and gas-phase vapor concentration on vapor sorption is also examined.

  20. Neutral monosaccharide composition analysis of plant-derived oligo- and polysaccharides by high performance liquid chromatography.

    PubMed

    Yan, Jun; Shi, Songshan; Wang, Hongwei; Liu, Ruimin; Li, Ning; Chen, Yonglin; Wang, Shunchun

    2016-01-20

    A novel analytical method for neutral monosaccharide composition analysis of plant-derived oligo- and polysaccharides was developed using hydrophilic interaction liquid chromatography coupled to a charged aerosol detector. The effects of column type, additives, pH and column temperature on retention and separation were evaluated. Additionally, the method could distinguish potential impurities in samples, including chloride, sulfate and sodium, from sugars. The results of validation demonstrated that this method had good linearity (R(2)?0.9981), high precision (relative standard deviation?4.43%), and adequate accuracy (94.02-103.37% recovery) and sensitivity (detection limit: 15-40ng). Finally, the monosaccharide compositions of the polysaccharide from Eclipta prostrasta L. and stachyose were successfully profiled through this method. This report represents the first time that all of these common monosaccharides could be well-separated and determined simultaneously by high performance liquid chromatography without additional derivatization. This newly developed method is convenient, efficient and reliable for monosaccharide analysis. PMID:26572471

  1. Liquid chromatography of dansyl derivatives of some alkaloids and the application to the analysis of pharmaceuticals.

    PubMed

    Frei, R W; Santi, W; Thomas, M

    1976-01-21

    Derivatization of the alkaloids cephaeline, codeine, emetine, ephedrine, morphine, narcotine and others with dansyl chloride has been studied with the aim of developing a sensitive and specific liquid chromatographic method for these substances in complex pharmaceutical dosage forms. While codeine and narcotine do not react, the other compounds form completely substituted derivatives which possess maxima in their fluorescence emission spectra between 470 and 500 nm. The structure of the derivatives has been confirmed by nuclear magnetic resonance spectroscopy. The dansylated compounds have been separated by thin-layer chromatography and high-pressure liquid chromatography. The improved selectivity and sensitivity have permitted an analysis of these substances present in low concentrations in 10- 100-fold excesses of other drugs. Direct derivatization of syrups and aqueous slurries of capsules having a complex excipient and drug composition is feasible and time saving and serves as a pre-clean-up step. Detection limits are in the 1-10-ng range or better, depending on the efficiency of the detection device. The reproducibility of the method is limited by the derivatization step, but a relative standard deviation of less than 2% can be obtained. The analysis time for these pharmaceuticals may be reduced by at least one fifth of that required by conventional techniques. PMID:1245578

  2. 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

  3. 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

  4. Gas-Liquid Contact Area of Random and Structured Packing Ian David Wilson, B.S.

    E-print Network

    Rochelle, Gary T.

    Gas-Liquid Contact Area of Random and Structured Packing By Ian David Wilson, B.S. Thesis Presented into a liquid solvent, adsorption into a solid, cryogenic separation, permeation through membranes and chemical are preferred over spray and tray towers for gas/liquid contacting when minimizing pressure drop and maximizing

  5. A standing-wave thermoacoustic engine with gas-liquid coupling oscillation

    NASA Astrophysics Data System (ADS)

    Tang, K.; Lei, T.; Jin, T.; Lin, X. G.; Xu, Z. Z.

    2009-06-01

    A thermoacoustic engine usually uses either gas or liquid as the working fluid. However, an analysis based on acoustic-electric analogy indicates that gas-liquid coupling oscillation may lead to lower resonant frequency and larger pressure amplitude. A standing-wave thermoacoustic engine containing a water column was fabricated and tested. Compared with the same apparatus using nitrogen gas, the introduction of a 1.5 kg water column resulted in a drop of resonant frequency by 79.0% and a rise of pressure amplitude by 157.4%, while for the case of helium gas, a drop by 91.4% and a rise by 208.3% were observed, respectively.

  6. 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

  7. 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...

  8. Rapid analysis of caffeine in ``smart drugs'' and ``energy drinks'' by microemulsion electrokinetic chromatography (MEEKC)

    E-print Network

    Miksik, Ivan

    chromatography (MEEKC) Eloisa Liotta a , Rossella Gottardo a , Catia Seri b , Claudia Rimondo b , Ivan Miksik c: gas chromatography­mass spectrometry (GC­MS) [10,11] and HPLC­MS [12,13]. Unfortunately Keywords: Caffeine Energy drink Smart drug Microemulsion electrokinetic chromatography A B S T R A C

  9. 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

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

    PubMed

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

    2015-10-01

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

  11. Comparing micellar electrokinetic chromatography and microemulsion electrokinetic chromatography for the analysis of preservatives in pharmaceutical and cosmetic products.

    PubMed

    Huang, Hsi-Ya; Lai, Yu-Cheng; Chiu, Chen-Wen; Yeh, Jui-Ming

    2003-04-18

    In this study, separation and determination of nine preservatives ranging from hydrophilic to hydrophobic properties, which are commonly used as additives in various pharmaceutical and cosmetic products, by micellar electrokinetic chromatograpy (MEKC) and microemulsion electrokinetic chromatography (MEEKC) were compared. The effect of temperature, buffer pH, and concentration of surfactant on separation were examined. In MEKC, the separation resolution of preservatives improved markedly by changing the sodium dodecyl sulfate concentration. Temperature and pH of running buffers were used mainly to shorten the magnitude of separation time. However, in order to detect all preservatives in a single run in a MEEKC system, a microemulsion of higher pH was needed. The separation resolution was improved dramatically by changing temperature, and a higher concentration of SDS was necessary for maintaining a stable microemulsion solution, therefore the separation of the nine preservatives in MEEKC took longer than in MEKC. An optimum MEKC method for separation of the nine preservatives was obtained within 9.0 min with a running buffer of pH 9.0 containing 20 mM SDS at 25 degrees C. A separation with baseline resolution was also obtained within 16 min using a microemulsion of pH 9.5 which composed of SDS, 1-butanol, and octane, and a shorter capillary column at 34 degrees C. Finally, the developed MEKC and MEEKC methods determined successfully preservatives in various cosmetic and pharmaceutical products. PMID:12735448

  12. Influence of soil type and extraction conditions on perchlorate analysis by ion chromatography.

    PubMed

    MacMillan, Denise K; Dalton, Shana R; Bednar, Anthony J; Waisner, Scott A; Arora, Prem N

    2007-02-01

    Perchlorate is a stable anion that has been introduced into the environment through activities related to its production and use as a solid rocket propellant. Perchlorate is thought to transport through soils without being adsorbed; thus, for determination of perchlorate in soil, samples are typically extracted with water prior to analysis. The completeness of extraction depends on perchlorate existing as a free ion within the soil matrix. In this study, perchlorate extraction efficiency was evaluated with five soil types under two different oxygen states. For each soil, 30% (w/w) slurries were prepared and equilibrated under either oxic or anoxic conditions prior to spiking with a stock solution of sodium perchlorate, and the slurries were then maintained for 1-week or 1-month. At the end of the exposure, slurries were centrifuged and separated into aqueous and soil phases. After phase separation, the soil was washed first with deionized water and then with 50mM NaOH, producing second and third aqueous phases, respectively. Perchlorate concentrations in the three aqueous phases were determined using ion chromatography. The results obtained from this study suggest that matrix interference and signal suppression due to high conductivity have greater effects upon observed perchlorate concentrations by ion chromatography than does perchlorate interaction with soil. Thus, a single water extraction is sufficient for quantitative determination of perchlorate in soil. PMID:17092539

  13. 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.

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

    PubMed Central

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

    2014-01-01

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

  15. Detection of martian amino acids by chemical derivatization coupled to gas chromatography: in situ and laboratory analysis.

    PubMed

    Rodier, C; Vandenabeele-Trambouze, O; Sternberg, R; Coscia, D; Coll, P; Szopa, C; Raulin, F; Vidal-Madjar, C; Cabane, M; Israel, G; Grenier-Loustalot, M F; Dobrijevic, M; Despois, D

    2001-01-01

    If there is, or ever was, life in our solar system beyond the Earth, Mars is the most likely place to search for. Future space missions will have then to take into account the detection of prebiotic molecules or molecules of biological significance such as amino acids. Techniques of analysis used for returned samples have to be very sensitive and avoid any chemical or biological contamination whereas in situ techniques have to be automated, fast and low energy consuming. Several possible methods could be used for in situ amino acid analyses on Mars, but gas chromatography would likely be the most suitable. Returned samples could be analyzed by any method in routine laboratory use such as gas chromatography, already successfully performed for analyses of organic matter including amino acids from martian meteorites. The derivatization step, which volatilizes amino acids to perform both in situ and laboratory analysis by gas chromatography, is discussed here. PMID:11605632

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

    PubMed

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

    2015-04-01

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

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

    SciTech Connect

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

    2005-02-01

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

  18. 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.

  19. Hydrodynamic instabilities in gas-liquid monolithic reactors

    SciTech Connect

    Grolman, E.; Edvinsson, R.K.; Stankiewicz, A.; Moulijn, J.A.

    1996-12-31

    Liquid holdup and pressure drop were measured during the co-current down flow of air and water through a monolith in the Taylor flow regime. The model presented accounts for the significant, up to three fold, increase in frictional pressure drop that is caused by the presence of gas bubbles. It is accurate to within 20%. In addition, the model presented is used to predict hydrodynamic stability, which is defined as the situation where all channels transport gas and liquid in the direction of mass flow. Essential for stability is a sufficiently good initial liquid distribution, which was achieved with a shower-type distributor. Furthermore, distribution was significantly enhanced by the natural occurrence of a well-mixed foam (aerated liquid) layer on top of the monolith at liquid holdup values above 0.5. The quality of the liquid distribution across the monolith follows directly from on-line, integral liquid holdup measurements. Monoliths have been developed and used extensively for catalytic automobile exhaust conversion, from which they have inherited mechanical and thermal robustness. Today, monoliths provide an interesting alternative to trickle-bed and slurry-column technologies, for solid-catalyzed gas-liquid reactions.

  20. 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

  1. The analysis of clobazam and its metabolite desmethylclobazam by high-performance liquid chromatography.

    PubMed

    Streete, J M; Berry, D J; Newbery, J E

    1991-07-01

    The analysis of clobazam and its metabolite desmethylclobazam by high-performance liquid chromatography is described. After adding an internal standard 500 microliters of plasma is extracted under basic conditions into dichloroethane. The organic solvent is then evaporated to dryness and the residue reconstituted in 100 microliters of mobile phase prior to injecting an aliquot (30 microliters) onto a Hypersil 5 MOS column, which is eluted with acetonitrile/acetate buffer (pH 5.4) 40:60 vol/vol. The components are separated in approximately 12 min. Using this method, 15 micrograms L-1 of clobazam and 30 micrograms L-1 of desmethylclobazam can be detected. The method is suitable for the therapeutic monitoring of these two drugs in patient samples. PMID:1780967

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

    PubMed

    Solakyildirim, Kemal; Zhang, Zhenqing; Linhardt, Robert J

    2010-02-01

    Chondroitin sulfate (CS) has an important role in cell division, in the central nervous system, and in joint-related pathologies such as osteoarthritis. Due to the complex chemical structure and biological importance of CS, simple, sensitive, high resolution, and robust analytical methods are needed for the analysis of CS disaccharides and oligosaccharides. An ion-pairing, reversed-phase, ultraperformance liquid chromatography (IPRP-UPLC) separation, coupled to electrospray ionization mass spectrometry with an ion trap mass analyzer, was applied for the analyses of CS-derived disaccharides. UPLC separation technology uses small particle diameter, short column length, and elevated column temperature to obtain high resolution and sensitivity. Hexylamine (15 mM) was selected as the optimal ion-pairing reagent. PMID:19769936

  3. Multiresidue analysis of neonicotinoids by solid-phase extraction technique using high-performance liquid chromatography.

    PubMed

    Mohan, Chander; Kumar, Yogesh; Madan, Jyotsana; Saxena, Navneet

    2010-06-01

    For routine monitoring of pesticides, a multiresidue analysis through solid-phase extraction technique and using high-performance liquid chromatography (HPLC) in cotton seed cake (CSC) has been developed. Extraction of fortified samples was carried out with aqueous acetone under vacuum. The concentrated extract was loaded onto the solid-phase extraction units, preconditioned with acetonitrile. The extraction units were then washed with hexane and finally eluted with acetonitrile. The pesticide residues were determined using a multiresidue method by reversed-phase HPLC. The average percentage recoveries were found to range between 65.47% and 110% at spiking levels of 10 to 40 mg/kg. The method developed shows a healthy rate of recovery and can successfully be utilized for the extraction and screening of neonicotinoid residues in CSC. The detection limits for imidacloprid, acetamiprid, and thiacloprid using this method were found to be 5, 10, and 20 mg/kg, respectively. PMID:19421881

  4. 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…

  5. Theoretical and numerical estimates of the gas-liquid critical point of a primitive model for silica

    E-print Network

    Sciortino, Francesco

    of the system. Indeed, if the gas- liquid critical point lies in the fluid-solid coexistence region, likeTheoretical and numerical estimates of the gas-liquid critical point of a primitive model of the stable gas-liquid criti- cal point in the equilibrium phase diagram is probably asso- ciated

  6. 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

  7. 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.

  8. Analysis of drugs of abuse in urine by gas chromatography/mass spectrometry: experience and application.

    PubMed

    Karaci?, V; Skender, L

    2000-12-01

    This paper describes quantitative methods for determination of urinary drugs/metabolites. The analysis included indicators of opiate (morphine, codeine, 6-monoacetylmorphine) and methadone (methadone) consumption, indicator of marihuana/hashish consumption (11-nor-9-tetrahydrocannabinol-9-carboxylic acid), indicators of cocaine consumption (cocaine, benzoylecgonine, and ecgonine methyl ester) and of amphetamines consumption (amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and 3,4-methylenedioxyethylamphetamine). The methods included solid-phase extraction of urine, concentration of eluent, derivatisation, and quantitative analysis by gas chromatography/mass spectrometry (GC/MS) on a capillary column in the electron impact and selected ion monitoring (SIM) mode. Sensitivity, reproducibility, and accuracy were determined for all analytes (limit of detection between 3 and 12 ng/ml, precision < 10%, accuracy > 92%). The accuracy was checked through analysis of standard reference materials and participation in an international quality assessment programme. The methods were used in the analysis of spot urine samples of 60 subjects suspected of drug abuse. Negative findings indicated several disadvantages of urine as a biological sample. PMID:11276966

  9. 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…

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

    EPA Science Inventory

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

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

    EPA Science Inventory

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

  12. ANALYSIS OF 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...

  13. Analysis of particulate polycyclic aromatic hydrocarbons by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    NASA Astrophysics Data System (ADS)

    Shimmo, Masahiko; Adler, Heidi; Hyötyläinen, Tuulia; Hartonen, Kari; Kulmala, Markku; Riekkola, Marja-Liisa

    An on-line supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS) method was developed for the analysis of the particulate polycyclic aromatic hydrocarbons (PAHs). The limits of detection of the system for the quantification standards were in the range of 0.25-0.57 ng, while the limits of determinations for filter samples varied from 0.02 to 0.04 ng m -3 (24 h sampling). The linearity was excellent from 5 to 300 ng ( R2>0.967). The analysis could be carried out in a closed system without tedious manual sample pretreatment and with no risk of errors by contamination or loss of the analytes. The results of the SFE-LC-GC-MS method were comparable with those for Soxhlet and shake-flask extractions with GC-MS. The new method was applied to the analysis of PAHs collected by high-volume filter in the Helsinki area to study the seasonal trend of the concentrations. The individual PAH concentrations varied from 0.015 to more than 1 ng m -3, while total PAH concentrations varied from 0.81 to 5.68 ng m -3. The concentrations were generally higher in winter than in summer. The mass percentage of the total PAHs in total suspended particulates ranged from 2.85×10 -3% in July to 15.0×10 -3% in December. Increased emissions in winter, meteorological conditions, and more serious artefacts during the sampling in summer season may explain the concentration profiles.

  14. 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)

  15. 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.

  16. 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

  17. Development of miniaturized multi-channel high-performance liquid chromatography for high-throughput analysis.

    PubMed

    Shintani, Yukihiro; Hirako, Keiji; Motokawa, Masanori; Iwano, Takeshi; Zhou, Xiaojing; Takano, Yoshihiko; Furuno, Masahiro; Minakuchi, Hiroyoshi; Ueda, Mitsuyoshi

    2005-05-01

    We have developed miniaturized multi-channel high-performance liquid chromatography (HPLC) system. With this system, we can simultaneously separate multiple samples, using a single high-pressure gradient pump, a chip-based sample injection unit, a monolithic silica capillary column array, and a multi-channel UV detection unit based on fiber optics. The injection unit has a simplified structure composed of brass housing and a quartz microchip having microchannels and access ports, which enable a direct injection of sample to multi-channel by commercial multichannel micropipette. Moreover, that possesses a function of microvalve, and on-chip definition of sample injection plugs achieved with a cross channel injection method, providing each column of monolithic silica capillary array. The substances in channels were simultaneously detected with UV having multiple cells. Standard samples were analyzed for characterizing newly developed system, and sharp peaks were obtained with reproducibility data of < 0.9% (R.S.D.). Analysis of tryptic digestion of casein was also employed. These results show that the novel multi-channel HPLC system has the benefits for the high-throughput analysis in the post-genomic analysis/combinatorial chemistry. PMID:15909501

  18. 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

  19. 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.

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

    PubMed

    Hatfield, Robert G; Turner, Andrew D

    2012-01-01

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

  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. 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.

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

    E-print Network

    Cavalcanti de Sousa, Pedro

    2013-12-09

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

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  5. Characterization of human expired breath by solid phase microextraction and analysis using gas chromatography-mass spectrometry and differential mobility spectrometry

    E-print Network

    Merrick, William (William F. W.)

    2005-01-01

    Breath analysis has potential to become a new medical diagnostic modality. In this thesis, a method for the analysis of human expired breath was developed using gas chromatography-mass spectroscopy. It was subsequently ...

  6. 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

  7. 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.

    2015-10-01

    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.

  8. 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.

  9. Simultaneous quantitative analysis of metabolites using ion-pair liquid chromatography-electrospray ionization mass spectrometry.

    PubMed

    Coulier, Leon; Bas, Richard; Jespersen, Sonja; Verheij, Elwin; van der Werf, Mariët J; Hankemeier, Thomas

    2006-09-15

    We have developed an analytical method, consisting of ion-pair liquid chromatography coupled to electrospray ionization mass spectrometry (IP-LC-ESI-MS), for the simultaneous quantitative analysis of several key classes of polar metabolites, like nucleotides, coenzyme A esters, sugar nucleotides, and sugar bisphosphates. The use of the ion-pair agent hexylamine and optimization of the pH of the mobile phases were critical parameters in obtaining good retention and peak shapes of many of the above-mentioned polar and acidic metabolites that are impossible to analyze using standard reversed-phase LC/MS. Optimum conditions were found when using a gradient from 5 mM hexylamine in water (pH 6.3) to 90% methanol/10% 10 mM ammonium acetate (pH 8.5). The IP-LC-ESI-MS method was extensively validated by determining the linearity (R2 > 0.995), sensitivity (limit of detection 0.1-1 ng), repeatability, and reproducibility (relative standard deviation <10%). The IP-LC-ESI-MS method was shown to be a useful tool for microbial metabolomics, i.e., the comprehensive quantitative analysis of metabolites in extracts of microorganisms, and for the determination of the energy charge, i.e., the cellular energy status, as an overall quality measure for the sample workup and analytical protocols. PMID:16970336

  10. The analysis of forensic samples using laser micro-pyrolysis gas chromatography mass spectrometry.

    PubMed

    Armitage, S; Saywell, S; Roux, C; Lennard, C; Greenwood, P

    2001-09-01

    Laser micropyrolysis gas chromatography-mass spectrometry is used for the analysis of paint, photocopier toner, and synthetic fiber materials to test the forensic potential of this emerging technology. It uses a laser microprobe to selectively target very small parts of the materials for GC-MS analysis. Whereas the paint and the toner samples were amenable to direct laser pyrolysis, the synthetic fibers proved transparent to the 1064 nm laser radiation. The difficulty with the fibers demonstrates that a specific laser wavelength may not be appropriate for all types of materials. Nevertheless, the fibers were able to be indirectly pyrolyzed by impregnation in a strongly absorbing graphite matrix. A vast array of hydrocarbon pyrolysates was detected from the different materials studied. Unique product distributions were detected from each sample and in sufficient detail to facilitate individual molecular characterization (i.e., molecular fingerprinting). The integrity of the laser data were confirmed by comparison to data obtained from the same samples by the more conventional pyroprobe pyrolysis GC-MS method. The high spatial resolution and selectivity of the laser method may be advantageous for specific forensic applications, however, further work may be required to improve the reproducibility of the data. PMID:11569542

  11. Nano-liquid chromatography analysis of dansylated biogenic amines in wines.

    PubMed

    Hernández-Borges, Javier; D'Orazio, Giovanni; Aturki, Zeineb; Fanali, Salvatore

    2007-04-20

    In this work, the simultaneous analysis of 10 biogenic amines (ethanolamine, methylamine, tryptamine, 2-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine) in wines by nano-liquid chromatography (nano-LC) using UV detection and a capillary bidentate C(18) column of 100 microm I.D. is proposed. The 10 selected amines, which are the most important to be determined in wine samples, were derivatized with dansyl-chloride (Dns-Cl) previous to their nano-LC determination. Excess of the derivatizing agent as well as other components of the samples were eliminated by the use of an on-line cleaning step employing a C(18) trapping column which also provided a pre-concentration effect. The mobile phase composed of acetonitrile, water, acetic acid and triethylamine (TEA) mixture was pumped at a low flow rate (634 nL/min). Limits of detection (LODs) achieved ranged between 18.3 and 48.3 ng/mL; while calibration curves showed good linearity (R(2)>0.9924). The method was applied to the analysis of this group of amines in white and red wine samples after suitable treatment with polyvinylpyrrolidone (PVP) and extraction with C(18) cartridges. PMID:17353021

  12. 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 ?g mL(-1). This GPC analytical method can be applied for exclusively distinguish between PET fibers using 1 ?g of fiber. This method can be extended to forensic comparison of other synthetic fibers such as polyamides and acrylics. PMID:24725864

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

    PubMed

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

    2014-11-01

    Chiral comprehensive two-dimensional gas chromatography (eGC×GC) coupled to quadrupole-accurate mass time-of-flight mass spectrometry (QTOFMS) was evaluated for its capability to report the chiral composition of several monoterpenes, namely, ?-pinene, ?-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 ?-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 ?-pinene, ?-pinene, and limonene were determined to be 1.325, 2.703, and 1.040, respectively, in the cardamom oil sample based on relative peak area data. PMID:24420979

  14. Analysis of 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 ?g/L; limits of quantitation (LOQs) varied between 0.15 and 0.75 ?g/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

  15. 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.

  16. Analysis of sterols by high-performance liquid chromatography/mass spectrometry combined with chemometrics.

    PubMed

    Nagy, Kornél; Jakab, Annamaria; Pollreisz, Ferenc; Bongiorno, David; Ceraulo, Leopoldo; Averna, Maurizio R; Noto, Davide; Vékey, Károly

    2006-01-01

    A newly developed high-performance liquid chromatography/mass spectrometry (HPLC/MS) method has been successfully used to analyze plasma concentrations of various phytosterols (cholestanol and beta-sitosterol) and cholesterol metabolites (desmosterol and lathosterol). This was based on an unusual solvent combination of water/methanol vs. methanol/acetone/n-hexane applied on a Purospher Star RP-18e (125 x 2 mm, 3 microm) column, which proved excellent for the separation, identification and quantification of plasma sterols. Simple solid-phase extraction preparation of plasma samples was performed, followed by the developed fast and robust HPLC separation. Results on four groups of people were compared, those with low, normal and high plasma cholesterol levels and those with high cholesterol levels on statin therapy, and the results were evaluated using linear discriminant analysis (LDA). Variable selection for LDA was achieved using backward removal selection. Highly discriminatory variables were the ratios of desmosterol to sitosterol and of lathosterol to total plasma cholesterol. The latter ratio was also excellent for distinguishing subjects on statin therapy. The success rate of classification was 100%. The present pilot study shows the potential of HPLC/MS analysis and chemometrics for studying cholesterol-related disorders and warrants future full-scale medical study. PMID:16841361

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

    PubMed

    Križman, Mitja; Pušar, Alenka

    2015-07-31

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

  18. 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

  19. 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.

  20. 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.

  1. 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

  2. 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 ?m 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 ?g/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

  3. 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. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26112364

  4. Temperature-programmed retention indices for gas chromatography-mass spectroscopy analysis of plant essential oils.

    PubMed

    Zhao, Chen-Xi; Liang, Yi-Zeng; Fang, Hong-Zhuang; Li, Xiao-Ning

    2005-11-25

    A total of 95 volatile compounds from the essential oil in buds of Syringa oblata Lindl (lilac) were identified by gas chromatography-mass spectrometry (GC-MS) combined with heuristic evolving latent projections (HELP) and moving subwindow searching (MSS). The identified compounds are mainly aliphatic, terpenes and aromatic compounds. Their temperature-programmed retention indices (PTRIs) on HP-5MS and DB-35MS at three heating rates of 2, 4 and 6 degrees C/min from 80 to 290 degrees C were obtained, which showed that aliphatic compounds give nearly constant PTRIs and PTRIs of terpenoids do not vary much at different heating rates. But PTRIs of aromatic compounds exhibit relatively large temperature dependence. PTRIs vary much more on DB-35MS than those on HP-5MS according to the compound types. In general, differences of PTRIs between the two columns increase from aliphatic compounds to terpenoids to polycyclic aromatic compounds. The PTRIs in different heating rates were used as cross-references in the identification of components in the essential oil. When they were used in analysis of essential oil from flowers of lilac, good results were obtained. These PTRIs would be a part of our PTRI database being constructed on components from plant essential oils. The results also showed that efficiency and reliability were improved greatly when chemometric method and PTRIs were used as assistants of GC-MS in identification of chemical components in plant essential oils. PMID:16289121

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

    NASA Astrophysics Data System (ADS)

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

    2013-04-01

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

  6. 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 ?m 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.

  7. 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

    2015-11-01

    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 ?g 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

  8. 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-?m or 2.6–2.8-?m (fused-core) particle size with C18 or C8 sorbent with analysis time <30 min; (3) electrospray ionization in positive- and negative-ion modes with full spectra acquisition using high-resolution MS with capability to MS/MS. Phospholipids (phosphatidylcholines, phosphatidylethanolamines, phosphatidylinositols, phosphatidylserines, phosphatidylglycerols) followed by sphingomyelins, di- and tri-acylglycerols, and ceramides were the most frequently targeted lipid species. PMID:25309011

  9. Analysis of phytosterols in extra-virgin olive oil by nano-liquid chromatography.

    PubMed

    Rocco, Anna; Fanali, Salvatore

    2009-10-23

    In this work the applicability of nano-liquid chromatography (nano-LC) was evaluated for the determination of phytosterols in extra-virgin olive oil samples. These compounds represent a minor part of lipids in vegetable oils, but their quantification can be useful to establish oil origin and to reveal intentional adulterations. The analysis of five main sterols, specifically brassicasterol, stigmasterol, campesterol, cholesterol and beta-sitosterol, was performed in a laboratory-assembled nano-LC system coupled with a UV detector. The separation of all compounds was obtained in about 20 min, employing a capillary column packed with a C18-RP (sub-2 microm particles) stationary phase for 15 cm. Methanol only was used as mobile phase. The simple method developed and optimized was validated in terms of repeatability, linearity, limit of detection and limit of quantification (0.78 and 1.56 microg/mL, respectively) achieving good results. After this, it was applied to the determination of phytosterols in extra-virgin olive oil samples. Isolation of phytosterols was obtained by solid-phase extraction, after saponification and liquid-liquid extraction of the unsaponified fraction with diethyl ether. Recovery tests were performed and values between 90% and 103%, with RSDs within 5%, were obtained. Moreover the nano-LC system was coupled with a mass spectrometer for an accurate identification of phytosterols. PMID:19386314

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

    SciTech Connect

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

    1988-08-01

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

  11. [Analysis of six acidic components in hops extracts by high performance liquid chromatography].

    PubMed

    Cai, Xiaoming; Xia, Lu; Sun, Yuanshe; Li, Tong; Xia, Mingzhu

    2011-10-01

    A method of high performance liquid chromatography (HPLC) was developed for the separation and determination of six acidic components (cohumulone, humulone, adhumulone, colupulone, lupulone and adlupulone) in hops extracts. The effects of several important factors, such as the addition of acid, the organic solvent of elution solution and the column temperature, were investigated to acquire the optimum conditions. The separation was carried out on a Hypersil ODS2 column (250 mm x 4. 6 mm, 5 microm). A mixture of acetonitrile-0. 1% (v/v) phosphoric acid solution (pH 2. 2) (65: 35, v/v) was used as the mobile phase at a flow rate of 1. 0 mL/min in isocratic elution mode. The column temperature was kept at room temperature, and the detection wavelength was set at 315 nm. The six acidic components reached baseline separation, and were identified by ultraviolet spectroscopy, infrared spectroscopy and mass spectrometry. The results show that this method is suitable for the analysis of acidic components in hops extracts owing to the stable and simple performance. PMID:22268354

  12. 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

  13. 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.

  14. Liquid chromatography-mass spectrometry analysis of diethylcarbamazine in human plasma for clinical pharmacokinetic studies.

    PubMed

    Schmidt, Mark S; King, Christopher L; Thomsen, Edward K; Siba, Peter M; Sanuku, Nelly; Fleckenstein, Lawrence

    2014-09-01

    A sensitive and selective liquid chromatographic method using mass spectrometric detection was developed for the determination of diethylcarbamazine (DEC) in human plasma. DEC and its stable isotope internal standard d3-DEC were extracted from 0.25mL of human plasma using solid phase extraction. Chromatography was performed using a Phenomenex Synergi 4? Fusion-RP column (2mm×250mm) with gradient elution. The retention time was approximately 4.8min. The assay was linear from 4 to 2200ng/mL. Analysis of quality control samples at 12, 300, and 1700ng/mL (N=15) had interday coefficients of variation of 8.4%, 5.4%, and 6.2%, respectively (N=15). Interday bias results were -2.2%, 6.0%, and 0.8%, respectively. Recovery of DEC from plasma ranged from 84.2% to 90.1%. The method was successfully applied to clinical samples from patients with lymphatic filariasis from a drug-drug interaction study between DEC and albendazole and/or ivermectin. PMID:24975211

  15. Selective and quantitative analysis of 4-hydroxybenzoate preservatives by microemulsion electrokinetic chromatography.

    PubMed

    Mahuzier, P E; Altria, K D; Clark, B J

    2001-07-27

    A microemulsion electrokinetic chromatography (MEEKC) method has been developed and validated for the determination of 4-hydroxybenzoates and their impurities. These materials are commonly known as parabens and are widely used as preservatives in foods, cosmetics and pharmaceuticals. The method was shown to be selective and quantitative for the methyl, ethyl, propyl and butyl esters of 4-hydroxybenzoic acid. An internal standard, 4-hydroxyacetophenone, was employed to improve injection precision and detector linearity. In addition, 4-hydroxybenzoic acid, the major degradent, could also be monitored at the 0.1% (m/m) level. The method was successfully validated for assay and detection of the impurities in 4-hydroxybenzoic acid methyl ester and 4-hydroxybenzoic acid propyl ester samples and for the determination of 4-hydroxybenzoic acid methyl ester in a liquid pharmaceutical formulation. The determination of paraben content by MEEKC in a liquid sample was consistent with HPLC analysis. This work is the first reported validated MEEKC method and shows that the methodology can be successfully implemented into routine quality control testing. PMID:11521898

  16. Analysis of alkylphenol ethoxylate metabolites in the aquatic environment using liquid chromatography-electrospray mass spectrometry.

    PubMed

    Ferguson, P L; Iden, C R; Brownawell, B J

    2000-09-15

    A quantitative method is described for the analysis of the metabolites of alkylphenol ethoxylate (APEO) surfactants in estuarine water and sediment samples using reversed-phase high-performance liquid chromatography with electrospray mass spectrometry detection. Nonyl- and octylphenols, nonyl- and octylphenol mono-, di-, and triethoxylates, halogenated nonylphenols, and nonylphenol ethoxycarboxylates were concentrated from water samples using a C18 solid-phase extraction procedure. A novel, continuous-flow, high-temperature, sonicated extraction system was developed to isolate APEO metabolites from sediment samples. Quantitative LC-MS was performed in the negative ion mode for nonylphenols, octylphenols, and halogenated nonylphenols and in the positive ion mode for nonyl- and octylphenol ethoxylates using selected ion monitoring with isotopically labeled surrogate standards. Recoveries for sediment and water analyses ranged between 78 and 94%, and detection limits for APEO metabolites were between 1 and 20 pg injected on column. This is a significant improvement over previously reported methods. Suppression of analyte response was encountered in the presence of matrix components in sediment samples, but this effect was eliminated by careful selection of surrogate and internal standards. Individual APEO metabolite concentrations of 1-320 ng/L and 5-2000 ng/g are reported for water and sediment samples, respectively, from Jamaica Bay, NY. PMID:11008767

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

    PubMed Central

    2015-01-01

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

  18. 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.

  19. 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...

  20. 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...

  1. 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 ...

  2. 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.

  3. Analysis of in vitro oxidized human LDL phospholipids by solid-phase extraction and micellar electrokinetic capillary chromatography.

    PubMed

    Yang, Ying-Ling; Chong, Chin-Pong; Tsai, Ming-Hua; Liu, Mine-Yine

    2012-04-01

    Phospholipids of in vitro oxidized human low-density lipoproteins (LDL) were separated by two different solid-phase extraction (SPE) methods. One of the two methods was designed to test the effects of gradient elution. This SPE method isolated more phospholipids from in vitro oxidized LDL than the other one according to the results of liquid chromatography and electrospray ionization mass spectrometry (LC ESI-MS) analysis. A micellar electrokinetic capillary chromatography (MEKC) method was also used to analyze phospholipids separated by SPE. The results of MEKC and LC ESI-MS were consistent for the major phospholipid classes, including PC, lysoPC, PE, PI and PS. The MEKC profiles showed significant differences for native and oxidized LDL phospholipids. Therefore, the unique combination of SPE and MEKC methods showed dramatic distinctions between native and in vitro oxidized human LDL phospholipids. The combination also shows great potential for rapid analysis of in vivo oxidized human LDL phospholipids in the future. PMID:22392513

  4. Analysis of phospholipids in bio-oils and fats by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    PubMed

    Viidanoja, Jyrki

    2015-09-15

    A new, sensitive and selective liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) method was developed for the analysis of Phospholipids (PLs) in bio-oils and fats. This analysis employs hydrophilic interaction liquid chromatography-scheduled multiple reaction monitoring (HILIC-sMRM) with a ZIC-cHILIC column. Eight PL class selective internal standards (homologs) were used for the semi-quantification of 14 PL classes for the first time. More than 400 scheduled MRMs were used for the measurement of PLs with a run time of 34min. The method's performance was evaluated for vegetable oil, animal fat and algae oil. The averaged within-run precision and between-run precision were ?10% for all of the PL classes that had a direct homologue as an internal standard. The method accuracy was generally within 80-120% for the tested PL analytes in all three sample matrices. PMID:26279006

  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. Analysis of the essential oil from radix bupleuri using capillary gas chromatography.

    PubMed

    Li, Xiuqin; Jia, Ying; Song, Aihua; Chen, Xiaohui; Bi, Kaishun

    2005-10-01

    A simple and rapid capillary gas chromatographic (CGC) method with flame ionization detection has been newly developed for analysis of the essential oil from Radix Bupleuri. Twenty components were identified with gas chromatography-mass spectrometry. E-2-heptenal, furan, 2-pentyl, and E-2-nonenal were quantified simultaneously using the internal standard method. Decane was used as an internal standard. Separation and quantification were achieved on a DB-5 capillary column (30 m x 0.25 mm i. d., 0.25-microm film thickness). The oven temperature was programmed as follows: 60 degrees C to 70 degrees C at 1 degree C/min rate, 70 degrees C for 10 min, 3 degrees C/min to 120 degrees C, 20 degrees C/min to 250 degrees C, and held at 250 degrees C for 5 min. The oven pressure was programmed as follows: 46.1 kPa for 25 min, 20.0 kPa/min to 77.6 kPa, and then held for 22 min. Split injection was conducted with a split ratio of 10:1; flow-rate, 1.00 ml/min; carrier gas, nitrogen; injector temperature, 280 degrees C; and detector temperature, 280 degrees C. The system proved effective in resolving E-2-heptenal, furan, 2-pentyl, and E-2-nonenal peaks from their interfering components. The method displayed excellent linearity in the range of 26.8-1072 microg/ml (E-2-heptenal), 6.5-1292 microg/ml (furan, 2-pentyl), and 7.8-1564 microg/ml (E-2-nonenal). The average recovery rates of E-2-heptenal, furan, 2-pentyl, and E-2-nonenal were 100.3%, 102.8%, and 97%, respectively. CGC is a quick and accurate method for analysis of the essential oil from Radix Bupleuri. PMID:16205039

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

    PubMed

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

    2015-12-01

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

  8. Contributions to the Theory of Gas --> Liquid Condensation.

    NASA Astrophysics Data System (ADS)

    Mohanty, Udayan

    The cluster expansion of the classical and the quantum canonical partition function is shown to be related to the Bell polynomials. This observation enables one to derive a recursion relation for the partition function. The recursion relation renders the numerical evaluation of thermodynamic quantities tractable. The mathematical structure of the partition function for volume independent cluster integrals (b(,l)(T)) is shown to be connected to the Umbral algebra recently developed by Rota. This algebra is used to rederive Mayer's "first theorem". For temperatures below the critical temperature, it is shown that Lennard Jones and square well fluid do not condense in the chain approximation on b(,l)(T). They are capable of displaying a gas (--->) liquid transition, however, when higher order corrections to the connected cluster integrals, like chain branching, are taken into account. The key result is the appearance of a bi-modal cluster size distribution signalling the explosive growth of microscopic molecular clusters to produce clusters of macroscopic size. A horizontal scaling of the liquid peak, as contrasted with the vertical scaling of the gas peak, clearly shows that the liquid clusters are macroscopic in macroscopic systems. A hypothesis is put forward that formation of a macroscopic array of connected rings would be signalled by the appearance of a second peak in an ensemble of average star size distribution. A physical cluster theory of vapor condensation is developed which removes the unphysical nature of the Mayer's cluster. The Week-Chandler-Andersen potential separation idea in the perturbation theory of liquids is exploited to redefine the physical clusters while retaining the exact form of Mayer's equations. The mathematical and physical cluster size distributions are calculated and compared at various temperatures and densities in the tree approximation. The crucial roles played by Mayer's monomers and dimers are pointed out. Tentative calculations reveal that the formalism developed is simple, computationally tractable and suited for an equilibrium theory of liquids. The relationship between the condensation point in the sense of Mayer and the percolation point (for fluids) which is the point where an infinite physical cluster begins to appear in the system is investigated in the ring approximation on b(,l)(T,V). The exact volume dependent b(,l)(T,V) of an ideal Bose gas is calculated under Neumann and Dirichlet boundary conditions. This set of b(,l)(T,V) is used with the above formalism to study Bose-Einstein condensation in finite systems in the canonical ensemble. A new criteria for Bose-Einstein condensation in finite systems of IBG is proposed and investigated. In the presence of an external field, the ideal Bose gas shows a bimodality in the mean cluster size distribution in the canonical ensemble. This explicit demonstration of a bimodal cluster size distribution in quantum systems is the theoretical counterpart (for finite systems) of the oft assumed phase transition and concomitant separation of particles in coordinate space.

  9. Neuere Chromatographie

    NASA Astrophysics Data System (ADS)

    Hostettmann, K.

    1983-04-01

    Besides high-performance liquid chromatography (HPLC) which is now a well-established and currently used technique, several emerging methods for the isolation and separation of natural products are receiving considerable attention. Centrifugal thin-layer chromatography is a very rapid technique, but limited in resolution. Of special interest are the recently developed support-free liquid-liquid chromatography methods such as droplet counter-current chromatography (DCCC) and rotation locular counter-current chromatography (RLCC). This latter method was applied to the separation of the enantiomers of (±)-norephedrine.

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

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.

    1989-01-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan-Cassini entry probe, which is being jointly planned by NASA and the European Space Agency (ESA), might be launched as early as 1994. As in the Pioneer mission, limited time--perhaps only 3-4 h--will be available for the completion of all analyses while the probe descends through the atmosphere. A conventional GC or GC-MS system would be able to analyze no more than two aerosol and two gas samples during the probe's descent. Conventional GC also is limited by the sensitivity of the detector and by the sample volume. For the Titan mission, the sensitivity problems will be worse because the atmospheric pressure at the time of instrument deployment is expected to be < 3 torr. Consequently, the sample volume might not be large enough to satisfy the detector sensitivity requirements. Because of such limitations, alternative GC analysis techniques have been investigated for future NASA missions. Multiplex gas chromatography has been investigated as a possible candidate for chemical analysis within a spacecraft or other restricted environment, and chemical modulators have been developed and used when needed with this technique to reduce the size and weight of the instrumentation. Also, several new multiplex techniques have been developed for use in specific applications.

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

    PubMed

    Valentin, J R

    1989-03-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan-Cassini entry probe, which is being jointly planned by NASA and the European Space Agency (ESA), might be launched as early as 1994. As in the Pioneer mission, limited time--perhaps only 3-4 h--will be available for the completion of all analyses while the probe descends through the atmosphere. A conventional GC or GC-MS system would be able to analyze no more than two aerosol and two gas samples during the probe's descent. Conventional GC also is limited by the sensitivity of the detector and by the sample volume. For the Titan mission, the sensitivity problems will be worse because the atmospheric pressure at the time of instrument deployment is expected to be < 3 torr. Consequently, the sample volume might not be large enough to satisfy the detector sensitivity requirements. Because of such limitations, alternative GC analysis techniques have been investigated for future NASA missions. Multiplex gas chromatography has been investigated as a possible candidate for chemical analysis within a spacecraft or other restricted environment, and chemical modulators have been developed and used when needed with this technique to reduce the size and weight of the instrumentation. Also, several new multiplex techniques have been developed for use in specific applications. PMID:11539794

  12. 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…

  13. Accurate measurements of frontal analysis for the determination of adsorption isotherms in supercritical fluid chromatography.

    PubMed

    Kamarei, Fahimeh; Gritti, Fabrice; Guiochon, Georges; Burchell, John

    2014-02-14

    The implementation of the traditional FA method is difficult with classical supercritical fluid chromatography (SFC) instruments. The instrument mixer and other sources of extra-column volumes are large and significantly broaden the fronts of injected plugs, which diminishes the precision and accuracy of the FA method. An SFC instrument was modified to permit more accurate determinations of adsorption isotherm data. The sample, the modifier, and CO2 are separately pumped via small volume connection tubes into a small volume mixer (250?L), where they are mixed into a homogeneous fluid fed to the column. The extra-column volumes and the column hold-up volume were accurately measured at each back pressure from the retention times of tracers. This modified instrument was used to measure the adsorption isotherm of S-naproxen by frontal analysis (FA) on a (R, R)-Whelk-O1 column, using a mixture of methanol (20%, v/v) and CO2 as the mobile phase. Its performance is studied at several different back pressures from 100 to 210bar. In all the experiments, the total flow rate was kept to a low value (1mL/min) in order to minimize the variation of the equilibrium constant along the column. Although a suitable breakthrough curve could not be obtained at low back pressures (<150bar) due to the closeness to the critical point pressure of the methanol/CO2 mixture, excellent results were obtained at higher back pressures (>150bar), conditions remote from the critical point and breakthrough curves with very sharp front shocks are obtained. The RSDs of the profiles recorded at each back pressures are excellent, better than 1%. PMID:24456708

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

    USGS Publications Warehouse

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

    2002-01-01

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

  15. [Analysis of the reaction solution for dehydroacetic acid by ethyl acetoacetate using high formance liquid chromatography].

    PubMed

    Chen, Qiuyun; Duan, Zhengkang; Li, Haitao; Yan, Zhixiang; Peng, Ye; Zeng, Hangri

    2013-05-01

    A way of ethyl acetoacetate by the Claisen condensation reaction is one of the main methods of the industrial production of dehydroacetic acid. There are the problems of the differences in absorbance value and the maximum absorption wavelength, and the chromatographic peak is prone to the phenomena such as bifurcation and tailing when using liquid chromatography to the analysis of ethyl acetoacetate. To avoid the interference of the enol of ethyl acetoacetate, and making the peak shape of ethyl acetoacetate better and quantitatively more accurate, we converted the enol to ketone through optimizing the chromatographic conditions. As a result, qualitative and quantitative analyses of ethyl acetoacetate were replaced by those of the ethyl acetoacetate ketone. A method was developed for the simultaneous determination of dehydroacetic acid and ethyl acetoacetate by HPLC in the reaction mixture for producing dehydroacetic acid. An Agilent HC-C18 column (250 mm x 4.6 mm, 5 microm) was used for the separation. The ultraviolet wavelength was 290 nm and the column temperature was 35 degrees C, and methanol-0.3% ammonium acetate buffer (5: 95, v/v) with pH 6.0 adjusted by acetic acid as mobile phase, and the flow rate was 0.6 mL/min. The correlation coefficients of dehydroacetic acid and ethyl acetoacetate were 0.99995 and 0.99992, and the spiked recoveries were 98.5% and 101.3%, respectively; and the relative standard deviations were less than 1.0%. This meth- od has the advantages of good accuracy and high sensitivity, and it can analyse both qualitatively and quantitatively dehydroacetic acid and ethyl acetoacetate rapidly and simply. And it can provide the reference for producing dehydroacetic acid by the way of ethyl acetoacetate. PMID:24010347

  16. 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

  17. Modified micellar electrokinetic chromatography in the analysis of catechins and xanthines in chocolate.

    PubMed

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

    2004-10-01

    Modified micellar electrokinetic chromatography (MEKC) analysis of monomeric flavanols (catechin and epicatechin) and methylxanthines (caffeine and theobromine) in chocolate and cocoa was performed by using sodium dodecyl sulfate (SDS) as a principal component of the running buffer. Because of the reported poor stability of catechins in alkaline solutions, acidic conditions (pH 2.5) were chosen and consequently the electroosmotic flow (EOF) was significantly suppressed; this resulted in a fast anodic migration of the analytes partitioned into the SDS micelles. Under these conditions, variations of either pH value in acidic range or SDS concentration, showed to be not suitable to modulate the selectivity. To overcome this limit, use of additives to the SDS-based running buffer was successfully applied and three different systems were optimized for the separation of (+)-catechin, (-)-epicatechin, caffeine, and theobromine in chocolate and cocoa powder samples. In particular, two mixed micelle systems were applied; the first consisted of a mixture of SDS and 3-[(3-cholamidopropyl)dimethylammonio]-1-propansulfonate (CHAPS) with a composition of 90 mM and 10 mM, respectively; the second was SDS and taurodeoxycholic acid sodium salt (TDC) with a composition of 70 mM and 30 mM, respectively. A further MEKC approach was developed by addition of 10 mM hydroxypropyl-beta-cyclodextrin (HP-beta-CD) to the SDS solution (90 mM); it provided a useful cyclodextrin(CD)-modified MEKC. By applying the optimized conditions, different separation profiles of the flavanols and methylxanthines were obtained showing interesting potential of these combined systems; their integrated application showed to be useful for the identification of the low level of (+)-catechin in certain real samples. The CD-MEKC approach was validated and applied to the determination of catechins and methylxanthines in aqueous extracts from four different commercial chocolate types (black and milk) and two cocoa powders. PMID:15472952

  18. 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

  19. 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; Po?e?, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; ?obi?ski, 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.

  20. Simultaneous analysis of synthetic musks and triclosan in human breast milk by gas chromatography tandem mass spectrometry.

    PubMed

    Wang, Hao; Zhang, Jing; Gao, Fudie; Yang, Yi; Duan, Hejun; Wu, Yongning; Berset, Jean-Daniel; Shao, Bing

    2011-07-01

    A comprehensive method was developed for the simultaneous analysis in human breast milk of 12 synthetic musks, five nitro musks, six polycyclic muks and one macrocyclic musk; as well as one musk metabolite and triclosan. The target analytes were freeze dried and extracted using the accelerated solvent extraction (ASE) procedure. The extracts were further purified by gel permeation chromatography (GPC) and florisil solid-phase extraction (SPE) and then analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS). Recoveries of the analytes based on the isotopic internal standard correction ranged from 82.4% to 112%, with relative standard derivations less than 20%. The method quantification limits (MQLs) were 0.6-5.4 ng/g lipid. The analytes were detected in human breast milk samples and ranged from 11.7 to 308.6 ng/g lipid. PMID:21621487

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

    SciTech Connect

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

    2009-11-15

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

  2. [Analysis of composition and structure of sulfur compounds in residual oils by pyrolysis-gas chromatography].

    PubMed

    Yan, Xiaolin; Shi, Quan; Xu, Chunming; Zhao, Suoqi; Ke, Ming

    2004-03-01

    Flash pyrolysis-gas chromatography has been used to investigate macromolecular sulphur in heavy oil. The influences of pyrolysis time and pyrolysis temperature have been studied and the analytical methods of pyrolysis were set up. Sulfur-containing products were identified by comparing with reference data and semi-quantified by a pulsed flame photometric detector (PFPD). The investigation conducted on Dagang, Gudao, Qianguo, Russia and mixed Russia-Daqing residual oils using pyrolysis-gas chromatography showed that the contents and composition of sulphur compounds demonstrated various characters in different pyrolysates of residual oils. PMID:15712878

  3. Advancement and application of gas chromatography isotope ratio mass spectrometry techniques for atmospheric trace gas analysis

    NASA Astrophysics Data System (ADS)

    Giebel, Brian M.

    2011-12-01

    The use of gas chromatography isotope ratio mass spectrometry (GC-IRMS) for compound specific stable isotope analysis is an underutilized technique because of the complexity of the instrumentation and high analytical costs. However stable isotopic data, when coupled with concentration measurements, can provide additional information on a compounds production, transformation, loss, and cycling within the biosphere and atmosphere. A GC-IRMS system was developed to accurately and precisely measure delta13C values for numerous oxygenated volatile organic compounds having natural and anthropogenic sources. The OVOCs include methanol, ethanol, acetone, methyl ethyl ketone, 2-pentanone, and 3-pentanone. Guided by the requirements for analysis of trace components in air, the GC-IRMS system was developed with the goals of increasing sensitivity, reducing dead-volume and peak band broadening, optimizing combustion and water removal, and decreasing the split ratio to the IRMS. The technique relied on a two-stage preconcentration system, a low-volume capillary reactor and water trap, and a balanced reference gas delivery system. Measurements were performed on samples collected from two distinct sources (i.e. biogenic and vehicle emissions) and ambient air collected from downtown Miami and Everglades National Park. However, the instrumentation and the method have the capability to analyze a variety of source and ambient samples. The measured isotopic signatures that were obtained from source and ambient samples provide a new isotopic constraint for atmospheric chemists and can serve as a new way to evaluate their models and budgets for many OVOCs. In almost all cases, OVOCs emitted from fuel combustion were enriched in 13C when compared to the natural emissions of plants. This was particularly true for ethanol gas emitted in vehicle exhaust, which was observed to have a uniquely enriched isotopic signature that was attributed to ethanol's corn origin and use as an alternative fuel or fuel additive. Results from this effort show that ethanol's unique isotopic signature can be incorporated into air chemistry models for fingerprinting and source apportionment purposes and can be used as a stable isotopic tracer for biofuel inputs to the atmosphere on local to regional scales.

  4. 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...

  5. 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...

  6. (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...

  7. 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)

  8. 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…

  9. 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…

  10. The study of flow characteristic of gas-liquid two-phase flow based on the near-infrared detection device

    NASA Astrophysics Data System (ADS)

    Fang, Lide; Liang, Yujiao; Zhang, Yao; Zhang, Chen; Gao, Jingzhe

    2014-04-01

    With the importance of the two-phase flow, many scholars pay attention on it; and for the so many parameters in the gas-liquid two-phase flow, flow characteristic is the basis. For the four flow patterns in the vertical direction, slug flow, bubbly flow, annular flow, and milk foam-like flow, the paper used the laser diode of 980nm and the silicon photodiode to detect the flow status. The absorption coefficients of the infrared in the gas and the liquid are very different; at the meantime, the infrared is affected by the interface obviously. As a result, it can reflect the fluctuation of the gas-liquid two-phase flow with the detection by the infrared. By analyzing the experiment data, four characteristic parameters are extracted, such as the average value, the variance, the kurtosis, and the frequency center of gravity. They can not only reflect the change of the different flow patterns, but also can reflect the fluctuation in the same flow pattern. The feature vector constituted of the four characteristic parameters can identify the flow pattern correctly in this system. What's more, it can achieve an accurate measurement of the real-time online, providing a basis for the other parameters' analysis in the gas-liquid two-phase flow.

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

    PubMed

    Shaaban, Heba; Górecki, Tadeusz

    2015-01-01

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

  12. Analysis of chemical profiles of insect adhesion secretions by gas chromatography-mass spectrometry.

    PubMed

    Reitz, Manuela; Gerhardt, Heike; Schmitt, Christian; Betz, Oliver; Albert, Klaus; Lämmerhofer, Michael

    2015-01-01

    This article reports on the chemical analysis of molecular profiles of tarsal secretions of the desert locust Schistocerca gregaria (Forsskål, 1775) by gas chromatography hyphenated with quadrupol mass spectrometry (GC-MS) as well as (1)H-nuclear magnetic resonance ((1)H NMR) spectroscopy. Special focus of this study was to elaborate on sampling methods which enable selective microscale extraction of insect secretions in a spatially controlled manner, in particular tarsal adhesive secretions and secretions located on cuticle surfaces at the tibia. Various solvent sampling procedures and contact solid-phase microextraction (SPME) methods were compared in terms of comprehensiveness and extraction efficiencies as measured by signal intensities in GC-MS. Solvent sampling with water as extraction solvent gave access to the elucidation of chemical profiles of polar compound classes such as amino acids and carbohydrates, but is extremely tedious. Contact SPME on the other hand can be regarded as a simplified and more elegant alternative, in particular for the lipophilic compound fraction. Many proteinogenic amino acids and ornithine as well as carbohydrate monomers arabinose, xylose, glucose, and galactose were detected in tarsal secretions after acid hydrolysis of aqueous extracts. Qualitatively similar but quantitatively significantly different molecular profiles were found for the lipid fraction which contained mainly n-alkanes and internally branched monomethyl-, dimethyl-, and trimethyl-alkanes in the C23-C49 range as well as long chain fatty acids and aldehydes. Especially, hydrocarbons with >C40 carbon numbers have previously been rarely reported for insect secretions. The results suggest that the investigated insect secretions are complex emulsions which allow the attachment of tarsi on various otherwise incompatible materials of smooth and rough surfaces. The solid consistence of the established alkanes at ambient temperatures might contribute to a semi-solid consistence of the adhesive, amalgamating partly opposing functions such as slip resistance, tarsal release, desiccation resistance, and mechanical compliance. The methods developed can be extended to other similar applications of studying compositions of insect secretions of other species. PMID:25479867

  13. Benchmarking of candidate detectors for multiresidue analysis of pesticides by comprehensive two-dimensional gas chromatography.

    PubMed

    Engel, Erwan; Ratel, Jérémy; Blinet, Patrick; Chin, Sung-Tong; Rose, Gavin; Marriott, Philip J

    2013-10-11

    The present study discusses the relevance, performance and complementarities of flame photometric detector in phosphorus (FPD/P) and sulfur (FPD/S) modes, micro electron capture detector (?ECD), nitrogen phosphorus detector (NPD), flame ionization detector (FID) and time-of-flight mass spectrometer (TOF/MS) for the comprehensive two-dimensional gas chromatography (GC×GC) analysis of pesticides. A mix of 41 pesticides including organophosphorus pesticides, synthetic pyrethroids and fungicides was investigated in order to benchmark GC×GC systems in terms of linearity (R(2)), limits of detection (LOD), and peak shape measures (widths and asymmetries). A mixture of pesticides which contained the heteroatoms phosphorus, sulfur, nitrogen and one or several halogens, was used to acquire a comparative data set to monitor relative detector performances. GC×GC datasets were systematically compared to their GC counterpart acquired with an optimized one-dimensional GC configuration. Compared with FID, considered the most appropriate detector in terms of suitability for GC×GC, the element-selective detector FPD/P and ?ECD best met the peak widths (0.13-0.27s for FPD/P; 0.22-0.26s for ?ECD) and tailing factors (0.99-1.66 for FPD/P; 1.32-1.52 for ?ECD); NPD exhibited similar peak widths (0.23-0.30s), but exceeded those of the above detectors for tailing factors (1.97-2.13). These three detectors had improved detection limits of 3-7 times and 4-20 times lower LODs in GC×GC mode compared with FID and TOF-MS, respectively. In contrast FPD/S had poor peak shape (tailing factor 3.36-5.12) and much lower sensitivity (10-20 fold lower compared to FPD/P). In general, element-selective detectors with favorable detection metrics can be considered viable alternatives for pesticide determination using GC×GC in complex matrices. The controversial issue of sensitivity enhancement in GC×GC was considered for optimized GC and GC×GC operation. For all detectors, we found no significant LOD enhancement in GC×GC. PMID:24011509

  14. High speed, high resolution, and continuous chemical analysis of ice cores using a melter and ion chromatography.

    PubMed

    Cole-Dai, Jihong; Budner, Drew M; Ferris, Dave G

    2006-11-01

    Measurement of trace chemical impurities in ice cores contributes to the reconstruction of records of the atmospheric environment and of the climate system. Ion chromatography (IC) is an effective analytical technique for ionic species in ice cores but has been used on discretely prepared ice samples, resulting in extensive and slow sample preparation and potential for contamination. A new technique has been developed that utilizes IC as the online detection technique in a melter-based continuous flow system for quantitative determination of major ionic chemical impurities. The system, called CFA-IC for continuous flow analysis with ion chromatography detection, consists of an ice core melter, several ion chromatographs, and an interface that distributes meltwater to the IC instruments. The CFA-IC technique combines the accuracy, precision, and ease of use of IC measurement with the enhanced speed and depth resolution of continuous melting systems and is capable of virtually continuous, high-speed and high-resolution chemical analysis of long ice cores. The new technique and operating procedures have been tested and validated with the analysis of over 100 m of ice cores from Antarctica. The current CFA-IC system provides an all-major-ion analysis speed of up to 8 m a day at a depth resolution of approximately 2 cm. PMID:17144308

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

    PubMed

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

    2013-01-01

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

  16. Gas chromatography in space

    NASA Technical Reports Server (NTRS)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  17. Effect of Pulsing on Reaction Outcome in a Gas-Liquid Catalytic Packed-Bed Reactor

    E-print Network

    McCready, Mark J.

    Effect of Pulsing on Reaction Outcome in a Gas-Liquid Catalytic Packed-Bed Reactor Ruiyun Wu, Mark) first proposed a regime map for their operation. Consistent with other flow regime maps before (Baker. (1995) used a theoretical model to demonstrate qualitative changes in the reaction outcome

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

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...2013-07-01 false Default Factors for Petroleum Products and Natural Gas Liquids 1 2...GREENHOUSE GAS REPORTING Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table...MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1...

  19. 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

    ...2011-07-01 false Default Factors for Petroleum Products and Natural Gas Liquids 1 2...GREENHOUSE GAS REPORTING Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table...MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1...

  20. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...2012-07-01 false Default Factors for Petroleum Products and Natural Gas Liquids 1 2...GREENHOUSE GAS REPORTING Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table...MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1...

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

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...2014-07-01 false Default Factors for Petroleum Products and Natural Gas Liquids 1 2...GREENHOUSE GAS REPORTING Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table...MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1...

  2. Phase diagrams in the lattice restricted primitive model: From order-disorder to gas-liquid phase transition

    E-print Network

    Phase diagrams in the lattice restricted primitive model: From order-disorder to gas-liquid phase is very similar to that of the continuum RPM for high NN strength. Specifically, we have found both gas-liquid phase separation, with associated Ising critical point, and a first-order liquid-solid transition. We

  3. Shotgun Proteomics Analysis of Estrogen Effects in the Uterus Using Two-Dimensional Liquid Chromatography and Tandem Mass Spectrometry.

    PubMed

    Callegari, Eduardo A

    2016-01-01

    Shotgun (gel-free) proteomics is a useful approach to perform identification and relative quantification of protein in complex mixtures such as tissue homogenates, biological fluids, cell lysates, and extracellular proteins. Incorporation of separative and analytical techniques such as two-dimensional liquid chromatography at nanoscale (2D-nanoLC) coupled to tandem mass spectrometry (MS/MS analysis) into the shotgun protocol provides an excellent strategy. This chapter describes the application of the shotgun proteomics protocol to evaluate the identity and expression analysis of proteins from rat uterus after estrogen (ethinylestradiol) treatment. The steps of the protocol involve sample preparation (digestion), 2D-nanoLC-MS/MS analysis, and shotgun proteomics analysis including bioinformatics tools for data conversion, organization, and interpretation. PMID:26585132

  4. Per-O-methylation of neutral carbohydrates directly from aqueous samples for gas chromatography and mass spectrometry analysis.

    PubMed

    Ciucanu, Ionel; Caprita, Rodica

    2007-02-28

    Per-O-methylation of neutral carbohydrates in one step by adding dimethyl sulfoxide, powdered sodium hydroxide, and methyl iodide directly to aqueous sample is described. The influence of the water on the methylation reaction is investigated. Solid powdered sodium hydroxide is very hygroscopic and can scavenge the water from sample if an additional excess of sodium hydroxide is added. The degree of per-O-methylation of carbohydrates is checked by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Gas chromatography-mass spectrometry analysis of mono- and disaccharides from grape juice is presented. PMID:17386650

  5. Thin-layer chromatography and colorimetric analysis of multi-component explosive mixtures

    DOEpatents

    Pagoria, Philip F.; Mitchell, Alexander R.; Whipple, Richard E.; Carman, M. Leslie

    2014-08-26

    A thin-layer chromatography method for detection and identification of common military and peroxide explosives in samples includes the steps of provide a reverse-phase thin-layer chromatography plate; prepare the plate by marking spots on which to deposit the samples by touching the plate with a marker; spot one micro liter of a first standard onto one of the spots, spot one micro liter of a second standard onto another of the spots, and spot samples onto other of spots producing a spotted plate; add eluent to a developing chamber; add the spotted plate to the developing chamber; remove the spotted plate from the developing chamber producing a developed plate; place the developed plate in an ultraviolet light box; add a visualization agent to a dip tank; dip the developed plate in the dip tank and remove the developed plate quickly; and detect explosives by viewing said developed plate.

  6. Signal analysis of NEMS sensors at the output of a chromatography column

    SciTech Connect

    Bertholon, François; Harant, Olivier; Bourlon, Bertrand; Gerfault, Laurent; Grangeat, Pierre; Jutten, Christian

    2015-01-13

    This article introduces a joined Bayesian estimation of gas samples issued from a gas chromatography column (GC) coupled with a NEMS sensor based on Giddings Eyring microscopic molecular stochastic model. The posterior distribution is sampled using a Monte Carlo Markov Chain and Gibbs sampling. Parameters are estimated using the posterior mean. This estimation scheme is finally applied on simulated and real datasets using this molecular stochastic forward model.

  7. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    USGS Publications Warehouse

    Hladik, Michelle L.; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (?g/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 ?g/kg dry weight.

  8. Highly sensitive and selective analysis of widely targeted metabolomics using gas chromatography/triple-quadrupole mass spectrometry.

    PubMed

    Tsugawa, Hiroshi; Tsujimoto, Yuki; Sugitate, Kuniyo; Sakui, Norihiro; Nishiumi, Shin; Bamba, Takeshi; Fukusaki, Eiichiro

    2014-01-01

    In metabolomics studies, gas chromatography coupled with time-of-flight or quadrupole mass spectrometry has frequently been used for the non-targeted analysis of hydrophilic metabolites. However, because the analytical platform employs the deconvolution method to extract single-metabolite information from co-eluted peaks and background noise, the extracted peak is artificial product depending on the mathematical parameters and is not completely compatible with the pure component obtained by analyzing a standard compound. Moreover, it has insufficient ability for quantitative metabolomics. Therefore, highly sensitive and selective methods capable of pure peak extraction without any complicated mathematical techniques are needed. For this purpose, we have developed a novel analytical method using gas chromatography coupled with triple-quadrupole mass spectrometry (GC-QqQ/MS). We developed a selected reaction monitoring (SRM) method to analyze the trimethylsilyl derivatives of 110 metabolites, using electron ionization. This methodology enables us to utilize two complementary techniques-non-targeted and widely targeted metabolomics in the same sample preparation protocol, which would facilitate the formulation or verification of novel hypotheses in biological sciences. The GC-QqQ/MS analysis can accurately identify a metabolite using multichannel SRM transitions and intensity ratios in the analysis of living organisms. In addition, our methodology offers a wide dynamic range, high sensitivity, and highly reproducible metabolite profiles, which will contribute to the biomarker discoveries and quality evaluations in biology, medicine, and food sciences. PMID:23867096

  9. Qualitative drug analysis of hair extracts by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry.

    PubMed

    Guthery, Bill; Bassindale, Tom; Bassindale, Alan; Pillinger, Colin T; Morgan, Geraint H

    2010-06-25

    A technique using comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry (GCxGC/TOFMS) is applied to a qualitative analysis of three sample extracts from hair suspected of containing various drug compounds. The samples were also subjected to a quantitative target analysis for codeine, morphine, 6-monoacetylmorphine (6-MAM), amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethylamphetamine (MDMA), methadone, and benzylpiperazine (BZP) by liquid chromatography-tandem mass spectrometry (LC-MS/MS). GCxGC/TOFMS provided a non-specific procedure that identified various drugs, metabolites, and impurities not included in the target analysis. They included cocaine, diazepam, and methaqualone (quaalude). Comprehensive GCxGC separation was achieved using twin-stage cryo-modulation to focus eluant from a DB-5 ms (5% phenyl) to a BPX50 (50% phenyl) GC column. The TOF mass spectrometer provided unit mass resolution in the mass range m/z 5-1000 and rapid spectral acquisition (< or = 500spectra/s). Clean mass spectra of the individual components were obtained using mass spectral deconvolution software. The 'unknown' components were identified by comparison with mass spectra stored in a library database. PMID:20471020

  10. Analysis of a G-protein Coupled Receptor for Neurotensin by Liquid Chromatography-Electrospray Ionization Mass Spectrometry

    PubMed Central

    Ho, Jenny TC; White, Jim F.; Grisshammer, Reinhard; Hess, Sonja

    2008-01-01

    The type 1 neurotensin receptor (NTS1) belongs to the G-protein coupled receptor (GPCR) family. GPCRs are involved in important physiological processes but for many GPCRs ligand binding sites and other structural features have yet to be elucidated. Comprehensive analyses by mass spectrometry (MS) could address such issues, but they are complicated by the hydrophobic nature of the receptors. Recombinant NTS1 must be purified in the presence of detergents to maintain solubility and functionality of the receptor, to allow testing of ligand or G-protein interaction. However, detergents are detrimental to MS analyses. Hence steps need to be taken to substitute the detergents with MS-compatible polar/organic solvents. Here, we report the characterization of NTS1 by electrospray ionization mass spectrometry (ES-MS) with emphasis on methods to transfer intact NTS1 or its proteolytic peptides into compatible solvents by protein precipitation and liquid chromatography (LC) prior to ES-MS analyses. Molecular mass measurement of intact recombinant NTS1 was performed using a mixture of chloroform/methanol/aqueous TFA as the mobile phase for size exclusion chromatography-ES-MS analysis. In a separate experiment, NTS1 was digested with a combination of CNBr and trypsin and/or chymotrypsin. Subsequent reversed phase LC-ES-MS/MS analysis resulted in greater than 80% sequence coverage of the NTS1 receptor protein including all seven transmembrane domains. This work represents the first comprehensive analysis of recombinant NTS1 receptor using mass spectrometry. PMID:18294946

  11. An Ultra-Trace Analysis Technique for SF6 Using Gas Chromatography with Negative Ion Chemical Ionization Mass Spectrometry.

    PubMed

    Jong, Edmund C; Macek, Paul V; Perera, Inoka E; Luxbacher, Kray D; McNair, Harold M

    2015-07-01

    Sulfur hexafluoride (SF6) is widely used as a tracer gas because of its detectability at low concentrations. This attribute of SF6 allows the quantification of both small-scale flows, such as leakage, and large-scale flows, such as atmospheric currents. SF6's high detection sensitivity also facilitates greater usage efficiency and lower operating cost for tracer deployments by reducing quantity requirements. The detectability of SF6 is produced by its high molecular electronegativity. This property provides a high potential for negative ion formation through electron capture thus naturally translating to selective detection using negative ion chemical ionization mass spectrometry (NCI-MS). This paper investigates the potential of using gas chromatography (GC) with NCI-MS for the detection of SF6. The experimental parameters for an ultra-trace SF6 detection method utilizing minimal customizations of the analytical instrument are detailed. A method for the detection of parts per trillion (ppt) level concentrations of SF6 for the purpose of underground ventilation tracer gas analysis was successfully developed in this study. The method utilized a Shimadzu gas chromatography with negative ion chemical ionization mass spectrometry system equipped with an Agilent J&W HP-porous layer open tubular column coated with an alumina oxide (Al2O3) S column. The method detection limit (MDL) analysis as defined by the Environmental Protection Agency of the tracer data showed the method MDL to be 5.2 ppt. PMID:25452581

  12. Application of integrated comprehensive/multidimensional gas chromatography with mass spectrometry and olfactometry for aroma analysis in wine and coffee.

    PubMed

    Chin, Sung-Tong; Eyres, Graham T; Marriott, Philip J

    2015-10-15

    Component coelution in chromatographic analysis complicates identification and attribution of individual odour-active volatile molecules in complex multi-component samples. An integrated system incorporating comprehensive two-dimensional gas chromatography (GC × GC) and multidimensional gas chromatography (MDGC), with flame ionisation, olfactometry and mass spectrometry detection was developed to circumvent data correlation across different systems. Identification of potent odorants in Shiraz wine and the headspace of ground coffee are demonstrated as selected applications. Multiple solid-phase microextraction (SPME) sampling with GC-O located odour-active regions; GC × GC established the complexity of odour-active regions; MDGC provided high-resolution separation for each region; simultaneous 'O' and MS detection completed the analysis for target resolved peaks. Seven odour regions in Shiraz were analysed with MDGC-O/MS detection, revealing 11 odour volatiles through matching of mass spectrometry and retention indices from both separating dimensions, including acetic acid; octen-3-ol; ethyl octanoate; methyl-2-oxo-nonanoate; butanoic acid, 2-methylbutanoic acid, and 3-methylbutanoic acid; 3-(methylthio)-1-propanol; hexanoic acid; ?-damascenone; and ethyl-3-phenylpropanoate. A capsicum odour in ground coffee was identified as 2-methoxy-3-isobutylpyrazine with a 5-fold increase in S/N of the odorant when acquired using a 6-time cumulative SPME sampling approach. PMID:25952879

  13. Analysis of Essential Oil in Jerusalem Artichoke (Helianthus tuberosus L.) Leaves and Tubers by Gas Chromatography-Mass Spectrometry

    PubMed Central

    Helmi, Zead; Al Azzam, Khaldun Mohammad; Tsymbalista, Yuliya; Ghazleh, Refat Abo; Shaibah, Hassan; Aboul-Enein, Hassan

    2014-01-01

    Purpose: To investigate, for the first time, the chemical composition of essential oil of the tubers and leaves of Jerusalem artichoke (Helianthus tuberosus L.), a species of sunflower native to eastern North America, growing in Ukraine. Methods: A hydrodistillation apparatus was used for the extraction of volatile components and then it was analysed by gas chromatography equipped with a split-splitless injector (split ratio, 1:50) and flame ionization detector (FID). The oil was analyzed under linear temperature programming applied at 4°C/min from 50°C - 340°C. Temperatures of the injector and FID detector were maintained at 280°C and 300°C, respectively. The chemical analysis of the oil was carried out using gas chromatography coupled to mass spectrometry (GC-MS), to determine the chemical composition of the volatile fraction. Results: The essential oils content ranged from 0.00019 to 0.03486 and 0.00011 to 0.00205 (g/100g), in leaves and tubers, respectively. The qualitative and quantitative analysis led to the identification of 17 components in both species samples. The major component found in leaves and tubers was (-)-?-bisabolene with 70.7% and 63.1%, respectively. Conclusion: Essential oil profile of Jerusalem artichoke species showed significant differences between leaves and tubers species. Additionally, the leaves of Jerusalem artichoke are a promising source of natural ?-bisabolene. PMID:25671184

  14. Comprehensive analysis of chemical constituents in Xingxiong injection by high performance liquid chromatography coupled with mass spectrometry.

    PubMed

    Guo, Long; Dou, Li-Li; Duan, Li; Liu, Ke; Bi, Zhi-Ming; Li, Ping; Liu, E-Hu

    2015-09-01

    Xingxiong injection (XXI) is a widely used Chinese herbal formula prepared by the folium ginkgo extract and ligustrazine for the treatment of cardiovascular and cerebrovascular diseases. Compared with the pharmacological studies, chemical analysis and quality control studies on this formula are relatively limited. In the present study, a high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS) method was applied to comprehensive analysis of constituents in XXI. According to the fragmentation rules and previous reports, thirty ginkgo flavonoids, four ginkgo terpene lactones, and one alkaloid were identified. A high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ MS) method was then applied to quantify ten major constituents in XXI. The method validation results indicated that the developed method had desirable specificity, linearity, precision and accuracy. The total contents of ginkgo flavonoids were about 22.05-25.51 ?g·mL(-1) and the ginkgo terpene lactones amounts were about 4.41-8.70 ?g·mL(-1) in six batches of XXI samples, respectively. Furthermore, cosine ratio algorithm and distance measurements were employed to evaluate the similarity of XXI samples, and the results demonstrated a high-quality consistency. This work could provide comprehensive information on the quality control of Xingxiong injection, which be helpful in the establishment of a rational quality control standard. PMID:26412433

  15. Analysis of the anthraquinones aloe-emodin and aloin by gas chromatography/mass spectrometry.

    PubMed

    ElSohly, Mahmoud A; Gul, Waseem; Murphy, Timothy P

    2004-12-20

    A procedure was developed for the determination of low levels of the anthraquinones aloe-emodin and aloin A (barbalin) in aloe products based on gas chromatography/mass spectrometry (GC/MS) of the trimethyl silyl (TMS) derivatives of these analytes in the presence of Chrysophanol used as internal standard. The method was used to analyze several aloe based commercial products (liquids, gels and solids). Wide variation in the level of these anthraquinones was observed among the different products. The method had a sensitivity of 0.005 ppm of aloe-emodin and 0.05 ppm of aloin. PMID:15531290

  16. [Gas chromatography in quantitative analysis of hydrocyanic acid and its salts in cadaveric blood].

    PubMed

    Iablochkin, V D

    2003-01-01

    A direct gas chromatography method was designed for the quantitative determination of cyanides (prussic acid) in cadaveric blood. Its sensitivity is 0.05 mg/ml. The routine volatile products, including substances, which emerge due to putrefaction of organic matters, do not affect the accuracy and reproducibility of the method; the exception is H-propanol that was used as the internal standard. The method was used in legal chemical expertise related with acute cyanide poisoning (suicide) as well as with poisoning of products of combustion of nonmetals (foam-rubber). The absolute error does not exceed 10% with a mean quadratic deviation of 0.0029-0.0033 mg. PMID:14689782

  17. Evaluation of micellar electrokinetic capillary chromatography for the analysis of selected tobacco alkaloids.

    PubMed

    Yang, S S; Smetena, I; Goldsmith, A I

    1996-10-01

    Micellar electrokinetic capillary chromatography was evaluated for simultaneous determination of several tobacco alkaloids with similar molecular structure. Satisfactory separation of nicotine, nornicotine, myosmine, anatabine and anabasine extracted from tobacco was achieved by introducing an ionic surfactant, sodium dodecyl sulfate, into the buffer system at a concentration of 100 mM. Sample preparation involved a single extraction with water containing 1% triethanolamine. Separation was performed on a 72 cm long, uncoated fused-silica capillary. Experimental parameters such as applied voltage, pH value, buffer composition and surfactant concentration were optimized. Enhancement of UV absorption of alkaloids in the presence of micelles was also studied. PMID:8885385

  18. Purification of fire derived markers for lg scale isotope analysis C) using high performance liquid chromatography (HPLC)

    E-print Network

    Gilli, Adrian

    performance liquid chromatography (HPLC) Merle Gierga a, , Maximilian P.W. Schneider b , Daniel B. Wiedemeier isolated using high performance liquid chromatography (HPLC) and con- verted to CO2 via wet chemical

  19. Use of gel permeation chromatography for clean-up in the analysis of coccidiostats in eggs by liquid chromatography-tandem mass spectrometry.

    PubMed

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

    2013-05-01

    An analytical method for determination and confirmation of nine coccidiostatics in eggs is reported. Ethyl acetate is used as extraction solvent, with satisfactory results, and simple automated clean-up is based on gel-permeation chromatography (GPC) . The target compounds are then analysed by liquid chromatography-electrospray ionization-tandem mass spectrometry. The method was validated in-house in accordance with Commission Decision 2002/657/EC. Trueness and precision were determined at four concentrations, and the mean errors obtained were <10 %, with relative standard deviations ranging from 3 to 18 %. For three non-authorized coccidiostatics (clopidol, ethopabate, and ronizadole), decision limit and detection capability were in the ranges 0.12-0.16 and 0.18-0.23 ?g kg(-1), respectively. The results obtained prove the suitability of this new analytical method for routine monitoring of these substances in eggs. PMID:23535744

  20. Quantitative analysis of arbutin and hydroquinone in strawberry tree (Arbutus unedo L., Ericaceae) leaves by gas chromatography-mass spectrometry.

    PubMed

    Jurica, Karlo; Kara?onji, Irena Br?i?; Šegan, Sandra; Opsenica, Dušanka Milojkovi?; Kremer, Dario

    2015-09-01

    The phenolic glycoside arbutin and its metabolite with uroantiseptic activity hydroquinone occur naturally in the leaves of various medicinal plants and spices. In this study, an extraction procedure coupled with gas chromatography-mass spectrometry (GC-MS) was developed to determine arbutin and hydroquinone content in strawberry tree (Arbutus unedo L., Ericaceae) leaves. The method showed good linearity (R2>0.9987) in the tested concentration range (0.5-200 ?g mL(-1)), as well as good precision (RSD<5%), analytical recovery (96.2-98.0%), and sensitivity (limit of detection=0.009 and 0.004 ?g mL(-1) for arbutin and hydroquinone, respectively). The results obtained by the validated GC-MS method corresponded well to those obtained by high performance liquid chromatography (HPLC) method. The proposed method was then applied for determining arbutin and hydroquinone content in methanolic leaf extracts. The amount of arbutin in the leaves collected on the island of Kolo?ep (6.82 mg g(-1) dry weight) was found to be higher (tpaired=43.57, tc=2.92) in comparison to the amount of arbutin in the leaves collected on the island of Mali Lošinj (2.75 mg g(-1) dry weight). Hydroquinone was not detected in any of the samples. The analytical features of the proposed GC-MS method demonstrated that arbutin and hydroquinone could be determined alternatively by gas chromatography. Due to its wide concentration range, the method could also be suitable for arbutin and hydroquinone analysis in leaves of other plant families (Rosaceae, Lamiaceae, etc.). PMID:26444340

  1. Ultra-Trace Analysis of Nine Macrolides, including Tulathromycin A (Draxxin), in Edible Animal Tissues with Mini-Column Liquid Chromatography Tandem Mass Spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Analysis of 9 macrolides is presented, including tulathromycin A (Draxxin), in beef, poultry and pork muscle with a simple multi-residue extraction and analysis method using high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry. The extraction method inv...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  3. [Analysis of 43 pesticide residues in vegetables using solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry].

    PubMed

    Shi, Jiawei; Li, Jige; Wang, Yufei; Zhao, Yonggang

    2010-12-01

    A method for the simultaneous analysis of 43 pesticide residues in vegetables by gas chromatography coupled with triple quadrupole mass spectrometry (GC-QqQ-MS/MS) was developed and validated. The samples were extracted with acetonitrile, and then purified by solid-phase extraction (SPE). The detection of 43 pesticides was carried out by GC-QqQ-MS/MS in the multi-reaction monitoring (MRM) mode using external standard method. The overall recoveries determined at three spiked levels of 10, 80 and 100 microg/kg were 62.2%-170.0%, which in the recoveries of 36 pesticides were 70.0%-120.0%. The relative standard deviations (RSDs) were less than 18%. The limits of quantification (S/N > or =10) were 0.3-4.4 microg/kg. The method possesses low background and high sensitivity. It can be applied to the routine analysis of the 43 pesticides in vegetables. PMID:21438365

  4. Comprehensive two-dimensional gas chromatography combined to multivariate data analysis for detection of disease-resistant clones of Eucalyptus.

    PubMed

    Hantao, Leandro Wang; Toledo, Bruna Regina; Ribeiro, Fabiana Alves de Lima; Pizetta, Marilia; Pierozzi, Caroline Geraldi; Furtado, Edson Luiz; Augusto, Fabio

    2013-11-15

    In this paper it is reported the use of the chromatographic profiles from volatile fractions of plant clones - in this case, hybrids of Eucalyptus grandis×Eucalyptus urophylla - to determine specimens susceptible to rust disease. The analytes were isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography combined to fast quadrupole mass spectrometry (GC×GC-qMS). Parallel Factor Analysis (PARAFAC) was employed for estimate the correlation between the chromatographic profiles and resistance against Eucalyptus rust, after preliminary variable selection performed by Fisher ratio analysis. The proposed method allowed the differentiation between susceptible and non-susceptible clones and determination of three resistance biomarkers. This approach can be a valuable alternative for the otherwise time-consuming and labor-intensive methods commonly used. PMID:24148519

  5. Analysis of paralytic shellfish toxins, potential chemical threat agents, in food using hydrophilic interaction liquid chromatography-mass spectrometry.

    PubMed

    Jansson, Daniel; Åstot, Crister

    2015-10-23

    A novel method for determining paralytic shellfish toxin (PST) profiles in food was developed using a combination of silica and strong cation exchange (SCX) solid phase extraction (SPE) coupled to hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). Besides the risk for natural contamination of seafood and drinking water, PSTs also pose potent threats through intentional contamination of food, due to their high toxicity and the wide distributions of toxin-producing algae. The new preparation method aim to maintain the samples' original toxin profiles by avoiding conditions known to induce interconversion or degradation of the PSTs. The method was evaluated for PST extraction from water, milk, orange juice, apple purée, baby food, and blue mussels (Mytilus edulis). The extracts were found to produce reproducible retention times in HILIC-MS/MS analysis. When an authentic toxic mussel sample was analyzed using the novel method, saxitoxin and gonyautoxin-3 were identified, in agreement with data acquired using the Lawrence pre-column oxidation high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method. Overall recoveries of the PSTs from tested foods by the novel method ranged from 36% to 111%. PMID:26404910

  6. Retention mechanism assessment and method development for the analysis of iohexol and its related compounds in hydrophilic interaction liquid chromatography.

    PubMed

    Jovanovi?, Marko; Raki?, Tijana; Jan?i?-Stojanovi?, Biljana; Ivanovi?, Darko; Medenica, Mirjana

    2014-07-01

    Hydrophilic interaction liquid chromatography (HILIC) has emerged in recent years as a valuable alternative to reversed-phase liquid chromatography in the analysis of polar compounds. Research in HILIC is divided into two directions: the assessment of the retention mechanism and retention behavior, and the development of HILIC methods. In this work, four polar neutral analytes (iohexol and its related compounds A, B, and C) were analyzed on two silica and two diol columns in HILIC mode with the aim to investigate thoroughly the retention mechanisms and retention behavior of polar neutral compounds on these four columns. The adsorption and partition contribution to the overall HILIC retention mechanism was investigated by fitting the retention data to linear (adsorption and partition) and nonlinear (mixed-retention and quadratic) theoretical models. On the other hand, the establishment of empirical second-order polynomial retention models on the basis of D-optimal design made possible the estimation of the simultaneous influence of several mobile-phase-related factors. Furthermore, these models were also used as the basis for the application of indirect modeling of the selectivity factor and a grid point search approach in order to achieve the optimal separation of analytes. After the optimization goals had been set, the grids were searched and the optimal conditions were identified. Finally, the optimized method was subjected to validation. PMID:24752695

  7. Gas Chromatography Analysis with Olfactometric Detection (GC-O) as a Useful Methodology for Chemical Characterization of Odorous Compounds

    PubMed Central

    Brattoli, Magda; Cisternino, Ezia; Dambruoso, Paolo Rosario; de Gennaro, Gianluigi; Giungato, Pasquale; Mazzone, Antonio; Palmisani, Jolanda; Tutino, Maria

    2013-01-01

    The gas chromatography-olfactometry (GC-O) technique couples traditional gas chromatographic analysis with sensory detection in order to study complex mixtures of odorous substances and to identify odor active compounds. The GC-O technique is already widely used for the evaluation of food aromas and its application in environmental fields is increasing, thus moving the odor emission assessment from the solely olfactometric evaluations to the characterization of the volatile components responsible for odor nuisance. The aim of this paper is to describe the state of the art of gas chromatography-olfactometry methodology, considering the different approaches regarding the operational conditions and the different methods for evaluating the olfactometric detection of odor compounds. The potentials of GC-O are described highlighting the improvements in this methodology relative to other conventional approaches used for odor detection, such as sensoristic, sensorial and the traditional gas chromatographic methods. The paper also provides an examination of the different fields of application of the GC-O, principally related to fragrances and food aromas, odor nuisance produced by anthropic activities and odorous compounds emitted by materials and medical applications. PMID:24316571

  8. 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.

  9. 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.

  10. 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.

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

    E-print Network

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

    2008-01-01

    through processing and transportation, natural gas liquid (NGL) such as a combination of condensed propane, butane, and heavier hydrocarbons (C 4 +) with different dew point temperatures at a given pressure will condense or evaporate back and forth... the Thirtieth Industrial Energy Technology Conference, New Orleans, LA, May 6-9, 2008. and butane. By adding a refrigerator system and recovering all of the NGL?s through butane and a significant portion of propane, a cleaner, dryer natural gas will be sent...

  12. Quality Assessment of Ojeok-San, a Traditional Herbal Formula, Using High-Performance Liquid Chromatography Combined with Chemometric Analysis

    PubMed Central

    Kim, Jung-Hoon; Seo, Chang-Seob; Kim, Seong-Sil; Shin, Hyeun-Kyoo

    2015-01-01

    Ojeok-san (OJS) is a traditional herbal formula consisting of 17 herbal medicines that has been used to treat various disorders. In this study, quantitative analytical methods were developed using high-performance liquid chromatography equipped with a photodiode array detector to determine 19 marker compounds in OJS preparations, which was then combined with chemometric analysis. The method developed was validated in terms of its precision and accuracy. The intra- and interday precision of the marker compounds were <3.0% of the relative standard deviation (RSD) and the recovery of the marker compounds was 92.74%–104.16% with RSD values <3.0%. The results of our quantitative analysis show that the quantities of the 19 marker compounds varied between a laboratory water extract and commercial OJS granules. The chemometric analysis used, principal component analysis (PCA) and hierarchical clustering analysis (HCA), also showed that the OJS water extract produced using a laboratory method clearly differed from the commercial OJS granules; therefore, an equalized production process is required for quality control of OJS preparations. Our results suggest that the HPLC analytical methods developed are suitable for the quantification and quality assessment of OJS preparations when combined with chemometric analysis involving PCA and HCA. PMID:26539304

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. A sensitive non-derivatization method for apramycin and impurities analysis using hydrophilic interaction liquid chromatography and charged aerosol detection.

    PubMed

    Long, Zhen; Guo, Zhimou; Liu, Xiaoda; Zhang, Qi; Liu, Xingguo; Jin, Yan; Liang, Lina; Li, Huisu; Wei, Jie; Wu, Ningpeng

    2016-01-01

    A sensitive non-derivatization method was developed for the analysis of apramycin and impurites using hydrophilic interaction liquid chromatography (HILIC) and charged aerosol detection (CAD). Sample was pretreated with an effective SPE method (recovery >90%) to remove interference with apramycin impurities from sulfate, then analyzed with direct injection. Different chromatography modes of separation and choices of HILIC column were investigated in search of a direct analysis method. The HILIC-CAD method was optimized using a cysteine-bonded zwitterionic HILIC column and compared to the strong cation exchange-ultraviolet (SCX-UV) method with post-column derivatization recommended by the Chinese Pharmacopoeia (veterinary) 2010. The improved chromatographic resolution and peak shape with the HILIC-charged aerosol detection method allows for increase of sample load to 48.9µg from only 2.8µg with the SCX-UV approach. More than 16 impurities were detected with this method with improved resolution, and four were identified with MS, while only 7 impurities were detected with the SCX-UV method. Moreover, the current method has a good precision and reproducibility. The intra-day and inter-day of peak area variability was less than or equal to 4.760% RSD and 9.950%, respectively. The average limit of detection and quantization was 80ng and 200ng injected on the column, respectively. The overall results demonstrated that the presented method can be used as an alternative to SCX-UV method in the analysis of apramycin and impurities. PMID:26695285

  18. Analysis of lipophilic pigments from a phototrophic microbial mat community by high performance liquid chromatography

    NASA Technical Reports Server (NTRS)

    Palmisano, A. C.; Cronin, S. E.; Des Marais, D. J.

    1988-01-01

    As assay for lipophilic pigments in phototrophic microbial mat communities using reverse phase-high performance liquid chromatography was developed which allows the separation of 15 carotenoids and chloropigments in a single 30 min program. Lipophilic pigments in a laminated mat from a commercial salina near Laguna Guerrero Negro, Baja California Sur, Mexico reflected their source organisms. Myxoxanthophyll, echinenone, canthaxanthin, and zeaxanthin were derived from cyanobacteria; chlorophyll c, and fucoxanthin from diatoms; chlorophyll a from cyanobacteria and diatoms; bacteriochlorophylls a and c, bacteriophaeophytin a, and gamma-carotene from Chloroflexus spp.; and beta-carotene from a variety of phototrophs. Sensitivity of detection was 0.6-6.1 ng for carotenoids and 1.7-12 ng for most chloropigments. This assay represents a significant improvement over previous analyses of lipophilic pigments in microbial mats and promises to have a wider application to other types of phototrophic communities.

  19. Residue analysis of orthosulfamuron herbicide in fatty rice using liquid chromatography–tandem mass spectrometry

    PubMed Central

    Lee, Young-Jun; Choi, Jeong-Heui; Abd El-Aty, A.M.; Im, So Jeong; Musfiqur Rahman, Md.; Kim, Sung-Woo; Shim, Jae-Han

    2014-01-01

    In the present study, orthosulfamuron residues were extracted from fatty (unpolished) rice and rice straw using a modified QuEChERS method and analyzed using liquid chromatography–tandem mass spectrometry. The matrix-matched calibration was linear over the concentration ranges of 0.01–2.0 mg/kg with determination coefficient (R2) ? 0.997. The recovery rates at two fortification levels (0.1 and 0.5 mg/kg) were satisfactory and ranged between 88.1% and 100.6%, with relative standard deviation (RSD) <8%. The limit of quantitation, 0.03 mg/kg, was lower than the maximum residue limit, 0.05 mg/kg, set by the Ministry of Food and Drug Safety in the Republic of Korea. The developed method was applied successfully to field samples harvested at 116 days and none of the samples were positive for the residue. PMID:26257949

  20. Biointeraction Analysis of Immobilized Antibodies and Related Agents by High-Performance Immunoaffinity Chromatography

    PubMed Central

    Pfaunmiller, Erika; Moser, Annette C.; Hage, David S.

    2011-01-01

    Summary A method is described based on high-performance immunoaffinity chromatography for examining the interactions of immobilized antibodies or related binding agents with their targets. It is shown how this method can be used to obtain information on the binding, elution and regeneration kinetics of immobilized binding agents, such as those used with immunoaffinity supports. The theory behind this approach is briefly described and it is demonstrated how both the kinetic and thermodynamic properties of a biointeraction can be determined experimentally through this method. Several applications are used to illustrate this technique, including antibody-antigen interactions and the binding of aptamers with their targets in the presence of silica-based supports. The same approach can be adapted for use with other types of targets, binding agents and support materials. PMID:21907805

  1. Amino acid analysis in micrograms of meteorite sample by nanoliquid chromatography-high-resolution mass spectrometry.

    PubMed

    Callahan, Michael P; Martin, Mildred G; Burton, Aaron S; Glavin, Daniel P; Dworkin, Jason P

    2014-03-01

    Amino acids and their enantiomers in a 360 microgram sample of Murchison meteorite were unambiguously identified and quantified using chemical derivatization and nanoliquid chromatography coupled to nanoelectrospray ionization high resolution orbitrap mass spectrometry techniques. The distribution and abundance of amino acids were similar to past studies of Murchison meteorite but the samples used here were three orders of magnitude lower. The analytical method was also highly sensitive, and some amino acid reference standards were successfully detected at a level of ?200 attomoles (on column). These results may open up the possibility for investigating other less studied, sample-limited extraterrestrial samples (e.g., micrometeorites, interplanetary dust particles, and cometary particles) for biologically-relevant organic molecules. PMID:24529954

  2. Liquid chromatography/coordination ion spray-mass spectrometry for the analysis of rubber vulcanization products.

    PubMed

    Hayen, Heiko; Alvarez-Grima, M Montserrat; Debnath, Subhas C; Noordermeer, Jacques W M; Karst, Uwe

    2004-02-15

    Liquid chromatography/coordination ion spray-mass spectrometry has been used for the identification of reaction products in a model rubber vulcanization process. After LC separation using reversed-phase conditions, AgBF(4) in acetonitrile was added, and strong signals were observed for silica-rubber coupling agents and products of the reaction between these and alkenes. The method performs best for substances containing sulfur chains with chain lengths between two and eight sulfur atoms, but sulfur-free compounds containing triethoxysilyl groups were detected as well. For the latter, the postcolumn addition of NaBF(4) proved to be a suitable alternative. Besides the coupling agents, various reaction products, including sulfur-chain bridged alkenes were identified. PMID:14961739

  3. Analysis of anabolic androgenic steroids as sulfate conjugates using high performance liquid chromatography coupled to tandem mass spectrometry.

    PubMed

    Rzeppa, S; Heinrich, G; Hemmersbach, P

    2015-12-01

    Improvements in doping analysis can be effected by speeding up analysis time and extending the detection time. Therefore, direct detection of phase II conjugates of doping agents, especially anabolic androgenic steroids (AAS), is proposed. Besides direct detection of conjugates with glucuronic acid, the analysis of sulfate conjugates, which are usually not part of the routine doping control analysis, can be of high interest. Sulfate conjugates of methandienone and methyltestosterone metabolites have already been identified as long-term metabolites. This study presents the synthesis of sulfate conjugates of six commonly used AAS and their metabolites: trenbolone, nandrolone, boldenone, methenolone, mesterolone, and drostanolone. In the following these sulfate conjugates were used for development of a fast and easy analysis method based on sample preparation using solid phase extraction with a mixed-mode sorbent and detection by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). Validation demonstrated the suitability of the method with regard to the criteria given by the technical documents of the World Anti-Doping Agency (WADA). In addition, suitability has been proven by successful detection of the synthesized sulfate conjugates in excretion urines and routine doping control samples. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26472592

  4. Impact of gas chromatography and mass spectrometry combined with gas chromatography and olfactometry for the sex differentiation of Baccharis articulata by the analysis of volatile compounds.

    PubMed

    Minteguiaga, Manuel; Umpiérrez, Noelia; Fariña, Laura; Falcão, Manuel A; Xavier, Vanessa B; Cassel, Eduardo; Dellacassa, Eduardo

    2015-09-01

    The Baccharis genus has more than 400 species of aromatic plants. However, only approximately 50 species have been studied in oil composition to date. From these studies, very few take into consideration differences between male and female plants, which is a significant and distinctive factor in Baccharis in the Asteraceae family. Baccharis articulata is a common shrub that grows wild in south Brazil, northern and central Argentina, Bolivia, Paraguay and Uruguay. It is considered to be a medicinal plant and is employed in traditional medicine. We report B. articulata male and female volatile composition obtained by simultaneous distillation-extraction technique and analyzed by gas chromatography with mass spectrometry. Also, an assessment of aromatic differences between volatile extracts was evaluated by gas chromatography with olfactometry. The results show a very similar chemical composition between male and female extracts, with a high proportion of terpene compounds of which ?-pinene, limonene and germacrene D are the main components. Despite the chemical similarity, great differences in aromatic profile were found: male plant samples exhibited the strongest odorants in number and intensity of aromatic attributes. These differences explain field observations which indicate differences between male and female flower aroma, and might be of ecological significance in the attraction of pollinating insects. PMID:26140379

  5. Study of Grape Polyphenols by Liquid Chromatography-High-Resolution Mass Spectrometry (UHPLC/QTOF) and Suspect Screening Analysis.

    PubMed

    Flamini, Riccardo; De Rosso, Mirko; Bavaresco, Luigi

    2015-01-01

    Suspect screening analysis is a targeted metabolomics method in which the identification of compounds relies on specific available information, such as their molecular formula and isotopic pattern. This method, coupled to liquid chromatography-high-resolution mass spectrometry, is effective in the study of grape metabolomics, in particular for characterization of flavonols, stilbene derivatives, and anthocyanins. For identification of compounds expected in the samples, a new database of putative compounds was expressly constructed by using the molecular information on potential metabolites of grape and wine from the literature and other electronic databases. Currently, this database contains around 1,100 compounds. The method allows identification of several hundred grape metabolites with two analyses (positive and negative ionization modes), and performing of data reprocessing using "untargeted" algorithms also provided the identification of some flavonols and resveratrol trimers and tetramers in grape for the first time. This approach can be potentially used in the study of metabolomics of varieties of other plant species. PMID:25734021

  6. Comparative analysis of different plant oils by high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

    PubMed

    Jakab, Annamaria; Héberger, Károly; Forgács, Esther

    2002-11-01

    Different vegetable oil samples (almond, avocado, corngerm, grapeseed, linseed, olive, peanut, pumpkin seed, soybean, sunflower, walnut, wheatgerm) were analyzed using high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry. A gradient elution technique was applied using acetone-acetonitrile eluent systems on an ODS column (Purospher, RP-18e, 125 x 4 mm, 5 microm). Identification of triacylglycerols (TAGs) was based on the pseudomolecular ion [M+1]+ and the diacylglycerol fragments. The positional isomers of triacylglycerol were identified from the relative intensities of the [M-RCO2]+ fragments. Linear discriminant analysis (LDA) as a common multivariate mathematical-statistical calculation was successfully used to distinguish the oils based on their TAG composition. LDA showed that 97.6% of the samples were classified correctly. PMID:12462617

  7. Rapid resolution liquid chromatography (RRLC) analysis for quality control of Rhodiola rosea roots and commercial standardized products.

    PubMed

    Ma, Yuan-Chun; Wang, Xiao-Qiang; Hou, Fei Fei; Ma, Jie; Luo, Mai; Lu, Shane; Jin, Peter; Terevsky, Nelly; Chen, Alice; Xu, Iris; Patel, Asmita V; Gorecki, Dariusz

    2011-05-01

    A simple, sensitive and reliable reversed phase Rapid Resolution Liquid Chromatography (RRLC) method was developed and validated for six biologically active compounds (salidroside, tyrosol, rosarin, rosavin, rosin and rosiridin) in Rhodiola rosea L. roots and powder extracts. The method uses a Phenomenex C18 (2)-HST column at 40 degrees C with a neutral gradient system mobile phase (H20 and acetonitrile), a flow rate of 1.0 mL/min, and UV detection wavelengths set at 205 and 254 nm, simultaneously. Baseline separation of the six active compounds was achieved within 8 minutes. The average percentages of rosavins (rosarin, rosavin, and rosin) in authentic R. rosea roots and root powder extracts were quantitatively determined and a characteristic R. rosea roots RRLC profile was established. The RRLC method is accurate and sensitive; in addition, it effectively increases the sample analysis throughput compared with conventional HPLC. PMID:21615025

  8. Residue analysis of fipronil and difenoconazole in okra by liquid chromatography tandem mass spectrometry and their food safety evaluation.

    PubMed

    Hingmire, Sandip; Oulkar, Dasharath P; Utture, Sagar C; Ahammed Shabeer, T P; Banerjee, Kaushik

    2015-06-01

    A liquid chromatography tandem mass spectrometry (LC-MS/MS) based method is reported for simultaneous analysis of fipronil (plus its metabolites) and difenoconazole residues in okra. The sample preparation method involving extraction with ethyl acetate provided 80-107% recoveries for both the pesticides with precision RSD within 4-17% estimated at the limits of quantification (LOQ, fipronil=1ngg(-1), difenoconazole=5ngg(-1)) and higher fortification levels. In field, both the pesticides dissipated with half-life of 2.5days. The estimated pre-harvest intervals (PHI) for fipronil and difenoconazole were 15 and 19.5days, and 4 and 6.5days at single and double dose of field applications, respectively. Decontamination of incurred residues by washing and different cooking treatments was quite efficient in minimizing the residue load of both the chemicals. Okra samples harvested after the estimated PHIs were found safe for human consumption. PMID:25624217

  9. Ultra performance liquid chromatography analysis to study the changes in the carotenoid profile of commercial monovarietal fruit juices.

    PubMed

    Delpino-Rius, Antoni; Eras, Jordi; Marsol-Vall, Alexis; Vilaró, Francisca; Balcells, Mercè; Canela-Garayoa, Ramon

    2014-02-28

    We have developed an analytical method that allows the simultaneous determination of epoxycarotenoids, hydroxycarotenoids and carotenes in monovarietal fresh homemade and industrially processed fruit products. Analyses were carried out using ultra performance liquid chromatography (UPLC). The extraction method was optimized using methanol as the first extraction solvent for lyophilized samples followed by a saponification step. Recoveries ranged between 75% and 104% depending on the compound. Repeatability was better than 10% for all compounds (%RSD, n=3). The chromatographic analysis takes less than 17min. In this short period, up to 27 carotenoids were identified in apple, peach and pear products. The developed method allowed us to differentiate juice from six varieties of apple by their carotenoid profile. Moreover, the methodology allows us to differentiate the carotenoid profiles from commercial juices and homemade fresh peach and pear juices, as well as to study the rearrangements of 5,6- to 5,8-epoxycarotenoids. PMID:24503121

  10. Rapid and sensitive method for analysis of nitrate in meat samples using ultra performance liquid chromatography-mass spectrometry.

    PubMed

    Siddiqui, Masoom Raza; Wabaidur, Saikh Mohammad; ALOthman, Zeid A; Rafiquee, M Z A

    2015-12-01

    A sensitive and selective ultra performance liquid chromatography-mass spectrometric method has been developed for the quantitative analysis of nitrate in meat samples. Selected ion reaction (SIR) mode was adopted to identify and quantify the nitrate. Chromatographic analyses were performed on a BEH C-18 column with a mobile phase consisting of a surfactant (Cetylpyridinium chloride) and acetonitrile in equal ratio (50/50, v/v) at a flow rate of 0.4 mL min(-1). The limit of detection and limit of quantitation of the developed method was found to be 0.0599 and 0.1817 mg kg(-1), respectively. The linearity of the proposed method was checked in the concentration range of 0.5-10 mg kg(-1) with an excellent correlation coefficient (r) of 0.997. The recovery of the nitrate in the meat samples were in the range of 98.02-98.99%. PMID:26184470

  11. Fourier transform-infrared spectroscopy and Gas chromatography-mass spectroscopy: Reliable techniques for analysis of Parthenium mediated vermicompost

    NASA Astrophysics Data System (ADS)

    Rajiv, P.; Rajeshwari, Sivaraj; Venckatesh, Rajendran

    2013-12-01

    Fourier transform infrared spectroscopy (FT-IR) and Gas chromatography-mass spectroscopy have been carried out to investigate the chemical composition of Parthenium mediated vermicompost. Four different concentrations of Parthenium and cow dung mixtures were vermicomposted using the earthworms (Eudrilus eugeniae). FT-IR spectra reveal the absence of Parthenin toxin (sesquiterpene lactone) and phenols in vermicompost which was obtained from high concentration of cow dung mixed treatments. GC-MS analysis shows no phenolic compounds and predominant level of intermediate metabolites such as 4,8,12,16-Tetramethylheptadecan-4-olide (7.61%), 2-Pentadecanone, 6,10,14-trimethyl- (5.29%) and Methyl 16-methyl-heptadecanoate (4.69%) during the vermicomposting process. Spectral results indicated that Parthenin toxin and phenols can be eradicated via vermicomposting if mixed with appropriate quantity of cow dung.

  12. Fourier transform-infrared spectroscopy and Gas chromatography-mass spectroscopy: reliable techniques for analysis of Parthenium mediated vermicompost.

    PubMed

    Rajiv, P; Rajeshwari, Sivaraj; Venckatesh, Rajendran

    2013-12-01

    Fourier transform infrared spectroscopy (FT-IR) and Gas chromatography-mass spectroscopy have been carried out to investigate the chemical composition of Parthenium mediated vermicompost. Four different concentrations of Parthenium and cow dung mixtures were vermicomposted using the earthworms (Eudrilus eugeniae). FT-IR spectra reveal the absence of Parthenin toxin (sesquiterpene lactone) and phenols in vermicompost which was obtained from high concentration of cow dung mixed treatments. GC-MS analysis shows no phenolic compounds and predominant level of intermediate metabolites such as 4,8,12,16-Tetramethylheptadecan-4-olide (7.61%), 2-Pentadecanone, 6,10,14-trimethyl- (5.29%) and Methyl 16-methyl-heptadecanoate (4.69%) during the vermicomposting process. Spectral results indicated that Parthenin toxin and phenols can be eradicated via vermicomposting if mixed with appropriate quantity of cow dung. PMID:23998948

  13. Electrospray-differential mobility analysis as an orthogonal tool to size-exclusion chromatography for characterization of protein aggregates.

    PubMed

    Guha, Suvajyoti; Wayment, Joshua R; Tarlov, Michael J; Zachariah, Michael R

    2012-06-01

    The biopharmaceutical industry characterizes and quantifies aggregation of protein therapeutics using multiple analytical techniques to cross-validate results. Here, we demonstrate the use of electrospray-differential mobility analysis (ES-DMA), a gas-phase and atmospheric pressure ion-mobility method for characterizing protein aggregates. Two immunoglobulin Gs are systematically heat treated to induce aggregation and characterized using size-exclusion chromatography (SEC) and ES-DMA. Although ES-DMA is a gas-phase characterization method, we find that aggregation kinetic rate constants determined by ES-DMA is in good agreement with those determined by SEC. ES-DMA appears to have a higher resolution and lower limit of detection as compared with SEC. Thus, ES-DMA can potentially become an important orthogonal tool for characterization of nascent protein aggregates in the biopharmaceutical industry. PMID:22411567

  14. [Study on microwave hydrolysis for the analysis of amino acids in egg by high performance liquid chromatography].

    PubMed

    Shang, S; Wang, H

    1997-03-01

    A new hydrolysis method which only needs 7min--microwave hydrolysis used for the analysis of amino acids in egg by Pico-Tag high performance liquid chromatography (HPLC) is reported. The experimental results show that the satisfactory recovery could be obtained by use of 6mol/L HCL and 1% phenol as hydrolysing solution and a microwave oven with power of 300W. These conditions can also be used for the hydrolysis of other samples, such as rice, meat and so on. The average recovery of this method is 95% with a RSD of 2%. The accuracy is better than the conventional one (hydrolysis 24 at 110 degrees C) and Pico-Tag (hydrolysis 24h at 105 degrees C). Furthermore, the microwave hydrolysis decreases the loss of some unstable amino acids, e.g. Ser, Thr, Tyr, etc. In the process the method is convenient, rapid, accurate and reproducible. PMID:15739403

  15. Study of Grape Polyphenols by Liquid Chromatography-High-Resolution Mass Spectrometry (UHPLC/QTOF) and Suspect Screening Analysis

    PubMed Central

    Flamini, Riccardo; De Rosso, Mirko; Bavaresco, Luigi

    2015-01-01

    Suspect screening analysis is a targeted metabolomics method in which the identification of compounds relies on specific available information, such as their molecular formula and isotopic pattern. This method, coupled to liquid chromatography-high-resolution mass spectrometry, is effective in the study of grape metabolomics, in particular for characterization of flavonols, stilbene derivatives, and anthocyanins. For identification of compounds expected in the samples, a new database of putative compounds was expressly constructed by using the molecular information on potential metabolites of grape and wine from the literature and other electronic databases. Currently, this database contains around 1,100 compounds. The method allows identification of several hundred grape metabolites with two analyses (positive and negative ionization modes), and performing of data reprocessing using “untargeted” algorithms also provided the identification of some flavonols and resveratrol trimers and tetramers in grape for the first time. This approach can be potentially used in the study of metabolomics of varieties of other plant species. PMID:25734021

  16. Analysis of 10 systemic pesticide residues in various baby foods using liquid chromatography-tandem mass spectrometry.

    PubMed

    Yang, Angel; Abd El-Aty, A M; Park, Jong-Hyouk; Goudah, Ayman; Rahman, Md Musfiqur; Do, Jung-Ah; Choi, Ok-Ja; Shim, Jae-Han

    2014-06-01

    Ten systemic pesticides, comprising methomyl, thiamethoxam, acetamiprid, carbofuran, fosthiazate, metalaxyl, azoxystrobin, diethofencarb, propiconazole, and difenoconazole, were detected in 13 baby foods (cereals, boiled potatoes, fruit and milk) using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) for sample preparation and liquid chromatography tandem mass spectrometry for analysis. The matrix-matched calibration curves showed good linearity with determination coefficients (R(2) )?>0.992. The limits of detection and quantitation were 0.0015-0.003 and 0.005-0.01 mg/kg, respectively. The mean recoveries of three different concentrations ranged from 69.2 to 127.1% with relative standard deviations <20%. The method was successfully applied to 13 actual samples collected from a local market, and none of the samples were found to contain pesticide residues. This method is suitable for the identification and quantification of systemic pesticides with matrix-matched standards in various baby foods. PMID:24861738

  17. Visualization of gas–liquid mass transfer and wake structure of rising bubbles using pH-sensitive PLIF

    E-print Network

    Stohr, M.

    A planar laser-induced fluorescence (PLIF) technique for visualizing gas–liquid mass transfer and wake structure of rising gas bubbles is described. The method uses an aqueous solution of the pH-sensitive dye Naphthofluorescein ...

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

    E-print Network

    Uvwo, Ighofasan

    2006-04-12

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

  19. 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.

  20. Comprehensive Two-Dimensional Hydrophilic Interaction Chromatography (HILIC) × Reversed-Phase Liquid Chromatography Coupled to High-Resolution Mass Spectrometry (RP-LC-UV-MS) Analysis of Anthocyanins and Derived Pigments in Red Wine.

    PubMed

    Willemse, Chandré M; Stander, Maria A; Vestner, Jochen; Tredoux, Andreas G J; de Villiers, André

    2015-12-15

    Changes in anthocyanin chemistry represent some of the most important transformations involved in red wine aging. However, accurate analysis of the derived pigments, as required to study the evolution of anthocyanins and tannins during aging, is hampered by their extreme structural diversity, low levels, and the fact that many of these compounds have identical mass spectral characteristics. In this context, chromatographic separation is critical. In this contribution, the application of online hydrophilic interaction chromatography (HILIC) × reversed-phase liquid chromatography (RP-LC) separation coupled to high-resolution mass spectrometry (MS) is described for the detailed characterization of anthocyanins and their derived pigments in aged red wine. A systematic approach was followed for the optimization of HILIC × RP-LC separation parameters using a capillary liquid chromatography (LC) system in the first dimension and an ultrahigh-pressure LC system in the second dimension to ensure maximum sensitivity and performance. Ninety four (94) anthocyanin-derived pigments were tentatively identified in one- and six-year-old Pinotage wines using accurate mass and fragmentation information obtained using quadrupole-time-of-flight mass spectrometry (Q-TOF-MS). Online HILIC × RP-LC-MS was found to offer high-resolution separation, because of the combination of two different separation modes, while the structured elution order observed improved the certainty in compound identification. Therefore, this approach shows promise for the detailed elucidation of the chemical alteration of anthocyanins during wine aging. PMID:26554292

  1. Loop-based multiple heart-cutting two-dimensional liquid chromatography for target analysis in complex matrices.

    PubMed

    Pursch, Matthias; Buckenmaier, Stephan

    2015-05-19

    Loop-based multiple heart-cutting (MHC) two-dimensional liquid chromatography (2D-LC) is presented as a solution to quantify target components in complex matrices, such as additives in polymers, at very high chromatographic resolution. The determination of hexabromocyclododecane (HBCD) in polystyrene (PS) is described. One dimensional ((1)D) LC analysis with UV detection did not allow quantitation of the main isomers of HBCD due to peak overlap with polymer components. MHC 2D-LC analysis provided the separation power, accuracy, and repeatability needed for quantitative analysis of the additives of interest. Heart-cuts from peaks of the (1)D-chromatogram or entire regions of interest are sampled into loops, where they remain parked until their sequential reinjection onto the second dimension ((2)D) column. A column set consisting of phenyl ((1)D) and C18 ((2)D) stationary phases gave baseline separation in (2)D between HBCD and PS background. Linearity for spiked polymer samples was achieved over a range of 0.02-1.00 wt % HBCD relative to the amount of polymer. The limit of quantitation was estimated at 0.01 wt % HBCD in PS. A peak area RSD of 0.7% obtained for ten replicates of a real sample demonstrated excellent repeatability of the analysis. MHC 2D-LC is an elegant solution for quantitative analyses of difficult-to-separate samples when conventional (1)D separation fails. PMID:25897943

  2. Chromatographic fingerprinting analysis of Zhizhu Wan preparation by high-performance liquid chromatography coupled with photodiode array detector

    PubMed Central

    Sun, Hui; Chen, Xi; Zhang, Aihua; Sakurai, Tetsuro; Jiang, Jinzhong; Wang, Xijun

    2014-01-01

    Background: Traditional Chinese medicine (TCM) formula has been used for over 1000 years and most of them contain complicate chemical constituents. Chromatographic fingerprinting has been widely accepted as a crucial method for qualitative and quantitative analyses for TCM. Zhi Zhu Wan (ZZW), a classical Chinese medical formula, has been commonly used for the treatment of gastrointestinal disease, which pose a serious challenge to its quality control. Materials and Methods: In this work, a sensitive and reliable method of high-performance liquid chromatography coupled with photodiode array detector (HPLC-PDA) was developed to control the quality of ZZW for chemical fingerprint analysis and quantitative analysis of four major bioactive constituents, including hesperidin, naringin, neohesperidin, and atractylenolide I. The chromatographic separation was performed on a Waters Symmetry C18 column (4.6 mm × 250 mm, 5 ?m particle size), with an aqueous 0.095% phosphate acid and acetonitrile mobile phase gradient. Results: Optimization of other experimental conditions was validated with satisfactory accuracy, precision, repeatability, and recovery. In quantitative analysis, the four components showed good regression (R > 0.9994) within test ranges, and the recovery method ranged from 99.32% to 100.630%. HPLC fingerprints of the ZZW samples were compared by performing similarity analysis. Conclusion: The results indicated that the newly developed HPLC-PDA fingerprint method would be suitable for quality control of ZZW. PMID:25422548

  3. Assessment of repeatability of composition of perfumed waters by high-performance liquid chromatography combined with numerical data analysis based on cluster analysis (HPLC UV/VIS - CA).

    PubMed

    Ruzik, L; Obarski, N; Papierz, A; Mojski, M

    2015-06-01

    High-performance liquid chromatography (HPLC) with UV/VIS spectrophotometric detection combined with the chemometric method of cluster analysis (CA) was used for the assessment of repeatability of composition of nine types of perfumed waters. In addition, the chromatographic method of separating components of the perfume waters under analysis was subjected to an optimization procedure. The chromatograms thus obtained were used as sources of data for the chemometric method of cluster analysis (CA). The result was a classification of a set comprising 39 perfumed water samples with a similar composition at a specified level of probability (level of agglomeration). A comparison of the classification with the manufacturer's declarations reveals a good degree of consistency and demonstrates similarity between samples in different classes. A combination of the chromatographic method with cluster analysis (HPLC UV/VIS - CA) makes it possible to quickly assess the repeatability of composition of perfumed waters at selected levels of probability. PMID:25533703

  4. A NON-INVASIVE DIAGNOSIS OF INTESTINAL ISCHEMIA BY EXHALED BREATH ANALYSIS USING GAS CHROMATOGRAPHY AND MASS SPECTROMETRY-PRELIMINARY RESULTS

    EPA Science Inventory

    To explore the potential of exhaled breath analysis by Column Chromatography-Mass Spectrometry (GC-MS) as a non invasive and sensitive approach to evaluate mesenteric ischemia in pigs.

    Domestic pigs (n=3) were anesthetized with Guaifenesin/ Fentanyl/ Ketamine/ Xylazine...

  5. Optimization of separation and detection conditions for comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The 2,3,7,8-substituted polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) are among the most toxic compounds known. The current predominant method of analysis is too expensive and cumbersome, and comprehensive gas chromatography coupled to time-of-flight mass spect...

  6. Rapid qualitative and quantitative analysis of proanthocyanidin oligomers and polymers by ultra-performance liquid chromatography – tandem mass spectrometry (UPLC-MS/MS)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    We developed a rapid method with ultra-performance liquid chromatography – tandem mass spectrometry (UPLC-MS/MS) for the qualitative and quantitative analysis of plant proanthocyanidins (PAs) directly from crude plant extracts. The method utilizes a range of cone voltages to achieve the depolymeriza...

  7. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection of analysis of agrochemical residues and mycotoxines in food - challenges and applications

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence o...

  8. Fast,low-pressure gas chromatography triple quadrupole tandem mass spectrometry for analysis of 150 pesticide residues in fruits and vegetables

    Technology Transfer Automated Retrieval System (TEKTRAN)

    We developed and evaluated a new method of low-pressure gas chromatography-tandem mass spectrometry (LP-GC/MS-MS) for fast analysis of 150 pesticides in four representative fruits and vegetables. This LP-GC (vacuum outlet) approach entails coupling a 10 m, 0.53 mm i.d., 1 micron film analytical col...

  9. Qualitative aspects in the analysis of pesticide residues in fruits and vegetables using fast, low-pressure gas chromatography - time-of-flight mass spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Assessment of qualitative results in analytical methods is needed to estimate selectivity and devise criteria for chemical identification, particularly for mass spectrometric analysis. Low-pressure gas chromatography - mass spectrometry (LP-GC/MS) has been demonstrated to increase the speed of anal...

  10. Dehydration of Methylcyclohexanol Isomers in the Undergraduate Organic Laboratory and Product Analysis by Gas Chromatography-Mass Spectroscopy (GC-MS)

    ERIC Educational Resources Information Center

    Clennan, Malgorzata M.; Clennan, Edward L.

    2011-01-01

    Dehydrations of "cis"- and "trans"-2-methylcyclohexanol mixtures were carried out with 60% sulfuric acid at 78-80 [degrees]C as a function of time and the products were identified by gas chromatography-mass spectroscopy (GC-MS) analysis. The compounds identified in the reaction mixtures include alkenes, 1-, 3-, and 4-methylcyclohexenes and…

  11. A NEW SW-846 METHOD FOR THE ANALYSIS OF TOXAPHENE AND TOXAPHENE CONGENERS IN SOLID AND AQUEOUS SAMPLES USING GAS CHROMATOGRAPHY / NEGATIVE ION MASS SPECTROMETRY

    EPA Science Inventory

    US EPA SW-846 methods have typically relied on dual column gas chromatography coupled with electron capture detection (GC-ECD) for analysis of low concentrations of organochlorine pesticides, including toxaphene, in environmental samples. Toxaphene is one of the most widely appl...

  12. Evaluation of low-pressure gas chromatography-tandem mass spectrometry method for analysis of greater than 140 pesticides in fish

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A multi-residue method for analysis of 143 pesticide residues in fish was developed and evaluated using fast, low pressure gas chromatography triple quadrupole tandem mass spectrometry (LP-GC/MS-MS). The method was based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction with ace...

  13. AUTOMATED GEL-PERMEATION SYSTEM FOR REMOVAL OF LIPIDS IN GAS CHROMATOGRAPHY/MASS SPECTROMETRIC ANALYSIS OF FATTY TISSUES FOR XENOBIOTIC CHEMICALS

    EPA Science Inventory

    The interference of natural lipids in gas chromatography/mass spectrometric analysis of xenobiotic chemicals in fatty tissue can be substantially reduced using gel-permeation chromatographic removal of the lipids. This paper presents an inexpensive controller which can be used wi...

  14. Analysis of catechins in extracts of Cistus species by microemulsion electrokinetic chromatography.

    PubMed

    Pomponio, Romeo; Gotti, Roberto; Santagati, N Alfredo; Cavrini, Vanni

    2003-03-21

    A microemulsion electrokinetic chromatographic (MEEKC) method was developed for the separation of six catechins, specific marker phytochemicals of Cistus species. The MEEKC method involved the use of sodium dodecyl sulfate (SDS) as surfactant, heptane as organic solvent and butan-1-ol as co-solvent. In order to have a better stability of the studied catechins, the separation was performed under acidic conditions (pH 2.5 phosphate buffer). The effects of SDS concentration and of the amount of organic solvent and co-solvent on the analyte resolution were evaluated. The optimized conditions (heptane 1.36% (w/v), SDS 2.31% (w/v), butan-1-ol 9.72% (w/v) and 50 mM sodium phosphate buffer (pH 2.5) 86.61% (w/v)) allowed a useful and reproducible separation of the studied analytes to be achieved. These conditions provided a different separation profile compared to that obtained under conventional micellar electrokinetic chromatography (MECK) using SDS. The method was validated and applied to the determination of catechin and gallocatechin in lyophilized extracts of Cistus incanus and Cistus monspeliensis. PMID:12685600

  15. Urinary Succinylacetone Analysis by Gas Chromatography-Mass Spectrometry (GC-MS).

    PubMed

    Chen, Hongjie; Yu, Chunli

    2016-01-01

    Succinylacetone (SA) is used for the diagnosis and monitoring of patients with tyrosinemia type I (Tyr I). SA is exclusively elevated in blood and urine of patients with Tyr I. As urinary SA concentration is much higher than blood, SA is usually tested in urine samples. Urinary SA quantitation by gas chromatography mass spectrometry (GC-MS) is described in this chapter. The urine sample in the amount of 1 ?mol creatinine is used for testing. 3,4,5,6,7-(13)C5-succinylacetone ((13)C5-SA) is used as an internal standard (IS). SA and (13)C5-SA are oximated and extracted from urine with organic solvents, and then derivatized to form trimethylsilane (TMS) derivatives. TMS derivatives of SA and (13)C5-SA are detected and quantified by GC-MS using selective ion monitoring (SIM). The assay is linear from 0.05 to 450 mmol/mol creatinine to cover the broad range of urinary SA concentrations. PMID:26602140

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

    NASA Astrophysics Data System (ADS)

    Liu, Hongcheng; Gaza-Bulseco, Georgeen; Chumsae, Chris

    2009-12-01

    Size-exclusion chromatography (SEC) has been widely used to detect antibody aggregates, monomer, and fragments. SEC coupled to mass spectrometry has been reported to measure the molecular weights of antibody; antibody conjugates, and antibody light chain and heavy chain. In this study, separation of antibody light chain and heavy chain by SEC and direct coupling to a mass spectrometer was further studied. It was determined that employing mobile phases containing acetonitrile, trifluoroacetic acid, and formic acid allowed the separation of antibody light chain and heavy chain after reduction by SEC. In addition, this mobile phase allowed the coupling of SEC to a mass spectrometer to obtain a direct molecular weight measurement. The application of the SEC-MS method was demonstrated by the separation of the light chain and the heavy chain of multiple recombinant monoclonal antibodies. In addition, separation of a thioether linked light chain and heavy chain from the free light chain and the free heavy chain of a recombinant monoclonal antibody after reduction was also achieved. This optimized method provided a separation of antibody light chain and heavy chain based on size and allowed a direct measurement of molecular weights by mass spectrometry. In addition, this method may help to identify peaks eluting from SEC column directly.

  17. 234Th analysis of marine sediments via extraction chromatography and liquid scintillation counting.

    PubMed

    Nour, Svetlana; Burnett, William C; Horwitz, E Philip

    2002-08-01

    234Th is widely used as a natural tracer for study of biological mixing and particle scavenging processes in the ocean. This naturally occurring nuclide serves this purpose due to its convenient half-life (24.1 days), constant rate of production from 238U dissolved in seawater, and its strong tendency to attach to particles in seawater. As a beta/gamma emitter, 234Th may be determined using low-level gas-flow proportional counting, gamma spectrometry, and liquid scintillation counting (LSC). We describe here a technique which combines Cerenkov counting to evaluate 234Th (via 234Pa) with LSC alpha counting of 230Th added to the samples as a yield tracer. Our separation approach is based on a sample preparation procedure for marine sediments using nitric acid leaching in a "hot block", and extraction chromatography (TEVA x Resin) for Th isolation. Samples are counted in plastic LSC vials, using Ultima Gold AB cocktail, in 1 M H3PO4 media. A series of sediment samples spiked with known amounts of 234Th yielded activities within a few percent of the anticipated values. PMID:12150283

  18. Trace analysis of endectocides in milk by high performance liquid chromatography with fluorescence detection.

    PubMed

    Cerkvenik-Flajs, Vesna; Milcinski, Luka; Süssinger, Adica; Hodoscek, Lena; Danaher, Martin; Antoni?, Jan

    2010-03-24

    An analytical method has been developed for the simultaneous determination of the following endectocide drugs in milk: ivermectin, abamectin, doramectin, moxidectin, eprinomectin, emamectin and nemadectin. Samples were extracted with acetonitrile, purified with solid-phase extraction on a reversed phase C(8), derivatised with N-methylimidazole, trifluoroacetic anhydride and acetic acid to a stable fluorescent derivative, and were further analysed by gradient high performance liquid chromatography (HPLC) on an endcapped reversed phase Supelcosil LC-8-DB. The derivatisation step was mathematically optimised and the method was validated according to the requirements of Commission Decision 2002/657/EC, using fortified raw bovine milk. Mean recovery was between 78 and 98%. The repeatability (CV(r)) and within-laboratory reproducibility (CV(W)) ranged from 4.6 to 13.4% and from 6.6 to 14.5%, respectively. Decision limits (CCalpha) for analytes with MRL values, namely eprinomectin and moxidectin, were determined to be 24.8 and 50.6 microg kg(-1), respectively. CCalpha values for unauthorised endectocides ranged from 0.1 to 0.2 microg kg(-1). Due to high acceptability regarding the required criteria and applicability to ovine and caprine milk, giving similar results, this multi-analyte method has been successfully implemented in pharmacokinetic research studies as well as statutory residue monitoring in Slovenia. PMID:20206006

  19. Analysis of Tropical Forest Fire Emissions Using in Situ Gas Chromatography/Mass Spectrometry during Sambba

    NASA Astrophysics Data System (ADS)

    Minaeian, J.; Lewis, A. C.; Edwards, P. M.; Evans, M. J.; Hopkins, J. R.; Lee, J. D.; Purvis, R.

    2014-12-01

    Vertical atmospheric profiles of volatile organic compounds (VOCs) were made over Amazonia using an in situ gas chromatography/mass spectrometer (GC/MS), including isoprene, methacrolein, methyl vinyl ketone and products of biomass burning such as benzene. Measurements were made in the Amazonian (Rondônia and Amazonas) region during September 2012, a period of extensive biomass burning. Data was obtained between 100m and 8500m from the FAAM BAe 146 research aircraft. Isoprene was observed to be constrained overwhelmingly to the boundary layer (height typically ~2500m) with mean boundary layer mixing ratio of ~2 ppbv and a peak of ~5 ppbv at the lowest flight levels of 100 m. First generation isoprene oxidation products, methyl vinyl ketone and methacrolein, were quantified individually rather than as the sum of the pair, which is more commonly found in the literature. Both MACR and MVK were constrained primarily to the boundary layer, however trace quantities could be seen in the free troposphere to a height of 8000 m. Benzene from biomass burning was observed in both boundary layer and free troposphere, with a peak mixing ratio of ~0.8 ppbv at 750 m. This work will present the spatial distribution of isoprene within the boundary as a function of underlying surface type. The vertical profiles of all species are then compared to representative simulations from the GEOS-Chem chemistry transport model and conclusions drawn on the success of the model in representing emissions and oxidation chemistry.

  20. Enantiomeric analysis of polycyclic musks in water by chiral gas chromatography-tandem mass spectrometry.

    PubMed

    Wang, Lili; McDonald, James A; Khan, Stuart J

    2013-08-16

    Galaxolide (HHCB), tonalide (AHTN), phantolide (AHDI), traseolide (ATII) and cashmeran (DPMI) are synthetic polycyclic musks (PCMs). They are all commonly used in fragrance industries as racemic mixtures. A sensitive and robust enantioselective analytical method was developed to facilitate measurement of these chemicals in wastewater and environmental samples. The method is based on gas chromatography with tandem mass spectrometry (GC-MS/MS). Enantioseparation was assessed using four commercially available chiral capillary columns. Optimised resolution was achieved using a dual-column configuration of a chiral heptakis(2,3- di-O-methyl-6-O-t-butyl dimethylsilyl)-?-cyclodextrin column combined with a (non-chiral) HP-5MS column. This configuration was demonstrated to be capable of effectively resolving all commercially manufactured enantiomers of these five PCMs. Method detection limits for single enantiomers in drinking water and surface water range between 1.01 and 2.39ngL(-1). Full validation of the application of this method in these aqueous matrices is provided. PMID:23866122

  1. Magnetic solid phase extraction and gas chromatography-mass spectrometrical analysis of sixteen polycyclic aromatic hydrocarbons.

    PubMed

    Cai, Ying; Yan, Zhihong; NguyenVan, Manh; Wang, Lijia; Cai, Qingyun

    2015-08-01

    Fluorenyl functionalized superparamagnetic core/shell magnetic nanoparticles (MNPs, Fe3O4@SiO2@Flu) were prepared and characterized by transmission electron microscope, X-ray diffraction and infrared spectroscopy. The MNPs having an average diameter of 200nm were then used as solid-phase extraction sorbent for the determination of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in water samples designated by United States Environmental Protection Agency (U.S. EPA). The main influencing parameters, including sorbent amount, desorption solvent, sample volume and extraction time were optimized. Analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels. Limit of detection ranging from 0.5 to 4.0ng/L were obtained. The repeatability was investigated by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) lower than 13.1%. Finally, the proposed method was successfully applied for the determination of PAHs in water samples with the recoveries in the range of 96.0-106.7%. PMID:26122856

  2. [Simultaneous analysis of iodate, iodide, bromate and bromide by ion chromatography with ultraviolet detection].

    PubMed

    Li, Meng; Yu, Hong; Zheng, Xiurong

    2014-03-01

    An analytical method of ion chromatography with ultraviolet detection has been developed and applied for the simultaneous determination of iodate, iodide, bromate and bromide. The separation was performed on a quaternary ammonium type anion exchange column with citric acid and acetonitrile as mobile phase. The effects of the detection wavelength, the kind and concentration of the mobile phase and other parameters on separation and detection of the four ions were investigated. The retention rules were studied and the chromatographic conditions were optimized. Under the conditions of 210 nm as detection wavelength, 0.9 mL/min as flow rate, 40 degrees C as column temperature, and 1.0 mmol/L citric acid-acetonitrile (85:15, v/ v; pH 5.0) as mobile phase, the four ions were completely separated and the system peaks and other common anions didn't interfere with the determination. The detection limits of the four ions (S/N = 3) were 0.07-0.16 mg/L. The relative standard deviations of the retention times and peak areas obtained by determining samples five times continuously were below 1%. The spiked recoveries of the four anions were from 98.0% to 102%. This method has been successfully used to determine ionic liquids synthesized by chemistry laboratory and underground water samples. The results were accurate and reliable. PMID:24984472

  3. Continuous-bed chromatography for the analysis and purification of recombinant human basic fibroblast growth factor.

    PubMed

    Garke, G; Radtschenko, I; Anspach, F B

    1999-10-01

    The chromatographic properties of the commercial cation exchanger UNO-S1 (35x7 mm) was investigated using lysozyme from hen egg white as model protein and recombinant human basic fibroblast growth factor (rh-bFGF) from a high cell density cultivation of E. coli. The dynamic capacity for lysozyme (c(o) = 1 mg/ml) in 100 mM acetate buffer, pH 5 was 27 mg per ml sorbent. It was found independent of the flow-rate from 78 to 935 cm/h owing to the absence of mass transfer restrictions with this column concept. Regarding the selectivity for rh-bFGF and the capacity for lysozyme, no changes were apparent after cleaning-in-place (CIP) procedures with 0.5 M NaOH. Clogging of the column by a clarified crude cell homogenate of E. coli was not critical as precipitates were removed by reversal of the flow during CIP. Rh-bFGF elutes in three consequent peaks from the UNO-S1 column, which could be attributed to soluble rh-bFGF aggregates of different size. The dynamics of rh-bFGF aggregation and reaggregation in the crude feedstock was monitored by fast gradient elution chromatography. PMID:10536832

  4. Odorant Metabolism Analysis by an Automated Ex Vivo Headspace Gas-Chromatography Method.

    PubMed

    Faure, Philippe; Legendre, Arièle; Hanser, Hassan-Ismail; Andriot, Isabelle; Artur, Yves; Guichard, Elisabeth; Coureaud, Gérard; Heydel, Jean-Marie

    2016-01-01

    In the olfactory epithelium (OE), odorant metabolizing enzymes have the dual function of volatile component detoxification and active clearance of odorants from the perireceptor environment to respectively maintain the integrity of the tissues and the sensitivity of the detection. Although emphasized by recent studies, this enzymatic mechanism is poorly documented in mammals. Thus, olfactory metabolism has been characterized mainly in vitro and for a limited number of odorants. The automated ex vivo headspace gas-chromatography method that was developed here was validated to account for odorant olfactory metabolism. This method easily permits the measurement of the fate of an odorant in the OE environment, taking into account the odorant gaseous state and the cellular structure of the tissue, under experimental conditions close to physiological conditions and with a high reproducibility. We confirmed here our previous results showing that a high olfactory metabolizing activity of the mammary pheromone may be necessary to maintain a high level of sensitivity toward this molecule, which is critical for newborn rabbit survival. More generally, the method that is presented here may permit the screening of odorants metabolism alone or in mixture or studying the impact of aging, pathology, polymorphism or inhibitors on odorant metabolism. PMID:26446453

  5. Forensic analysis of hallucinogenic mushrooms and khat (Catha edulis Forsk) using cation-exchange liquid chromatography.

    PubMed

    Laussmann, Tim; Meier-Giebing, Sigrid

    2010-02-25

    Hallucinogenic mushrooms (e.g. Psilocybe and Panaeolus species) as well as leaves and young shoots of the khat tree (Catha edulis Forsk) are illicit drugs in many countries. The exact concentration of the hallucinogenic alkaloids psilocin and psilocybin in mushrooms and the sympathomimetic alkaloids cathinone and cathine in khat is usually essential for jurisdiction. Facing an increasing number of mushroom and khat seizures by German customs authorities, a convenient comprehensive quantitative HPLC method based on cation-exchange liquid chromatography for these rather "exotic" drugs has been developed which avoids time-consuming multi-step sample preparation or chemical derivatization procedures. Using this method a number of different hallucinogenic fungi species and products that are mainly distributed via the internet have been analysed (dried and fresh Psilocybe cubensis Singer as well as P. cubensis collected from "grow boxes", Panaeolus cyanescens Berkeley and Broome and so-called "philosopher stones" (sclerotia of Psilocybe species)). Highest total amounts of psilocin have been detected in dried P. cyanescens reaching up to 3.00+/-0.24 mg per 100 mg. The distribution of khat alkaloids in different parts of the khat shoots has been studied. High concentrations of cathinone have not only been detected in leaves but also in green parts and barks of stalks. Additionally, the sample treatment for fresh mushroom and khat samples has been optimised. Highest amounts of alkaloids were found when fresh material was freeze-dried. PMID:20047807

  6. Quantitative Metabolome Analysis Based on Chromatographic Peak Reconstruction in Chemical Isotope Labeling Liquid Chromatography Mass Spectrometry.

    PubMed

    Huan, Tao; Li, Liang

    2015-07-21

    Generating precise and accurate quantitative information on metabolomic changes in comparative samples is important for metabolomics research where technical variations in the metabolomic data should be minimized in order to reveal biological changes. We report a method and software program, IsoMS-Quant, for extracting quantitative information from a metabolomic data set generated by chemical isotope labeling (CIL) liquid chromatography mass spectrometry (LC-MS). Unlike previous work of relying on mass spectral peak ratio of the highest intensity peak pair to measure relative quantity difference of a differentially labeled metabolite, this new program reconstructs the chromatographic peaks of the light- and heavy-labeled metabolite pair and then calculates the ratio of their peak areas to represent the relative concentration difference in two comparative samples. Using chromatographic peaks to perform relative quantification is shown to be more precise and accurate. IsoMS-Quant is integrated with IsoMS for picking peak pairs and Zero-fill for retrieving missing peak pairs in the initial peak pairs table generated by IsoMS to form a complete tool for processing CIL LC-MS data. This program can be freely downloaded from the www.MyCompoundID.org web site for noncommercial use. PMID:26086729

  7. Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Qian, Michael C.; Peterson, Devin G.; Reineccius, Gary A.

    The first publication on gas chromatography (GC) was in 1952 (1), while the first commercial instruments were manufactured in 1956. James and Martin (1) separated fatty acids by GC, collected the column effluent, and titrated the individual fatty acids for quantitation. GC has advanced greatly since that early work and is now considered to be a mature field that is approaching theoretical limitations.

  8. Gas chromatography

    SciTech Connect

    Willett, J.

    1987-01-01

    This book includes discussions of chemical equilibria, the properties of solutions and gases, the structures of molecules and how they attract one another. It assumes basic knowledge of chemistry and electricity. This book also provides a basic understanding of gas chromatography in a flexible format.

  9. High Performance Liquid Chromatography

    NASA Astrophysics Data System (ADS)

    Talcott, Stephen

    High performance liquid chromatography (HPLC) has many applications in food chemistry. Food components that have been analyzed with HPLC include organic acids, vitamins, amino acids, sugars, nitrosamines, certain pesticides, metabolites, fatty acids, aflatoxins, pigments, and certain food additives. Unlike gas chromatography, it is not necessary for the compound being analyzed to be volatile. It is necessary, however, for the compounds to have some solubility in the mobile phase. It is important that the solubilized samples for injection be free from all particulate matter, so centrifugation and filtration are common procedures. Also, solid-phase extraction is used commonly in sample preparation to remove interfering compounds from the sample matrix prior to HPLC analysis.

  10. Quantitative hydrophilic interaction chromatography-mass spectrometry analysis of N-acetylneuraminic acid and N-acetylmannosamine in human plasma.

    PubMed

    Shi, Yifan; Xu, Xin; Fang, Meng; Zhang, Michael; Li, Yinghe; Gillespie, Brad; Yorke, Selwyn; Yang, Nora; McKew, John C; Gahl, William A; Huizing, Marjan; Carrillo-Carrasco, Nuria; Wang, Amy Qiu

    2015-09-01

    N-acetylneuraminic acid (Neu5Ac or NANA) is the most predominant sialic acid in mammals. As a terminal component in many glycoproteins and glycolipids, sialic acid is believed to be an important biomarker related to various diseases. Its precursor, N-acetylmannosamine (ManNAc), is being investigated as a potential treatment for GNE myopathy. In this work, we developed two highly sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods for the quantitation of ManNAc and free Neu5Ac in human plasma. A fit-for-purpose approach was adopted during method validation and sample analysis. To measure the endogenous compounds and overcome the interference from plasma samples, a surrogate matrix that contained 5% bovine serum albumin (BSA) was used for the preparation of calibration standards and certain levels of quality control (QC) samples. QC samples at higher concentrations were prepared in the authentic matrix (human plasma) to best mimic incurred samples. For both methods, an Ostro 96-well phospholipid removal plate was used for sample extraction, which efficiently removed the phospholipids from the plasma samples prior to LC injection, eliminated matrix effect, and improved sensitivity. Chromatographic separation was achieved using hydrophilic interaction chromatography (HILIC) and gradient elution in order to retain the two polar compounds. The lower limit of quantitation (LLOQ) for ManNAc and Neu5Ac was 10.0 and 25.0ng/mL, respectively. The overall accuracy of the two assays was within 100%±8.3% based on three levels of QC samples. Inter- and intra-run precision (coefficient of variation (%CV)) across three analytical runs was less than 6.7% for ManNAc and less than 10.8% for Neu5Ac. These methods have been validated to support clinical studies. PMID:26218770

  11. [Rapid analysis of 28 primary aromatic amines in aqueous food simulants by high performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Xiao, Xiaofeng; Wang, Jianling; Yang, Juanjuan; Liu, Tingfei; Chen, Tong; He, Jun; Deng, Hongyi; Gao, Qiyan

    2013-01-01

    A novel method for rapid analysis of the migration amounts of 28 primary aromatic amines (PAAs) in aqueous food simulants (10% ethanol, 30 g/L acetic acid and 20% ethanol aqueous solution) was developed using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After the migration test, the soaking solution was cooled down from 100 degrees C, vortexed, filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe, and then the filtrate was analyzed by HPLC-MS/MS. A Zorbax SB-Phenyl column (250 mm x 4.6 mm, 5 microm) was selected for chromatography. The mobile phase consisted of water and 0.1% formic acid-25% acetonitrile-methanol solution with gradient elution. The 28 PAAs in aqueous food simulants were detected by tandem mass spectrometer operated in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The limits of quantification for the 28 PAAs were between 0.002 microg/L and 10 microg/L. The linearity of the method was good with correlation coefficients (r2) greater than 0.995 over the concentration range from 5 microg/L or 10 microg/L to 100 microg/L. The average recoveries of the 28 PAAs were between 76.6% and 114% with the relative standard deviations between 1.53% and 8.97% at the levels of 10, 20, and 40 microg/L. The method shows rapid pretreatment, the lower limits of quantification, good recoveries and accuracies, and meets the requirement of European Union (EU) No 10/2011 regulation for the specific migration of PAAs. The method has been applied to analyze the 28 PAAs in different aqueous food simulants from the migration test of 30 batches of food contact material samples exported to EU. PMID:23667988

  12. Chemical dereplication of marine actinomycetes by liquid chromatography-high resolution mass spectrometry profiling and statistical analysis.

    PubMed

    Forner, David; Berrué, Fabrice; Correa, Hebelin; Duncan, Katherine; Kerr, Russell G

    2013-12-17

    Discovery of novel bioactive metabolites from marine bacteria is becoming increasingly challenging, and the development of novel approaches to improve the efficiency of early steps in the microbial drug discovery process is therefore of interest. For example, current protocols for the taxonomic dereplication of microbial strains generally use molecular tools which do not take into consideration the ability of these selected bacteria to produce secondary metabolites. As the identification of novel chemical entities is one of the key elements driving drug discovery programs, this study reports a novel methodology to dereplicate microbial strains by a metabolomics approach using liquid chromatography-high resolution mass spectrometry (LC-HRMS). In order to process large and complex three dimensional LC-HRMS datasets, the reported method uses a bucketing and presence-absence standardization strategy in addition to statistical analysis tools including principal component analysis (PCA) and cluster analysis. From a closely related group of Streptomyces isolated from geographically varied environments, we demonstrated that grouping bacteria according to the chemical diversity of produced metabolites is reproducible and provides greatly improved resolution for the discrimination of microbial strains compared to current molecular dereplication techniques. Importantly, this method provides the ability to identify putative novel chemical entities as natural product discovery leads. PMID:24296145

  13. Miniaturized ultra-high performance liquid chromatography coupled to electrochemical detection: Investigation of system performance for neurochemical analysis.

    PubMed

    Van Schoors, Jolien; Maes, Katrien; Van Wanseele, Yannick; Broeckhoven, Ken; Van Eeckhaut, Ann

    2016-01-01

    The interest in implementation of miniaturized ultra-high performance liquid chromatography (UHPLC) in neurochemical research is growing because of the need for faster, more selective and more sensitive neurotransmitter analyses. The instrument performance of a tailor designed microbore UHPLC system coupled to electrochemical detection (ECD) is investigated, focusing on the quantitative monoamine determination in in vivo microdialysis samples. The use of a microbore column (1.0mm I.D.) requires miniaturization of the entire instrument, though a balance between extra-column band broadening and injection volume must be considered. This is accomplished through the user defined Performance Optimizing Injection Sequence, whereby 5?L sample is injected on the column with a measured extra-column variance of 4.5-9.0?L(2) and only 7?L sample uptake. Different sub-2?m and superficially porous particle stationary phases are compared by means of the kinetic plot approach. Peak efficiencies of about 16000-35000 theoretical plates are obtained for the Acquity UPLC BEH C18 column within 13min analysis time. Furthermore, the coupling to ECD is shown suitable for microbore UHPLC analysis thanks to the miniaturized flow cell design, sufficiently fast data acquisition and mathematical data filtering. Ultimately, injection of in vivo samples demonstrates the applicability of the system for microdialysis analysis. PMID:26687168

  14. Analysis of trace inorganic anions in weak acid salts by single pump cycling-column-switching ion chromatography.

    PubMed

    Huang, Zhongping; Ni, Chengzhu; Zhu, Zhuyi; Pan, Zaifa; Wang, Lili; Zhu, Yan

    2015-05-01

    The application of ion chromatography with the single pump cycling-column-switching technique was described for the analysis of trace inorganic anions in weak acid salts within a single run. Due to the hydrogen ions provided by an anion suppressor electrolyzing water, weak acid anions could be transformed into weak acids, existing as molecules, after passing through the suppressor. Therefore, an anion suppressor and ion-exclusion column were adopted to achieve on-line matrix elimination of weak acid anions with high concentration for the analysis of trace inorganic anions in weak acid salts. A series of standard solutions consisting of target anions of various concentrations from 0.005 to 10 mg/L were analyzed, with correlation coefficients r ? 0.9990. The limits of detection were in the range of 0.67 to 1.51 ?g/L, based on the signal-to-noise ratio of 3 and a 25 ?L injection volume. Relative standard deviations for retention time, peak area, and peak height were all less than 2.01%. A spiking study was performed with satisfactory recoveries between 90.3 and 104.4% for all anions. The chromatographic system was successfully applied to the analysis of trace inorganic anions in five weak acid salts. PMID:25641739

  15. Comparison of segmented flow analysis and ion chromatography for the quantitative characterization of carbohydrates in tobacco products.

    PubMed

    Shifflett, John R; Jones, Lindsey A; Limowski, Edward R; Bezabeh, Dawit Z

    2012-11-28

    Segmented flow analysis (SFA) and ion chromatography with pulsed amperometric detection (IC-PAD) are widely used analytical techniques for the analysis of glucose, fructose, and sucrose in tobacco. In the work presented here, 27 cured tobacco leaves and 21 tobacco products were analyzed for sugars using SFA and IC. The results of these analyses demonstrated that both techniques identified the same trends in sugar content across tobacco leaf and tobacco product types. However, comparison of results between techniques was limited by the selectivity of the SFA method, which relies on the specificity of the reaction of p-hydroxybenzoic acid hydrazide (PAHBAH) with glucose and fructose to generate a detectable derivative. Sugar amines and chlorogenic acid, which are found in tobacco, are also known to react with PAHBAH to form a reaction product that interferes with the analysis of fructose and glucose. To mitigate this problem, solid phase extraction (SPE) was used to remove interferences such as sugar amines and chlorogenic acid from sample matrices prior to SFA. A combination of C18 and cation exchange solid phase extraction cartridges was used, and the results from SFA and IC analyses showed significant convergence in the results of both analytical methods. For example, the average difference between the results from the SFA and IC analyses for flue-cured tobacco samples dropped by 73% when the two-step C18/cation exchange resin sample cleanup was used. PMID:23131129

  16. Carbon Stable Isotope Analysis of Methylmercury Toxin in Biological Materials by Gas Chromatography Isotope Ratio Mass Spectrometry.

    PubMed

    Masbou, Jeremy; Point, David; Guillou, Gaël; Sonke, Jeroen E; Lebreton, Benoit; Richard, Pierre

    2015-12-01

    A critical component of the biogeochemical cycle of mercury (Hg) is the transformation of inorganic Hg to neurotoxic monomethylmercury (CH3Hg). Humans are exposed to CH3Hg by consuming marine fish, yet the origin of CH3Hg in fish is a topic of debate. The carbon stable isotopic composition (?(13)C) embedded in the methyl group of CH3Hg remains unexplored. This new isotopic information at the molecular level is thought to represent a new proxy to trace the carbon source at the origin of CH3Hg. Here, we present a compound-specific stable isotope analysis (CSIA) technique for the determination of the ?(13)C value of CH3Hg in biological samples by gas chromatography combustion isotope ratio mass spectrometry analysis (GC-C-IRMS). The method consists first of calibrating a CH3Hg standard solution for ?(13)C CSIA. This was achieved by comparing three independent approaches consisting of the derivatization and halogenation of the CH3Hg standard solution. The determination of ?(13)CCH3Hg values on natural biological samples was performed by combining a CH3Hg selective extraction, purification, and halogenation followed by GC-C-IRMS analysis. Reference ?(13)C values were established for a tuna fish certified material (ERM-CE464) originating from the Adriatic Sea (?(13)CCH3Hg = -22.1 ± 1.5‰, ± 2 SD). This value is similar to the ?(13)C value of marine algal-derived particulate organic carbon (?(13)CPOC = -21‰). PMID:26511394

  17. Analysis of free and conjugated phytosterols in tobacco by an improved method using gas chromatography-flame ionization detection.

    PubMed

    Liu, Wen-Hui; Ding, Bin; Ruan, Xiao-Ming; Xu, Hai-Tao; Yang, Jun; Liu, Shao-Min

    2007-09-01

    An improved and simple method using capillary gas chromatography coupled with a flame ionization detection system (GC-FID) has been developed for quantitative analysis of free and conjugated phytosterols in tobacco. Direct acid and alkaline hydrolysis were first introduced into tobacco analysis to liberate free phytosterols from conjugates, followed by extraction with hexane, derivatization to trimethylsilyl ether derivatives and finally GC quantitative determination. The generality and applicability of this improved method for analyzing free and conjugated phytosterols in tobacco were validated after a series of optimization and comparison were done. Compared with traditional methods, this improved method not only simplified procedures, but also saved time and solvent. The limits of detection (LODs) of phytosterols varied from 0.35 to 0.10 microg mL(-1), the relative standard deviations (RSD) were from 2.3% to 3.3% and recovery ranged from 87% to 99%. The analysis results showed that total phytosterols' content in tobacco ranged from 1.0 to 2.5 mg g(-1), and most phytosterols existed as conjugates, only approximately 15-25% phytosterols existed in free-form. Ergosterol was only found in mildewy flued-cured tobacco and the level was approximately 0.2-0.25 mg g(-1). PMID:17624356

  18. Studies on Quantitative Phosphopeptide Analysis by MALDI Mass Spectrometry Without Label, Chromatography or Calibration Curves

    PubMed Central

    Ho, Hsin-Pin; Rathod, Pratikkumar; Louis, Marissa; Tada, Christine K.; Rahaman, Sherida; Mark, Kevin J.; Leng, Jin; Dana, Dibyendu; Kumar, Sanjai; Lichterfeld, Mathias; Chang, Emmanuel J.

    2014-01-01

    Rationale Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry combined with isotope labeling methods are effective for protein and peptide quantification, but limited in their multiplexing capacity, cost-effectiveness and dynamic range. This study investigates MALDI MS-based quantification of peptide phosphorylation without labeling, and aims to overcome the shot-to-shot variability of MALDI using a mathematical transformation and extended data acquisition times. Methods A linear relationship between the reciprocal of phosphopeptide mole fraction and the reciprocal of phosphorylated-to-unphosphorylated signal ratio is derived, and evaluated experimentally using three separate phosphopeptide systems containing phosphorylated serine, threonine and tyrosine residues: mixtures of phosphopeptide and its des-phospho-analog with known stoichiometry measured by vacuum MALDI-linear ion trap mass spectrometry and fit to the linear model. The model is validated for quantifying in vitro phosphorylation assays with inhibition studies on Cdk2/cyclinA. Results Dynamic range of picomoles to femtomoles, good accuracy (deviations of 1.5–3.0% from expected values) and reproducibility (RSD = 4.3–6.3%) are achieved. Inhibition of Cyclin-dependent Kinase phosphorylation by the classical inhibitors olomoucine and r-roscovitine was evaluated and IC50 values found to be in agreement with reported literature values. These results, achieved with single-point calibration, without isotope or chromatography, compare favorably to those arrived at using isotope dilution (p > 0.5 for accuracy). Conclusion The mathematical relationship derived here can be applied to a method that we term Double Reciprocal Isotope-free Phosphopeptide Quantification (DRIP-Q), as a strategy for quantification of in vitro phosphorylation assays, the first MALDI-based, isotope- and calibration curve-free method of its type. These results also pave the way for further systematic studies investigating the effect of peptide composition and experimental conditions on quantitative, label-free MALDI. PMID:25380489

  19. Combined Liquid Chromatography–Tandem Mass Spectrometry Analysis of Progesterone Metabolites

    PubMed Central

    Sinreih, Maša; Zukunft, Sven; Sosi?, Izidor; Cesar, Jožko; Gobec, Stanislav; Adamski, Jerzy; Lanišnik Rižner, Tea

    2015-01-01

    Progesterone has a number of important functions throughout the human body. While the roles of progesterone are well known, the possible actions and implications of progesterone metabolites in different tissues remain to be determined. There is a growing body of evidence that these metabolites are not inactive, but can have significant biological effects, as anesthetics, anxiolytics and anticonvulsants. Furthermore, they can facilitate synthesis of myelin components in the peripheral nervous system, have effects on human pregnancy and onset of labour, and have a neuroprotective role. For a better understanding of the functions of progesterone metabolites, improved analytical methods are essential. We have developed a combined liquid chromatography—tandem mass spectrometry (LC-MS/MS) method for detection and quantification of progesterone and 16 progesterone metabolites that has femtomolar sensitivity and good reproducibility in a single chromatographic run. MS/MS analyses were performed in positive mode and under constant electrospray ionization conditions. To increase the sensitivity, all of the transitions were recorded using the Scheduled MRM algorithm. This LC-MS/MS method requires small sample volumes and minimal sample preparation, and there is no need for derivatization. Here, we show the application of this method for evaluation of progesterone metabolism in the HES endometrial cell line. In HES cells, the metabolism of progesterone proceeds mainly to (20S)-20-hydroxy-pregn-4-ene-3-one, (20S)-20-hydroxy-5?-pregnane-3-one and (20S)-5?-pregnane-3?,20-diol. The investigation of possible biological effects of these metabolites on the endometrium is currently undergoing. PMID:25680188

  20. Characterization and quantitative amino acids analysis of analgesic peptides in cinobufacini injection by size exclusion chromatography, matrix-assisted laser desorption/ionization time of flight mass spectrometry and gas chromatography mass spectrometry.

    PubMed

    Wu, Xu; Si, Nan; Bo, Gao; Hu, Hao; Yang, Jian; Bian, Baolin; Zhao, Hai Yu; Wang, Hongjie

    2015-01-01

    Cinobufacini injection that comes from the water extract of Bufo bufo gargarizans Cantor skin is widely used for cancer treatment in China. Peptide is one of its major types of constituents, however the biological effects and content of this injection are little reported. In present study, the analgesic effect of peptides was determined and evaluated by in-vivo models. To characterize and quantitatively analyze these peptides, a reliable and efficient method combining size exclusion chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry with amino acid analysis was developed. The peptides presented as a series of analogs with similar molecular weights mostly ranging from 2 to 8 kDa. The amino acid analysis by gas chromatography mass spectrometry (GC-MS) was developed to determine both free and combined amino acids (FAA and CAA) in cinobufacini injection. This method achieved good linearity (R(2) , 0.9909-0.9999) and low limit of detection and quantification. FAA and CAA samples were efficiently analyzed by modified Phenomenex EZ: faast procedure. For the sample analysis, the method showed good repeatability (relative standard deviation, RSD???10%). For most FAA and CAA the mean recoveries were >80% with RSD <10%. The GC-MS based method is useful for quality assurance of both FAA and CAA in cinobufacini injection. PMID:24924921

  1. 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.

  2. 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.

  3. 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.

  4. Gas-liquid transition in the model of particles interacting at high energy

    E-print Network

    S. Bondarenko; K. Komoshvili

    2013-10-07

    An application of the ideas of the inertial confinement fusion process in the case of particles interacting at high energy is investigated. A possibility of the gas-liquid transition in the gas is considered using different approaches. In particular, a shock wave description of interactions between particles is studied and a self-similar solution of Euler's equation is discussed. Additionally, Boltzmann equation is solved for self-consistent field (Vlasov's equation) in linear approximation for the case of a gas under external pressure and the corresponding change of Knudsen number of the system is calculated.

  5. Split of Gas-Liquid Two-Phase Flow at an Impacting Tee

    NASA Astrophysics Data System (ADS)

    Fujita, Isamu; Daiguji, Hirofumi; Sakai, Hitoshi; Hihara, Eiji

    Phase separation of gas-liquid two-phase flow at an impacting tee was investigated experimentally and theoretically. It was found that the phase separation did not occur, if the outlet branches were symmetrical and pressure drops in these branches were identical. On the other hand, if the flow rates in the branches were different, phase separation was observed. Based on the principle of minimum energy dissipation, a thermodynamic model was derived. The results of the model were qualitatively in good agreement with the experimental behavior of impacting flows.

  6. Identification of microorganisms based on headspace analysis of volatile organic compounds by gas chromatography-mass spectrometry.

    PubMed

    Boots, A W; Smolinska, A; van Berkel, J J B N; Fijten, R R R; Stobberingh, E E; Boumans, M L L; Moonen, E J; Wouters, E F M; Dallinga, J W; Van Schooten, F J

    2014-06-01

    The identification of specific volatile organic compounds (VOCs) produced by microorganisms may assist in developing a fast and accurate methodology for the determination of pulmonary bacterial infections in exhaled air. As a first step, pulmonary bacteria were cultured and their headspace analyzed for the total amount of excreted VOCs to select those compounds which are exclusively associated with specific microorganisms. Development of a rapid, noninvasive methodology for identification of bacterial species may improve diagnostics and antibiotic therapy, ultimately leading to controlling the antibiotic resistance problem. Two hundred bacterial headspace samples from four different microorganisms (Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus and Klebsiella pneumoniae) were analyzed by gas chromatography-mass spectrometry to detect a wide array of VOCs. Statistical analysis of these volatiles enabled the characterization of specific VOC profiles indicative for each microorganism. Differences in VOC abundance between the bacterial types were determined using ANalysis of VAriance-principal component analysis (ANOVA-PCA). These differences were visualized with PCA. Cross validation was applied to validate the results. We identified a large number of different compounds in the various headspaces, thus demonstrating a highly significant difference in VOC occurrence of bacterial cultures compared to the medium and between the cultures themselves. Additionally, a separation between a methicillin-resistant and a methicillin-sensitive isolate of S. aureus could be made due to significant differences between compounds. ANOVA-PCA analysis showed that 25 VOCs were differently profiled across the various microorganisms, whereas a PCA score plot enabled the visualization of these clear differences between the bacterial types. We demonstrated that identification of the studied microorganisms, including an antibiotic susceptible and resistant S. aureus substrain, is possible based on a selected number of compounds measured in the headspace of these cultures. These in vitro results may translate into a breath analysis approach that has the potential to be used as a diagnostic tool in medical microbiology. PMID:24737039

  7. Method developments approaches in supercritical fluid chromatography applied to the analysis of cosmetics.

    PubMed

    Lesellier, E; Mith, D; Dubrulle, I

    2015-12-01

    Analyses of complex samples of cosmetics, such as creams or lotions, are generally achieved by HPLC. These analyses are often multistep gradients, due to the presence of compounds with a large range of polarity. For instance, the bioactive compounds may be polar, while the matrix contains lipid components that are rather non-polar, thus cosmetic formulations are usually oil-water emulsions. Supercritical fluid chromatography (SFC) uses mobile phases composed of carbon dioxide and organic co-solvents, allowing for good solubility of both the active compounds and the matrix excipients. Moreover, the classical and well-known properties of these mobile phases yield fast analyses and ensure rapid method development. However, due to the large number of stationary phases available for SFC and to the varied additional parameters acting both on retention and separation factors (co-solvent nature and percentage, temperature, backpressure, flow rate, column dimensions and particle size), a simplified approach can be followed to ensure a fast method development. First, suited stationary phases should be carefully selected for an initial screening, and then the other operating parameters can be limited to the co-solvent nature and percentage, maintaining the oven temperature and back-pressure constant. To describe simple method development guidelines in SFC, three sample applications are discussed in this paper: UV-filters (sunscreens) in sunscreen cream, glyceryl caprylate in eye liner and caffeine in eye serum. Firstly, five stationary phases (ACQUITY UPC(2)) are screened with isocratic elution conditions (10% methanol in carbon dioxide). Complementary of the stationary phases is assessed based on our spider diagram classification which compares a large number of stationary phases based on five molecular interactions. Secondly, the one or two best stationary phases are retained for further optimization of mobile phase composition, with isocratic elution conditions or, when necessary, two-step gradient elution. The developed methods were then applied to real cosmetic samples to assess the method specificity, with regards to matrix interferences, and calibration curves were plotted to evaluate quantification. Besides, depending on the matrix and on the studied compounds, the importance of the detector type, UV or ELSD (evaporative light-scattering detection), and of the particle size of the stationary phase is discussed. PMID:26553956

  8. Highly sensitive analysis of flavonoids by zwitterionic microemulsion electrokinetic chromatography coupled with light-emitting diode-induced fluorescence detection.

    PubMed

    Cao, Wan; Hu, Shuai-Shuai; Li, Xing-Ying; Pang, Xiao-Qing; Cao, Jun; Ye, Li-Hong; Dai, Han-Bin; Liu, Xiao-Juan; Da, Jian-Hua; Chu, Chu

    2014-09-01

    A rapid zwitterionic microemulsion electrokinetic chromatography (ZI-MEEKC) approach coupled with light-emitting-diode-induced fluorescence (LED-IF, 480nm) detection was proposed for the analysis of flavonoids. In the optimization process, we systematically investigated the separation conditions, including the surfactants, cosurfactants, pH, buffers and fluorescence parameters. It was found that the baseline separation of the seven flavonoids was obtained in less than 5min with a running buffer consisting of 92.9% (v/v) 5mM sodium borate, 0.6% (w/v) ZI surfactant, 0.5% (w/v) ethyl acetate and 6.0% (w/v) 1-butanol. High sensitivity was obtained by the application of LED-IF detection. The limits of detection for seven flavonoids were in the range of 3.30×10(-8) to 2.15×10(-6)molL(-1) without derivatization. Ultimately, the detection method was successfully applied to the analysis of flavonoids in hawthorn plant and food products with satisfactory results. PMID:25047822

  9. Innovative microwave-assisted oximation and silylation procedures for metabolomic analysis of plasma samples using gas chromatography-mass spectrometry.

    PubMed

    Hong, Zhanying; Lin, Zebin; Liu, Yue; Tan, Guangguo; Lou, Ziyang; Zhu, Zhenyu; Chai, Yifeng; Fan, Guorong; Zhang, Junping; Zhang, Liming

    2012-09-01

    Analysis of plasma metabolomic samples by gas chromatography-mass spectrometry always requires comprehensive pretreatment including oximation and silylation. Although heating block (HB) is a commonly used method, it is time consuming. This study describes an extremely time-effective microwave-assisted (MA) oximation and silylation approach for metabolomic study of plasma samples. The Box-Behnken design was employed to optimize the MA conditions by means of oximation at 65 W for 100 s and then silylation through 180 s incubation with 230 W microwave irradiation. The results showed that microwave irradiation decreased the sample preparation time from approximately 180 min to 5 min without loss of information for the metabolites in plasma samples. Both the HB method and the developed MA method were applied in plasma metabolomic study of sulfur mustard intoxication. Partial least-squares discriminant analysis (PLS-DA) was used to globally understand the metabolic changes, and multi-criteria assessment was used to select the most significant and reliable variables as potential biomarkers. The data obtained by the MA method were in good correlation with the HB method. Compared with HB method, the newly developed MA oximation and silylation of plasma metabolome samples was more efficient and time-effective and may prove to be an attractive alternative for high-throughput sample preparation in plasma metabolomics. PMID:22841665

  10. A NEW METHOD OF PEAK DETECTION FOR ANALYSIS OF COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY MASS SPECTROMETRY DATA*

    PubMed Central

    Kim, Seongho; Ouyang, Ming; Jeong, Jaesik; Shen, Changyu; Zhang, Xiang

    2014-01-01

    We develop a novel peak detection algorithm for the analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) data using normal-exponential-Bernoulli (NEB) and mixture probability models. The algorithm first performs baseline correction and denoising simultaneously using the NEB model, which also defines peak regions. Peaks are then picked using a mixture of probability distribution to deal with the co-eluting peaks. Peak merging is further carried out based on the mass spectral similarities among the peaks within the same peak group. The algorithm is evaluated using experimental data to study the effect of different cut-offs of the conditional Bayes factors and the effect of different mixture models including Poisson, truncated Gaussian, Gaussian, Gamma, and exponentially modified Gaussian (EMG) distributions, and the optimal version is introduced using a trial-and-error approach. We then compare the new algorithm with two existing algorithms in terms of compound identification. Data analysis shows that the developed algorithm can detect the peaks with lower false discovery rates than the existing algorithms, and a less complicated peak picking model is a promising alternative to the more complicated and widely used EMG mixture models. PMID:25264474

  11. A NEW METHOD OF PEAK DETECTION FOR ANALYSIS OF COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY MASS SPECTROMETRY DATA.

    PubMed

    Kim, Seongho; Ouyang, Ming; Jeong, Jaesik; Shen, Changyu; Zhang, Xiang

    2014-06-01

    We develop a novel peak detection algorithm for the analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOF MS) data using normal-exponential-Bernoulli (NEB) and mixture probability models. The algorithm first performs baseline correction and denoising simultaneously using the NEB model, which also defines peak regions. Peaks are then picked using a mixture of probability distribution to deal with the co-eluting peaks. Peak merging is further carried out based on the mass spectral similarities among the peaks within the same peak group. The algorithm is evaluated using experimental data to study the effect of different cut-offs of the conditional Bayes factors and the effect of different mixture models including Poisson, truncated Gaussian, Gaussian, Gamma, and exponentially modified Gaussian (EMG) distributions, and the optimal version is introduced using a trial-and-error approach. We then compare the new algorithm with two existing algorithms in terms of compound identification. Data analysis shows that the developed algorithm can detect the peaks with lower false discovery rates than the existing algorithms, and a less complicated peak picking model is a promising alternative to the more complicated and widely used EMG mixture models. PMID:25264474

  12. Global analysis of chemical constituents in Shengmai injection using high performance liquid chromatography coupled with tandem mass spectrometry.

    PubMed

    Li, Fei; Cheng, Tao-Fang; Dong, Xin; Li, Ping; Yang, Hua

    2016-01-01

    This study aimed to develop a specific and reliable method to comprehensively analyze the chemical constituents in Shengmai injection (SMI) using high performance liquid chromatography coupled with tandem mass spectrometry. The qualitative analysis of SMI was achieved on a Kromasil 100-5C18 column, and the results demonstrated that a total of sixty-two compounds in SMI were unambiguously assigned or tentatively identified, and further, twenty-one compounds including fourteen saponins, six lignans and one l-borneol-7-O-[?-d-apiofuranosyl (1?6)]-?-d-gluco-pyranoside were quantified by HPLC-MS. Furthermore, l-borneol-7-O-[?-d-apio-furanosyl (1?6)]-?-d-glucopyranoside, originated from Radix ophiopogonis, was identified and quantified in SMI for the first time. The method validation results indicated that the methods were simple, specific and reliable. All the investigated compounds showed good linearity (r(2)?0.9992) with a relatively wide concentration range and acceptable recovery at 90.13-109.09%. Consequently, the developed methods were successfully applied to ten batches of SMI samples analysis. The proposed methods may provide a useful and comprehensive reference for the quality control of SMI, and thus to provide supporting data for the quality control and application of SMI clinically. PMID:26342447

  13. Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

    PubMed

    Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

    2012-01-01

    Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces). PMID:22391598

  14. Analysis of sulfonamides, trimethoprim, fluoroquinolones, quinolones, triphenylmethane dyes and methyltestosterone in fish and shrimp using liquid chromatography-mass spectrometry.

    PubMed

    Storey, Joseph M; Clark, Susan B; Johnson, Aaron S; Andersen, Wendy C; Turnipseed, Sherri B; Lohne, Jack J; Burger, Robert J; Ayres, Patrick R; Carr, Justin R; Madson, Mark R

    2014-12-01

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method is described for the detection and identification of 26 veterinary drugs in fish and other aquaculture products. The analytes include: 13 sulfonamides, trimethoprim, 3 fluoroquinolones, 3 quinolones, 3 triphenylmethane dyes, 2 leuco dye metabolites, and 1 hormone. In this method, tissue is mixed with EDTA-McIlvaine buffer, double-extracted with acetonitrile, p-toluenesulfonic (p-TSA) acid and N,N,N',N'-tetramethyl-p-phenylenediamine dihydrochloride (TMPD), and analyzed using LC-MS/MS. Inclusion of p-TSA and TMPD in the extraction procedure was critical for simultaneous analysis of dyes with the other groups of veterinary drugs. The proposed procedure was validated as both a quantitative analysis method and as a semi-quantitative screening method for multiple fish and shrimp matrices. The method was applied to eight types of fish (catfish, eel, pangasius, sablefish, tilapia, swai, salmon, and trout) and shrimp at the appropriate level of concern: 10ng/g for sulfonamides, trimethoprim, and quinolones, 5ng/g for fluoroquinolones, 1ng/g for dyes and their metabolites, and 0.4ng/g for methyltestosterone. PMID:25310706

  15. Hollow-fiber liquid phase microextraction for lignin pyrolysis acids in aerosol samples and gas chromatography-mass spectrometry analysis.

    PubMed

    Hyder, Murtaza; Jönsson, Jan Åke

    2012-08-01

    A method based on three-phase hollow fiber liquid phase microextraction was developed and successfully applied to aerosols for the analysis of lignin pyrolysis acids such as syringic acid, vanillic acid and p-salicylic acid. Important parameters related to extraction process like organic solvent for membrane phase, tri-n-octylphosphine (TOPO) oxide contents in organic solvent, stirring speed, extraction time etc. were optimized. 6-Undecanone with 15% TOPO contents (w/v) was found a suitable solvent for organic liquid membrane, 900 rpm was the optimum stirring speed and time of 4h was found optimum extraction time. Donor phase pH was 1.3 while acceptor phase pH was adjusted to 9.5. The optimized extraction method was used for the extraction of real aerosol samples. Analytes were derivatized using BSTFA containing 1% trimethylsilyl chloride and gas chromatography mass spectrometry was used for analysis. Very low limits of detection in the range 0.2-1.0 ng L(-1) were found, corresponding to 10-50 pg m(-3) of analytes in aerosols. Extraction efficiency obtained ranged 60.3-71.7% and enrichment factors ranged 3015-3585 times. The optimized method was successfully applied to aerosol samples and all of the selected analytes were detected in the analyzed samples. PMID:22749581

  16. Filtration efficiency validation of glass wool during thermal desorption-gas chromatography-mass spectrometer analysis of fine atmospheric particles.

    PubMed

    Hao, Liang; Wu, Dapeng; Ding, Kun; Meng, Hu; Yan, Xiaohui; Guan, Yafeng

    2015-02-01

    Thermal desorption-gas chromatography-mass spectrometer (TD-GC-MS) technique has been widely used for analysis of semi-violate organic compounds on atmospheric aerosol. To prevent GC column from being damaged by fine solid particles during thermal desorption process, glass wool as filter mat is indispensible. However, the filtration efficiency has never been validated. In this paper, the most penetrating particle size and the minimum packing thickness of glass wool were calculated based on classical filtration theory. According to the calculation results, packing parameters of glass wool were optimized experimentally using silica particles. It is demonstrated that glass wool with a packing thickness of 30 mm, solidity of 0.039 can effectively block these fine solid particles from penetrating at normal thermal desorption conditions (T=300°C, u=0.4-4 cm/s). Finally, the filtration efficiency of glass wool was further confirmed with real PM2.5 samples. Under the validated filtration condition, TD-GC-MS was applied for the analysis of non-polar organic compounds on real PM2.5 samples, and very good results were obtained. PMID:25578046

  17. Analysis of polystyrene-b-polyisoprene copolymers by coupling of liquid chromatography at critical conditions to NMR at critical conditions of polystyrene and polyisoprene.

    PubMed

    Sinha, Pritish; Hiller, Wolf; Bellas, Vasilios; Pasch, Harald

    2012-07-01

    For the investigation of the molecular heterogeneity of polystyrene-b-polyisoprene block copolymers, a chromatographic separation method, namely liquid chromatography at critical conditions was developed. This method was coupled on-line with (1)H-NMR(where NMR stands for nuclear magnetic resonance) for the comprehensive analysis of the polystyrene-b-polyisoprene copolymers. The copolymers were synthesized by two different methods: sequential living anionic polymerization and coupling of living precursor blocks. While (1)H-NMR allows just for the analysis of the bulk chemical composition of the block copolymers, the coupling with liquid chromatography at critical conditions provides selective molar mass information on the polystyrene and polyisoprene blocks within the copolymers. The polyisoprene block molar mass is determined by operating at chromatographic conditions corresponding to the critical point of adsorption of polystyrene and size exclusion chromatography mode for polyisoprene. The molar mass of the polystyrene block is determined by operating at the critical conditions of polyisoprene. In addition to the molar mass of each block of the copolymers, the chemical composition distribution of the block copolymers was determined. By using the coupling of liquid chromatography at critical conditions to (1)H-NMR, one can also detect the homopolymers formed during synthesis. Finally the microstructure of the polyisoprene block in the copolymers was evaluated as a function of molar mass. PMID:22707375

  18. High-Performance Liquid Chromatography

    NASA Astrophysics Data System (ADS)

    Reuhs, Bradley L.; Rounds, Mary Ann

    High-performance liquid chromatography (HPLC) developed during the 1960s as a direct offshoot of classic column liquid chromatography through improvements in the technology of columns and instrumental components (pumps, injection valves, and detectors). Originally, HPLC was the acronym for high-pressure liquid chromatography, reflecting the high operating pressures generated by early columns. By the late 1970s, however, high-performance liquid chromatography had become the preferred term, emphasizing the effective separations achieved. In fact, newer columns and packing materials offer high performance at moderate pressure (although still high pressure relative to gravity-flow liquid chromatography). HPLC can be applied to the analysis of any compound with solubility in a liquid that can be used as the mobile phase. Although most frequently employed as an analytical technique, HPLC also may be used in the preparative mode.

  19. Critical role of a pre-purge setup in the thermal desorption analysis of volatile organic compounds by gas chromatography with mass spectrometry.

    PubMed

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2015-07-01

    In general, volatile organic compounds in ambient air are quantified by following a well-defined standard calibration procedure using a gas-/liquid-phase standard. If the liquid standard is analyzed by a thermal desorption, the solvent effect is unavoidable through the alteration of breakthrough properties or retention times. To learn more about the variables of the thermal desorption-based analysis, the effect of pre-purge conditions was evaluated for 18 volatile organic compounds with different types of sorbent tube materials by fixing standard volume (1 ?L) and flow rate (100 mL/min). The gas phase calibration was also carried out as reference for the non-solvent effect. A single tube filled with Tenax TA exhibited the least solvent effect with the short pre-purge (1 min), while being subject to the breakthrough at or above 10 min pre-purge. For a three-bed sorbent tube with Carboxen 1000, at least 10 min of pre-purge was needed for the compounds with a retention time close to methanol (e.g., propanal). Another three-bed tube with Carbopack X reduced the solvent effect efficiently for a short pre-purge (2 min) without the breakthrough. As such, the solvent effect can be adjusted by the proper control of the sorbent tube application. PMID:25960339

  20. Determination of Synacthen(®) in dried blood spots for doping control analysis using liquid chromatography tandem mass spectrometry.

    PubMed

    Tretzel, Laura; Thomas, Andreas; Geyer, Hans; Delahaut, Philippe; Schänzer, Wilhelm; Thevis, Mario

    2015-06-01

    Dried blood spot (DBS) sampling, a technique used for taking whole blood samples dried on a filter paper, was initially reported in 1963 by Robert Guthrie. While the diagnostic analysis of metabolic disorders in newborns was the focus of investigations at that time, the number of established applications for preclinical drug development, toxicological studies, and therapeutic drug monitoring increased enormously in the last decades. As a consequence of speed, simplicity, and minimal invasiveness, DBS recommends itself as the preferential technique in sports drug testing. The present approach highlights for the first time the development of a screening assay for the analysis of the synthetic human adrenocorticotropic hormone tetracosactide hexaacetate (Synacthen(®)) in DBS using liquid chromatography tandem mass spectrometry. Highly purified sample extracts were obtained by an advanced sample preparation procedure including the addition of an internal standard (d8-tetracosactide) and immunoaffinity purification. The method's overall recovery was 27.6 %, and the assay's imprecision was calculated between 8.1 and 17.9 % for intraday and 12.9 to 20.5 % for interday measurements. Stability of the synthetic peptide in DBS was shown for at least 10 days at room temperature and presents a major benefit, since a rapid degradation in conventionally applied matrices such as urine or plasma is well known. With a limit of detection of 50 pg/mL, a detection window of several hours is expected considering reported steady-state plasma levels of 300 pg/mL after intramuscular application of Synacthen(®) Depot (1 mg). The analysis of authentic DBS samples within the scope of an administration study with 250 ?g Synacthen(®) (short stimulation test) demonstrated the great potential of the developed assay to simplify the analysis of Synacthen(®) for doping control purposes. PMID:25863802

  1. Headspace gas-liquid chromatographic determination of dithiocarbamate residues in fruits and vegetables with confirmation by conversion to ethylenethiourea.

    PubMed

    Ahmad, N; Guo, L; Mandarakas, P; Farah, V; Appleby, S; Gibson, T

    1996-01-01

    Ethylene-bis-dithiocarbamate (EBDC) residues were determined as carbon disulfide (CS2) by an improved headspace gas-liquid chromatographic (GLC) procedure. Among 837 samples of 30 agricultural commodities tested, 43% contained residues above the detection limit for the method: 100% of broccoli samples; 80% of cabbage, kiwifruit, and grape samples; and 71% of cucumber samples. Most of the residues in kiwifruit were on or near the skin. Elimination of false-positive detections by the improved method was confirmed with kiwifruit in 2 independent procedures. Whole fruits were washed with 5% EDTA to remove surface residues of EBDC. Analysis of washes for CS2 by the headspace procedure after treatment with acidic stannous chloride and for ethylene thiourea by LC after prolonged treatment at 60 degrees C qualitatively identified the EDTA-soluble residues as EBDC. Although the improved method does not produce false-positive results, peak area responses of CS2 and the internal standard, thiophene, are influenced by chemical composition of the matrix. With matrixes high in sugar or lipids, the apparent CS2 content may be overestimated by 4-fold. Accurate determination of EBDC residues in these sample types requires appropriate adjustments to matrixes. PMID:8946720

  2. High Throughput Quantitative Analysis of Serum Proteins using Glycopeptide Capture and Liquid Chromatography Mass Spectrometry

    SciTech Connect

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

    2005-02-01

    It is expected that the composition of the serum proteome can provide valuable information about the state of the human body in health and disease, and that this information can be extracted via quantitative proteomic measurements. Suitable proteomic techniques need to be sensitive, reproducible and robust to detect potential biomarkers below the level of highly expressed proteins, to generate data sets that are comparable between experiments and laboratories, and have high throughput to support statistical studies. In this paper, we report a method for high throughput quantitative analysis of serum proteins. It consists of the selective isolation of peptides that are N-linked glycosylated in the intact protein, the analysis of these, no de-glycosylated peptides by LC-ESI-MS, and the comparative analysis of the resulting patterns. By focusing selectively on a few formerly N-linked glycopeptides per serum protein, the complexity of the analyte sample is significantly reduced and the sensitivity and throughput of serum proteome analysis are increased compared with the analysis of total tryptic peptides from unfractionated samples. We provide data that document the performance of the method and show that sera from untreated normal mice and genetically identical mice with carcinogen induced skin cancer can be unambiguously discriminated using unsupervised clustering of the resulting peptide patterns. We further identify, by tandem mass spectrometry, some of the peptides that were consistently elevated in cancer mice compared to their control littermates.

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

  4. 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.

  5. Analysis of Fluorotelomer Alcohols in Soils: Optimization of Extraction and Chromatography

    EPA Science Inventory

    This article describes the development of an analytical method for the determination of fluorotelomer alcohols (FTOHs) in soil. The sensitive and selective determination of the telomer alcohols was performed by extraction with mthyl tert-butyl ether (MTBE) and analysis of the ext...

  6. Immobilized zirconium ion affinity chromatography for specific enrichment of phosphopeptides in phosphoproteome analysis.

    PubMed

    Feng, Shun; Ye, Mingliang; Zhou, Houjiang; Jiang, Xiaogang; Jiang, Xingning; Zou, Hanfa; Gong, Bolin

    2007-09-01

    Large scale characterization of phosphoproteins requires highly specific methods for purification of phosphopeptides because of the low abundance of phosphoproteins and substoichiometry of phosphorylation. Enrichment of phosphopeptides from complex peptide mixtures by IMAC is a popular way to perform phosphoproteome analysis. However, conventional IMAC adsorbents with iminodiacetic acid as the chelating group to immobilize Fe(3+) lack enough specificity for efficient phosphoproteome analysis. Here we report a novel IMAC adsorbent through Zr(4+) chelation to the phosphonate-modified poly(glycidyl methacrylate-co-ethylene dimethacrylate) polymer beads. The high specificity of Zr(4+)-IMAC adsorbent was demonstrated by effectively enriching phosphopeptides from the digest mixture of phosphoprotein (alpha- or beta-casein) and bovine serum albumin with molar ratio at 1:100. Zr(4+)-IMAC adsorbent was also successfully applied for the analysis of mouse liver phosphoproteome, resulting in the identification of 153 phosphopeptides (163 phosphorylation sites) from 133 proteins in mouse liver lysate. Significantly more phosphopeptides were identified than by the conventional Fe(3+)-IMAC approach, indicating the excellent performance of the Zr(4+)-IMAC approach. The high specificity of Zr(4+)-IMAC adsorbent was found to mainly result from the strong interaction between chelating Zr(4+) and phosphate group on phosphopeptides. Enrichment of phosphopeptides by Zr(4+)-IMAC provides a powerful approach for large scale phosphoproteome analysis. PMID:17575324

  7. PRECOLUMN SAMPLE ENRICHMENT DEVICE FOR ANALYSIS OF AMBIENT VOLATILE ORGANICS BY GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    Gas chromatographic-mass spectrometric (GC/MS) identification of air pollutants generally requires a preconcentration step to provide sufficient sample for analysis. Cryogenic trapping is often used to enrich the sample since nitrogen and oxygen are not condensed. It does, howeve...

  8. High-Pressure Liquid Chromatography: Quantitative Analysis of Chinese Herbal Medicine

    ERIC Educational Resources Information Center

    Chan, W. F.; Lin, C. W.

    2007-01-01

    An HPLC undergraduate experiment on the analysis of traditional Chinese medicine (TCM) has been developed. Two commonly used herbs ("glycyrrhizae radix" and "cinnamomi ramulus") are studied. Glycyrrhizin, cinnamic acid, and cinnamaldehyde are chosen as markers for the herbs. The dried herbs in their natural state and a TCM preparation in powder…

  9. Development and Application of Pyrolysis Gas Chromatography/Mass Spectrometry for the Analysis of Bound Trinitrotoluene Residues in Soil

    USGS Publications Warehouse

    Weiss, J.M.; Mckay, A.J.; Derito, C.; Watanabe, C.; Thorn, K.A.; Madsen, E.L.

    2004-01-01

    TNT (trinitrotoluene) is a contaminant of global environmental significance, yet determining its environmental fate has posed longstanding challenges. To date, only differential extraction-based approaches have been able to determine the presence of covalently bound, reduced forms of TNT in field soils. Here, we employed thermal elution, pyrolysis, and gas chromatography/mass spectrometry (GC/MS) to distinguish between covalently bound and noncovalently bound reduced forms of TNT in soil. Model soil organic matter-based matrixes were used to develop an assay in which noncovalently bound (monomeric) aminodinitrotoluene (ADNT) and diaminonitrotoluene (DANT) were desorbed from the matrix and analyzed at a lower temperature than covalently bound forms of these same compounds. A thermal desorption technique, evolved gas analysis, was initially employed to differentiate between covalently bound and added 15N-labeled monomeric compounds. A refined thermal elution procedure, termed "double-shot analysis" (DSA), allowed a sample to be sequentially analyzed in two phases. In phase 1, all of an added 15N-labeled monomeric contaminant was eluted from the sample at relatively low temperature. In phase 2 during high-temperature pyrolysis, the remaining covalently bound contaminants were detected. DSA analysis of soil from the Louisiana Army Ammunition Plant (LAAP; ???5000 ppm TNT) revealed the presence of DANT, ADNT, and TNT. After scrutinizing the DSA data and comparing them to results from solvent-extracted and base/acid-hydrolyzed LAAP soil, we concluded that the TNT was a noncovalently bound "carryover" from phase 1. Thus, the pyrolysis-GC/MS technique successfully defined covalently bound pools of ADNT and DANT in the field soil sample.

  10. Simultaneous optimization of the resolution and analysis time of flavonoids in reverse phase liquid chromatography using Derringer's desirability function.

    PubMed

    Hadjmohammadi, Mohammadreza; Sharifi, Vahid

    2012-01-01

    The chemometrics approach was applied for simultaneous optimization of resolution and analysis time of seven flavonoids in reverse phase liquid chromatography. Derringer's desirability function, a multi-criteria decision making method, was used for the evaluation of two different chromatographic performance goals including resolution and analysis time. The selected flavonoids belong to different classes of flavonoids including: flavonols (myricetin, morin, quercetin and kaempferol) flavones (apigenin and luteolin) and flavanones (naringenin). The effect of five experimental factors on a chromatographic response function, formed using two sigmoidal desirability functions, was investigated. The sigmoidal functions were used to transform the optimization criteria, resolution and analysis time, into the desirability values. The factors studied were percentages of methanol, phosphoric acid and THF in mobile phase as well as flow rate and temperature. A rotatable, orthogonal central composite design was used to map the chromatographic response surface and then calculated chromatographic response functions were fitted to a polynomial model. The obtained regression model was characterized by both descriptive and predictive ability (R(2)=0.96). The model was verified, as good agreement was observed between the predicted and experimental values of the chromatographic response function in the optimal condition. The most effective factor on retention of flavonoids was percentage of methanol in mobile phase followed by temperature, flow rate, THF and H(3)PO(4) percentages. Optimum condition for separation of flavonoids was as follows: methanol:0.4% phosphoric acid in water:THF (45.3:54.4:0.3, v/v/v) as mobile phase with flow rate of 1 mL min(-1) at 30°C. The optimum condition was applied for separation of flavonoids of Satureja sahendica Bornm. which is an endemic medicinal plant of Iran. PMID:22177786

  11. Discrimination of Wild Paris Based on Near Infrared Spectroscopy and High Performance Liquid Chromatography Combined with Multivariate Analysis

    PubMed Central

    Zhao, Yanli; Zhang, Ji; Yuan, Tianjun; Shen, Tao; Li, Wei; Yang, Shihua; Hou, Ying; Wang, Yuanzhong; Jin, Hang

    2014-01-01

    Different geographical origins and species of Paris obtained from southwestern China were discriminated by near infrared (NIR) spectroscopy and high performance liquid chromatography (HPLC) combined with multivariate analysis. The NIR parameter settings were scanning (64 times), resolution (4 cm?1), scanning range (10000 cm?1?4000 cm?1) and parallel collection (3 times). NIR spectrum was optimized by TQ 8.6 software, and the ranges 7455?6852 cm?1 and 5973?4007 cm?1 were selected according to the spectrum standard deviation. The contents of polyphyllin I, polyphyllin II, polyphyllin VI, and polyphyllin VII and total steroid saponins were detected by HPLC. The contents of chemical components data matrix and spectrum data matrix were integrated and analyzed by partial least squares discriminant analysis (PLS-DA). From the PLS-DA model of NIR spectrum, Paris samples were separated into three groups according to the different geographical origins. The R2X and Q2Y described accumulative contribution rates were 99.50% and 94.03% of the total variance, respectively. The PLS-DA model according to 12 species of Paris described 99.62% of the variation in X and predicted 95.23% in Y. The results of the contents of chemical components described differences among collections quantitatively. A multivariate statistical model of PLS-DA showed geographical origins of Paris had a much greater influence on Paris compared with species. NIR and HPLC combined with multivariate analysis could discriminate different geographical origins and different species. The quality of Paris showed regional dependence. PMID:24558477

  12. Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry.

    PubMed

    Chen, Fangfang; Gong, Zhiyuan; Kelly, Barry C

    2015-02-27

    A sensitive analytical method based on liquid-liquid extraction (LLE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for rapid analysis of 11 pharmaceuticals and personal care products (PPCPs) in fish plasma micro-aliquots (?20?L). Target PPCPs included, bisphenol A, carbamazepine, diclofenac, fluoxetine, gemfibrozil, ibuprofen, naproxen, risperidone, sertraline, simvastatin and triclosan. A relatively quicker and cheaper LLE procedure exhibited comparable analyte recoveries with solid-phase extraction. Rapid separation and analysis of target compounds in fish plasma extracts was achieved by employing a high efficiency C-18 HPLC column (Agilent Poroshell 120 SB-C18, 2.1mm×50mm, 2.7?m) and fast polarity switching, enabling effective monitoring of positive and negative ions in a single 9min run. With the exception of bisphenol A, which exhibited relatively high background contamination, method detection limits of individual PPCPs ranged between 0.15 and 0.69pg/?L, while method quantification limits were between 0.05 and 2.3pg/?L. Mean matrix effect (ME) values ranged between 65 and 156% for the various target analytes. Isotope dilution quantification using isotopically labelled internal surrogates was utilized to correct for signal suppression or enhancement and analyte losses during sample preparation. The method was evaluated by analysis of 20?L plasma micro-aliquots collected from zebrafish (Danio rerio) from a laboratory bioaccumulation study, which included control group fish (no exposure), as well as fish exposed to environmentally relevant concentrations of PPCPs. Using the developed LC-MS/MS based method, concentrations of the studied PPCPs were consistently detected in the low pg/?L (ppb) range. The method may be useful for investigations requiring fast, reliable concentration measurements of PPCPs in fish plasma. In particular, the method may be applicable for in situ contaminant biomonitoring, as well as bioaccumulation and toxicology studies employing small fishes with low blood compartment volumes. PMID:25640994

  13. Size analysis and stability study of lipid vesicles by high-performance gel exclusion chromatography, turbidity, and dynamic light scattering.

    PubMed

    Lesieur, S; Grabielle-Madelmont, C; Paternostre, M T; Ollivon, M

    1991-02-01

    Vesicles of egg phosphatidylcholine (EPC) and phosphatidic acid (EPA) were prepared by reverse-phase evaporation (REV) followed either by sequential extrusion through polycarbonate membranes with pore diameters of 0.8, 0.4, 0.2, 0.1, and 0.05 micron or by filtration through 0.8-micron cellulosic or 0.22-micron polyvinylidene fluoride (PVF) membranes. The resulting vesicles ranging from 130 to 640 nm in mean diameter (REVs) were characterized by high-performance liquid chromatography (HPLC) using a TSK G6000 PW gel exclusion column. The efficiency of this technique to determine vesicle size parameters was studied by the analysis of the chromatograms in combination with dynamic light scattering (DLS) determination of the mean diameters (MD) of the fractionated vesicles in the region of the elution profile maxima. The HPLC TSK G6000 PW gel exclusion provides a reproducible and fast method of size characterization for lipid vesicles having MD up to 1 micron, the best selectivity being obtained in the 20- to 500-nm MD range. HPLC analysis of REV's demonstrates that: (i) both the average size and polydispersity of the vesicles decrease with decreasing pore size of the membranes, cellulosic or PVF "tortuous" ones being less efficient than "straight bores" polycarbonate ones; (ii) mixed EPC/EPA REVs sequentially extruded down through 0.2-micron polycarbonate membranes are highly deformable without rupture of the bilayer; and (iii) the mean size of extruded REV's is stable for at least 1 week. The role of EPA on the size stability of mixed EPC/EPA vesicles was studied by coupling HPLC gel exclusion and turbidity analysis of pure EPC and EPC/EPA (mole ratio: 91/9) sonicated small unilamellar vesicles as a function of time. The apparent size variation of EPC vesicles observed over a week, is mainly due to their aggregation which is significantly reduced by the introduction of a small amount of EPA in the vesicle membrane. PMID:2035833

  14. A quick cogener specific analysis of polychlorinated biphenyls in municipal sludge utilizing ultrasonic extraction and capillary gas chromatography

    SciTech Connect

    Hughes, W.L.

    1994-12-31

    At the Madison Metropolitan Sewerage District (MMSD) land application is a routine procedure for recycling municipal digested sludge. In 1982 analyses performed by MMSD indicated some areas of the sludge storage lagoons had polychlorinated biphenyl (PCB) levels greater than 50 parts per million (ppm), the EPA established limit for unrestricted land application of sludge. Conflicting test results obtained from commercial laboratories prompted MMSD to find the most reliable test method and also maximize the amount of information received from each analysis. Therefore, an accurate and precise measurement of PCBs in sludge was desired on a daily and sometimes hourly basis. Analysis of sludge samples by soxhlet extraction (SW846 method 3540B) and capillary gas chromatography (GC) required overnight extraction, 2-3 hours extract cleanup and concentration, plus 3 hours elution time on a narrow bore column to achieve a congener specific analysis. A procedure to obtain congener specific PCB data in 2-2.5 hours was developed using ultrasonic extraction (SW846 method 3550B), florisil mini-cartridge cleanup and a 20-meter narrow bore column. Small homogeneous samples of sludge (2-4 grams) were mixed with the extracting solvent in a 50 mL centrifuge tube and then extracted using a sonic dismemberator in the pulsed mode. A 20-meter length was cut from a 60-meter, 0.25 mm i.d. capillary column. Resolution of some of the 95 congeners present was sacrificed to obtain a GC run time of 23 minutes. Sludges ranging from 2% to 30% solids were routinely analyzed with concentrations from detection limits to 200 ppm dry weight. Comparison of the sonication vs. soxhlet extractions exhibited no significant difference in the amount of PCBs recovered from various samples.

  15. Dual-Stage Consumable-Free Thermal Modulator for the Hyphenation of Thermal Analysis, Gas Chromatography, and Mass Spectrometry.

    PubMed

    Wohlfahrt, Sebastian; Fischer, Michael; Varga, Janos; Saraji-Bozorgzad, Mohammad-Reza; Matuschek, Georg; Denner, Thomas; Zimmermann, Ralf

    2016-01-01

    The design of the so-called "Peltier modulator" is presented. It is a new dual-stage consumable-free thermal modulator for thermal analysis-gas chromatography-mass spectrometry (TA-GC-MS). It requires only electrical power for operation as it facilitates thermo-electric coolers instead of cryogenics for trapping and resistive on-column heating for reinjection. Trapping and desorption temperatures as well as modulation cycles are freely adjustable. The stationary phase for the trapping region can be selected to suit the specific application, since common fused silica capillary is used. The Peltier modulator's performance is demonstrated with a broad range of different standard substances and with heavy crude oil as a complex real life sample. Successful modulation from n-pentane to pyrene (boiling points = 36/394 °C) is presented. The produced peaks show the narrowest bandwidths ever reported for a consumable-free thermal modulator, i.e., 12.8 ± 1.2 ms for n-pentadecane. The Peltier modulator is rugged, cost-effective, requires low maintenance, and decreases security issues significantly, compared to commercial available solutions using liquid N2/CO2. PMID:26606252

  16. ENVIRONMENTAL ANALYSIS BY ON-LINE IMMUNOEXTRACTION AND REVERSED-PHASE LIQUID CHROMATOGRAPHY: OPTIMIZATION OF THE IMMUNOEXTRACTION/RPLC INTERFACE

    PubMed Central

    Nelson, Mary Anne; Papastavros, Efthimia; Dodlinger, Maud; Hage, David S.

    2008-01-01

    The use of antibodies in HPLC columns for on-line immunoextraction combined with reversed-phase liquid chromatography (RPLC) is of growing interest in environmental and agricultural analysis. This technique is typically performed by using a small RPLC precolumn to capture and concentrate analytes as they elute from the immunoextraction column; however, there is little information on the conditions required for optimizing this interface. This study examined the behavior of this interface by using 2,4-dichlorophenoxyacetic acid (2,4-D) and related herbicides as model analytes. It was found that analyte dissociation from immunoextraction columns followed first-order decay and that the elution of these analytes through the immunoextraction/RPLC interface gave an exponentially-modified Gaussian profile. Computer simulations were used to see how analyte elution through the interface changed with different dissociation and retention conditions. Several guidelines were developed from this work that could be used for developing and optimizing on-line immunoextraction/RPLC systems for other chemicals of environmental or agricultural interest. PMID:17455948

  17. Post-Blast Analysis of Hexamethylene Triperoxide Diamine using Liquid Chromatography-Atmospheric Pressure Chemical Ionization-Mass Spectrometry.

    PubMed

    Marsh, Christine M; Mothershead, Robert F; Miller, Mark L

    2015-09-01

    A qualitative method using liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC/APCI-MS) has been developed and validated for the identification of trace hexamethylene triperoxide diamine (HMTD) using three structurally-specific ions. Residues are extracted with deionized water (DI) and identified using a gradient mobile phase program and positive ion full scan mode on a Thermo Finnigan LCQ Ion Trap Mass Spectrometer. This method was validated according to several performance characteristics for the qualitative identification of an analyte using the characteristic ions, demonstrating the method's reliability for use on forensic applications. The method's limit of detection (LOD) can identify HMTD in an extract from a cotton matrix to which 20 ?g of HMTD has been applied (equivalent to 10 ppm in extract). Previous scientific publications using LC/MS have not demonstrated post-blast HMTD residue analyses and suffer from a lack of chromatographic retention, sufficient number of mass spectral ions with validation, or require more complex/expensive instrumental methods (accurate mass or MS/MS). Post-blast analyses were successfully conducted with two syringe detonations that verified the efficacy of the method on the analysis of debris and residues following detonation. PMID:26385711

  18. Analysis and quantitation of rotenoids and flavonoids in Derris (Lonchocarpus urucu) by high-temperature high-resolution gas chromatography.

    PubMed

    Pereira, A S; Afonso Serrano, M A; Aquino Neto, F R; Cunha Pinto, A; Furtado Texeira, D; Gilbert, B

    2000-04-01

    A glass capillary column coated with PS-086 (15% phenyl-80% methylpolysiloxane, 15 m x 0.30-mm i.d., 0.1-microm film thickness) is used to analyze extracts from Lonchocarpus urucu (Derris urucu). Several secondary metabolites (8 flavonoids, 10 rotenoids) are characterized without derivatization, and the rotenoids are quantitated by high-temperature high-resolution gas chromatography (HTHRGC) and HTHRGC coupled with mass spectrometry (HTHRGC-MS). The limit of detection in flame ionization detection of rotenone is approximately 0.5 microg/mL, and the limit of quantitation was 2 microg/mL. Derris urucu bark is an excellent source of rotenone isomers (80 mg/g), deguelin (30 mg/g), and rotenolone (26 mg/g). Single solvent extractions (hexane, methylene dichloride, acetone, or methanol) are not able to fully extract the flavonoids and rotenoids. Complete extraction is achieved using a mixture of methanol-methylene dichloride (1:1), indicating a complex association of these compounds with the plant tissue. HTHRGC and HTHRGC-MS are shown to be quick and informative tools for the rapid analysis of crude extracts without the need for prior derivatization and fractionation. PMID:10766485

  19. Environmental analysis by on-line immunoextraction and reversed-phase liquid chromatography: optimization of the immunoextraction/RPLC interface.

    PubMed

    Nelson, Mary Anne; Papastavros, Efthimia; Dodlinger, Maud; Hage, David S

    2007-05-16

    The use of antibodies in HPLC columns for on-line immunoextraction combined with reversed-phase liquid chromatography (RPLC) is of growing interest in environmental and agricultural analysis. This technique is typically performed by using a small RPLC precolumn to capture and concentrate analytes as they elute from the immunoextraction column; however, there is little information on the conditions required for optimizing this interface. This study examined the behavior of this interface by using 2,4-dichlorophenoxyacetic acid (2,4-D) and related herbicides as model analytes. It was found that analyte dissociation from immunoextraction columns followed first-order decay and that the elution of these analytes through the immunoextraction/RPLC interface gave an exponentially modified Gaussian profile. Computer simulations were used to see how analyte elution through the interface changed with different dissociation and retention conditions. Several guidelines were developed from this work that could be used for developing and optimizing on-line immunoextraction/RPLC systems for other chemicals of environmental or agricultural interest. PMID:17455948

  20. Organophosphorus pesticide and ester analysis by using comprehensive two-dimensional gas chromatography with flame photometric detection.

    PubMed

    Liu, Xiangping; Li, Dengkun; Li, Jiequan; Rose, Gavin; Marriott, Philip J

    2013-12-15

    Thirty-seven phosphorus (P)-containing compounds comprising organophosphorus pesticides and organophosphate esters were analyzed by using comprehensive two-dimensional gas chromatography with flame photometric detection in P mode (GC × GC-FPD(P)), with a non-polar/moderately polar column set. A suitable modulation temperature and period was chosen based on experimental observation. A number of co-eluting peak pairs on the (1)D column were well separated in 2D space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC × GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021-0.048 ?mol L(-1), and linear calibration correlation coefficients (R(2)) for all 37 P-compounds were at least 0.998. The P-compounds were spiked in 2% diesel and good reproducibility for their response areas and retention times was obtained. Spiked recoveries were 88%-157% for 5 ?g L(-1) and 80%-138% for 10 ?g L(-1) spiked levels. Both (1)tR and (2)tR shifts were noted when the content of diesel was in excess of 5% in the matrix. Soil samples were analyzed by using the developed method; some P-compounds were positively detected. In general, this study shows that GC × GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples. PMID:24238476

  1. Micellar electrokinetic chromatography with amperometric detection and off-line solid-phase extraction for analysis of carbamate insecticides.

    PubMed

    Santalad, Apichai; Zhou, Lin; Shang, Fengjun; Fitzpatrick, Dara; Burakham, Rodjana; Srijaranai, Supalax; Glennon, Jeremy D; Luong, John H T

    2010-08-01

    Six selected primary carbamate insecticides, methomyl, carbaryl, carbofuran, propoxur, isoprocarb, and promecarb, were hydrolyzed in alkaline solution, resulting in electroactive derivatives detectable at a platinum (Pt) electrode poised at +0.8 V vs Ag/AgCl (3 M NaCl). The Pt electrode was inserted into a small electrochemical cell and positioned close to the capillary outlet as an end-column detector to detect the carbamate derivatives after electrophoretic separation. Based on their predicted pK(a) values and aqueous solubilities, micellar electrokinetic chromatography (MEKC) was optimized for baseline separation of the derivatives using 20 mM borate, pH 10.2 containing 20 mM sodium dodecyl sulfate as a running buffer. When combined with solid-phase extraction (SPE) on octadecyl silica, a preconcentration factor of 100-fold achieved detection to 0.5 microM methomyl and to 0.01 microM for the remaining five pesticides, significantly below the level regulated by government agencies of most countries. The SPE-MEKC method when applied to the separation and analysis of spiked river water and soil samples, yielded results with excellent reproducibility, recovery and selectivity. PMID:20598698

  2. Gas Chromatography-Mass Spectrometry Analysis of Ulva fasciata (Green Seaweed) Extract and Evaluation of Its Cytoprotective and Antigenotoxic Effects

    PubMed Central

    Rodeiro, Idania; Olguín, Sitlali; Santes, Rebeca; Herrera, José A.; Pérez, Carlos L.; Mangas, Raisa; Hernández, Yasnay; Fernández, Gisselle; Hernández, Ivones; Hernández-Ojeda, Sandra; Camacho-Carranza, Rafael; Valencia-Olvera, Ana; Espinosa-Aguirre, Jesús Javier

    2015-01-01

    The chemical composition and biological properties of Ulva fasciata aqueous-ethanolic extract were examined. Five components were identified in one fraction prepared from the extract by gas chromatography-mass spectrometry, and palmitic acid and its ethyl ester accounted for 76% of the total identified components. Furthermore, we assessed the extract's antioxidant properties by using the DPPH, ABTS, and lipid peroxidation assays and found that the extract had a moderate scavenging effect. In an experiment involving preexposition and coexposition of the extract (1–500?µg/mL) and benzo[a]pyrene (BP), the extract was found to be nontoxic to C9 cells in culture and to inhibit the cytotoxicity induced by BP. As BP is biotransformed by CYP1A and CYP2B subfamilies, we explored the possible interaction of the extract with these enzymes. The extract (25–50?µg/mL) inhibited CYP1A1 activity in rat liver microsomes. Analysis of the inhibition kinetics revealed a mixed-type inhibitory effect on CYP1A1 supersome. The effects of the extract on BP-induced DNA damage and hepatic CYP activity in mice were also investigated. Micronuclei induction by BP and liver CYP1A1/2 activities significantly decreased in animals treated with the extract. The results suggest that Ulva fasciata aqueous-ethanolic extract inhibits BP bioactivation and it may be a potential chemopreventive agent. PMID:26612994

  3. Quantitative analysis of cytokinins in plants by high performance liquid chromatography: electronspray ionization ion trap mass spectrometry.

    PubMed

    Chen, Weiqi; Gai, Ying; Liu, Shichang; Wang, Renxiao; Jiang, Xiangning

    2010-10-01

    The present paper introduces a highly sensitive and selective method for simultaneous quantification of 12 cytokinins (free form and their conjugates). The method includes a protocol of extraction with methanol/water/formic acid (15/4/1, v/v/v) to the micro-scale samples, pre-purification with solid phase extraction (SPE) cartridges of the extracts, separation with a high performance liquid chromatography (HPLC) and detection by an electrospray ionization ion trap mass spectrometry (ESI-Ion trap-MS) system in a consecutive ion monitoring (CRM) mode at the three stage fragmentation of mass spectrometry (MS(3) ). The lowest detection level of the cytokinins of the method reaches 0.1-2.0 pg with a very wide range of linear regression from 1-512 pg, at the coefficient factors of 0.98-0.99. The feasibility of this method has been proven in the application of the method to the analysis of the trace-amount contents of cytokinins in the micro-scale samples of various types of plant materials, such as aerial parts of rice and poplar leaves etc. 12 endogenous cytokinins had been identified and quantified in the plant tissues, with an acceptable relatively higher recovery rate from 40% to 70%. PMID:20883444

  4. [Fast analysis of common fatty acids in edible vegetable oils by ultra-performance convergence chromatography-mass spectrometry].

    PubMed

    Lin, Chunhua; Xie, Xianqing; Fan, Naili; Tu, Yuanhong; Chen, Yan; Liao, Weilin

    2015-04-01

    A fast analytical method for five common fatty acids in six edible vegetable oils was developed by ultra-performance convergence chromatography-mass spectrometry (UPC2-MS). The five fatty acids are palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid. Their contents in the corn oil, sunflower oil, soybean oil, tea oil, rapeseed oil and peanut oil were compared. The chromatographic separation was performed on an ACQUITY UPC2 BEH 2-EP column (100 mm x 2.1 mm, 1.7 µm) using the mobile phases of carbon dioxide and methanol/acetonitrile (1:1, v/v) with gradient elution. The separated compounds were detected by negative electrospray ionization ESF-MS. The results showed that the reasonable linearities were achieved for all the analytes over the range of 0.5-100 mg/L with the correlation coefficients (R2) of 0.9985-0.9998. The limits of quantification (S/N ? 10) of the five fatty acids were 0.15-0.50 mg/L. The recoveries of the five fatty acids at three spiked levels were in the range of 89.61%-108.50% with relative standard deviations of 0.69%-3.01%. The developed method showed high performance, good resolution and fast analysis for the underivatized fatty acids. It has been successfully used to detect the five fatty acids from corn oil, sunflower oil, soybean oil, tea oil rapeseed oil and peanut oil. PMID:26292410

  5. Electrospray photoionization (ESPI) liquid chromatography/mass spectrometry for the simultaneous analysis of cyclodextrin and pharmaceuticals and their binding interactions.

    PubMed

    Short, Luke C; Syage, Jack A

    2008-01-01

    We report on the use of a multimode electrospray ionization/atmospheric pressure photoionization source (ESI/APPI or ESPI for short) with liquid chromatography/mass spectrometry (LC/MS) to measure all components of a mixed-polarity liquid sample containing: (1) low-polarity component (hormone, pharmaceutical or sterol), (2) polar component (cyclodextrin substrate), and (3) bound polar complex. The ESPI source has several advantages over both single ESI and multimode electrospray ionization/chemical ionization (ESCI) analysis, including an enhanced bound-complex detection and better performance at lower solvent flow rates. Relative binding constants are determined with (i) ESI mode, resulting in relative R(ESI-MS) values, and (ii) both ESI and APPI modes, providing relative K(D) values. We find that low molecular-substitution (Ms) values of cyclodextrin, i.e., Ms = 0.4, preferentially bind to the low-polarity compounds tested. This investigation is intended to demonstrate the feasibility of ESPI as an additional tool for investigating mixed-polarity binding systems, providing mass-specific data for all solution components, both polar and non-polar. PMID:18215005

  6. High performance liquid chromatography coupled to mass spectrometry for profiling and quantitative analysis of folate monoglutamates in tomato.

    PubMed

    Tyagi, Kamal; Upadhyaya, Pallawi; Sarma, Supriya; Tamboli, Vajir; Sreelakshmi, Yellamaraju; Sharma, Rameshwar

    2015-07-15

    Folates are essential micronutrients for animals as they play a major role in one carbon metabolism. Animals are unable to synthesize folates and obtain them from plant derived food. In the present study, a high performance liquid chromatography coupled to mass spectrometric (HPLC-MS/MS) method was developed for the high throughput screening and quantitative analysis of folate monoglutamates in tomato fruits. For folate extraction, several parameters were optimized including extraction conditions, pH range, amount of tri-enzyme and boiling time. After processing the extract was purified using ultra-filtration with 10 kDa membrane filter. The ultra-filtered extract was chromatographed on a RP Luna C18 column using gradient elution program. The method was validated by determining linearity, sensitivity and recovery. This method was successfully applied to folate estimation in spinach, capsicum, and garden pea and demonstrated that this method offers a versatile approach for accurate and fast determination of different folate monoglutamates in vegetables. PMID:25722141

  7. Improvement of sugar analysis sensitivity using anion-exchange chromatography-electrospray ionization mass spectrometry with sheath liquid interface.

    PubMed

    Xu, Xian-Bing; Liu, Ding-Bo; Guo, Xiao Ming; Yu, Shu-Juan; Yu, Pei

    2014-10-31

    A novel interface that enables high-performance anion-exchange chromatography (HPAEC) to be coupled with electrospray ionization (ESI) mass spectrometry (MS) is reported. A sheath liquid consisting of 50mM NH4Ac in isopropanol with 0.05% acetic acid, infused at a flow rate of 3?L/min at the tip of the electrospray probe, requires less ESI source cleaning and promotes efficient ionization of mono- and di-carbohydrates. The results suggest that use of a sheath liquid interface rather than a T-joint allows volatile ammonium salts to replace non-volatile metal salts as modifiers for improving sugar ESI signals. The efficient ionization of mono- and di-carbohydrates in the ESI source is affected by the sheath liquid properties such as buffer concentration and type of organic solvent. HPAEC-ESI-MS was used for the analysis of monocarbohydrates in pectins, particularly co-eluted sugars, and the performance was evaluated. Addition of a make-up solution through the sheath liquid interface proved to be an efficient tool for enhancing the intensities of sugars analyzed using HPAEC-ESI-MS. PMID:25246101

  8. A combinatorial approach to studying protein complex composition by employing size-exclusion chromatography and proteome analysis.

    SciTech Connect

    Li, S.; Giometti, C.; Biosciences Division

    2007-07-01

    The genome sequences of numerous organisms are available now, but gene sequences alone do not provide sufficient information to accurately deduce protein functions. Protein function is largely dependent on the association of multiple polypeptide chains into large structures with interacting subunits that regulate and support each other. Therefore, the mapping of protein interaction networks in a physiological context is conducive to deciphering protein functions, including those of hypothetical proteins. Although several high-throughput methods to globally identify protein interactions have been reported in recent years, these approaches often have a high rate of nonspecific or artificial interactions detected. For instance, the fraction of false positives of the protein interactions identified by yeast two-hybrid assay has been predicted to be of the order of 50%. We have developed a strategy to globally map Bacillus subtilis protein-protein interactions in a physiological context by fractionating the cell lysates using size-exclusion chromatography (SEC), followed by proteome analysis. Components of both known and unknown protein complexes, multisubunits and multiproteins, have been identified using this strategy. In one case, the partners of the B. subtilis protein complex have been coexpressed in Escherichia coli, and the formation of the overexpressed protein complex has been further confirmed by a pull-down assay.

  9. Determination of disease biomarkers in Eucalyptus by comprehensive two-dimensional gas chromatography and multivariate data analysis.

    PubMed

    Hantao, Leandro Wang; Aleme, Helga Gabriela; Passador, Martha Maria; Furtado, Edson Luiz; Ribeiro, Fabiana Alves de Lima; Poppi, Ronei Jesus; Augusto, Fabio

    2013-03-01

    In this paper is reported the use of the chromatographic profiles of volatiles to determine disease markers in plants - in this case, leaves of Eucalyptus globulus contaminated by the necrotroph fungus Teratosphaeria nubilosa. The volatile fraction was isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography-fast quadrupole mass spectrometry (GC×GC-qMS). For the correlation between the metabolic profile described by the chromatograms and the presence of the infection, unfolded-partial least squares discriminant analysis (U-PLS-DA) with orthogonal signal correction (OSC) were employed. The proposed method was checked to be independent of factors such as the age of the harvested plants. The manipulation of the mathematical model obtained also resulted in graphic representations similar to real chromatograms, which allowed the tentative identification of more than 40 compounds potentially useful as disease biomarkers for this plant/pathogen pair. The proposed methodology can be considered as highly reliable, since the diagnosis is based on the whole chromatographic profile rather than in the detection of a single analyte. PMID:23394740

  10. Aromatic profile of ciders by chemical quantitative, gas chromatography-olfactometry, and sensory analysis.

    PubMed

    Antón, María José; Suárez Valles, Belén; García Hevia, Ana; Picinelli Lobo, Anna

    2014-01-01

    Nine samples of Asturias cider have been analyzed for volatile, olfactometric, and sensorial profiles. The aromatic composition was mainly constituted by fusel alcohols and ethyl esters. Among the minor volatile compounds, fatty acids, volatile phenols, and alcohols were the main components. The olfactometric analysis revealed the existence of 55 aromatic areas, exhibiting a wide range of intensities. Components like amyl alcohols, 2-phenylethanol, ethyl esters such as 2-methylbutyrate, hexanoate and octanoate, hexanoic and octanoic acids 2-phenylethyl acetate, 4-ethyl guaiacol, and 4-ethyl phenol could be considered as being part of the structure of cider aroma. The extract dilution analysis of one extract identified 2 volatile phenols (4-ethyl guaiacol and 4-ethyl phenol) among the most powerful odorants in cider. These components gave significant correlations with the sensory attributes sweet, spicy, and lees. PMID:24313985

  11. Fast analysis of nicotine related alkaloids in tobacco and cigarette smoke by megabore capillary gas chromatography.

    PubMed

    Cai, Jibao; Liu, Baizhan; Lin, Ping; Su, Qingde

    2003-10-31

    A novel fast megabore capillary gas chromatographic (MCGC) method for analysis of 7 nicotine related alkaloids in tobacco and cigarette smoke, including nicotine, nornicotine, myosmine, nicotyrine, anabasine, anatabine and 2,3-dipyridyl, was developed. The use of megabore capillary column GC methodology, equipped with flame ionization detector (FID), provided rapid, unambiguous nicotine related alkaloids analysis. One gram flue-cured tobacco (or Cambridge filter pad), 20 ml ether, and 5 ml 10% sodium hydroxide solution, added with n-heptadecane as the internal standard, were placed in a flask, and the flask was capped and placed in an ultrasonic bath for 15 min. A 1 microl volume was analyzed by capillary GC operating in split-injection mode on a mega bore Simplicity-5 column. This simple procedure was compared with the previously reported packed column GC method and the Griffith still-colorimetric method. The application of the method for analysis of various flue-cured tobaccos and cigarette smoke was discussed. PMID:14584703

  12. Improved gas chromatography-flame ionization detector analytical method for the analysis of epoxy fatty acids.

    PubMed

    Mubiru, Edward; Shrestha, Kshitij; Papastergiadis, Antonios; De Meulenaer, Bruno

    2013-11-29

    In this study an improved method for analysis of epoxy fatty acids is reported. Data obtained from analysis of polar fatty acids has previously been presented, but due to the high number of compounds that co-elute in the polar fraction, the resultant chromatograms are complex which may lead to compromising the accuracy of the data. A three steps separation of fatty acid methyl esters (FAMEs) by solid-phase extraction (SPE) on a silica gel column to remove hydroxy fatty acid interferences was proposed. This approach is opposed to a two step separation procedure that has been often used to prevent analytical interferences caused by non-altered fatty acids. A gas chromatograph with a flame ionization detector (GC-FID) equipped with a polar CP-Sil 88™ column was used. Quantification was based on the use of methyl nonadecanoate (C19:0), as an internal standard. Individual mono epoxy fatty acids were well separated without co-eluting compounds. The optimized method was finally applied to screen epoxy fatty acids in 37 fresh oil samples. Results obtained for the total epoxy fatty acids were in the range 0.03-2mgg(-1) of oil with repeatability coefficient of variation (CV) ranging from 2.8 to 9.9% for duplicate analysis showing that the results obtained are repeatable. PMID:24161147

  13. Analysis of lignocellulose derived phenolic monomers by headspace solid-phase microextraction and gas chromatography.

    PubMed

    Kolb, Michaela; Schieder, Doris; Faulstich, Martin; Sieber, Volker

    2013-09-13

    A headspace solid-phase microextraction method with subsequent GC-MS (HS-SPME/GC-MS) was established for the quantitative analysis of volatile lignin derived phenolic monomers in complex aqueous solutions. Extraction was done using a polyacrylate fiber. The optimization of HS-SPME - parameters was performed using a multi component model solution of six representative phenolic monomers identified in liquid hot water (LHW) supernatants of hydrothermally treated lignocellulosic biomass: p-coumaric acid, guaiacol, vanillin, acetosyringone, 4-hydroxy-3-methoxyphenylacetone, and acetophenone. Plackett-Burman design was applied for pre-evaluation and 2(3) central composite designs with star points for parameter optimization. LOQ (S/N>10) and LOD (S/N>3) were determined for 12 phenols yielding LOQ of <0.005-618nM and LOD of <0.005-412nM. Within-day and between-day tests (n=6) showed different results for the tested phenols. RSD ranged from 2% to 30% and recovery rates from 99% to 160% in LHW matrix. Tests on storage of LHW supernatants for several weeks indicated a considerable influence of temperature on the stability of the solutions which may even have to be taken into account for auto sampler handling. All in all the method allows a fast and solvent free analysis requiring low sample volumes making it a powerful tool for screening or high-throughput analysis of aqueous solutions of lignin derived aromatics. PMID:23932028

  14. Immunoassay for acetamiprid detection: application to residue analysis and comparison with liquid chromatography.

    PubMed

    Watanabe, Eiki; Miyake, Shiro; Baba, Koji; Eun, Heesoo; Endo, Shozo

    2006-11-01

    This work describes the fundamental ability of a commercial ELISA to determine acetamiprid and the application of the ELISA to residue analysis in fruit and vegetable samples. The ELISA exhibited satisfactory sensitivity (I (50) 0.6 ng/g; limit of detection 0.053 ng/g) and a high selectivity for acetamiprid versus other neonicotinoid analogs (thiacloprid amide). Methanol, which influenced the sensitivity of the ELISA the least, was selected as the extractant for the ELISA analysis. Simple dilution of sample extracts with water eliminated matrix interferences. Average recoveries from the acetamiprid-spiked agricultural samples were >95% using a simple extraction method. Analytical results obtained from the ELISA were comparable to those obtained from the reference HPLC method (r>0.99). The ELISA applied to the residue analysis of acetamiprid in agricultural products is a rapid, simple, and cost-effective method, and could be successfully applied to the detection of acetamiprid before the distribution of produce. PMID:16917672

  15. [Analysis of part of flavor compounds in wheat by headspace sorptive extraction-gas chromatography].

    PubMed

    Wang, Tongbo; Yan, Xiao; Lan, Xiaozheng

    2013-05-01

    A method has been established for the analysis of flavor compounds in wheat by headspace sorptive extraction (HSSE). The sorptive extraction bar was composed of a silicon rubber coating and a capillary glass with an inner iron rod. The silicon rubber coating was condensed inside a stainless steel mold from the silicon precursors with a sol-hot air vulcanization method. The coating of the extraction bar has a volume of about 87 microL and is thermally stable until 390 degrees C. The flavor compounds extracted by the bar were desorbed in a homemade thermal desorption unit (TDU) and introduced directly into a pre-column in a gas chromatograph for analysis. Experimental parameters for the extraction efficiency were optimized including extraction temperature and time, phase ratio and thermal desorption conditions. The standard wheat flour samples spiked with seven flavor compounds were analyzed under the optimized conditions, and showed good linear relationships (r > 0.9979), limits of detection (LOD) of 0.09 - 1.00 microg/kg, good recoveries (95% - 121%) and repeatabilities (relative standard deviations, RSD, 2.2% - 7.8%). By external calibration method, the absolute contents of the seven flavor compounds in a real wheat sample were determined. The method is rapid, simple with low limits of detection, and is applicable for the rapid quantitative analysis of the flavor compounds in wheat. PMID:24010348

  16. ANALYSIS OF FLAVONOIDS AND HYROXYCINNAMATES IN CITRUS PROCESSING BYPRODUCTS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY-ELECTROSPRAY IONIZATION-MASS SPECTROMETRY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Electrospray ionization-high performance liquid chromatography-mass spectrometry (ESI-HPLC-MS) greatly facilitates analyses of the complex phenolic constituents of citrus peel and associated citrus processing byproducts. The numerous flavonoid glycosides and polymethoxylated flavones (PMFs) in thes...

  17. DIRECT ANALYSIS OF RAT BILE FOR ACETAMINOPHEN AND TWO OF ITS CONJUGATED METABOLITES VIA THERMOSPRAY LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    Bile from rats treated with acetaminophen was analyzed by direct injection onto a thermospray liquid chromatography/mass spectrometry system. Two conjugated metabolites of acetaminophen were separated by the high-pressure liquid chromatographic system and analyzed by mass spectro...

  18. Study on flow-pattern identification method using pressure drop characteristics of gas-liquid flow in narrow channel

    NASA Astrophysics Data System (ADS)

    Konishi, Tatsunori; Yoshida, Kenji; Kataoka, Isao

    2012-03-01

    To clarify flow-pattern of gas-liquid two-phase flow in narrow channel is important because flow-pattern of gas-liquid two-phase flow relates closely to better working of industrial products like polymer electrolyte fuel cell (PEFC), µ-TAS, small size of fuel assembly, or cooling system of small electronic devices. Moreover, gas-liquid two-phase flow in narrow channel is different from that in usual size channel, including standard inch pipe, better knowledge of flow-pattern leads to more performance and operating safety in such products. However, flow-pattern has been mostly identified to observe visible image. Therefore, it is necessary to identified flow-pattern without making inside visible because of safety or cost performance. As the identification of flow-pattern method, it uses us pressure drop fluctuations in narrow channel.

  19. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group; determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry

    USGS Publications Warehouse

    Zimmerman, L.R.; Hostetler, K.A.; Thurman, E.M.

    2000-01-01

    Analytical methods using high-performance liquid chromatography-diode array detection (HPLC-DAD) and high-performance liquid chromatography/mass spectrometry (HPLC/MS) were developed for the analysis of the following chloroacetanilide herbicide metabolites in water: acetochlor ethanesulfonic acid (ESA), acetochlor oxanilic acid (OXA), alachlor ESA, alachlor OXA, metolachlor ESA, and metolachlor OXA. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The mean HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.50, and 2.0 mg/L (micrograms per liter) ranged from 84 to 112 percent, with relative standard deviations of 18 percent or less. The mean HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.20, and 2.0 mg/L ranged from 81 to 125 percent, with relative standard deviations of 20 percent or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 mg/L, whereas the LOQ using the HPLC/MS method was 0.05 mg/L. These metabolite-determination methods are valuable for acquiring information about water quality and the fate and transport of the parent chloroacetanilide herbicides in water.

  20. The analysis of illicit methaqualone containing preparations by gas chromatography-mass spectrometry for forensic purposes.

    PubMed

    Grové, Alida A; Rohwer, Egmont R; Laurens, Johannes B; Vorster, Barend C

    2006-03-01

    A validated gas chromatographic-mass spectrometric method for quantitative analysis of methaqualone (MTQ) in illicit preparations is reported. The method proved to have a coefficient of variation of below 5%. Four batches of seized tablets, two pairs with similar imprints, were analyzed. It was found that the average MTQ concentration in all four batches of tablets differed significantly (p = 0.01) rendering it impossible to conclude that, on the basis of MTQ concentration alone, the batches with a similar logo originated from the same manufacturer or manufacturing batch. Conversely, it can be said that in this case, the four batches originated from either different clandestine laboratories or manufacturing batches. PMID:16566774

  1. Applications of a simultaneous atomic emission mass spectral gas chromatography detector in drug analysis.

    PubMed

    Hooker, D B; Dezwaan, J

    1989-01-01

    For gas chromatographic eluents a microwave induced plasma (MIP) emission detector has two important features for a wide range of nonmetals. These features are (1) elemental selectivity and (2) the ability to determine elemental composition. These capabilities, used individually or in combination, can provide important information which is largely complementary to mass spectral data. Simultaneous determination of the MIP emission and mass spectral data for individual chromatographic peaks can be very useful in resolving a variety of problems encountered in pharmaceutical analysis. Several of these possible applications are illustrated with specific examples. PMID:2490548

  2. Analysis of polar pesticides in rainwater in Denmark by liquid chromatography-tandem mass spectrometry.

    PubMed

    Bossi, R; Vejrup, K V; Mogensen, B B; Asman, W A H

    2002-05-24

    A new LC-MS-MS method for analysis of rainwater has been developed and validated for 53 pesticides, degradation products of pesticides and selected nitrophenols. The method was used to monitor the concentration of pesticides in rainwater at one location near Roskilde, Denmark from February 2000 to August 2000. Sampling was done in periods of up to 4 weeks using a cooled wet-only sampler. Water samples were extracted by solid-phase extraction on Oasis HLB columns. The analysis of the extracts was performed by LC-MS-MS with electrospray ionization. All samples were analysed in negative and in positive ionization mode, respectively for acidic and neutral compounds. All analyses were done in the selected reaction monitoring mode in order to obtain a better signal-to-noise ratio. The method has been validated for the following parameters: recovery, detection limit, uncertainty and linearity. Atrazine, terbuthylazine, isoproturon, mechlorprop and (2-methyl-4-chlorophenoxy)acetic acid were measured at concentrations above 0.100 microg/l, mainly during the period of agricultural use. Nitrophenols were measured at high concentrations all year with peaks in the cold season (February-March). PMID:12102309

  3. Carbon isotopic analysis of atmospheric methane by isotope-ratio-monitoring gas chromatography-mass spectrometry

    NASA Technical Reports Server (NTRS)

    Merritt, Dawn A.; Hayes, J. M.; Des Marais, David J.

    1995-01-01

    Less than 15 min are required for the determination of delta C(sub PDB)-13 with a precision of 0.2 ppt(1 sigma, single measurement) in 5-mL samples of air containing CH4 at natural levels (1.7 ppm). An analytical system including a sample-introduction unit incorporating a preparative gas chromatograph (GC) column for separation of CH4 from N2, O2, and Ar is described. The 15-min procedure includes time for operation of that system, high-resolution chromatographic separation of the CH4, on-line combustion and purification of the products, and isotopic calibration. Analyses of standards demonstrate that systematic errors are absent and that there is no dependence of observed values of delta on sample size. For samples containing 100 ppm or more CH4, preconcentration is not required and the analysis time is less than 5 min. The system utilizes a commercially available, high-sensitivity isotope-ratio mass spectrometer. For optimal conditions of smaple handling and combustion, performance of the system is within a factor of 2 of the shot-noise limit. The potential exists therefore for analysis of samples as small as 15 pmol CH4 with a standard deviation of less than 1 ppt.

  4. Analysis of 26-hydroxycholesterol in plasma by high performance liquid chromatography

    SciTech Connect

    Kou, I.L.; Holmes, R.P.

    1986-03-01

    A method utilizing HPLC has been developed for the analysis of 26-hydroxycholesterol in plasma. The method involves initially saponifying samples for estimation of the total sterol or extracting samples with acetonitrile to estimate the free sterol. This is followed by a C-18 Sep Pak fractionation of the extracts, further purification on a Nova Pak C-18 HPLC column, and finally by quantitation on a silicic acid HPLC column by measuring the absorbance at 210 nm. Losses of sterol during this multi-step procedure were determined by estimating the recovery of /sup 3/H-26-hydroxycholesterol added to samples before extraction or saponification. The reproducibility of the method was evaluated by repetitive analysis of one plasma sample. The coefficient of variation was 6.8% for six analyses. In agreement with the mass spectrometric determinations of Javitt et al. The authors observed total plasma levels in the range of 140-260 ng/ml in young adult humans, rats, and rabbits. In the plasma of older human patients undergoing coronary by-pass surgery levels ranged from 335-950 ng/ml, suggesting that an increase in the level of 26-hydroxycholesterol is either age-related or related to the development of acute atherosclerosis.

  5. Quantitative analysis of phytosterols in edible oils using APCI liquid chromatography-tandem mass spectrometry

    PubMed Central

    Mo, Shunyan; Dong, Linlin; Hurst, W. Jeffrey; van Breemen, Richard B.

    2014-01-01

    Previous methods for the quantitative analysis of phytosterols have usually used GC-MS and require elaborate sample preparation including chemical derivatization. Other common methods such as HPLC with absorbance detection do not provide information regarding the identity of the analytes. To address the need for an assay that utilizes mass selectivity while avoiding derivatization, a quantitative method based on LC-tandem mass spectrometry (LC-MS-MS) was developed and validated for the measurement of six abundant dietary phytosterols and structurally related triterpene alcohols including brassicasterol, campesterol, cycloartenol, ?-sitosterol, stigmasterol, and lupeol in edible oils. Samples were saponified, extracted with hexane and then analyzed using reversed phase HPLC with positive ion atmospheric pressure chemical ionization tandem mass spectrometry and selected reaction monitoring. The utility of the LC-MS-MS method was demonstrated by analyzing 14 edible oils. All six compounds were present in at least some of the edible oils. The most abundant phytosterol in all samples was ?-sitosterol, which was highest in corn oil at 4.35 ± 0.03 mg/g, followed by campesterol in canola oil at 1.84 ± 0.01 mg/g. The new LC-MS-MS method for the quantitative analysis of phytosterols provides a combination of speed, selectivity and sensitivity that exceed those of previous assays. PMID:23884629

  6. Quantitative analysis of pesticide residues in vegetables and fruits by liquid chromatography quadrupole time-of-flight mass spectrometry.

    PubMed

    Saito-Shida, Shizuka; Nemoto, Satoru; Teshima, Reiko; Akiyama, Hiroshi

    2016-01-01

    The applicability of liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for the quantitative analysis of pesticide residues in vegetables and fruits was demonstrated. The LC-QTOF-MS parameters, such as cone voltage, capillary voltage, collision energy and mass extraction window, were carefully optimised for the analysis of pesticide residues. The LC-QTOF-MS method was validated for 149 pesticides in four vegetables and fruits, i.e. apple, potato, cabbage and spinach, at a spiking level of 0.01 mg kg(-1). The samples were prepared according to the Japanese official multi-residue method with a modification to the column clean-up procedure. Of the 149 pesticides, recoveries in the range of 70-120% were achieved for 147 pesticides in apple, 145 in potato, 141 in cabbage and 131 in spinach, with intra-day precisions (RSDs) of < 25% and inter-day precisions (RSDs) of < 30%, which are within the acceptable range given in the Japanese method validation guideline. Matrix effects were negligible for the majority of the target pesticides. Except for spiroxamine in spinach, no interfering peaks were observed in the blank samples. The target pesticides, except those with low sensitivity, achieved calibration curves with satisfactory linearity, with correlation coefficients (r) greater than 0.995 in the concentration range of 0.002-0.1 ?g ml(-1). Furthermore, the majority of the target pesticides provided more than one fragment ion or isotope ion that could be used for confirmation. The overall results suggest that LC-QTOF-MS is a powerful tool for the quantification of pesticide residues in vegetables and fruits at the level of 0.01 mg kg(-1). PMID:26479897

  7. Development of an efficient extraction method for oxytetracycline in animal manure for high performance liquid chromatography analysis.

    PubMed

    Yuan, Shoujun; Wang, Qiquan; Yates, Scott R; Peterson, Nyles G

    2010-10-01

    Oxytetracycline (2-(amino-hydroxy-methylidene)-4-dimethylamino-5,6,10,11,12a-pentahydroxy-6-methyl-4,4a,5,5a-tetrahydrotetracene-1,3,12-trione) is a major member of the tetracycline antibiotics family of which are widely administered to animals in concentrated animal feeding operations for purposes of therapeutical treatment and health protection. With the disposal of animal manure as fertilizer into agricultural land, tetracyclines enter the environment. However, tetracyclines chelate with multivalent cations and proteins, resulting in low extraction efficiencies from animal manure for tetracycline residue analysis. In this study an efficient extraction method for oxytetracycline from steer manure using methanol/water solution amended with chelating organic acid was developed for the analysis of high performance liquid chromatography. The effect of species and amount of amendment acids, shaking time, methanol/water ratio, manure weight, and repeated times of extraction was investigated. It was optimized to amend 2.5 g citric acid and 1.1 g oxalic acid with 10.0 g manure sample in a 50-ml centrifuge tube and extract with 15 ml methanol/water (9:1 in volume) by vigorously shaking for 30 min in a reciprocating shaker. After centrifugation at 11,000 rpm, supernatant is collected. Sample was extracted for a total of 3 times. The developed extraction method was further applied to extract oxytetracycline from fresh and aged cow manure, swine and poultry manure, and soil. Satisfactory recoveries ranging from (84.1 +/- 2.4) % to (102.0 +/- 3.1) % were obtained, demonstrating that the optimized extraction method is robust for oxytetracycline from different manure sample matrixes. PMID:20803364

  8. Ultra high performance liquid chromatography tandem mass spectrometry for rapid analysis of trace organic contaminants in water

    PubMed Central

    2013-01-01

    Background The widespread utilization of organic compounds in modern society and their dispersion through wastewater have resulted in extensive contamination of source and drinking waters. The vast majority of these compounds are not regulated in wastewater outfalls or in drinking water while trace amounts of certain compounds can impact aquatic wildlife. Hence it is prudent to monitor these contaminants in water sources until sufficient toxicological data relevant to humans becomes available. A method was developed for the analysis of 36 trace organic contaminants (TOrCs) including pharmaceuticals, pesticides, steroid hormones (androgens, progestins, and glucocorticoids), personal care products and polyfluorinated compounds (PFCs) using a single solid phase extraction (SPE) technique with ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The method was applied to a variety of water matrices to demonstrate method performance and reliability. Results UHPLC-MS/MS in both positive and negative electrospray ionization (ESI) modes was employed to achieve optimum sensitivity while reducing sample analysis time (<20 min) compared with previously published methods. The detection limits for most compounds was lower than 1.0 picogram on the column while reporting limits in water ranged from 0.1 to 15 ng/L based on the extraction of a 1 L sample and concentration to 1 mL. Recoveries in ultrapure water for most compounds were between 90-110%, while recoveries in surface water and wastewater were in the range of 39-121% and 38-141% respectively. The analytical method was successfully applied to analyze samples across several different water matrices including wastewater, groundwater, surface water and drinking water at different stages of the treatment. Among several compounds detected in wastewater, sucralose and TCPP showed the highest concentrations. Conclusion The proposed method is sensitive, rapid and robust; hence it can be used to analyze a large variety of trace organic compounds in different water matrixes. PMID:23777604

  9. Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry.

    PubMed

    González-Curbelo, Miguel Ángel; Lehotay, Steven J; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Ángel

    2014-09-01

    The "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) approach to sample preparation is widely applied in pesticide residue analysis, but the use of magnesium sulfate and other nonvolatile compounds for salting out in the method is not ideal for mass spectrometry. In this study, we developed and evaluated three new different versions of the QuEChERS method using more volatile salts (ammonium chloride and ammonium formate and acetate buffers) to induce phase separation and extraction of 43 representative pesticide analytes of different classes. Fast low-pressure gas chromatography tandem mass spectrometry (LPGC-MS/MS) and liquid chromatography (LC)-MS/MS were used for analysis. The QuEChERS AOAC Official Method 2007.01 was also tested for comparison purposes. Of the studied methods, formate buffering using 7.5g of ammonium formate and 15mL of 5% (v/v) formic acid in acetonitrile for the extraction of 15g of sample (5g for wheat grain) provided the best performance and practical considerations. Method validation was carried out with and without the use of dispersive solid-phase extraction for cleanup, and no significant differences were observed for the majority of pesticides. The method was demonstrated in quantitative analysis for GC- and LC-amenable pesticides in 4 representative food matrices (apple, lemon, lettuce, and wheat grain). With the typical exceptions of certain pH-dependent and labile pesticides, 90-110% recoveries and <10% RSD were obtained. Detection limits were mostly <5ng/g, which met the general need to determine pesticide concentrations as low as 10ng/g for monitoring purposes in food applications. PMID:25047819

  10. Analysis of the thermal reaction products of para polyphenylene by combined gas chromatography-mass spectrometry

    NASA Technical Reports Server (NTRS)

    Fewell, L. L.

    1976-01-01

    Analysis of the volatiles and sublimate produced when para-polyphenylene is pyrolyzed to constant weight under vacuum in the temperature range from 380 to 1000 C indicates that the polymer undergoes thermal degradation in two stages. The first stage involved dehydrohalogenation, which is essentially a curing reaction that produces crosslinking between polyphenylene chains resulting from the loss of chlorine from the polymer in the form of hydrogen chloride. The second stage of the thermal degradation is dehydrogenation because hydrogen is the major volatile species. Increasing amounts of polycyclic aromatic hydrocarbons (phenanthrene and 9, 10 benzphenanthrene) in the sublimate, concomitant with increasing C/H ratios of the polymeric residue with pyrolysis temperature, is consistent with the buildup of polynuclear structures in the polymer matrix.

  11. An experimental study of gas-liquid slug flow in vertical and inclined tubes using high speed motion analyzer

    SciTech Connect

    Xia, G.; Zhou, F.; Hu, M.

    1996-12-31

    Experimental investigation was carried out for gas-liquid slug flow in vertical and inclined tubes. The non-invasive measurements of the gas-liquid slug flow were taken by using the EKTAPRO 1000 High Speed Motion Analyzer. The present paper has obtained the information on the velocity of the Taylor bubble, the size distribution of the dispersed bubbles in the liquid slugs and some characteristics of the liquid film around the Taylor bubble. The experimental results are in good agreement with the available data.

  12. Gas chromatography-mass spectroscopy analysis of bioactive petalostigma extracts: Toxicity, antibacterial and antiviral activities

    PubMed Central

    Kalt, F. R.; Cock, I. E.

    2014-01-01

    Background: Petalostigma pubescens and Petalostigma triloculare were common components of pharmacopeia's of multiple Australian Aboriginal tribal groupings which traditionally inhabited the areas in which they grow. Among these groups, they had a myriad of medicinal uses in treating a wide variety of bacterial, fungal and viral infections. This study was undertaken to test P. pubescens and P. triloculare leaf and fruit extracts for the ability to inhibit bacterial and viral growth and thus validate Australian Aboriginal usage of these plants in treating bacterial and fungal diseases. Materials and Methods: P. pubescens, and P. triloculare leaves and fruit were extracted and tested for antimicrobial, antiviral activity and toxicity. The bioactive extracts were further examined by RP-HPLC and GC-MS to identify the component compounds. Results: The methanol, water and ethyl acetate leaf and fruit extracts of displayed potent antibacterial activity. The methanol and ethyl acetate extracts displayed the broadest specificity, inhibiting the growth of 10 of the 14 bacteria tested (71%) for the leaf extract and 9 of the 14 bacteria tested (64%) for the fruit extracts. The water extracts also had broad spectrum antibacterial activity, inhibiting the growth of 8 (57%) and 7 (50%) of the 14 bacteria tested, respectively. All antibacterial extracts were approximately equally effective against Gram-positive and Gram-negative bacteria, inhibiting the growth of 50-75% of the bacteria tested. The methanol, water and ethyl acetate extracts also displayed antiviral activity in the MS2 plaque reduction assay. The methanol and water extracts inhibited 26.6-49.0% and 85.4-97.2% of MS2 plaque formation, respectively, with the fruit extracts being more potent inhibitors. All ethyl acetate extracts inhibited 100% of MS2 plaque formation. All extracts were also non-toxic or of low toxicity. Analysis of these extracts by RP-HPLC showed that the P. triloculare ethyl acetate fruit extract was the least complex of the bioactive extracts. Subsequent analysis of this extract by GC-MS revealed that it contained 9 main compounds: acetic acid; 2,2-dimethoxybutane; 4-methyl-1,3-dioxane; decane; unadecane; 2-furanmethanol; 1,2-benzenediol; 1,2,3-benzenetriol; and benzoic acid. Conclusion: These studies validate Australian Aboriginal therapeutic usage of Petalostigma species and indicate their medicinal potential. PMID:24914307

  13. Study of the interdependency of the data sampling ratio with retention time alignment and principal component analysis for gas chromatography.

    PubMed

    Nadeau, Jeremy S; Wilson, Ryan B; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

    2011-12-16

    An in-depth study is presented to better understand how data reduction via averaging impacts retention alignment and the subsequent chemometric analysis of data obtained using gas chromatography (GC). We specifically study the use of signal averaging to reduce GC data, retention time alignment to correct run-to-run retention shifting, and principal component analysis (PCA) to classify chromatographic separations of diesel samples by sample class. Diesel samples were selected because they provide sufficient complexity to study the impact of data reduction on the data analysis strategies. The data reduction process reduces the data sampling ratio, S(R), which is defined as the number of data points across a given chromatographic peak width (i.e., the four standard deviation peak width). Ultimately, sufficient data reduction causes the chromatographic resolution to decrease, however with minimal loss of chemical information via the PCA. Using PCA, the degree of class separation (DCS) is used as a quantitative metric. Three "Paths" of analysis (denoted A-C) are compared to each other in the context of a "benchmark" method to study the impact of the data sampling ratio on preserving chemical information, which is defined by the DCS quantitative metric. The benchmark method is simply aligning data and applying PCA, without data reduction. Path A applies data alignment to collected data, then data reduction, and finally PCA. Path B applies data reduction to collected data, and then data alignment, and finally PCA. The optimized path, namely Path C, is created from Paths A and B, whereby collected data are initially reduced to fewer data points (smaller S(R)), then aligned, and then further reduced to even fewer points and finally analyzed with PCA to provide the DCS metric. Overall, following Path C, one can successfully and efficiently classify chromatographic data by reducing to a S(R) of ?15 before alignment, and then reducing down to S(R) of ?2 before performing PCA. Indeed, following Path C, results from an average of 15 different column length-with-temperature ramp rate combinations spanning a broad range of separation conditions resulted in only a ?15% loss in classification capability (via PCA) when the loss in chromatographic resolution was ?36%. PMID:22055520

  14. DETERMINATION OF FREE CATECHOLAMINES IN URINE BY TANDEM AFFINITY/ION-PAIR CHROMATOGRAPHY AND FLOW INJECTION ANALYSIS

    PubMed Central

    Thomas, David H.; Taylor, Jay D.; Barnaby, Omar S.; Hage, David S.

    2008-01-01

    Background A system was developed for the simultaneous measurement in urine of free catecholamines (i.e., dopamine, norepinephrine, epinephrine) and creatinine (i.e., an indicator of urine output and volume). This method was based on the use of tandem affinity/ion-pair HPLC and flow injection analysis. Methods The free catecholamines were extracted directly from urine by using an on-line phenylboronic acid affinity column. The extracted solutes were then separated and measured by ion-pair chromatography followed by amperometric detection. Creatinine was measured by an on-line flow injection analysis system based on the Jaffe reaction, which analyzed creatinine as it eluted non-retained from the phenylboronic acid column. Results Various factors were considered in the design and optimization of the phenylboronic acid column, the tandem affinity/ion-pair HPLC columns and the flow injection analysis system. The total analysis time for the final combined system was approximately 16 min per injection at 1 ml/min. This method was found to have good agreement with the expected results for control urine samples. The limits of detection for 20 ?l samples (S/N = 3.0) were 1.8, 1.0 and 4.3 ?g/l for norepinephrine, epinephrine and dopamine, respectively, while the limit of detection of creatinine was 5.0 mg/l. The linear response of this method extended over a 450 to 930-fold range in concentration for the catecholamines and covered the range of clinical interest. The within-day precision of this method was ±2.0?2.7%. Conclusions The ability of this method to simultaneously monitor both creatinine and other analytes makes this HPLC/FIA system an attractive method for use in monitoring urinary compounds. With this approach it was possible to provide fast results for small volumes of random urine samples that were collected as part of a psychological study. The same method could also be utilized with 12 or 24 h urine specimens. PMID:18773884

  15. Gas chromatography/ion mobility spectrometry as a hyphenated technique for improved explosives detection and analysis

    NASA Technical Reports Server (NTRS)

    Mercado, AL; Marsden, Paul

    1995-01-01

    Ion Mobility Spectrometry (IMS) is currently being successfully applied to the problem of on-line trace detection of plastic and other explosives in airports and other facilities. The methods of sample retrieval primarily consist of batch sampling for particulate residue on a filter card for introduction into the IMS. The sample is desorbed into the IMS using air as the carrier and negative ions of the explosives are detected, some as an adduct with a reagent ion such as Cl(-). Based on studies and tests conducted by different airport authorities, this method seems to work well for low vapor pressure explosives such as RDX and PETN, as well as TNT that are highly adsorptive and can be found in nanogram quantities on contaminated surfaces. Recently, the changing terrorist threat and the adoption of new marking agents for plastic explosives has meant that the sample introduction and analysis capabilities of the IMS must be enhanced in order to keep up with other detector developments. The IMS has sufficient analytical resolution for a few threat compounds but the IMS Plasmogram becomes increasingly more difficult to interpret when the sample mixture gets more complex.

  16. Analysis of fatty acid samples by hydrophilic interaction liquid chromatography and charged aerosol detector.

    PubMed

    Roy, Claude-Eric; Kauss, Tina; Prevot, Sandrine; Barthelemy, Philippe; Gaudin, Karen

    2015-02-27

    HILIC/CAD techniques were used in analysis of samples containing fatty acids. Amine base column appeared to be the more retentive stationary phase compared to zwitterionic and BEH silica. The retention decreased with pH mobile phases changing from 3 to 5. Acetonitrile and acetone organic modifier were compared. Acetone gave higher eluotropic strength and better peak symmetry whereas acetonitrile led to higher efficiency. The retention decreased when ammonium acetate concentration increased from 5 to 20mM. The use of sub-2?m column did not show flat Van Deemter curves at high flow rates. A rapid separation of PGI2 and its main degradation product, 6-keto prostaglandin F1? was obtained in 1.6min with a Hypersil GOLD, 50mm×2.1mm, 1.9?m with; acetonitrile/acetate ammonium pH 5 at 20mM (85/15; v/v at 0.7ml/min). PMID:25638266

  17. Targeted Chiral Analysis of Bioactive Arachidonic Acid Metabolites Using Liquid-Chromatography-Mass Spectrometry

    PubMed Central

    Mesaros, Clementina; Blair, Ian A.

    2012-01-01

    A complex structurally diverse series of eicosanoids arises from the metabolism of arachidonic acid. The metabolic profile is further complicated by the enantioselectivity of eicosanoid formation and the variety of regioisomers that arise. In order to investigate the metabolism of arachidonic acid in vitro or in vivo, targeted methods are advantageous in order to distinguish between the complex isomeric mixtures that can arise by different metabolic pathways. Over the last several years this targeted approach has become more popular, although there are still relatively few examples where chiral targeted approaches have been employed to directly analyze complex enantiomeric mixtures. To efficiently conduct targeted eicosanoid analyses, LC separations are coupled with collision induced dissociation (CID) and tandem mass spectrometry (MS/MS). Product ion profiles are often diagnostic for particular regioisomers. The highest sensitivity that can be achieved involves the use of selected reaction monitoring/mass spectrometry (SRM/MS); whereas the highest specificity is obtained with an SRM transitions between an intense parent ion, which contains the intact molecule (M) and a structurally significant product ion. This review article provides an overview of arachidonic acid metabolism and targeted chiral methods that have been utilized for the analysis of the structurally diverse eicosanoids that arise. PMID:24957514

  18. Combined multivariate data analysis of high-performance thin-layer chromatography fingerprints and direct analysis in real time mass spectra for profiling of natural products like propolis.

    PubMed

    Morlock, Gertrud E; Ristivojevic, Petar; Chernetsova, Elena S

    2014-02-01

    Sophisticated statistical tools are required to extract the full analytical power from high-performance thin-layer chromatography (HPTLC). Especially, the combination of HPTLC fingerprints (image) with chemometrics is rarely used so far. Also, the newly developed, instantaneous direct analysis in real time mass spectrometry (DART-MS) method is perspective for sample characterization and differentiation by multivariate data analysis. This is a first novel study on the differentiation of natural products using a combination of fast fingerprint techniques, like HPTLC and DART-MS, for multivariate data analysis. The results obtained by the chemometric evaluation of HPTLC and DART-MS data provided complementary information. The complexity, expense, and analysis time were significantly reduced due to the use of statistical tools for evaluation of fingerprints. The approach allowed categorizing 91 propolis samples from Germany and other locations based on their phenolic compound profile. A high level of confidence was obtained when combining orthogonal approaches (HPTLC and DART-MS) for ultrafast sample characterization. HPTLC with selective post-chromatographic derivatization provided information on polarity, functional groups and spectral properties of marker compounds, while information on possible elemental formulae of principal components (phenolic markers) was obtained by DART-MS. PMID:24440096

  19. 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.

  20. Unit operations for gas-liquid mass transfer in reduced gravity environments

    NASA Technical Reports Server (NTRS)

    Pettit, Donald R.; Allen, David T.

    1992-01-01

    Basic scaling rules are derived for converting Earth-based designs of mass transfer equipment into designs for a reduced gravity environment. Three types of gas-liquid mass transfer operations are considered: bubble columns, spray towers, and packed columns. Application of the scaling rules reveals that the height of a bubble column in lunar- and Mars-based operations would be lower than terrestrial designs by factors of 0.64 and 0.79 respectively. The reduced gravity columns would have greater cross-sectional areas, however, by factors of 2.4 and 1.6 for lunar and Martian settings. Similar results were obtained for spray towers. In contract, packed column height was found to be nearly independent of gravity.

  1. Control and ultrasonic actuation of a gas-liquid interface in a microfluidic chip

    E-print Network

    Jie Xu; Daniel Attinger

    2009-12-15

    This article describes the design and manufacturing of a microfluidic chip, allowing for the actuation of a gas-liquid interface and of the neighboring fluid. A first way to control the interface motion is to apply a pressure difference across it. In this case, the efficiency of three different micro-geometries at anchoring the interface is compared. Also, the critical pressures needed to move the interface are measured and compared to theoretical result. A second way to control the interface motion is by ultrasonic excitation. When the excitation is weak, the interface exhibits traveling waves, which follow a dispersion equation. At stronger ultrasonic levels, standing waves appear on the interface, with frequencies that are half integer multiple of the excitation frequency. An associated microstreaming flow field observed in the vicinity of the interface is characterized. The meniscus and associated streaming flow have the potential to transport particles and mix reagents.

  2. Amphiphilic polymeric micelle as pseudostationary phase in electrokinetic chromatography for analysis of eight corticosteroids in cosmetics.

    PubMed

    Xu, Xiaojin; Ni, Xinjiong; Cao, Yuhua; Zhuo, Xiaolu; Yang, Xiaoxiao; Cao, Guangqun

    2014-03-01

    Amphiphilic polymeric micelle, as a novel pseudostationary phase in EKC was used to determine eight kinds of corticosteroids namely hydrocortisone, prednisolone, hydrocortisone acetate, prednisone, cortisone acetate, prednisolone acetate, dexamethasone, and triamcinolone acetonide in cosmetics. Amphiphilic random copolymer poly(methyl methacrylate-co-methacrylic acid) (P(MMA-co-MAA)) was micellizated via neutralization in alkaline aqueous solution. The influences of the molar ratio of monomer MMA to MAA, the concentration of polymer and pH on the polymeric micelle microstructure and EKC performances were investigated. As molar ratio of MMA to MAA in P(MMA-co-MAA) increased, both CMC and environmental polarity of the inner core in polymeric micelle decreased dramatically. With increasing monomer ratio, the size of polymeric micelles increased firstly, and then decreased, finally increased again. ? potential of the micelle had a slight decline trend. As increment of polymer concentration, the size of the polymeric micelle increased steadily. By optimizing the monomer ratio, the polymer concentration, and pH of the running buffer, as well as operation conditions such as separation voltage and temperature, the eight analytes could be separated within 16.5 min using 7.5 mg/mL polymer with the monomer ratio of 7:3 dissolved in pH 9.2 borax buffer as the running buffer. The method has been used for analysis of corticosteroids in cosmetic samples with simple extraction; the recoveries for eight analytes were between 85.9 and 106%. This method was of accuracy, repeatability, pretreatment simplicity, and could be applied to the quality control of cosmetics. PMID:24338855

  3. Analysis of pesticide residues by fast gas chromatography in combination with negative chemical ionization mass spectrometry.

    PubMed

    Húsková, Renáta; Matisová, Eva; Hrouzková, Svetlana; Svorc, Lubomír

    2009-08-28

    A combination of fast GC with narrow-bore column and bench top quadrupole mass spectrometer (MS) detector in negative chemical ionization (NCI) mode (with methane as reagent gas) is set up and utilized for the ultratrace analysis of 25 selected pesticides. The observed pesticides, belonging to the endocrine disrupting chemicals (EDCs), were from different chemical classes. A comparative study with electron impact (EI) ionization was also carried out (both techniques in selected ion monitoring (SIM) mode). The programmed temperature vaporizer (PTV) injector in solvent vent mode and narrow-bore column (15mx0.15mm I.D.x0.15microm film of 5% diphenyl 95% dimethylsiloxane stationary phase) were used for effective and fast separation. Heptachlor (HPT) as internal standard (I.S.) was applied for the comparison of results obtained from absolute and normalized peak areas. Non-fatty food matrices were investigated. Fruit (apple - matrix-matched standards; orange, strawberry, plum - real samples) and vegetable (lettuce - real sample) extracts were prepared by a quick and effective QuEChERS sample preparation technique. Very good results were obtained for the characterization of fast GC-NCI-MS method analysing EDCs pesticides. Analyte response was linear from 0.01 to 150microgkg(-1) with the R(2) values in the range from 0.9936 to 1.0000 (calculated from absolute peak areas) and from 0.9956 to 1.0000 (calculated from peak areas normalized to HPT). Instrument limits of detection (LODs) and quantification (LOQs) were found at pgmL(-1) level and for the majority of analytes were up to three orders of magnitude lower for NCI compared to EI mode. In both ionization modes, repeatability of measurements expressed as relative standard deviation (RSDs) was less than 10% which is in very good agreement with the criterion of European Union. PMID:19643423

  4. Microstructure of microemulsion modified with ionic liquids in microemulsion electrokinetic chromatography and analysis of seven corticosteroids.

    PubMed

    Ni, Xinjiong; Yu, Meijuan; Cao, Yuhua; Cao, Guangqun

    2013-09-01

    In this work, the influences of ionic liquid (IL) as a modifier on microemulsion microstructure and separation performance in MEEKC were investigated. Experimental results showed that synergetic effect between IL 1-butyl-3-methylimidazolium tetrafluoro-borate (BmimBF4 ) and surfactant SDS gave a decreased CMC. With increment of IL in microemulsion, negative ? potential of the microdroplets reduced gradually. The influence of IL on the dimensions of microdroplet was complicated. At BmimBF4 less than 8 mM, IL made microemulsion droplet smaller in size. While at BmimBF4 more than 10 mM, the size increased and reached to a maximum value at 12 mM, where the microdroplets were larger than that without IL. After that, the micreodroplet size decreased again. Relative fluorescence intensity of the first vibration band of pyrene to the third one (I1 /I3 ) enhanced as IL was added to microemulsion, which indicated that this addition increased environmental polarity in the inner core of microdroplets. Prednisone, hydrocortisone, prednisolone, hydrocortisone acetate, cortisone acetate, prednisolone acetate, and triamcinolone acetonide were analyzed with MEEKC modified with IL to evaluate the separation performance. Cortisone acetate and prednisolone acetate could not be separated at all in typical microemulsion. The seven analytes could be separated by the addition of 10 mM BmimBF4 into the microemulsion system. The method has been used for analysis of corticosteroids in cosmetic samples with simple extraction; the recoveries for seven analytes were between 86 and 114%. This method provides accuracy, reproducibility, pretreatment simplicity, and could be applied to the quality control of cosmetics. PMID:23801369

  5. DESIGN AND DEVELOPMENT OF GAS-LIQUID CYLINDRICAL CYCLONE COMPACT SEPARATORS FOR THREE-PHASE FLOW

    SciTech Connect

    Dr. Ram S. Mohan; Dr. Ovadia Shoham

    2003-06-25

    The U.S. Department of Energy (DOE) has awarded a five-year (1997-2002) grant (Mohan and Shoham, DE-FG26-97BC15024, 1997) to The University of Tulsa, to develop compact multiphase separation components for 3-phase flow. The research activities of this project have been conducted through cost sharing by the member companies of the Tulsa University Separation Technology Projects (TUSTP) research consortium and the Oklahoma Center for the Advancement of Science and Technology (OCAST). As part of this project, several individual compact separation components have been developed for onshore and offshore applications. These include gas-liquid cylindrical cyclones (GLCC{copyright}), liquid-liquid cylindrical cyclones (LLCC{copyright}), and the gas-liquid-liquid cylindrical cyclones (GLLCC{copyright}). A detailed study has also been completed for the liquid-liquid hydrocyclones (LLHC). Appropriate control strategies have been developed for proper operation of the GLCC{copyright} and LLCC{copyright}. Testing of GLCC{copyright} at high pressure and real crude conditions for field applications is also completed. Limited studies have been conducted on flow conditioning devices to be used upstream of the compact separators for performance improvement. This report presents a brief overview of the activities and tasks accomplished during the 5-year project period, October 1, 1997-March 31, 2003 (including the no-cost extended period of 6 months). An executive summary is presented initially followed by the tasks of the 5-year budget periods. Then, detailed description of the experimental and modeling investigations are presented. Subsequently, the technical and scientific results of the activities of this project period are presented with some discussions. The findings of this investigation are summarized in the ''Conclusions'' section, followed by relevant references. The publications resulting from this study in the form of MS Theses, Ph.D. Dissertation, Journal Papers and Conference Presentations are provided at the end of this report.

  6. 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.

  7. Gas chromatography-triple-quadrupole mass spectrometry for analysis of selected polyhalogenated pollutants in plants. Comparison of extraction methods.

    PubMed

    Pérez, Rosa Ana; Tadeo, José Luis; Albero, Beatriz; Miguel, Esther; Sánchez-Brunete, Consuelo

    2013-01-01

    Different extraction methods, followed by gas chromatography coupled to triple quadrupole mass spectrometry, were evaluated for simultaneous extraction of seven polychlorinated biphenyls (PCBs) and six polybrominated diphenyl ethers (PBDEs) from common weeds. Pressurized liquid extraction (PLE) with in-cell clean-up, ultrasound-assisted extraction (UAE) with in-column clean-up, and UAE with dispersive solid-phase extraction (dSPE) clean-up were evaluated and compared. In-cell clean-up with 4 g Florisil and 0.5 g graphitized carbon black (GCB) and two extraction cycles of 10 min with n-hexane-ethyl acetate 80:20 (v/v) at 60 °C were used for the PLE procedure. UAE with in-column clean-up was conducted under conditions similar to those reported for the PLE method whereas in UAE with dSPE clean-up purification of the extract was performed after extraction using primary and secondary amine sorbent (PSA) and GCB. Recovery from 82 to 104% was obtained for all the compounds by PLE whereas, in general, lower extraction efficiency was obtained by UAE with in-column clean-up (especially for BDE-17 and BDE-183, for which recovery was 70 and 41%, respectively) and by UAE with dSPE clean-up, for which the main drawback is that BDE-183 cannot be extracted. Finally, PLE was used for analysis of PCBs and PBDEs in different plants (Lolium rigidum, Lactuca serriola, Malva sylvestris, and Verbascum thapsus) collected from residential and/or rural areas of Madrid (Spain). Several of the analyzed compounds were detected at low levels in these plants, but only PCB-153 could be quantified. PMID:23070044

  8. An automated gas chromatography time-of-flight mass spectrometry instrument for the quantitative analysis of halocarbons in air

    NASA Astrophysics Data System (ADS)

    Obersteiner, F.; Bönisch, H.; Engel, A.

    2015-09-01

    We present the characterization and application of a new gas chromatography-time-of-flight mass spectrometry instrument (GC-TOFMS) for the quantitative analysis of halocarbons in air samples. The setup comprises three fundamental enhancements compared to our earlier work (Hoker et al., 2015): (1) full automation, (2) a mass resolving power R = m/? m of the TOFMS (Tofwerk AG, Switzerland) increased up to 4000 Th/Th and (3) a fully accessible data format of the mass spectrometric data. Automation in combination with the accessible data allowed an in-depth characterization of the instrument. Mass accuracy was found around 5 ppm after automatic recalibration of the mass axis in each measurement. A TOFMS configuration giving R = 3500 was chosen to provide an R-to-sensitivity ratio suitable for our purpose. Calculated detection limits were as low as a few femtograms as mass traces could be made highly specific for selected molecule fragments with the accurate mass information. The precision for substance quantification was 0.15 % at the best for an individual measurement and in general mainly determined by the signal-to-noise ratio of the chromatographic peak. The TOFMS was found to be linear within a concentration range from about 1 pg to 1 ng of analyte per Liter of air. At higher concentrations, non-linearities of a few percent were observed (precision level: 0.2 %) but could be attributed to a potential source within the detection system. A straight-forward correction for those non-linearities was applied in data processing, again by exploiting the accurate mass information. Based on the overall characterization results, the GC-TOFMS instrument was found to be very well-suited for the task of quantitative halocarbon trace gas observation and a big step forward compared to scanning, low resolution quadrupole MS and a TOFMS technique reported to be non-linear and restricted by a small dynamical range.

  9. Analysis of inorganic nitrogen and related anions in high salinity water using ion chromatography with tandem UV and conductivity detectors.

    PubMed

    Wilson, Brian; Gandhi, Jay; Zhang, Chunlong Carl

    2011-09-01

    Over 97% of the Earth's water is high salinity water in the form of gulfs, oceans, and salt lakes. There is an increasing concern for the quality of water in bays, gulfs, oceans, and other natural waters. These waters are affected by many different sources of contamination. The sources are, but not limited to, groundwater run-off of nitrogen containing fertilizer, pesticides, cleaning agents, solid wastes, industrial waters, and many more. The final destinations of these contaminants are rivers, lakes, and bayous that eventually will lead to bays, gulfs, and oceans. Many industries depend on the quality of these waters, such as the fishing industry. In addition to wild marine life, there are large aquariums and fish and shrimp farms that are required to know the quality of the water. However, the ability of these industries to monitor their processes is limited. Most analytical methods do not apply to the analysis of high salinity waters. They are dependent on wet chemistry techniques, spectrophotometers, and flow analyzers. These methods do not have the accuracy, precision, and sensitivity when compared to ion chromatography (IC). Since the inception of IC, it has become a standard practice for determining the content of many different water samples. Many IC methods are limited in the range of analytes that can be detected, as well as the numerous sample sources of which the methods are applicable. The main focus of current IC methods does not include high salinity waters. This research demonstrates an ion chromatographic method that has the ability to determine low level concentrations of inorganic nitrogen and related anions (nitrite-N, nitrate-N, phosphorous-P, sulfate, bromide, chloride, sulfide, fluoride, ammonia, calcium, and magnesium) in a single run using a combination of UV and conductivity detectors. This method is applicable to various waters, and uses both freshwater and high salinity water samples. PMID:21859532

  10. Analysis of 10 metabolites of polymethoxyflavones with high sensitivity by electrochemical detection in high-performance liquid chromatography.

    PubMed

    Zheng, Jinkai; Bi, Jinfeng; Johnson, David; Sun, Yue; Song, Mingyue; Qiu, Peiju; Dong, Ping; Decker, Eric; Xiao, Hang

    2015-01-21

    Polymethoxyflavones (PMFs) have been known as a type of bioactive flavones that possess various beneficial biological functions. Accumulating evidence demonstrated that the metabolites of PMFs, that is, hydroxyl PMFs (OH-PMFs), had more potent beneficial biological effects than their corresponding parent PMFs. To facilitate the further identification and quantification of OH-PMFs in biological samples, the aim of this study was to develop a methodology for the simultaneous determination of 10 OH-PMFs using high-performance liquid chromatography (HPLC) coupled with electrochemistry detection. The HPLC profiles of these 10 OH-PMFs affected by different chromatographic parameters (different organic composition in mobile phases, the concentration of trifluoroacetic acid, and the concentration of ammonium acetate) are fully discussed in this study. The optimal condition was selected for the following validation studies. The linearity of calibration curves, accuracy, and precision (intra- and interday) at three concentration levels (low, middle, and high concentration range) were verified. The regression equations were linear (r > 0.9992) over the range of 0.005-10 ?M. The limit of detection for 10 OH-PMFs was in the range of 0.8-3.7 ng/mL (S/N = 3, 10 ?L injection). The recovery rates ranged from 86.6 to 108.7%. The precisions of intraday and interday analyses were less than 7.37 and 8.63% for relative standard deviation, respectively. This validated method was applied for the analysis of a variety of samples containing OH-PMFs. This paper also gives an example of analyzing the metabolites of nobiletin in mouse urine using the developed method. The transformation from nobiletin to traces of 5-hydroxyl metabolites has been discovered by this effective method, and this is the first paper to report such an association. PMID:25553421

  11. Liquid Chromatography–Tandem Mass Spectrometry Analysis of Human Adrenal Vein 19-Carbon Steroids Before and After ACTH Stimulation

    PubMed Central

    Rege, Juilee; Nakamura, Yasuhiro; Satoh, Fumitoshi; Morimoto, Ryo; Kennedy, Michael R.; Layman, Lawrence C.; Honma, Seijiro; Sasano, Hironobu

    2013-01-01

    Context: A broad analysis of adrenal gland-derived 19-carbon (C19) steroids has not been reported. This is the first study that uses liquid chromatography–tandem mass spectrometry to quantify 9 C19 steroids (androgens and their precursors), estrone, and estradiol in the adrenal vein (AV) of women, before and after ACTH stimulation. Objective: The objective of this study was to define the adrenal androgen metabolome in women before and after ACTH infusion. Design: This was a retrospective study. Patients: Seven women, aged 50.4 ± 5.4 years, with suspected diagnosis of an adrenal aldosterone-producing adenoma were included in the study. Methods: AV and iliac serum samples were collected before and after administration of ACTH (15 minutes). AV samples were analyzed using for concentrations of 9 unconjugated C19 steroids, estrone, and estradiol. Dehydroepiandrosterone sulfate (DHEA-S) was quantified by radioimmunoassay. Results: AV levels of DHEA-S were the highest among the steroids measured. The most abundant unconjugated C19 steroids in AV were 11?-hydroxyandrostenedione (11OHA), dehydroepiandrosterone (DHEA), and androstenedione (A4). ACTH significantly increased the adrenal output of 9 of the 12 steroids that were measured. ACTH increased the mean AV concentration of DHEA-S by 5-fold, DHEA by 21-fold, A4 by 7-fold, and 11OHA by 5-fold. 11?-Hydroxytestosterone and testosterone were found to be potent androgen receptor agonists when tested with an androgen-responsive cell reporter model. Conclusion: The current study indicates that the adrenal gland secretes primarily 3 weak androgens, namely DHEA, 11OHA, and A4. Active androgens, including testosterone and 11?-hydroxytestosterone, are also produced but to a lesser degree. PMID:23386646

  12. Direct identification of rituximab main isoforms and subunit analysis by online selective comprehensive two-dimensional liquid chromatography-mass spectrometry.

    PubMed

    Stoll, Dwight R; Harmes, David C; Danforth, John; Wagner, Elsa; Guillarme, Davy; Fekete, Szabolcs; Beck, Alain

    2015-08-18

    In this proof-of-concept study, rituximab, which is a reference therapeutic monoclonal antibody (mAb), was characterized through the implementation of online, selective comprehensive two-dimensional liquid chromatography (sLC×LC) coupled with mass spectrometry (MS), using a middle-up approach. In this setup, cation exchange chromatography (CEX) and reverse-phase liquid chromatography (RPLC) were used as the first and second separation dimensions, respectively. As illustrated in this work, the combination of these two chromatographic modes allows a direct assignment of the identities of CEX peaks, using data from the TOF/MS detector, because RPLC is directly compatible with MS detection, whereas CEX is not. In addition, the resolving power of CEX is often considered to be limited; therefore, this 2D approach provides an improvement in peak capacity and resolution when high-performance second-dimension separations are used, instead of simply using the second-dimension separation as a desalting step. This was particularly relevant when separating rituximab fragments of medium size (25 kDa), whereas most of the resolution was provided by CEX in the case of intact rituximab samples. The analysis of a commercial rituximab sample shows that online sLC×LC-TOF-MS can be used to rapidly characterize mAb samples, yielding the identification of numerous variants, based on the analysis of intact, partially digested, and digested/reduced mAb samples. PMID:26145446

  13. Simple quantitative determination of potent thiols at ultratrace levels in wine by derivatization and high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis.

    PubMed

    Capone, Dimitra L; Ristic, Renata; Pardon, Kevin H; Jeffery, David W

    2015-01-20

    Volatile sulfur compounds contribute characteristic aromas to foods and beverages and are widely studied, because of their impact on sensory properties. Certain thiols are particularly important to the aromas of roasted coffee, cooked meat, passion fruit, grapefruit, and guava. These same thiols enhance the aroma profiles of different wine styles, imparting pleasant aromas reminiscent of citrus and tropical fruits (due to 3-mercaptohexan-1-ol, 3-mercaptohexyl acetate, 4-mercapto-4-methylpentan-2-one), roasted coffee (2-furfurylthiol), and struck flint (benzyl mercaptan), at nanogram-per-liter levels. In contrast to the usual gas chromatography (GC) approaches, a simple and unique high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for routine analysis of five wine thiols, using 4,4'-dithiodipyridine (DTDP) as a derivatizing agent and polydeuterated internal standards for maximum accuracy and precision. DTDP reacted rapidly with thiols at wine pH and provided stable derivatives, which were enriched by solid-phase extraction (SPE) prior to analysis by HPLC-MS/MS. All steps were optimized and the method was validated in different wine matrices, with method performance being comparable to a well-optimized but more cumbersome gas chromatography-mass spectrometry (GC-MS) method. A range of commercial wines was analyzed with the new method, revealing the distribution of the five thiols in white, red, rosé, and sparkling wine styles. PMID:25562625

  14. [Qualitative and quantitative analysis of amygdalin and its metabolite prunasin in plasma by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry].

    PubMed

    Gao, Meng; Wang, Yuesheng; Wei, Huizhen; Ouyang, Hui; He, Mingzhen; Zeng, Lianqing; Shen, Fengyun; Guo, Qiang; Rao, Yi

    2014-06-01

    A method was developed for the determination of amygdalin and its metabolite prunasin in rat plasma after intragastric administration of Maxing shigan decoction. The analytes were identified by ultra-high performance liquid chromatography-tandem quadrupole time of flight mass spectrometry and quantitatively determined by ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry. After purified by liquid-liquid extraction, the qualitative analysis of amygdalin and prunasin in the plasma sample was performed on a Shim-pack XR-ODS III HPLC column (75 mm x 2.0 mm, 1.6 microm), using acetonitrile-0.1% (v/v) formic acid aqueous solution. The detection was performed on a Triple TOF 5600 quadrupole time of flight mass spectrometer. The quantitative analysis of amygdalin and prunasin in the plasma sample was performed by separation on an Agilent C18 HPLC column (50 mm x 2.1 mm, 1.7 microm), using acetonitrile-0.1% (v/v) formic acid aqueous solution. The detection was performed on an AB Q-TRAP 4500 triple quadrupole mass spectrometer utilizing electrospray ionization (ESI) interface operated in negative ion mode and multiple-reaction monitoring (MRM) mode. The qualitative analysis results showed that amygdalin and its metabolite prunasin were detected in the plasma sample. The quantitative analysis results showed that the linear range of amygdalin was 1.05-4 200 ng/mL with the correlation coefficient of 0.999 0 and the linear range of prunasin was 1.25-2 490 ng/mL with the correlation coefficient of 0.997 0. The method had a good precision with the relative standard deviations (RSDs) lower than 9.20% and the overall recoveries varied from 82.33% to 95.25%. The limits of detection (LODs) of amygdalin and prunasin were 0.50 ng/mL. With good reproducibility, the method is simple, fast and effective for the qualitative and quantitative analysis of the amygdalin and prunasin in plasma sample of rats which were administered by Maxing shigan decoction. PMID:25269256

  15. 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.

  16. Evaluation of equilibrium and non-equilibrium evaporation models for many-droplet gas-liquid ow simulations

    E-print Network

    Miller, Richard S.

    ±Knudsen law and a corrected (for evaporation eects) analytical heat transfer expression derived from the quasiEvaluation of equilibrium and non-equilibrium evaporation models for many-droplet gas-liquid ¯ow Abstract A variety of liquid droplet evaporation models, including both classical equilibrium and non

  17. 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

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

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 22 2012-07-01 2012-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  19. 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

    ... 40 Protection of Environment 21 2014-07-01 2014-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  20. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 22 2013-07-01 2013-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

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

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 21 2011-07-01 2011-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  2. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection in the analysis of agrochemical residues and mycotoxins in food - challenges and applications.

    PubMed

    O'Mahony, John; Clarke, Lesa; Whelan, Michelle; O'Kennedy, Richard; Lehotay, Steven J; Danaher, Martin

    2013-05-31

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence of UHPLC through technological advances. The implications of this new chromatographic technology for MS detection are discussed, as well as some of the remaining challenges in exploiting it for chemical residue applications. Finally, a comprehensive overview of published applications of UHPLC-MS in food contaminant analysis is presented, with a particular focus on veterinary drug residues. PMID:23352828

  3. Analysis of pharmaceutical and other organic wastewater compounds in filtered and unfiltered water samples by gas chromatography/mass spectrometry

    USGS Publications Warehouse

    Zaugg, Steven D.; Phillips, Patrick; Smith, Steven G.

    2014-01-01

    Research on the effects of exposure of stream biota to complex mixtures of pharmaceuticals and other organic compounds associated with wastewater requires the development of additional analytical capabilities for these compounds in water samples. Two gas chromatography/mass spectrometry (GC/MS) analytical methods used at the U.S. Geological Survey National Water Quality Laboratory (NWQL) to analyze organic compounds associated with wastewater were adapted to include additional pharmaceutical and other organic compounds beginning in 2009. This report includes a description of method performance for 42 additional compounds for the filtered-water method (hereafter referred to as the filtered method) and 46 additional compounds for the unfiltered-water method (hereafter referred to as the unfiltered method). The method performance for the filtered method described in this report has been published for seven of these compounds; however, the addition of several other compounds to the filtered method and the addition of the compounds to the unfiltered method resulted in the need to document method performance for both of the modified methods. Most of these added compounds are pharmaceuticals or pharmaceutical degradates, although two nonpharmaceutical compounds are included in each method. The main pharmaceutical compound classes added to the two modified methods include muscle relaxants, opiates, analgesics, and sedatives. These types of compounds were added to the original filtered and unfiltered methods largely in response to the tentative identification of a wide range of pharmaceutical and other organic compounds in samples collected from wastewater-treatment plants. Filtered water samples are extracted by vacuum through disposable solid-phase cartridges that contain modified polystyrene-divinylbenzene resin. Unfiltered samples are extracted by using continuous liquid-liquid extraction with dichloromethane. The compounds of interest for filtered and unfiltered sample types were determined by use of the capillary-column gas chromatography/mass spectrometry. The performance of each method was assessed by using data on recoveries of compounds in fortified surface-water, wastewater, and reagent-water samples. These experiments (referred to as spike experiments) consist of fortifying (or spiking) samples with known amounts of target analytes. Surface-water-spike experiments were performed by using samples obtained from a stream in Colorado (unfiltered method) and a stream in New York (filtered method). Wastewater spike experiments for both the filtered and unfiltered methods were performed by using a treated wastewater obtained from a single wastewater treatment plant in New York. Surface water and wastewater spike experiments were fortified at both low and high concentrations and termed low- and high-level spikes, respectively. Reagent water spikes were assessed in three ways: (1) set spikes, (2) a low-concentration fortification experiment, and (3) a high-concentration fortification experiment. Set spike samples have been determined since 2009, and consist of analysis of fortified reagent water for target compounds included for each group of 10 to18 environmental samples analyzed at the NWQL. The low-concentration and high-concentration reagent spike experiments, by contrast, represent a one-time assessment of method performance. For each spike experiment, mean recoveries ranging from 60 to 130 percent indicate low bias, and relative standard deviations (RSDs) less than ( Of the compounds included in the filtered method, 21 had mean recoveries ranging from 63 to 129 percent for the low-level and high-level surface-water spikes, and had low ()132 percent]. For wastewater spikes, 24 of the compounds included in the filtered method had recoveries ranging from 61 to 130 percent for the low-level and high-level spikes. RSDs were 130 percent) or variable recoveries (RSDs >30 percent) for low-level wastewater spikes, or low recoveries ( Of the compounds included in the unfiltered method, 17 had mean spike recoveries ranging from 74

  4. Evaluation and application of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry for complex sample analysis.

    PubMed

    Denawaka, Chamila J; Fowlis, Ian A; Dean, John R

    2014-04-18

    An evaluation of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS) has been undertaken to assess its applicability for the determination of 32 volatile compounds (VCs). The key experimental variables of sample incubation time and temperature have been evaluated alongside the MCC-GC variables of column polarity, syringe temperature, injection temperature, injection volume, column temperature and carrier gas flow rate coupled with the IMS variables of temperature and drift gas flow rate. This evaluation resulted in six sets of experimental variables being required to separate the 32 VCs. The optimum experimental variables for SHS-MCC-GC-IMS, the retention time and drift time operating parameters were determined; to normalise the operating parameters, the relative drift time and normalised reduced ion mobility for each VC were determined. In addition, a full theoretical explanation is provided on the formation of the monomer, dimer and trimer of a VC. The optimum operating condition for each VC calibration data was obtained alongside limit of detection (LOD) and limit of quantitation (LOQ) values. Typical detection limits ranged from 0.1ng bis(methylthio)methane, ethylbutanoate and (E)-2-nonenal to 472ng isovaleric acid with correlation coefficient (R(2)) data ranging from 0.9793 (for the dimer of octanal) through to 0.9990 (for isobutyric acid). Finally, the developed protocols were applied to the analysis of malodour in sock samples. Initial work involved spiking an inert matrix and sock samples with appropriate concentrations of eight VCs. The average recovery from the inert matrix was 101±18% (n=8), while recoveries from the sock samples were lower, that is, 54±30% (n=8) for sock type 1 and 78±24% (n=6) for sock type 2. Finally, SHS-MCC-GC-IMS was applied to sock malodour in a field trial based on 11 volunteers (mixed gender) over a 3-week period. By applying the SHS-MCC-GC-IMS database, four VCs were identified and quantified: ammonia, dimethyl disulphide, dimethyl trisulphide and butyric acid. A link was identified between the presence of high ammonia and dimethyl disulphide concentrations and a high malodour odour grading, that is, ? 6. Statistical analysis did not find any correlation between the occurrence of dimethyl disulphide and participant gender. PMID:24630058

  5. Selective and trace determination of monochloramine in river water by chemical derivatization and liquid chromatography/tandem mass spectrometry analysis.

    PubMed

    Kinani, Said; Layousse, Stéphany; Richard, Bertille; Kinani, Aziz; Bouchonnet, Stéphane; Thoma, Astrid; Sacher, Frank

    2015-08-01

    Monochloramine (MCA) may enter the aquatic environment through three main sources: wastewater treatment plant effluents, industrial effluents and thermal power plant wastes. Up to date, there are no available data about the concentration levels of this chemical in river water due to lack of appropriate analytical methods. Therefore, sensitive and selective analytical methods for monochloramine analysis in river water are required to evaluate its environmental fate and its effects on aquatic ecosystems. Thus, in this study we describe a highly specific and sensitive method for monochloramine determination in river water. This method combines chemical derivatization of monochloramine into indophenol followed by liquid chromatography coupled to electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) analysis. Two precursor-to-product ion transitions were monitored (200?127 and 200?154) in positive ionisation mode, fulfilling the criteria of selectivity, in accordance with the European Legislation requirements (decision 2002/657/EC). Ion structures and fragmentation mechanisms have been proposed to explain the selected transitions. Linearity range, accuracy and precision of the method have been assessed according to the French method validation standard NF T90-210. Detecting the derivatized monochloramine (indophenol) in Multiple Reaction Monitoring (MRM) mode provided a limit of quantification of 40 ng L(-1) equivalent monochloramine. Applied to Loire river water (France), the developed method occasionally detected monochloramine at concentrations less than 300 ng L(-1), which could be explained by punctual discharges of water containing active chlorine upstream of the sampling point. Indeed, it is widely reported in the literature that the addition of chlorine to water containing ammonia (e.g., wastewater effluents and river water) may result in the instantaneous formation of monochloramine. The proposed method is a powerful tool that can be used in environmental research (e.g., assessment of environmental fate and generating of ecotoxicological data) as well as in research studies concerning the evaluation of water disinfection efficiency; but it is not currently appropriate for routine use in industrial applications given the complexity of the procedure, the instability of indophenol and the use of certain toxic reagents. PMID:26048841

  6. Comprehensive high temperature two-dimensional liquid chromatography combined with high temperature gradient chromatography-infrared spectroscopy for the analysis of impact polypropylene copolymers.

    PubMed

    Cheruthazhekatt, Sadiqali; Harding, Gareth W; Pasch, Harald

    2013-04-19

    Impact polypropylene copolymers (IPC) are extremely complex materials that can only be effectively analysed by multidimensional analytical approaches. IPC consists of isotactic polypropylene (iPP) as the major phase, ethylene-propylene (EP) copolymers of various compositions and small amounts of polyethylene. The molecular heterogeneity of two IPC samples having different ethylene contents was studied by using a novel cross-fractionation technique, developed from a combination of various analytical separation methods into an effective characterisation tool for complex polyolefins. The initial step involves the fractionation of the sample into EP rubber, EP segmented copolymer, and iPP, by preparative temperature rising elution fractionation (TREF). The resulting fractions are still distributed with regards to chemical composition and molar mass. The separation with respect to these parameters is conducted by comprehensive HT 2D-LC. This is the first time that the individual components in all TREF fractions of an IPC are separated and analysed mutidimensionally, by both SEC-FTIR, high-temperature (HT) HPLC-FTIR, and HT 2D-LC. Molar mass analysis of the chemically homogeneous fractions from HT HPLC is accomplished by HT SEC in the second dimension of HT 2D-LC. The chemical composition of all species is determined by coupling FTIR spectroscopy to HT HPLC via an LC-transform interface. This novel approach reveals the capability of this hyphenated technique to determine the exact chemical composition of the individual components in the complex TREF fractions of IPCs. The HT HPLC-FTIR results confirm the separation mechanism in the given chromatographic system using a 1-decanol to TCB solvent gradient and a Hypercarb stationary phase. The components of differing chemical composition are separated according to the nature and length of the propylene/ethylene segments, with their arrangement in the chains strongly affecting their adsorption/desorption on the stationary phase. FTIR analysis provides information on the ethylene and propylene contents of the fractions as well as on the ethylene and propylene crystallinities. PMID:23489491

  7. Qualitative and Quantitative Analysis of Major Triterpenoids in Alismatis Rhizoma by High Performance Liquid Chromatography/Diode-Array Detector/Quadrupole-Time-of-Flight Mass Spectrometry and Ultra-Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry.

    PubMed

    Zhao, Wanli; Huang, Xiaoqiang; Li, Xiaoyan; Zhang, Fangfang; Chen, Sainan; Ye, Miao; Huang, Mingqing; Xu, Wen; Wu, Shuisheng

    2015-01-01

    Alismatis Rhizoma (AMR) is a well-known natural medicine with a long history in Chinese medicine and has been commonly used for treating a wide range of ailments related to dysuria, edema, nephropathy, hyperlipidaemia, diabetes, inflammation as well as tumors in clinical applications. Most beneficial effects of AMR are attributed to the presence of protostane terpenoids, the major active ingredients of Alismatis Rhizoma (AMR). In this study, a systematic high performance liquid chromatography/diode-array detector/quadrupole-time-of-flight mass spectrometry (HPLC-DAD-Q-TOF MS) and ultra-performance liquid chromatography/triple quadrupole mass spectrometry (UPLC-QqQ MS) method was developed for qualitative and quantitative analyses of the major AMR triterpenoids. First, a total of 25 triterpenoid components, including 24 known compounds and one new compound were identified by comparison with UV spectra, molecular ions and fragmentation behaviors of reference standards or the literature. Second, an efficient method was established for the rapid simultaneous determination of 14 representative triterpenoids by UPLC-QqQ MS. Forty-three batches of AMR were analyzed with linearity (r, 0.9980-0.9999), intra-day precision (RSD, 1.18%-3.79%), inter-day precision (RSD, 1.53%-3.96%), stability (RSD, 1.32%-3.97%), repeatability (RSD, 2.21%-4.25%), and recovery (98.11%-103.8%). These results indicated that new approaches combining HPLC-DAD-Q-TOF MS and UPLC-QqQ MS are applicable in the qualitative and quantitative analysis of AMR. PMID:26263967

  8. Analysis of underivatized artemisinin and related sesquiterpene lactones by high-performance liquid chromatography with ultraviolet detection

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Although high-performance liquid chromatography with ultraviolet detection (HPLC-UV) is widely available, artemisinin has not yet been analyzed by HPLC-UV without derivatization, due to its reported lack of UV absorbance. The growing interest in the production of artemisinin, calls for a method tha...

  9. Principles and Methods Chromatography

    E-print Network

    Lebendiker, Mario

    Edition AC 18-1022-29 Principles and Methods Affinity Chromatography #12;Antibody Purification-1142-75 Protein Purification Handbook 18-1132-29 Ion Exchange Chromatography Principles and Methods 18-1114-21 Affinity Chromatography Principles and Methods 18-1022-29 Hydrophobic Interaction Chromatography Principles

  10. Instrumentation: Ion Chromatography.

    ERIC Educational Resources Information Center

    Fritz, James S.

    1987-01-01

    Discusses the importance of ion chromatography in separating and measuring anions. The principles of ion exchange are presented, along with some applications of ion chromatography in industry. Ion chromatography systems are described, as well as ion pair and ion exclusion chromatography, column packings, detectors, and programming. (TW)

  11. Analysis of anions in aqueous samples by ion chromatography and capillary electrophoresis. A comparative study of peak modeling and validation criteria.

    PubMed

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

    1999-08-13

    The object of this study is the comparison of two methods for the quantitative analysis of anions in aqueous samples: ion chromatography with conductimetric detection, and capillary zone electrophoresis with indirect photometric detection. The comparison includes modeling of experimental peaks as well as statistical validation criteria according to the recommendations of the International Conference on Harmonisation. In ion chromatography, peak shapes are Gaussian or exponentially modified Gaussian, and the number of theoretical plates calculated using the appropriate mathematical relations correspond well to those obtained from statistical moments. Peaks in capillary electrophoresis, however, do not follow the same models. A different model, treating the peaks as right angle triangles, has been studied. Equations corresponding to this model permit a good estimation of plate numbers. The statistical validation of these methods includes detection limits, linearity, accuracy and precision. Overall, ion chromatography yields better validation results than capillary electrophoresis. In the latter method the injection mode plays an important role, with voltage injection giving lower detection limits than hydrodynamic injection. PMID:10481986

  12. [Residue analysis of pyrethroid insecticides in cereal grains, milled fractions and bread].

    PubMed

    Dicke, W; Ocker, H D; Thier, H P

    1988-02-01

    A procedure is described for the residual analysis of eight pyrethroid insecticides at levels of 2-5 micrograms/kg. Residues are extracted from cereal grains, flour or bread with a mixture of acetonitrile/water (2 + 1) and are partitioned into petroleum ether. Clean-up is performed by gel permeation chromatography on Bio-Beads S-X3 and an additional Florisil column. Electron capture gas liquid chromatography on a non-polar SE-30 capillary column separates the isomers of the compounds. Under the conditions used in the experiments with cyfluthrin, cypermethrin, deltamethrin, fenvalerate, and permethrin, the compound levels in rye and wheat did not decrease significantly. Losses during milling and baking were small. Consequently, pyrethroid insecticides remain effective in grain stored over a long period of time. However, considerable residues result in the milled fractions as well as in different types of bread. PMID:3354265

  13. Supported liquid membrane-liquid chromatography-mass spectrometry analysis of cyanobacterial toxins in fresh water systems

    NASA Astrophysics Data System (ADS)

    Mbukwa, Elbert A.; Msagati, Titus A. M.; Mamba, Bhekie B.

    Harmful algal blooms (HABs) are increasingly becoming of great concern to water resources worldwide due to indiscriminate waste disposal habits resulting in water pollution and eutrophication. When cyanobacterial cells lyse (burst) they release toxins called microcystins (MCs) that are well known for their hepatotoxicity (causing liver damage) and have been found in eutrophic lakes, rivers, wastewater ponds and other water reservoirs. Prolonged exposure to low concentrated MCs are equally of health importance as they are known to be bioaccumulative and even at such low concentration do exhibit toxic effects to aquatic animals, wildlife and human liver cells. The application of common treatment processes for drinking water sourced from HABs infested reservoirs have the potential to cause algal cell lyses releasing low to higher amounts of MCs in finished water. Trace microcystins in water/tissue can be analyzed and quantified using Liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) following solid-phase extraction (SPE) sample clean-up procedures. However, extracting MCs from algal samples which are rich in chlorophyll pigments and other organic matrices the SPE method suffers a number of drawbacks, including cartridge clogging, long procedural steps and use of larger volumes of extraction solvents. We applied a supported liquid membrane (SLM) based technique as an alternative sample clean-up method for LC-ESI-MS analysis of MCs from both water and algal cells. Four (4) MC variants (MC-RR, -YR, -LR and -WR) from lyophilized cells of Microcystis aeruginosa and water collected from a wastewater pond were identified) and quantified using LC-ESI-MS following a SLM extraction and liquid partitioning step, however, MC-WR was not detected from water extracts. Within 45 min of SLM extraction all studied MCs were extracted and pre-concentrated in approximately 15 ?L of an acceptor phase at an optimal pH 2.02 of the donor phase (sample). The highest total quantifiable intracellular and extracellular MCs were 37.039 ± 0.087 ?g/g DW and 5.123 ± 0.018 ?g/L, respectively. The concentrations of MC-RR were the highest from all samples studied recording maximum values of 21.579 ± 0.066 ?g/g DW and 3.199 ± 0.012 ?g/L for intracellular and extracellular quantities, respectively.

  14. Pressurized liquid extraction-gas chromatography-mass spectrometry analysis of fragrance allergens, musks, phthalates and preservatives in baby wipes.

    PubMed

    Celeiro, Maria; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria

    2015-03-01

    Baby wipes and wet toilet paper are specific hygiene care daily products used on newborn and children skin. These products may contain complexes mixtures of harmful chemicals. A method based on pressurized liquid extraction (PLE) followed by gas chromatography-mass spectrometry (GC-MS) has been developed for the simultaneous determination of sixty-five chemical compounds (fragrance allergens, preservatives, musks, and phthalates) in wipes and wet toilet paper for children. These compounds are legislated in Europe according Regulation EC No 1223/2009, being twelve of them banned for their use in cosmetics, and one of them, 3-iodo-2-propynyl butylcarbamate (IPBC), is banned in products intended for children under 3 years. Also, propyl-, and butylparaben will be prohibited in leave-on cosmetic products designed for application on the nappy area of children under 3 years from April 2015. PLE is a fast, simple, easily automated technique, which permits to integrate a clean-up step during the extraction process reducing analysis time and stages. The proposed PLE-based procedure was optimized on real non-spiked baby wipe samples by means of experimental design to study the influence on extraction of parameters such as extraction solvent, temperature, extraction time, and sorbent type. Under the selected conditions, the method was validated showing satisfactory linearity, and intra-day, and inter-day precision. Recoveries were between 80-115% for most of the compounds with relative standard deviations (RSD) lower than 15%. Finally, twenty real samples were analyzed. Thirty-six of the target analytes were detected, highlighting the presence of phenoxyethanol in all analyzed samples at high concentration levels (up to 0.8%, 800?gg(-1)). Methyl paraben (MeP), and ethyl paraben (EtP) were found in 40-50% of the samples, and the recently banned isobutyl paraben (iBuP) and isopropyl paraben (iPrP), were detected in one and seven samples, respectively, at concentrations between 0.093 and 247?gg(-1). In the case of phthalates, the forbidden phthalates dibutyl phtalate (DBP) and di(2-ethylhexyl)phthalate (DEHP) were also found in thirteen samples at low levels. All the samples contained fragrance allergens in many cases at high levels (up to 2400?gg(-1)) and three musks were detected in the samples. Excluding the banned compounds, all samples complied with the concentration limits established by the European Regulation although 25% of them did not fulfill the labeling requirements for fragrance allergens. PMID:25662066

  15. Studies of two-phase gas-liquid flow in microgravity

    NASA Astrophysics Data System (ADS)

    Bousman, William Scott

    1995-02-01

    Two-phase gas-liquid flows are expected to occur in many future space operations. Due to a lack of buoyancy in the microgravity environment, two-phase flows are known to behave differently than those in earth gravity. Despite these concerns, little research has been conducted on microgravity two-phase flow and the current understanding is poor. This dissertation describes an experimental and modeling study of the characteristics of two-phase flows in microgravity. An experiment was operated onboard NASA aircraft capable of producing short periods of microgravity. In addition to high speed photographs of the flows, electronic measurements of void fraction, liquid film thickness, bubble and wave velocity, pressure drop and wall shear stress were made for a wide range of liquid and gas flow rates. The effects of liquid viscosity, surface tension and tube diameter on the behavior of these flows were also assessed. From the data collected, maps showing the occurrence of various flow patterns as a function of gas and liquid flow rates were constructed. Earth gravity two-phase flow models were compared to the results of the microgravity experiments and in some cases modified. Models were developed to predict the transitions on the flow pattern maps. Three flow patterns, bubble, slug and annular flow, were observed in microgravity. These patterns were found to occur in distinct regions of the gas-liquid flow rate parameter space. The effect of liquid viscosity, surface tension and tube diameter on the location of the boundaries of these regions was small. Void fraction and Weber number transition criteria both produced reasonable transition models. Void fraction and bubble velocity for bubble and slug flows were found to be well described by the Drift-Flux model used to describe such flows in earth gravity. Pressure drop modeling by the homogeneous flow model was inconclusive for bubble and slug flows. Annular flows were found to be complex systems of ring-like waves and a substrate film. Pressure drop was best fitted with the Lockhart- Martinelli model.

  16. Fingerprint analysis, multi-component quantitation, and antioxidant activity for the quality evaluation of Salvia miltiorrhiza var. alba by high-performance liquid chromatography and chemometrics.

    PubMed

    Zhang, Danlu; Duan, Xiaoju; Deng, Shuhong; Nie, Lei; Zang, Hengchang

    2015-10-01

    Salvia miltiorrhiza Bge. var. alba C.Y. Wu and H.W. Li has wide prospects in clinical practice. A useful comprehensive method was developed for the quality evaluation of S. miltiorrhiza var. alba by three quantitative parameters: high-performance liquid chromatography fingerprint, ten-component contents, and antioxidant activity. The established method was validated for linearity, precision, repeatability, stability, and recovery. Principal components analysis and hierarchical clustering analysis were both used to evaluate the quality of the samples from different origins. The results showed that there were category discrepancies in quality of S. miltiorrhiza var. alba samples according to the three quantitative parameters. Multivariate linear regression was adopted to explore the relationship between components and antioxidant activity. Three constituents, namely, danshensu, rosmarinic acid, and salvianolic acid B, significantly correlated with antioxidant activity, and were successfully elucidated by the optimized multivariate linear regression model. The combined use of high-performance liquid chromatography fingerprint analysis, simultaneous multicomponent quantitative analysis, and antioxidant activity for the quality evaluation of S. miltiorrhiza var. alba is a reliable, comprehensive, and promising approach, which might provide a valuable reference for other herbal products in general to improve their quality control. PMID:26228912

  17. Titan's Organic Aerosols : Molecular Composition And Structure Inferred From Systematic Pyrolysis Gas Chromatography Mass Spectrometry Analysis of Analogues

    NASA Astrophysics Data System (ADS)

    Morisson, Marietta; Szopa, Cyril; Buch, Arnaud; Carrasco, Nathalie; Gautier, Thomas

    2015-04-01

    In spite of numerous studies carried out to characterize the chemical composition of laboratory analogues of Titan aerosols (tholins), their molecular composition as well as their structuration are still little known. If Pyrolysis gas chromatography mass spectrometry (Pyr-GCMS) has been used for years to give clues about this composition, the highly disparate results obtained show that they can be attributed to the analytical conditions used, to differences in the nature of the analogues studied, or both. In order to have a better description of Titan's tholins molecular composition, we led a systematic analysis of these materials by pyr-GCMS, exploring the analytical parameters to estimate the biases this technique can induce. With this aim, we used the PAMPRE experiment, a capacitively coupled RF cold plasma reactor (Szopa et al. 2006), to synthetize tholins with 2%, 5% and 10% of CH4 in N2. The three samples were systematically pyrolyzed in the temperature range 200-600°C with a 100°C step. The evolved gases were then injected into a GC-MS device for molecular identification. This systematic pyr-GC-MS analysis had two major objectives: (i) optimizing all the analytical parameters for the detection of a wide range of compounds and thus a characterization of the tholins composition as comprehensive as possible, and (ii) highlighting the role of the CH4 ratio on the tholins molecular structure. About a hundred of molecules have been identified in the pyrolysis products. Although an identical major pattern of nitriles and ethylene appears clearly for the three samples, some discriminant signatures were highlighted. The samples mainly differ by the number of released compounds. The results show especially an increase in the hydrocarbonaceous chains when the CH4 ratio increases. At the opposite, the formation of poly-nitrogenous compounds seems to be easier for lower CH4 ratios. We also performed a semi-quantitative study on the best represented chemical family in our chromatograms - namely nitriles: the existence of a relation between the quantity of a released compound and its molecular mass is consistent with the quantification of nitriles in the PAMPRE gas phase done by Gautier et al., 2011. Moreover, numerous species are present both in tholins and in the gas phase. That allowed us to make out potential precursors of the solid organic particles. From all these results, we conclude that the optimal pyrolysis temperature for a GC-MS analysis of our tholins is 600°C. This temperature choice results from the best compromise between the number of released compounds, the quality of the signal and the appearance of pyrolysis artefacts. Lastly, thanks to a review of pyr-GCMS studies carried out on Titan tholins since the first work of Khare et al. (1981), we compared all the previous analyses between them and with our own results in order to better understand the differences. References B. N. Khare et al., Icarus, vol. 48, no. 2, pp. 290-297, Nov. 1981. C. Szopa et al., Planet. Space Sci., vol. 54, no. 4, pp. 394-404, Apr. 2006. T. Gautier et al., Icarus, vol. 213, no. 2, pp. 625-635, Jun. 2011.

  18. LIQUID AND GAS CHROMATOGRAPHIC ANALYSIS OF DIETHYL PHTHALATE IN WATER AND SEDIMENT

    EPA Science Inventory

    Diethyl phthalate was determined in water and sediment by high performance liquid chromatography (HPLC) and in water by gas-liquid chromatography with electron capture detection (GLC-ECD). Water samples were extracted with hexane, using a high-speed homogenizer-ultrasonic apparat...

  19. Multi-constituent determination and fingerprint analysis of Scutellaria indica L. using ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    PubMed

    Liang, Xianrui; Zhao, Cui; Su, Weike

    2015-11-01

    An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method integrating multi-constituent determination and fingerprint analysis has been established for quality assessment and control of Scutellaria indica L. The optimized method possesses the advantages of speediness, efficiency, and allows multi-constituents determination and fingerprint analysis in one chromatographic run within 11 min. 36 compounds were detected, and 23 of them were unequivocally identified or tentatively assigned. The established fingerprint method was applied to the analysis of ten S. indica samples from different geographic locations. The quality assessment was achieved by using principal component analysis. The proposed method is useful and reliable for the characterization of multi-constituents in a complex chemical system and the overall quality assessment of S. indica. PMID:26333027

  20. Development, optimization, validation and application of faster gas chromatography - flame ionization detector method for the analysis of total petroleum hydrocarbons in contaminated soils.

    PubMed

    Zubair, Abdulrazaq; Pappoe, Michael; James, Lesley A; Hawboldt, Kelly

    2015-12-18

    This paper presents an important new approach to improving the timeliness of Total Petroleum Hydrocarbon (TPH) analysis in the soil by Gas Chromatography - Flame Ionization Detector (GC-FID) using the CCME Canada-Wide Standard reference method. The Canada-Wide Standard (CWS) method is used for the analysis of petroleum hydrocarbon compounds across Canada. However, inter-laboratory application of this method for the analysis of TPH in the soil has often shown considerable variability in the results. This could be due, in part, to the different gas chromatography (GC) conditions, other steps involved in the method, as well as the soil properties. In addition, there are differences in the interpretation of the GC results, which impacts the determination of the effectiveness of remediation at hydrocarbon-contaminated sites. In this work, multivariate experimental design approach was used to develop and validate the analytical method for a faster quantitative analysis of TPH in (contaminated) soil. A fractional factorial design (fFD) was used to screen six factors to identify the most significant factors impacting the analysis. These factors included: injection volume (?L), injection temperature (°C), oven program (°C/min), detector temperature (°C), carrier gas flow rate (mL/min) and solvent ratio (v/v hexane/dichloromethane). The most important factors (carrier gas flow rate and oven program) were then optimized using a central composite response surface design. Robustness testing and validation of model compares favourably with the experimental results with percentage difference of 2.78% for the analysis time. This research successfully reduced the method's standard analytical time from 20 to 8min with all the carbon fractions eluting. The method was successfully applied for fast TPH analysis of Bunker C oil contaminated soil. A reduced analytical time would offer many benefits including an improved laboratory reporting times, and overall improved clean up efficiency. The method was successfully applied for the analysis of TPH of Bunker C oil in contaminated soil. PMID:26607315