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Sample records for high-temperature liquid chromatography

  1. Rapid and sensitive determination of carbohydrates in foods using high temperature liquid chromatography with evaporative light scattering detection.

    Science.gov (United States)

    Terol, Amanda; Paredes, Eduardo; Maestre, Salvador E; Prats, Soledad; Todolí, José L

    2012-04-01

    In the present work, an evaporative light scattering detector was used as a high-temperature liquid chromatography detector for the determination of carbohydrates. The compounds studied were glucose, fructose, galactose, sucrose, maltose, and lactose. The effect of column temperature on the retention times and detectability of these compounds was investigated. Column heating temperatures ranged from 25 to 175°C. The optimum temperature in terms of peak resolution and detectability with pure water as mobile phase and a liquid flow rate of 1 mL/min was 150°C as it allowed the separation of glucose and the three disaccharides here considered in less than 3 min. These conditions were employed for lactose determination in milk samples. Limits of quantification were between 2 and 4.7 mg/L. On the other hand, a temperature gradient was developed for the simultaneous determination of glucose, fructose, and sucrose in orange juices, due to coelution of monosaccharides at temperatures higher than 70°C, being limits of quantifications between 8.5 and 12 mg/L. The proposed hyphenation was successfully applied to different types of milk and different varieties of oranges and mandarins. Recoveries for spiked samples were close to 100% for all the studied analytes. © 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Supercritical fluid chromatography and high temperature liquid chromatography for the group-type separation of diesel fuels and heavy gas oils

    Energy Technology Data Exchange (ETDEWEB)

    Paproski, R.E.

    2008-07-01

    This thesis investigated the use of unconventional extraction columns for separating diesel fuels by supercritical fluid chromatography (SFC) and for separating heavy gas oils by high temperature normal phase high performance liquid chromatography (HPLC). The purpose was to improve group-type resolution of the fuels, although these methods are also commonly used to determine the proportion of saturates, mono-, di-, tri-, and polyaromatic hydrocarbons. Higher mobile phase flow rates and unconventional column dimensions were also studied to obtain faster analysis times with both SFC and HPLC. The highest group-type resolutions with SFC were obtained by serially coupling bare titania and bare silica columns. Short packed columns and monolithic silica columns were compared at high carbon dioxide flow rates for reducing SFC analysis time, with shortpacked columns achieving 7-fold lower separation times while maintaining significant resolution. Three diesel samples had better resolution and analysis time. A thermally stable bare zircoma column for normal phase HPLC was studied at temperatures up to 200 degrees C. An increase in temperature resulted in lower retention of twenty five aromatic model compounds. Considerable improvements in peak shape, efficiency, group-type selectivity, and column re-equilibration times were obtained at elevated temperatures. At temperatures over 100 degrees C, indole and carbazole thermally decomposed in a hexane/dichloromethane mobile phase. The first order decomposition of carbazole was studied in further detail. A high resolution method was developed using titania and silica columns with valve-switching and dual gradients to separate 3 heavy gas oils. Separation was achieved in only 3 minutes using a fast analysis time method in a titania column at high flow rates.

  3. High temperature liquid chromatography hyphenated with ESI-MS and ICP-MS detection for the structural characterization and quantification of halogen containing drug metabolites

    International Nuclear Information System (INIS)

    Vlieger, Jon S.B. de; Giezen, Mark J.N.; Falck, David; Tump, Cornelis; Heuveln, Fred van; Giera, Martin; Kool, Jeroen; Lingeman, Henk; Wieling, Jaap; Honing, Maarten; Irth, Hubertus; Niessen, Wilfried M.A.

    2011-01-01

    Highlights: → Hyphenation of high temperature liquid chromatography to ICP-MS and ESI-MS. → Structural characterization of kinase inhibitor metabolites with high resolution MS n experiments. → Quantification of drug metabolites with ICP-MS based on Iodine detection. → Significant changes in ESI-MS response after small structural changes. - Abstract: In this paper we describe the hyphenation of high temperature liquid chromatography with ICP-MS and ESI-MS for the characterization of halogen containing drug metabolites. The use of temperature gradients up to 200 deg. C enabled the separation of metabolites with low organic modifier content. This specific property allowed the use of detection methods that suffer from (significant) changes in analyte response factors as a function of the organic modifier content such as ICP-MS. Metabolites of two kinase inhibitors (SB-203580-Iodo and MAPK inhibitor VIII) produced by bacterial cytochrome P450 BM3 mutants and human liver microsomes were identified based on high resolution MS n data. Quantification was done using their normalized and elemental specific response in the ICP-MS. The importance of these kinds of quantification strategies is stressed by the observation that the difference of the position of one oxygen atom in a structure can greatly affect its response in ESI-MS and UV detection.

  4. Contribution to high-temperature chromatography and high-temperature-gas-chromatography-mass spectrometry of lipids

    International Nuclear Information System (INIS)

    Aichholz, R.

    1998-04-01

    This thesis describes the use of high temperature gas chromatography for the investigation of unusual triacylglycerols, cyanolipids and bees waxes. The used glass capillary columns were pretreated and coated with tailor made synthesized high temperature stable polysiloxane phases. The selective separation properties of the individual columns were tested with a synthetic lipid mixture. Suitable derivatization procedures for the gaschromatographic analyses of neutral lipids, containing multiple bonds as well as hydroxy-, epoxy-, and carboxyl groups, were developed and optimized. Therefore conjugated olefinic-, conjugated olefinic-acetylenic-, hydroxy-, epoxy-, and conjugated olefinic keto triacylglycerols in miscellaneous plant seed oils as well as hydroxy monoesters, diesters and hydroxy diesters in bees waxes could be analysed directly with high temperature gas chromatography for the first time. In order to elucidate the structures of separated lipid compounds, high temperature gas chromatography was coupled to mass spectrometry and tandem mass spectrometry, respectively. Comparable analytical systems are hitherto not commercial available. Therefore instrumental prerequisites for a comprehensive and detailed analysis of seed oils and bees waxes were established. In GC/MS commonly two ionization methods are used, electron impact ionization and chemical ionization. For the analysis of lipids the first is of limited use only. Due to intensive fragmentation only weak molecular ions are observed. In contrast, the chemical ionization yields in better results. Dominant quasi molecular ions enable an unambiguous determination of the molecular weight. Moreover, characteristic fragment ions provide important indications of certain structural features of the examined compounds. Nevertheless, in some cases the chromatographic resolution was insufficient in order to separate all compounds present in natural lipid mixtures. Owing to the selected detection with mass spectrometry

  5. Pressure sensor for high-temperature liquids

    International Nuclear Information System (INIS)

    Forster, G.A.

    1978-01-01

    A pressure sensor for use in measuring pressures in liquid at high temperatures, especially such as liquid sodium or liquid potassium, comprises a soft diaphragm in contact with the liquid. The soft diaphragm is coupled mechanically to a stiff diaphragm. Pressure is measured by measuring the displacement of both diaphragms, typically by measuring the capacitance between the stiff diaphragm and a fixed plate when the stiff diaphragm is deflected in response to the measured pressure through mechanical coupling from the soft diaphragm. Absolute calibration is achieved by admitting gas under pressure to the region between diaphragms and to the region between the stiff diaphragm and the fixed plate, breaking the coupling between the soft and stiff diaphragms. The apparatus can be calibrated rapidly and absolutely

  6. Determination of thromboxanes, leukotrienes and lipoxins using high-temperature capillary liquid chromatography-tandem mass spectrometry and on-line sample preparation

    DEFF Research Database (Denmark)

    Dahl, Sandra Rinne; Kleiveland, Charlotte Ramstad; Kassem, Moustapha

    2009-01-01

    An on-line strong cation-exchange (SCX)-reversed-phase (RP) capillary liquid chromatographic (cLC) method with ion-trap tandem mass spectrometric (IT-MS/MS) detection for the simultaneous determination of thromboxane (TX) B(2), TXB(3), leukotriene (LT) B(4), LTD(4) and lipoxin (LX) A(4) in cell...

  7. Analysis of artificial fireplace logs by high temperature gas chromatography.

    Science.gov (United States)

    Kuk, Raymond J

    2002-11-01

    High temperature gas chromatography is used to analyze the wax of artificial fireplace logs (firelogs). Firelogs from several different manufacturers are studied and compared. This study shows that the wax within a single firelog is homogeneous and that the wax is also uniform throughout a multi-firelog package. Different brands are shown to have different wax compositions. Firelogs of the same brand, but purchased in different locations, also have different wax compositions. With this information it may be possible to associate an unknown firelog sample to a known sample, but a definitive statement of the origin cannot be made.

  8. Liquid Chromatography in 1982.

    Science.gov (United States)

    Freeman, David H.

    1982-01-01

    Reviews trends in liquid chromatography including apparatus, factors affecting efficient separation of a mixture (peak sharpness and speed), simplified problem-solving, adsorption, bonded phase chromatography, ion selectivity, and size exclusion. The current trend is to control chemical selectivity by the liquid phase. (Author/JN)

  9. Column Liquid Chromatography.

    Science.gov (United States)

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  10. Additives for high-temperature liquid lubricants

    Science.gov (United States)

    Lawton, Emil A.; Yavrouian, Andre H.; Repar, John

    1988-01-01

    A preliminary research program was conducted to demonstrate a new concept for additives to liquid lubricants. It was demonstrated that suspensions of o-phthalonitrile and a substituted 1,2-maleonitrile in mineral oil and dilute solutions of o-phthalonitrile and tetrafluoro-o-phthalonitrile extended the lifetime of bearings under boundary lubricating conditions. The solutions exhibited coefficients of friction under high loads of 0.02-0.03. These results were consistent with the hypothesis that these compounds react with the hot metal surface to form a planar lubricating film by means of a metal or metal oxide template reaction. Also, the adherence was very strong due to the chelating action of the planar macrocycles postulated to form under the experimental conditions.

  11. performance liquid chromatography

    African Journals Online (AJOL)

    user

    2010-11-22

    Nov 22, 2010 ... ISSN 1684–5315 © 2010 Academic Journals. Full Length Research Paper. Determination ... Key words: Processed food, high-performance liquid chromatography, acrylamide, health hazard. INTRODUCTION. In the year 2002, the ... potatoes, breakfast cereals etc. It was thus confirmed that acrylamide has ...

  12. Volatility of coal liquids at high temperatures and pressures

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, G M; Johnston, R H; Hwang, S C; Tsonopoulos, C

    1981-01-01

    The volatility of coal liquids has been experimentally determined at 700-880 F and about 2000 psia. These measurements were made in a flow apparatus to minimize thermal decomposition effects at high temperatures. Three coal liquids in mixture with Hat2, methane, and Hat2S were investigated. Measurements were also made up to 900 F on the vapor pressure of pure compounds found in coal liquids and on the equilibrium pressure of narrow coal liquid cuts. These data were used to develop a new method for the prediction of the critical point and the superatmospheric vapour pressures of aromatic fractions that is superior to the Maxwell-Bonnell correlation. The VLE data on coal liquids and some recent high-temperature VLE data on binaries of aromatics with Hat2 or methane were analyzed with a modified Chao-Seader correlation and a modified Redlich-Kwong equation of state. Both VLE correlations are shown to be equivalent in the prediction of the volatility of coal liquids, when the new vapour pressure procedure is used.

  13. Micellar liquid chromatography

    International Nuclear Information System (INIS)

    Basova, Elena M; Ivanov, Vadim M; Shpigun, Oleg A

    1999-01-01

    Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

  14. Stability analysis of high temperature superconducting coil in liquid hydrogen

    International Nuclear Information System (INIS)

    Nakayama, T.; Yagai, T.; Tsuda, M.; Hamajima, T.

    2007-01-01

    Recently, it is expected that hydrogen plays an important role in energy source including electric power in near future. Liquid hydrogen has high potential for cooling down superconducting coil wound with high temperature superconductors (HTS), such as BSCCO, YBCO. In this paper, we study stabilities of the coils wound with BSCCO tapes, which are immersed in the liquid hydrogen, and compare stability results with those cooled by liquid helium. We treat a minimum propagation zone (MPZ) theory to evaluate the coil stability considering boiling heat flux of the liquid hydrogen, and specific heat, heat conduction and resistivity of HTS materials as a function of temperature. It is found that the coil cooled by the liquid hydrogen has higher stability margin than that cooled by the liquid helium. We compare the stability margins of both coils wound with Bi-2223/Ag tape and Bi-2212/Ag tape in liquid hydrogen. As a result, it is found that the stability of Bi-2212 coil is equivalent to that of Bi-2223 coil in low and high magnetic field, while the maximum current of Bi-2212 coil exceeds a little bit that of Bi-2223 coil in both magnetic fields

  15. A High Temperature Liquid Plasma Model of the Sun

    Directory of Open Access Journals (Sweden)

    Robitaille P.-M.

    2007-01-01

    Full Text Available In this work, a liquid model of the Sun is presented wherein the entire solar mass is viewed as a high density/high energy plasma. This model challenges our current understanding of the densities associated with the internal layers of the Sun, advocating a relatively constant density, almost independent of radial position. The incompressible nature of liquids is advanced to prevent solar collapse from gravitational forces. The liquid plasma model of the Sun is a non-equilibrium approach, where nuclear reactions occur throughout the solar mass. The primary means of addressing internal heat transfer are convection and conduction. As a result of the convective processes on the solar surface, the liquid model brings into question the established temperature of the solar photosphere by highlighting a violation of Kirchhoff’s law of thermal emission. Along these lines, the model also emphasizes that radiative emission is a surface phenomenon. Evidence that the Sun is a high density/high energy plasma is based on our knowledge of Planckian thermal emission and condensed matter, including the existence of pressure ionization and liquid metallic hydrogen at high temperatures and pressures. Prior to introducing the liquid plasma model, the historic and scientific justifications for the gaseous model of the Sun are reviewed and the gaseous equations of state are also discussed.

  16. Levitation apparatus for neutron diffraction investigations on high temperature liquids

    International Nuclear Information System (INIS)

    Hennet, Louis; Pozdnyakova, Irina; Bytchkov, Aleksei; Cristiglio, Viviana; Palleau, Pierre; Fischer, Henry E.; Cuello, Gabriel J.; Johnson, Mark; Melin, Philippe; Zanghi, Didier; Brassamin, Severine; Brun, Jean-Francois; Price, David L.; Saboungi, Marie-Louise

    2006-01-01

    We describe a new high temperature environment based on aerodynamic levitation and laser heating designed for neutron scattering experiments up to 3000 deg. C. The sample is heated to the desired temperature with three CO 2 lasers from different directions in order to obtain a homogeneous temperature distribution. The apparent temperature of the sample is measured with an optical pyrometer, and two video cameras are employed to monitor the sample behavior during heating. The levitation setup is enclosed in a vacuum-tight chamber, enabling a high degree of gas purity and a reproducible sample environment for structural investigations on both oxide and metallic melts. High-quality neutron diffraction data have been obtained on liquid Y 3 Al 5 O 12 and ZrNi alloy for relatively short counting times (1.5 h)

  17. Trial manufacture of liquid nitrogen cooling High Temperature Superconductivity Motor

    International Nuclear Information System (INIS)

    Sugimoto, H; Nishikawa, T; Tsuda, T; Hondou, Y; Akita, Y; Takeda, T; Okazaki, T; Ohashi, S; Yoshida, Y

    2006-01-01

    We present a new high temperature superconductivity (HTS) synchronous motor using the liquid nitrogen as the refrigerant in this paper. This motor is designed to be used as the propulsion motor in ship. Because we use the liquid nitrogen as the refrigerant, it is possible to simplify the cooling equipments in the motor. And in our design, we apply the axial flux type of motor to simplify the cryostat of the HTS wires used to make the field coils. Here, the fields using the bismuth HTS wire for the HTS coils are fixed. Moreover, the cores used in the fields are separated from cryostat, and the armature applies the core-less structure. According to various the electromagnetic field analysis results, the new motor was designed and produced. The diameter of the motor is 650mm, and the width of the motor is 360mm. The motor's rated output is 8.8kW at 100rpm, while the overload output is 44kW, and the maximum efficiency is 97.7%. Also, in order to further miniaturize the motor, other magnetic field analysis have been done when the high-current-density type HTS wire was used and the permendur was used instead of magnetic steel plates. In this case, the motor's rated output is 12kW, and the overload output is 60kW

  18. Ionic liquid stationary phases for gas chromatography.

    Science.gov (United States)

    Poole, Colin F; Poole, Salwa K

    2011-04-01

    This article provides a summary of the development of ionic liquids as stationary phases for gas chromatography beginning with early work on packed columns that established details of the retention mechanism and established working methods to characterize selectivity differences compared with molecular stationary phases through the modern development of multi-centered cation and cross-linked ionic liquids for high-temperature applications in capillary gas chromatography. Since there are many reviews on ionic liquids dealing with all aspects of their chemical and physical properties, the emphasis in this article is placed on the role of gas chromatography played in the design of ionic liquids of low melting point, high thermal stability, high viscosity, and variable selectivity for separations. Ionic liquids provide unprecedented opportunities for extending the selectivity range and temperature-operating range of columns for gas chromatography, an area of separation science that has otherwise been almost stagnant for over a decade. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Introduction to modern liquid chromatography

    National Research Council Canada - National Science Library

    Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

    2010-01-01

    "High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

  20. Neutronics of a liquid salt cooled - very high temperature reactor

    International Nuclear Information System (INIS)

    Zakova, J.

    2007-01-01

    During last few years, the interest in the innovative, Liquid Salt cooled - Very High Temperature Reactor (LS-VHTR), has been growing. The preconceptual design of the LS-VHTR was suggested in Oak Ridge National Laboratory (ORNL) [1] and nowadays, several research institutions contribute to the development of this concept. The LS-VHTR design utilises a prismatic, High Temperature Reactor (HTR) fuel [2] in combination with liquid salt as a coolant. This connection of high-performance fuel and a coolant with enhanced heat transfer abilities enables efficient and economical operation. Main objective of the LS-VHTR operation may be either an efficient electricity production or a heat supply for a production of hydrogen or, combination of both. The LS-VHTR is moderated by graphite. The graphite matrix of the fuel blocks, as well as the inner and outer core reflectors serve as a thermal buffer in case of an accident, and they provide a strong thermal feedback during normal reactor operation. The high inherent safety of the LS-VHTR meets the strict requirements on future reactor systems, as defined by the Gen IV project. This work, purpose, scope, contribution to the state-of-art: The design, used in the present work is based on the first ORNL suggestion [1]. Recent study is focused on comparison of the neutronic performance of two types of fuel in the LS-VHTR core, whereas, in all previous works, only uranium fuel has been investigated. The first type of fuel, which has been employed in the present analysis, is based on the spent Light Water Reactor (LWR) fuel, whereas the second one consists of enriched uranium oxide. The results of such a comparison bring a valuable knowledge about limits and possibilities of the LS-VHTR concept, when employed as a spent fuel burner. Method:It is used a 3-D drawing of the LS-VHTR core, which contains 324x10 hexagonal fuel blocks. Each fuel block contains 216x10 fuel pins, which consists of TRISO particles incorporated into a graphite

  1. Study of flow fractionation characteristics of magnetic chromatography utilizing high-temperature superconducting bulk magnet

    Directory of Open Access Journals (Sweden)

    Satoshi Fukui, Yoshihiro Shoji, Jun Ogawa, Tetsuo Oka, Mitsugi Yamaguchi, Takao Sato, Manabu Ooizumi, Hiroshi Imaizumi and Takeshi Ohara

    2009-01-01

    Full Text Available We present numerical simulation of separating magnetic particles with different magnetic susceptibilities by magnetic chromatography using a high-temperature superconducting bulk magnet. The transient transport is numerically simulated for two kinds of particles having different magnetic susceptibilities. The time evolutions were calculated for the particle concentration in the narrow channel of the spiral arrangement placed in the magnetic field. The field is produced by the highly magnetized high-temperature superconducting bulk magnet. The numerical results show the flow velocity difference of the particle transport corresponding to the difference in the magnetic susceptibility, as well as the possible separation of paramagnetic particles of 20 nm diameter.

  2. Study of flow fractionation characteristics of magnetic chromatography utilizing high-temperature superconducting bulk magnet.

    Science.gov (United States)

    Fukui, Satoshi; Shoji, Yoshihiro; Ogawa, Jun; Oka, Tetsuo; Yamaguchi, Mitsugi; Sato, Takao; Ooizumi, Manabu; Imaizumi, Hiroshi; Ohara, Takeshi

    2009-02-01

    We present numerical simulation of separating magnetic particles with different magnetic susceptibilities by magnetic chromatography using a high-temperature superconducting bulk magnet. The transient transport is numerically simulated for two kinds of particles having different magnetic susceptibilities. The time evolutions were calculated for the particle concentration in the narrow channel of the spiral arrangement placed in the magnetic field. The field is produced by the highly magnetized high-temperature superconducting bulk magnet. The numerical results show the flow velocity difference of the particle transport corresponding to the difference in the magnetic susceptibility, as well as the possible separation of paramagnetic particles of 20 nm diameter.

  3. Universality of the high-temperature viscosity limit of silicate liquids

    DEFF Research Database (Denmark)

    Zheng, Qiuju; Mauro, John C.; Ellison, Adam J.

    2011-01-01

    We investigate the high-temperature limit of liquid viscosity by analyzing measured viscosity curves for 946 silicate liquids and 31 other liquids including metallic, molecular, and ionic systems. Our results show no systematic dependence of the high-temperature viscosity limit on chemical...... composition for the studied liquids. Based on theMauro-Yue-Ellison-Gupta-Allan (MYEGA) model of liquid viscosity, the high-temperature viscosity limit of silicate liquids is 10−2.93 Pa·s. Having established this value, there are only two independent parameters governing the viscosity-temperature relation...

  4. Towards a semiquantitative non invasive characterisation of Tyrian purple dye composition: Convergence of UV-Visible reflectance spectroscopy and fast-high temperature-high performance liquid chromatography with photodiode array detection.

    Science.gov (United States)

    Clementi, Catia; Nowik, Witold; Romani, Aldo; Cardon, Dominique; Trojanowicz, Marek; Davantès, Athénaïs; Chaminade, Pierre

    2016-07-05

    In this paper, partial least square (PLS) regression is innovatively applied for a semi-quantitative non invasive study of the most precious dye of Antiquity: Tyrian purple. This original approach for the study of organic dyes in the cultural heritage field, is based on the correlation of spectrophotometric (UV-Visible) and chromatographic (Fast-HT-HPLC-PDA) data from an extensive set of textiles prepared with different snail species according to historical recipes. A cross-validated PLS model, based on the quantity of 6,6'-dibromoindigotin, displays an excellent correlation factor (R(2)Y = 0.987) between values determined by chromatography and those predicted from reflectance spectra. This indicates that the spectral features of Tyrian purple on textile fibre is strictly related to the amount of this indigoid component whose content may be non invasively predicted from reflectance spectrum. The studied correlation also highlights that, independently of the dyeing method and nature of the textile fibre used, the relative content of 6,6'-dibromindigotin may be used as a parameter to distinguish samples prepared with Hexaplex trunculus L. snails from those prepared with further mollusc species. To validate this model, archaeological textile fragments dating from the Roman period were successfully examined. The results achieved open an absolutely new way in Tyrian purple analysis in cultural heritage by non invasive spectroscopic techniques attesting their convergence with HPLC and giving them a semi-quantitative value. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Liquid chromatography in migration studies

    International Nuclear Information System (INIS)

    Carlsen, L.; Batsberg, W.

    1982-01-01

    Liquid chromatography ahs been suggested as a facile experimental technique to determine important physico-chemical properties, as permeability, porosity, dispersion-, diffusion-, and sorption charcteristics for geological material as chalk samples. The feasibility of the trechnique as a rapid method to evaluate the possible influence of changes in ground water composition on the migration behavior of radionuclides has been demonstrated

  6. Liquid phase chromatography on microchips

    DEFF Research Database (Denmark)

    Kutter, Jörg Peter

    2012-01-01

    explosive development of, in particular, chromatographic separation systems on microchips, has, however, slowed down in recent years. This review takes a closer, critical look at how liquid phase chromatography has been implemented in miniaturized formats over the past several years, what is important...

  7. NCTM of liquids at high temperatures using polarization techniques

    Science.gov (United States)

    Krishnan, Shankar; Weber, J. K. Richard; Nordine, Paul C.; Schiffman, Robert A.

    1990-01-01

    Temperature measurement and control is extremely important in any materials processing application. However, conventional techniques for non-contact temperature measurement (mainly optical pyrometry) are very uncertain because of unknown or varying surface emittance. Optical properties like other properties change during processing. A dynamic, in-situ measurement of optical properties including the emittance is required. Intersonics is developing new technologies using polarized laser light scattering to determine surface emittance of freely radiating bodies concurrent with conventional optical pyrometry. These are sufficient to determine the true surface temperature of the target. Intersonics is currently developing a system called DAPP, the Division of Amplitude Polarimetric Pyrometer, that uses polarization information to measure the true thermodynamic temperature of freely radiating objects. This instrument has potential use in materials processing applications in ground and space based equipment. Results of thermophysical and thermodynamic measurements using laser reflection as a temperature measuring tool are presented. The impact of these techniques on thermophysical property measurements at high temperature is discussed.

  8. Ionic liquids and ionic liquid acids with high temperature stability for fuel cell and other high temperature applications, method of making and cell employing same

    Science.gov (United States)

    Angell, C Austen [Mesa, AZ; Xu, Wu [Broadview Heights, OH; Belieres, Jean-Philippe [Chandler, AZ; Yoshizawa, Masahiro [Tokyo, JP

    2011-01-11

    Disclosed are developments in high temperature fuel cells including ionic liquids with high temperature stability and the storage of inorganic acids as di-anion salts of low volatility. The formation of ionically conducting liquids of this type having conductivities of unprecedented magnitude for non-aqueous systems is described. The stability of the di-anion configuration is shown to play a role in the high performance of the non-corrosive proton-transfer ionic liquids as high temperature fuel cell electrolytes. Performance of simple H.sub.2(g) electrolyte/O.sub.2(g) fuel cells with the new electrolytes is described. Superior performance both at ambient temperature and temperatures up to and above 200.degree. C. are achieved. Both neutral proton transfer salts and the acid salts with HSO.sup.-.sub.4 anions, give good results, the bisulphate case being particularly good at low temperatures and very high temperatures. The performance of all electrolytes is improved by the addition of a small amount of involatile base of pK.sub.a value intermediate between those of the acid and base that make the bulk electrolyte. The preferred case is the imidazole-doped ethylammonium hydrogensulfate which yields behavior superior in all respects to that of the industry standard phosphoric acid electrolyte.

  9. Study on boiling heat transfer of high temperature liquid sodium

    International Nuclear Information System (INIS)

    Sakurai, Akira

    1978-01-01

    In the Intitute of Atomic Energy, Kyoto University, fundamental studies on steady state and non-steady state heat flow are underway in connection with reactor design and the safety in a critical accident in a sodium-cooled fast breeder reactor. First, the experimental apparatus for sodium heat transfer and the testing system are described in detail. The apparatus is composed of sodium-purifying section including the plugging meter for measuring purity and cold trap, the pool boiling test section for experimenting natural convection boiling heat transfer, the forced convection boiling test section for experimenting forced convection boiling heat transfer, and gas system. Next, the experimental results by the author and the data obtained so far are compared regarding heat transfer in sodium natural convection and stable nucleating boiling and critical heat flux. The effect of liquid head on a heater on boiling heat transfer coefficient and critical heat flux under the condition of low system pressure in most fundamental pool boiling was elucidated quantitatively, which has been overlooked in previous studies. It was clarified that this is the essentially important problem that can not be overlooked. From this point of view, expressions on heat transfer were also re-investigated. (Wakatsuki, Y.)

  10. Some new fatigue tests in high temperature water and liquid sodium environment

    International Nuclear Information System (INIS)

    Hattori, Takahiro; Yamauchi, Takayoshi; Kanasaki, Hiroshi; Kondo, Yoshiyuki; Endo, Tadayoshi.

    1987-01-01

    To evaluate the fatigue strength of structural materials for PWR or FBR plants, fatigue test data must be obtained in an environment of simulated primary and secondary water for PWR or of high temperature liquid sodium for FBR. Generally, such tests make it necessary to prepare expensive facilities, so when large amount of fatigue data are required, it is necessary to rationalize and simplify the fatigue tests while maintaining high accuracy. At the Takasago Research Development Center, efforts to rationalize facilities and maintain accuracy in fatigue tests have been made by developing new test methods and improving conventional techniques. This paper introduces a new method of low cycle fatigue test in high temperature water, techniques for automatic measurement of crack initiation and propagation in high temperature water environment and a multiple type fatigue testing machine for high temperature liquid sodium. (author)

  11. The use of on-line ion chromatography for high temperature and high pressure reaction studies

    International Nuclear Information System (INIS)

    Lynch, G.J.

    1993-10-01

    This paper describes the use of on-line ion chromatography as a tool for chemistry reaction studies in small volume systems. The technique was used to study chemistry behavior in a high temperature and high pressure autoclave system. A dual analyzer, multi-channel on-line ion chromatograph (IC) was configured to automate the sampling and analysis. Analytical channels were set up for analysis of inorganic anions, monovalent cations, conductivity, and pH. Conductivity and pH were measured using the IC as a flow injection analyzer. Use of the IC system provides significant advantages over conventional sampling and analysis techniques: Reduction in sample volume, a closed sampling system that protects air or light sensitive analytes from breakdown, around-the-clock test performance combined with automatic calibration and quality control checking, and detection and tracking of reaction products or unexpected contaminants. Methods used to correct measured concentrations for the effects of sampling and for calculation of control chemical loss half-lives are presented. A limited evaluation of the flow injection analysis methods for conductivity and pH is provided

  12. High-temperature vitrification of Hanford residual-liquid waste in a continuous melter

    International Nuclear Information System (INIS)

    Barnes, S.M.

    1980-04-01

    Over 270 kg of high-temperature borosilicate glass have been produced in a series of three short-term tests in the High-Temperature Ceramic Melter vitrification system at PNL. The glass produced was formulated to vitrify simulated Hanford residual-liquid waste. The tests were designed to (1) demonstrate the feasibility of utilizing high-temperature, continuous-vitrification technology for the immobilization of the residual-liquid waste, (2) test the airlift draining technique utilized by the high-temperature melter, (3) compare glass produced in this process to residual-liquid glass produced under laboratory conditions, (4) investigate cesium volatility from the melter during waste processing, and (5) determine the maximum residual-liquid glass production rate in the high-temperature melter. The three tests with the residual-liquid composition confirmed the viability of the continuous-melting vitrification technique for the immobilization of this waste. The airlift draining technique was demonstrated in these tests and the glass produced from the melter was shown to be less porous than the laboratory-produced glass. The final glass produced from the second test was compared to a glass of the same composition produced under laboratory conditions. The comparative tests found the glasses to be indistinguishable, as the small differences in the test results fell within the precision range of the characterization testing equipment. The cesium volatility was examined in the final test. This examination showed that 0.44 wt % of the cesium (assumed to be cesium oxide) was volatilized, which translates to a volatilization rate of 115 mg/cm 2 -h

  13. Chemical composition separation of a propylene-ethylene random copolymer by high temperature solvent gradient interaction chromatography.

    Science.gov (United States)

    Liu, Yonggang; Phiri, Mohau Justice; Ndiripo, Anthony; Pasch, Harald

    2017-11-03

    A propylene-ethylene random copolymer was fractionated by preparative temperature rising elution fractionation (TREF). The structural heterogeneity of the bulk sample and its TREF fractions was studied by high temperature liquid chromatography with a solvent gradient elution from 1-decanol to 1,2,4-trichlorobenzene. HPLC alone cannot resolve those propylene-ethylene copolymers with high ethylene content in the bulk sample, due to their low weight fractions in the bulk sample and a small response factor of these components in the ELSD detector, as well as their broad chemical composition distribution. These components can only be detected after being separated and enriched by TREF followed by HPLC analysis. Chemical composition separations were achieved for TREF fractions with average ethylene contents between 2.1 and 22.0mol%, showing that copolymers with higher ethylene contents were adsorbed stronger in the Hypercarb column and eluted later. All TREF fractions, except the 40°C fraction, were relatively homogeneous in both molar mass and chemical composition. The 40°C fraction was rather broad in both molar mass and chemical composition distributions. 2D HPLC showed that the molar masses of the components containing more ethylene units were getting lower for the 40°C fraction. HPLC revealed and confirmed that co-crystallization influences the separation in TREF of the studied propylene-ethylene copolymer. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. [High-performance liquid-liquid chromatography in beverage analysis].

    Science.gov (United States)

    Bricout, J; Koziet, Y; de Carpentrie, B

    1978-01-01

    Liquid liquid chromatography was performed with columns packed with stationary phases chemically bonded to silica microparticules. These columns show a high efficiency and are used very easily. Flavouring compounds like aromatic aldehydes which have a low volatility were analyzed in brandy using a polar phase alkylnitrile. Sapid substances like amarogentin in Gentiana lutea or glyryrrhizin in Glycyrrhiza glabra were determined by reversed phase chromatography. Finally ionizable substances like synthetic dyes can be analyzed by paired ion chromatography witha non polar stationary phase.

  15. The Advanced High-Temperature Reactor (AHTR) for Producing Hydrogen to Manufacture Liquid Fuels

    International Nuclear Information System (INIS)

    Forsberg, C.W.; Peterson, P.F.; Ott, L.

    2004-01-01

    Conventional world oil production is expected to peak within a decade. Shortfalls in production of liquid fuels (gasoline, diesel, and jet fuel) from conventional oil sources are expected to be offset by increased production of fuels from heavy oils and tar sands that are primarily located in the Western Hemisphere (Canada, Venezuela, the United States, and Mexico). Simultaneously, there is a renewed interest in liquid fuels from biomass, such as alcohol; but, biomass production requires fertilizer. Massive quantities of hydrogen (H2) are required (1) to convert heavy oils and tar sands to liquid fuels and (2) to produce fertilizer for production of biomass that can be converted to liquid fuels. If these liquid fuels are to be used while simultaneously minimizing greenhouse emissions, nonfossil methods for the production of H2 are required. Nuclear energy can be used to produce H2. The most efficient methods to produce H2 from nuclear energy involve thermochemical cycles in which high-temperature heat (700 to 850 C) and water are converted to H2 and oxygen. The peak nuclear reactor fuel and coolant temperatures must be significantly higher than the chemical process temperatures to transport heat from the reactor core to an intermediate heat transfer loop and from the intermediate heat transfer loop to the chemical plant. The reactor temperatures required for H2 production are at the limits of practical engineering materials. A new high-temperature reactor concept is being developed for H2 and electricity production: the Advanced High-Temperature Reactor (AHTR). The fuel is a graphite-matrix, coated-particle fuel, the same type that is used in modular high-temperature gas-cooled reactors (MHTGRs). The coolant is a clean molten fluoride salt with a boiling point near 1400 C. The use of a liquid coolant, rather than helium, reduces peak reactor fuel and coolant temperatures 100 to 200 C relative to those of a MHTGR. Liquids are better heat transfer fluids than gases

  16. Molecular Dynamics Simulations of Liquid Phosphorus at High Temperature and Pressure

    International Nuclear Information System (INIS)

    Wu Yanning; Zhao Gang; Liu Changsong; Zhu Zhengang

    2008-01-01

    By performing ab initio molecular dynamics simulations, we have investigated the microstructure, dynamical and electronic properties of liquid phosphorus (P) under high temperature and pressure. In our simulations, the calculated coordination number (CN) changes discontinuously with density, and seems to increase rapidly after liquid P is compressed to 2.5 g/cm 3 . Under compression, liquid P shows the first-order liquid-liquid phase transition from the molecular liquid composed of the tetrahedral P 4 molecules to complex polymeric form with three-dimensional network structure, accompanied by the nonmetal to metal transition of the electronic structure. The order parameters Q 6 and Q 4 are sensitive to the microstructural change of liquid P. By calculating diffusion coefficients, we show the dynamical anomaly of liquid P by compression. At lower temperatures, a maximum exists at the diffusion coefficients as a function of density; at higher temperatures, the anomalous behavior is weakened. The excess entropy shows the same phenomena as the diffusion coefficients. By analysis of the angle distribution functions and angular limited triplet correlation functions, we can clearly find that the Peierls distortion in polymeric form of liquid P is reduced by further compression

  17. Gradient High Performance Liquid Chromatography Method ...

    African Journals Online (AJOL)

    Purpose: To develop a gradient high performance liquid chromatography (HPLC) method for the simultaneous determination of phenylephrine (PHE) and ibuprofen (IBU) in solid ..... nimesulide, phenylephrine. Hydrochloride, chlorpheniramine maleate and caffeine anhydrous in pharmaceutical dosage form. Acta Pol.

  18. Thermal diffusivity measurements of liquid materials at high temperature with the ''laser flash'' method

    International Nuclear Information System (INIS)

    Otter, Claude; Vandevelde, Jean

    1982-01-01

    Two solutions, one analytical and the other numerical are proposed to solve the thermokinetic problem encountered when measuring the thermal diffusivity of liquid materials at very high temperature (T>3123K). The liquid material is contained in a parallel faced vessel. This liquid is traversed by a short thermal pulse from a relaxed laser. The temperature response of the back face of the measurement cell is analysed. The first model proposed which does not take thermal losses into consideration, is a mathematical model derived from the ''two layer model'' (Larson and Koyama, 1968) extended to ''three layers''. In order to take the possibility of thermal losses to the external environment at high temperature into consideration, a Crank-Nicolson (1947) type numerical model utilizing finite differences is employed. These thermokinetic studies were performed in order to interpret temperature response curves obtained from the back face of a tungsten-liquid UO 2 -tungsten thermal wall, the purpose of the measurements made being to determine the thermal properties of liquid uranium oxide [fr

  19. Pumping liquid metal at high temperatures up to 1,673 kelvin

    Science.gov (United States)

    Amy, C.; Budenstein, D.; Bagepalli, M.; England, D.; Deangelis, F.; Wilk, G.; Jarrett, C.; Kelsall, C.; Hirschey, J.; Wen, H.; Chavan, A.; Gilleland, B.; Yuan, C.; Chueh, W. C.; Sandhage, K. H.; Kawajiri, Y.; Henry, A.

    2017-10-01

    Heat is fundamental to power generation and many industrial processes, and is most useful at high temperatures because it can be converted more efficiently to other types of energy. However, efficient transportation, storage and conversion of heat at extreme temperatures (more than about 1,300 kelvin) is impractical for many applications. Liquid metals can be very effective media for transferring heat at high temperatures, but liquid-metal pumping has been limited by the corrosion of metal infrastructures. Here we demonstrate a ceramic, mechanical pump that can be used to continuously circulate liquid tin at temperatures of around 1,473-1,673 kelvin. Our approach to liquid-metal pumping is enabled by the use of ceramics for the mechanical and sealing components, but owing to the brittle nature of ceramics their use requires careful engineering. Our set-up enables effective heat transfer using a liquid at previously unattainable temperatures, and could be used for thermal storage and transport, electric power production, and chemical or materials processing.

  20. UHPLC: The Greening Face of Liquid Chromatography

    OpenAIRE

    Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

  1. An Unexpected Reaction between 5-Hydroxymethylfurfural and Imidazolium-Based Ionic Liquids at High Temperatures

    Directory of Open Access Journals (Sweden)

    Zongbao K. Zhao

    2011-10-01

    Full Text Available A new compound was detected during the production of 5-hydroxymethylfurfural (HMF from glucose and cellulose in the ionic liquid 1-butyl-3-methylimidazolium chloride ([Bmim]Cl at high temperatures. Further experiments found that it was derived from the reaction of HMF with [Bmim]Cl. The structure of new compound was established as 1-butyl-2-(5’-methyl-2’-furoylimidazole (BMI based on nuclear magnetic resonance and mass spectrometry analysis, and a possible mechanism for its formation was proposed. Reactions of HMF with other imidazolium-based ionic liquids were performed to check the formation of BMI. Our results provided new insights in terms of side reactions between HMF and imidazolium-based ionic liquids, which should be valuable for designing better processes for the production of furans using biomass and related materials.

  2. In-situ high-temperature Raman spectroscopic studies of aluminosilicate liquids

    Science.gov (United States)

    Daniel, Isabelle; Gillet, Philippe; Poe, Brent T.; McMillan, Paul F.

    1995-03-01

    We have measured in-situ Raman spectra of aluminosilicate glasses and liquids with albite (NaAlSi3 O8) and anorthite (CaAl2Si2O8) compositions at high temperatures, through their glass transition range up to 1700 and 2000 K, respectively. For these experiments, we have used a wire-loop heating device coupled with micro-Raman spectroscopy, in order to achieve effective spatial filtering of the extraneous thermal radiation. A major concern in this work is the development of methodology for reliably extracting the first and second order contributions to the Raman scattering spectra of aluminosilicate glasses and liquids from the high temperature experimental data, and analyzing these in terms of vibrational (anharmonic) and configurational changes. The changes in the first order Raman spectra with temperature are subtle. The principal low frequency band remains nearly constant with increasing temperature, indicating little change in the T-O-T angle, and that the angle bending vibration is quite harmonic. This is in contrast to vitreous SiO2, studied previously. Above Tg, intensity changes in the 560 590 cm-1 regions of both sets of spectra indicate configurational changes in the supercooled liquids, associated with formation of additional Al-O-Al linkages, or 3-membered (Al, Si)-containing rings. Additional intensity at 800 cm-1 reflects also some rearrangement of the Si-O-Al network.

  3. Experimental evaluation of permanent magnet probe flowmeter measuring high temperature liquid sodium flow in the ITSL

    Energy Technology Data Exchange (ETDEWEB)

    Jeong, Uiju; Kim, Yun Ho [Nuclear engineering Department, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Kim, Jong-Man; Kim, Tae-Joon [Korea Atomic Energy Research Institute, 1045 Daedeok-daero, Yuseong-gu, Daejeon 305-353 (Korea, Republic of); Kim, Sung Joong, E-mail: sungjkim@mit.edu [Nuclear engineering Department, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of)

    2013-12-15

    Highlights: • An Instrument Test Sodium Loop (ITSL) has been built and tested in various conditions at KAERI. • Free fall of liquid sodium was conducted experimentally and numerically. • A Permanent Magnet Probe Flowmeter (PMPF) was experimented in the ITSL. • Excellent linearity of the PMPF was achieved under high temperature condition. - Abstract: The Instrument Test Sodium Loop (ITSL) installed at Korea Atomic Energy Research Institute (KAERI) is a medium-size experimental facility dedicated to obtaining relevant experimental data of liquid sodium flow characteristics under various thermal hydraulic conditions and sodium purification. The ITSL has been utilized to perform thermal flow measurement of the liquid sodium and to calibrate a Permanent Magnet Probe Flowmeter (PMPF). The primary objective of this study is to obtain liquid sodium flow rate given a wide temperature range using the PMPF. Non-stationary method was adopted for the calibration of the probe given the liquid sodium temperature range of 150–415 °C. A relationship between the measured voltage signal and flow rate was obtained successfully. It is observed that the calibration experiments result in excellent linear relationships between measured voltage and volumetric flow rate at various temperature conditions. Also a computational analysis using FlowMaster, is employed to facilitate the calibration process by predicting the liquid sodium flow rate. Finally the effect of the fluid temperature on thermal flow measurements is discussed in light of the obtained experimental data.

  4. High-temperature reactors for underground liquid-fuels production with direct carbon sequestration

    International Nuclear Information System (INIS)

    Forsberg, C. W.

    2008-01-01

    The world faces two major challenges: (1) reducing dependence on oil from unstable parts of the world and (2) minimizing greenhouse gas emissions. Oil provides 39% of the energy needs of the United States, and oil refineries consume over 7% of the total energy. The world is running out of light crude oil and is increasingly using heavier fossil feedstocks such as heavy oils, tar sands, oil shale, and coal for the production of liquid fuels (gasoline, diesel, and jet fuel). With heavier feedstocks, more energy is needed to convert the feedstocks into liquid fuels. In the extreme case of coal liquefaction, the energy consumed in the liquefaction process is almost twice the energy value of the liquid fuel. This trend implies large increases in carbon dioxide releases per liter of liquid transport fuel that is produced. It is proposed that high-temperature nuclear heat be used to refine hydrocarbon feedstocks (heavy oil, tar sands, oil shale, and coal) 'in situ ', i.e., underground. Using these resources for liquid fuel production would potentially enable the United States to become an exporter of oil while sequestering carbon from the refining process underground as carbon. This option has become potentially viable because of three technical developments: precision drilling, underground isolation of geological formations with freeze walls, and the understanding that the slow heating of heavy hydrocarbons (versus fast heating) increases the yield of light oils while producing a high-carbon solid residue. Required peak reactor temperatures are near 700 deg. C-temperatures within the current capabilities of high-temperature reactors. (authors)

  5. Intermetallic and electrical insulator coatings on high-temperature alloys in liquid-lithium environments

    International Nuclear Information System (INIS)

    Park, J.H.

    1994-06-01

    In the design of liquid-metal cooling systems for fusion-reactor blanket, applications, the corrosion resistance of structural materials and the magnetohydrodynamic (MHD) force and its subsequent influence on thermal hydraulics and corrosion are major concerns. When the system is cooled by liquid metals, insulator coatings are required on piping surfaces in contact with the coolant. The objective of this study is to develop stable corrosion-resistant electrical insulator coatings at the liquid-metal/structural-material interface, with emphasis on electrically insulating coatings that prevent adverse MHD-generated currents from passing through the structural wall, and Be-V intermetallic coatings for first-wall components that face the plasma. Vanadium and V-base alloys are leading candidate materials for structural applications in a fusion reactor. Various intermetallic films were produced on V-alloys and on Types 304 and 316 stainless steel. The intermetallic layers were developed by exposure of the materials to liquid Li containing 2 at temperatures of 500--1030 degree C. CaO electrical insulator coatings were produced by reaction of the oxygen-rich layer with <5 at. % Ca dissolved in liquid Li at 400--700 degree C. The reaction converted the oxygen-rich layer to an electrically insulating film. This coating method is applicable to reactor components because the liquid metal can be used over and over; only the solute within the liquid metal is consumed. This paper will discuss initial results on the nature of the coatings and their in-situ electrical resistivity characteristics in liquid Li at high temperatures

  6. Liquid chromatography detection unit, system, and method

    Science.gov (United States)

    Derenzo, Stephen E.; Moses, William W.

    2015-10-27

    An embodiment of a liquid chromatography detection unit includes a fluid channel and a radiation detector. The radiation detector is operable to image a distribution of a radiolabeled compound as the distribution travels along the fluid channel. An embodiment of a liquid chromatography system includes an injector, a separation column, and a radiation detector. The injector is operable to inject a sample that includes a radiolabeled compound into a solvent stream. The position sensitive radiation detector is operable to image a distribution of the radiolabeled compound as the distribution travels along a fluid channel. An embodiment of a method of liquid chromatography includes injecting a sample that comprises radiolabeled compounds into a solvent. The radiolabeled compounds are then separated. A position sensitive radiation detector is employed to image distributions of the radiolabeled compounds as the radiolabeled compounds travel along a fluid channel.

  7. Fructose decomposition kinetics in organic acids-enriched high temperature liquid water

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yinghua; Lu, Xiuyang; Yuan, Lei; Liu, Xin [Department of Chemical and Biochemical Engineering, Zhejiang University, Zheda Road 38, Hangzhou 310027, Zhejiang (China)

    2009-09-15

    Biomass continues to be an important candidate as a renewable resource for energy, chemicals, and feedstock. Decomposition of biomass in high temperature liquid water is a promising technique for producing industrially important chemicals such as 5-hydroxymethylfurfural (5-HMF), furfural, levulinic acid with high efficiency. Hexose, which is the hydrolysis product of cellulose, will be one of the most important starting chemicals in the coming society that is highly dependent on biomass. Taking fructose as a model compound, its decomposition kinetics in organic acids-enriched high temperature liquid water was studied in the temperature range from 180 C to 220 C under the pressure of 10 MPa to further improve reaction rate and selectivity of the decomposition reactions. The results showed that the reaction rate is greatly enhanced with the addition of organic acids, especially formic acid. The effects of temperature, residence time, organic acids and their concentrations on the conversion of fructose and yield of 5-HMF were investigated. The evaluated apparent activation energies of fructose decomposition are 126.8 {+-} 3.3 kJ mol{sup -1} without any catalyst, 112.0 {+-} 13.7 kJ mol{sup -1} catalyzed with formic acid, and 125.6 {+-} 3.8 kJ mol{sup -1} catalyzed with acetic acid, respectively, which shows no significant difference. (author)

  8. Recovery time of high temperature superconducting tapes exposed in liquid nitrogen

    International Nuclear Information System (INIS)

    Sheng, Jie; Zeng, Weina; Yao, Zhihao; Zhao, Anfeng; Hu, Daoyu; Hong, Zhiyong

    2016-01-01

    Highlights: • A novel method based on a sequence of AC pulses is presented. • Liquid nitrogen temperature is used as criterion to judge whether the sample has recovered. • Recovery time of some tape doesn't increase with the amplitude of fault current. • This phenomenon is caused by boiling heat transfer process of liquid nitrogen. • This phenomenon can be used in optimizing both the limiting rate and reclosing system. - Abstract: The recovery time is a crucial parameter to high temperature superconducting tapes, especially in power applications. The cooperation between the reclosing device and the superconducting facilities mostly relies on the recovery time of the superconducting tapes. In this paper, a novel method is presented to measure the recovery time of several different superconducting samples. In this method criterion used to judge whether the sample has recovered is the liquid nitrogen temperature, instead of the critical temperature. An interesting phenomenon is observed during the testing of superconducting samples exposed in the liquid nitrogen. Theoretical explanations of this phenomenon are presented from the aspect of heat transfer. Optimization strategy of recovery characteristics based on this phenomenon is also briefly discussed.

  9. Thermophysical Properties Measurement of High-Temperature Liquids Under Microgravity Conditions in Controlled Atmospheric Conditions

    Science.gov (United States)

    Watanabe, Masahito; Ozawa, Shumpei; Mizuno, Akotoshi; Hibiya, Taketoshi; Kawauchi, Hiroya; Murai, Kentaro; Takahashi, Suguru

    2012-01-01

    Microgravity conditions have advantages of measurement of surface tension and viscosity of metallic liquids by the oscillating drop method with an electromagnetic levitation (EML) device. Thus, we are preparing the experiments of thermophysical properties measurements using the Materials-Science Laboratories ElectroMagnetic-Levitator (MSL-EML) facilities in the international Space station (ISS). Recently, it has been identified that dependence of surface tension on oxygen partial pressure (Po2) must be considered for industrial application of surface tension values. Effect of Po2 on surface tension would apparently change viscosity from the damping oscillation model. Therefore, surface tension and viscosity must be measured simultaneously in the same atmospheric conditions. Moreover, effect of the electromagnetic force (EMF) on the surface oscillations must be clarified to obtain the ideal surface oscillation because the EMF works as the external force on the oscillating liquid droplets, so extensive EMF makes apparently the viscosity values large. In our group, using the parabolic flight levitation experimental facilities (PFLEX) the effect of Po2 and external EMF on surface oscillation of levitated liquid droplets was systematically investigated for the precise measurements of surface tension and viscosity of high temperature liquids for future ISS experiments. We performed the observation of surface oscillations of levitated liquid alloys using PFLEX on board flight experiments by Gulfstream II (G-II) airplane operated by DAS. These observations were performed under the controlled Po2 and also under the suitable EMF conditions. In these experiments, we obtained the density, the viscosity and the surface tension values of liquid Cu. From these results, we discuss about as same as reported data, and also obtained the difference of surface oscillations with the change of the EMF conditions.

  10. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

  11. Electronic spectral detection in liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Biggs, Wilton R. [ChevronTexaco Chemical Co., P. O. Box 1627, Richmond, CA 94802 (United States); Fetzer, John C. [Fetzpahs Consulting, 1283 Santa Fe St., Hercules, CA 94547 (United States)

    2002-07-01

    The use of absorbance and fluorescence spectrometers as liquid chromatography detectors is described. These detectors offer sensitive detection that can also identify the peaks in a chromatogram. Many examples, mainly from the separation of polycyclic aromatic hydrocarbons, are given that show the selectivity and usefulness of these detectors. (orig.)

  12. Instrument platforms for nano liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-01-01

    Roč. 1421, NOV (2015), s. 2-17 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : nano liquid chromatography * splitless gradient generation * nano LC platforms Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0250900

  13. Instrument platforms for nano liquid chromatography.

    Science.gov (United States)

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-11-20

    The history of liquid chromatography started more than a century ago and miniaturization and automation are two leading trends in this field. Nanocolumn liquid chromatography (nano LC) and largely synonymous capillary liquid chromatography (capillary LC) are the most recent results of this process where miniaturization of column dimensions and sorbent particle size play crucial role. Very interesting results achieved in the research of extremely miniaturized LC columns at the end of the last century lacked distinctive raison d'être and only advances in mass spectrometry brought a real breakthrough. Configuration of nano LC-electrospray ionization mass spectrometry (LC-ESI-MS) has become a basic tool in bioanalytical chemistry, especially in proteomics. This review discusses and summarizes past and current trends in the realization of nano liquid chromatography (nano LC) platforms. Special attention is given to the mobile phase delivery under nanoflow rates (isocratic, gradient) and sample injection to the nanocolumn. Available detection techniques applied in nano LC separations are also briefly discussed. We followed up the key themes from the original scientific reports over gradual improvements up to the contemporary commercial solutions. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Ultra Performance Liquid Chromatography Tandem Mass ...

    African Journals Online (AJOL)

    NICOLAAS

    drugs alone.16. After a single oral dose of 120–800 mg of NTB in healthy sub- jects in a fasting state the peak plasma NTB concentration (tmax) was found to be 4–7 h, with a half-life of approximately 9–17 h.17 ... performance liquid chromatography mass spectrometry/mass .... to the likely biological plasma constituents.

  15. High temperature ultrasonic transducers for imaging and measurements in a liquid Pb/Bi eutectic alloy.

    Science.gov (United States)

    Kazys, Rymantas; Voleisis, Algirdas; Sliteris, Reimondas; Mazeika, Liudas; Van Nieuwenhove, Rudi; Kupschus, Peter; Abderrahim, Hamid Aït

    2005-04-01

    In some nuclear reactors or accelerator-driven systems (ADS) the core is intended to be cooled by means of a heavy liquid metal, for example, lead-bismuth (Pb/Bi) eutectic alloy. For safety and licensing reasons, an imaging method of the interior of ADS, based on application of ultrasonic waves, has thus to be developed. This paper is devoted to description of developed various ultrasonic transducers suitable for long term imaging and measurements in the liquid Pb/Bi alloy. The results of comparative experimental investigations of the developed transducers of different designs in a liquid Pb/Bi alloy up to 450 degrees C are presented. Prototypes with different high temperature piezoelectric materials were investigated: PZT, bismuth titanate (Bi4Ti3O12), lithium niobate (LiNbO3), gallium orthophosphate (GaPO4) and aluminum nitride (A1N). For acoustic coupling with the metal alloy, it was proposed to coat the active surface of the transducers by diamond like carbon (DLC). The radiation robustness was assessed by exposing the transducers to high gamma dose rates in one of the irradiation facilities at SCK x CEN. The experimental results proved that the developed transducers are suitable for long-term operation in harsh conditions.

  16. Preliminary design of high temperature ultrasonic transducers for liquid sodium environments

    Science.gov (United States)

    Prowant, M. S.; Dib, G.; Qiao, H.; Good, M. S.; Larche, M. R.; Sexton, S. S.; Ramuhalli, P.

    2018-04-01

    Advanced reactor concepts include fast reactors (including sodium-cooled fast reactors), gas-cooled reactors, and molten-salt reactors. Common to these concepts is a higher operating temperature (when compared to light-water-cooled reactors), and the proposed use of new alloys with which there is limited operational experience. Concerns about new degradation mechanisms, such as high-temperature creep and creep fatigue, that are not encountered in the light-water fleet and longer operating cycles between refueling intervals indicate the need for condition monitoring technology. Specific needs in this context include periodic in-service inspection technology for the detection and sizing of cracking, as well as technologies for continuous monitoring of components using in situ probes. This paper will discuss research on the development and evaluation of high temperature (>550°C; >1022°F) ultrasonic probes that can be used for continuous monitoring of components. The focus of this work is on probes that are compatible with a liquid sodium-cooled reactor environment, where the core outlet temperatures can reach 550°C (1022°F). Modeling to assess sensitivity of various sensor configurations and experimental evaluation have pointed to a preferred design and concept of operations for these probes. This paper will describe these studies and ongoing work to fabricate and fully evaluate survivability and sensor performance over extended periods at operational temperatures.

  17. Microstructural Evolution of Ni-Sn Transient Liquid Phase Sintering Bond during High-Temperature Aging

    Science.gov (United States)

    Feng, Hongliang; Huang, Jihua; Peng, Xianwen; Lv, Zhiwei; Wang, Yue; Yang, Jian; Chen, Shuhai; Zhao, Xingke

    2018-05-01

    For high-temperature-resistant packaging of new generation power chip, a chip packaging simulation structure of Ni/Ni-Sn/Ni was bonded by a transient liquid-phase sintering process. High-temperature aging experiments were carried out to investigate joint heat stability. The microstructural evolution and mechanism during aging, and mechanical properties after aging were analyzed. The results show that the 30Ni-70Sn bonding layer as-bonded at 340°C for 240 min is mainly composed of Ni3Sn4 and residual Ni particles. When aged at 350°C, because of the difficulty of nucleation for Ni3Sn and quite slow growth of Ni3Sn2, the bonding layer is stable and the strength of that doesn't change obviously with aging time. When aging temperature increased to 500°C, however, the residual Ni particles were gradually dissolved and the bonding layer formed a stable structure with dominated Ni3Sn2 after 36 h. Meanwhile, due to the volume shrinkage (4.43%) from Ni3Sn2 formation, a number of voids were formed. The shear strength shows an increase, resulting from Ni3Sn2 formation, but then it decreases slightly caused by voids. After aging at 500°C for 100 h, shear strength is still maintained at 29.6 MPa. In addition, the mechanism of void formation was analyzed and microstructural evolution model was also established.

  18. High Performance Liquid Chromatography Experiments to Undergraduate Laboratories

    Science.gov (United States)

    Kissinger, Peter T.; And Others

    1977-01-01

    Reviews the principles of liquid chromatography with electrochemical detection (LCEC), an analytical technique that incorporates the advantages of both liquids chromatography and electrochemistry. Also suggests laboratory experiments using this technique. (MLH)

  19. Development of a high performance liquid chromatography method ...

    African Journals Online (AJOL)

    Development of a high performance liquid chromatography method for simultaneous ... Purpose: To develop and validate a new low-cost high performance liquid chromatography (HPLC) method for ..... Several papers have reported the use of ...

  20. Optimizing separations in online comprehensive two‐dimensional liquid chromatography

    OpenAIRE

    Pirok, Bob W.J.; Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2017-01-01

    Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass...

  1. Comparative determination of phenytoin by spectrophotometry, gas chromatography, liquid chromatography, enzyme immunoassay, and radioimmunoassay

    International Nuclear Information System (INIS)

    Castro, A.; Ibanez, J.; DiCesare, J.L.; Adams, R.F.; Malkus, H.

    1978-01-01

    Sera from patients being treated with phenytoin were analyzed for the drug by spectrophotometry, gas chromatography, radioimmunoasay, enzyme immunoassay, and liquid chromatography. The assay values obtained were intercompared statistically. Enzyme immunoassay and liquid chromatography appear to be attractive alternatives to the more traditional methods of spectrophotometry and gas chromatography. Our radioimmunoassay data correlated poorly with results by the four other methods

  2. Design of Annular Linear Induction Pump for High Temperature Liquid Lead Transportation

    Energy Technology Data Exchange (ETDEWEB)

    Kwak, Jae Sik; Kim, Hee Reyoung [Ulsan National Institute of Science and Technology, Ulsan (Korea, Republic of)

    2014-05-15

    EM(Electro Magnetic) Pump is divided into two parts, which consisted of the primary one with electromagnetic core and exciting coils, and secondary one with liquid lead flow. The main geometrical variables of the pump included core length, inner diameter and flow gap while the electromagnetic ones covered pole pitch, turns of coil, number of pole pairs, input current and input frequency. The characteristics of design variables are analyzed by electrical equivalent circuit method taking into account hydraulic head loss in the narrow annular channel of the ALIP. The design program, which was composed by using MATLAB language, was developed to draw pump design variables according to input requirements of the flow rate, developing pressure and operation temperature from the analyses. The analysis on the design of ALIP for high temperature liquid lead transportation was carried for the produce of ALIP designing program based on MATLAB. By the using of ALIP designing program, we don't have to bother about geometrical relationship between each component during detail designing process because code calculate automatically. And prediction of outputs about designing pump can be done easily before manufacturing. By running the code, we also observe and analysis change of outputs caused by changing of pump factors. It will be helpful for the research about optimization of pump outputs.

  3. Analysis of oxidised heavy paraffininc products by high temperature comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Potgieter, H; Bekker, R; Beigley, J; Rohwer, E

    2017-08-04

    Heavy petroleum fractions are produced during crude and synthetic crude oil refining processes and they need to be upgraded to useable products to increase their market value. Usually these fractions are upgraded to fuel products by hydrocracking, hydroisomerization and hydrogenation processes. These fractions are also upgraded to other high value commercial products like lubricant oils and waxes by distillation, hydrogenation, and oxidation and/or blending. Oxidation of hydrogenated heavy paraffinic fractions produces high value products that contain a variety of oxygenates and the characterization of these heavy oxygenates is very important for the control of oxidation processes. Traditionally titrimetric procedures are used to monitor oxygenate formation, however, these titrimetric procedures are tedious and lack selectivity toward specific oxygenate classes in complex matrices. Comprehensive two-dimensional gas chromatography (GC×GC) is a way of increasing peak capacity for the comprehensive analysis of complex samples. Other groups have used HT-GC×GC to extend the carbon number range attainable by GC×GC and have optimised HT-GC×GC parameters for the separation of aromatics, nitrogen-containing compounds as well as sulphur-containing compounds in heavy petroleum fractions. HT-GC×GC column combinations for the separation of oxygenates in oxidised heavy paraffinic fractions are optimised in this study. The advantages of the HT-GC×GC method in the monitoring of the oxidation reactions of heavy paraffinic fraction samples are illustrated. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. A reactor/receiver-concept for liquid-phase high-temperature processes

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt-Traub, H.; Hahm, T. [Dortmund Univ. (Germany). Dept. of Chemical Engineering

    1997-12-31

    Besides the conversion of solar light to electricity solar energy can be used directly in photo- and thermochemistry. In the temperature range from 1000 to 2000 K there is a high demand for industrial process heat offering a variety of possibilities for solar thermal applications. Especially in the field of liquid-phase high-temperature processes there are hardly no solar thermal applications which exceed the stage of laboratory experiments. It was therefore the aim of two projects financed by the AG Solar of North Rhine-Westphalia, Germany, to develop concepts for commercial scale solar thermal plants and to judge them economically and ecologically. Some general problems have to be overcome to realize a commercial scale solar thermal plant for liquid-phase processes. The concept developed consists of a heliostat field, a tower reflector and an open receiver with a closed reaction chamber. The feasibility of a solar thermal plant for high-temperature liquid-phase processes has been shown in principle. The projected plant consists of a 4400 m{sup 2} heliostat field, a tower plus reflecting mirrors with a total area of 220 m{sup 2} and an open receiver with a closed annular reaction zone. For temperatures below 1700 K the overall efficiency is high enough to yield energetic amortization times of less than 1 year. For a further improvement and a verification of the calculation a closer look at the reactor/receiver and its heat transfer processes is necessary. This is done by using a mixed strategy of experiments and simulation. First experiments were carried out with a semitransparent salt and an opaque metal. The first stage of the experiments will end during the next weeks and their results have to be compared with the simulation. The simulation will then be extended to transparent melts. The second stage of the experiments which include the reaction chamber will start in 1997. An improvement of the reactor might be achieved using nonimaging concentrators to further

  5. High perfomance liquid chromatography in pharmaceutical analyses.

    Science.gov (United States)

    Nikolin, Branko; Imamović, Belma; Medanhodzić-Vuk, Saira; Sober, Miroslav

    2004-05-01

    In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatography replaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography (HPLC) analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1) Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or serum contains numerous endogenous

  6. Recent development of ionic liquid stationary phases for liquid chromatography.

    Science.gov (United States)

    Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

    2015-11-13

    Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. UHPLC: The Greening Face of Liquid Chromatography.

    Science.gov (United States)

    Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

  8. High performance liquid chromatography in pharmaceutical analyses

    Directory of Open Access Journals (Sweden)

    Branko Nikolin

    2004-05-01

    Full Text Available In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatographyreplaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography(HPLC analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1 Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or

  9. Ion exchange and liquid column chromatography

    International Nuclear Information System (INIS)

    Walton, H.F.

    1980-01-01

    Major accomplishments in liquid chromatography for the past two years and reported in journals available to December 31, 1979 are reviewed. Emphasis has been placed on principles and methodology with some representative examples of application included. Applications are illustrated in two rather lenghtly tables, one covering inorganic ions and the other covering organic compounds. 544 references, 8 books, and 15 reviews are listed in the bibliography

  10. Fabrication and performance evaluation of a high temperature co-fired ceramic vaporizing liquid microthruster

    International Nuclear Information System (INIS)

    Cheah, Kean How; Low, Kay-Soon

    2015-01-01

    This paper presents the study of a microelectromechanical system (MEMS)-scaled microthruster using ceramic as the structural material. A vaporizing liquid microthruster (VLM) has been fabricated using the high temperature co-fired ceramic (HTCC) technology. The developed microthruster consists of five components, i.e. inlet, injector, vaporizing chamber, micronozzle and microheater, all integrated in a chip with a dimension of 30 mm × 26 mm × 8 mm. In the dry test, the newly developed microheater which is deposited on zirconia substrate consumes 21% less electrical power than those deposited on silicon substrate to achieve a temperature of 100 °C. Heating temperature as high as 409.1 °C can be achieved using just 5 W of electrical power. For simplicity and safety, a functional test of the VLM with water as propellant has been conducted in the laboratory. Full vaporization of water propellant feeding at different flow rates has been successfully demonstrated. A maximum thrust of 633.5 µN at 1 µl s −1 propellant consumption rate was measured using a torsional thrust stand. (paper)

  11. Quasiparticles of strongly correlated Fermi liquids at high temperatures and in high magnetic fields

    International Nuclear Information System (INIS)

    Shaginyan, V. R.

    2011-01-01

    Strongly correlated Fermi systems are among the most intriguing, best experimentally studied and fundamental systems in physics. There is, however, lack of theoretical understanding in this field of physics. The ideas based on the concepts like Kondo lattice and involving quantum and thermal fluctuations at a quantum critical point have been used to explain the unusual physics. Alas, being suggested to describe one property, these approaches fail to explain the others. This means a real crisis in theory suggesting that there is a hidden fundamental law of nature. It turns out that the hidden fundamental law is well forgotten old one directly related to the Landau-Migdal quasiparticles, while the basic properties and the scaling behavior of the strongly correlated systems can be described within the framework of the fermion condensation quantum phase transition (FCQPT). The phase transition comprises the extended quasiparticle paradigm that allows us to explain the non-Fermi liquid (NFL) behavior observed in these systems. In contrast to the Landau paradigm stating that the quasiparticle effective mass is a constant, the effective mass of new quasiparticles strongly depends on temperature, magnetic field, pressure, and other parameters. Our observations are in good agreement with experimental facts and show that FCQPT is responsible for the observed NFL behavior and quasiparticles survive both high temperatures and high magnetic fields.

  12. Faraday forcing of high-temperature levitated liquid metal drops for the measurement of surface tension.

    Science.gov (United States)

    Brosius, Nevin; Ward, Kevin; Matsumoto, Satoshi; SanSoucie, Michael; Narayanan, Ranga

    2018-01-01

    In this work, a method for the measurement of surface tension using continuous periodic forcing is presented. To reduce gravitational effects, samples are electrostatically levitated prior to forcing. The method, called Faraday forcing, is particularly well suited for fluids that require high temperature measurements such as liquid metals where conventional surface tension measurement methods are not possible. It offers distinct advantages over the conventional pulse-decay analysis method when the sample viscosity is high or the levitation feedback control system is noisy. In the current method, levitated drops are continuously translated about a mean position at a small, constant forcing amplitude over a range of frequencies. At a particular frequency in this range, the drop suddenly enters a state of resonance, which is confirmed by large executions of prolate/oblate deformations about the mean spherical shape. The arrival at this resonant condition is a signature that the parametric forcing frequency is equal to the drop's natural frequency, the latter being a known function of surface tension. A description of the experimental procedure is presented. A proof of concept is given using pure Zr and a Ti 39.5 Zr 39.5 Ni 21 alloy as examples. The results compare favorably with accepted literature values obtained using the pulse-decay method.

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

    Directory of Open Access Journals (Sweden)

    Joris Meurs

    2016-08-01

    Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

  14. Application of ionic liquids in liquid chromatography and electrodriven separation.

    Science.gov (United States)

    Huang, Yi; Yao, Shun; Song, Hang

    2013-08-01

    Ionic liquids (ILs) are salts in the liquid state at ambient temperature, which are nonvolatile, nonflammable with high thermal stability and dissolve easily for a wide range of inorganic and organic materials. As a kind of potential green solvent, they show high efficiency and selectivity in the field of separation research, especially in instrumental analysis. Thus far, ILs have been successfully applied by many related researchers in high-performance liquid chromatography and capillary electrophoresis as chromatographic stationary phases, mobile phase additives or electroosmotic flow modifiers. This paper provides a detailed review of these applications in the study of natural products, foods, drugs and other fine chemicals. Furthermore, the prospects of ILs in liquid chromatographic and electrodriven techniques are discussed.

  15. Spillage detector for liquid chromatography systems

    Science.gov (United States)

    Jarvis, M. J.; Fulton, D. S. (Inventor)

    1986-01-01

    A spillage detector device for use in conjunction with fractionation of liquid chromatography systems which includes a spillage recieving enclosure beneath the fractionation area is described. A sensing device having a plurality of electrodes of alternating polarity is mounted within the spillage recieving enclosure. Detection circuitry, responsive to conductivity between electrodes, is operatively connected to the sensing device. The detection circuitry feeds into the output circuitry. The output circuit has relaying and switching circuitry directed to a solenoid, an alarm system and a pump. The solenoid is connected to the pliable conduit of the chromatography system. The alarm system comprises an audio alarm and a visual signal. A 115-volt power system interconnected with the pump, the solenoid, the sensing device, and the detection and output circuitry.

  16. High temperature C/C–SiC composite by liquid silicon infiltration: a ...

    Indian Academy of Sciences (India)

    density, and lower thermal expansion coefficient than low modulus fibres ... the development of a regular crack pattern. ... SEM micrograph of crack microstructure after pyroly- ..... exchangers for high temperature processes like heat recovery.

  17. Characterisation of uremic "Middle molecular"fractions by gas chromatography mass spectrometry, isotachophoresis, and liquid chromatography

    NARCIS (Netherlands)

    Schoots, A.C.; Mikkers, F.E.P.; Claessens, H.A.; Smet, de R.; Landschoot, van N.; Ringoir, S.M.G.

    1982-01-01

    Uremic ultrafiltrates (and normal serum, for comparison) were fractionated by means of gel filtration. The collected fractions were further investigated by combined analytical techniques: "high- performance" liquid chromatography, gas chromatography, mass spectrometry, and isotachophoresis.

  18. Design and Control of High Temperature PEM Fuel Cell Systems using Methanol Reformers with Air or Liquid Heat Integration

    DEFF Research Database (Denmark)

    Andreasen, Søren Juhl; Kær, Søren Knudsen; Sahlin, Simon Lennart

    2013-01-01

    The present work describes the ongoing development of high temperature PEM fuel cell systems fuelled by steam reformed methanol. Various fuel cell system solutions exist, they mainly differ depending on the desired fuel used. High temperature PEM (HTPEM) fuel cells offer the possibility of using...... methanol is converted to a hydrogen rich gas with CO2 trace amounts of CO, the increased operating temperatures allow the fuel cell to tolerate much higher CO concentrations than Nafion-based membranes. The increased tolerance to CO also enables the use of reformer systems with less hydrogen cleaning steps...... liquid fuels such as methanol, due to the increased robustness of operating at higher temperatures (160-180oC). Using liquid fuels such as methanol removes the high volume demands of compressed hydrogen storages, simplifies refueling, and enables the use of existing fuel distribution systems. The liquid...

  19. Liquid chromatography - mass spectrometry analysis of pharmaceuticals

    International Nuclear Information System (INIS)

    Macasek, F.

    2003-01-01

    The drugs represent mostly non-volatile and thermally labile solutes, often available only in small amounts like it is in case of radiopharmaceuticals. Therefor, the favourable separation techniques for such compounds are HPLC, capillary electrophoresis and also TLC 1. Liquid chromatography with mass spectrometric detector (LC/MS) is especially powerful for their microanalysis. Mass spectrometry separating the ions in high vacuum was presumably used as detector for gas chromatography effluent but the on-line coupling with liquid eluant flow 0.1-1 mL/min is far more challenging. New types of ion sources were constructed for simultaneous removal of solvent and ionisation of solutes at atmospheric pressure (API). At present, a relatively wide choice of successfully designed commercial equipment is available either for small organic molecules and larger biomolecules (Perkin-Elmer, Agilent, Jeol, Bruker Daltonics, ThermoQuest, Shimadzu). The features of the LC/MS systems are presented. LC/MS as a new quality control tool for [F-18]fluorodeoxyglucose (FDG) radiopharmaceutical, which has became the most spread radiopharmaceutical for positron emission tomography (PET), was proposed. Other applications of the LC/MS are reviewed. (author)

  20. Optimizing separations in online comprehensive two‐dimensional liquid chromatography

    Science.gov (United States)

    Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2017-01-01

    Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high‐molecular‐weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one‐dimensional liquid chromatography, two‐dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two‐dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two‐dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two‐dimensional liquid chromatography separations. PMID:29027363

  1. Optimizing separations in online comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

    2018-01-01

    Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

  2. Method transfer from high-pressure liquid chromatography to ultra-high-pressure liquid chromatography. II. Temperature and pressure effects.

    Science.gov (United States)

    Åsberg, Dennis; Samuelsson, Jörgen; Leśko, Marek; Cavazzini, Alberto; Kaczmarski, Krzysztof; Fornstedt, Torgny

    2015-07-03

    The importance of the generated temperature and pressure gradients in ultra-high-pressure liquid chromatography (UHPLC) are investigated and compared to high-pressure liquid chromatography (HPLC). The drug Omeprazole, together with three other model compounds (with different chemical characteristics, namely uncharged, positively and negatively charged) were used. Calculations of the complete temperature profile in the column at UHPLC conditions showed, in our experiments, a temperature difference between the inlet and outlet of 16 °C and a difference of 2 °C between the column center and the wall. Through van't Hoff plots, this information was used to single out the decrease in retention factor (k) solely due to the temperature gradient. The uncharged solute was least affected by temperature with a decrease in k of about 5% while for charged solutes the effect was more pronounced, with k decreases up to 14%. A pressure increase of 500 bar gave roughly 5% increase in k for the uncharged solute, while omeprazole and the other two charged solutes gave about 25, 20 and 15% increases in k, respectively. The stochastic model of chromatography was applied to estimate the dependence of the average number of adsorption/desorption events (n) and the average time spent by a molecule in the stationary phase (τs) on temperature and pressure on peak shape for the tailing, basic solute. Increasing the temperature yielded an increase in n and decrease in τs which resulted in less skew at high temperatures. With increasing pressure, the stochastic modeling gave interesting results for the basic solute showing that the skew of the peak increased with pressure. The conclusion is that pressure effects are more pronounced for both retention and peak shape than the temperature effects for the polar or charged compounds in our study. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Use of a Nuclear High Temperature Gas Reactor in a Coal-To-Liquids Process

    International Nuclear Information System (INIS)

    Robert S. Cherry; Richard A. Wood

    2006-01-01

    AREVA's High Temperature Gas Reactor (HTGR) can potentially provide nuclear-generated, high-level heat to chemical process applications. The use of nuclear heat to help convert coal to liquid fuels is particularly attractive because of concerns about the future availability of petroleum for vehicle fuels. This report was commissioned to review the technical and economic aspects of how well this integration might actually work. The objective was to review coal liquefaction processes and propose one or more ways that nuclear process heat could be used to improve the overall process economics and performance. Shell's SCGP process was selected as the gasifier for the base case system. It operates in the range of 1250 to 1600 C to minimize the formation of tars, oil, and methane, while also maximizing the conversion of the coal's carbon to gas. Synthesis gas from this system is cooled, cleaned, reacted to produce the proper ratio of hydrogen to carbon monoxide and fed to a Fischer-Tropsch (FT) reaction and product upgrading system. The design coal-feed rate of 18,800 ton/day produces 26.000 barrels/day of FT products. Thermal energy at approximately 850 C from a HTGR does not directly integrate into this gasification process efficiently. However, it can be used to electrolyze water to make hydrogen and oxygen, both of which can be beneficially used in the gasification/FT process. These additions then allow carbon-containing streams of carbon dioxide and FT tail-gas to be recycled in the gasifier, greatly improving the overall carbon recovery and thereby producing more FT fuel for the same coal input. The final process configuration, scaled to make the same amount of product as the base case, requires only 5,800 ton/day of coal feed. Because it has a carbon utilization of 96.9%, the process produces almost no carbon dioxide byproduct Because the nuclear-assisted process requires six AREVA reactors to supply the heat, the capital cost is high. The conventional plant is

  4. Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

    NARCIS (Netherlands)

    Brudin, S.S.; Shellie, R.A.; Haddad, P.R.; Schoenmakers, P.J.

    2010-01-01

    In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

  5. Novel composite membranes based on PBI and dicationic ionic liquids for high temperature polymer electrolyte membrane fuel cells

    International Nuclear Information System (INIS)

    Hooshyari, Khadijeh; Javanbakht, Mehran; Adibi, Mina

    2016-01-01

    Two types of innovative composite membranes based on polybenzimidazole (PBI) containing dicationic ionic liquid 1,3-di(3-methylimidazolium) propane bis (trifluoromethylsulfonyl) imide (PDC 3 ) and monocationic ionic liquid 1-hexyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide (PMC 6 ) are prepared as electrolyte for high temperature fuel cells applications under anhydrous conditions. The analyses of results display promising characteristics such as high proton conductivity and thermal stability. Moreover the fuel cell performance of PA doped PDC 3 composite membranes is enhanced in comparison with PA doped PMC 6 and PA doped PBI membranes at high temperatures. Dicationic ionic liquid with high number of charge carriers provides well-developed ionic channels which form facile pathways and considerably develop the anhydrous proton conductivity. The highest proton conductivity of 81 mS/cm is achieved for PA doped PDC 3 composite membranes with PBI/IL mole ratio: 4 at 180 °C. A power density of 0.44 W/cm 2 is obtained at 0.5 V and 180 °C for PA doped PDC 3 composite membranes, which proves that these developed composite membranes can be considered as most promising candidates for high temperature fuel cell applications with enhanced proton conductivity.

  6. X-ray imaging for studying behavior of liquids at high pressures and high temperatures using Paris-Edinburgh press

    International Nuclear Information System (INIS)

    Kono, Yoshio; Kenney-Benson, Curtis; Park, Changyong; Shen, Guoyin; Shibazaki, Yuki; Wang, Yanbin

    2015-01-01

    Several X-ray techniques for studying structure, elastic properties, viscosity, and immiscibility of liquids at high pressures have been integrated using a Paris-Edinburgh press at the 16-BM-B beamline of the Advanced Photon Source. Here, we report the development of X-ray imaging techniques suitable for studying behavior of liquids at high pressures and high temperatures. White X-ray radiography allows for imaging phase separation and immiscibility of melts at high pressures, identified not only by density contrast but also by phase contrast imaging in particular for low density contrast liquids such as silicate and carbonate melts. In addition, ultrafast X-ray imaging, at frame rates up to ∼10 5 frames/second (fps) in air and up to ∼10 4 fps in Paris-Edinburgh press, enables us to investigate dynamics of liquids at high pressures. Very low viscosities of melts similar to that of water can be reliably measured. These high-pressure X-ray imaging techniques provide useful tools for understanding behavior of liquids or melts at high pressures and high temperatures

  7. X-ray imaging for studying behavior of liquids at high pressures and high temperatures using Paris-Edinburgh press

    Energy Technology Data Exchange (ETDEWEB)

    Kono, Yoshio; Kenney-Benson, Curtis; Park, Changyong; Shen, Guoyin [HPCAT, Geophysical Laboratory, Carnegie Institution of Washington, 9700 S. Cass Ave., Argonne, Illinois 60439 (United States); Shibazaki, Yuki [Frontier Research Institute for Interdisciplinary Sciences, Tohoku University, Aramaki aza Aoba 6-3, Aoba-ku, Sendai 980-8578 (Japan); Wang, Yanbin [GeoSoilEnviroCARS, Center for Advanced Radiation Sources, The University of Chicago, 5640 S. Ellis Avenue, Chicago, Illinois 60637 (United States)

    2015-07-15

    Several X-ray techniques for studying structure, elastic properties, viscosity, and immiscibility of liquids at high pressures have been integrated using a Paris-Edinburgh press at the 16-BM-B beamline of the Advanced Photon Source. Here, we report the development of X-ray imaging techniques suitable for studying behavior of liquids at high pressures and high temperatures. White X-ray radiography allows for imaging phase separation and immiscibility of melts at high pressures, identified not only by density contrast but also by phase contrast imaging in particular for low density contrast liquids such as silicate and carbonate melts. In addition, ultrafast X-ray imaging, at frame rates up to ∼10{sup 5} frames/second (fps) in air and up to ∼10{sup 4} fps in Paris-Edinburgh press, enables us to investigate dynamics of liquids at high pressures. Very low viscosities of melts similar to that of water can be reliably measured. These high-pressure X-ray imaging techniques provide useful tools for understanding behavior of liquids or melts at high pressures and high temperatures.

  8. Direct high-temperature ohmic heating of metals as liquid pipes.

    Science.gov (United States)

    Grosse, A V; Cahill, J A; Liddell, W L; Murphy, W J; Stokes, C S

    1968-05-03

    When a sufficiently high electric current is passed through a liquid metal, the electromagnetic pressure pinches off the liquid metal and interrupts the flow of current. For the first time the pinch effect has been overcome by use of centrifugal acceleration. By rotation of a pipe of liquid metal, tin or bismuth or their alloys, at sufficiently high speed, it can be heated electrically without intermission of the electric current. One may now heat liquid metallic substances, by resistive (ohmic) heating, to 5000 degrees K and perhaps higher temperatures.

  9. Cromatografia unificada Unified chromatography

    Directory of Open Access Journals (Sweden)

    Carin von Mühlen

    2004-10-01

    Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

  10. Study of thermoelectric power of Co-B liquid quenched amorphous alloys at relatively high temperature

    International Nuclear Information System (INIS)

    Naqvi, S.M.N.R.; Rizvi, S.D.H.; Raza, S.M.; Rizvi, S.; Hussain, A.; Rehman, F.

    1999-01-01

    Measurements of thermoelectric power TEP were carried out for the samples of Co-1 alloy with appropriate compositions of constitutions in the temperature range, 350K< T<760K. The analysis of data shows an inverse Gaussian profile. Ziman theoretical model was used to fit the resistivity data which shows an agreement. Dynamic recovery processes as well as formation of vacancies, interstials, intersection of basal dislocations and indeed pyramidal interlocking of dislocations for seeding scattering centers are responsible for residual TEP at relatively high temperatures Co-B LQA alloys also undergo into other structural changes at such temperatures. (author)

  11. Intensive evaporation and boiling of a heterogeneous liquid droplet with an explosive disintegration in high-temperature gas area

    Directory of Open Access Journals (Sweden)

    Piskunov Maxim V.

    2016-01-01

    Full Text Available The using of the high-speed (not less than 105 frames per second video recording tools (“Phantom” and the software package ("TEMA Automotive" allowed carrying out an experimental research of laws of intensive vaporization with an explosive disintegration of heterogeneous (with a single solid nontransparent inclusion liquid droplet (by the example of water in high-temperature (500-800 K gases (combustion products. Times of the processes under consideration and stages (liquid heat-up, evaporation from an external surface, bubble boiling at internal interfaces, growth of bubble sizes, explosive droplet breakup were established. Necessary conditions of an explosive vaporization of a heterogeneous droplet were found out. Mechanisms of this process and an influence of properties of liquid and inclusion material on them were determined.

  12. Model of a liquid droplet impinging on a high-temperature solid surface

    International Nuclear Information System (INIS)

    Gulikov, A.V.; Berlin, I.I.; Karpyshev, A.V.

    2004-01-01

    The model of the collision of the liquid droplet, vertically falling on the heated solid surface, is presented. The wall temperature is predeterminated so that the droplet interaction with the wall proceeds through the gas interlayer (T≥400 Deg C). The droplet liquid is incompressible, nonviscous. The droplet surface is assigned as free one. The pressure is composed of two components. The first component is the surface tension. The record component is the steam pressure between the droplet and the wall. The liquid motion inside the droplet is assumed to be potential, axisymmetric. The calculation of the droplet collision are carried out with application of the above model. The obtained results are compared with the data of other authors [ru

  13. Conductor of high electrical current at high temperature in oxygen and liquid metal environment

    Science.gov (United States)

    Powell, IV, Adam Clayton; Pati, Soobhankar; Derezinski, Stephen Joseph; Lau, Garrett; Pal, Uday B.; Guan, Xiaofei; Gopalan, Srikanth

    2016-01-12

    In one aspect, the present invention is directed to apparatuses for and methods of conducting electrical current in an oxygen and liquid metal environment. In another aspect, the invention relates to methods for production of metals from their oxides comprising providing a cathode in electrical contact with a molten electrolyte, providing a liquid metal anode separated from the cathode and the molten electrolyte by a solid oxygen ion conducting membrane, providing a current collector at the anode, and establishing a potential between the cathode and the anode.

  14. Role of oxides and porosity on high temperature oxidation of liquid fuelled HVOF thermal sprayed Ni50Cr coatings

    OpenAIRE

    Song, B.; Bai, M.; Voisey, K.T.; Hussain, Tanvir

    2017-01-01

    High chromium content in Ni50Cr thermally sprayed coatings can generate a dense and protective scale at the surface of coating. Thus, the Ni50Cr coating is widely used in high temperature oxidation and corrosion applications. A commercially available gas atomized Ni50Cr powder was sprayed onto a power plant steel (ASME P92) using a liquid fuelled high velocity oxy-fuel (HVOF) thermal spray with three processing parameters in this study. Microstructure of as-sprayed coatings was examined using...

  15. Clinical applications of fast liquid chromatography: a review on the analysis of cardiovascular drugs and their metabolites.

    Science.gov (United States)

    Baranowska, Irena; Magiera, Sylwia; Baranowski, Jacek

    2013-05-15

    One of the major challenges facing the medicine today is developing new therapies that enhance human health. To help address these challenges the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality. In the last decade various analytical strategies have been established to enhance separation speed and efficiency in liquid chromatography applications. Liquid chromatography is an increasingly important tool for monitoring drugs and their metabolites. Furthermore, liquid chromatography has played an important role in pharmacokinetics and metabolism studies at these drug development stages since its introduction. This paper provides an overview of current trends in fast chromatography for the analysis of cardiovascular drugs and their metabolites in clinical applications. Current trends in fast liquid chromatographic separations involve monolith technologies, fused-core columns, high-temperature liquid chromatography (HTLC) and ultra-high performance liquid chromatography (UHPLC). The high specificity in combination with high sensitivity makes it an attractive complementary method to traditional methodology used for routine applications. The practical aspects of, recent developments in and the present status of fast chromatography for the analysis of biological fluids for therapeutic drug and metabolite monitoring, pharmacokinetic studies and bioequivalence studies are presented. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Preliminary test of an ultrasonic liquid film sensor for high-temperature steam-water two-phase flow experiments

    International Nuclear Information System (INIS)

    Aoyama, Goro; Nagayoshi, Takuji; Baba, Atsushi

    2014-01-01

    A prototype liquid film sensor for high-temperature steam-water experiments has been developed. The sensor shape simulates a boiling water reactor (BWR) fuel rod. The pulse-echo method can be utilized to measure the thickness of the liquid film covering the sensor surface. A piezoelectric element is soldered onto the inside of the sensor casing which consists of two curved casing pieces. After the piezoelectric element is attached, the two casing pieces are laser welded together. It is confirmed that the temperature rise at the time of the laser welding does not influence soldering of the piezoelectric element. The pressure proof test shows that the sensor can be used at a high-pressure condition of 7 MPa. Simple air-water experiments are done at atmospheric pressure to confirm the liquid film thickness can be measured with the sensor. The fluctuation of the liquid film thickness is satisfactorily captured with the sensor. The minimum and maximum thicknesses are 0.084 and 0.180 mm, respectively. The amplitude of the waveform at 286°C is predicted by the calculation based on the acoustic impedance. It is expected that the sensor is able to measure the liquid film thickness even at BWR operating conditions. (author)

  17. Microchip systems for imaging liquid and high temperature processes in TEM & SEM

    DEFF Research Database (Denmark)

    Jensen, Eric; Canepa, Silvia; Møller-Nilsen, Rolf Erling Robberstad

    2014-01-01

    Microchips systems have found their way into electron microscopes in order to make miniatureplatforms for controlled liquid and gaseous environments that also begin to include electricalcontacts and other types of interactions with the sample, such as application of forces andirradiation with light.......This presentation will explain the different types of microchip systems and give examples of someof the results we have achieved with our devices and examples of how such devices can be usedfor research related to energy storage and conversion.Heaters can be made in several ways, and monocrystalline silicon......]. Both systems will allowhigh resolution imaging of heterogeneous electrochemical processes such as those in batteries.Based on the suspended microfluidic channels, we are also developing microchips that enableultrafast freezing of processes in liquids....

  18. Investigation of an Alternative Fuel Form for the Liquid Salt Cooled Very High Temperature Reactor (LS-VHTR)

    International Nuclear Information System (INIS)

    Casino, William A. Jr.

    2006-01-01

    Much of the recent studies investigating the use of liquid salts as reactor coolants have utilized a core configuration of graphite prismatic fuel block assemblies with TRISO particles embedded into cylindrical fuel compacts arranged in a triangular pitch lattice. Although many calculations have been performed for this fuel form in gas cooled reactors, it would be instructive to investigate whether an alternative fuel form may yield improved performance for the liquid salt-cooled Very High Temperature Reactor (LS-VHTR). This study investigates how variations in the fuel form will impact the performance of the LS-VHTR during normal and accident conditions and compares the results with a similar analysis that was recently completed for a LS-VHTR core made up of prismatic block fuel. (author)

  19. Performance and stability of a liquid anode high-temperature metal-air battery

    Science.gov (United States)

    Otaegui, L.; Rodriguez-Martinez, L. M.; Wang, L.; Laresgoiti, A.; Tsukamoto, H.; Han, M. H.; Tsai, C.-L.; Laresgoiti, I.; López, C. M.; Rojo, T.

    2014-02-01

    A High-Temperature Metal-Air Battery (HTMAB) that operates based on a simple redox reaction between molten metal and atmospheric oxygen at 600-1000 °C is presented. This innovative HTMAB concept combines the technology of conventional metal-air batteries with that of solid oxide fuel cells to provide a high energy density system for many applications. Electrochemical reversibility is demonstrated with 95% coulomb efficiency. Cell sealing has been identified as a key issue in order to determine the end-of-charge voltage, enhance coulomb efficiency and ensure long term stability. In this work, molten Sn is selected as anode material. Low utilization of the stored material due to precipitation of the SnO2 on the electrochemically active area limits the expected capacity, which should theoretically approach 903 mAh g-1. Nevertheless, more than 1000 charge/discharge cycles are performed during more than 1000 h at 800 °C, showing highly promising results of stability, reversibility and cyclability.

  20. Microchip-based monolithic column for high performance liquid chromatography

    Data.gov (United States)

    National Aeronautics and Space Administration — We have developed microchip based monolithic columns that can be used for liquid chromatography of small organic molecules, as well as, macromolecules such as...

  1. High Performance Liquid Chromatography of Vitamin A: A Quantitative Determination.

    Science.gov (United States)

    Bohman, Ove; And Others

    1982-01-01

    Experimental procedures are provided for the quantitative determination of Vitamin A (retinol) in food products by analytical liquid chromatography. Standard addition and calibration curve extraction methods are outlined. (SK)

  2. A generalized theory of chromatography and multistep liquid extraction

    Science.gov (United States)

    Chizhkov, V. P.; Boitsov, V. N.

    2017-03-01

    A generalized theory of chromatography and multistep liquid extraction is developed. The principles of highly efficient processes for fine preparative separation of binary mixture components on a fixed sorbent layer are discussed.

  3. IMPACT OF TROPICAL CONDITIONS ON THIN-LAYER CHROMATOGRAPHY IN ANALYTICAL TOXICOLOGY - HIGH-TEMPERATURES AND MODERATE HUMIDITIES

    NARCIS (Netherlands)

    DEZEEUW, RA; FRANKE, JP; DIK, E; TENDOLLE, W; KAM, BL

    The impact of high temperatures (24 to 39-degrees-C) and low to moderately high humidities (20 to 70%) on the applicability of TLC systems for drug identification was studied during a 6 month climatologic cycle in Burkina Faso (West Africa). In general, the Rf values as observed on the plates were

  4. SUPPORTED LIQUID CATALYSTS FOR REMOVAL OF HIGH TEMPERATURE FUEL CELL CONTAMINANTS

    Energy Technology Data Exchange (ETDEWEB)

    Alan W. Weimer (PI); Peter Czerpak; Patrick Hilbert

    2000-01-01

    A novel catalytic synthesis gas oxidation process using molten carbonate salts supported on compatible fluidized iron oxide particles (supported-liquid-phase-catalyst (SLPC) fluidized bed process) was investigated. This process combines the advantages of large scale fluidized bed processing with molten salt bath oxidation. Molten salt catalysts can be supported within porous fluidized particles in order to improve mass transfer rates between the liquid catalysts and the reactant gases. Synthesis gas can be oxidized at reduced temperatures resulting in low NO{sub x} formation while trace sulfides and halides are captured in-situ. Hence, catalytic oxidation of synthesis gas can be carried out simultaneously with hot gas cleanup. Such SLPC fluidized bed processes are affected by inter-particle liquid capillary forces that may lead to agglomeration and de-fluidization of the bed. An understanding of the origin and strength of these forces is needed so that they can be overcome in practice. Process design is based on thermodynamic free energy minimization calculations that indicate the suitability of eutectic Na{sub 2}CO{sub 3}/K{sub 2}CO{sub 3} mixtures for capturing trace impurities in-situ (< 1 ppm SO{sub x} released) while minimizing the formation of NO{sub x}(< 10 ppm). Iron oxide has been identified as a preferred support material since it is non-reactive with sodium, is inexpensive, has high density (i.e. inertia), and can be obtained in various particle sizes and porosities. Force balance modeling has been used to design a surrogate ambient temperature system that is hydrodynamically similar to the real system, thus allowing complementary investigation of the governing fluidization hydrodynamics. The primary objective of this research was to understand the origin of and to quantify the liquid capillary interparticle forces affecting the molten carbonate SLPC fluidized bed process. Substantial theoretical and experimental exploratory results indicate process

  5. Reply to "On Vaporization of liquid Pb-Li eutectic alloy from 1000 K to 1200 K- A high temperature mass spectrometric study"

    Science.gov (United States)

    Jain, Uttam; Mukherjee, Abhishek

    2018-03-01

    This communication is in response to a letter to editor commenting on the authors' earlier paper "Vaporization of liquid Pb-Li eutectic alloy from 1000 K to 1200 K - A high temperature mass spectrometric study".

  6. Evaporation studies of liquid oxide fuel at very high temperatures using laser beam heating

    International Nuclear Information System (INIS)

    Bober, M.; Breitung, W.; Karow, H.U.; Schretzmann, K.

    1976-11-01

    Evaporation experiments with oxide fuel are carried out based laser beam heating of the fuel specimen surface. The measuring quantities are the recoil momentum of the target, the evaporation area, the evaporation time and the mass and momentum of the supersonic vapor jet expanding into vacuum, and the thermal radiation density of the evaporating surface. From the mechanical measuring quantities we derive the vapor pressure of the target material and, in a first approach, also the evaporation temperature by applying a gas dynamic evaluation model. In a second approach, after having measured the spectral emissivity of liquid UO 2 at 633 nm, we determine the evaporation temperature at the liquid surface also from its thermal radiation. For the determination of the vapor pressure from the measured quantities a gas dynamic evaluation model has been developed. An application limit of the measuring technique is given by onset of plasma interaction of the vapor plume with the incident laser beam at temperatures above 4500 K. Experimental values for the saturated vapor pressure of UO 2 are presented, determined from three series of laser evaporation measurements obtained at temperatures around 3500 K, 3950 K, and 4200 K. The average vapor pressures found are 0.6 bar, 3 bar, and 7 bar, respectively. Laser vapor pressure measurements performed by other authors and theoretical extrapolations of the UO 2 vapor pressure curve known from literature show fairly good agreement within their confidence interval with the vapor pressure measurements reported here. (orig./HR) [de

  7. Sterilization of liquid foods by pulsed electric fields – an innovative ultra-high temperature process

    Directory of Open Access Journals (Sweden)

    Kai eReineke

    2015-05-01

    Full Text Available The intention of this study was to investigate the inactivation of endospores by a combined thermal and pulsed electric field (PEF treatment. Therefore, self-cultivated spores of Bacillus subtilis and commercial Geobacillus stearothermophilus spores with certified heat resistance were utilized. Spores of both strains were suspended in saline water (5.3 mS cm-1, skim milk (0.3% fat; 5.3 mS cm-1 and fresh prepared carrot juice (7.73 mS cm-1. The combination of moderate preheating (70-90 °C and an insulated PEF-chamber, combined with a holding tube (65 cm and a heat exchanger for cooling, enabled a rapid heat up to 105-140 °C (measured above the PEF chamber within 92.2-368.9 µs. To compare the PEF process with a pure thermal inactivation, each spore suspension was heat treated in thin glass capillaries and D-values from 90 to 130°C and its corresponding z-values were calculated. For a comparison of the inactivation data, F-values for the temperature fields of both processes were calculated by using Comsol Multiphysics combined with a Matlab routine.A preheating of saline water to 70 °C with a flow rate of 5 l h-1, a frequency of 150 Hz and an energy input of 226.5 kJ kg-1, resulted in a measured outlet temperature of 117 °C and a 4.67 log10 inactivation of Bacillus subtilis. The thermal process with identical F-value caused only a 3.71 log10 inactivation. This synergism of moderate preheating and PEF was even more pronounced for Geobacillus stearothermophilus spores in saline water. A preheating to 95 °C and an energy input of 144 kJ kg-1 resulted in an outlet temperature of 126 °C and a 3.28 log10 inactivation, whereas nearly no inactivation (0.2 log10 was achieved during the thermal treatment.Hence, the PEF technology was evaluated as an alternative ultra-high temperature process. However, for an industrial scale application of this process for sterilization, optimization of the treatment chamber design is needed to reduce the occurring

  8. Sterilization of liquid foods by pulsed electric fields–an innovative ultra-high temperature process

    Science.gov (United States)

    Reineke, Kai; Schottroff, Felix; Meneses, Nicolas; Knorr, Dietrich

    2015-01-01

    The intention of this study was to investigate the inactivation of endospores by a combined thermal and pulsed electric field (PEF) treatment. Therefore, self-cultivated spores of Bacillus subtilis and commercial Geobacillus stearothermophilus spores with certified heat resistance were utilized. Spores of both strains were suspended in saline water (5.3 mS cm−1), skim milk (0.3% fat; 5.3 mS cm−1) and fresh prepared carrot juice (7.73 mS cm−1). The combination of moderate preheating (70–90°C) and an insulated PEF-chamber, combined with a holding tube (65 cm) and a heat exchanger for cooling, enabled a rapid heat up to 105–140°C (measured above the PEF chamber) within 92.2–368.9 μs. To compare the PEF process with a pure thermal inactivation, each spore suspension was heat treated in thin glass capillaries and D-values from 90 to 130°C and its corresponding z-values were calculated. For a comparison of the inactivation data, F-values for the temperature fields of both processes were calculated by using computational fluid dynamics (CFD). A preheating of saline water to 70°C with a flow rate of 5 l h−1, a frequency of 150 Hz and an energy input of 226.5 kJ kg−1, resulted in a measured outlet temperature of 117°C and a 4.67 log10 inactivation of B. subtilis. The thermal process with identical F-value caused only a 3.71 log10 inactivation. This synergism of moderate preheating and PEF was even more pronounced for G. stearothermophilus spores in saline water. A preheating to 95°C and an energy input of 144 kJ kg−1 resulted in an outlet temperature of 126°C and a 3.28 log10 inactivation, whereas nearly no inactivation (0.2 log10) was achieved during the thermal treatment. Hence, the PEF technology was evaluated as an alternative ultra-high temperature process. However, for an industrial scale application of this process for sterilization, optimization of the treatment chamber design is needed to reduce the occurring inhomogeneous temperature

  9. Sterilization of liquid foods by pulsed electric fields-an innovative ultra-high temperature process.

    Science.gov (United States)

    Reineke, Kai; Schottroff, Felix; Meneses, Nicolas; Knorr, Dietrich

    2015-01-01

    The intention of this study was to investigate the inactivation of endospores by a combined thermal and pulsed electric field (PEF) treatment. Therefore, self-cultivated spores of Bacillus subtilis and commercial Geobacillus stearothermophilus spores with certified heat resistance were utilized. Spores of both strains were suspended in saline water (5.3 mS cm(-1)), skim milk (0.3% fat; 5.3 mS cm(-1)) and fresh prepared carrot juice (7.73 mS cm(-1)). The combination of moderate preheating (70-90°C) and an insulated PEF-chamber, combined with a holding tube (65 cm) and a heat exchanger for cooling, enabled a rapid heat up to 105-140°C (measured above the PEF chamber) within 92.2-368.9 μs. To compare the PEF process with a pure thermal inactivation, each spore suspension was heat treated in thin glass capillaries and D-values from 90 to 130°C and its corresponding z-values were calculated. For a comparison of the inactivation data, F-values for the temperature fields of both processes were calculated by using computational fluid dynamics (CFD). A preheating of saline water to 70°C with a flow rate of 5 l h(-1), a frequency of 150 Hz and an energy input of 226.5 kJ kg(-1), resulted in a measured outlet temperature of 117°C and a 4.67 log10 inactivation of B. subtilis. The thermal process with identical F-value caused only a 3.71 log10 inactivation. This synergism of moderate preheating and PEF was even more pronounced for G. stearothermophilus spores in saline water. A preheating to 95°C and an energy input of 144 kJ kg(-1) resulted in an outlet temperature of 126°C and a 3.28 log10 inactivation, whereas nearly no inactivation (0.2 log10) was achieved during the thermal treatment. Hence, the PEF technology was evaluated as an alternative ultra-high temperature process. However, for an industrial scale application of this process for sterilization, optimization of the treatment chamber design is needed to reduce the occurring inhomogeneous temperature fields.

  10. Austenitic stainless steel alloys with high nickel contents in high temperature liquid metal systems

    International Nuclear Information System (INIS)

    Konvicka, H.R.; Schwarz, N.F.

    1981-01-01

    Fe-Cr-Ni base alloys (nickel content: from 15 to 70 wt%, Chromium content: 15 wt%, iron: balance) together with stainless steel (W.Nr. 1.4981) have been exposed to flowing liquid sodium at 730 0 C in four intervals up to a cumulative exposure time of 1500 hours. Weight change data and the results of post-exposition microcharacterization of specimens are reported. The corrosion rates increase with increasing nickel content and tend to become constant after longer exposure times for each alloy. The corrosion rate of stainless steel is considerably reduced due to the presence of the base alloys. Different kinetics of nickel poor (up to 35% nickel) and nickel rich (> 50% nickel) alloys and nickel transport from nickel rich to nickel poor material is observed. (orig.)

  11. Intermediate strength alloys for high temperature service in liquid-salt cooled energy systems

    Science.gov (United States)

    Muralidharan, Govindarajan; Wilson, Dane Francis; Holcomb, David Eugene

    2017-06-20

    An alloy consists essentially of, in terms of weight percent: 6 to 8.5 Cr, 5.5 to 13.5 Mo, 0.4 to 7.5 W, 1 to 2 Ti, 0.7 to 0.85 Mn, 0.05 to 0.3 Al, up to to 0.1 Co, 0.08 to 0.5 C, 1 to 5 Ta, 1 to 4 Nab, 1 to 3 Hf, balance Ni. The alloy is characterized by, at 850.degree. C., a yield strength of at least 36 Ksi, a tensile strength of at least 40 Ksi, a creep rupture life at 12 Ksi of at least 72.1 hours, and a corrosion rate, expressed in weight loss [g/(cm2sec)].times.10.sup.-11 during a 1000 hour immersion in liquid FLiNaK at 850.degree. C., in the range of 8 to 25.

  12. High temperature diffusion induced liquid phase joining of a heat resistant alloy

    International Nuclear Information System (INIS)

    Wikstrom, N.P.; Egbewande, A.T.; Ojo, O.A.

    2008-01-01

    Transient liquid phase bonding (TLP) of a nickel base superalloy, Waspaloy, was performed to study the influence of holding time and temperature on the joint microstructure. Insufficient holding time for complete isothermal solidification of liquated insert caused formation of eutectic-type microconstituent along the joint centerline region in the alloy. In agreement with prediction by conventional TLP diffusion models, an increase in bonding temperature for a constant gap size, resulted in decrease in the time, t f, required to form a eutectic-free joint by complete isothermal solidification. However, a significant deviation from these models was observed in specimens bonded at and above 1175 deg. C. A reduction in isothermal solidification rate with increased temperature was observed in these specimens, such that a eutectic-free joint could not be achieved by holding for a time period that produced complete isothermal solidification at lower temperatures. Boron-rich particles were observed within the eutectic that formed in the joints prepared at the higher temperatures. An overriding effect of decrease in boron solubility relative to increase in its diffusivity with increase in temperature, is a plausible important factor responsible for the reduction in isothermal solidification rate at the higher bonding temperatures

  13. High strength alloys for high temperature service in liquid-salt cooled energy systems

    Energy Technology Data Exchange (ETDEWEB)

    Holcomb, David E.; Muralidharan, Govindarajan; Wilson, Dane F.

    2017-01-10

    An essentially cobalt-free alloy consists essentially of, in terms of weight percent: 6.3 to 7.2 Cr, 0.5 to 2 Al, 0 to 5 Fe, 0.7 to 0.8 Mn, 9 to 12.5 Mo, 0 to 6 Ta, 0.75 to 3.5 Ti, 0.01 to 0.25 Nb, 0.2 to 0.6 W, 0.02 to 0.04 C, 0 to 0.001 B, 0.0001 to 0.002 N, balance Ni. The alloy is characterized by a .gamma.' microstructural component in the range of 3 to 17.6 weight percent of the total composition. The alloy is further characterized by, at 850.degree. C., a yield strength of at least 60 Ksi, a tensile strength of at least 70 Ksi, a creep rupture life at 12 Ksi of at least 700 hours, and a corrosion rate, expressed in weight loss [g/(cm.sup.2sec)]10.sup.-11 during a 1000 hour immersion in liquid FLiNaK at 850.degree. C., in the range of 5.5 to 17.

  14. High strength alloys for high temperature service in liquid-salt cooled energy systems

    Science.gov (United States)

    Holcomb, David E.; Muralidharan, Govindarajan; Wilson, Dane F.

    2017-01-10

    An essentially cobalt-free alloy consists essentially of, in terms of weight percent: 6.3 to 7.2 Cr, 0.5 to 2 Al, 0 to 5 Fe, 0.7 to 0.8 Mn, 9 to 12.5 Mo, 0 to 6 Ta, 0.75 to 3.5 Ti, 0.01 to 0.25 Nb, 0.2 to 0.6 W, 0.02 to 0.04 C, 0 to 0.001 B, 0.0001 to 0.002 N, balance Ni. The alloy is characterized by a .gamma.' microstructural component in the range of 3 to 17.6 weight percent of the total composition. The alloy is further characterized by, at 850.degree. C., a yield strength of at least 60 Ksi, a tensile strength of at least 70 Ksi, a creep rupture life at 12 Ksi of at least 700 hours, and a corrosion rate, expressed in weight loss [g/(cm.sup.2sec)]10.sup.-11 during a 1000 hour immersion in liquid FLiNaK at 850.degree. C., in the range of 5.5 to 17.

  15. Thermodynamic characterization of liquid metals at high temperature by isobaric expansion measurements

    International Nuclear Information System (INIS)

    Gathers, G.R.; Shaner, J.W.; Hodgson, W.M.

    1978-01-01

    Results of isobaric expansion measurements for platinum are presented, including simultaneous values for enthalpy, specific volume, temperature and electrical resistivity in tabular form as well as numerical fits up to 7500 K. The specific heat for the liquid is C/sub p/ = 5.85 +- 0.30 R and is essentially constant up to 7500 K. The bulk thermal expansion coefficient increases from approx. 7.5 x 10 -5 K -1 at melt to approx. 1.03 x 10 -4 K -1 at 7500 K. The heat of fusion observed is Δh = 0.14 +- 0.03 MJ/kg and the melting point slope with pressure is estimated to be dT/sub m//dp =31 +- 10 K/GPa. The estimated critical parameters are T/sub c/ = 9285 K, P/sub c/ = 0.9492 GPa, v/sub c/ = 2.120 x 10 -4 m 3 /kg, and z/sub c/ = 0.5085. Preliminary results of a new sound velocity technique are discussed for lead. This technique will allow determination of specific heat c/sub v/, isothermal compressibility K/sub T/ and the constant temperature volume derivatives of entropy and internal energy, as well as the Gruneisen parameter γ/sub G/

  16. Creep-resistant, cobalt-free alloys for high temperature, liquid-salt heat exchanger systems

    Science.gov (United States)

    Holcomb, David E; Muralidharan, Govindarajan; Wilson, Dane F.

    2016-09-06

    An essentially Fe- and Co-free alloy is composed essentially of, in terms of weight percent: 6.0 to 7.5 Cr, 0 to 0.15 Al, 0.5 to 0.85 Mn, 11 to 19.5 Mo, 0.03 to 4.5 Ta, 0.01 to 9 W, 0.03 to 0.08 C, 0 to 1 Re, 0 to 1 Ru, 0 to 0.001 B, 0.0005 to 0.005 N, balance Ni, the alloy being characterized by, at 850.degree. C., a yield strength of at least 25 Ksi, a tensile strength of at least 38 Ksi, a creep rupture life at 12 Ksi of at least 25 hours, and a corrosion rate, expressed in weight loss [g/(cm.sup.2 sec)]10.sup.-11 during a 1000 hour immersion in liquid FLiNaK at 850.degree. C., in the range of 3 to 10.

  17. Radioactivity monitor for high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Reeve, D.R.; Crozier, A.

    1977-01-01

    The coupling of a homogeneous radioactivity monitor to a liquid chromatograph involves compromises between the sensitivity of the monitor and the resolution and speed of analysis of the chromatograph. The theoretical relationships between these parameters are considered and expressions derived which make it possible to calculate suitable monitor operating conditions for most types of high-performance liquid chromatography

  18. Quasiparticle picture of high-temperature superconductors in the frame of a Fermi liquid with the fermion condensate

    Energy Technology Data Exchange (ETDEWEB)

    Amusia, M. Ya.; Shaginyan, V. R.

    2001-06-01

    A model of a Fermi liquid with the fermion condensate (FC) is applied to the consideration of quasiparticle excitations in high-temperature superconductors, in their superconducting and normal states. Within our model the appearance of the fermion condensate presents a quantum phase transition that separates the regions of normal and strongly correlated electron liquids. Beyond the phase transition point the quasiparticle system is divided into two subsystems, one containing normal quasiparticles and the other{emdash}fermion condensate localized at the Fermi surface and characterized by almost dispersionless single-particle excitations. In the superconducting state the quasiparticle dispersion in systems with FC can be presented by two straight lines, characterized by effective masses M{sub FC}{sup *} and M{sub L}{sup *}, respectively, and intersecting near the binding energy, which is of the order of the superconducting gap. This same quasiparticle picture persists in the normal state, thus manifesting itself over a wide range of temperatures as new energy scales. Arguments are presented that fermion systems with FC have features of a {open_quotes}quantum protectorate{close_quotes} [R. B. Laughlin and D. Pines, Proc. Natl. Acad. Sci. U.S.A. >97, 28 (2000); P. W. Anderson, cond-mat/0007185 (unpublished); cond-mat/0007287 (unpublished)].

  19. Quasiparticle picture of high-temperature superconductors in the frame of a Fermi liquid with the fermion condensate

    International Nuclear Information System (INIS)

    Amusia, M. Ya.; Shaginyan, V. R.

    2001-01-01

    A model of a Fermi liquid with the fermion condensate (FC) is applied to the consideration of quasiparticle excitations in high-temperature superconductors, in their superconducting and normal states. Within our model the appearance of the fermion condensate presents a quantum phase transition that separates the regions of normal and strongly correlated electron liquids. Beyond the phase transition point the quasiparticle system is divided into two subsystems, one containing normal quasiparticles and the other-fermion condensate localized at the Fermi surface and characterized by almost dispersionless single-particle excitations. In the superconducting state the quasiparticle dispersion in systems with FC can be presented by two straight lines, characterized by effective masses M FC * and M L * , respectively, and intersecting near the binding energy, which is of the order of the superconducting gap. This same quasiparticle picture persists in the normal state, thus manifesting itself over a wide range of temperatures as new energy scales. Arguments are presented that fermion systems with FC have features of a 'quantum protectorate' [R. B. Laughlin and D. Pines, Proc. Natl. Acad. Sci. U.S.A. >97, 28 (2000); P. W. Anderson, cond-mat/0007185 (unpublished); cond-mat/0007287 (unpublished)

  20. High-temperature compatibility between liquid metal as PWR fuel gap filler and stainless steel and high-density concrete

    Science.gov (United States)

    Wongsawaeng, Doonyapong; Jumpee, Chayanit; Jitpukdee, Manit

    2014-08-01

    In conventional nuclear fuel rods for light-water reactors, a helium-filled as-fabricated gap between the fuel and the cladding inner surface accommodates fuel swelling and cladding creep down. Because helium exhibits a very low thermal conductivity, it results in a large temperature rise in the gap. Liquid metal (LM; 1/3 weight portion each of lead, tin, and bismuth) has been proposed to be a gap filler because of its high thermal conductivity (∼100 times that of He), low melting point (∼100 °C), and lack of chemical reactivity with UO2 and water. With the presence of LM, the temperature drop across the gap is virtually eliminated and the fuel is operated at a lower temperature at the same power output, resulting in safer fuel, delayed fission gas release and prevention of massive secondary hydriding. During normal reactor operation, should an LM-bonded fuel rod failure occurs resulting in a discharge of liquid metal into the bottom of the reactor pressure vessel, it should not corrode stainless steel. An experiment was conducted to confirm that at 315 °C, LM in contact with 304 stainless steel in the PWR water chemistry environment for up to 30 days resulted in no observable corrosion. Moreover, during a hypothetical core-melt accident assuming that the liquid metal with elevated temperature between 1000 and 1600 °C is spread on a high-density concrete basement of the power plant, a small-scale experiment was performed to demonstrate that the LM-concrete interaction at 1000 °C for as long as 12 h resulted in no penetration. At 1200 °C for 5 h, the LM penetrated a distance of ∼1.3 cm, but the penetration appeared to stop. At 1400 °C the penetration rate was ∼0.7 cm/h. At 1600 °C, the penetration rate was ∼17 cm/h. No corrosion based on chemical reactions with high-density concrete occurred, and, hence, the only physical interaction between high-temperature LM and high-density concrete was from tiny cracks generated from thermal stress. Moreover

  1. Ultra-high Performance Liquid Chromatography in Steroid Analysis

    OpenAIRE

    Salonen, Fanny

    2017-01-01

    The latest version of liquid chromatography is ultra-high performance (or pressure) chromatography (UHPLC). In the technique, short and narrow-bore columns with particle sizes below 3 µm are used. The extremely high pressure used results in very short analysis times, excellent separation, and good resolution. This makes UHPLC a good choice for steroidal analysis. Steroids are a highly interesting area of study; they can be recognized as biomarkers for several diseases and are a relevant topic...

  2. Fractionation of fecal neutral steroids by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Jackson, E.M.; Kloss, C.A.; Weintraub, S.T.; Mott, G.E.

    1985-01-01

    Fecal neutral steroids were fractionated by high performance liquid chromatography (HPLC) into three major fractions: 5 beta-H, 3-keto steroids; 5 beta-H, 3 beta-hydroxy steroids; and 5 alpha-H and delta 5-3 beta-hydroxy steroids. This separation was achieved in about 10 minutes, with greater than 97% recovery of standards in each fraction. Gas-liquid chromatographic quantitation of fecal steroids fractionated by either HPLC or thin-layer chromatography gave nearly identical results. A method using both C18 reverse phase and silica HPLC to purify radiolabeled sterols is also described

  3. Development and Validation of Liquid Chromatography- Mass ...

    African Journals Online (AJOL)

    HP

    Method: A novel liquid chromatography–tandem mass spectrometry method for the quantitative determination of naproxen in human K2-EDTA plasma in negative ion mode was employed ..... Practice and Applications of Bio-analytical Method.

  4. Liquid Chromatography Applied to Space System

    Science.gov (United States)

    Poinot, Pauline; Chazalnoel, Pascale; Geffroy, Claude; Sternberg, Robert; Carbonnier, Benjamin

    Searching for signs of past or present life in our Solar System is a real challenge that stirs up the curiosity of scientists. Until now, in situ instrumentation was designed to detect and determine concentrations of a wide number of organic biomarkers. The relevant method which was and still is employed in missions dedicated to the quest of life (from Viking to ExoMars) corresponds to the pyrolysis-GC-MS. Along the missions, this approach has been significantly improved in terms of extraction efficiency and detection with the use of chemical derivative agents (e.g. MTBSTFA, DMF-DMA, TMAH…), and in terms of analysis sensitivity and resolution with the development of in situ high-resolution mass spectrometer (e.g. TOF-MS). Thanks to such an approach, organic compounds such as amino acids, sugars, tholins or polycyclic aromatic hydrocarbons (PAHs) were expected to be found. However, while there’s a consensus that the GC-MS of Viking, Huygens, MSL and MOMA space missions worked the way they had been designed to, pyrolysis is much more in debate (Glavin et al. 2001; Navarro-González et al. 2006). Indeed, (1) it is thought to remove low levels of organics, (2) water and CO2 could interfere with the detection of likely organic pyrolysis products, and (3) only low to mid-molecular weight organic molecules can be detected by this technique. As a result, researchers are now focusing on other in situ techniques which are no longer based on the volatility of the organic matter, but on the liquid phase extraction and analysis. In this line, micro-fluidic systems involving sandwich and/or competitive immunoassays (e.g. LMC, SOLID; Parro et al. 2005; Sims et al. 2012), micro-chip capillary electrophoreses (e.g. MOA; Bada et al. 2008), or nanopore-based analysis (e.g. BOLD; Schulze-Makuch et al. 2012) have been conceived for in situ analysis. Thanks to such approaches, molecular biological polymers (polysaccharides, polypeptides, polynucleotides, phospholipids, glycolipids

  5. Liquid chromatography and liquid chromatography-mass spectrometry analysis of donepezil degradation products

    Directory of Open Access Journals (Sweden)

    Mladenović Aleksandar R.

    2015-01-01

    Full Text Available This study describes the investigation of degradation products of donepezil (DP using stability indicating RP-HPLC method for determination of donepezil, which is a centrally acting reversible acetylcholinesterase inhibitor. In order to investigate the stability of drug and formed degradation products, a forced degradation study of drug sample and finished product under different forced degradation conditions has been conducted. Donepezil hydrochloride and donepezil tablets were subjected to stress degradation conditions recommended by International Conference on Harmonization (ICH. Donepezil hydrochloride solutions were subjected to acid and alkali hydrolysis, chemical oxidation and thermal degradation. Significant degradation was observed under alkali hydrolysis and oxidative degradation conditions. Additional degradation products were observed under the conditions of oxidative degradation. The degradation products observed during forced degradation studies were monitored using the high performance liquid chromatography (HPLC method developed. The parent method was modified in order to obtain LC-MS compatible method which was used to identify the degradation products from forced degradation samples using high resolution mass spectrometry. The mass spectrum provided the precise mass from which derived molecular formula of drug substance and degradation products formed and proved the specificity of the method unambiguously. [Projekat Ministarstva nauke Republike Srbije, br. 172013

  6. Instrumental liquid chromatography: a practical manual on high-performance liquid chromatographic methods

    National Research Council Canada - National Science Library

    Parris, N. A

    1976-01-01

    Available texts on liquid chromatography have tended to emphasize the developments in the theoretical understanding of the technique and methodology or to list numerous applications, complete with experimental details...

  7. Substitution of conventional high-temperature syntheses of inorganic compounds by near-room-temperature syntheses in ionic liquids

    KAUST Repository

    Groh, Matthias Friedrich

    2013-01-01

    The high-temperature syntheses of the low-valent halogenides P2I4, Te2Br, α-Te4I4, Te4(Al2Cl7)2, Te4(Bi6Cl20), Te8(Bi4Cl14),Bi8(AlCl4)2, Bi6Cl7,and Bi6Br7, as well as of WSCl4 andWOCl4 have been replaced by resource-efficient low-temperature syntheses in room temperature ionic liquids (RTILs). The simple one-pot syntheses generally do not require elaborate equipment such as twozone furnaces or evacuated silica ampoules. Compared to the published conventional approaches, reduction of reaction time (up to 80%) and temperature (up to 500 K) and, simultaneously, an increase in yield were achieved. In the majority of cases, the solid products were phase-pure. X-Ray diffraction on single crystals (redetermination of 11 crystal structures) has demonstrated that the quality of the crystals from RTILs is comparable to that of products obtained by chemical transport reactions. © 2013 Verlag der Zeitschrift für Naturforschung, Tübingen.

  8. Liquid-adsorption chromatography of metal 8-hydroxyquinolinates

    International Nuclear Information System (INIS)

    Basova, E.M.; Bol'shova, T.A.; Shirshova, T.S.

    1988-01-01

    Using the method of liquid-adsorption chromatography separation of 8-hydroxyquinolinates of Cu, Fe, Ga, In, Al, Ni is realized. Thin-layer chromatography (TLC) is used to define the optimum conditions of separation and highly efficient liquid column chromatography (HELC) - for chelate separation. Applicaton of the same sorbent is a very important condition of transition from TLC to HELC. Solica gel Partisil, mobile phase: benzene - isopropanol mixture, containing 1 x 10 -3 M of 8-hydroxyquinoline, are the optimal conditions for the studied chelates separation. But In and Ga in TLC move together, and in HELC they are partially separated, therefore, for their separation the column selectivity should be improved by selection of mobile phase

  9. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid ... response, tailing factor and resolution of six replicate injections was < 3 %. ... Cefadroxil monohydrate, Human plasma, Pharmacokinetics Bioequivalence ... Drug-free plasma was obtained from the local .... Influence of probenicid on the renal.

  10. Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

    Science.gov (United States)

    DiNunzio, James E.

    1985-01-01

    Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

  11. Beta-induced fluorescence detection in liquid chromatography

    International Nuclear Information System (INIS)

    Malcolme-Lawes, D.J.; Massey, S.; Warwick, P.

    1981-01-01

    A theoretical analysis of beta-induced fluorescence is used to determine the factors which influence the sensitivity of the technique as applied to liquid chromatography. Equations are presented for detector response and for signal-to-noise ratios and the theoretical response for a typical detector is compared with experimentally determined values. (author)

  12. Mallow carotenoids determined by high-performance liquid chromatography

    Science.gov (United States)

    Mallow (corchorus olitorius) is a green vegetable, which is widely consumed either fresh or dry by Middle East population. This study was carried out to determine the contents of major carotenoids quantitatively in mallow, by using a High Performance Liquid Chromatography (HPLC) equipped with a Bis...

  13. High-Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  14. Monitoring aged reversed-phase high performance liquid chromatography columns

    NARCIS (Netherlands)

    Bolck, A; Smilde, AK; Bruins, CHP

    1999-01-01

    In this paper, a new approach for the quality assessment of routinely used reversed-phase high performance liquid chromatography columns is presented. A used column is not directly considered deteriorated when changes in retention occur. If attention is paid to the type and magnitude of the changes,

  15. Ultra high performance liquid chromatography of seized drugs

    NARCIS (Netherlands)

    Lurie, I.S.

    2010-01-01

    The primary goal of this thesis is to investigate the use of ultra high performance liquid chromatography (UHPLC) for the analysis of seized drugs. This goal was largely achieved and significant progress was made in achieving improved separation and detection of drugs of forensic interest.

  16. Quantification of Tea Flavonoids by High Performance Liquid Chromatography

    Science.gov (United States)

    Freeman, Jessica D.; Niemeyer, Emily D.

    2008-01-01

    We have developed a laboratory experiment that uses high performance liquid chromatography (HPLC) to quantify flavonoid levels in a variety of commercial teas. Specifically, this experiment analyzes a group of flavonoids known as catechins, plant-derived polyphenolic compounds commonly found in many foods and beverages, including green and black…

  17. Characterization of porous silicon integrated in liquid chromatography chips

    NARCIS (Netherlands)

    Tiggelaar, Roald M.; Verdoold, Vincent; Eghbali, H.; Desmet, G.; Gardeniers, Johannes G.E.

    2009-01-01

    Properties of porous silicon which are relevant for use of the material as a stationary phase in liquid chromatography chips, like porosity, pore size and specific surface area, were determined with high-resolution SEM and N2 adsorption–desorption isotherms. For the anodization conditions

  18. Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, Th.

    2006-01-01

    The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical

  19. Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology

    OpenAIRE

    Brown, Leslie; Earle, Martyn J; Gilea, Manuela; Plechkova, Natalia V; Seddon, Kenneth R

    2017-01-01

    Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous char...

  20. Optimizing heterosurface adsorbent synthesis for liquid chromatography

    Science.gov (United States)

    Bogoslovskii, S. Yu.; Serdan, A. A.

    2016-03-01

    The structural and geometric parameters of a silica matrix (SM) for the synthesis of heterosurface adsorbents (HAs) are optimized. Modification is performed by shielding the external surfaces of alkyl-modified silica (AS) using human serum albumin and its subsequent crosslinking. The structural and geometric characteristics of the SM, AS, and HA are measured via low-temperature nitrogen adsorption. It is found that the structural characteristics of AS pores with diameters D 9 nm reduces significantly due to adsorption of albumin. It is concluded that silica gel with a maximum pore size distribution close to 5 nm and a minimal proportion of pores with D > 9 nm is optimal for HA synthesis; this allows us to achieve the greatest similarity between the chromatographic retention parameters for HA and AS. The suitability of the synthesized adsorbents for analyzing drugs in biological fluids through direct sample injection is confirmed by chromatography. It was found that the percentage of the protein fraction detected at the outlet of the chromatographic column is 98%.

  1. High-temperature oxidation of silicide-aluminide layer on the TiAl6V4 alloy prepared by liquid-phase siliconizing

    Czech Academy of Sciences Publication Activity Database

    Kubatík, Tomáš František

    2016-01-01

    Roč. 50, č. 2 (2016), s. 257-261 ISSN 1580-2949 Institutional support: RVO:61389021 Keywords : TiAl6V4 * silicides * high-temperature oxidation * liquid-phase silicon izing Subject RIV: JG - Metallurgy Impact factor: 0.436, year: 2016

  2. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lijun

    2014-02-19

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  3. Development and application of liquid chromatography coupled to isotope ratio mass spectrometry

    International Nuclear Information System (INIS)

    Zhang, Lijun

    2014-01-01

    Stable isotope analysis has found widespread applications in various disciplines such as archaeology, geochemistry, biology, food authenticity, and forensic science. Coupling chromatography to isotope ratio mass spectrometry for compound-specific isotope analysis (CSIA) is a trend, as it provides several advantages over bulk isotope analysis, e.g., relatively simple sample preparation, the ability to measure individual compounds in a complex mixture in one run, and the reduced sample size required for precise isotope analysis. Gas chromatography coupled to isotope ratio mass spectrometry (GC/IRMS) has been well-established for compound-specific isotope analysis of volatile organic compounds within the last two decades. However, an interface combining liquid chromatography with isotope ratio mass spectrometry (LC/IRMS) was not commercially available until 2004. The current design of the interface requires using a carbon-free eluent in chromatographic separation. This requirement limits the application of the most frequently used reversed-phase liquid chromatography in CSIA, because the elution strength of water at room temperature is too low to serve as mobile phase in reversed-phase separations. In order to increase the elution strength of water, we propose using high temperature water for chromatographic elution. The polarity of water decreases with an increase of temperature, yielding increased elution strength in reversed-phase columns. Therefore, high temperature water can be used as eluent instead of organic solvent for combining reversed-phase liquid chromatography with isotope ratio mass spectrometry (RPLC/IRMS). Additionally, temperature gradients can replace organic solvent gradients to increase chromatographic resolution. This is very important for LC/IRMS analysis, as precise isotope analysis requires baseline separation of analytes. In this thesis, high-temperature reversed-phase liquid chromatography was coupled to, and for the first time carefully

  4. Theories to support method development in comprehensive two-dimensional liquid chromatography - A review

    NARCIS (Netherlands)

    Bedani, F.; Schoenmakers, P.J.; Janssen, H.-G.

    2012-01-01

    On-line comprehensive two-dimensional liquid chromatography techniques promise to resolve samples that current one-dimensional liquid chromatography methods cannot adequately deal with. To make full use of the potential of two-dimensional liquid chromatography, optimization is required. Optimization

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

    Science.gov (United States)

    2010-04-01

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

  6. 21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

  7. Application of genetic algorithms for parameter estimation in liquid chromatography

    International Nuclear Information System (INIS)

    Hernandez Torres, Reynier; Irizar Mesa, Mirtha; Tavares Camara, Leoncio Diogenes

    2012-01-01

    In chromatography, complex inverse problems related to the parameters estimation and process optimization are presented. Metaheuristics methods are known as general purpose approximated algorithms which seek and hopefully find good solutions at a reasonable computational cost. These methods are iterative process to perform a robust search of a solution space. Genetic algorithms are optimization techniques based on the principles of genetics and natural selection. They have demonstrated very good performance as global optimizers in many types of applications, including inverse problems. In this work, the effectiveness of genetic algorithms is investigated to estimate parameters in liquid chromatography

  8. Pyrrolidinium FSI and TFSI-Based Polymerized Ionic Liquids as Electrolytes for High-Temperature Lithium-Ion Batteries

    Directory of Open Access Journals (Sweden)

    Manfred Kerner

    2018-02-01

    Full Text Available Promising electrochemical and dynamical properties, as well as high thermal stability, have been the driving forces behind application of ionic liquids (ILs and polymerized ionic liquids (PILs as electrolytes for high-temperature lithium-ion batteries (HT-LIBs. Here, several ternary lithium-salt/IL/PIL electrolytes (PILel have been investigated for synergies of having both FSI and TFSI anions present, primarily in terms of physico-chemical properties, for unique application in HT-LIBs operating at 80 °C. All of the electrolytes tested have low Tg and are thermally stable ≥100 °C, and with TFSI as the exclusive anion the electrolytes (set A have higher thermal stabilities ≥125 °C. Ionic conductivities are in the range of 1 mS/cm at 100 °C and slightly higher for set A PILel, which, however, have lower oxidation stabilities than set B PILel with both FSI and TFSI anions present: 3.4–3.7 V vs. 4.2 V. The evolution of the interfacial resistance increases for all PILel during the first 40 h, but are much lower for set B PILel and generally decrease with increasing Li-salt content. The higher interfacial resistances only influence the cycling performance at high C-rates (1 C, where set B PILel with high Li-salt content performs better, while the discharge capacities at the 0.1 C rate are comparable. Long-term cycling at 0.5 C, however, shows stable discharge capacities for 100 cycles, with the exception of the set B PILel with high Li-salt content. Altogether, the presence of both FSI and TFSI anions in the PILel results in lower ionic conductivities and decreased thermal stabilities, but also higher oxidation stabilities and reduced interfacial resistances and, in total, result in an improved rate capability, but compromised long-term capacity retention. Overall, these electrolytes open for novel designs of HT-LIBs.

  9. Thin-layer chromatography - liquid chromatography, an ideal supplement demonstrated by the separation of lanthanoids

    International Nuclear Information System (INIS)

    Specker, H.; Hufnagel, A.

    1984-01-01

    All lanthanoids have been separated by thin-layer chromatography (TLC) with short retention times by using a mixture of ether/tetrahydrofurane (THF)/bis-(2-ethylhexyl)-phosphate (HDEHP)/nitric acid. The eluent was empirically tested by synergistic effects. The results have been transferred to high-performance liquid chromatography /HPLC). It was possible to use the same eluent in TLC and HPLC both for the analytical separation of all lanthanoids and for the separation of fission products. The experimental experience gained in HPLC could be applied to the pre-concentration of isotopes in TLC. Both methods excellently supplemented each other in the separation of lanthanoids. (orig.) [de

  10. Reactor for tracking catalyst nanoparticles in liquid at high temperature under a high-pressure gas phase with X-ray absorption spectroscopy.

    Science.gov (United States)

    Nguyen, Luan; Tao, Franklin Feng

    2018-02-01

    Structure of catalyst nanoparticles dispersed in liquid phase at high temperature under gas phase of reactant(s) at higher pressure (≥5 bars) is important for fundamental understanding of catalytic reactions performed on these catalyst nanoparticles. Most structural characterizations of a catalyst performing catalysis in liquid at high temperature under gas phase at high pressure were performed in an ex situ condition in terms of characterizations before or after catalysis since, from technical point of view, access to the catalyst nanoparticles during catalysis in liquid phase at high temperature under high pressure reactant gas is challenging. Here we designed a reactor which allows us to perform structural characterization using X-ray absorption spectroscopy including X-ray absorption near edge structure spectroscopy and extended X-ray absorption fine structure spectroscopy to study catalyst nanoparticles under harsh catalysis conditions in terms of liquid up to 350 °C under gas phase with a pressure up to 50 bars. This reactor remains nanoparticles of a catalyst homogeneously dispersed in liquid during catalysis and X-ray absorption spectroscopy characterization.

  11. Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology.

    Science.gov (United States)

    Brown, Leslie; Earle, Martyn J; Gîlea, Manuela A; Plechkova, Natalia V; Seddon, Kenneth R

    2017-08-10

    Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous character of ionic liquid-based solvent systems to be used in a wide variety of separations (including transition metal salts, arenes, alkenes, alkanes, bio-oils and sugars).

  12. Nano-liquid chromatography applied to enantiomers separation.

    Science.gov (United States)

    Fanali, Salvatore

    2017-02-24

    This paper presents the state of the art concerning the separation of chiral compounds by means of nano-liquid chromatography (nano-LC). The enantiomers' separation and determination are a subject of fundamental importance in various application fields such as pharmaceutical industry, biomedicine, food, agrochemical etc. Nano-LC is a miniaturized chromatographic technique offering some advantages over conventional ones such as low consumption of mobile phase, sample volume and amount of chiral stationary phase, reduced costs etc. This is reported in the first part of the paper illustrating the features of the nano-LC. In addition, chiral resolution methods are briefly illustrated. Some chiral selectors, used in high-performance liquid chromatography have also been applied in nano-LC including cyclodextrins, glycopeptide antibiotics, modified polysaccharides etc. This is discussed in the second part of the review. Finally some examples of the applications available in literature are reported. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Combined high-performance liquid chromatography-radioimmunoassay for cytokinins

    International Nuclear Information System (INIS)

    MacDonald, E.M.S.; Akiyoshi, D.E.; Morris, R.O.

    1981-01-01

    The cytokinins isopentenyladenosine and ribosylzeatin were conjugated to bovine serum albumin and the conjugates used to raise antisera in rabbits. The resulting antisera had high specificity towards the cytokinin haptens and low cross-reactivity towards other purines. They were used as the basis for a radioimmunoassay for cytokinins, which, when applied in conjunction with high-performance liquid chromatography, allowed rapid and sensitive (to the picogram range) estimation and identification of multiple cytokinins from natural plant and bacterial sources. (orig.)

  14. High performance liquid chromatography in studies of radiolabeled antibodies

    International Nuclear Information System (INIS)

    Hnatowich, D.J.

    1986-01-01

    High performance liquid chromatography (HPLC) as applied to the separation of antibodies displays the same advantages as in its other applications, namely good resolution accompanied by fast analysis. It is therefore not surprising that many HPLC columns designed for use with antibodies and other proteins are now available commercially. The properties of proteins which provide the separation are size, hydrophobicity, charge and affinity. The features of each are discussed. (author)

  15. Evolution and Current Trends in Liquid and Supercritical Fluid Chromatography

    OpenAIRE

    Fekete, Szabolcs; Grand-Guillaume-Perrenoud, Alexandre; Guillarme, Davy

    2014-01-01

    The current trend in high performance liquid chromatography (HPLC) tends toward the achievement of higher separation efficiency and shorter analysis time. Indeed, better performance in LC has become increasingly important in recent years mainly driven by the challenges of either analyzing more complex samples or increasing the numbers of samples per time unit. In the recent development of particle technology, the use of fully porous sub-2 m particles and sub-3 m shell particles have received ...

  16. Liquid Chromatography for Analysis of Metformin in Myrmeleon sp.

    OpenAIRE

    Afidatul Muadifah; Hermin Sulistyarti; Sasangka Prasetyawan

    2017-01-01

    Myrmeleon sp is a typical of insect larva which has been used in Indonesia for diabetes treatment. However, there is no sufficient scientific report explaining the bioactive compounds in this insect. Based on our preliminary research, this insect contained metformin, i.e. one of bioactive compounds for the treatment of type-2 diabetes. Therefore, this study is focused on the development of separation technique using high performance liquid chromatography (HPLC) on a reverse phase C-18 column ...

  17. Liquid to liquid extraction and liquid chromatography-tandem mass spectrometry determination of hainanmycin in feed.

    Science.gov (United States)

    Wang, Ze Ping; Shen, Jian Zhong; Linhardt, Robert J; Jiang, Hui; Cheng, Lin Li

    2017-03-01

    Hainanmycin is a new veterinary polyether antibiotic and has few sensitive analytical method in present days. In this study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) relying on multiple reaction monitoring (MRM) detection was developed for analysis of hainanmycin in animal feed. Feed samples were extracted with ethyl acetate and purified by two steps of liquid-liquid extraction (LLE) to get rid of water solvable matrix and lipids one by one. The final simple was analyzed by LC-MS/MS. The LC mobile phase was composed of 0.1% aqueous formic acid and 0.1% formic acidified acetonitrile by gradient elution. Average recoveries ranged from 74.22% to 87.85%, as determined by spiking with 2.0 (LOQ) ∼2500μgkg -1 of hainanmycin. The inter-day and intra-day coefficient of variation was 9.21% to 11.77% and 7.67% to 13.49%, respectively. The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.36μgkg -1 and 2.0μgkg -1 , respectively. Copyright © 2016. Published by Elsevier B.V.

  18. Comprehensive two-dimensional liquid chromatography and hyphenated liquid chromatography to study the degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, T.

    2005-01-01

    Size exclusion chromatography (SEC), gradient polymer elution chromatography (GPEC) and liquid chromatography at critical conditions (LC-CC) have been developed and applied to observe chemical changes in poly(bisphenol A)carbonate (PC) due to hydrolytic degradation. Especially LC-CC appeared to be

  19. Protein separations using enhanced-fluidity liquid chromatography.

    Science.gov (United States)

    Bennett, Raffeal; Olesik, Susan V

    2017-11-10

    Enhanced-fluidity liquid chromatography (EFLC) methods using methanol/H 2 O/CO 2 and hydrophilic interaction liquid chromatography (HILIC) were explored for the separation of proteins and peptides. EFLC is a separation mode that uses a mobile phase made of conventional solvents combined with liquid carbon dioxide (CO 2 ) in subcritical conditions. The addition of liquid CO 2 enhances diffusivity and decreases viscosity while maintaining mixture polarity, which typically results in reduced time of analysis. TFA additive and elevated temperature were leveraged as key factors in the separation of a 13-analyte intact protein mixture in under 5min. Under these conditions EFLC showed modest improvement in terms of peak asymmetry and analysis time over the competing ACN/H 2 O separation. Protein analytes detected by electrospray ionization - quadrupole time of flight, were shown to be unaffected by the addition of CO 2 in the mobile phase. Herein, the feasibility of separating hydrophilic proteins up to 80kDa (with transferrin) is demonstrated for CO 2 -containing mobile phases. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Determination of oxymatrine in Sophora Radix by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Yang, Seung Kwon; Yun, Young Ja; Namgung, Mi Ok

    2004-01-01

    A high performance liquid chromatographic method was designed for the quantitative analysis of oxymatrine in Sophora Radix. The separation of oxymatrine was performed by reversed-phase chromatography with a C 18 column and a buffered aqueous solution containing acetonitrile, and monitored by UV absorption at 215 nm. Extraction of oxymatrine in Sophora Radix was carried out using various solvents and extraction methods. The optimum extraction efficiency for the crushed Sophora Radix was achieved by reflux at 80 .deg. C in 50% ethanol for five hours. Most extraction methods used to complicate pretreatments. In this study, sublimation was employed for a extraction method without going through complicate pretreatments. Sublimation was carried out under high vacuum (1x10 -3 torr) and at high temperature (200 .deg. C). Extraction efficiency using Sublimation was found to be inferior to other extraction methods

  1. Csaba Horváth and preparative liquid chromatography.

    Science.gov (United States)

    Guiochon, Georges

    2005-06-24

    Few chromatographers have been interested in furthering preparative liquid chromatography. The pioneers, Tswett, Kuhn and Lederer, A.J.P. Martin, Tiselius, isolated fractions but as an intermediate step in the analysis of their samples. The progress in electronics and sensors, and in their miniaturization has lead to the paradoxical situation that the analysts never see the transient pure fractions that their detector quantitates. Yet, over the last 25 years, preparative liquid chromatography has become an important industrial process for the separation, the extraction, and/or the purification of many pharmaceuticals or pharmaceutical intermediates, including pure enantiomers, purified peptides and proteins, compounds that are manufactured at the relatively large industrial scale of a few kilograms to several hundred tons per year. This development that has strongly affected the modem pharmaceutical industry is mainly due to the pioneering work of Csaba Horváth. His work in preparative HPLC was critical at both the practical and the theoretical levels. He was the first scientist in modem times to pay serious attention to the relationships between the curvature of the equilibrium isotherms, the competitive nature of nonlinear isotherms, and the chromatographic band profiles of complex mixtures. The thermodynamics of multi-component phase equilibria and mass transfer kinetics in chromatography attracted his interest and were the focus of ground-breaking contributions. He investigated displacement chromatography, an old method invented by Tiselius that Csaba was first to implement in HPLC. This choice was explained by the essential characteristic of displacement chromatography, in that it delivers fractions that can be far more concentrated than the feed. Remarkably, once the basics of nonlinear chromatography had been mastered in his group, most of the applications that were studied by his coworkers dealt with peptides of various sizes and with proteins. Thus, all

  2. Nanomaterials as stationary phases and supports in liquid chromatography.

    Science.gov (United States)

    Beeram, Sandya R; Rodriguez, Elliott; Doddavenkatanna, Suresh; Li, Zhao; Pekarek, Allegra; Peev, Darin; Goerl, Kathryn; Trovato, Gianfranco; Hofmann, Tino; Hage, David S

    2017-10-01

    The development of various nanomaterials over the last few decades has led to many applications for these materials in liquid chromatography (LC). This review will look at the types of nanomaterials that have been incorporated into LC systems and the applications that have been explored for such systems. A number of carbon-based nanomaterials and inorganic nanomaterials have been considered for use in LC, ranging from carbon nanotubes, fullerenes and nanodiamonds to metal nanoparticles and nanostructures based on silica, alumina, zirconia and titanium dioxide. Many ways have been described for incorporating these nanomaterials into LC systems. These methods have included covalent immobilization, adsorption, entrapment, and the synthesis or direct development of nanomaterials as part of a chromatographic support. Nanomaterials have been used in many types of LC. These applications have included the reversed-phase, normal-phase, ion-exchange, and affinity modes of LC, as well as related methods such as chiral separations, ion-pair chromatography and hydrophilic interaction liquid chromatography. Both small and large analytes (e.g., dyes, drugs, amino acids, peptides and proteins) have been used to evaluate possible applications for these nanomaterial-based methods. The use of nanomaterials in columns, capillaries and planar chromatography has been considered as part of these efforts. Potential advantages of nanomaterials in these applications have included their good chemical and physical stabilities, the variety of interactions many nanomaterials can have with analytes, and their unique retention properties in some separation formats. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    International Nuclear Information System (INIS)

    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

  4. Determination of trimethyllead reference material using high performance liquid chromatography-inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lu Hai; Wei Chao; Wang Jun; Chao Jingbo; Zhou Tao; Chen Dazhou

    2005-01-01

    A high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) was combined, and the chromatography conditions were optimized. The stability and homogeneity of a trimethyllead reference material were determined using this method. (authors)

  5. Substitution of conventional high-temperature syntheses of inorganic compounds by near-room-temperature syntheses in ionic liquids

    KAUST Repository

    Groh, Matthias Friedrich; Mü llera, Ulrike; Ahmed, Ejaz; Rothenberger, Alexander; Ruck, Michael J.

    2013-01-01

    The high-temperature syntheses of the low-valent halogenides P2I4, Te2Br, α-Te4I4, Te4(Al2Cl7)2, Te4(Bi6Cl20), Te8(Bi4Cl14),Bi8(AlCl4)2, Bi6Cl7,and Bi6Br7, as well as of WSCl4 andWOCl4 have been replaced by resource-efficient low

  6. The high pressure electronic control system in liquid chromatography

    International Nuclear Information System (INIS)

    Popescu, Stefan; Popeneciu, Gabriel; Toadere, Florin

    2002-01-01

    The Liquid Chromatography system can perform a wide variety of measurements and separations especially for the organic liquids, with maximum applications flexibility for less than half price of Gas Chromatography. The repeatability and accuracy of results in quantitative high pressure liquid chromatography are highly dependent on the reproducibility and accuracy of both integrated flow rate and mobile phase composition. Flow rate fluctuation leads to poor reproducibility in both integrated peak areas and retention times. Similarly, poor control of mobile phase composition will cause poor repeatability of retention time and peak heights. The our Solvent Delivery System SDS 200 is a single pump system which provides precise compensated flow rates from 0.01 to 10 mL/min, selectable upper pressure limits of 0 to 100 bar or 10 to 450 bar, and solvent compressibility correction. Ternary solvent system on-line mixing capability saves time, reduces solvent waste and provides more flexibility for difficult separations. The pump itself has two different displacement pistons which are used alternately on both suction and discharge, so that intake of the solvent are synchronous. The evacuated solvent from the two pump's chambers is mixed in the reference unit and then is supplied to the damping unit for flow ripple reduction. The SDS Electronic Module ensures the functions: controls the programmed flow rate, detects and shows the solvent pressure in solvent, supplies the step motor, measures and limits the solvent pressure. The control panel of SDS 200, contains a two-stages flow decimal programmer, a eight-positions knob for upper pressure limits, an alarm LED and a parallel port for connection to a PC system. (authors)

  7. VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis. Program. Summary of reports

    International Nuclear Information System (INIS)

    2001-01-01

    Program and summary of reports of the VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis are performed. The meeting took place 15-19 October, 2001 in Moscow. Many problems of liquid and ion exchange chromatography, capillary electrophoresis, thin-layer chromatography have been discussed extensively. Reports covering properties of sorbents and devices for chromatography are incorporated in the collection [ru

  8. Hydrazine Determination in Sludge Samples by High Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    G. Elias; G. A. Park

    2006-02-01

    A high-performance liquid chromatographic method using ultraviolet (UV) detection was developed to detect and quantify hydrazine in a variety of environmental matrices. The method was developed primarily for sludge samples, but it is also applicable to soil and water samples. The hydrazine in the matrices was derivatized to their hydrazones with benzaldehyde. The derivatized hydrazones were separated using high performance liquid chromatography (HPLC) with a reversed-phase C-18 column in an isocratic mode with methanol-water (95:5, v/v), and detected with UV detection at 313 nm. The detection limit (25 ml) for the new analytical method is 0.0067 mg ml-1of hydrazine. Hydrazine showed low recovery in soil samples because components in soil oxidized hydrazine. Sludge samples that contained relatively high soil content also showed lower recovery. The technique is relatively simple and cost-effective, and is applicable for hydrazine analysis in different environmental matrices.

  9. Analysis of penicillin G in milk by liquid chromatography.

    Science.gov (United States)

    Boison, J O; Keng, L J; MacNeil, J D

    1994-01-01

    A liquid chromatographic (LC) method that was previously developed for penicillin G residues in animal tissues has been adapted to milk and milk products. After protein precipitation with sodium tungstate, samples are applied to a C18 solid-phase extraction cartridge, from which penicillin is eluted, derivatized with 1,2,4-triazole-mercuric chloride solution, and analyzed by isocratic liquid chromatography (LC) on a C18 column with UV detection at 325 nm. Quantitation is done with reference to penicillin V as an internal standard. Penicillin G recoveries were determined to be > 70% on standards fortified at 3-60 ppb. Accuracy approached 100% using the penicillin V internal standard. The detection limit for penicillin G residues was 3 ppb in fluid milk. Samples may be confirmed by thermospray/LC at concentrations approaching the detection limit of the UV method.

  10. Free silanols and ionic liquids as their suppressors in liquid chromatography.

    Science.gov (United States)

    Buszewska-Forajta, Magdalena; Markuszewski, Michał J; Kaliszan, Roman

    2018-07-20

    In this review, we will firstly discuss the types and the general properties of silica, focusing on the silica support used in chromatography and capillary electrophoresis. Additionally, the characterization of functional groups (silanols and siloxanes) will be considered in terms of activity of the stationary phases. We will then discuss physical chemistry of the stationary phases applied in liquid chromatography and capillary electrophoresis. The use of ionic liquids as a silanols' suppressors will be presented in the next parts of the study, along with the examples of specific applications. The review is completed with conclusions and an outlook for the future developments in the area of analytical applications of ionic liquids. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Fiber-based monolithic columns for liquid chromatography.

    Science.gov (United States)

    Ladisch, Michael; Zhang, Leyu

    2016-10-01

    Fiber-based monoliths for use in liquid chromatographic separations are defined by columns packed with aligned fibers, woven matrices, or contiguous fiber structures capable of achieving rapid separations of proteins, macromolecules, and low molecular weight components. A common denominator and motivating driver for this approach, first initiated 25 years ago, was reducing the cost of bioseparations in a manner that also reduced residence time of retained components while achieving a high ratio of mass to momentum transfer. This type of medium, when packed into a liquid chromatography column, minimized the fraction of stagnant liquid and resulted in a constant plate height for non-adsorbing species. The uncoupling of dispersion from eluent flow rate enabled the surface chemistry of the stationary phase to be considered separately from fluid transport phenomena and pointed to new ways to apply chemistry for the engineering of rapid bioseparations. This paper addresses developments and current research on fiber-based monoliths and explains how the various forms of this type of chromatographic stationary phase have potential to provide new tools for analytical and preparative scale separations. The different stationary phases are discussed, and a model that captures the observed constant plate height as a function of mobile phase velocity is reviewed. Methods that enable hydrodynamically stable fiber columns to be packed and operated over a range of mobile phase flow rates, together with the development of new fiber chemistries, are shown to provide columns that extend the versatility of liquid chromatography using monoliths, particularly at the preparative scale. Graphical Abstract Schematic representation of a sample mixture being separated by a rolled-stationary phase column, resulting separated peaks shown in the chromatogram.

  12. Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

    Science.gov (United States)

    Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

    2017-09-01

    A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Determination of pertechnetate by liquid chromatography with reductive electrochemical detection

    International Nuclear Information System (INIS)

    Lewis, J.Y.; Zodda, J.P.; Deutsch, E.; Heineman, W.R.

    1983-01-01

    A method utilizing liquid chromatography with electrochemical detection has been developed for the determination of total TcO 4 - (/sup 99m/TcO 4 - and /sup 99m/TcO 4 - ) in 99 Mo//sup 99m/Tc generator eluents. Pertechnetate, which is the starting material for the preparation of many diagnostic radiopharmaceuticals, is generally present in these eluents in the concentration range of 5 X 10 -8 M to 5 X 10 -6 M. No sample pretreatment is necessary since impurities and other components are separated by the high-pressure liquid chromatography (HPLC) NH 2 -bonded column. By use of both static mercury drop (SMDE) and solid electrode detectors, in conjuction with rigorous deoxygenation procedures, total TcO 4 - in generator eluents is readily determined. A severe electrode fouling phenomenon limits the use of solid electrode detectors to TcO 4 - concentrations less than 10 -7 M, the working range for a carbon electrode being 8.5 X 10 -9 to 1.0 X 10 -7 M. The working range for the SMDE is 2.1 X 10 -8 to 1.0 X 10 -4 M TcO 4 -

  14. Description of Adsorption in Liquid Chromatography under Nonideal Conditions.

    Science.gov (United States)

    Ortner, Franziska; Ruppli, Chantal; Mazzotti, Marco

    2018-05-15

    A thermodynamically consistent description of binary adsorption in reversed-phase chromatography is presented, accounting for thermodynamic nonidealities in the liquid and adsorbed phases. The investigated system involves the adsorbent Zorbax 300SB-C18, as well as phenetole and 4- tert-butylphenol as solutes and methanol and water as inert components forming the eluent. The description is based on adsorption isotherms, which are a function of the liquid-phase activities, to account for nonidealities in the liquid phase. Liquid-phase activities are calculated with a UNIQUAC model established in this work, based on experimental phase equilibrium data. The binary interaction in the adsorbed phase is described by the adsorbed solution theory, assuming an ideal (ideal adsorbed solution theory) or real (real adsorbed solution theory) adsorbed phase. Implementation of the established adsorption model in a chromatographic code achieves a quantitative description of experimental elution profiles, with feed compositions exploiting the entire miscible region, and involving a broad range of different eluent compositions (methanol/water). The quantitative agreement of the model and experimental data serves as a confirmation of the underlying physical (thermodynamic) concepts and of their applicability to a broad range of operating conditions.

  15. High temperature EXAFS experiments in molten actinide fluorides: The challenge of a triple containment cell for radioactive and aggressive liquids

    Science.gov (United States)

    Bessada, Catherine; Zanghi, Didier; Pauvert, Olivier; Maksoud, Louis; Gil-Martin, Ana; Sarou-Kanian, Vincent; Melin, Philippe; Brassamin, Séverine; Nezu, Atsushi; Matsuura, Haruaki

    2017-10-01

    An airtight double barrier cell with simple geometry has been developed for X-rays absorption measurements at high temperature in solid and molten actinide fluorides. The aim was both to improve the air tightness, to avoid any possible leakage and to maintain the high quality of the signal. The dimensions of the heating chamber were also constrained and minimized to be compatible with the limited space available usually on synchrotron beam lines and with a geometry suitable for absorption/diffraction measurements at high temperature. The design of the double barrier cell was also driven by the safety requirements in every experiment involving radioactive materials. The furnace itself was designed to ensure easy operating modes and disassembly, the aim being to consider the furnace as the ultimate containment. The cell has been tested with different molten fluorides up to more than 1000 °C, starting from non-radioactive LiF-ZrF4 mixtures in order to prove that the cell is absolutely airtight and that not any contamination of the environment occurs. Then it has been successfully applied to thorium fluoride- and uranium fluoride-alkali fluorides mixtures.

  16. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Evaluation between ultrahigh pressure liquid chromatography and high-performance liquid chromatography analytical methods for characterizing natural dyestuffs.

    Science.gov (United States)

    Serrano, Ana; van Bommel, Maarten; Hallett, Jessica

    2013-11-29

    An evaluation was undertaken of ultrahigh pressure liquid chromatography (UHPLC) in comparison to high-performance liquid chromatography (HPLC) for characterizing natural dyes in cultural heritage objects. A new UHPLC method was optimized by testing several analytical parameters adapted from prior UHPLC studies developed in diverse fields of research. Different gradient elution programs were tested on seven UHPLC columns with different dimensions and stationary phase compositions by applying several mobile phases, flow rates, temperatures, and runtimes. The UHPLC method successfully provided more improved data than that achieved by the HPLC method. Indeed, even though carminic acid has shown circa 146% higher resolution with HPLC, UHPLC resulted in an increase of 41-61% resolution and a decrease of 91-422% limit of detection, depending on the dye compound. The optimized method was subsequently assigned to analyse 59 natural reference materials, in which 85 different components were ascribed with different physicochemical properties, in order to create a spectral database for future characterization of dyes in cultural heritage objects. The majority of these reference samples could be successfully distinguished with one single method through the examination of these compounds' retention times and their spectra acquired with a photodiode array detector. These results demonstrate that UHPLC analyses are extremely valuable for the acquisition of more precise chromatographic information concerning natural dyes with complex mixtures of different and/or closely related physicochemical properties, essential for distinguishing similar species of plants and animals used to colour cultural heritage objects. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Efficient removal of H2S at high temperature using the ionic liquid solutions of [C4mim]3PMo12O40-An organic polyoxometalate.

    Science.gov (United States)

    Ma, Yunqian; Liu, Xinpeng; Wang, Rui

    2017-06-05

    An innovative approach to H 2 S capture and sulfur recovery via liquid redox at high temperature has been developed using [C 4 mim] 3 PMo 12 O 40 at temperatures ranging from 80 to 180°C, which is superior to the conventional water-based system with an upper limit of working temperature normally below 60°C. The ionic liquids used as solvents include [C 4 mim]Cl, [C 4 mim]BF 4 , [C 4 mim]PF 6 and [C 4 mim]NTf 2 . Microscopic observation and turbidity measurement were used to investigate the dissolution of [C 4 mim] 3 PMo 12 O 40 in the ionic liquids. Stabilization energy between H 2 S and the anion of ionic liquid as well as H 2 O was calculated to illustrate the interaction between H 2 S and the solvents. The cavity theory can be adopted to illustrate the mechanism for H 2 S absorption: the Cl - ion with small radius can be incorporated into the cavities of [C 4 mim] 3 PMo 12 O 40 , and interact with H 2 S strongly. The underlying mechanism for sulfur formation is the redox reaction between H 2 S and PMo 12 O 40 3- . H 2 S can be oxidized to elemental sulfur and Mo 6+ is partly reduced during absorption, according to UV-vis and FTIR spectra. The [C 4 mim] 3 PMo 12 O 40 -[C 4 mim]Cl after reaction can be readily regenerated by air and thus enabling its efficient and repeatitive use. The absorbent of [C 4 mim] 3 PMo 12 O 40 -ionic liquid system provides a new approach for wet oxidation desulfurization at high temperature. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source

    Energy Technology Data Exchange (ETDEWEB)

    Mauro, N. A., E-mail: namauro@noctrl.edu [Department of Physics, North Central College, Naperville, Illinois 60540 (United States); Vogt, A. J. [Instrument and Source Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Derendorf, K. S. [Mechanical Engineering and Materials Science, Washington University, St. Louis, Missouri 63130 (United States); Johnson, M. L.; Kelton, K. F. [Department of Physics and Institute of Materials Science and Engineering, Washington University, 1 Brookings Drive, St. Louis, Missouri 63130 (United States); Rustan, G. E.; Quirinale, D. G.; Goldman, A. I. [Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011 (United States); Kreyssig, A. [Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011 (United States); Division of Materials Sciences and Engineering, Ames Laboratory, Ames, Iowa 50011 (United States); Lokshin, K. A. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States); Quantum Condensed Matter Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Neuefeind, J. C.; An, Ke [Chemical and Engineering Materials Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Wang, Xun-Li [Department of Physics and Materials Science, City University of Hong Kong, 83 Tat Chee Ave., Kowloon (Hong Kong); Egami, T. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States); Department of Physics and Astronomy, Joint Institute for Neutron Sciences, University of Tennessee, Knoxville, Tennessee 37996 (United States)

    2016-01-15

    Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. However, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elastic and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. To demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr{sub 64}Ni{sub 36} measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample (∼100 mg)

  20. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    International Nuclear Information System (INIS)

    Mokhtarani, Babak; Gmehling, Juergen

    2010-01-01

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  1. (Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Mokhtarani, Babak [Chemistry and Chemical Engineering Research Center of Iran, P.O. Box 14335-186, Tehran (Iran, Islamic Republic of); Gmehling, Juergen, E-mail: gmehling@tech.chem.uni-oldenburg.d [Carl von Ossietzky Universitaet Oldenburg, Technische Chemie, D-26111 Oldenburg (Germany)

    2010-08-15

    (Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

  2. Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

    International Nuclear Information System (INIS)

    MarszaII, MichaI Piotr; Baczek, Tomasz; Kaliszan, Roman

    2005-01-01

    A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development

  3. Reduction of silanophilic interactions in liquid chromatography with the use of ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    MarszaII, MichaI Piotr [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Baczek, Tomasz [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland); Kaliszan, Roman [Department of Biopharmaceutics and Pharmacodynamics, Medical University of Gdansk, Gen. J. Hallera 107, 80-416 Gdansk (Poland)]. E-mail: roman.kaliszan@amg.gda.pl

    2005-08-22

    A suppression of silanophilic interactions by the selected ionic liquids added to the mobile phase in thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) is reported. Acetonitrile was used as the eluent, alone or with various concentrations of water and phosphoric buffer pH 3. Selectivity of the normal (NP) and the reversed (RP) stationary phase material was examined using a series of proton-acceptor basic drugs analytes. The ionic liquids studied appeared to significantly affect analyte retention in NP-TLC, RP-TLC and RP-HPLC systems tested. Consequently, the increased separation selectivity was attained. Due to ionic liquid additives to eluent even analytes could be chromatographed, which were not eluted from the silica-based stationary phase materials with 100% of acetonitrile in the mobile phase. Addition of ionic liquid already in very small concentration (0.5%, v/v) could reduce the amount of acetonitrile used during the optimization of basic analytes separations in TLC and HPLC systems. Moreover, the influence of temperature on the separation of basic analytes was demonstrated and considered in practical HPLC method development.

  4. Vaporization of liquid Pb-Li eutectic alloy from 1000K to 1200K - A high temperature mass spectrometric study

    Science.gov (United States)

    Jain, U.; Mukherjee, A.; Dey, G. K.

    2017-09-01

    Liquid lead-lithium eutectic will be used as a coolant in fusion reactor blanket loop. Vapor pressure of the eutectic is an important parameter to accurately predict its in-loop behavior. Past measurements of vapor pressure of the eutectic relied on indirect methods. In this paper, we report for the first time the in-situ vaporization behavior of the liquid alloy between 1042 and 1176 K by Knudsen effusion mass spectrometry (KEMS). It was seen that the vaporization occurred by independent evaporation of lead and lithium. No complex intermetallic vapor was seen in the mass spectra. The partial pressures and enthalpy of vaporization of Pb and Li were evaluated directly from the measured ion intensities formed from the equilibrium vapor over the alloy. The activity of Li over a temperature range of 1042-1176 K was found to be 4.8 × 10-5 to that of pure Li, indicating its very low activity in the alloy.

  5. Hydrophilic interaction liquid chromatography in the speciation analysis of selenium.

    Science.gov (United States)

    Sentkowska, Aleksandra; Pyrzynska, Krystyna

    2018-02-01

    The hydrophilic interaction liquid chromatography (HILIC) coupled to mass spectrometry was employed to study retention behavior of selected selenium compounds using two different HILIC stationary phases: silica and zwitterionic. Two organic solvents - acetonitrile and methanol - were compared as a component of mobile phase. Separation parameters such as a content of organic modifier, the eluent pH and inorganic buffer concentration were investigated. Based on all observations, methanol seems to be beneficial for the separation of studied compounds. The optimal HILIC separation method involved silica column and eluent composed of 85% MeOH and CH 3 COONH 4 (8 mM, pH 7) was compared to RP method in terms of time of the single run, the separation efficiency and limit of detection. Copyright © 2018 Elsevier B.V. All rights reserved.

  6. Cortisol production rates measured by liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Esteban, N.V.; Yergey, A.L.

    1990-01-01

    Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references

  7. Modern Aspects Of Fluorometric Detection In Liquid-Phase Chromatography

    Science.gov (United States)

    Bousquet, Bernard; Garnier, Jean P.; Dreux, Claude

    1983-10-01

    Recent advances are described in the combined use of fluorometric derivatization and high performance liquid chromatography (HPLC) for clinical chemistry determinations. Derivatives (especially dansyl derivatives) can be formed prior to chromatography in the case of estrogens, amino acids, and catecholamines. In post-column reactions, we preferred to use air-segmented reactions as they conform better to all the optimized chromatographic and spectrofluorometric parameters. Fluorescent derivatives produced from cate-cholamines, tryptophan and its metabolites, hydroxyindoles, tryptamine, amino acids, sugars, polyamines, and other substances are often sufficiently sensitive to be detected in picogram quantities by HPLC. Their reaction principle and some of their applications to samples are described. Recently, chemical excitation of fluorophore-like dansyl amino acid was proposed as a detection system for HPLC. By a post-column reaction, a fluorophore can be made to emit light by its reaction with trichlorophenyl oxalate (TCPO) and hydrogen peroxide. The detection limit of this system is about 10 fmol for each dansyl amino acid. Application of this new reaction to catecholamines opens up new prospects for fluorometric detection.

  8. Group type analysis of asphalt by column liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-07-01

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

  9. Analytical method for high resolution liquid chromatography for quality control French Macaw

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M; Torres Amaro, Leonid; Menendez Castillo, Rosa; Sanchez, Esther; Martinez Espinosa, Vivian; Gonzalez, Maria Lidia; Rodriguez, Carlos

    2007-01-01

    Was developed and validated an analytical method for high resolution liquid chromatography applicable to quality control of drugs dry French Macaw (Senna alata L. Roxb.) With ultraviolet detection at 340 nm. The method for high resolution liquid chromatography used to quantify the sennosides A and B, main components, was validated and proved to be specific, linear, precise and accurate. (Author)

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

    Science.gov (United States)

    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...

  11. Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

    Science.gov (United States)

    O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

    2009-01-01

    Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

  12. Towards Chip Scale Liquid Chromatography and High Throughput Immunosensing

    Energy Technology Data Exchange (ETDEWEB)

    Ni, Jing [Iowa State Univ., Ames, IA (United States)

    2000-09-21

    This work describes several research projects aimed towards developing new instruments and novel methods for high throughput chemical and biological analysis. Approaches are taken in two directions. The first direction takes advantage of well-established semiconductor fabrication techniques and applies them to miniaturize instruments that are workhorses in analytical laboratories. Specifically, the first part of this work focused on the development of micropumps and microvalves for controlled fluid delivery. The mechanism of these micropumps and microvalves relies on the electrochemically-induced surface tension change at a mercury/electrolyte interface. A miniaturized flow injection analysis device was integrated and flow injection analyses were demonstrated. In the second part of this work, microfluidic chips were also designed, fabricated, and tested. Separations of two fluorescent dyes were demonstrated in microfabricated channels, based on an open-tubular liquid chromatography (OT LC) or an electrochemically-modulated liquid chromatography (EMLC) format. A reduction in instrument size can potentially increase analysis speed, and allow exceedingly small amounts of sample to be analyzed under diverse separation conditions. The second direction explores the surface enhanced Raman spectroscopy (SERS) as a signal transduction method for immunoassay analysis. It takes advantage of the improved detection sensitivity as a result of surface enhancement on colloidal gold, the narrow width of Raman band, and the stability of Raman scattering signals to distinguish several different species simultaneously without exploiting spatially-separated addresses on a biochip. By labeling gold nanoparticles with different Raman reporters in conjunction with different detection antibodies, a simultaneous detection of a dual-analyte immunoassay was demonstrated. Using this scheme for quantitative analysis was also studied and preliminary dose-response curves from an immunoassay of a

  13. Influence of radiative heat and mass transfer mechanism in system “water droplet-high-temperature gases” on integral characteristics of liquid evaporation

    Directory of Open Access Journals (Sweden)

    Glushkov Dmitrii O.

    2015-01-01

    Full Text Available Physical and mathematical (system of differential equations in private derivatives models of heat and mass transfer were developed to investigate the evaporation processes of water droplets and emulsions on its base moving in high-temperature (more than 1000 K gas flow. The model takes into account a conductive and radiative heat transfer in water droplet and also a convective, conductive and radiative heat exchange with high-temperature gas area. Water vapors characteristic temperature and concentration in small wall-adjacent area and trace of the droplet, numerical values of evaporation velocities at different surface temperature, the characteristic time of complete droplet evaporation were determined. Experiments for confidence estimation of calculated integral characteristics of processes under investigation - mass liquid evaporation velocities were conducted with use of cross-correlation recording video equipment. Their satisfactory fit (deviations of experimental and theoretical velocities were less than 15% was obtained. The influence of radiative heat and mass transfer mechanism on characteristics of endothermal phase transformations in a wide temperature variation range was established by comparison of obtained results of numerical simulation with known theoretical data for “diffusion” mechanisms of water droplets and other liquids evaporation in gas.

  14. Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

    Science.gov (United States)

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-01-01

    A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

  15. Analysis of short-chain acids from anaerobic bacteria by high-performance liquid chromatography.

    OpenAIRE

    Guerrant, G O; Lambert, M A; Moss, C W

    1982-01-01

    A standard mixture of 25 short-chain fatty acids was resolved by high-performance liquid chromatography, using an Aminex HPX-87 column. The acids produced in culture media by anaerobic bacteria were analyzed by high-performance liquid chromatography after extraction with ether and reextraction into a small volume of 0.1 N NaOH. The presence of fumaric acid in culture extracts of Peptostreptococcus anaerobius was confirmed by gas chromatography-mass spectrometry analysis of the trapped eluent ...

  16. Amorphous and liquid samples structure and density measurements at high pressure - high temperature using diffraction and imaging techniques

    Science.gov (United States)

    Guignot, N.; King, A.; Clark, A. N.; Perrillat, J. P.; Boulard, E.; Morard, G.; Deslandes, J. P.; Itié, J. P.; Ritter, X.; Sanchez-Valle, C.

    2016-12-01

    Determination of the density and structure of liquids such as iron alloys, silicates and carbonates is a key to understand deep Earth structure and dynamics. X-ray diffraction provided by large synchrotron facilities gives excellent results as long as the signal scattered from the sample can be isolated from its environment. Different techniques already exist; we present here the implementation and the first results given by the combined angle- and energy-dispersive structural analysis and refinement (CAESAR) technique introduced by Wang et al. in 2004, that has never been used in this context. It has several advantages in the study of liquids: 1/ the standard energy-dispersive technique (EDX), fast and compatible with large multi-anvil presses frames, is used for fast analysis free of signal pollution from the sample environment 2/ some limitations of the EDX technique (homogeneity of the sample, low resolution) are irrelevant in the case of liquid signals, others (wrong intensities, escape peaks artifacts, background subtraction) are solved by the CAESAR technique 3/ high Q data (up to 15 A-1 and more) can be obtained in a few hours (usually less than 2). We present here the facilities available on the PSICHE beamline (SOLEIL synchrotron, France) and a few results obtained using a Paris-Edinburgh (PE) press and a 1200 tons load capacity multi-anvil press with a (100) DIA compression module. X-ray microtomography, used in conjunction with a PE press featuring rotating anvils (RotoPEc, Philippe et al., 2013) is also very effective, by simply measuring the 3D volume of glass or liquid spheres at HPHT, thus providing density. This can be done in conjunction with the CAESAR technique and we illustrate this point. Finally, absorption profiles can be obtained via imaging techniques, providing another independent way to measure the density of these materials. References Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy

  17. Numerical simulation of the heat transfer at cooling a high-temperature metal cylinder by a flow of a gas-liquid medium

    Science.gov (United States)

    Makarov, S. S.; Lipanov, A. M.; Karpov, A. I.

    2017-10-01

    The numerical modeling results for the heat transfer during cooling a metal cylinder by a gas-liquid medium flow in an annular channel are presented. The results are obtained on the basis of the mathematical model of the conjugate heat transfer of the gas-liquid flow and the metal cylinder in a two-dimensional nonstationary formulation accounting for the axisymmetry of the cooling medium flow relative to the cylinder longitudinal axis. To solve the system of differential equations the control volume approach is used. The flow field parameters are calculated by the SIMPLE algorithm. To solve iteratively the systems of linear algebraic equations the Gauss-Seidel method with under-relaxation is used. The results of the numerical simulation are verified by comparing the results of the numerical simulation with the results of the field experiment. The calculation results for the heat transfer parameters at cooling the high-temperature metal cylinder by the gas-liquid flow are obtained with accounting for evaporation. The values of the rate of cooling the cylinder by the laminar flow of the cooling medium are determined. The temperature change intensity for the metal cylinder is analyzed depending on the initial velocity of the liquid flow and the time of the cooling process.

  18. Quantitation of Metformin in Human Plasma and Urine by Hydrophilic Interaction Liquid Chromatography and Application to a Pharmacokinetic Study

    DEFF Research Database (Denmark)

    Nielsen, Flemming; Hougaard Christensen, Mette Marie; Brøsen, Kim

    2014-01-01

    : We describe an analytical method for the quantification of the widely used antihyperglycemic agent, metformin, in human plasma and urine. The separation was performed using isocratic hydrophilic interaction liquid chromatography on a Luna hydrophilic interaction liquid chromatography column (125...

  19. Kinetics of iron redox reactions in silicate liquids: A high-temperature X-ray absorption and Raman spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Magnien, V. [Physique des Mineraux et Magmas, CNRS-IPGP, 4 place Jussieu, 75252 Paris cedex 05 (France); CEA VALRHO Marcoule, SCDV, LEBV, BP 17171, 30207 Bagnols/Ceze (France); Neuville, D.R. [Physique des Mineraux et Magmas, CNRS-IPGP, 4 place Jussieu, 75252 Paris cedex 05 (France)]. E-mail: neuville@ipgp.jussieu.fr; Cormier, L. [IMPMC, CNRS UMR 7590, Universites Paris 6 and 7 and IPGP, 4 place Jussieu, 75252 Paris cedex 05 (France); Roux, J. [Physique des Mineraux et Magmas, CNRS-IPGP, 4 place Jussieu, 75252 Paris cedex 05 (France); Hazemann, J.-L. [Laboratoire de cristallographie, UPR 5031, CNRS, 38043 Grenoble (France); Pinet, O. [CEA VALRHO Marcoule, SCDV, LEBV, BP 17171, 30207 Bagnols/Ceze (France); Richet, P. [Physique des Mineraux et Magmas, CNRS-IPGP, 4 place Jussieu, 75252 Paris cedex 05 (France)

    2006-06-30

    The oxidation kinetics of a Fe-bearing supercooled liquid of the system SiO{sub 2}-CaO-MgO-Na{sub 2}O-FeO has been determined near the glass transition range by X-ray absorption near edge structure (XANES) and Raman spectroscopies. Both techniques yield room-temperature iron redox ratios in accord with wet chemical, Moessbauer and electron microprobe analyses. Similar oxidation kinetics have also been observed with both methods. At constant temperature, the kinetics obey an exponential law with a characteristic time that follows an Arrhenian temperature dependence. As redox changes are too fast to be accounted for in terms of diffusion of either ionic or molecular oxygen, these results lend further support to the idea that the rate-limiting factor for oxidation near the glass transition is diffusion of network-modifying cations along with a flux of electron holes.

  20. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    OpenAIRE

    Suriyavathana Muthukrishnan; Subha Palanisamy; Senthilkumar Subramanian; Sumathi Selvaraj; Kavitha Rani Mari; Ramalingam Kuppulingam

    2016-01-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. Th...

  1. Study of Separation and Identification of the Active Ingredients in Gardenia jasminoides Ellis Based on a Two-Dimensional Liquid Chromatography by Coupling Reversed Phase Liquid Chromatography and Hydrophilic Interaction Liquid Chromatography.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2017-01-01

    In this paper, by coupling reversed phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), a two-dimensional liquid chromatography system was developed for separation and identification of the active ingredients in Gardenia jasminoides Ellis (GJE). By applying the semi-preparative C18 column as the first dimension and the core-shell column as the second dimension, a total of 896 peaks of GJE were separated. Among the 896 peaks, 16 active ingredients including geniposide, gardenoside, gardoside, etc. were identified by mass spectrometry analysis. The results indicated that the proposed two-dimensional RPLC/HILIC system was an effective method for the analysis of GJE and might hold a high potential to become a useful tool for analysis of other complex mixtures. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

    DEFF Research Database (Denmark)

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

    1994-01-01

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

  3. Role of Oxides and Porosity on High-Temperature Oxidation of Liquid-Fueled HVOF Thermal-Sprayed Ni50Cr Coatings

    Science.gov (United States)

    Song, B.; Bai, M.; Voisey, K. T.; Hussain, T.

    2017-02-01

    High chromium content in Ni50Cr thermally sprayed coatings can generate a dense and protective scale at the surface of coating. Thus, the Ni50Cr coating is widely used in high-temperature oxidation and corrosion applications. A commercially available gas atomized Ni50Cr powder was sprayed onto a power plant steel (ASME P92) using a liquid-fueled high velocity oxy-fuel thermal spray with three processing parameters in this study. Microstructure of as-sprayed coatings was examined using oxygen content analysis, mercury intrusion porosimetry, scanning electron microscope (SEM), energy-dispersive x-ray spectroscopy (EDX) and x-ray diffraction (XRD). Short-term air oxidation tests (4 h) of freestanding coatings (without boiler steel substrate) in a thermogravimetric analyzer at 700 °C were performed to obtain the kinetics of oxidation of the as-sprayed coating. Long-term air oxidation tests (100 h) of the coated substrates were performed at same temperature to obtain the oxidation products for further characterization in detail using SEM/EDX and XRD. In all samples, oxides of various morphologies developed on top of the Ni50Cr coatings. Cr2O3 was the main oxidation product on the surface of all three coatings. The coating with medium porosity and medium oxygen content has the best high-temperature oxidation performance in this study.

  4. Standard Practice for Installation, Inspection, and Maintenance of Valve-body Pressure-relief Methods for Geothermal and Other High-Temperature Liquid Applications

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2003-01-01

    1.1 This practice covers installation, inspection, and maintenance of valve body cavity pressure relief methods for valves used in geothermal and other high-temperature liquid service. The valve type covered by this practice is a design with an isolated body cavity such that when the valve is in either the open or closed position pressure is trapped in the isolated cavity, and there is no provision to relieve the excess pressure internally. 1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  5. Unified pH values of liquid chromatography mobile phases.

    Science.gov (United States)

    Suu, Agnes; Jalukse, Lauri; Liigand, Jaanus; Kruve, Anneli; Himmel, Daniel; Krossing, Ingo; Rosés, Martí; Leito, Ivo

    2015-03-03

    This work introduces a conceptually new approach of measuring pH of mixed-solvent liquid chromatography (LC) mobile phases. Mobile phase pH is very important in LC, but its correct measurement is not straightforward, and all commonly used approaches have deficiencies. The new approach is based on the recently introduced unified pH (pH(abs)) scale, which enables direct comparison of acidities of solutions made in different solvents based on chemical potential of the proton in the solutions. This work represents the first experimental realization of the pH(abs) concept using differential potentiometric measurement for comparison of the chemical potentials of the proton in different solutions (connected by a salt bridge), together with earlier published reference points for obtaining the pH(abs) values (referenced to the gas phase) or pH(abs)(H₂O) values (referenced to the aqueous solution). The liquid junction potentials were estimated in the framework of Izutsu's three-component method. pH(abs) values for a number of common LC and LC-MS mobile phases have been determined. The pH(abs) scale enables for the first time direct comparison of acidities of any LC mobile phases, with different organic additives, different buffer components, etc. A possible experimental protocol of putting this new approach into chromatographic practice has been envisaged and its applicability tested. It has been demonstrated that the ionization behavior of bases (cationic acids) in the mobile phases can be better predicted by using the pH(abs)(H₂O) values and aqueous pKa values than by using the alternative means of expressing mobile phase acidity. Description of the ionization behavior of acids on the basis of pH(abs)(H₂O) values is possible if the change of their pKa values with solvent composition change is taken into account.

  6. Liquid chromatography-mass spectrometry in forensic toxicology.

    Science.gov (United States)

    Van Bocxlaer, J F; Clauwaert, K M; Lambert, W E; Deforce, D L; Van den Eeckhout, E G; De Leenheer, A P

    2000-01-01

    Liquid chromatography-mass spectrometry has evolved from a topic of mainly research interest into a routinely usable tool in various application fields. With the advent of new ionization approaches, especially atmospheric pressure, the technique has established itself firmly in many areas of research. Although many applications prove that LC-MS is a valuable complementary analytical tool to GC-MS and has the potential to largely extend the application field of mass spectrometry to hitherto "MS-phobic" molecules, we must recognize that the use of LC-MS in forensic toxicology remains relatively rare. This rarity is all the more surprising because forensic toxicologists find themselves often confronted with the daunting task of actually searching for evidence materials on a scientific basis without any indication of the direction in which to search. Through the years, mass spectrometry, mainly in the GC-MS form, has gained a leading role in the way such quandaries are tackled. The advent of robust, bioanalytically compatible combinations of liquid chromatographic separation with mass spectrometric detection really opens new perspectives in terms of mass spectrometric identification of difficult molecules (e.g., polar metabolites) or biopolymers with toxicological relevance, high throughput, and versatility. Of course, analytical toxicologists are generally mass spectrometry users rather than mass spectrometrists, and this difference certainly explains the slow start of LC-MS in this field. Nevertheless, some valuable applications have been published, and it seems that the introduction of the more universal atmospheric pressure ionization interfaces really has boosted interests. This review presents an overview of what has been realized in forensic toxicological LC-MS. After a short introduction into LC-MS interfacing operational characteristics (or limitations), it covers applications that range from illicit drugs to often abused prescription medicines and some

  7. Microcystin Detection Characteristics of Fluorescence Immunochromatography and High Performance Liquid Chromatography

    International Nuclear Information System (INIS)

    Pyo, Dong Jin; Park, Geun Young; Choi, Jong Chon; Oh, Chang Suk

    2005-01-01

    Different detection characteristics of fluorescence immunochromatography method and high performance liquid chromatography (HPLC) method for the analysis of cyanobacterial toxins were studied. In particular, low and high limits of detection, detection time and reproducibility and detectable microcystin species were compared when fluorescence immunochromatography method and high performance liquid chromatography method were applied for the detection of microcystin (MC), a cyclic peptide toxin of the freshwater cyanobacterium Microcystis aeruginosa. A Fluorescence immunochromatography assay system has the unique advantages of short detection time and low detection limit, and high performance liquid chromatography detection method has the strong advantage of individual quantifications of several species of microcystins

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

    Science.gov (United States)

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

  9. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    International Nuclear Information System (INIS)

    Mroczek, Tomasz; Ndjoko-Ioset, Karine; Glowniak, Kazimierz; Mietkiewicz-Capala, Agnieszka; Hostettmann, Kurt

    2006-01-01

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C 18 column using a gradient elution. Based on MS n spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide

  10. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mroczek, Tomasz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland)]. E-mail: tmroczek@pharmacognosy.org; Ndjoko-Ioset, Karine [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland); Glowniak, Kazimierz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Mietkiewicz-Capala, Agnieszka [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Hostettmann, Kurt [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland)

    2006-05-04

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C{sub 18} column using a gradient elution. Based on MS {sup n} spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide.

  11. Electrochemically modulated liquid chromatography: Theoretical investigations and applications from the perspectives of chromatography and interfacial electrochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Keller, David W. [Iowa State Univ., Ames, IA (United States)

    2005-01-01

    Electrochemically modulated liquid chromatography (EMLC) employs a conductive material as both a stationary phase for chromatographic separations and as a working electrode for performing electrochemistry experiments. This dual functionality gives EMLC the capacity to manipulate chromatographic separations by changing the potential applied (Eapp) to the stationary phase with respect to an external reference. The ability to monitor retention as a function of Eapp provides a means to chromatographically monitor electrosorption processes at solid-liquid interfaces. In this dissertation, the retention mechanism for EMLC is examined from the perspective of electrical double layer theory and interfacial thermodynamics. From the chromatographic data, it is possible to determine the interfacial excess (Λ) of a solute and changes in interfacial tension (dγ) as a function of both Eapp and the supporting electrolyte concentration. Taken together, these two experimentally manipulated parameters can be examined within the context of the Gibbs adsorption equation to delineate the contribution of a variety of interfacial properties, including the charge of solute on the stationary phase and the potential of zero charge (PZC), to the mechanism behind EMLC-based retention. The chromatographic probing of interfacial phenomena is complemented by electroanalytical experiments that exploit the ability to monitor the electronic current flowing through an EMLC column. Cyclic voltammetry and chronoamperometry of an EMLC column are used to determine the electronic performance characteristics of an EMLC column. An electrochemical flow injection analysis of a column is provided in which the current required to maintain a constant Eapp is monitored and provides a way to examine the influence that acetonitrile and supporting electrolyte composition, flow rate, column backpressure, and ionic strength have on the structure of electrified interfaces.

  12. How to separate ionic liquids: Use of Hydrophilic Interaction Liquid Chromatography and mixed mode phases

    International Nuclear Information System (INIS)

    Lamouroux, C.

    2011-01-01

    This chromatographic study deals with the development of a convenient and versatile method to separate Room Temperature Ionic Liquids. Different modes of chromatography were studied. The study attempts to answer the following question: 'what were the most important interactions for the separation of ionic liquids?'. The results show that the essential interactions to assure a good retention of RTILs are the ionic ones and that hydrophobic interactions play a role in the selectivity of the separation. The separation of five imidazolium salt with a traditional dial columns in Hydrophilic Interaction Chromatography (HILIC) was demonstrated. It shows that neutral diol grafted column allows an important retention that we assume is due to the capability of diol to develop a thick layer of water. Furthermore, stationary phase based on mixed interaction associating ion exchange and hydrophobic properties were studied. Firstly, it will be argued that it is possible to separate RTILs with a convenient retention and resolution according to a reverse phase elution with the Primesep columns made of a brush type long alkyl chain with an embedded negatively charged functional group. Secondly, a successful separation of RTILs in HILIC mode with a mixed phase column containing a cationic exchanger and a hydrophobic octyl chain length will be demonstrated. (author)

  13. Surface-bonded ionic liquid stationary phases in high-performance liquid chromatography--a review.

    Science.gov (United States)

    Pino, Verónica; Afonso, Ana M

    2012-02-10

    Ionic liquids (ILs) are a class of ionic, nonmolecular solvents which remain in liquid state at temperatures below 100°C. ILs possess a variety of properties including low to negligible vapor pressure, high thermal stability, miscibility with water or a variety of organic solvents, and variable viscosity. IL-modified silica as novel high-performance liquid chromatography (HPLC) stationary phases have attracted considerable attention for their differential behavior and low free-silanol activity. Indeed, around 21 surface-confined ionic liquids (SCIL) stationary phases have been developed in the last six years. Their chromatographic behavior has been studied, and, despite the presence of a positive charge on the stationary phase, they showed considerable promise for the separation of neutral solutes (not only basic analytes), when operated in reversed phase mode. This aspect points to the potential for truly multimodal stationary phases. This review attempts to summarize the state-of-the-art about SCIL phases including their preparation, chromatographic behavior, and analytical performance. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO2 using ionic liquid as a template

    International Nuclear Information System (INIS)

    Liu, Hong; Wang, Mengyang; Hu, Hongjiu; Liang, Yuguang; Wang, Yong; Cao, Weiran; Wang, Xiaohong

    2011-01-01

    Mesoporous silicas and Fe-SiO 2 with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 o C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 o C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 o C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO 2 has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 o C for 12 d or steam-treated at 600 o C for 6 h. -- Graphical abstract: Worm-like mesoporous silica and Fe-SiO 2 with high hydrothermal stability have been synthesized using ionic liquid 1-hexadecane-3-methylimidazolium bromide as a template under the assistance of NaF at high temperature. Display Omitted Research highlights: → Increasing aging temperature improved the hydrothermal stability of materials. →Addition of NaF enhanced the polymerization degree of silicates. → Mesoporous SiO 2 and Fe-SiO 2 obtained have remarkable hydrothermal stability.

  15. Effects of Heat Treatment on the Microstructures and High Temperature Mechanical Properties of Hypereutectic Al-14Si-Cu-Mg Alloy Manufactured by Liquid Phase Sintering Process

    Science.gov (United States)

    Heo, Joon-Young; Gwon, Jin-Han; Park, Jong-Kwan; Lee, Kee-Ahn

    2018-05-01

    Hypereutectic Al-Si alloy is an aluminum alloy containing at least 12.6 wt.% Si. It is necessary to evenly control the primary Si particle size and distribution in hypereutectic Al-Si alloy. In order to achieve this, there have been attempts to manufacture hypereutectic Al-Si alloy through a liquid phase sintering. This study investigated the microstructures and high temperature mechanical properties of hypereutectic Al-14Si-Cu-Mg alloy manufactured by liquid phase sintering process and changes in them after T6 heat treatment. Microstructural observation identified large amounts of small primary Si particles evenly distributed in the matrix, and small amounts of various precipitation phases were found in grain interiors and grain boundaries. After T6 heat treatment, the primary Si particle size and shape did not change significantly, but the size and distribution of CuAl2 ( θ) and AlCuMgSi ( Q) changed. Hardness tests measured 97.36 HV after sintering and 142.5 HV after heat treatment. Compression tests were performed from room temperature to 300 °C. The results represented that yield strength was greater after heat treatment (RT 300 °C: 351 93 MPa) than after sintering (RT 300 °C: 210 89 MPa). Fracture surface analysis identified cracks developing mostly along the interface between the primary Si particles and the matrix with some differences among temperature conditions. In addition, brittle fracture mode was found after T6 heat treatment.

  16. Process of quantity determination of uranium by chromatography in liquid zone

    International Nuclear Information System (INIS)

    Muller, J.P.; Cojean, J.; Daubizit, M.

    1993-01-01

    The invention concerns a process of quantity determination of uranium by chromatography in liquid zone, usable to determine the quantity of uranium traces. Solutions to be treated can be aqueous or organic

  17. Qualitative and quantitative determination of ubiquinones by the method of high-efficiency liquid chromatography

    International Nuclear Information System (INIS)

    Yanotovskii, M.T.; Mogilevskaya, M.P.; Obol'nikova, E.A.; Kogan, L.M.; Samokhvalov, G.I.

    1986-01-01

    A method has been developed for the qualitative and quantitative determination of ubiquinones CoQ 6 -CoQ 10 , using high-efficiency reversed-phase liquid chromatography. Tocopherol acetate was used as the internal standard

  18. Determination of Aspartame, Caffeine, Saccharin, and Benzoic Acid in Beverages by High Performance Liquid Chromatography.

    Science.gov (United States)

    Delaney, Michael F.; And Others

    1985-01-01

    Describes a simple and reliable new quantitative analysis experiment using liquid chromatography for the determinaiton of caffeine, saccharin, and sodium benzoate in beverages. Background information, procedures used, and typical results obtained are provided. (JN)

  19. Experimental hydrophobicity parameters of perfluorinated alkylated substances from reversed-phase high performance liquid chromatography

    NARCIS (Netherlands)

    de Voogt, P.; Zurano, L.; Serné, P.; Haftka, J.J.H.

    2012-01-01

    Capacity factors of perfluorinated alkylated substances were obtained from isocratic reversed-phase high-performance liquid chromatography-mass spectrometry experiments at different organic modifier strengths of the mobile phase. The resulting capacity factor v. modifier strengths plots were

  20. Determination of maduramicin in feedingstuffs and premixtures by liquid chromatography : development, validation and interlaboratory study

    NARCIS (Netherlands)

    Jong, de J.; Stoisser, B.; Wagner, K.; Tomassen, M.J.H.; Driessen, J.J.M.; Hofman, P.; Putzka, H.A.

    2004-01-01

    A reversed-phase liquid chromatography method for determination of maduramicin in feedingstuffs and premixtures was developed, validated, and interlaboratory studied. The extraction solvent was methanol. Maduramicin was detected at 520 nm after postcolumn derivatization with vanillin. Recovery was

  1. Assay for dihydroorotase using high-performance liquid chromatography with radioactivity detection

    International Nuclear Information System (INIS)

    Mehdi, S.; Wiseman, J.S.

    1989-01-01

    An assay for measuring dihydroorotase activity was devised. Radiolabeled substrate and product were separated by high-performance liquid chromatography using a reverse-phase column with ion-pairing, and the radioactivity was quantitated by flow detection

  2. An efficient hydrophilic interaction liquid chromatography separation of 7 phospholipid classes based on a diol column

    NARCIS (Netherlands)

    Zhu, C.; Dane, A.; Spijksma, G.; Wang, M.; Greef, J. van der; Luo, G.; Hankemeier, T.; Vreeken, R.J.

    2012-01-01

    A hydrophilic interaction liquid chromatography (HILIC) - ion trap mass spectrometry method was developed for separation of a wide range of phospholipids. A diol column which is often used with normal phase chromatography was adapted to separate different phospholipid classes in HILIC mode using a

  3. Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

    Science.gov (United States)

    Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

    2017-07-01

    A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Determination of methylphenidate in Calliphorid larvae by liquid-liquid extraction and liquid chromatography mass spectrometry - Forensic entomotoxicology using an in vivo rat brain model

    DEFF Research Database (Denmark)

    Bushby, Sarah K.; Thomas, Nicky; Priemel, Petra A.

    2012-01-01

    and Calliphorid larvae) by liquid-liquid extraction with recovery of >80%, and quantified using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The LC-MS/MS assay was validated for entomotoxicological use and initially applied to male Sprague-Dawley rats (n=6) that were dosed with MPH (20mg/kg) ante...

  5. Chromatography.

    Science.gov (United States)

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

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

  6. Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

    DEFF Research Database (Denmark)

    Corr, J. J.; Larsen, Erik Huusfeldt

    1996-01-01

    Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes...... fragmentation patterns showing molecular dissociation through an expected common product ion were obtained for the four arsenosugars, Molecular mode detection was utilized for qualitative verification of speciation analysis by high-performance liquid chromatography coupled to inductively coupled plasma mass...

  7. Liquid chromatography-mass spectrometry coupling by the intermediary of a liquid micro chromatography-electro spray interface; Couplage chromatographie liquide-spectrometrie de masse par l`intermediaire d`une interface electrospray-microchromatographie liquide

    Energy Technology Data Exchange (ETDEWEB)

    Gillard Factor, C

    1996-12-06

    The objective of this work is to realize a liquid chromatography- mass spectrometry coupling by the intermediary of an electro spray interface and the evaluation of performances of tis analytical tool to study pollutants in water, and more particularly pesticides whom maximum admissible concentration in a table water is 0.1{mu}g/l. This study has allowed to bring to the fore the interest of the ionization mode by electro spray in a LC/MS coupling to identify and quantify pesticides in the state of traces without treating the sample. Then, it was demonstrated the usefulness of this analytical tool to detect high molecular masses molecules. (N.C.)

  8. Tryptophan and kynurenine determination in human hair by liquid chromatography.

    Science.gov (United States)

    Dario, Michelli F; Freire, Thamires Batello; Pinto, Claudinéia Aparecida Sales de Oliveira; Prado, María Segunda Aurora; Baby, André R; Velasco, Maria Valéria R

    2017-10-15

    Tryptophan, an amino acid found in hair proteinaceous structure is used as a marker of hair photodegradation. Also, protein loss caused by several chemical/physical treatments can be inferred by tryptophan quantification. Kynurenine is a photo-oxidation product of tryptophan, expected to be detected when hair is exposed mainly to UVB (290-320nm) radiation range. Tryptophan from hair is usually quantified directly as a solid or after alkaline hydrolysis, spectrofluorimetrically. However, these types of measure are not sufficiently specific and present several interfering substances. Thus, this work aimed to propose a quantification method for both tryptophan and kynurenine in hair samples, after alkali hydrolysis process, by using high-performance liquid chromatography (HPLC) with fluorimetric and UV detection. The tryptophan and kynurenine quantification method was developed and validated. Black, white, bleached and dyed (blond and auburn) hair tresses were used in this study. Tryptophan and kynurenine were separated within ∼9min by HPLC. Both black and white virgin hair samples presented similar concentrations of tryptophan, while bleaching caused a reduction in the tryptophan content as well as dyeing process. Unexpectedly, UV/vis radiation did not promote significantly the conversion of tryptophan into its photo-oxidation product and consequently, kynurenine was not detected. Thus, this works presented an acceptable method for quantification of tryptophan and its photooxidation metabolite kynurenine in hair samples. Also, the results indicated that bleaching and dyeing processes promoted protein/amino acids loss but tryptophan is not extensively degraded in human hair by solar radiation. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Liquid chromatography method to determine polyamines in thermosetting polymers

    Energy Technology Data Exchange (ETDEWEB)

    Dopico-Garcia, M.S. [Laboratorio de Quimica - Centro de Investigacions Tecnoloxicas, Universidade da Coruna, Campus de Esteiro s/n, 15403 Ferrol (Spain); Centro Galego do Plastico, A Cabana s/n, 15590 Ferrol (Spain); Lopez-Vilarino, J.M. [Laboratorio de Quimica - Centro de Investigacions Tecnoloxicas, Universidade da Coruna, Campus de Esteiro s/n, 15403 Ferrol (Spain); Fernandez-Martinez, G. [Unidad de Tecnicas Cromatograficas, Servizos de Apoio a Investigacion, Edificio Servizos Centrais de Investigacion, Universidade da Coruna, Campus de Elvina s/n, 15071 A Coruna (Spain); Gonzalez-Rodriguez, M.V., E-mail: victoria@udc.es [Dpto. de Quimica Analitica - E.U. Politecnica, Universidade da Coruna, Avda. 19 de Febrero s/n, 15405 Ferrol (Spain)

    2010-05-14

    A simple, robust and sensitive analytical method to determine three polyamines commonly used as hardeners in epoxy resin systems and in the manufacture of polyurethane is reported. The studied polyamines are: one tetramine, TETA (triethylenetetramine), and two diamines, IPDA (Isophorone diamine) and TCD-diamine (4,7-methano-1H-indene-5,?-dimethanamine, octahydro-). The latter has an incompletely defined structure, and, as far as we know, has not been previously determined by other methods. All three polyamines contain primary amines; TETA also contains secondary amines. The analytical method involves derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, used for the first time for these compounds, followed by high performance liquid chromatography (HPLC) analysis with a fluorescence (FL) detector ({lambda} excitation 248 nm, {lambda} emision 395 nm). The HPLC-DAD-LTQ Orbitrap MS was used in order to provide structural information about the obtained derivatized compounds. The hybrid linear ion trap LTQ Orbitrap mass spectrometer has been introduced in recent years and provides a high mass accuracy. The structures of the derivatized analytes were identified from the protonated molecular ions [M+H]{sup +} and corresponded to the fully labelled analytes. The following analytical parameters were determined for the method using the HPLC-FL: linearity, precision (2.5-10%), instrumental precision intraday (0.8-1.5%) and interday (2.9-6.3%), and detection limits (0.02-0.14 mg L{sup -1}). The stability of stock solutions and derivatized compounds was also investigated. The method was applied to determine the amine free content in epoxy resin dust collected in workplaces.

  10. Liquid chromatography method to determine polyamines in thermosetting polymers.

    Science.gov (United States)

    Dopico-García, M S; López-Vilariño, J M; Fernández-Martínez, G; González-Rodríguez, M V

    2010-05-14

    A simple, robust and sensitive analytical method to determine three polyamines commonly used as hardeners in epoxy resin systems and in the manufacture of polyurethane is reported. The studied polyamines are: one tetramine, TETA (triethylenetetramine), and two diamines, IPDA (Isophorone diamine) and TCD-diamine (4,7-methano-1H-indene-5,?-dimethanamine, octahydro-). The latter has an incompletely defined structure, and, as far as we know, has not been previously determined by other methods. All three polyamines contain primary amines; TETA also contains secondary amines. The analytical method involves derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, used for the first time for these compounds, followed by high performance liquid chromatography (HPLC) analysis with a fluorescence (FL) detector (lambda excitation 248nm, lambda emision 395nm). The HPLC-DAD-LTQ Orbitrap MS was used in order to provide structural information about the obtained derivatized compounds. The hybrid linear ion trap LTQ Orbitrap mass spectrometer has been introduced in recent years and provides a high mass accuracy. The structures of the derivatized analytes were identified from the protonated molecular ions [M+H](+) and corresponded to the fully labelled analytes. The following analytical parameters were determined for the method using the HPLC-FL: linearity, precision (2.5-10%), instrumental precision intraday (0.8-1.5%) and interday (2.9-6.3%), and detection limits (0.02-0.14mgL(-1)). The stability of stock solutions and derivatized compounds was also investigated. The method was applied to determine the amine free content in epoxy resin dust collected in workplaces. Copyright 2010 Elsevier B.V. All rights reserved.

  11. Liquid chromatography method to determine polyamines in thermosetting polymers

    International Nuclear Information System (INIS)

    Dopico-Garcia, M.S.; Lopez-Vilarino, J.M.; Fernandez-Martinez, G.; Gonzalez-Rodriguez, M.V.

    2010-01-01

    A simple, robust and sensitive analytical method to determine three polyamines commonly used as hardeners in epoxy resin systems and in the manufacture of polyurethane is reported. The studied polyamines are: one tetramine, TETA (triethylenetetramine), and two diamines, IPDA (Isophorone diamine) and TCD-diamine (4,7-methano-1H-indene-5,?-dimethanamine, octahydro-). The latter has an incompletely defined structure, and, as far as we know, has not been previously determined by other methods. All three polyamines contain primary amines; TETA also contains secondary amines. The analytical method involves derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, used for the first time for these compounds, followed by high performance liquid chromatography (HPLC) analysis with a fluorescence (FL) detector (λ excitation 248 nm, λ emision 395 nm). The HPLC-DAD-LTQ Orbitrap MS was used in order to provide structural information about the obtained derivatized compounds. The hybrid linear ion trap LTQ Orbitrap mass spectrometer has been introduced in recent years and provides a high mass accuracy. The structures of the derivatized analytes were identified from the protonated molecular ions [M+H] + and corresponded to the fully labelled analytes. The following analytical parameters were determined for the method using the HPLC-FL: linearity, precision (2.5-10%), instrumental precision intraday (0.8-1.5%) and interday (2.9-6.3%), and detection limits (0.02-0.14 mg L -1 ). The stability of stock solutions and derivatized compounds was also investigated. The method was applied to determine the amine free content in epoxy resin dust collected in workplaces.

  12. Separation of anionic oligosaccharides by high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Green, E.D.; Baenziger, J.U.

    1986-01-01

    The authors have developed methods for rapid fractionation of anionic oligosaccharides containing sulfate and/or sialic acid moieties by high-performance liquid chromatography (HPLC). Ion-exchange HPLC on amine-bearing columns (Micropak AX-10 and AX-5) at pH 4.0 is utilized to separate anionic oligosaccharides bearing zero, one, two, three, or four charges, independent of the identity of the anionic moieties (sulfate and/or sialic acid). Ion-exchange HPLC at pH 1.7 allows separation of neutral, mono-, di-, and tetrasialylated, monosulfated, and disulfated oligosaccharides. Oligosaccharides containing three sialic acid residues and those bearing one each of sulfate and sialic acid, however, coelute at pH 1.7. Since the latter two oligosaccharide species separate at pH 4.0, analysis at pH 4.0 followed by analysis at pH 1.7 can be utilized to completely fractionate complex mixtures of sulfated and sialylated oligosaccharides. Ion-suppression amine adsorption HPLC has previously been shown to separate anionic oligosaccharides on the basis of net carbohydrate content (size). In this study they demonstrate the utility of ion-suppression amine adsorption HPLC for resolving sialylated oligosaccharide isomers which differ only in the linkages of sialic acid residues (α2,3 vs α2,6) and/or location of α2,3- and α2,6-linked sialic acid moieties on the peripheral branches of oligosaccharides. These two methods can be used in tandem to separate oligosaccharides, both analytically and preparatively, based on their number, types, and linkages of anionic moieties

  13. Rapid screening for drugs of abuse in biological fluids by ultra high performance liquid chromatography/Orbitrap mass spectrometry.

    Science.gov (United States)

    Jagerdeo, Eshwar; Schaff, Jason E

    2016-08-01

    We present a UPLC(®)-High Resolution Mass Spectrometric method to simultaneously screen for nineteen benzodiazepines, twelve opiates, cocaine and three metabolites, and three "Z-drug" hypnotic sedatives in both blood and urine specimens. Sample processing consists of a high-speed, high-temperature enzymatic hydrolysis for urine samples followed by a rapid supported liquid extraction (SLE). The combination of ultra-high resolution chromatography with high resolution mass spectrometry allows all 38 analytes to be uniquely detected with a ten minute analytical run. Limits of detection for all target analytes are 3ng/mL or better, with only 0.3mL of specimen used for analysis. The combination of low sample volume with fast processing and analysis makes this method a suitable replacement for immunoassay screening of the targeted drug classes, while providing far superior specificity and better limits of detection than can routinely be obtained by immunoassay. Published by Elsevier B.V.

  14. Study of high performance liquid chromatography fingerprint for traditional chinese medicine yigongningxue oral liquid

    International Nuclear Information System (INIS)

    Feng, C.; Ruan, J.L.

    2010-01-01

    A simple, reliable and accurate fingerprinting method has been developed for quality control of YiGongNingXue oral liquid. The separation was done by reverse phase chromatography using Zorbax eclipse XDB C/sub 18/ column (250mmx4.6mmi. d. with 5.0 micro m particle size) and detection at 246nm. Methanol (5-95 % in 70 min)-buffer solution (water-phosphorica cid, pH 3.0, 95-0 percent in 70 min) as mobile phase for linear gradient elution. The flow rate was 1.0 mLmin/sup 1/ and the column temperature was at 25 deg. C. The similarity of 20 batches of YGNX oral liquid was more than 90 %. Also 15 common peaks of chromatogram have been detected, ten of them were identified by comparing fingerprint chromatogram with reference substances The HPLC fingerprint can be used to control the quality of YiGongNingXue oral liquid. (author)

  15. Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

    Science.gov (United States)

    Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

    2017-10-13

    A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Computational study of heat transfer from the inner surface of a circular tube to force high temperature liquid metal flow in laminar and transition regions

    Science.gov (United States)

    Hata, K.; Fukuda, K.; Masuzaki, S.

    2018-03-01

    transfer. The general correlation in the laminar and turbulent regions for a high temperature liquid metal was identified for the circular tube with a hydraulic diameter.

  17. High-temperature dynamic behavior in bulk liquid water: A molecular dynamics simulation study using the OPC and TIP4P-Ew potentials

    Science.gov (United States)

    Gabrieli, Andrea; Sant, Marco; Izadi, Saeed; Shabane, Parviz Seifpanahi; Onufriev, Alexey V.; Suffritti, Giuseppe B.

    2018-02-01

    Classical molecular dynamics simulations were performed to study the high-temperature (above 300 K) dynamic behavior of bulk water, specifically the behavior of the diffusion coefficient, hydrogen bond, and nearest-neighbor lifetimes. Two water potentials were compared: the recently proposed "globally optimal" point charge (OPC) model and the well-known TIP4P-Ew model. By considering the Arrhenius plots of the computed inverse diffusion coefficient and rotational relaxation constants, a crossover from Vogel-Fulcher-Tammann behavior to a linear trend with increasing temperature was detected at T* ≈ 309 and T* ≈ 285 K for the OPC and TIP4P-Ew models, respectively. Experimentally, the crossover point was previously observed at T* ± 315-5 K. We also verified that for the coefficient of thermal expansion α P ( T, P), the isobaric α P ( T) curves cross at about the same T* as in the experiment. The lifetimes of water hydrogen bonds and of the nearest neighbors were evaluated and were found to cross near T*, where the lifetimes are about 1 ps. For T T*, water behaves more like a simple liquid. The fact that T* falls within the biologically relevant temperature range is a strong motivation for further analysis of the phenomenon and its possible consequences for biomolecular systems.

  18. Effects of Coolant Temperature Changes on Reactivity for Various Coolants in a Liquid Salt Cooled Very High Temperature Reactor (LS-VHTR)

    International Nuclear Information System (INIS)

    Casino, William A. Jr.

    2006-01-01

    The purpose of this study is to perform an investigation into the relative merit of various salts and salt compounds being considered for use as coolants in the liquid salt cooled very high temperature reactor platform (LS-VHTR). Most of the non-nuclear properties necessary to evaluate these salts are known, but the neutronic characteristics important to reactor core design are still in need of a more extensive examination. This report provides a two-fold approach to further this investigation. First, a list of qualifying salts is assembled based upon acceptable non-nuclear properties. Second, the effect on system reactivity for a secondary system transient or an off-normal or accident condition is examined for each of these salt choices. The specific incident to be investigated is an increase in primary coolant temperature beyond normal operating parameters. In order to perform the relative merit comparison of each candidate salt, the System Temperature Coefficient of Reactivity is calculated for each candidate salt at various state points throughout the core burn history. (author)

  19. Small-angle x-ray scattering and density measurements of liquid Se50-Te50 mixture at high temperatures and high pressures using synchrotron radiation

    International Nuclear Information System (INIS)

    Kajihara, Y; Inui, M; Matsuda, K; Tomioka, Y

    2010-01-01

    We have carried out small-angle x-ray scattering and x-ray transmission measurements of liquid Se 50 -Te 50 mixture at SPring-8 in Japan and obtained the structure factor S(Q) at small-Q region (0.6 -1 ) and the density at high temperatures and high pressures up to 1000 0 C and 180 MPa. We report preliminary results in this paper. With increasing temperature, the density shows a minimum at around 500 0 C and a maximum at around 700 0 C. On the other hand, S(0) becomes maximum and S(Q) strongly depends on Q at around 600 0 C, which is about the middle temperature where the density shows the minimum and maximum. The temperatures shift to lower side when the pressure increases. These results prove that, with increasing temperature, the sample exhibits gradual transition from low-density structure to high-density structure, which causes mesoscopic density fluctuations in the intermediate temperature region.

  20. Purification Efficacy of Synthetic Cannabinoid Conjugates Using High-Pressure Liquid Chromatography

    Science.gov (United States)

    conducted using high-pressure liquid chromatography and gradient screens to determine the most effective means of purifying the SC:dark quencher conjugates...to obtain the highest yields and purity. The purity was verified using liquid chromatographycoupled mass spectroscopy and nuclear magnetic resonance.

  1. Supersymmetry at high temperatures

    International Nuclear Information System (INIS)

    Das, A.; Kaku, M.

    1978-01-01

    We investigate the properties of Green's functions in a spontaneously broken supersymmetric model at high temperatures. We show that, even at high temperatures, we do not get restoration of supersymmetry, at least in the one-loop approximation

  2. Prostate cell membrane chromatography-liquid chromatography-mass spectrometry for screening of active constituents from Uncaria rhynchophylla.

    Science.gov (United States)

    He, Jianyu; Han, Shengli; Yang, Fangfang; Zhou, Nan; Wang, Sicen

    2013-01-01

    Uncaria rhynchophylla is a traditional Chinese medicinal herb used to treat hypertension and convulsive disorders such as epilepsy. Rat prostate cell membrane chromatography combined with liquid chromatography-mass spectrometry (LC-MS) was used to identify active constituents from U. rhynchophylla extracts. Four compounds (corynoxeine, isorhynchophylline, isocorynoxeine and rhynchophylline) were discovered. Competitive binding assay results indicated that the four compounds were in direct competition at a single common binding site and interacted with α1A adrenergic receptors (α1A-AR) in a manner similar to tamsulosin. Affinity constant values of the four compounds binding with α1A-AR were also measured using rat prostate cell membrane chromatography (CMC). Finally, their pharmacodynamic effects were tested on rat caudal arteries. This CMC combined LC-MS system offers a means of drug discovery by screening natural medicinal herbs for new pharmacologically active molecules targeting specific receptors.

  3. Application of selected ion monitoring to the analysis of triacylglycerols in olive oil by high temperature-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Ruiz-Samblás, C; González-Casado, A; Cuadros-Rodríguez, L; García, F P Rodríguez

    2010-06-30

    The analysis of the triacylglycerol (TAG) composition of oils is a very challenging task, since the TAGs have very similar physico-chemical properties. In this work, a high temperature-gas chromatographic method coupled to electron ionization-mass spectrometry (HT-GC/EI-MS), in the Selected Ion Monitoring (SIM) mode, method was developed for the analysis of TAGs in the olive oil; this is a method suitable for routine analysis. This method was developed using commercially available standard TAGs. The TAGs studied were separated according to their equivalent carbon number and degree of unsaturation. The peak assignment was carried out by locating the characteristic fragment ions having the same retention time on the SIM profile such as [RCO+74](+) and [RCO+128](+) ions, due to the fatty acyl residues on sn-1, sn-2 and sn-3 positions of the TAG molecule and the [M-OCOR](+) ions corresponding to the acyl ions. The developed method was very useful to eliminate the interferences that appeared in the mass spectrum since electron ionization can prevent satisfactory interpretation of spectra. Copyright 2010 Elsevier B.V. All rights reserved.

  4. [Analysis of microalbuminuria with immunonephelometry and high performance liquid chromatography. Evaluation of new criteria].

    Science.gov (United States)

    Markó, Lajos; Molnár, Gergo Attila; Wagner, Zoltán; Koszegi, Tamás; Matus, Zoltán; Mohás, Márton; Kuzma, Mónika; Szijártó, István András; Wittmann, István

    2008-01-13

    Hypertension as well as type 2 diabetes mellitus is a major factor in population mortality. Both diseases damage the endothelium, the early sign of which is microalbuminuria, which can be screened by dipstick and can be diagnosed by using immuno-based and high performance liquid chromatography methods. Using high performance liquid chromatography, the non-immunoreactive albumin can be detected as well. The authors aimed at the examination of albuminuria in the case of immunonephelometrically negative patients with high performance liquid chromatography, in diabetic and hypertensive and non-diabetic hypertensive populations. The authors also wanted to compare the present (albumin-creatinine ratio: male: > or =2.5 mg/mmol, female: > or =3.5 mg/mmol) and a new criteria of the Heart Outcomes Prevention Evaluation study (patients without diabetes: immunological method, > or =0.7 mg/mmol; high performance liquid chromatography, > or =3.1 mg/mmol; individuals with diabetes: immunological method, > or =1.4 mg/mmol; high performance liquid chromatography, > or =5.2 mg/mmol) of microalbuminuria. Examination of fresh urines of 469 microalbuminuria negative patients by dipstick were performed by immunonephelometry. Patients, who were microalbuminuria negative by immunonephelometry as well, were further analyzed by high performance liquid chromatography using the Accumintrade mark Kit, based on size-exclusion chromatography. Three times higher albuminuria were found with high performance liquid chromatography than with immunonephelometry. The intraindividual coefficient of variation did not differ in the two methods (37 +/- 31% vs. 40 +/- 31%, p = 0.869; immunonephelometry vs. high performance liquid chromatography; mean +/- standard deviation). Using the present criteria for microalbuminuria, 43% of immunonephelometrically negative patients proved to be microalbuminuric by high performance liquid chromatography. Using the new criteria of the Heart Outcomes Prevention

  5. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Application of Ionic Liquids in High Performance Reversed-Phase Chromatography

    Directory of Open Access Journals (Sweden)

    Wentao Bi

    2009-06-01

    Full Text Available Ionic liquids, considered “green” chemicals, are widely used in many areas of analytical chemistry due to their unique properties. Recently, ionic liquids have been used as a kind of novel additive in separation and combined with silica to synthesize new stationary phase as separation media. This review will focus on the properties and mechanisms of ionic liquids and their potential applications as mobile phase modifier and surface-bonded stationary phase in reversed-phase high performance liquid chromatography (RP-HPLC. Ionic liquids demonstrate advantages and potential in chromatographic field.

  7. A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC).

    Science.gov (United States)

    Grosser, Katharina; van Dam, Nicole M

    2017-03-15

    Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil quality, food flavoring, and human health. The biological activity of glucosinolates is released upon tissue damage, when they are mixed with the enzyme myrosinase. This results in the formation of pungent and toxic breakdown products, such as isothiocyanates and nitriles. Currently, more than 130 structurally different glucosinolates have been identified. The chemical structure of the glucosinolate is an important determinant of the product that is formed, which in turn determines its biological activity. The latter may range from detrimental (e.g., progoitrin) to beneficial (e.g., glucoraphanin). Each glucosinolate-containing plant species has its own specific glucosinolate profile. For this reason, it is important to correctly identify and reliably quantify the different glucosinolates present in brassicaceous leaf, seed, and root crops or, for ecological studies, in their wild relatives. Here, we present a well-validated, targeted, and robust method to analyze glucosinolate profiles in a wide range of plant species and plant organs. Intact glucosinolates are extracted from ground plant materials with a methanol-water mixture at high temperatures to disable myrosinase activity. Thereafter, the resulting extract is brought onto an ion-exchange column for purification. After sulfatase treatment, the desulfoglucosinolates are eluted with water and the eluate is freeze-dried. The residue is taken up in an exact volume of water, which is analyzed by high-pressure liquid chromatography (HPLC) with a photodiode array (PDA) or ultraviolet (UV) detector. Detection and quantification are achieved by conducting comparisons of the retention times and UV spectra of commercial reference standards. The concentrations are calculated based on a sinigrin reference curve and well-established response factors. The advantages and

  8. Quantification of maltol in Korean ginseng (Panax ginseng) products by high-performance liquid chromatography-diode array detector

    Science.gov (United States)

    Jeong, Hyun Cheol; Hong, Hee-Do; Kim, Young-Chan; Rhee, Young Kyoung; Choi, Sang Yoon; Kim, Kyung-Tack; Kim, Sung Soo; Lee, Young-Chul; Cho, Chang-Won

    2015-01-01

    Background: Maltol, as a type of phenolic compounds, is produced by the browning reaction during the high-temperature treatment of ginseng. Thus, maltol can be used as a marker for the quality control of various ginseng products manufactured by high-temperature treatment including red ginseng. For the quantification of maltol in Korean ginseng products, an effective high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed. Materials and Methods: The HPLC-DAD method for maltol quantification coupled with a liquid-liquid extraction (LLE) method was developed and validated in terms of linearity, precision, and accuracy. An HPLC separation was performed on a C18 column. Results: The LLE methods and HPLC running conditions for maltol quantification were optimized. The calibration curve of the maltol exhibited good linearity (R2 = 1.00). The limit of detection value of maltol was 0.26 μg/mL, and the limit of quantification value was 0.79 μg/mL. The relative standard deviations (RSDs) of the data of the intra- and inter-day experiments were <1.27% and 0.61%, respectively. The results of the recovery test were 101.35–101.75% with an RSD value of 0.21–1.65%. The developed method was applied successfully to quantify the maltol in three ginseng products manufactured by different methods. Conclusion: The results of validation demonstrated that the proposed HPLC-DAD method was useful for the quantification of maltol in various ginseng products. PMID:26246746

  9. Quality evaluation of moluodan concentrated pill using high-performance liquid chromatography fingerprinting coupled with chemometrics.

    Science.gov (United States)

    Tao, Lingyan; Zhang, Qing; Wu, Yongjiang; Liu, Xuesong

    2016-12-01

    In this study, a fast and effective high-performance liquid chromatography method was developed to obtain a fingerprint chromatogram and quantitative analysis simultaneously of four indexes including gallic acid, chlorogenic acid, albiflorin and paeoniflorin of the traditional Chinese medicine Moluodan Concentrated Pill. The method was performed by using a Waters X-bridge C 18 reversed phase column on an Agilent 1200S high-performance liquid chromatography system coupled with diode array detection. The mobile phase of the high-performance liquid chromatography method was composed of 20 mmol/L phosphate solution and acetonitrile with a 1 mL/min eluent velocity, under a detection temperature of 30°C and a UV detection wavelength of 254 nm. After the methodology validation, 16 batches of Moluodan Concentrated Pill were analyzed by this high-performance liquid chromatography method and both qualitative and quantitative evaluation results were achieved by similarity analysis, principal component analysis and hierarchical cluster analysis. The results of these three chemometrics were in good agreement and all indicated that batch 10 and batch 16 showed significant differences with the other 14 batches. This suggested that the developed high-performance liquid chromatography method could be applied in the quality evaluation of Moluodan Concentrated Pill. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

    Science.gov (United States)

    Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

    2015-12-01

    Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  12. Performance comparison of three trypsin columns used in liquid chromatography?

    OpenAIRE

    ?lechtov?, Tereza; Gilar, Martin; Kal?kov?, Kv?ta; Moore, Stephanie M.; Jorgenson, James W.; Tesa?ov?, Eva

    2017-01-01

    Trypsin is the most widely used enzyme in proteomic research due to its high specificity. Although the in-solution digestion is predominantly used, it has several drawbacks, such as long digestion times, autolysis, and intolerance to high temperatures or organic solvents. To overcome these shortcomings trypsin was covalently immobilized on solid support and tested for its proteolytic activity. Trypsin was immobilized on bridge-ethyl hybrid silica sorbent with 300 ? pores, packed in 2.1 ? 30 m...

  13. High temperature investigation of the solid/liquid transition in the PuO2-UO2-ZrO2 system

    Science.gov (United States)

    Quaini, A.; Guéneau, C.; Gossé, S.; Sundman, B.; Manara, D.; Smith, A. L.; Bottomley, D.; Lajarge, P.; Ernstberger, M.; Hodaj, F.

    2015-12-01

    The solid/liquid transitions in the quaternary U-Pu-Zr-O system are of great interest for the analysis of core meltdown accidents in Pressurised Water Reactors (PWR) fuelled with uranium-dioxide and MOX. During a severe accident the Zr-based cladding can become completely oxidised due to the interaction with the oxide fuel and the water coolant. In this framework, the present analysis is focused on the pseudo-ternary system UO2-PuO2-ZrO2. The melting/solidification behaviour of five pseudo-ternary and one pseudo-binary ((PuO2)0.50(ZrO2)0.50) compositions have been investigated experimentally by a laser heating method under pre-set atmospheres. The effects of an oxidising or reducing atmosphere on the observed melting/freezing temperatures, as well as the amount of UO2 in the sample, have been clearly identified for the different compositions. The oxygen-to-metal ratio is a key parameter affecting the melting/freezing temperature because of incongruent vaporisation effects. In parallel, a detailed thermodynamic model for the UO2-PuO2-ZrO2 system has been developed using the CALPHAD method, and thermodynamic calculations have been performed to interpret the present laser heating results, as well as the high temperature behaviour of the cubic (Pu,U,Zr)O2±x-c mixed oxide phase. A good agreement was obtained between the calculated and experimental data points. This work enables an improved understanding of the major factors relevant to severe accident in nuclear reactors.

  14. High temperature investigation of the solid/liquid transition in the PuO{sub 2}–UO{sub 2}–ZrO{sub 2} system

    Energy Technology Data Exchange (ETDEWEB)

    Quaini, A. [CEA, DANS/DPC/SCCME/LM2T, Centre de Saclay, 91191 Gif-sur-Yvette Cedex (France); Guéneau, C., E-mail: christine.gueneau@cea.fr [CEA, DANS/DPC/SCCME/LM2T, Centre de Saclay, 91191 Gif-sur-Yvette Cedex (France); Gossé, S. [CEA, DANS/DPC/SCCME/LM2T, Centre de Saclay, 91191 Gif-sur-Yvette Cedex (France); Sundman, B. [INSTN, CEA Saclay (France); Manara, D.; Smith, A.L.; Bottomley, D.; Lajarge, P.; Ernstberger, M. [European Commission, Joint Research Centre, Institute for Transuranium Elements, P.O. Box 2340, 76125 Karlsruhe (Germany); Hodaj, F. [Univ. Grenoble Alpes, SIMAP, F-38000 Grenoble (France); CNRS, Grenoble INP, SIMAP, F-38000 Grenoble (France)

    2015-12-15

    The solid/liquid transitions in the quaternary U-Pu-Zr-O system are of great interest for the analysis of core meltdown accidents in Pressurised Water Reactors (PWR) fuelled with uranium-dioxide and MOX. During a severe accident the Zr-based cladding can become completely oxidised due to the interaction with the oxide fuel and the water coolant. In this framework, the present analysis is focused on the pseudo-ternary system UO{sub 2}–PuO{sub 2}–ZrO{sub 2}. The melting/solidification behaviour of five pseudo-ternary and one pseudo-binary ((PuO{sub 2}){sub 0.50}(ZrO{sub 2}){sub 0.50}) compositions have been investigated experimentally by a laser heating method under pre-set atmospheres. The effects of an oxidising or reducing atmosphere on the observed melting/freezing temperatures, as well as the amount of UO{sub 2} in the sample, have been clearly identified for the different compositions. The oxygen-to-metal ratio is a key parameter affecting the melting/freezing temperature because of incongruent vaporisation effects. In parallel, a detailed thermodynamic model for the UO{sub 2}–PuO{sub 2}–ZrO{sub 2} system has been developed using the CALPHAD method, and thermodynamic calculations have been performed to interpret the present laser heating results, as well as the high temperature behaviour of the cubic (Pu,U,Zr)O{sub 2±x}-c mixed oxide phase. A good agreement was obtained between the calculated and experimental data points. This work enables an improved understanding of the major factors relevant to severe accident in nuclear reactors.

  15. Recent advances in liquid and gas chromatography methodology for extending coverage of the metabolome.

    Science.gov (United States)

    Haggarty, Jennifer; Burgess, Karl Ev

    2017-02-01

    The metabolome is the complete complement of metabolites (small organic biomolecules). In order to comprehensively understand the effect of stimuli on a biological system, it is important to detect as many of the metabolites within that system as possible. This review briefly describes some new advances in liquid and gas chromatography to improve coverage of the metabolome, including the serial combination of two columns in tandem, column switching and different variations of two-dimensional chromatography. Supercritical fluid chromatography could provide complimentary data to liquid and gas chromatography. Although there have been many recent advancements in the field of metabolomics, it is evident that a combination, rather than a single method, is required to approach full coverage of the metabolome. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

  16. Application of liquid column chromatography to preconcentration, separation and determination of platinum metals

    International Nuclear Information System (INIS)

    Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

    1986-01-01

    Separation and determination of platimum metals using the methods of adsorption, ion-pair, ion-exchange, distributing and sieve chromatography are discussed in the review of literature in 1971-1984. Separation and determination of metals as chelates using the method of adsorption and ion-pair chromatograpy are noted to be most perspective directions of developing highly effective liquid chromatography of inorganic systems

  17. Immunoaffinity chromatography of abscisic acid combined with electrospray liquid chromatography–mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Hradecká, Veronika; Novák, Ondřej; Havlíček, Libor; Strnad, Miroslav

    2007-01-01

    Roč. 847, č. 2 (2007), s. 162-173 ISSN 1570-0232 R&D Projects: GA MŠk(CZ) LC06034; GA AV ČR IBS5038351 Institutional research plan: CEZ:AV0Z50380511 Source of funding: V - iné verejné zdroje ; V - iné verejné zdroje Keywords : abscisic acid * immunoaffinity chromatography * liquid chromatography-mass spectrometry Subject RIV: ED - Physiology Impact factor: 2.935, year: 2007

  18. Monodisperse microbeads of hypercrosslinked polystyrene for liquid and supercritical fluid chromatography

    Science.gov (United States)

    Tsyurupa, M. P.; Blinnikova, Z. K.; Il'in, M. M.; Davankov, V. A.; Parenago, O. O.; Pokrovskii, O. I.; Usovich, O. I.

    2015-11-01

    Monodisperse styrene-divinylbenzene (1 wt %) copolymer microbeads are obtained via the elaborate method of high-productivity precipitation polymerization. The crosslinking of this copolymer with chloromethyl methyl ether in the presence of Friedel-Crafts catalyst yields porous hypercrosslinked polymers with degrees of crosslinking that range from 200 to 500%. Microbead sorbents are shown to be suited for selective stationary phases for high-performance liquid chromatography and supercritical fluid chromatography.

  19. Improved method for the determination of the cortisol production rate using high-performance liquid chromatography and liquid scintillation counting

    NARCIS (Netherlands)

    van Ingen, H. E.; Endert, E.

    1988-01-01

    Two new methods for the determination of the cortisol production rate using reversed-phase high-performance liquid chromatography are described. One uses ultraviolet detection at 205 nm, the other on-line post-column derivatization with benzamidine, followed by fluorimetric detection. The specific

  20. Characterization of natural organic colorants in historical and art objects by high-performance liquid chromatography.

    Science.gov (United States)

    Pauk, Volodymyr; Barták, Petr; Lemr, Karel

    2014-12-01

    High-performance liquid chromatography plays an important role in analysis of historical organic colorants. A number of papers have been published in this field over the last 30 years. Classification of the most commonly used natural dyes and an overview of high-performance liquid chromatography methods with main focus on recent works (2008 to the beginning of 2014) are provided. The review deals with an entire analytical protocol covering sample preparation, chromatographic separation, and suitable detection (UV/visible and fluorescent spectroscopy and mass spectrometric techniques). High-performance liquid chromatography has been successfully used in the complete characterization of some organic dyestuffs present in historical and art objects. The possibilities and difficulties for identification of natural sources of historical colorants are also discussed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Screening and quantitative determination of twelve acidic and neutral pharmaceuticals in whole blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Steentoft, Anni; Buck, Maike

    2010-01-01

    . The method was fully validated for salicylic acid, paracetamol, phenobarbital, carisoprodol, meprobamate, topiramate, etodolac, chlorzoxazone, furosemide, ibuprofen, warfarin, and salicylamide. The method also tentatively includes thiopental, theophylline, piroxicam, naproxen, diclophenac, and modafinil......We describe a multi-method for simultaneous identification and quantification of 12 acidic and neutral compounds in whole blood. The method involves a simple liquid-liquid extraction, and the identification and quantification are performed using liquid chromatography-tandem mass spectrometry...

  2. Crosslinked polymeric ionic liquids as solid-phase microextraction sorbent coatings for high performance liquid chromatography.

    Science.gov (United States)

    Yu, Honglian; Merib, Josias; Anderson, Jared L

    2016-03-18

    Neat crosslinked polymeric ionic liquid (PIL) sorbent coatings for solid-phase microextraction (SPME) compatible with high-performance liquid chromatography (HPLC) are reported for the first time. Six structurally different PILs were crosslinked to nitinol supports and applied for the determination of select pharmaceutical drugs, phenolics, and insecticides. Sampling conditions including sample solution pH, extraction time, desorption solvent, desorption time, and desorption solvent volume were optimized using design of experiment (DOE). The developed PIL sorbent coatings were stable when performing extractions under acidic pH and remained intact in various organic desorption solvents (i.e., methanol, acetonitrile, acetone). The PIL-based sorbent coating polymerized from the IL monomer 1-vinyl-3-(10-hydroxydecyl) imidazolium chloride [VC10OHIM][Cl] and IL crosslinker 1,12-di(3-vinylbenzylimidazolium) dodecane dichloride [(VBIM)2C12] 2[Cl] exhibited superior extraction performance compared to the other studied PILs. The extraction efficiency of pharmaceutical drugs and phenolics increased when the film thickness of the PIL-based sorbent coating was increased while many insecticides were largely unaffected. Satisfactory analytical performance was obtained with limits of detection (LODs) ranging from 0.2 to 2 μg L(-1) for the target analytes. The accuracy of the analytical method was examined by studying the relative recovery of analytes in real water samples, including tap water and lake water, with recoveries varying from 50.2% to 115.9% and from 48.8% to 116.6%, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. High-performance liquid chromatography of oligoguanylates at high pH

    Science.gov (United States)

    Stribling, R.; Deamer, D. (Principal Investigator)

    1991-01-01

    Because of the stable self-structures formed by oligomers of guanosine, standard high-performance liquid chromatography techniques for oligonucleotide fractionation are not applicable. Previously, oligoguanylate separations have been carried out at pH 12 using RPC-5 as the packing material. While RPC-5 provides excellent separations, there are several limitations, including the lack of a commercially available source. This report describes a new anion-exchange high-performance liquid chromatography method using HEMA-IEC BIO Q, which successfully separates different forms of the guanosine monomer as well as longer oligoguanylates. The reproducibility and stability at high pH suggests a versatile role for this material.

  4. Glucose and glycerol concentrations and their tracer enrichment measurements using liquid chromatography tandem mass spectrometry

    DEFF Research Database (Denmark)

    Bornø, Andreas; Foged, Lene; van Hall, Gerrit

    2014-01-01

    The present study describes a new liquid chromatography tandem mass spectrometry method for high-throughput quantification of glucose and glycerol in human plasma using stable isotopically labeled internal standards and is suitable for simultaneous measurements of glucose and glycerol enrichments...... of variation were 2.0% and 9.7%, respectively. After derivatization, plasma samples were stable for at least 14 days. In conclusion, we have developed and validated a novel, accurate, and sensitive high-throughput liquid chromatography tandem mass spectrometry method for simultaneous determination of glucose...

  5. A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

    Science.gov (United States)

    Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

    2016-02-01

    It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Bacterial Cell Wall Precursor Phosphatase Assays Using Thin-layer Chromatography (TLC) and High Pressure Liquid Chromatography (HPLC).

    Science.gov (United States)

    Pazos, Manuel; Otten, Christian; Vollmer, Waldemar

    2018-03-20

    Peptidoglycan encases the bacterial cytoplasmic membrane to protect the cell from lysis due to the turgor. The final steps of peptidoglycan synthesis require a membrane-anchored substrate called lipid II, in which the peptidoglycan subunit is linked to the carrier lipid undecaprenol via a pyrophosphate moiety. Lipid II is the target of glycopeptide antibiotics and several antimicrobial peptides, and is degraded by 'attacking' enzymes involved in bacterial competition to induce lysis. Here we describe two protocols using thin-layer chromatography (TLC) and high pressure liquid chromatography (HPLC), respectively, to assay the digestion of lipid II by phosphatases such as Colicin M or the LXG toxin protein TelC from Streptococcus intermedius . The TLC method can also monitor the digestion of undecaprenyl (pyro)phosphate, whereas the HPLC method allows to separate the di-, mono- or unphosphorylated disaccharide pentapeptide products of lipid II.

  7. Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

    Science.gov (United States)

    Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

    2017-11-24

    Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

  8. Liquid chromatography tandem mass spectrometry determination of total budesonide levels in dog plasma after inhalation exposure.

    Science.gov (United States)

    Berg, Seija; Melamies, Marika; Rajamäki, Minna; Vainio, Outi; Peltonen, Kimmo

    2012-01-01

    A sensitive and selective method to quantify budesonide in dog plasma samples was developed and fully validated. Liquid-liquid extraction was followed by solid-phase extraction and liquid chromatography-tandem mass spectrometry with electrospray ionization. After reconstitution of the analytes in the mobile phase, samples were analysed by reversed-phase liquid chromatography with isocratic elution. d8-Budesonide was used as an internal standard, and characteristic transitions of d8-budesonide and budesonide were used for quantification. The method was validated with respect to selectivity, specificity, linearity, recovery, repeatability, reproducibility and limits of detection and quantification. The validated method was successfully applied to monitor the plasma levels of budesonide in dogs exposed to clinical doses of inhaled and intravenous drug.

  9. Determination of five antiarrhythmic drugs in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Jouyban, Abolghasem; Sorouraddin, Mohammad Hossein; Farajzadeh, Mir Ali; Somi, Mohammad Hossein; Fazeli-Bakhtiyari, Rana

    2015-03-01

    A fast and sensitive high-performance liquid chromatography (HPLC) method with ultraviolet (UV) detection was developed and validated for the simultaneous quantitation of five antiarrhythmic drugs (metoprolol, propranolol, carvedilol, diltiazem, and verapamil) in human plasma samples. It involves dispersive liquid-liquid microextraction (DLLME) of the desired drugs from 660 µL plasma and separation using isocratic elution with UV detection at 200 nm. The complete separation of all analytes was achieved within 7 min. Acetonitrile (as disperser solvent) resulting from the protein precipitation procedure was mixed with 100 µL dichloromethane (as an extraction solvent) and rapidly injected into 5 mL aqueous solution (pH 11.5) containing 1% (w/v), NaCl. After centrifugation, the sedimented phase containing enriched analytes was collected and evaporated to dryness. The residue was re-dissolved in 50 µL de-ionized water (acidified to pH 3) and injected into the HPLC system for analysis. Under the optimal conditions, the enrichment factors and extraction recoveries ranged between 4.4-10.8 and 33-82%, respectively. The suggested method was linear (r(2) ≥0.997) over a dynamic range of 0.02-0.80 µg mL(-1) in plasma. The intra- and inter-days relative standard deviation (RSD%) and relative error (RE%) values of the method were below 20%, which shows good precision and accuracy. Finally, this method was applied to the analysis of real plasma samples obtained from the patients treated with these drugs. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Analysis of drugs of abuse in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Fernández, P; Regenjo, M; Bermejo, A M; Fernández, A M; Lorenzo, R A; Carro, A M

    2015-04-01

    Opioids and cocaine are widely used at present, both for recreational purposes and as drugs of abuse. This raises the need to develop new analytical methods specifically designed for the simultaneous detection of several drugs of abuse in biological samples. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a new sample treatment for the simultaneous extraction of morphine (MOR), 6-acetylmorphine (6AM), cocaine (COC), benzoylecgonine (BZE) and methadone (MET) from human plasma. Preliminary assays were done before developing an experimental design based on a Uniform Network Doehlert which allowed the optimum extraction conditions to be identified, namely: a volume of extractant solvent (chloroform) and dispersant solvent (acetonitrile) of 220 µl and 3.2 ml, respectively; 0.2 g of NaCl as a salting-out additive; pH 10.6 and ultrasound stirring for 3.5 min. The resulting extracts were analyzed by high-performance liquid chromatography with photodiode array detection (HPLC-PDA), using an XBridge® RP18 column (250 × 4.6 mm i.d., 5 µm particle size). Calibration graphs were linear over the concentration range 0.1-10 µg ml⁻¹, and detection limits ranged from 13.9 to 28.5 ng ml⁻¹. Precision calculated at three different concentration levels in plasma was included in the range 0.1-6.8% RSD. Recoveries of the five drugs were all higher than 84% on average. Finally the proposed method was successfully applied to 22 plasma samples from heroin, cocaine and/or methadone users, and the most frequently detected drug was benzoylecgonine, followed by methadone, cocaine and morphine. Copyright © 2014 John Wiley & Sons, Ltd.

  11. Determination of statin drugs in hospital effluent with dispersive liquid-liquid microextraction and quantification by liquid chromatography.

    Science.gov (United States)

    Martins, Ayrton F; Frank, Carla da S; Altissimo, Joseline; de Oliveira, Júlia A; da Silva, Daiane S; Reichert, Jaqueline F; Souza, Darliana M

    2017-08-24

    Statins are classified as being amongst the most prescribed agents for treating hypercholesterolaemia and preventing vascular diseases. In this study, a rapid and effective liquid chromatography method, assisted by diode array detection, was designed and validated for the simultaneous quantification of atorvastatin (ATO) and simvastatin (SIM) in hospital effluent samples. The solid phase extraction (SPE) of the analytes was optimized regarding sorbent material and pH, and the dispersive liquid-liquid microextraction (DLLME), in terms of pH, ionic strength, type and volume of extractor/dispersor solvents. The performance of both extraction procedures was evaluated in terms of linearity, quantification limits, accuracy (recovery %), precision and matrix effects for each analyte. The methods proved to be linear in the concentration range considered; the quantification limits were 0.45 µg L -1 for ATO and 0.75 µg L -1 for SIM; the matrix effect was almost absent in both methods and the average recoveries remained between 81.5-90.0%; and the RSD values were <20%. The validated methods were applied to the quantification of the statins in real samples of hospital effluent; the concentrations ranged from 18.8 µg L -1 to 35.3 µg L -1 for ATO, and from 30.3 µg L -1 to 38.5 µg L -1 for SIM. Since the calculated risk quotient was ≤192, the occurrence of ATO and SIM in hospital effluent poses a potential serious risk to human health and the aquatic ecosystem.

  12. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    Science.gov (United States)

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  14. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  15. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

  16. High-performance liquid chromatography of human glycoprotein hormones.

    Science.gov (United States)

    Chlenov, M A; Kandyba, E I; Nagornaya, L V; Orlova, I L; Volgin, Y V

    1993-02-12

    The chromatographic behavior of the glycoprotein hormones from human pituitary glands and of placental origin [thyroid-stimulating hormone, luteinizing hormone and chorionic gonadotropin (CG)] was studied. It was shown that hydrophobic interaction chromatography on a microparticulate packing and anion-exchange HPLC can be applied for the purification of these hormones. Reversed-phase HPLC on wide-pore C4-bonded silica at neutral pH can be applied for the determination of the above hormones and for the isolation of pure CG and its subunits.

  17. Separation of hemagglutination-inhibiting immunoglobulin M antibody to rubella virus in human serum by high-performance liquid chromatography.

    OpenAIRE

    Kobayashi, N; Suzuki, M; Nakagawa, T; Matumoto, M

    1986-01-01

    High-performance liquid chromatography was successfully used to separate hemagglutination-inhibiting immunoglobulin M (IgM) rubella virus antibody from IgG rubella virus antibody in human serum. The fractionation by high-performance liquid chromatography was as effective as sucrose density gradient centrifugation in separating IgM antibody from IgG antibody.

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

    Science.gov (United States)

    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...

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

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Steven [Iowa State Univ., Ames, IA (United States)

    1999-02-12

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

  20. Equations of viscous flow of silicate liquids with different approaches for universality of high temperature viscosity limit

    Directory of Open Access Journals (Sweden)

    Ana F. Kozmidis-Petrović

    2014-06-01

    Full Text Available The Vogel-Fulcher-Tammann (VFT, Avramov and Milchev (AM as well as Mauro, Yue, Ellison, Gupta and Allan (MYEGA functions of viscous flow are analysed when the compositionally independent high temperature viscosity limit is introduced instead of the compositionally dependent parameter η∞ . Two different approaches are adopted. In the first approach, it is assumed that each model should have its own (average high-temperature viscosity parameter η∞ . In that case, η∞ is different for each of these three models. In the second approach, it is assumed that the high-temperature viscosity is a truly universal value, independent of the model. In this case, the parameter η∞ would be the same and would have the same value: log η∞ = −1.93 dPa·s for all three models. 3D diagrams can successfully predict the difference in behaviour of viscous functions when average or universal high temperature limit is applied in calculations. The values of the AM functions depend, to a greater extent, on whether the average or the universal value for η∞ is used which is not the case with the VFT model. Our tests and values of standard error of estimate (SEE show that there are no general rules whether the average or universal high temperature viscosity limit should be applied to get the best agreement with the experimental functions.

  1. Resolution of RNA using high-performance liquid chromatography

    NARCIS (Netherlands)

    Mclaughlin, L.W.; Bischoff, Rainer

    1987-01-01

    High-performance liquid chromatographic techniques can be very effective for the resolution and isolation of nucleic acids. The characteristic ionic (phosphodiesters) and hydrophobic (nucleobases) properties of RNAs can be exploited for their separation. In this respect anion-exchange and

  2. Buffer-Free High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a simple, economical and reproducible high performance liquid chromatographic (HPLC) method for the determination of theophylline in pharmaceutical dosage forms. Method: Caffeine was used as the internal standard and reversed phase C-18 column was used to elute the drug and ...

  3. Determination of ribavirin in human serum using liquid chromatography tandem mass spectrometry

    NARCIS (Netherlands)

    van der Lijke, H.; Alffenaar, J.-W. C.; Kok, W.Th.; Greijdanus, B.; Uges, D.R.A.

    2012-01-01

    A method has been developed for the determination of ribavirin in human serum for therapeutic drug monitoring purposes, using liquid chromatography electrospray ionization mass spectrometry. Separation was obtained with a mobile phase gradient starting and ending in 100% aqueous conditions using a

  4. Determination of low molecular weight thiols using monobromobimane fluorescent labeling and high-performance liquid chromatography

    Science.gov (United States)

    Fahey, Robert C.; Newton, Gerald L.

    1988-01-01

    Methods are described for the preparation and high-performance liquid chromatography (HPLC) analysis of monobromobimane derivatives of low molecular weight thiols in extracts of biological samples. Typical problems encountered in the development and application of these methods are discussed. Analysis of mung bean extract is used as an example.

  5. Sugar Determination in Foods with a Radially Compressed High Performance Liquid Chromatography Column.

    Science.gov (United States)

    Ondrus, Martin G.; And Others

    1983-01-01

    Advocates use of Waters Associates Radial Compression Separation System for high performance liquid chromatography. Discusses instrumentation and reagents, outlining procedure for analyzing various foods and discussing typical student data. Points out potential problems due to impurities and pump seal life. Suggests use of ribose as internal…

  6. Determination of Peroxide-Based Explosives Using Liquid Chromatography with On-Line Infrared Detection

    NARCIS (Netherlands)

    Schulte-Ladbeck, Rasmus; Edelmann, Andrea; Quintas, Guillermo; Lendl, Bernhard; Karst, U.

    2006-01-01

    A nondestructive analytical method for peroxide-based explosives determination in solid samples is described. Reversed-phase high-performance liquid chromatography in combination with on-line Fourier transform infrared (FT-IR) detection is used for the analysis of triacetonetriperoxide (TATP) and

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

    NARCIS (Netherlands)

    Coulier, L.; Bas, R.; Jespersen, S.; Verheij, E.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    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,

  8. High-Performance Liquid Chromatography in the Undergraduate Chemical Engineering Laboratory

    Science.gov (United States)

    Frey, Douglas D.; Guo, Hui; Karnik, Nikhila

    2013-01-01

    This article describes the assembly of a simple, low-cost, high-performance liquid chromatography (HPLC) system and its use in the undergraduate chemical engineering laboratory course to perform simple experiments. By interpreting the results from these experiments students are able to gain significant experience in the general method of…

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

    DEFF Research Database (Denmark)

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

    1997-01-01

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

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

    NARCIS (Netherlands)

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

    2007-01-01

    Poor repeatability of peak areas is a problem frequently encountered in peptide analysis with nanoLiquid Chromatography coupled on-line with Mass Spectrometry (nanoLC-MS). As a result, quantitative analysis will be seriously hampered unless the observed variability can be corrected in some way.

  11. Serum Protein Profile Study of Clinical Samples Using High Performance Liquid Chromatography-Laser Induced Fluorescence

    DEFF Research Database (Denmark)

    Karemore, Gopal Raghunath; Ukendt, Sujatha; Rai, Lavanya

    2009-01-01

    The serum protein profiles of normal subjects, patients diagnosed with cervical cancer, and oral cancer were recorded using High Performance Liquid Chromatography combined with Laser Induced Fluorescence detection (HPLC-LIF). Serum protein profiles of the above three classes were tested for estab...

  12. Nitrate and nitrite content in bottled beverages by ion-pair high-performance liquid chromatography.

    Science.gov (United States)

    Song, Yang; Deng, Gui-Fang; Xu, Xiang-Rong; Chen, Yong-Hong; Chen, Feng; Li, Hua-Bin

    2013-01-01

    Nitrate and nitrite levels in six types of beverages--total of 292 individual samples from 73 brands (four bottles each)--from Guangzhou city in China were evaluated by ion-pair high-performance liquid chromatography. All samples contained nitrate. Nitrate and nitrite ranges were 0.43-46.08 and safety of Chinese bottled beverages.

  13. DETERMINATION OF CHLOROPHEONIS, NITROPHENOIS AND METHYLPHENOIS IN GROUND-WATER SAMPLES USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Science.gov (United States)

    A high performance liquid chromatography (HPLC) method was developed to quantitatively determine phenolic compounds and their isomers in aqueous samples. The HPLC method can analyze a mixture of 15 contaminants in the same analytical run with an analysis time of 25 minutes. The...

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

    Science.gov (United States)

    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…

  15. DETERMINATION OF CHLOROPHENOLS, NITROPHENOLS, AND METHYLPHENOLS IN GROUND-WATER SAMPLES USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Science.gov (United States)

    A high performance liquid chromatography (HPLC) method was developed to quantitatively determine phenolic compounds and their isomers in aqueous samples. The HPLC method can analyze a mixture of 15 contaminants in the same analytical run with an analysis time of 25 minutes. The...

  16. Coupling nanoliter high-performance liquid chromatography to inductively coupled plasma mass spectrometry for arsenic speciation.

    Science.gov (United States)

    Cheng, Heyong; Shen, Lihuan; Liu, Jinhua; Xu, Zigang; Wang, Yuanchao

    2018-04-01

    Nanoliter high-performance liquid chromatography shows low consumption of solvents and samples, offering one of the best choices for arsenic speciation in precious samples in combination with inuctively coupled plasma mass spectrometry. A systematic investigation on coupling nanoliter high-performance liquid chromatography to inductively coupled plasma mass spectrometry from instrument design to injected sample volume and mobile phase was performed in this study. Nanoflow mobile phase was delivered by flow splitting using a conventional high-pressure pump with reuse of mobile phase waste. Dead volume was minimized to 60 nL for the sheathless interface based on the previously developed nanonebulizer. Capillary columns for nanoliter high-performance liquid chromatography were found to be sensitive to sample loading volume. An apparent difference was also found between the mobile phases for nanoliter and conventional high-performance liquid chromatography. Baseline separation of arsenite, arsenate, monomethylarsenic, and dimethylarsenic was achieved within 11 min on a 15 cm C 18 capillary column and within 12 min on a 25 cm strong anion exchange column. Detection limits of 0.9-1.8 μg/L were obtained with precisions variable in the range of 1.6-4.2%. A good agreement between determined and certified values of a certified reference material of human urine (GBW 09115) validated its accuracy along with good recoveries (87-102%). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Simultaneous determination of seven flavonoids in Epimedium by liquid chromatography-tandem mass spectrometry method

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Bao Lin Guo; Yu Xin Sheng; Jin Lan Zhang

    2008-01-01

    In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2"-0-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.

  18. High-performance liquid chromatography determination of dapsone, monoacetyldapsone, and pyrimethamine in filter paper blood spots

    DEFF Research Database (Denmark)

    Rønn, A M; Lemnge, M M; Angelo, H R

    1995-01-01

    A high-performance liquid chromatography method for the simultaneous analysis of dapsone (DDS), the major metabolite of DDS, monoacetyldapsone (MADDS), and pyrimethamine (PYR) was modified for capillary blood samples obtained by finger prick and dried on filter paper. Limit of quantitation using...

  19. Alternative sample-introduction technique to avoid breakthrough in gradient-elution liquid chromatography of polymers

    NARCIS (Netherlands)

    Reingruber, E.; Bedani, F.; Buchberger, W.; Schoenmakers, P.

    2010-01-01

    Gradient-elution liquid chromatography (GELC) is a powerful tool for the characterization of synthetic polymers. However, gradient-elution chromatograms often suffer from breakthrough phenomena. Breakthrough can be averted by using a sample solvent as weak as the mobile phase. However, this approach

  20. Determination of organophosphorus acids by thermo-spray liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Wils, E.R.J.; Hulst, A.G.

    1988-01-01

    The determination of thirteen organophosphorus acids, hydrolysis products of nerve agents and pesticides, by a combination of ion-pair liquid chromatography on a reversed-phase C18 column and thermospray mass spectrometry was investigated. Ammonium acetate and three tetraalkylammonium salts with

  1. Novel approach to determine ghrelin analogs by liquid chromatography with mass spectrometry using a monolithic column

    Czech Academy of Sciences Publication Activity Database

    Zemenová, Jana; Sýkora, D.; Adámková, H.; Maletínská, Lenka; Elbert, Tomáš; Marek, Aleš; Blechová, Miroslava

    2017-01-01

    Roč. 40, č. 5 (2017), s. 1032-1039 ISSN 1615-9306 Institutional support: RVO:61388963 Keywords : enzyme-linked immunosorbent assay * ghrelin * lipopeptides * liquid chromatography mass spectrometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 2.557, year: 2016

  2. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography

    NARCIS (Netherlands)

    Uliyanchenko, E.; van der Wal, S.; Schoenmakers, P.J.

    2011-01-01

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles

  3. Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Lee, Iris; Boyce, Mary C.

    2011-01-01

    A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

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

    Science.gov (United States)

    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)

  5. Characterization of typical chemical background interferences in atmospheric pressure ionization liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Guo, Xinghua; Bruins, Andries P.; Covey, Thomas R.

    2006-01-01

    The structures and origins of typical chemical background noise ions in positive atmospheric pressure ionization liquid chromatography/mass spectrometry (API LC/MS) are investigated and summarized in this study. This was done by classifying chemical background ions using precursor and product ion

  6. An Advanced, Interactive, High-Performance Liquid Chromatography Simulator and Instructor Resources

    Science.gov (United States)

    Boswell, Paul G.; Stoll, Dwight R.; Carr, Peter W.; Nagel, Megan L.; Vitha, Mark F.; Mabbott, Gary A.

    2013-01-01

    High-performance liquid chromatography (HPLC) simulation software has long been recognized as an effective educational tool, yet many of the existing HPLC simulators are either too expensive, outdated, or lack many important features necessary to make them widely useful for educational purposes. Here, a free, open-source HPLC simulator is…

  7. Simulated Moving Bed Chromatography: Separation and Recovery of Sugars and Ionic Liquid from Biomass Hydrolysates

    Science.gov (United States)

    Caes, Benjamin R.; Van Oosbree, Thomas R.; Lu, Fachuang; Ralph, John; Maravelias, Christos T.

    2015-01-01

    Simulated moving bed chromatography, a continuous separation method, enables the nearly quantitative recovery of sugar products and ionic liquid solvent from chemical hydrolysates of biomass. The ensuing sugars support microbial growth, and the residual lignin from the process is intact. PMID:23939991

  8. Determination of chlormequat in pears by liquid chromatography/mass spectrometry

    NARCIS (Netherlands)

    Mol, H.G.J.; Dam, R.C.J. van; Vreeken, R.J.; Steijger, O.M.

    2000-01-01

    A straightforward and reliable method was developed for the determination of chlormequat in pears by liquid chromatography/mass spectrometry (LC/MS). Water and methanol were compared as extraction solvents. Because no significant differences in extraction efficiency or repeatability were found,

  9. Assay of free urinary cortisol with inverted phase liquid chromatography and radiocompetition

    International Nuclear Information System (INIS)

    Franck, C.; Patricot, M.C.; Mathian, B.; Revol, A.

    1984-01-01

    The authors present an assay method for free urinary cortisol using inverted phase liquid chromatography for purification and radiocompetition for the assay. The usual values for adult men and women were established. The results of 150 routine assays were compared with those of 17 OHCS revealing the value of this assay [fr

  10. Analysis of 2-methylthio-derivatives of isoprenoid cytokinins by liquid chromatography-tandem mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Tarkowski, Petr; Václavíková, Kateřina; Novák, Ondřej; Pertry, I.; Hanuš, Jan; Whenham, R.; Vereecke, D.; Šebela, M.; Strnad, Miroslav

    2010-01-01

    Roč. 680, 1-2 (2010), s. 86-91 ISSN 0003-2670 R&D Projects: GA ČR GA301/08/1649 Institutional research plan: CEZ:AV0Z50380511 Keywords : Cytokinins * Rhodococcus fascians * High-performance liquid chromatography Subject RIV: CE - Biochemistry Impact factor: 4.310, year: 2010

  11. Monoliths in capillary electrochromatography and capillary liquid chromatography in conjunction with mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Rantamäki, A. H.; Duša, Filip; Wiedmer, S. K.

    2016-01-01

    Roč. 37, 7-8 (2016), s. 880-912 ISSN 0173-0835 Institutional support: RVO:68081715 Keywords : capillary electrochromatography * capillary liquid chromatography * mass spec- trometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.744, year: 2016

  12. Separation and quantification of ropinirole and some impurities using capillary liquid chromatography

    NARCIS (Netherlands)

    Coufal, P.; Stulik, K.; Claessens, H.A.; Hardy, M.J.; Webb, M.

    1999-01-01

    Ropinirole, 4-[2-(dipropylamino)ethyl]-1,3-dihydro-2H-indol-2-one, is a potent anti-Parkinson’s disease drug developed by SmithKline Beecham Pharmaceuticals. Capillary liquid chromatography (CLC) was used for the separation and quantification of ropinirole and its five related impurities,

  13. An on-line high performance liquid chromatography-crocin bleaching assay for detection of antioxidants

    NARCIS (Netherlands)

    Bountagkidou, O.; Klift, van der E.J.C.; Tsimidou, M.Z.; Ordoudi, S.A.; Beek, van T.A.

    2012-01-01

    An on-line HPLC (high performance liquid chromatography) method for the rapid screening of individual antioxidants in mixtures was developed using crocin as a substrate (i.e. oxidation probe) and 2,2'-azobis(2-amidinopropane dihydrochloride (AAPH)) in phosphate buffer (pH 7.5) as a radical

  14. Separation of Poly(styrene-block-t-butyl methacrylate) Copolymers by Various Liquid Chromatography Techniques

    Science.gov (United States)

    Šmigovec Ljubič, Tina; Pahovnik, David; Žigon, Majda; Žagar, Ema

    2012-01-01

    The separation of a mixture of three poly(styrene-block-t-butyl methacrylate) copolymers (PS-b-PtBMA), consisting of polystyrene (PS) blocks of similar length and t-butyl methacrylate (PtBMA) blocks of different lengths, was performed using various chromatographic techniques, that is, a gradient liquid chromatography on reversed-phase (C18 and C8) and normal-phase columns, a liquid chromatography under critical conditions for polystyrene as well as a fully automated two-dimensional liquid chromatography that separates block copolymers by chemical composition in the first dimension and by molar mass in the second dimension. The results show that a partial separation of the mixture of PS-b-PtBMA copolymers can be achieved only by gradient liquid chromatography on reversed-phase columns. The coelution of the two block copolymers is ascribed to a much shorter PtBMA block length, compared to the PS block, as well as a small difference in the length of the PtBMA block in two of these copolymers, which was confirmed by SEC-MALS and NMR spectroscopy. PMID:22489207

  15. Column liquid chromatography- mass spectrometry: selected techniques in environmental applications for polar pesticides and related compounds.

    NARCIS (Netherlands)

    Slobodnik, J.; van Baar, B.L.M.; Brinkman, U.A.T.

    1995-01-01

    A review covering the field of environmental applications of liquid chromatography-mass spectrometry (LC-MS) is presented. Recent developments and advances are discussed with emphasis on the presently popular thermospray, particle beam and atmospheric pressure ionisation interfaces. Each interface

  16. Characterization of goat colostrum oligosaccharides by nano-liquid chromatography on chip quadrupole time-of-flight mass spectrometry and hydrophilic interaction liquid chromatography-quadrupole mass spectrometry.

    Science.gov (United States)

    Martín-Ortiz, A; Salcedo, J; Barile, D; Bunyatratchata, A; Moreno, F J; Martin-García, I; Clemente, A; Sanz, M L; Ruiz-Matute, A I

    2016-01-08

    A detailed qualitative and quantitative characterization of goat colostrum oligosaccharides (GCO) has been carried out for the first time. Defatted and deproteinized colostrum samples, previously treated by size exclusion chromatography (SEC) to remove lactose, were analyzed by nanoflow liquid chromatography-quadrupole-time of flight mass spectrometry (Nano-LC-Chip-Q-TOF MS). Up to 78 oligosaccharides containing hexose, hexosamine, fucose, N-acetylneuraminic acid or N-glycolylneuraminic acid monomeric units were identified in the samples, some of them detected for the first time in goat colostra. As a second step, a hydrophilic interaction liquid chromatography coupled to mass spectrometry (HILIC-MS) methodology was developed for the separation and quantitation of the main GCO, both acidic and neutral carbohydrates. Among other experimental chromatographic conditions, mobile phase additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry of target carbohydrates. Narrow peaks (wh: 0.2-0.6min) and good symmetry (As: 0.8-1.4) were obtained for GCO using an acetonitrile:water gradient with 0.1% ammonium hydroxide at 40°C. These conditions were selected to quantify the main oligosaccharides in goat colostrum samples. Values ranging from 140 to 315mgL(-1) for neutral oligosaccharides and from 83 to 251mgL(-1) for acidic oligosaccharides were found. The combination of both techniques resulted to be useful to achieve a comprehensive characterization of GCO. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Separation of carbohydrates using hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Fu, Qing; Liang, Tu; Li, Zhenyu; Xu, Xiaoyong; Ke, Yanxiong; Jin, Yu; Liang, Xinmiao

    2013-09-20

    A strategy was developed to rapidly evaluate chromatographic properties of hydrophilic interaction chromatography (HILIC) columns for separating carbohydrates. Seven HILIC columns (Silica, Diol, TSK Amide-80, XAmide, Click Maltose, Click β-CD, and Click TE-Cys columns) were evaluated by using three monosaccharide and seven disaccharides as probes. The influence of column temperature on the peak shape and tautomerization of carbohydrates, as well as column selectivity were investigated. The influence of surface charge property on the retention was also studied by using glucose, glucuronic acid, and glucosamine, which indicated that buffer salt concentration and pH value in mobile phase was necessary to control the ionic interactions between ionic carbohydrates and HILIC columns. According to evaluation results, the XAmide column was selected as an example to establish experimental schemes for separation of complex mixtures of oligosaccharide. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. High temperature battery. Hochtemperaturbatterie

    Energy Technology Data Exchange (ETDEWEB)

    Bulling, M.

    1992-06-04

    To prevent heat losses of a high temperature battery, it is proposed to make the incoming current leads in the area of their penetration through the double-walled insulating housing as thermal throttle, particularly spiral ones.

  19. High temperature refrigerator

    International Nuclear Information System (INIS)

    Steyert, W.A. Jr.

    1978-01-01

    A high temperature magnetic refrigerator is described which uses a Stirling-like cycle in which rotating magnetic working material is heated in zero field and adiabatically magnetized, cooled in high field, then adiabatically demagnetized. During this cycle the working material is in heat exchange with a pumped fluid which absorbs heat from a low temperature heat source and deposits heat in a high temperature reservoir. The magnetic refrigeration cycle operates at an efficiency 70% of Carnot

  20. Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

    Science.gov (United States)

    Baghdady, Yehia Z; Schug, Kevin A

    2016-01-01

    Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids

    DEFF Research Database (Denmark)

    Lue, Bena-Marie; Guo, Zheng; Xu, X.B.

    2008-01-01

    Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found...... essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method...

  2. Ionic liquid-based air-assisted liquid-liquid microextraction followed by high performance liquid chromatography for the determination of five fungicides in juice samples.

    Science.gov (United States)

    You, Xiangwei; Chen, Xiaochu; Liu, Fengmao; Hou, Fan; Li, Yiqiang

    2018-01-15

    A novel and simple ionic liquid-based air-assisted liquid-liquid microextraction technique combined with high performance liquid chromatography was developed to analyze five fungicides in juice samples. In this method, ionic liquid was used instead of a volatile organic solvent as the extraction solvent. The emulsion was formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent repeatedly using a 10mL glass syringe. No organic dispersive solvent was required. Under the optimized conditions, the limits of detection (LODs) were 0.4-1.8μgL -1 at a signal-to-noise ratio of 3. The limits of quantification (LOQs) set as the lowest spiking levels with acceptable recovery in juices were 10μgL -1 , except for fludioxonil whose LOQ was 20μgL -1 . The proposed method was applied to determine the target fungicides in juice samples, and acceptable recoveries ranging from 74.9% to 115.4% were achieved. Copyright © 2017. Published by Elsevier Ltd.

  3. High-temperature Brillouin scattering study of haplogranitic glasses and liquids: Effects of F, K, Na and Li on Tg and elastic properties

    Science.gov (United States)

    Manghnani, M. H.; Hushur, A.; Williams, Q. C.; Dingwell, D. B.

    2010-12-01

    The density, compressibility and viscosity of silicate melts are important in understanding the thermodynamic and fluid dynamic properties of magmatic systems. Knowledge of the compressibility of silicate melts at 1 bar is an important component in the construction of accurate pressure-volume-temperature equations of state. In light of this, the velocity (nVp, Vp, Vs) and refractive index n of four anhydrous haplogranitic glasses and liquids with similar alkali abundances, but different cations, are measured at high temperature by Brillouin scattering spectroscopy through the glass transition temperature (Tg) in both platelet and back scattering geometry. The compositions of four haplogranites are 5 wt% of the components Li2O, Na2O, K2O and F each added to a base of haplogranitic (HPG8) composition. The glass transition temperature Tg of different haplogranite samples at the GHz frequency of the Brillouin probe are determined from the change in slope of the temperature-dependent longitudinal or transverse sound velocity. HPG8-Li5 has the lowest glass transition temperature (466°C), while HPG8-K5 has the highest glass transition temperature (575°C). Our Brillouin results, when compared with DSC measurements, show lower Tg values. This raises the possibility of a role of either heating rates or a frequency dependence of the glass transition in explaining the discrepancies in Tg values derived from the two methods. The sound velocity (nVp, Vp, Vs) shows markedly different temperature dependences (including differences in sign) below Tg depending on their different alkali contents. The unrelaxed elastic moduli of three haplogranitic glasses with added Li2O, Na2O and F components have been obtained as a function of temperature. The unrelaxed bulk modulus, shear modulus and Poisson’s ratio show strong compositional dependences at ambient temperature. On heating, The K initially decreases with increasing temperature up to ~ 135°C, then increases up to Tg, and then

  4. Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Pia Sala

    2015-04-01

    Full Text Available A novel liquid chromatography-mass spectrometry (LC-MS approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI coupled to hydrophilic interaction liquid chromatography (HILIC was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID fragment spectra in a linear ion trap. The process of chromatography development showed the best separation properties with a silica-based Kinetex column. This type of chromatography was able to separate all major lipid classes expected in mammalian samples, yielding increased sensitivity of oxidized phosphatidylcholines over reversed phase chromatography. Identification of molecular species was achieved by exact mass on intact molecular ions and CID tandem mass spectra containing characteristic fragments. Due to a lack of commercially available standards, method development was performed with copper induced oxidation products of palmitoyl-arachidonoyl-phosphatidylcholine, which resulted in a plethora of lipid species oxidized at the arachidonoyl moiety. Validation of the method was done with copper oxidized human low-density lipoprotein (LDL prepared by ultracentrifugation. In these LDL samples we could identify 46 oxidized molecular phosphatidylcholine species out of 99 possible candidates.

  5. Two-Dimensional Liquid Chromatography Analysis of Polystyrene/Polybutadiene Block Copolymers.

    Science.gov (United States)

    Lee, Sanghoon; Choi, Heejae; Chang, Taihyun; Staal, Bastiaan

    2018-05-15

    A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (Styrolux) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene- block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition, and chain architecture. While individual LC analysis, including size exclusion chromatography, interaction chromatography, or liquid chromatography at critical condition, is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homopolystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

  6. The determination of antipyrine elimination in saliva by liquid chromatography.

    Science.gov (United States)

    Gartzke, J; Jäger, H

    1991-01-01

    A simple, fast and reliable liquid chromatographic method for the determination of antipyrine in saliva is described. The elimination of antipyrine is a good indicator for general evaluation of the liver function for dispositional purposes for example in occupational and environmental medicine. The described LC method was compared with a more extensive photometric procedure. The results obtained from both methods show very good correlation. Only one measurement is necessary to determine the antipyrine clearance. Furthermore the antipyrine dosage can be minimized, because of the sensitivity of the HPLC-method.

  7. Simultaneous determination of seven anticoagulant rodenticides in agricultural products by gel permeation chromatography and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saito-Shida, Shizuka; Nemoto, Satoru; Matsuda, Rieko; Akiyama, Hiroshi

    2016-11-01

    A sensitive and reliable method for the simultaneous determination of hydroxycoumarin-type (brodifacoum, bromadiolone, coumatetralyl, and warfarin) and indandione-type (chlorophacinone, diphacinone, and pindone) rodenticides in agricultural products by gel permeation chromatography (GPC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The procedure involved extraction of the rodenticides from samples with acetone, followed by liquid-liquid partitioning with hexane/ethyl acetate (1:1, v/v) and 10% sodium chloride aqueous solution, then cleanup using GPC, and finally, analysis using LC-MS/MS. High recoveries from the GPC column were obtained for all rodenticides tested using a mobile phase of acetone/cyclohexane/triethylamine (400:1600:1, v/v/v). An ODS column, which contains low levels of metal impurities, gave satisfactory peak shapes for both hydroxycoumarin- and indandione-type rodenticides in the LC-MS/MS separation. The average recoveries of rodenticides from eight agricultural foods (apple, eggplant, cabbage, orange, potato, tomato, brown rice, and soybean) fortified at 0.0005-0.001 mg/kg ranged from 76 to 116%, except for bromadiolone in orange (53%) and diphacinone in soybean (54%), and the relative standard deviations ranged from 1 to 16%. The proposed method effectively removed interfering components, such as pigments and lipids, and showed high selectivity. In addition, the matrix effects were negligible for most of the rodenticide/food combinations. The results suggest that the proposed method is reliable and suitable for determining hydroxycoumarin- and indandione-type rodenticides in agricultural products.

  8. Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

    Science.gov (United States)

    Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

    2017-12-29

    Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Combined high-performance liquid chromatography/32P-postlabeling assay of N7-methyldeoxyguanosine

    International Nuclear Information System (INIS)

    Shields, P.G.; Povey, A.C.; Wilson, V.L.; Weston, A.; Harris, C.C.

    1990-01-01

    A highly sensitive and specific assay for the detection of N7-methyl-2'-deoxyguanosine (N7methyldG) has been developed by combining high-performance liquid chromatography, 32 P-postlabeling, and nucleotide chromatography. Separation of normal nucleotides and adducts by high-performance liquid chromatography and then combining a portion of 2'-deoxyguanosine to the N7methyldG allows for quantitation using an internal standard. The directly determined molar ratio is not subject to errors in digestion, variable ATP-specific activity, or assumptions in relative adduct-labeling efficiency. The detection limit was one N7methyldG adduct in 10(7) unmodified 2'-deoxyguanosine bases. N7methyldG adducts have been detected in 5 human lung samples in which O6-methyl-2'-deoxyguanosine adducts had been previously determined. The mean ratio of N7methyldG to O6-methyl-2'-deoxyguanosine was determined to be approximately 10. The current assay complements the high-performance liquid chromatography/ 32 P-postlabeling assay for O6-methyl-2'-deoxyguanosine and increases the detection sensitivity of DNA methylated by exogenous alkylating agents

  10. Liquid chromatography-tandem mass spectrometric assay for the tyrosine kinase inhibitor afatinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Sparidans, Rolf W; van Hoppe, Stephanie; Rood, Johannes J M; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H

    2016-01-01

    A quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay for afatinib, an irreversible inhibitor of the ErbB (erythroblastic leukemia viral oncogene homolog) tyrosine kinase family, was developed and validated. Plasma samples were pre-treated using salting-out

  11. Sensitive determination of nitrophenol isomers by reverse-phase high-performance liquid chromatography in conjunction with liquid-liquid extraction

    Science.gov (United States)

    A method for the highly sensitive determination of 2-, 3- and 4- nitrophenols was developed using reverse-phase high-performance liquid chromatography (RP-HPLC) with a UV photodiode array detector. Using a reverse-phase column and 40% aqueous acetonitrile as an eluent (i.e. isocratic elution), the i...

  12. [Blood levels of homocysteine by high pressure liquid chromatography and comparison with two other techniques].

    Science.gov (United States)

    Ceppa, F; Drouillard, I; Chianea, D; Burnat, P; Perrier, F; Vaillant, C; El Jahiri, Y

    1999-01-01

    Cardio-vascular diseases are the most common cause of death in industrialized countries. A new marker has emerged among offending risk factors in the past few years: homocysteine. This sulphured amino-acid is an important intermediate in transsulphuration and remethylation reactions of methionine's metabolism. We proposed to evaluate a home made method of determination for this parameter by high performance liquid chromatography (HPLC) and to compare it to fluorescence polarization immunoassay technique (FPIA) and to gaz phase chromatography (CG-SM). This method associated with good sensibility and precision remain much less expensive than FPIA technique.

  13. Characterization of Extracellular Vesicles by Size-Exclusion High-Performance Liquid Chromatography (HPLC).

    Science.gov (United States)

    Huang, Tao; He, Jiang

    2017-01-01

    Extracellular vesicles (EVs) have recently attracted substantial attention due to the potential diagnostic and therapeutic relevance. Although a variety of techniques have been used to isolate and analyze EVs, it is still far away from satisfaction. Size-exclusion chromatography (SEC), which separates subjects by size, has been widely applied in protein purification and analysis. The purpose of this chapter is to show the applications of size-exclusion high-performance liquid chromatography (HPLC) as methods for EV characterization of impurities or contaminants of small size, and thus for quality assay for the purity of the samples of EVs.

  14. Nanoparticle Analysis by Online Comprehensive Two-Dimensional Liquid Chromatography combining Hydrodynamic Chromatography and Size-Exclusion Chromatography with Intermediate Sample Transformation

    Science.gov (United States)

    2017-01-01

    Polymeric nanoparticles have become indispensable in modern society with a wide array of applications ranging from waterborne coatings to drug-carrier-delivery systems. While a large range of techniques exist to determine a multitude of properties of these particles, relating physicochemical properties of the particle to the chemical structure of the intrinsic polymers is still challenging. A novel, highly orthogonal separation system based on comprehensive two-dimensional liquid chromatography (LC × LC) has been developed. The system combines hydrodynamic chromatography (HDC) in the first-dimension to separate the particles based on their size, with ultrahigh-performance size-exclusion chromatography (SEC) in the second dimension to separate the constituting polymer molecules according to their hydrodynamic radius for each of 80 to 100 separated fractions. A chip-based mixer is incorporated to transform the sample by dissolving the separated nanoparticles from the first-dimension online in tetrahydrofuran. The polymer bands are then focused using stationary-phase-assisted modulation to enhance sensitivity, and the water from the first-dimension eluent is largely eliminated to allow interaction-free SEC. Using the developed system, the combined two-dimensional distribution of the particle-size and the molecular-size of a mixture of various polystyrene (PS) and polyacrylate (PACR) nanoparticles has been obtained within 60 min. PMID:28745485

  15. Determination of pyrazinamide in human by high performance liquid chromatography.

    Directory of Open Access Journals (Sweden)

    Revankar S

    1994-01-01

    Full Text Available A facile and sensitive high performance liquid chromatographic (HPLC technique has been developed for the determination pyrazinamide (PZA in human plasma. Nicotinamide(NIA is used as internal standard(IS. Plasma is deproteinized with 0.7 M perchloric acid; clear supernatant is neutralized with 1M NaOH and injected onto HPLC. The separation of pyrazinamide and the internal standard is carried out on a Supelco LC-18 (DB column with a basic mobile phase. Pyrazinoic acid, the major metabolite, other anti-tuberculous drugs and endogenous components do not interfere with measurement of pyrazinamide. The limit of detection of pyrazinamide with this method is 0.2 mg/0.2 ml plasma (CV 8.2%.

  16. Microwave-assisted ionic liquid homogeneous liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of anthraquinones in Rheum palmatum L.

    Science.gov (United States)

    Wang, Zhibing; Hu, Jianxue; Du, Hongxia; He, Shuang; Li, Qing; Zhang, Hanqi

    2016-06-05

    The microwave-assisted ionic liquid homogeneous liquid-liquid microextraction (MA-IL-HLLME) coupled with high performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of anthraquinones, including aloe-emodin, emodin, chrysophanol and physcion in root of Rheum palmatum L. Several experimental parameters influencing the extraction efficiency, including amount of sample, type and volume of ionic liquid, volume and pH value of extraction medium, microwave power and extraction time, concentration of NH4PF6 as well as centrifugal condition were optimized. When 140μL of ionic liquid ([C8MIM][BF4]) was used as an extraction solvent, target analytes can be extracted from sample matrix in one minute with the help of microwave irradiation. The MA-IL-HLLME is simple and quick. The calibration curves exhibited good linear relationship (r>0.9984). The limits of detection and quantification were in the range of 0.015-0.026 and 0.051-0.088μgmL(-1), respectively. The spiked recovery for each analyte was in the range of 81.13-93.07% with relative standard deviations lower than 6.89%. The present method is free of volatile organic solvents, and represents lower expenditures of sample, extraction time and solvent, compared with ultrasonic and heat reflux extraction. The results indicated that the present method can be successfully applied to the determination of anthraquinones in medicinal plant. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Development and evaluation of a liquid chromatography tandem mass spectrometry method for simultaneous determination of salivary melatonin, cortisol and testosterone

    DEFF Research Database (Denmark)

    Jensen, Marie Aarrebo; Hansen, Åse Marie; Abrahamsson, Peter

    2011-01-01

    saliva. We used liquid-liquid extraction (LLE) followed by liquid chromatography coupled to electrospray tandem mass spectrometry (LC-ESI-MS/MS) recorded in positive ion mode. Saliva samples were collected by spitting directly into tubes and 250 µL were used for analysis. The limits of detection were 4...

  18. [Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography- reversed-phase liquid chromatography].

    Science.gov (United States)

    Jia, Youmei; Cai, Jianfeng; Xin, Huaxia; Feng, Jiatao; Fu, Yanhui; Fu, Qing; Jin, Yu

    2017-06-08

    A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography (Pre-2D-HILIC/RPLC) method was established to separate and purify the components in Trachelospermum jasminoides . The pigments and strongly polar components were removed from the crude extract after the active carbon decolorization and solid phase extraction processes. A Click XIon column (250 mm×20 mm, 10 μm) was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC. Finally, 15 fractions were collected under UV-triggered mode. In the second dimensional RPLC, a C18 column (250 mm×20 mm, 5 μm) was selected and water-acetonitrile was used as mobile phases. As a result, 14 compounds with high purity were obtained, which were further identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). Finally, 11 lignan compounds and three flavonoid compounds were obtained. The method has a good orthogonality, and can improve the resolution and the peak capacity. It is significant for the separation of complex components from Trachelospermum jasminoides .

  19. Chemical fingerprint of Ganmaoling granule by double-wavelength ultra high performance liquid chromatography and ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Lou, Qiong; Ye, Xiaolan; Zhou, Yingyi; Li, Hua; Song, Fenyun

    2015-06-01

    A method incorporating double-wavelength ultra high performance liquid chromatography with quadrupole time-of-flight mass spectrometry was developed for the investigation of the chemical fingerprint of Ganmaoling granule. The chromatographic separations were performed on an ACQUITY UPLC HSS C18 column (2.1 × 50 mm, 1.8 μm) at 30°C using gradient elution with water/formic acid (1%) and acetonitrile at a flow rate of 0.4 mL/min. A total of 11 chemical constituents of Ganmaoling granule were identified from their molecular weight, UV spectra, tandem mass spectrometry data, and retention behavior by comparing the results with those of the reference standards or literature. And 25 peaks were selected as the common peaks for fingerprint analysis to evaluate the similarities among 25 batches of Ganmaoling granule. The results of principal component analysis and orthogonal projection to latent structures discriminant analysis showed that the important chemical markers that could distinguish the different batches were revealed as 4,5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4-O-caffeoylquinic acid. This is the first report of the ultra high performance liquid chromatography chemical fingerprint and component identification of Ganmaoling granule, which could lay a foundation for further studies of Ganmaoling granule. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry

    Science.gov (United States)

    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: alachlor ethanesulfonic acid (ESA); alachlor oxanilic acid; acetochlor ESA; acetochlor oxanilic acid; metolachlor ESA; and metolachlor oxanilic acid. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The average HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.5 and 2.0 ??g/l ranged from 84 to 112%, with relative standard deviations of 18% or less. The average HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.2 and 2.0 ??g/l ranged from 81 to 118%, with relative standard deviations of 20% or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 ??g/l, whereas the LOQ using the HPLC/MS method was at 0.05 ??g/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. Copyright (C) 2000 Elsevier Science B.V.

  1. Analyses of Indole Compounds in Sugar Cane (Saccharum officinarum L. Juice by High Performance Liquid Chromatography and Liquid Chromatography-Mass Spectrometry after Solid-Phase Extraction

    Directory of Open Access Journals (Sweden)

    Jean Wan Hong Yong

    2017-03-01

    Full Text Available Simultaneous quantitative analysis of 10 indole compounds, including indole-3-acetic acid (IAA, one of the most important naturally occurring auxins and some of its metabolites, by high performance liquid chromatography (HPLC and liquid chromatography-mass spectrometry (LC-MS after solid-phase extraction (SPE was reported for the first time. The analysis was carried out using a reverse phase HPLC gradient elution, with an aqueous mobile phase (containing 0.1% formic acid modified by methanol. Furthermore, a novel SPE procedure was developed for the pre-concentration and purification of indole compounds using C18 SPE cartridges. The combination of SPE, HPLC, and LC-MS was applied to screen for the indole compounds present in sugar cane (Saccharum officinarum L. juice, a refreshing beverage with various health benefits. Finally, four indole compounds were successfully detected and quantified in sugar cane juice by HPLC, which were further unequivocally confirmed by LC-MS/MS experiments operating in the multiple reaction monitoring (MRM mode.

  2. On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

    Science.gov (United States)

    Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

    2015-03-27

    A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Low-level flow counting of liquid chromatography column eluates

    International Nuclear Information System (INIS)

    Harding, N.G.L.; Farid, Y.; Stewart, M.J.

    1982-01-01

    The principal parameters which determine the operation of a high-resolution, high-sensitivity radioactive flow monitor are described: a) Sample preparation to ensure adequate recovery of radiolabelled sample, metabolites and internal standard. b) The instrument background count rate, when no sample or radiolabel is present in the flow cell, is a function of shielding and a reduction in noise obtained with a coincidence time below one microsecond. c) The minimum detectable amount of label depends upon the machine background, HPLC eluent and scintillator flow, whether or not packed flow cells are used, flow cell geometry, and the scintillator used. d) Three types of flow cell have been designed to cover the majority of HPLC and isotope applications. e) The performance of solid and liquid scintillators. It is shown that an instrument has been designed taking account of these parameters. The resulting design satisfies present high sensitivity counting requirements and maintains the resolution of current HPLC procedures when detection is by simultaneous flow radioassay and by optical methods. (orig.)

  4. Determination of Finasteride in Tablets by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    K. Basavaiah

    2007-01-01

    Full Text Available A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS in bulk drug and in tablets. FNS was eluted from a ODS C18 reversed phase column at laboratory temperature (30 ± 2°C with a mobile phase consisting of methanol and water (80+20 at a flow rate of 1 mL min-1 with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1 with limits of detection (LOD and quantification (LOQ being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

  5. Hyphenated and comprehensive liquid chromatography × gas chromatography-mass spectrometry for the identification of Mycobacterium tuberculosis.

    Science.gov (United States)

    Mourão, Marta P B; Denekamp, Ilse; Kuijper, Sjoukje; Kolk, Arend H J; Janssen, Hans-Gerd

    2016-03-25

    Tuberculosis is one of the world's most emerging public health problems, particularly in developing countries. Chromatography based methods have been used to tackle this epidemic by focusing on biomarker detection. Unfortunately, interferences from lipids in the sputum matrix, particularly cholesterol, adversely affect the identification and detection of the marker compounds. The present contribution describes the serial combination of normal phase liquid chromatography (NPLC) with thermally assisted hydrolysis and methylation followed by gas chromatography-mass spectrometry (THM-GC-MS) to overcome the difficulties of biomarker evaluation. The in-series combination consists of an LC analysis where fractions are collected and then transferred to the THM-GC-MS system. This was either done with comprehensive coupling, transferring all the fractions, or with hyphenated interfacing, i.e. off-line multi heart-cutting, transferring only selected fractions. Owing to the high sensitivity and selectivity of LC as a sample pre-treatment method, and to the high specificity of the MS as a detector, this analytical approach, NPLC × THM-GC-MS, is extremely sensitive. The results obtained indicate that this analytical set-up is able to detect down to 1 × 10(3) mycobacteria/mL of Mycobacterium tuberculosis strain 124, spiked in blank sputum samples. It is a powerful analytical tool and also has great potential for full automation. If further studies demonstrate its usefulness when applied blind in real sputum specimens, this technique could compete with the current smear microscopy in the early diagnosis of tuberculosis. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Column liquid chromatography applied to concentrating, separating, and determining platinum metals

    International Nuclear Information System (INIS)

    Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

    1986-01-01

    The present survey deals with high-performance liquid chromatography (HPLC) in relation to the chromatographic behavior of the platinum metals, including separation and determination. The data shows that HPLC is the most promising and effective method of separating metals, including platinum ones. The method provides efficient separation of microgram amoounts of mixtures with a resolving power 3-20 times that of thin-layer chromatography. It is shown that the most promising line of advance in HPLC for inorganic systems lies in the separation and determination of metals as chelates by absorption or ion-pair chromatography. Examples of using HPLC for determining noble metals in particular cases indicate that the metrological characteristics are favorable

  7. Determination of oxyfluorfen herbicide and oxyfluorfen amine residues in garbanzo beans by liquid chromatography.

    Science.gov (United States)

    Zhou, M; Miles, C J

    1991-01-01

    Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.

  8. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses.

    Science.gov (United States)

    Muthukrishnan, Suriyavathana; Palanisamy, Subha; Subramanian, Senthilkumar; Selvaraj, Sumathi; Mari, Kavitha Rani; Kuppulingam, Ramalingam

    2016-08-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. The HPLC analysis of ELEV showed the presence of gallic and caffeic acids as the major components at concentrations of 2.0 ppm and 0.1 ppm, respectively, as well as other components. GC-MS analysis revealed the presence of 3-eicosyne; 3,7,11,15-tetramethyl-2-hexadecen-1-ol; butanoic acid, 3-methyl-3,7-dimethyl-6-octenyl ester; phytol; 1,2-benzenedicarboxylic acid, diundecyl ester; 1-octanol, 2-butyl-; squalene; and 2H-pyran, 2-(7-heptadecynyloxy) tetrahydro-derivative. Because pharmacopuncture is a new evolving natural mode that uses herbal extracts for treating patients with various ailments with minimum pain and maximum effect, the results of this study are particularly important and show that ELEV possesses a wide range of phytochemical constituents, as indicated above, as effective active principle molecules that can be used individually or in combination to treat patients with various diseases. Copyright © 2016. Published by Elsevier B.V.

  9. Gas chromatography-mass spectrometry and high-performance liquid chromatography-diode array detection for dating of paper ink.

    Science.gov (United States)

    Díaz-Santana, Oscar; Vega-Moreno, Daura; Conde-Hardisson, Francisco

    2017-09-15

    An extraction and determination method is shown for the analysis of dyes and solvents present in two types of ballpoint pen inks that are deposited onto paper. Ink extracts are analysed using a combination of gas chromatography with mass spectrometry (GC-MS), and high-pressure liquid chromatography with photodiode array detection (HPLC-DAD), within a single sample extraction procedure. Seventeen solvents and thirteen dyes contained in two Montblanc ® inks (black and blue) were monitored for 45 months at monthly intervals, in order to determine variations in the concentrations of the compounds over time. We also studied the relative variations between different compounds and the generation of degradation products such as phenol. The concentration data obtained from these compounds during their exposure have been analysed and a multiple regression model is developed for each ink type that allows an estimate of the exposure time of the ink on paper with a maximum error of between 4 and 7 months. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Pressurized planar electrochromatography, high-performance thin-layer chromatography and high-performance liquid chromatography--comparison of performance.

    Science.gov (United States)

    Płocharz, Paweł; Klimek-Turek, Anna; Dzido, Tadeusz H

    2010-07-16

    Kinetic performance, measured by plate height, of High-Performance Thin-Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Pressurized Planar Electrochromatography (PPEC) was compared for the systems with adsorbent of the HPTLC RP18W plate from Merck as the stationary phase and the mobile phase composed of acetonitrile and buffer solution. The HPLC column was packed with the adsorbent, which was scrapped from the chromatographic plate mentioned. An additional HPLC column was also packed with adsorbent of 5 microm particle diameter, C18 type silica based (LiChrosorb RP-18 from Merck). The dependence of plate height of both HPLC and PPEC separating systems on flow velocity of the mobile phase and on migration distance of the mobile phase in TLC system was presented applying test solute (prednisolone succinate). The highest performance, amongst systems investigated, was obtained for the PPEC system. The separation efficiency of the systems investigated in the paper was additionally confirmed by the separation of test component mixture composed of six hormones. 2010 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. [Structural characterization of Astragalus polysaccharides using partial acid hydrolysis-hydrophilic interaction liquid chromatography-mass spectrometry].

    Science.gov (United States)

    Liang, Tu; Fu, Qing; Xin, Huaxia; Li, Fangbing; Jin, Yu; Liang, Xinmiao

    2014-12-01

    Water-soluble polysaccharides from traditional Chinese medicine (TCM) have properties of broad-spectrum treatment and low toxicity, making them as important components in natural medicines and health products. In order to solve the problem of polysaccharides characterization caused by their complex structures, a "bottom-up" approach was developed to complete the characterization of polysaccharides from Astragalus. Firstly, Astragalus pieces were extracted with hot water and then were precipitated by ethanol to obtain Astragalus polysaccharides. Secondly, a partial acid hydrolysis method was carried out and the effects of time, acid concentration and temperature on hydrolysis were investigated. The degree of hydrolysis increased along with the increase of hydrolysis time and acid concentration. The temperature played a great role in the hydrolysis process. No hydrolysis of the polysaccharides occurred at low temperature, while the polysaccharides were almost hydrolyzed to monosaccharide at high temperature. Under the optimum hydrolysis conditions (4 h, 1.5 mol/L trifluoroacetic acid, and 80 °C), Astragalus polysaccharides were hydrolyzed to characteristic oligosaccharide fragments. At last, a hydrophilic liquid chromatography-mass spectrometry method was used for the separation and structural characterization of the polysaccharide hydrolysates. The results showed that the resulting polysaccharides were mainly 1--> 4 linear glucan, and gluco-oligosaccharides with the degrees of polymerization (DP) of 4 - 11 were obtained after partial acid hydrolysis. The significance of this study is that it is the guidance for the characterization of other TCM polysaccharides.

  13. Concentration determination of urinary metabolites of N,N-dimethylacetamide by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Yamamoto, Shinobu; Matsumoto, Akiko; Yui, Yuko; Miyazaki, Shota; Kumagai, Shinji; Hori, Hajime; Ichiba, Masayoshi

    2018-03-27

    N,N-Dimethylacetamide (DMAC) is widely used in industry as a solvent. It can be absorbed through human skin. Therefore, it is necessary to determine exposure to DMAC via biological monitoring. However, the precision of traditional gas chromatography (GC) is low due to the thermal decomposition of metabolites in the high-temperature GC injection port. To overcome this problem, we have developed a new method for the simultaneous separation and quantification of urinary DMAC metabolites using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Urine samples were diluted 10-fold in formic acid, and 1-μl aliquots were injected into the LC-MS/MS equipment. A C18 reverse-phase Octa Decyl Silyl (ODS) column was used as the analytical column, and the mobile phase consisted of a mixture of methanol and aqueous formic acid solution. Urinary concentrations of DMAC and its known metabolites (N-hydroxymethyl-N-methylacetamide (DMAC-OH), N-methylacetamide (NMAC), and S- (acetamidomethyl) mercapturic acid (AMMA) ) were determined in a single run. The dynamic ranges of the calibration curves were 0.05-5 mg/l (r≥0.999) for all four compounds. The limits of detection for DMAC, DMAC-OH, NMAC, and AMMA in urine were 0.04, 0.02, 0.05, and 0.02 mg/l, respectively. Within-run accuracies were 96.5%-109.6% with relative standard deviations of precision being 3.43%-10.31%. The results demonstrated that the proposed method could successfully quantify low concentrations of DMAC and its metabolites with high precision. Hence, this method is useful for evaluating DMAC exposure. In addition, this method can be used to examine metabolite behaviors in human bodies after exposure and to select appropriate biomarkers.

  14. Concentration determination of urinary metabolites of N,N-dimethylacetamide by high-performance liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    Yamamoto, Shinobu; Matsumoto, Akiko; Yui, Yuko; Miyazaki, Shota; Kumagai, Shinji; Hori, Hajime; Ichiba, Masayoshi

    2017-01-01

    Objectives: N,N-Dimethylacetamide (DMAC) is widely used in industry as a solvent. It can be absorbed through human skin. Therefore, it is necessary to determine exposure to DMAC via biological monitoring. However, the precision of traditional gas chromatography (GC) is low due to the thermal decomposition of metabolites in the high-temperature GC injection port. To overcome this problem, we have developed a new method for the simultaneous separation and quantification of urinary DMAC metabolites using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods: Urine samples were diluted 10-fold in formic acid, and 1-μl aliquots were injected into the LC-MS/MS equipment. A C18 reverse-phase Octa Decyl Silyl (ODS) column was used as the analytical column, and the mobile phase consisted of a mixture of methanol and aqueous formic acid solution. Results: Urinary concentrations of DMAC and its known metabolites (N-hydroxymethyl-N-methylacetamide (DMAC-OH), N-methylacetamide (NMAC), and S- (acetamidomethyl) mercapturic acid (AMMA) ) were determined in a single run. The dynamic ranges of the calibration curves were 0.05-5 mg/l (r≥0.999) for all four compounds. The limits of detection for DMAC, DMAC-OH, NMAC, and AMMA in urine were 0.04, 0.02, 0.05, and 0.02 mg/l, respectively. Within-run accuracies were 96.5%-109.6% with relative standard deviations of precision being 3.43%-10.31%. Conclusions: The results demonstrated that the proposed method could successfully quantify low concentrations of DMAC and its metabolites with high precision. Hence, this method is useful for evaluating DMAC exposure. In addition, this method can be used to examine metabolite behaviors in human bodies after exposure and to select appropriate biomarkers. PMID:29213009

  15. High temperature niobium alloys

    International Nuclear Information System (INIS)

    Wojcik, C.C.

    1991-01-01

    Niobium alloys are currently being used in various high temperature applications such as rocket propulsion, turbine engines and lighting systems. This paper presents an overview of the various commercial niobium alloys, including basic manufacturing processes, properties and applications. Current activities for new applications include powder metallurgy, coating development and fabrication of advanced porous structures for lithium cooled heat pipes

  16. High temperature storage loop :

    Energy Technology Data Exchange (ETDEWEB)

    Gill, David Dennis; Kolb, William J.

    2013-07-01

    A three year plan for thermal energy storage (TES) research was created at Sandia National Laboratories in the spring of 2012. This plan included a strategic goal of providing test capability for Sandia and for the nation in which to evaluate high temperature storage (>650ÀC) technology. The plan was to scope, design, and build a flow loop that would be compatible with a multitude of high temperature heat transfer/storage fluids. The High Temperature Storage Loop (HTSL) would be reconfigurable so that it was useful for not only storage testing, but also for high temperature receiver testing and high efficiency power cycle testing as well. In that way, HTSL was part of a much larger strategy for Sandia to provide a research and testing platform that would be integral for the evaluation of individual technologies funded under the SunShot program. DOEs SunShot program seeks to reduce the price of solar technologies to 6/kWhr to be cost competitive with carbon-based fuels. The HTSL project sought to provide evaluation capability for these SunShot supported technologies. This report includes the scoping, design, and budgetary costing aspects of this effort

  17. High Temperature Electrolysis

    DEFF Research Database (Denmark)

    Elder, Rachael; Cumming, Denis; Mogensen, Mogens Bjerg

    2015-01-01

    High temperature electrolysis of carbon dioxide, or co-electrolysis of carbon dioxide and steam, has a great potential for carbon dioxide utilisation. A solid oxide electrolysis cell (SOEC), operating between 500 and 900. °C, is used to reduce carbon dioxide to carbon monoxide. If steam is also i...

  18. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    Science.gov (United States)

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Current practice of liquid chromatography-mass spectrometry in metabolomics and metabonomics.

    Science.gov (United States)

    Gika, Helen G; Theodoridis, Georgios A; Plumb, Robert S; Wilson, Ian D

    2014-01-01

    Based on publication and citation numbers liquid chromatography (LC-MS) has become the major analytical technology in the field of global metabolite profiling. This dominance reflects significant investments from both the research community and instrument manufacturers. Here an overview of the approaches taken for LC-MS-based metabolomics research is given, describing critical steps in the realisation of such studies: study design and its needs, specific technological problems to be addressed and major obstacles in data treatment and biomarker identification. The current state of the art for LC-MS-based analysis in metabonomics/metabolomics is described including recent developments in liquid chromatography, mass spectrometry and data treatment as these are applied in metabolomics underlining the challenges, limitations and prospects for metabolomics research. Examples of the application of metabolite profiling in the life sciences focusing on disease biomarker discovery are highlighted. In addition, new developments and future prospects are described. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Molecular differences between deuterated and protonated polystyrenes using reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Kayillo, Sindy; Gray, Michael J; Shalliker, R Andrew; Dennis, Gary R

    2005-05-06

    Isotopic substitution is a technique used to highlight particular bonds within a molecule for kinetic, spectroscopic and structure analysis. It is presumed that although some properties such as stretching frequencies will not be the same for substituted analogues, the chemical interactions will not vary appreciably as a function of labelling. Reversed-phase liquid chromatography has been used to demonstrate that there are significant differences between the chromatographic behaviour of a sequence of deuterated and protonated oligomeric polystyrenes. Two-dimensional reversed-phase liquid chromatography was used to show that even the diasteromers of the oligomers (n = 5) have retention mechanisms that are dependent on the subtle changes to the molecular conformation and electronic structure, which are a consequence of deuteration.

  1. Controlled crosslinking of trimethylolpropane trimethacrylate for preparation of organic monolithic columns for capillary liquid chromatography.

    Science.gov (United States)

    Gama, Mariana R; Aggarwal, Pankaj; Lee, Milton L; Bottoli, Carla B G

    2017-11-01

    Organic monolithic columns based on single crosslinking of trimethylolpropane trimethacrylate (TRIM) monomer were prepared in a single step by living/controlled free-radical polymerization. Full optimization of the preparation, such as using different percentages of TRIM and different amounts of radical promoter as well as various porogen solvents were explored. The resulting monolithic columns were characterized by scanning electronic microscopy and nitrogen sorption for structure morphology studies and surface area measurements, respectively. Using capillary liquid chromatography, 150 μm i.d. columns were applied to separate a mixture of small hydrophobic molecules. The results indicated that column performance is highly sensitive to the type and the amount of porogen solvents used in the polymerization mixture composition. Good resolution factors and methylene selectivity were obtained, indicating the promising potential of this material for capillary liquid chromatography separations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

    Science.gov (United States)

    Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

    2015-09-01

    In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Nielen, M W; Buijtenhuijs, F A

    1999-05-01

    Hyphenation of liquid chromatography (LC) techniques with electrospray ionization (ESI) orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS) provides both MS-based structural information and LC-based quantitative data in polymer analysis. In one experimental setup, three different LC modes are interfaced with MS:  size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS). In SEC/MS, both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra are achieved. GPEC/MS shows detailed chemical heterogeneity of the polymer and the chemical composition distribution within oligomer groups. In LCCC/MS, the retention behavior is primarily governed by chemical heterogeneities, such as different end group functionalities, and quantitative end group calculations can be easily made. The potential of these methods and the benefit of time-of-flight analyzers in polymer analysis are discussed using SEC/MS of a polydisperse poly(methyl methacrylate) sample, GPEC/MS of dipropoxylated bisphenol A/adipic acid polyester resin, LCCC/MS of alkylated poly(ethylene glycol), and LCCC/MS of terephthalic acid/neopentyl glycol polyester resin.

  4. Polarity-based fractionation in proteomics: hydrophilic interaction vs reversed-phase liquid chromatography.

    Science.gov (United States)

    Jafari, M; Mirzaie, M; Khodabandeh, M; Rezadoost, H; Ghassempour, A; Aboul-Enein, H Y

    2016-07-01

    During recent decades, hydrophilic interaction liquid chromatography (HILIC) ahs been introduced to fractionate or purify especially polar solutes such as peptides and proteins while reversed-phase liquid chromatography (RPLC) is also a common strategy. RPLC is also a common dimension in multidimensional chromatography. In this study, the potential of HILIC vs RPLC chromatography was compared for proteome mapping of human peripheral blood mononuclear cell extract. In HILIC a silica-based stationary phase and for RPLC a C18 column were applied. Then separated proteins were eluted to an ion trap mass spectrometry system. Our results showed that the HILIC leads to more proteins being identified in comparison to RPLC. Among the total 181 identified proteins, 56 and 38 proteins were fractionated specifically by HILIC and RPLC, respectively. In order to demonstrate this, the physicochemical properties of identified proteins such as polarity and hydrophobicity were considered. This analysis indicated that polarity may play a major role in the HILIC separation of proteins vs RPLC. Using gene ontology enrichment analysis, it was also observed that differences in physicochemical properties conform to the cellular compartment and biological features. Finally, this study highlighted the potential of HILIC and the great orthogonality of RPLC in gel-free proteomic studies. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

  5. High temperature aqueous potassium and sodium phosphate solutions: two-liquid-phase boundaries and critical phenomena, 275-4000C; potential applications for steam generators

    International Nuclear Information System (INIS)

    Marshall, W.L.

    1981-12-01

    Two-liquid-phase boundaries at temperatures between 275 and 400 0 C were determined for potassium phosphate and sodium phosphate aqueous solutions for compositions from 0 to 60 wt % dissolved salt. The stoichiometric mole ratios, K/PO 4 or Na/PO 4 , were varied from 1.00 to 2.12 and from 1.00 to 2.16 for the potassium and sodium systems, respectively. Liquid-vapor critical temperatures were also determined for most of the dilute liquid phases that formed. The minimum temperatures (below which a single solution existed) of two-liquid-phase formation were 360 0 C for the potassium system and 279 0 C for the sodium system at mole ratios of 2.00 and 2.16, respectively. For the sodium system at mole ratios greater than 2.16, solids crystallized at lower temperatures as expected from earlier studies. In contrast, potassium solutions that were explored at mole ratios from 2.12 to 3.16 and at temperatures below 360 0 C did not produce solid phases nor liquid-liquid immiscibilities. Aside from the generally unusual observations of two immiscible liquids in an aqueous inorganic salt system, the results could possibly be applied to the use of phosphate additives in steam power generators. 16 refs

  6. Metabolite Extraction from Saccharomyces cerevisiae for Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Rosebrock, Adam P; Caudy, Amy A

    2017-09-01

    Prior to mass spectrometric analysis, cellular small molecules must be extracted and separated from interfering components such as salts and culture medium. To ensure minimal perturbation of metabolism, yeast cells grown in liquid culture are rapidly harvested by filtration as described here. Simultaneous quenching of metabolism and extraction is afforded by immediate immersion in low-temperature organic solvent. Samples prepared using this method are suitable for a range of downstream liquid chromatography-mass spectrometry analyses and are stable in solvent for >1 yr at -80°C. © 2017 Cold Spring Harbor Laboratory Press.

  7. Determination of preservatives in cosmetics, cleaning agents and pharmaceuticals using fast liquid chromatography.

    Science.gov (United States)

    Baranowska, Irena; Wojciechowska, Iwona; Solarz, Natalia; Krutysza, Ewa

    2014-01-01

    This paper reports the development of a method for simultaneously determining five preservatives in cosmetics, cleaning agents and pharmaceuticals by fast liquid chromatography. Methylisothiazolinone, methylchloroisothiazolinone, benzyl alcohol, sodium benzoate and methylparaben were separated on a Chromolith Fast Gradient reversed-phase 18e column using gradient elution with acetonitrile and a 0.1% aqueous solution of formic acid, with a run time of 3 min. The preparation of solid and liquid samples included ultrasonic extraction with methanol with recoveries ranging from 69 to 119%. The developed method was used to analyze samples of cosmetics (66 samples), cleaning agents (five samples) and pharmaceutical industry products (17 samples).

  8. Identification and Quantitation of Asparagine and Citrulline Using High-Performance Liquid Chromatography (HPLC)

    OpenAIRE

    Bai, Cheng; Reilly, Charles C.; Wood, Bruce W.

    2007-01-01

    High-performance liquid chromatography (HPLC) analysis was used for identification of two problematic ureides, asparagine and citrulline. We report here a technique that takes advantage of the predictable delay in retention time of the co-asparagine/citrulline peak to enable both qualitative and quantitative analysis of asparagine and citrulline using the Platinum EPS reverse-phase C18 column (Alltech Associates). Asparagine alone is eluted earlier than citrulline alone, but when both of them...

  9. DETECTION AND QUANTIFICATION OF PHYTOCHEMICAL MARKERS OF Ilex paraguariensis BY LIQUID CHROMATOGRAPHY

    OpenAIRE

    Pinto,Rodrigo M. C.; Lemes,Bruna M.; Zielinski,Acácio A. F.; Klein,Traudi; Paula,Fernado de; Kist,Airton; Marques,Anna S. F.; Nogueira,Alessandro; Demiate,Ivo M.; Beltrame,Flávio L.

    2015-01-01

    Ilex paraguariensis (yerba-mate) is used as a beverage, and its extract requires adequate quality control methods in order to guarantee quality and safe use. Strategies to develop and optimize a chromatographic method to quantify theobromine, caffeine, and chlorogenic acid in I. paraguariensis extracts were evaluated by applying a quality by design (QbD) model and ultra high-performance liquid chromatography (UHPLC). The presence of these three phytochemical markers in the extracts was evalua...

  10. Simultaneous Determination of Four Preservatives in Foodstuffs by High Performance Liquid Chromatography

    OpenAIRE

    Mohammad Faraji; Farzaneh Rahbarzare

    2016-01-01

    Background and objectives:  High concentration of preservatives in food may result in gastrointestinal disturbances whereby some patients suffering from asthma, rhinitis, or urticaria. The aim of this study is the introduction and optimization a new method for simultaneous determination of four preservatives (SB, PS, MP, PP) in foodstuff by high performance liquid chromatography. Materials and methods: Important factors in extraction, separation and determination process were optimiz...

  11. Analysis of oak tannins by liquid chromatography-electrospray ionisation mass spectrometry.

    Science.gov (United States)

    Mämmelä, P; Savolainen, H; Lindroos, L; Kangas, J; Vartiainen, T

    2000-09-01

    Extractable tannins were analysed by liquid chromatography-electrospray ionisation mass spectrometry in two oak species, North American white oak (Quercus alba) and European red oak (Quercus robur). They mainly included various glucose gallic and ellagic acid esters. The structures were partially determined, and they included grandinin/roburin E, castalagin/vescalagin, gallic acid, valoneic acid bilactone, monogalloyl glucose, digalloyl glucose, trigalloyl glucose, ellagic acid rhamnose, quercitrin and ellagic acid.

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

    OpenAIRE

    Preti, Raffaella

    2016-01-01

    The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large am...

  13. Enantioselective analysis of drugs: contributions of high-performance liquid chromatography and capillary electrophoresis

    OpenAIRE

    Bonato, Pierina Sueli; Jabor, Valquíria Aparecida Polisel; Gaitani, Cristiane Masetto de

    2005-01-01

    The demand for analytical methods suitable for accurate and reproducible determination of drug enantiomers has increased significantly in the last years. High-performance liquid chromatography (HPLC) using chiral stationary phases and capillary electrophoresis (CE) are the most important techniques used for this purpose. In this paper, the fundamental aspects of chiral separations using both techniques are presented. Some important aspects for the development of enantioselective methods, part...

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

    Science.gov (United States)

    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. Toxic Compounds Analysis With High Performance Liquid Chromatography Detected By Electro Chemical Detector (Ecd)

    OpenAIRE

    Hideharu Shintaniq

    2014-01-01

    The principal area of application of high performance liquid chromatography-electrochemical detector (HPLC-ECD) has been in the analysis of naturally-occurring analytes, such as catecholamines, and pharmaceuticals in biological samples, HPLC-ECD has also applied to the analysis of pesticides and other analytes of interest to the toxicologist. In this paper, toxic area is described. In these, ammatoxins, aromatic amine, nitro-compounds, algal toxins, fungal toxins, pesticides, veterinary drug ...

  16. Resolution of the stereoisomers of baclofen by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Weatherby, R.P.; Allan, R.D.; Johnston, G.A.R.

    1984-01-01

    The GABA analogue baclofen [3-(p-chlorophenyl)-4-aminobutanoic acid] has stereospecific actions on the peripheral and central nervous systems. This paper describes the resolution of tritium-labelled baclofen by high performance liquid chromatography on a reverse-phase C18 column using a chiral mobile phase. The method, which may have general application to certain other GABA analogues, affords optically pure (+)- and (-)-baclofen labelled with tritium to high specific activity suitable for ligand binding and other neurochemical studies. (Auth.)

  17. Quantitative analysis of cytokinins in plants by liquid chromatography single-quadrupole mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Novák, Ondřej; Tarkowski, Petr; Tarkowská, Danuše; Doležal, Karel; Lenobel, René; Strnad, Miroslav

    2003-01-01

    Roč. 480, č. 2 (2003), s. 207ů218 ISSN 0003-2670 R&D Projects: GA ČR GA522/01/0275 Grant - others:Volkswagen Stiftung(DE) I/76 865 Institutional research plan: CEZ:AV0Z5038910; CEZ:MSM 153100008 Keywords : Liquid chromatography mass spectrometry * Cytokinins Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.210, year: 2003

  18. Fingerprint analysis of Resina Draconis by ultra-performance liquid chromatography

    OpenAIRE

    Xue, Yudi; Zhu, Lin; Yi, Tao

    2017-01-01

    Background Resina Draconis, a bright red resin derived from Dracaena cochinchinensis, is a traditional medicine used in China. To improve its quality control approach, an ultra-performance liquid chromatography (UPLC) fingerprint method was developed for rapidly evaluating the quality of Resina Draconis. Methods The precision, repeatability and stability of the proposed UPLC method were validated in the study. Twelve batches of Resina Draconis samples from various sources were analyzed by the...

  19. Metal coordination in the high-temperature leaching of roasted NdFeB magnets with the ionic liquid betainium bis(trifluoromethylsulfonyl)imide

    OpenAIRE

    Orefice, Martina; Binnemans, Koen; Vander Hoogerstraete, Tom

    2018-01-01

    Ionic liquids are largely used to leach metals from primary (ores) and secondary sources (end-of-life products). However, dry ionic liquids with a carboxylic function on the cation have not yet been used to leach metals at temperature above 100 °C and under atmospheric pressure. The ionic liquid betainium bis(trifluoromethylsulfonyl)imide, [Hbet][Tf2N], was used in the dry state to recover neodymium, dysprosium and cobalt from NdFeB magnets and NdFeB production scrap. The magnets and the scra...

  20. Determination of Niacinamide in Lotions and Creams Using Liquid-Liquid Extraction and High-Performance Liquid Chromatography

    Science.gov (United States)

    Usher, Karyn M.; Simmons, Carolyn R.; Keating, Daniel W.; Rossi, Henry F., III

    2015-01-01

    Chemical separations are an important part of an undergraduate chemistry curriculum. Sophomore students often get experience with liquid-liquid extraction in organic chemistry classes, but liquid-liquid extraction is not as often introduced as a quantitative sample preparation method in honors general chemistry or quantitative analysis classes.…

  1. Simultaneous determination of several phytohormones in natural coconut juice by hollow fiber-based liquid-liquid-liquid microextraction-high performance liquid chromatography.

    Science.gov (United States)

    Wu, Yunli; Hu, Bin

    2009-11-06

    A simple, selective, sensitive and inexpensive method of hollow fiber-based liquid-liquid-liquid microextraction (HF-LLLME) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV) detection was developed for the determination of four acidic phytohormones (salicylic acid (SA), indole-3-acetic acid (IAA), (+/-) abscisic acid (ABA) and (+/-) jasmonic acid (JA)) in natural coconut juice. To the best of our knowledge, this is the first report on the use of liquid phase microextraction (LPME) as a sample pretreatment technique for the simultaneous analysis of several phytohormones. Using phenetole to fill the pores of hollow fiber as the organic phase, 0.1molL(-1) NaOH solution in the lumen of hollow fiber as the acceptor phase and 1molL(-1) HCl as the donor phase, a simultaneous preconcentration of four target phytohormones was realized. The acceptor phase was finally withdrawn into the microsyringe and directly injected into HPLC for the separation and quantification of the target phytohormones. The factors affecting the extraction efficiency of four phytohormones by HF-LLLME were optimized with orthogonal design experiment, and the data was analyzed by Statistical Product and Service Solutions (SPSS) software. Under the optimized conditions, the enrichment factors for SA, IAA, ABA and JA were 243, 215, 52 and 48, with the detection limits (S/N=3) of 4.6, 1.3, 0.9ngmL(-1) and 8.8 microg mL(-1), respectively. The relative standard deviations (RSDs, n=7) were 7.9, 4.9, 6.8% at 50ngmL(-1) level for SA, IAA, ABA and 8.4% at 500 microg mL(-1) for JA, respectively. To evaluate the accuracy of the method, the developed method was applied for the simultaneous analysis of several phytohormones in five natural coconut juice samples, and the recoveries for the spiked samples were in the range of 88.3-119.1%.

  2. Applications of the solvation parameter model in reversed-phase liquid chromatography.

    Science.gov (United States)

    Poole, Colin F; Lenca, Nicole

    2017-02-24

    The solvation parameter model is widely used to provide insight into the retention mechanism in reversed-phase liquid chromatography, for column characterization, and in the development of surrogate chromatographic models for biopartitioning processes. The properties of the separation system are described by five system constants representing all possible intermolecular interactions for neutral molecules. The general model can be extended to include ions and enantiomers by adding new descriptors to encode the specific properties of these compounds. System maps provide a comprehensive overview of the separation system as a function of mobile phase composition and/or temperature for method development. The solvation parameter model has been applied to gradient elution separations but here theory and practice suggest a cautious approach since the interpretation of system and compound properties derived from its use are approximate. A growing application of the solvation parameter model in reversed-phase liquid chromatography is the screening of surrogate chromatographic systems for estimating biopartitioning properties. Throughout the discussion of the above topics success as well as known and likely deficiencies of the solvation parameter model are described with an emphasis on the role of the heterogeneous properties of the interphase region on the interpretation and understanding of the general retention mechanism in reversed-phase liquid chromatography for porous chemically bonded sorbents. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

    Science.gov (United States)

    Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

    2016-10-01

    The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Separation of enantiomers of new psychoactive substances by high-performance liquid chromatography.

    Science.gov (United States)

    Kadkhodaei, Kian; Forcher, Lisa; Schmid, Martin G

    2018-03-01

    New psychoactive substances are defined as compounds with consciousness-changing effects and have been developed simultaneously with classical drugs. They arise through structural modifications of illegal substances and are mainly produced to circumvent laws. Availability is simple, since new psychoactive substances can be purchased from the Internet. Among them many chemical drug compound classes are chiral and thus the two resulting enantiomers can differ in their effects. The aim of this study is to develop a suitable chiral high-performance liquid chromatography separation method for a broad spectrum of new psychoactive substances using cellulose tris(3,5-dichlorophenylcarbamate) as a chiral selector. Experiments were performed by high-performance liquid chromatography in normal-phase mode under isocratic conditions using ultraviolet detection. Direct separation was carried out on a high-performance liquid chromatography column (Lux® i-Cellulose-5, 3.5 μm, Phenomenex®), available since 2016. Excellent separation results were obtained for cathinones. After further optimization, even 47 instead of 39 out of 52 cathinones showed baseline separation. For amphetamine derivatives, satisfactory results were not achieved. Further, new psychoactive substances from other compound classes such as benzofuranes, thiophenes, phenidines, phenidates, morpholines, and ketamines were partially resolved, depending on the polarity and degree of substitution. All analytes, which were mainly purchased from the Internet, were proven to be traded as racemates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Determination of veterinary antibiotic residues in foods of animal origin by liquid chromatography

    Directory of Open Access Journals (Sweden)

    Pedro Enrique La Rosa Zambrano

    2018-05-01

    Full Text Available TITLE: Determination of veterinary antibiotic residues in foods of animal origin by liquid chromatography Introduction: The presence of certain infectious agents makes necessary the use of antibiotics to ensure the welfare of animals destined for human consumption; however, the withdrawal time must be considered and respected since there is the possibility of finding residues above the permitted levels, which could constitute a risk to public health. Objective: Present a collection of information based on how is performed the detection and quantification of antibiotic residues in various products of animal origin using chromatography methods. Method: Review of databases in Elsevier, SciELO, Springer, Hindawi, FAO, EFSA, Senasa and Sanipes, using keywords such as “liquid chromatography”, “mass spectrometry”, “antibiotic residues” and “products of animal origin” in Spanish and English. Results: They were selected 71 references among articles, book chapters, norms and regulations published between 2000 and 2017, which it is emphasized that chromatographic methodologies for antibiotic residues monitoring must be sensitive, reproducible, reliable and identify volumes in mg/kg; likewise, they must follow the requirements of international standards for the maximum residue limits detecction. Conclusions: Liquid chromatography coupled to a mass spectrometer is the most used technique to allow the separation of complex matrices based on the molecular weight of the compound (antibiotic or its fragments; however, It is complex, expensive and requires highly trained personnel.

  6. Characterization of pitches by liquid chromatography using cellulose 3,5-dinitrobenzoate as the packing material

    Energy Technology Data Exchange (ETDEWEB)

    Arai, K.; Judo, R.; Ota, E. [Gunma University, Gunma (Japan). Dept. of Chemistry

    1997-08-01

    Characterization of coal tar, petroleum and PVC pitches by a liquid chromatography using cellulose 3,5-dinitrobenzoate (DNB-cellulose) as the packing material was investigated. Separation mechanism based on charge-transfer interaction between the dinitrobenzoyl group and polyaromatic compounds was expected to be useful for separation of the constituents of the pitches. First, 26 model polyaromatic compounds were tested to examine the characteristic feature of the packing material by liquid chromatography. The compounds were found to be classified roughly into four groups with different retention volume, principally according to the number of condensed rings. The nonplanar structure and aliphatic side chain of the polyaromatic compounds also affected the separation behavior. Both benzene soluble-hexane soluble and benzene soluble-hexane insoluble fractions of the three pitches were separated on DNB-cellulose. It was found that coal tar pitch contains relatively large amounts of some highly condensed polyaromatic compounds with condensed rings of 4 to 5; petroleum pitch has small amounts of such specific highly condensed polyaromatic compounds, while PVC pitch has large amounts of less condensed polyaromatic compounds and there is no significant amount of highly condensed compound in it. Thus DNB-cellulose was useful as the convenient packing material for liquid chromatography to characterize pitches.

  7. Optimization of the combination micro-high-performance liquid-chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Haider, K.

    1997-03-01

    The coupling of liquid chromatography and mass spectrometry is still growing in significance. In this thesis, a particle beam interface has been investigated for combining ion chromatography with mass spectrometric detection. To introduce the eluent directly (without membrane suppressor) into the spectrometer, only methods with low flow rates like microcolumn chromatography can be used. For the preparation of the columns, reversed-phase and silica-based anion exchange materials were packed into PEEK, steel and fused-silica capillaries with i.d. from 130 to 1000 μm using different methods. The performance of the particle beam interface (modified with a new miniaturized aerosol generator) and the mass spectrometric detection has been studied for a series of inorganic anions as well as aminopolycarboxylic acids and the metal-EDTA complexes. Detection limits between 10 and 100 ng injected could be achieved in the multiple ion detection mode of the mass spectrometer for the investigated solutes. A second type of interface, the direct liquid introduction (DLI) has been used to analyze the priority pollutant phenols. This interface is based on a modified GC-interface into the MS. Separation columns used so far include packed fused-silica capillaries with inner diameter of 75 μm and polystyrene-divinylbenzene (functionalized with tert. butyl groups) as stationary phase. Aspects of instrumentation and effects of chemical ionization in the direct liquid introduction mode are discussed. (author)

  8. Determination of carbofuran on hydrophilic interaction liquid chromatography using TSK gel amide 80 as stationary phase

    International Nuclear Information System (INIS)

    A Kurnia; LW Lim; T Takeuchi

    2016-01-01

    The hydrophilic interaction liquid chromatography (HILIC) coupled to environmental friendly capillary liquid chromatography was employed to investigate retention behavior of carbofuran. Aim of this research is to investigate retention behavior of carbofuran using TSK gel amide 80 as stationary phase. Several condition was conducted to investigate retention behavior of carbofuran such as comparison study of TSK gel amide 80 with other polar column, comparison study retention behavior of carbofuran on various system wavelength, water content effect in HILIC mode, effect of buffer concentration on HILIC mode, and analytical performance. Results showed that TSK gel imidazole was superior compare to other polar stationary phase on determine carbofuran, wavelength 251 and 254 nm was resulting higher absorbance for carbofuran than others, increase of water content on mobile phase was decrease the retention time, also increase buffer salt concentration was decrease the retention time and according to analysis performance that is the accuracy was 101±10,1, the LOD 0.66 ppm while LOQ 2.22 ppm. As conclusions that TSK gel amide 80 was offering good determine on carbofuran even using capillary liquid chromatography with 10 cm length of column. (author)

  9. High-Temperature-Short-Time (HTST) sterilization of liquid food with solid particles; HTST steriliseren van vloeibare levensmiddelen met vaste deeltjes

    Energy Technology Data Exchange (ETDEWEB)

    Boon, F

    2000-11-01

    As part of a sectoral study for the Association of the Dutch Vegetable and Fruit Processing Industry (VIGEF) a project started on the Factory 2005 concept. Options to improve the product quality of canned vegetables and fruit are investigated. One of the options is to reduce the heat during the sterilization process by applying the HTST method (high-temperature-short-time). Two processes are compared: the Gierschner process and the Stork Steripart process. [Dutch] Binnen de VIGEF (Vereniging van de Nederlandse Groenten- en Fruitverwerkende Industrie) is een project gestart in samenwerking met TNO dat zich richt op de fabriek 2005. Onderzoek wordt gedaan naar de mogelijkheden om de productkwaliteit van geconserveerde groenten en fruit te verbeteren. Het richt zich o.a. op de mogelijkheden om de hitte-intensiteit tijdens de sterilisatie te verlagen door te steriliseren volgens de HTST methode (high-temperature-short-time). Motivatie voor de ontwikkeling van HTST processen is primair kwaliteitsverbetering met gelijke microbiele veiligheid (t.o.v. het conventionele proces). Er worden 2 processen vergeleken: het Gierschner proces en het Stork Steripart proces.

  10. Simultaneous determination of niacin and pyridoxine at trace levels by using diode array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Sel, Sabriye; Öztürk Er, Elif; Bakırdere, Sezgin

    2017-12-01

    A highly sensitive and simple diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method was developed for the simultaneous determination of niacin and pyridoxine in pharmaceutical drugs, tap water, and wastewater samples. To determine the in vivo behavior of niacin and pyridoxine, analytes were subjected to simulated gastric conditions. The calibration plots of the diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method showed good linearity over a wide concentration range with close to 1.0 correlation coefficients for both analytes. The limit of detection/limit of quantitation values for liquid chromatography quadrupole time-of-flight tandem mass spectrometry analysis were 1.98/6.59 and 1.3/4.4 μg/L for niacin and pyridoxine, respectively, while limit of detection/limit of quantitation values for niacin and pyridoxine in high-performance liquid chromatography analysis were 3.7/12.3 and 5.7/18.9 μg/L, respectively. Recovery studies were also performed to show the applicability of the developed methods, and percentage recovery values were found to be 90-105% in tap water and 94-97% in wastewater for both analytes. The method was also successfully applied for the qualitative and quantitative determination of niacin and pyridoxine in drug samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Gas chromatography-mass spectrometry and high-performance liquid chromatographic analyses of thermal degradation products of common plastics

    OpenAIRE

    Pacakova, V.; Leclercq, P.A.

    1991-01-01

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile degradation products, while high-performance liquid chromatography was employed to measure polycyclic aromatic hydrocarbons. The results are discussed from the point of view of toxicity of the prod...

  12. Multielement determination of rare earth elements in rock sample by liquid chromatography / inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Hamanaka, Tadashi; Itoh, Akihide; Itoh, Shinya; Sawatari, Hideyuki; Haraguchi, Hiroki.

    1995-01-01

    Rare earth elements in geological standard rock sample JG-1 (granodiolite)issued from the Geological Survey of Japan have been determined by a combined system of liquid chromatography and inductively coupled plasma mass spectrometry. (author)

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

    Science.gov (United States)

    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 ...

  14. High temperature superconductors and other superfluids

    CERN Document Server

    Alexandrov, A S

    2017-01-01

    Written by eminent researchers in the field, this text describes the theory of superconductivity and superfluidity starting from liquid helium and a charged Bose-gas. It also discusses the modern bipolaron theory of strongly coupled superconductors, which explains the basic physical properties of high-temperature superconductors. This book will be of interest to fourth year graduate and postgraduate students, specialist libraries, information centres and chemists working in high-temperature superconductivity.

  15. Overview of online two-dimensional liquid chromatography based on cell membrane chromatography for screening target components from traditional Chinese medicines.

    Science.gov (United States)

    Muhammad, Saqib; Han, Shengli; Xie, Xiaoyu; Wang, Sicen; Aziz, Muhammad Majid

    2017-01-01

    Cell membrane chromatography is a simple, specific, and time-saving technique for studying drug-receptor interactions, screening of active components from complex mixtures, and quality control of traditional Chinese medicines. However, the short column life, low sensitivity, low column efficiency (so cannot resolve satisfactorily mixture of compounds), low peak capacity, and inefficient in structure identification were bottleneck in its application. Combinations of cell membrane chromatography with multidimensional chromatography such as two-dimensional liquid chromatography and high sensitivity detectors like mass have significantly reduced many of the above-mentioned shortcomings. This paper provides an overview of the current advances in online two-dimensional-based cell membrane chromatography for screening target components from traditional Chinese medicines with particular emphasis on the instrumentation, preparation of cell membrane stationary phase, advantages, and disadvantages compared to alternative approaches. The last section of the review summarizes the applications of the online two-dimensional high-performance liquid chromatography based cell membrane chromatography reported since its emergence to date (2010-June 2016). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

    NARCIS (Netherlands)

    Koster, E.H M; Hofman, N.S K; de Jong, G.J.

    Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

  17. Determination of ten carbamate pesticides in aquatic and sediment samples by liquid chromatography-ionspray and thermospray mass spectrometry.

    NARCIS (Netherlands)

    Honing, M.; Riu, J.; Barceló, D.; van Baar, B.L.M.; Brinkman, U.A.T.

    1996-01-01

    Ten carbamate pesticides which exhibit large differences in polarity were determined simultaneously in various environmental samples, using both column liquid chromatography (LC)-thermospray (TSP) mass spectrometry (MS) and LC-ionspray (ISP) MS. For sample clean-up, column chromatography with three

  18. Preparation and Characterization of a Polymeric Monolithic Column for Use in High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Bindis, Michael P.; Bretz, Stacey Lowery; Danielson, Neil D.

    2011-01-01

    The high-performance liquid chromatography (HPLC) experiment, most often done in the undergraduate analytical instrumentation laboratory course, generally illustrates reversed-phase chromatography using a commercial C[subscript]18 silica column. To avoid the expense of periodic column replacement and introduce a choice of columns with different…

  19. tRNA separation by high-performance liquid chromatography using an aggregate of ODS-Hypersil and trioctylmethylammonium chloride

    NARCIS (Netherlands)

    Bischoff, Rainer; Graeser, E.; Mclaughlin, L.W.

    1983-01-01

    High-performance liquid chromatography on a reversed-phase support treated with a tetraalkylammonium salt was used to separate tRNAs from baker's yeast. While resolution by this column appears to result from both anion-exchange and reversed-phase chromatography, it is the hydrophobic interactions

  20. Quantitative analysis of pharmaceuticals in biological fluids using high-performance liquid chromatography coupled to mass spectrometry: a review.

    Science.gov (United States)

    Plumb, R S; Dear, G J; Mallett, D N; Higton, D M; Pleasance, S; Biddlecombe, R A

    2001-01-01

    1. The development of bio-analysis of drug molecules over the last 10 years is reviewed, focusing on advances in sample preparation, liquid chromatography and detection. 2. Developments have led to improvements in detection sensitivity, enhancements in specificity and increased capacity. 3. Emerging technologies such as monolithic column chromatography and miniaturized chip-based systems are discussed.

  1. Investigation of forced and total degradation products of amlodipine besylate by liquid chromatography and liquid chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Stoiljković Zora Ž.

    2014-01-01

    Full Text Available An isocratic, reversed-phase liquid chromatographic method was applied for the investigation of the degradation products of amlodipine besylate under the stressed conditions in solution. Amlodipine besylate stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and photodegradation as well as to the electrochemical degradation by cyclic voltammetry in 0.05 mol/L NaHCO3 on gold electrode. The total degradation of amlodipine besylate was achieved in 5 mol/L NaOH at 80°C for 6 h and the compound with molecular formula C15H16NOCl was identified as a main degradation product. Under acidic (5 mol/L HCl at 80°C for 6 h stress conditions 75.2% of amlodipine besylate degradation was recorded. Oxidative degradation in the solution of 3% H2O2-methanol 80:20 at 80°C for 6 h showed that amlodipine besylate degraded to 80.1%. After 14 days of expose in photostability chamber amlodipine besylate solution showed degradation of 32.2%. In electrochemical degradation after 9 hours of cyclization the beginning of amlodipine oxidation was shifted for 200 mV to more negative potentials, with the degradation of 66.5%. Mass spectrometry analysis confirmed the presence of dehydro amlodipine derivate with molecular formula C20H23N2O5Cl in oxidative and acidic conditions while in electrochemical degradation was detected in traces. [Projekat Ministarsva nauke Republike Srbije, br. 172013

  2. High-temperature superconductivity

    International Nuclear Information System (INIS)

    Ginzburg, V.L.

    1987-07-01

    After a short account of the history of experimental studies on superconductivity, the microscopic theory of superconductivity, the calculation of the control temperature and its possible maximum value are presented. An explanation of the mechanism of superconductivity in recently discovered superconducting metal oxide ceramics and the perspectives for the realization of new high-temperature superconducting materials are discussed. 56 refs, 2 figs, 3 tabs

  3. High temperature materials

    International Nuclear Information System (INIS)

    2003-01-01

    The aim of this workshop is to share the needs of high temperature and nuclear fuel materials for future nuclear systems, to take stock of the status of researches in this domain and to propose some cooperation works between the different research organisations. The future nuclear systems are the very high temperature (850 to 1200 deg. C) gas cooled reactors (GCR) and the molten salt reactors (MSR). These systems include not only the reactor but also the fabrication and reprocessing of the spent fuel. This document brings together the transparencies of 13 communications among the 25 given at the workshop: 1) characteristics and needs of future systems: specifications, materials and fuel needs for fast spectrum GCR and very high temperature GCR; 2) high temperature materials out of neutron flux: thermal barriers: materials, resistance, lifetimes; nickel-base metal alloys: status of knowledge, mechanical behaviour, possible applications; corrosion linked with the gas coolant: knowledge and problems to be solved; super-alloys for turbines: alloys for blades and discs; corrosion linked with MSR: knowledge and problems to be solved; 3) materials for reactor core structure: nuclear graphite and carbon; fuel assembly structure materials of the GCR with fast neutron spectrum: status of knowledge and ceramics and cermets needs; silicon carbide as fuel confinement material, study of irradiation induced defects; migration of fission products, I and Cs in SiC; 4) materials for hydrogen production: status of the knowledge and needs for the thermochemical cycle; 5) technologies: GCR components and the associated material needs: compact exchangers, pumps, turbines; MSR components: valves, exchangers, pumps. (J.S.)

  4. Quantitative analysis of phylloquinone (vitamin K1) in soy bean oils by high-performance liquid chromatography.

    Science.gov (United States)

    Zonta, F; Stancher, B

    1985-07-19

    A high-performance liquid chromatographic method for determining phylloquinone (vitamin K1) in soy bean oils is described. Resolution of vitamin K1 from interfering peaks of the matrix was obtained after enzymatic digestion, extraction and liquid-solid chromatography on alumina. An isocratic reversed-phase chromatography with UV detection was used in the final stage. The quantitation was carried out by the standard addition method, and the recovery of the whole procedure was 88.2%.

  5. Stationary and through-flow radiochemical detectors in cooperation with high performance liquid chromatography: Application in biochemistry

    International Nuclear Information System (INIS)

    Kehr, J.

    1986-01-01

    A review article is presented containing some original experimental data and discussing the usability of radiochemical detection of labelled compounds using high performance liquid chromatography. The stationary and through-flow types of detection are compared with respect to efficiency, chromatographic zone resolution, usability in biochemical research, and also to the current trends of development of liquid chromatography. (author). 3 figs., 1 tab., 19 refs

  6. Deformation and degradation of polymers in ultra-high-pressure liquid chromatography.

    Science.gov (United States)

    Uliyanchenko, Elena; van der Wal, Sjoerd; Schoenmakers, Peter J

    2011-09-28

    Ultra-high-pressure liquid chromatography (UHPLC) using columns packed with sub-2 μm particles has great potential for separations of many types of complex samples, including polymers. However, the application of UHPLC for the analysis of polymers meets some fundamental obstacles. Small particles and narrow bore tubing in combination with high pressures generate significant shear and extensional forces in UHPLC systems, which may affect polymer chains. At high stress conditions flexible macromolecules may become extended and eventually the chemical bonds in the molecules can break. Deformation and degradation of macromolecules will affect the peak retention and the peak shape in the chromatogram, which may cause errors in the obtained results (e.g. the calculated molecular-weight distributions). In the present work we explored the limitations of UHPLC for the analysis of polymers. Degradation and deformation of macromolecules were studied by collecting and re-injecting polymer peaks and by off-line two-dimensional liquid chromatography. Polystyrene standards with molecular weight of 4 MDa and larger were found to degrade at UHPLC conditions. However, for most polymers degradation could be avoided by using low linear velocities. No degradation of 3-MDa PS (and smaller) was observed at linear velocities up to 7 mm/s. The column frits were implicated as the main sources of polymer degradation. The extent of degradation was found to depend on the type of the column and on the column history. At high flow rates degradation was observed without a column being installed. We demonstrated that polymer deformation preceded degradation. Stretched polymers eluted from the column in slalom chromatography mode (elution order opposite to that in SEC or HDC). Under certain conditions we observed co-elution of large and small PS molecules though a convolution of slalom chromatography and hydrodynamic chromatography. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Determination of parabens in serum by liquid chromatography-tandem mass spectrometry: Correlation with lipstick use.

    Science.gov (United States)

    Tahan, Gabriella Padovani; Santos, Nayara de Kássia Souza; Albuquerque, Ana Carolina; Martins, Isarita

    2016-08-01

    Parabens are the most widely used preservative and are considered to be relatively safe compounds. However, studies have demonstrated that they may have estrogenic activity, and there is ongoing debate regarding the safety and potential cancer risk of using products containing these compounds. In the present work, liquid chromatography-tandem mass spectrometry was applied to determine methylparaben and propylparaben concentrations in serum, and the results were correlated with lipstick application. Samples were analyzed using liquid-liquid extraction, followed by liquid chromatography-tandem mass spectrometry. The validation results demonstrated the linearity of the method over a range of 1-20 ng/mL, in addition to the method's precision and accuracy. A statistically significant difference was demonstrated between serum parabens in women who used lipstick containing these substances compared with those not using this cosmetic (p = 0.0005 and 0.0016, respectively), and a strong association was observed between serum parabens and lipstick use (Spearman correlation = 0.7202). Copyright © 2016 Elsevier Inc. All rights reserved.

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

    Science.gov (United States)

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

    2016-01-01

    Objective: Benzodiazepines are frequently screened drugs in emergency toxicology, drugs of abuse testing, and in forensic cases. As the variations of benzodiazepines concentrations in biological samples during bleeding, postmortem changes, and redistribution could be biasing forensic medicine examinations, hence selecting a suitable sample and a validated accurate method is essential for the quantitative analysis of these main drug categories. The aim of this study was to develop a valid method for the determination of four benzodiazepines (flurazepam, lorazepam, alprazolam, and diazepam) in vitreous humor using liquid–liquid extraction and high-performance liquid chromatography. Methods: Sample preparation was carried out using liquid–liquid extraction with n-hexane: ethyl acetate and subsequent detection by high-performance liquid chromatography method coupled to diode array detector. This method was applied to quantify benzodiazepines in 21 authentic vitreous humor samples. Linear curve for each drug was obtained within the range of 30–3000 ng/mL with coefficient of correlation higher than 0.99. Results: The limit of detection and quantitation were 30 and 100 ng/mL respectively for four drugs. The method showed an appropriate intra- and inter-day precision (coefficient of variation forensic toxicology laboratory. PMID:27635251

  9. Analysis of aromatic amines in water samples by liquid-liquid-liquid microextraction with hollow fibers and high-performance liquid chromatography.

    Science.gov (United States)

    Zhao, Limian; Zhu, Lingyan; Lee, Hian Kee

    2002-07-19

    Liquid-liquid-liquid microextraction (LLLME) with hollow fibers in high-performance liquid chromatography (HPLC) has been applied as a rapid and sensitive quantitative method for the detection of four aromatic amines (3-nitroaniline, 4-chloroaniline, 4-bromoaniline and 3,4-dichloroaniline) in environmental water samples. The preconcentration procedure was induced by the pH difference inside and outside the hollow fiber. The target compounds were extracted from 4-ml aqueous sample (donor solution, pH approximately 13) through a microfilm of organic solvent (di-n-hexyl ether), immobilized in the pores of a hollow fiber (1.5 cm length x 0.6 mm I.D.), and finally into 4 microl of acid acceptor solution inside the fiber. After a prescribed period of time, the acceptor solution inside the fiber was withdrawn into the microsyringe and directly injected into the HPLC system for analysis. Factors relevant to the extraction procedure were studied. Up to 500-fold enrichment of analytes could be obtained under the optimized conditions (donor solution: 0.1 M sodium hydroxide solution with 20% sodium chloride and 2% acetone; organic phase: di-n-hexyl ether; acceptor solution: 0.5 M hydrochloric acid and 500 mM 18-crown-6 ether; extraction time of 30 min; stirring at 1,000 rev./min). The procedure also served as a sample clean-up step. The influence of humic acid on the extraction efficiency was also investigated, and more than 85% relative recoveries of the analytes at two different concentrations (20 and 100 microg/l) were achieved at various concentration of humic acid. This technique is a low cost, simple and fast approach to the analysis of polar compounds in aqueous samples.

  10. Incorporation of ionic liquid into porous polymer monoliths to enhance the separation of small molecules in reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Jiafei; Bai, Ligai; Wei, Zhen; Qin, Junxiao; Ma, Yamin; Liu, Haiyan

    2015-06-01

    An ionic liquid was incorporated into the porous polymer monoliths to afford stationary phases with enhanced chromatographic performance for small molecules in reversed-phase high-performance liquid chromatography. The effect of the ionic liquid in the polymerization mixture on the performance of the monoliths was studied in detail. While monoliths without ionic liquid exhibited poor resolution and low efficiency, the addition of ionic liquid to the polymerization mixture provides highly increased resolution and high efficiency. The chromatographic performances of the monoliths were demonstrated by the separations of various small molecules including aromatic hydrocarbons, isomers, and homologues using a binary polar mobile phase. The present column efficiency reached 27 000 plates/m, which showed that the ionic liquid monoliths are alternative stationary phases in the separation of small molecules by high-performance liquid chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids.

    Science.gov (United States)

    Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

    2008-07-11

    Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method developed was successfully applied for primary screening of RTILs (>20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media.

  12. Screening anti-tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry.

    Science.gov (United States)

    Zhang, Tao; Ding, Yuanyuan; An, Hongli; Feng, Liuxin; Wang, Sicen

    2015-07-14

    Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine-HEK293 cells were used as cell membrane stationary phase. Specificity and reproducibility of the cell membrane chromatography was evaluated using 1-tert-butyl-3-{2-[4-(diethylamino)butylamino]-6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-7-yl}urea, Nimodipine and dexamethasone acetate. Then, anti-tumor components acting on Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high-performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide-formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose-dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two-dimensional high-performance liquid chromatography method can screen and identify potential anti-tumor ingredients which specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  13. Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

    2016-03-04

    Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

    Science.gov (United States)

    Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

    2016-03-18

    Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Comprehensive two-dimensional liquid chromatography with on-line Fourier-transform-infrared-spectroscopy detection for the characterization of copolymers

    NARCIS (Netherlands)

    Kok, S.J.; Hankemeier, T.; Schoenmakers, P.J.

    2005-01-01

    The on-line coupling of comprehensive two-dimensional liquid chromatography (liquid chromatography × size-exclusion chromatography, LC × SEC) and infrared (IR) spectroscopy has been realized by means of an IR flow cell. The system has been assessed by the functional-group analysis of a series of

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

    Science.gov (United States)

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

    2015-09-01

    An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples. Copyright © 2015. Published by Elsevier B.V.

  17. Miniaturized protein separation using a liquid chromatography column on a flexible substrate

    International Nuclear Information System (INIS)

    Yang Yongmo; Chae, Junseok

    2008-01-01

    We report a prototype protein separator that successfully miniaturizes existing technology for potential use in biocompatible health monitoring implants. The prototype is a liquid chromatography (LC) column (LC mini-column) fabricated on an inexpensive, flexible, biocompatible polydimethylsiloxane (PDMS) enclosure. The LC mini-column separates a mixture of proteins using size exclusion chromatography (SEC) with polydivinylbenzene beads (5–20 µm in diameter with 10 nm pore size). The LC mini-column is smaller than any commercially available LC column by a factor of ∼11 000 and successfully separates denatured and native protein mixtures at ∼71 psi of the applied fluidic pressure. Separated proteins are analyzed using NuPAGE-gel electrophoresis, high-performance liquid chromatography (HPLC) and an automated electrophoresis system. Quantitative HPLC results demonstrate successful separation based on intensity change: within 12 min, the intensity between large and small protein peaks changed by a factor of ∼20. In further evaluation using the automated electrophoresis system, the plate height of the LC mini-column is between 36 µm and 100 µm. The prototype LC mini-column shows the potential for real-time health monitoring in applications that require inexpensive, flexible implant technology that can function effectively under non-laboratory conditions

  18. High temperature superconductors

    CERN Document Server

    Paranthaman, Parans

    2010-01-01

    This essential reference provides the most comprehensive presentation of the state of the art in the field of high temperature superconductors. This growing field of research and applications is currently being supported by numerous governmental and industrial initiatives in the United States, Asia and Europe to overcome grid energy distribution issues. The technology is particularly intended for densely populated areas. It is now being commercialized for power-delivery devices, such as power transmission lines and cables, motors and generators. Applications in electric utilities include current limiters, long transmission lines and energy-storage devices that will help industries avoid dips in electric power.

  19. High temperature radioisotope capsule

    International Nuclear Information System (INIS)

    Bradshaw, G.B.

    1976-01-01

    A high temperature radioisotope capsule made up of three concentric cylinders, with the isotope fuel located within the innermost cylinder is described. The innermost cylinder has hemispherical ends and is constructed of a tantalum alloy. The intermediate cylinder is made of a molybdenum alloy and is capable of withstanding the pressure generated by the alpha particle decay of the fuel. The outer cylinder is made of a platinum alloy of high resistance to corrosion. A gas separates the innermost cylinder from the intermediate cylinder and the intermediate cylinder from the outer cylinder

  20. High temperature reaction kinetics

    International Nuclear Information System (INIS)

    Jonah, C.D.; Beno, M.F.; Mulac, W.A.; Bartels, D.

    1985-01-01

    During the last year the dependence of the apparent rate of OD + CO on water pressure was measured at 305, 570, 865 and 1223 K. An explanation was found and tested for the H 2 O dependence of the apparent rate of OH(OD) + CO at high temperatures. The isotope effect for OH(D) with CO was determined over the temperature range 330 K to 1225 K. The reason for the water dependence of the rate of OH(OD) + CO near room temperatures has been investigated but no clear explanation has been found. 1 figure

  1. Osteoblast cell membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry for screening specific active components from traditional Chinese medicines.

    Science.gov (United States)

    Wang, Nani; Zhang, Qiaoyan; Xin, Hailiang; Shou, Dan; Qin, Luping

    2017-11-01

    A method using osteoblast membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry was developed to recognize and identify the specific active components from traditional Chinese medicines. Primary rat osteoblasts were used for the preparation of the stationary phase in the cell chromatography method. Retention components from the cell chromatography were collected and analyzed by liquid chromatography with time-of-flight mass spectrometry. This method was applied in screening active components from extracts of four traditional Chinese medicines. In total, 24 potentially active components with different structures were retained by osteoblast cell chromatography. There were five phenolic glucosides and one triterpenoid saponin from Curculigo orchioides Gaertn, two organic acids and ten flavonoids from Epimedium sagittatum Maxim, one phthalide compound and one organic acid from Angelica sinensis Diels, and two flavonoids and two saponins from Anemarrhena asphodeloides Bunge. Among those, four components (icariin, curculigoside, ferulaic acid, and timosaponin BII) were used for in vitro pharmacodynamics validation. They significantly increased the osteoblast proliferation, alkaline phosphatase activity, levels of bone gla protein and collagen type 1, and promoted mineralized nodule formation. The developed method was an effective screening method for finding active components from complex medicines that act on bone diseases. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

    2014-11-01

    An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. High temperature thermometric phosphors

    Science.gov (United States)

    Allison, Stephen W.; Cates, Michael R.; Boatner, Lynn A.; Gillies, George T.

    1999-03-23

    A high temperature phosphor consists essentially of a material having the general formula LuPO.sub.4 :Dy.sub.(x),Eu.sub.y) wherein: 0.1 wt %.ltoreq.x.ltoreq.20 wt % and 0.1 wt %.ltoreq.y.ltoreq.20 wt %. The high temperature phosphor is in contact with an article whose temperature is to be determined. The article having the phosphor in contact with it is placed in the environment for which the temperature of the article is to be determined. The phosphor is excited by a laser causing the phosphor to fluoresce. The emission from the phosphor is optically focused into a beam-splitting mirror which separates the emission into two separate emissions, the emission caused by the dysprosium dopant and the emission caused by the europium dopent. The separated emissions are optically filtered and the intensities of the emission are detected and measured. The ratio of the intensity of each emission is determined and the temperature of the article is calculated from the ratio of the intensities of the separate emissions.

  4. Characteristics of liquid product from the pyrolysis of waste plastic mixture at low and high temperatures: influence of lapse time of reaction.

    Science.gov (United States)

    Lee, Kyong-Hwan; Shin, Dae-Hyun

    2007-01-01

    Pyrolysis of a waste plastic mixture (high-density polyethylene: low-density polyethylene: polypropylene: polystyrene = 3:2:3:1) into a liquid product was carried out in a stirred semi-batch reactor at low (350 degrees C) and high (400 degrees C) temperatures. The effect of lapse time of reaction in the reactor and also degradation temperature on the characteristics of the liquid product from pyrolysis of the mixture was investigated. Liquid products were described by cumulative amount distribution, paraffin, olefin, naphthene and aromatic (PONA) distribution and molecular weight distribution. Their characteristic was quite differed with a lapse time of reaction and also at a low and high degradation temperatures, because of the different physicochemical properties of the plastic types in the mixture. With increase of lapse time of reaction, the order for the main products in PONA components obtained at 350 degrees C was firstly aromatic products and then olefin products, while at 400 degrees C the order was firstly aromatic products, then olefin products and finally paraffin products. The experiments also showed from the molecular weight distribution of liquid PONA components that the paraffin and olefin products had a wide distribution by mainly random scission of polymer, but in the case of olefin products were produced by an end-chain scission mechanism as well as random scission mechanism, as evidenced by much more light olefin products. This phenomenon was evident at a higher degradation temperature. Also, both the light olefin and naphthene products with a molecular weight of around 120, as a main product, showed a similar trend as a function of lapse time, which had a maximum fraction at 343 min (at 350 degrees C) and 83 min (at 400 degrees C). Among PONA components, the highest concentrations of aromatic products were obtained with a molecular weight of around 100 at the fastest lapse time of reaction, regardless of degradation temperature. It was

  5. Characteristics of liquid product from the pyrolysis of waste plastic mixture at low and high temperatures: Influence of lapse time of reaction

    International Nuclear Information System (INIS)

    Lee, Kyong-Hwan; Shin, Dae-Hyun

    2007-01-01

    Pyrolysis of a waste plastic mixture (high-density polyethylene: low-density polyethylene: polypropylene: polystyrene = 3:2:3:1) into a liquid product was carried out in a stirred semi-batch reactor at low (350 deg. C) and high (400 deg. C) temperatures. The effect of lapse time of reaction in the reactor and also degradation temperature on the characteristics of the liquid product from pyrolysis of the mixture was investigated. Liquid products were described by cumulative amount distribution, paraffin, olefin, naphthene and aromatic (PONA) distribution and molecular weight distribution. Their characteristic was quite differed with a lapse time of reaction and also at a low and high degradation temperatures, because of the different physicochemical properties of the plastic types in the mixture. With increase of lapse time of reaction, the order for the main products in PONA components obtained at 350 deg. C was firstly aromatic products and then olefin products, while at 400 deg. C the order was firstly aromatic products, then olefin products and finally paraffin products. The experiments also showed from the molecular weight distribution of liquid PONA components that the paraffin and olefin products had a wide distribution by mainly random scission of polymer, but in the case of olefin products were produced by an end-chain scission mechanism as well as random scission mechanism, as evidenced by much more light olefin products. This phenomenon was evident at a higher degradation temperature. Also, both the light olefin and naphthene products with a molecular weight of around 120, as a main product, showed a similar trend as a function of lapse time, which had a maximum fraction at 343 min (at 350 deg. C) and 83 min (at 400 deg. C). Among PONA components, the highest concentrations of aromatic products were obtained with a molecular weight of around 100 at the fastest lapse time of reaction, regardless of degradation temperature. It was concluded that the

  6. Fundamental studies on the switching in liquid nitrogen environment using vacuum switches for application in future high-temperature superconducting medium-voltage power grids

    International Nuclear Information System (INIS)

    Golde, Karsten

    2016-01-01

    By means of superconducting equipment it is possible to reduce the transmission losses in distribution networks while increasing the transmission capacity. As a result even saving a superimposed voltage level would be possible, which can put higher investment costs compared to conventional equipment into perspective. For operation of superconducting systems it is necessary to integrate all equipment in the cooling circuit. This also includes switchgears. Due to cooling with liquid nitrogen, however, only vacuum switching technology comes into question. Thus, the suitability of vacuum switches is investigated in this work. For this purpose the mechanics of the interrupters is considered first. Material investigations and switching experiments at ambient temperature and in liquid nitrogen supply information on potential issues. For this purpose, a special pneumatic construction is designed, which allows tens of thousands of switching cycles. Furthermore, the electrical resistance of the interrupters is considered. Since the contact system consists almost exclusively of copper, a remaining residual resistance and appropriate thermal losses must be considered. Since they have to be cooled back, an appropriate evaluation is given taking environmental parameters into account. The dielectric strength of vacuum interrupters is considered both at ambient temperature as well as directly in liquid nitrogen. For this purpose different contact distances are set at different interrupter types. A distinction is made between internal and external dielectric strength. Conditioning and deconditioning effects are minimized by an appropriate choice of the test circuit. The current chopping and resulting overvoltages are considered to be one of the few drawbacks of vacuum switching technology. Using a practical test circuit the height of chopping current is determined and compared for different temperatures. Due to strong scattering the evaluation is done using statistical methods. At

  7. Determination of the trace TBP in industrial feed liquid by gas chromatography

    International Nuclear Information System (INIS)

    Gao Yuehua; Jiang Junqing; Mu Ling; Yang Songtao

    2012-01-01

    The determination of the trace TBP in kerosene of the industrial feed liquid by gas chromatography is studied in the paper. It first takes the purification treatment for the kerosene containing trace TBP. The plutonium is removed by 0.2 mol/L ferrous sulfamate-1 mol/L nitric acid using the back-extraction. The uranium and the nitric acid in the organic phase are removed by the deionized water. The impurity which affect the measurement of the TBP and is harmful to the gas chromatograph are eliminated. Then the content of the TBP of the organic phase can be determined by gas chromatography. Results show that the measuring range of the content of the TBP is 0.02% ∼ 2%. The precision of the method is better than 5% and the recovery is between 95%∼106%. (authors)

  8. A method for fast determination of psoralens in oral solutions of phytomedicines using liquid chromatography.

    Science.gov (United States)

    Pires, Adriana Elias; Honda, Neli Kiko; Cardoso, Cláudia Andréa Lima

    2004-10-29

    A method for sample preparation and analysis by high performance liquid chromatography with UV detection (HPLC-UV) has been developed for routine analysis of psoralen and bergapten, photosensitizing compounds, in oral solutions of phytomedicines employed in Brazil for some illnesses. The linearity, accuracy, the inter- and intra-day precision of the procedure were evaluated. Calibration curves for psoralen and bergapten were linear in the range of 1.0-600.0 microg ml(-1) and 1.0-400.0 microg ml(-1) respectively. The recoveries of the psoralens in the oral solutions analysed were 94.43-99.97%. The percentage coefficient of variation (CV) of the quantitative analysis of the psoralens in the products analysis was within 5%. In inter-equipment study was employed gas chromatography-flame ionization (CG-FID) detection.

  9. Liquid Chromatography-Tandem Mass Spectrometry: An Emerging Technology in the Toxicology Laboratory.

    Science.gov (United States)

    Zhang, Yan Victoria; Wei, Bin; Zhu, Yu; Zhang, Yanhua; Bluth, Martin H

    2016-12-01

    In the last decade, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in routine toxicology laboratories. LC-MS/MS offers significant advantages over other traditional testing, such as immunoassay and gas chromatography-mass spectrometry methodologies. Major strengths of LC-MS/MS include improvement in specificity, flexibility, and sample throughput when compared with other technologies. Here, the basic principles of LC-MS/MS technology are reviewed, followed by advantages and disadvantages of this technology compared with other traditional techniques. In addition, toxicology applications of LC-MS/MS for simultaneous detection of large panels of analytes are presented. Copyright © 2016 Elsevier Inc. All rights reserved.

  10. Greening Reversed-Phase Liquid Chromatography Methods Using Alternative Solvents for Pharmaceutical Analysis

    Directory of Open Access Journals (Sweden)

    Moussa Yabré

    2018-05-01

    Full Text Available The greening of analytical methods has gained increasing interest in the field of pharmaceutical analysis to reduce environmental impacts and improve the health safety of analysts. Reversed-phase high-performance liquid chromatography (RP-HPLC is the most widely used analytical technique involved in pharmaceutical drug development and manufacturing, such as the quality control of bulk drugs and pharmaceutical formulations, as well as the analysis of drugs in biological samples. However, RP-HPLC methods commonly use large amounts of organic solvents and generate high quantities of waste to be disposed, leading to some issues in terms of ecological impact and operator safety. In this context, greening HPLC methods is becoming highly desirable. One strategy to reduce the impact of hazardous solvents is to replace classically used organic solvents (i.e., acetonitrile and methanol with greener ones. So far, ethanol has been the most often used alternative organic solvent. Others strategies have followed, such as the use of totally aqueous mobile phases, micellar liquid chromatography, and ionic liquids. These approaches have been well developed, as they do not require equipment investments and are rather economical. This review describes and critically discusses the recent advances in greening RP-HPLC methods dedicated to pharmaceutical analysis based on the use of alternative solvents.

  11. Assessing the detectability of antioxidants in two-dimensional high-performance liquid chromatography.

    Science.gov (United States)

    Bassanese, Danielle N; Conlan, Xavier A; Barnett, Neil W; Stevenson, Paul G

    2015-05-01

    This paper explores the analytical figures of merit of two-dimensional high-performance liquid chromatography for the separation of antioxidant standards. The cumulative two-dimensional high-performance liquid chromatography peak area was calculated for 11 antioxidants by two different methods--the areas reported by the control software and by fitting the data with a Gaussian model; these methods were evaluated for precision and sensitivity. Both methods demonstrated excellent precision in regards to retention time in the second dimension (%RSD below 1.16%) and cumulative second dimension peak area (%RSD below 3.73% from the instrument software and 5.87% for the Gaussian method). Combining areas reported by the high-performance liquid chromatographic control software displayed superior limits of detection, in the order of 1 × 10(-6) M, almost an order of magnitude lower than the Gaussian method for some analytes. The introduction of the countergradient eliminated the strong solvent mismatch between dimensions, leading to a much improved peak shape and better detection limits for quantification. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Study of mixed radiative thermal mass transfer in the case of spherical liquide particle evaporation in a high temperature thermal air plasma

    International Nuclear Information System (INIS)

    Garandeau, S.

    1984-01-01

    Radiative transfer in a semi-transparent non-isothermal medium with spherical configuration has been studied. Limit conditions have been detailed, among which the semi-transparent inner sphere case is a new case. Enthalpy and matter transfer equations related to these different cases have been established. An adimensional study of local conservation laws allowed to reveal a parameter set characteristic of radiation coupled phenomena thermal conduction, convection, diffusion. Transfer equations in the case of evaporation of a liquid spherical particle in an air thermal plasma have been simplified. An analytical solution for matter transfer is proposed. Numerical solution of radiative problems and matter transfer has been realized [fr

  13. Analysis of recombinant Schistosoma mansoni antigen rSmp28 by on-line liquid chromatography-mass spectrometry combined with sodium dodecyl sulfate polyacrylamide gel electrophoresis

    NARCIS (Netherlands)

    Klarskov, K.; Roecklin, D.; Bouchon, B.; Sabatie, J.; Van Dorsselaer, A.; Bischoff, Rainer

    1994-01-01

    A recombinant Schistosoma mansoni antigen produced in Saccharomyces cerevisiae and purified by glutathione-Sepharose affinity chromatography was analyzed by tryptic peptide mapping using on-line reversed-phase high-performance liquid chromatography pneumatically assisted electrospray mass

  14. Simultaneous Determination of Eight Bioactive Compounds in Dianthus superbus by High-performance Liquid Chromatography.

    Science.gov (United States)

    Yun, Bo-Ra; Yang, Hye Jin; Weon, Jin Bae; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

    2016-05-01

    Dianthus superbus, one of traditional herbal medicine, is widely used to treat urethritis, carbuncles and carcinoma. A simultaneous determination method was established for controlling the quality of D. superbus using the eight compounds, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1), diosmetin-7-O(2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), vanillic acid (3), 4-hydroxyphenyl acetic acid (4), 4-methoxyphenyl acetic acid (5), (E)-4-methoxycinnamic acid (6), 3-methoxy-4-hydroxyphenylethanol (7), and methyl hydroferulate (8) isolated from D. superbus. This analysis method was developed using high performance liquid chromatography coupled with diode array detector with a Shishedo C18 column at a column temperature of 3°C. The mobile phase was composed of 0.1% trifluoroacetic acid in water and acetonitrile. The flow rate was 1 ml/min and detection wavelength was set at 205 nm and 280 nm. Validation was performed in order to demonstrate selectivity, accuracy and precision of the method. The calibration curves showed good linearity (R (2) > 0.99). The limits of detection and limits of quantification were within the ranges 0.0159-0.6205 μg/ml and 0.3210-1.8802 μg/ml, respectively. Moreover, the relative standard deviations of intra- and inter-day precision were both Dianthus superbus was established by high performance liquid chromatography-diode array detectorDeveloped analysis method is validated with linearity, precious and accuracyThe newly established method was successfully evaluated contents of eight compounds in 12 D. superbus samples (D.1.D.12) from various regions and compared. Abbreviations used: HPLC: High performance liquid chromatography, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation.

  15. Comparison of liquid and supercritical fluid chromatography mobile phases for enantioselective separations on polysaccharide stationary phases.

    Science.gov (United States)

    Khater, Syame; Lozac'h, Marie-Anne; Adam, Isabelle; Francotte, Eric; West, Caroline

    2016-10-07

    Analysis and production of enantiomerically pure compounds is a major topic of interest when active pharmaceutical ingredients are concerned. Enantioselective chromatography has become a favourite both at the analytical and preparative scales. High-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC) are dominating the scene and are often seen as complementary techniques. Nowadays, for economic and ecologic reasons, SFC may be preferred over normal-phase HPLC (NPLC) as it allows significant reductions in solvent consumption. However, the transfer of NPLC methods to SFC is not always straightforward. In this study, we compare the retention of achiral molecules and separation of enantiomers under supercritical fluid (carbon dioxide with ethanol or isopropanol) and liquid normal-phase (heptane with ethanol or isopropanol) elution modes with polysaccharide stationary phases in order to explore the differences between the retention and enantioseparation properties between the two modes. Chemometric methods (namely quantitative structure-retention relationships and discriminant analysis) are employed to compare the results obtained on a large set of analytes (171 achiral probes and 97 racemates) and gain some understanding on the retention and separation mechanisms. The results indicate that, contrary to popular belief, carbon dioxide - solvent SFC mobile phases are often weaker eluents than liquid mobile phases. It appears that SFC and NPLC elution modes provide different retention mechanisms. While some enantioseparations are unaffected, facilitating the transfer between the two elution modes, other enantioseparations may be drastically different due to different types and strength of interactions contributing to enantioselectivity. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Integration of electrochemistry with ultra-performance liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Cai, Yi; Zheng, Qiuling; Liu, Yong; Helmy, Roy; Loo, Joseph A; Chen, Hao

    2015-01-01

    This study presents the development of ultra-performance liquid chromatography (UPLC) mass spectrometry (MS) combined with electrochemistry (EC) for the first time and its application for the structural analysis of proteins/peptides that contain disulfide bonds. In our approach, a protein/peptide mixture sample undergoes a fast UPLC separation and subsequent electrochemical reduction in an electrochemical flow cell followed by online MS and tandem mass spectrometry (MS/MS) analyses. The electrochemical cell is coupled to the mass spectrometer using our recently developed desorption electrospray ionization (DESI) interface. Using this UPLC/EC/DESI-MS method, peptides that contain disulfide bonds can be differentiated from those without disulfide bonds, as the former are electroactive and reducible. MS/MS analysis of the disulfide-reduced peptide ions provides increased information on the sequence and disulfide-linkage pattern. In a reactive DESI- MS detection experiment in which a supercharging reagent was used to dope the DESI spray solvent, increased charging was obtained for the UPLC-separated proteins. Strikingly, upon online electrolytic reduction, supercharged proteins (e.g., α-lactalbumin) showed even higher charging, which will be useful in top- down protein structure MS analysis as increased charges are known to promote protein ion dissociation. Also, the separation speed and sensitivity are enhanced by approximately 1(~)2 orders of magnitude by using UPLC for the liquid chromatography (LC)/EC/MS platform, in comparison to the previously used high- performance liquid chromatography (HPLC). This UPLC/EC/DESI-MS method combines the power of fast UPLC separation, fast electrochemical conversion, and online MS structural analysis for a potentially valuable tool for proteomics research and bioanalysis.

  17. High temperature structural silicides

    International Nuclear Information System (INIS)

    Petrovic, J.J.

    1997-01-01

    Structural silicides have important high temperature applications in oxidizing and aggressive environments. Most prominent are MoSi 2 -based materials, which are borderline ceramic-intermetallic compounds. MoSi 2 single crystals exhibit macroscopic compressive ductility at temperatures below room temperature in some orientations. Polycrystalline MoSi 2 possesses elevated temperature creep behavior which is highly sensitive to grain size. MoSi 2 -Si 3 N 4 composites show an important combination of oxidation resistance, creep resistance, and low temperature fracture toughness. Current potential applications of MoSi 2 -based materials include furnace heating elements, molten metal lances, industrial gas burners, aerospace turbine engine components, diesel engine glow plugs, and materials for glass processing

  18. High temperature materials characterization

    Science.gov (United States)

    Workman, Gary L.

    1990-01-01

    A lab facility for measuring elastic moduli up to 1700 C was constructed and delivered. It was shown that the ultrasonic method can be used to determine elastic constants of materials from room temperature to their melting points. The ease in coupling high frequency acoustic energy is still a difficult task. Even now, new coupling materials and higher power ultrasonic pulsers are being suggested. The surface was only scratched in terms of showing the full capabilities of either technique used, especially since there is such a large learning curve in developing proper methodologies to take measurements into the high temperature region. The laser acoustic system does not seem to have sufficient precision at this time to replace the normal buffer rod methodology.

  19. High temperature metallic recuperator

    Science.gov (United States)

    Ward, M. E.; Solmon, N. G.; Smeltzer, C. E.

    1981-06-01

    An industrial 4.5 MM Btu/hr axial counterflow recuperator, fabricated to deliver 1600 F combustion air, was designed to handle rapid cyclic loading, a long life, acceptable costs, and a low maintenance requirement. A cost benefit anlysis of a high temperature waste heat recovery system utilizing the recurperator and components capable of 1600 F combustion air preheat shows that this system would have a payback period of less than two years. Fifteen companies and industrial associations were interviewed and expressed great interest in recuperation in large energy consuming industries. Determination of long term environmental effects on candidate recuperator tubing alloys was completed. Alloys found to be acceptable in the 2200 F flue gas environment of a steel billet reheat furnace, were identified.

  20. Characterization of rhamnolipids by liquid chromatography/mass spectrometry after solid-phase extraction.

    Science.gov (United States)

    Behrens, Beate; Engelen, Jeannine; Tiso, Till; Blank, Lars Mathias; Hayen, Heiko

    2016-04-01

    Rhamnolipids are surface-active agents with a broad application potential that are produced in complex mixtures by bacteria of the genus Pseudomonas. Analysis from fermentation broth is often characterized by laborious sample preparation and requires hyphenated analytical techniques like liquid chromatography coupled to mass spectrometry (LC-MS) to obtain detailed information about sample composition. In this study, an analytical procedure based on chromatographic method development and characterization of rhamnolipid sample material by LC-MS as well as a comparison of two sample preparation methods, i.e., liquid-liquid extraction and solid-phase extraction, is presented. Efficient separation was achieved under reversed-phase conditions using a mixed propylphenyl and octadecylsilyl-modified silica gel stationary phase. LC-MS/MS analysis of a supernatant from Pseudomonas putida strain KT2440 pVLT33_rhlABC grown on glucose as sole carbon source and purified by solid-phase extraction revealed a total of 20 congeners of di-rhamnolipids, mono-rhamnolipids, and their biosynthetic precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) with different carbon chain lengths from C8 to C14, including three rhamnolipids with uncommon C9 and C11 fatty acid residues. LC-MS and the orcinol assay were used to evaluate the developed solid-phase extraction method in comparison with the established liquid-liquid extraction. Solid-phase extraction exhibited higher yields and reproducibility as well as lower experimental effort.

  1. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Science.gov (United States)

    Çabuk, Hasan; Köktürk, Mustafa

    2013-01-01

    A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

  2. Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hasan Çabuk

    2013-01-01

    Full Text Available A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries.

  3. Determination of alpha-Tocopherol (vitamin E) in irradiated garlic by high performance liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rios, Magda Dias Goncalves; Penteado, Marilene de Vuono Camargo

    2003-01-01

    The effects of 60 Co ionizing radiations in doses of 0, 75, 100, 150, 200 and 250Gy on garlic, upon the α-tocopherol concentration were studied. The α-tocopherol contents were established by high performance liquid chromatography (HPLC), after direct hexane extraction from the garlic samples. The α-tocopherol was determined through normal phase column, and mobile phase was composed by hexane: iso-propyl alcohol (99:01 v/v), with 2mL/min flow rate and fluorescence detector. It is statistically shown that an irradiation dose of up to 150 Gy does not affect the garlic α-tocopherol content. (author)

  4. Determination of boron in uranium and aluminium by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rao, Radhika M.; Aggarwal, S.K.

    2003-01-01

    Experiments were conducted for the determination of boron in U 3 O 8 powder and aluminium metal using dynamically modified reversed phase high pressure liquid chromatography (RP-HPLC) and using precolumn chromogenic agent viz. curcumin for complexing boron. The complex was separated from the excess of reagent and determined by HPLC. The boron curcumin complex (rosocyanin) was formed after extraction of boron with 2-ethyl-1,3-hexane diol (EHD). Linear calibration curves for boron amounts in the range of 0.02 μg to 0.5 μg were developed and used for the determination of boron in aluminium and uranium samples. (author)

  5. Determination of 1-hydroxypyrene in human urine by high-performance liquid chromatography

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Poulsen, O M; Christensen, J M

    1993-01-01

    A high-performance liquid chromatography (HPLC)/fluorescence method for quantitative analysis of 1-hydroxypyrene in urine was developed. The method validation analysis showed the method to be in analytical control. No significant systematical errors could be demonstrated. The entire run time....... The developed method is presently used for measurement of 1-hydroxypyrene in urine samples from workers exposed to a low airborne level of polycyclic aromatic hydrocarbons, generally less than 25 micrograms/m3. The urine samples of exposed workers (n = 122) showed a range of 1-hydroxypyrene from the limit...

  6. Increasing flexibility in two-dimensional liquid chromatography by pulsed elution of the first dimension

    DEFF Research Database (Denmark)

    Jakobsen, Simon S.; Christensen, Jan H.; Verdier, Sylvain

    2017-01-01

    This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension...... online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity...

  7. Derivatization reagents in liquid chromatography/electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Santa, Tomofumi

    2011-01-01

    Liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) is one of the most prominent analytical techniques owing to its inherent selectivity and sensitivity. In LC/ESI-MS/MS, chemical derivatization is often used to enhance the detection sensitivity. Derivatization improves the chromatographic separation, and enhances the mass spectrometric ionization efficiency and MS/MS detectability. In this review, an overview of the derivatization reagents which have been applied to LC/ESI-MS/MS is presented, focusing on the applications to low molecular weight compounds. 2010 John Wiley & Sons, Ltd.

  8. Denaturing high-performance liquid chromatography mutation analysis in patients with reduced Protein S levels

    DEFF Research Database (Denmark)

    Bathum, Lise; Münster, Anna-Marie; Nybo, Mads

    2008-01-01

    diagnosis and risk estimation. The aim was to design a high-throughput genetic analysis based on denaturing high-performance liquid chromatography to identify sequence variations in the gene coding for Protein S. PATIENTS: In total, 55 patients referred to the Section of Thrombosis and Haemostasis, Odense......BACKGROUND: Patients with congenital Protein S deficiency have increased risk of venous thromboembolism. However, Protein S levels show large intra-individual variation and the biochemical assays have low accuracy and a high interlaboratory variability. Genetic analysis might aid in a more precise......, giving a precise diagnosis and subsequently a better risk estimation....

  9. Determination of limonin and nomilin contents in different citrus cultivars using high performance liquid chromatography

    International Nuclear Information System (INIS)

    Bilal, H.; Hassan, S.; Sahar, S.; Akram, W.; Sahar, S.

    2013-01-01

    High perlorrnance liquid chromatography (HPLC) analysis was done to quantify the amount of limonoids (nomilin and nomilin) in seven selected citrus cultivars. According to the HPLC analysis red blood orange (Citrus sinensis var red blood orange) had maximum amount of limonin (479.77 ug/rnl.), while rough lemon (Citrus jambhiri) had no limonin content. in case of nomonin, rough lemon (Citrus jambhir) had maximum amount of nomilin (54.23 micro g/ML)) while succari (citrus sinensis var succari) had very low amount of nomilin (0.37 micro g/Ml). (author)

  10. Determination of 90SR in food using extraction chromatography and LSC - Liquid Scintillation Counting

    International Nuclear Information System (INIS)

    Temba, Eliane S.C.; Amaral, Angela M.; Reis Junior, Aluisio S.; Monteiro, Roberto P.G.

    2013-01-01

    A methodology for the determination of 90 Sr in food is described. The procedure involved a preliminary freeze-drying of the samples followed by dry-ashing and sample digestion. The separation procedure was carried out using extraction chromatography with Sr Resin, from Eichrom, and 90 Sr was measured by liquid scintillation counting (LSC). A certified reference material, IAEA-375, was analyzed in order to evaluate the reliability of the method, and the results showed good agreement between the measured and certified values. The chemical yield was above 90% and the typical counting efficiency was 82%. The calculated limit of detection was 4.8 x 10 -3 Bq g -1 . (author)

  11. Hb A1c Separation by High Performance Liquid Chromatography in Hemoglobinopathies

    OpenAIRE

    Chandrashekar, Vani

    2016-01-01

    Hb A1c measurement is subject to interference by hemoglobin traits and this is dependent on the method used for determination. In this paper we studied the difference between Hb A1c measured by HPLC in hemoglobin traits and normal chromatograms. We also studied the correlation of Hb A1c with age. Hemoglobin analysis was carried out by high performance liquid chromatography. Spearman's rank correlation was used to study correlation between A1c levels and age. Mann-Whitney U test was used to st...

  12. Chiral separation of pharmaceutical compounds using electrochemically modulated liquid chromatography (EMLC)

    Energy Technology Data Exchange (ETDEWEB)

    Wang, S. [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    This research explores the application of a new technique, termed electrochemically modulated liquid chromatography (EMLC), to the chiral separations of pharmaceutical compounds. The introduction section provides a literature review of the technique and its applications, as well as brief overview of the research described in each of the next two chapters. Chapter 2 investigates the EMLC-based enantiomeric separation of a group of chiral benzodiazepines with β-cyclodextrin as a chiral mobile phase additive. Chapter 3 demonstrates the effects of several experimental parameters on the separation efficiency of drug enantiomers. The author concludes with a general summary and possible directions for future studies. Chapters 2 and 3 are processed separately.

  13. Determination of sulfonamides in meat by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry

    International Nuclear Information System (INIS)

    Kim, Dal Ho; Choi, Jong Oh; Kim, Jin Seog; Lee, Dai Woon

    2002-01-01

    Liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) has been used for the determination of sulfonamides in meat. Five typical sulfonamides were selected as target compounds, and beef meat was selected as a matrix sample. As internal standards, sulfapyridine and isotope labeled sulfamethazine ( 13 C 6 -SMZ) were used. Compared to the results of recent reports, our results have shown improved precision to a RSD of 1.8% for the determination of sulfamethazine spiked with 75 ng/g level in meat

  14. High-performance liquid chromatography of rat and mouse islet polypeptides

    DEFF Research Database (Denmark)

    Linde, S; Hansen, B; Welinder, B S

    1990-01-01

    After preparative high-performance liquid chromatography of mouse islet culture medium, concentrated on disposable C18 cartridges (Sep-Pak), an unexpected insulin immunoreactive peak eluting earlier than mouse insulin I and II was detected. Molecular mass determination by mass spectrometry...... on the buffer, the organic modifier and the procedure. In particular the use of methanol-trifluoroacetic acid resulted in extensive oxidation. The oxidation could be minimized by adding 2 mM dithiothreitol to the buffer and by degassing and/or nitrogen-bubbling of the buffer. Minimal formation of Met...

  15. Separation and identification of corticosterone metabolites by liquid chromatography--electrospray ionization mass spectrometry.

    Science.gov (United States)

    Miksík, I; Vylitová, M; Pácha, J; Deyl, Z

    1999-04-16

    High-performance liquid chromatography coupled to atmospheric pressure ionization-electrospray ionization mass spectrometry (API-ESI-MS) was investigated for the analysis of corticosterone metabolites; their characterization was obtained by combining the separation on Zorbax Eclipse XDB C18 column (eluted with a methanol-water-acetic acid gradient) with identification using positive ion mode API-ESI-MS and selected ion analysis. The applicability of this method was verified by monitoring the activity of steroid converting enzymes (20beta-hydroxysteroid dehydrogenase and 11beta-hydroxysteroid dehydrogenase) in avian intestines.

  16. Quantification of glibenclamide in cleaning samples of pharmaceutical equipment through high performance liquid chromatography

    International Nuclear Information System (INIS)

    Baeza Fonte, Alen Nils; Diaz Aguila, Elsa Eneida; Martinez Alfonso; Nancy

    2012-01-01

    to submit a selective analytical method for quantization of glibenclamide in cleaning samples of pharmaceutical equipment using high performance liquid chromatography. The mobile phase consisted of an equal mixing of acetonitrile/phosphate buffer KH 2 PO 4 ; with 0.037 mol/L concentration pH 5.25 and flow of 1.5 mL/min, in a Nucleosil 100 C8 column. Glibenclamide was injected with progesterone as internal standard and using an UV detector= 230 nm

  17. Application of High Temperature Superconductors to Accelerators

    CERN Document Server

    Ballarino, A

    2000-01-01

    Since the discovery of high temperature superconductivity, a large effort has been made by the scientific community to investigate this field towards a possible application of the new oxide superconductors to different devices like SMES, magnetic bearings, flywheels energy storage, magnetic shielding, transmission cables, fault current limiters, etc. However, all present day large scale applications using superconductivity in accelerator technology are based on conventional materials operating at liquid helium temperatures. Poor mechanical properties, low critical current density and sensitivity to the magnetic field at high temperature are the key parameters whose improvement is essential for a large scale application of high temperature superconductors to such devices. Current leads, used for transferring currents from the power converters, working at room temperature, into the liquid helium environment, where the magnets are operating, represent an immediate application of the emerging technology of high t...

  18. High temperature materials and mechanisms

    CERN Document Server

    2014-01-01

    The use of high-temperature materials in current and future applications, including silicone materials for handling hot foods and metal alloys for developing high-speed aircraft and spacecraft systems, has generated a growing interest in high-temperature technologies. High Temperature Materials and Mechanisms explores a broad range of issues related to high-temperature materials and mechanisms that operate in harsh conditions. While some applications involve the use of materials at high temperatures, others require materials processed at high temperatures for use at room temperature. High-temperature materials must also be resistant to related causes of damage, such as oxidation and corrosion, which are accelerated with increased temperatures. This book examines high-temperature materials and mechanisms from many angles. It covers the topics of processes, materials characterization methods, and the nondestructive evaluation and health monitoring of high-temperature materials and structures. It describes the ...

  19. Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

    Science.gov (United States)

    Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

    2015-06-01

    A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Systematic evaluation of matrix effects in hydrophilic interaction chromatography versus reversed phase liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Periat, Aurélie; Kohler, Isabelle; Thomas, Aurélien; Nicoli, Raul; Boccard, Julien; Veuthey, Jean-Luc; Schappler, Julie; Guillarme, Davy

    2016-03-25

    Reversed phase liquid chromatography (RPLC) coupled to mass spectrometry (MS) is the gold standard technique in bioanalysis. However, hydrophilic interaction chromatography (HILIC) could represent a viable alternative to RPLC for the analysis of polar and/or ionizable compounds, as it often provides higher MS sensitivity and alternative selectivity. Nevertheless, this technique can be also prone to matrix effects (ME). ME are one of the major issues in quantitative LC-MS bioanalysis. To ensure acceptable method performance (i.e., trueness and precision), a careful evaluation and minimization of ME is required. In the present study, the incidence of ME in HILIC-MS/MS and RPLC-MS/MS was compared for plasma and urine samples using two representative sets of 38 pharmaceutical compounds and 40 doping agents, respectively. The optimal generic chromatographic conditions in terms of selectivity with respect to interfering compounds were established in both chromatographic modes by testing three different stationary phases in each mode with different mobile phase pH. A second step involved the assessment of ME in RPLC and HILIC under the best generic conditions, using the post-extraction addition method. Biological samples were prepared using two different sample pre-treatments, i.e., a non-selective sample clean-up procedure (protein precipitation and simple dilution for plasma and urine samples, respectively) and a selective sample preparation, i.e., solid phase extraction for both matrices. The non-selective pretreatments led to significantly less ME in RPLC vs. HILIC conditions regardless of the matrix. On the contrary, HILIC appeared as a valuable alternative to RPLC for plasma and urine samples treated by a selective sample preparation. Indeed, in the case of selective sample preparation, the compounds influenced by ME were different in HILIC and RPLC, and lower and similar ME occurrence was generally observed in RPLC vs. HILIC for urine and plasma samples

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD 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.

  3. High-temperature superconductivity

    International Nuclear Information System (INIS)

    Lynn, J.W.

    1990-01-01

    This book discusses development in oxide materials with high superconducting transition temperature. Systems with Tc well above liquid nitrogen temperature are already a reality and higher Tc's are anticipated. The author discusses how the idea of a room-temperature superconductor appears to be a distinctly possible outcome of materials research

  4. Use of liquid chromatography for measuring atmospheric sulfur dioxide and nitrogen oxide

    Energy Technology Data Exchange (ETDEWEB)

    Benova, E

    1973-02-01

    A literature search to ascertain the applicability of liquid chromatography to the analysis of atmospheric sulfur dioxide and various oxides of nitrogen is reported. Simple or enriched samples can be analyzed. Plastic bags are recommended for preparation of simple samples; and a table of 18 plastic materials, their manufacturers, and pollutants to which they are inert is provided. Enriched samples can be prepared in chromatographic columns by adsorption methods. Tables are provided listing carriers, stationary phase materials, temperatures, carrier liquids (helium or nitrogen), column dimensions, and other data recommended for chromatographic tests of SO/sub 2/ and NOx. Because of its reactivity and tendency to polymerize, sulfur trioxide should be reduced to SO/sub 2/ prior to analysis.

  5. A simple high performance liquid chromatography method for analyzing paraquat in soil solution samples.

    Science.gov (United States)

    Ouyang, Ying; Mansell, Robert S; Nkedi-Kizza, Peter

    2004-01-01

    A high performance liquid chromatography (HPLC) method with UV detection was developed to analyze paraquat (1,1'-dimethyl-4,4'-dipyridinium dichloride) herbicide content in soil solution samples. The analytical method was compared with the liquid scintillation counting (LSC) method using 14C-paraquat. Agreement obtained between the two methods was reasonable. However, the detection limit for paraquat analysis was 0.5 mg L(-1) by the HPLC method and 0.05 mg L(-1) by the LSC method. The LSC method was, therefore, 10 times more precise than the HPLC method for solution concentrations less than 1 mg L(-1). In spite of the high detection limit, the UC (nonradioactive) HPLC method provides an inexpensive and environmentally safe means for determining paraquat concentration in soil solution compared with the 14C-LSC method.

  6. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  7. Simultaneous determination of 9 heterocyclic aromatic amines in pork products by liquid chromatography coupled with triple quadrupole tandem mass spectrometry

    Science.gov (United States)

    Shen, X. C.; Zhang, Y. L.; Cui, Y. Q.; Xu, L. Y.; Li, X.; Qi, J. H.

    2017-07-01

    Heterocyclic aromatic amines (HAAs) are potent mutagens that formed at high temperature in cooked, protein-rich food. Owing to their frequent intake, an accurate method is essential to access human health risk of HAAs exposure through detecting these compounds in various heat-treated meat products. In this study, a liquid chromatography-electrospray tandem mass spectrometry (LC--ESI-MS/MS) method was developed to perform the determination of 9 mutagenic heterocyclic amines (HAAs) in meat samples with multiple reaction monitoring (MRM) mode. Ultrasound assisted extraction and diatomaceous earth was employed to extract HAAs from food samples, and the analytes were purified and enriched using tandem solid phase extraction, with propyl sulfonic acid coupled to a C18 cartridge. Two parameters, extraction time and eluent, were carefully optimized to improve the extraction and purification efficiency. The LC separation was carried out using a Zorbax SB-C18 (3.5 μm particle size, 2.1 × 150 mm i.d.) column and optimized some parameters, such as pH, concentration and volume. Under the optimal experimental conditions, recoveries ranged from 52.97% to 97.11% with good quality parameters: limit of detection values between 0.02 and 0.24 ng mL-1, linearity (R2>0.998), and run-to-run and day-to-day precisions lower than 9.81% achieved. To evaluate the performance of the method in high throughput analysis of complex meat samples, the LC-MS/MS method was applied to the analysis of HAAs in three food samples, and the results demonstrated that the method can be used for the trace determination of HAAs in pork samples.

  8. A Search for Amino Acids and Nucleobases in the Martian Meteorite Roberts Massif 04262 Using Liquid Chromatography-Mass Spectrometry

    Science.gov (United States)

    Callahan, Michael P.; Burton, Aaron S.; Elsila, Jamie E.; Baker, Eleni M.; Smith, Karen E.; Glavin, Daniel P.; Dworkin, Jason P.

    2013-01-01

    The investigation into whether Mars contains signatures of past or present life is of great interest to science and society. Amino acids and nucleobases are compounds that are essential for all known life on Earth and are excellent target molecules in the search for potential Martian biomarkers or prebiotic chemistry. Martian meteorites represent the only samples from Mars that can be studied directly in the laboratory on Earth. Here, we analyzed the amino acid and nucleobase content of the shergottite Roberts Massif (RBT) 04262 using liquid chromatography-mass spectrometry. We did not detect any nucleobases above our detection limit in formic acid extracts; however, we did measure a suite of protein and nonprotein amino acids in hot-water extracts with high relative abundances of beta-alanine and gamma-amino-eta-butyric acid. The presence of only low (to absent) levels of several proteinogenic amino acids and a lack of nucleobases suggest that this meteorite fragment is fairly uncontaminated with respect to these common biological compounds. The distribution of straight-chained amine-terminal eta-omega-amino acids in RBT 04262 resembled those previously measured in thermally altered carbonaceous meteorites. A carbon isotope ratio of -24(0/00) +/- 6(0/00) for beta-alanine in RBT 04262 is in the range of reduced organic carbon previously measured in Martian meteorites (Steele et al. 2012). The presence of eta-omega-amino acids may be due to a high temperature Fischer-Tropschtype synthesis during igneous processing on Mars or impact ejection of the meteorites from Mars, but more experimental data are needed to support these hypotheses.

  9. Screening antiallergic components from Carthamus tinctorius using rat basophilic leukemia 2H3 cell membrane chromatography combined with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Han, Shengli; Huang, Jing; Cui, Ronghua; Zhang, Tao

    2015-02-01

    Carthamus tinctorius, used in traditional Chinese medicine, has many pharmacological effects, such as anticoagulant effects, antioxidant effects, antiaging effects, regulation of gene expression, and antitumor effects. However, there is no report on the antiallergic effects of the components in C. tinctorius. In the present study, we investigated the antiallergic components of C. tinctorius and its mechanism of action. A rat basophilic leukemia 2H3/cell membrane chromatography coupled online with high-performance liquid chromatography and tandem mass spectrometry method was developed to screen antiallergic components from C. tinctorius. The screening results showed that Hydroxysafflor yellow A, from C. tinctorius, was the targeted component that retained on the rat basophilic leukemia 2H3/cell membrane chromatography column. We measured the amount of β-hexosaminidase and histamine released in mast cells and the key markers of degranulation. The release assays showed that Hydroxysafflor yellow A could attenuate the immunoglobulin E induced release of allergic cytokines without affecting cell viability from 1.0 to 50.0 μM. In conclusion, the established rat basophilic leukemia 2H3 cell membrane chromatography coupled with online high-performance liquid chromatography and tandem mass spectrometry method successfully screened and identified Hydroxysafflor yellow A from C. tinctorius as a potential antiallergic component. Pharmacological analysis elucidated that Hydroxysafflor yellow A is an effective natural component for inhibiting immunoglobulin E-antigen-mediated degranulation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2016-04-01

    In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Purification of lignans from Fructus Arctii using off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography.

    Science.gov (United States)

    Yang, Bichao; Xin, Huaxia; Wang, Feier; Cai, Jianfeng; Liu, Yanfang; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-08-01

    As a common traditional Chinese medicine, Fructus Arctii has important clinical medical values. Its main components are lignans, which are difficult to separate and analyze because of the complex composition, similar chemical structures, and close properties. In this study, an off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method, as well as an effective sample pretreatment method based on hydrophilic interaction chromatography material, was developed to enrich the minor lignan fractions and obtain high-purity compounds. In total, 12 high-purity compounds were isolated from Fructus Arctii. Their structures were identified by using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy, which showed that all were lignans and that most of them were isomers. The results demonstrated the effective off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method for the purification of lignans from Fructus Arctii. The separation protocol established here will be beneficial for the separation of complex samples from other kinds of natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Quantification of steroid hormones in human serum by liquid chromatography-high resolution tandem mass spectrometry.

    Science.gov (United States)

    Matysik, Silke; Liebisch, Gerhard

    2017-12-01

    A limited specificity is inherent to immunoassays for steroid hormone analysis. To improve selectivity mass spectrometric analysis of steroid hormones by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been introduced in the clinical laboratory over the past years usually with low mass resolution triple-quadrupole instruments or more recently by high resolution mass spectrometry (HR-MS). Here we introduce liquid chromatography-high resolution tandem mass spectrometry (LC-MS/HR-MS) to further increase selectivity of steroid hormone quantification. Application of HR-MS demonstrates an enhanced selectivity compared to low mass resolution. Separation of isobaric interferences reduces background noise and avoids overestimation. Samples were prepared by automated liquid-liquid extraction with MTBE. The LC-MS/HR-MS method using a quadrupole-Orbitrap analyzer includes eight steroid hormones i.e. androstenedione, corticosterone, cortisol, cortisone, 11-deoxycortisol, 17-hydroxyprogesterone, progesterone, and testosterone. It has a run-time of 5.3min and was validated according to the U.S. Food and Drug Administration (FDA) and the European Medicines Agency (EMA) guidelines. For most of the analytes coefficient of variation were 10% or lower and LOQs were determined significantly below 1ng/ml. Full product ion spectra including accurate masses substantiate compound identification by matching their masses and ratios with authentic standards. In summary, quantification of steroid hormones by LC-MS/HR-MS is applicable for clinical diagnostics and holds also promise for highly selective quantification of other small molecules. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Simultaneous drug identification in urine of sexual assault victims by using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Lee, Hei Hwa; Chen, Suen Chi; Lee, Jong Feng; Lin, Hsin Yu; Chen, Bai Hsiun

    2018-01-01

    According to domestic and international epidemiological investigation, the proportion of substance involved sexual assault has the trend of ascent. In the past, laboratory methods that investigated urine sample of the sexual assault victims was to screen with enzyme immunoassay and then confirmed with mass spectrometry. The objective of the study is to simultaneously identify abused drugs in 126 decoded urine samples of sexual assault victims by liquid chromatography tandem mass spectrometry. The instrument was operated in multiple-reaction monitoring with an electro-spray positive ionization mode. Chromatograms were separated with ACE5 C18 column on a gradient of acetonitrile. After liquid-liquid extraction, samples were passed through a 0.22μm PVDF filter before injection into the system. The limits of quantitation ranged from 0.2 to 10ng/mL. The precision (CV) results were below 12.9% (intraday) and 15.0% (interday). The intraday accuracy ranged from 84.8 to 121.0%, interday accuracy ranged from 72.0 to 117.3%. We found that 29 (23.0%) were positive for drugs. The most common drug identified is flunitrazepam (11.1%), followed by nimetazepam and ketamine (7.9%), some new psychoactive substances, such as 2C-B, mephedrone, methylone, PMA and PMMA were also identified. We identified abused drugs, benzodiazepines, and new psychoactive substances in urine of sexual assault victims by using liquid chromatography tandem mass spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Carbon nanoparticles from corn stalk soot and its novel application as stationary phase of hydrophilic interaction chromatography and per aqueous liquid chromatography

    International Nuclear Information System (INIS)

    Li Yuanyuan; Xu Luan; Chen Tong; Liu Xiaoyan; Xu Zhigang; Zhang Haixia

    2012-01-01

    Highlights: ► Carbon nanoparticles (6–18 nm in size) were prepared from corn stalk soot. ► CNPs-based silica were used as novel chromatography stationary phase. ► The new phase shows good separation selectivity for polar compounds. ► The new phase had the similar retention for polar probes in HILIC and PALC modes. ► In contrast to PALC, under HILIC conditions high efficiencies were achieved. - Abstract: Carbon nanoparticles (CNPs) (6–18 nm in size) were prepared by refluxing corn stalk soot in nitric acid. The obtained acid-oxidized CNPs are soluble in water due to the existence of carboxylic and hydroxyl groups. 13 C NMR measurement shows the CNPs are mainly of sp 2 and sp 3 carbon structure different from CNPs obtained from candle soot and natural gas soot. Furthermore, these CNPs exhibit unique photoluminescence properties. Interestingly, the CNPs might be exploited to immobilize on the surface of porous silica particles as chromatographic stationary phase. The resultant packing material was evaluated by high-performance liquid chromatography, indicating that the new stationary phase could be used in hydrophilic interaction liquid chromatography (HILIC) and per aqueous liquid chromatography (PALC) modes. The separation of five nucleosides, four sulfa compounds and safflower injection was achieved by using the new column in the HILIC and PALC modes, respectively.

  15. Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography.

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Une, Hemant Devidas

    2016-01-01

    In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida.

  16. Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Une, Hemant Devidas

    2016-01-01

    Objective: In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. Materials and Methods: In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. Results: HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. Conclusion: The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. SUMMARY Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida PMID:26941534

  17. Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

    Science.gov (United States)

    Liu, Zhongling; Yu, Wei; Zhang, Hanqi; Gu, Fanbin; Jin, Xiangqun

    2016-12-01

    Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL -1 , respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. A high pressure liquid chromatography method for separation of prolactin forms.

    Science.gov (United States)

    Bell, Damon A; Hoad, Kirsten; Leong, Lillian; Bakar, Juwaini Abu; Sheehan, Paul; Vasikaran, Samuel D

    2012-05-01

    Prolactin has multiple forms and macroprolactin, which is thought not to be bioavailable, can cause a raised serum prolactin concentration. Gel filtration chromatography (GFC) is currently the gold standard method for separating macroprolactin, but is labour-intensive. Polyethylene glycol (PEG) precipitation is suitable for routine use but may not always be accurate. We developed a high pressure liquid chromatography (HPLC) assay for macroprolactin measurement. Chromatography was carried out using an Agilent Zorbax GF-250 (9.4 × 250 mm, 4 μm) size exclusion column and 50 mmol/L Tris buffer with 0.15 mmol/L NaCl at pH 7.2 as mobile phase, with a flow rate of 1 mL/min. Serum or plasma was diluted 1:1 with mobile phase and filtered and 100 μL injected. Fractions of 155 μL were collected for prolactin measurement and elution profile plotted. The area under the curve of each prolactin peak was calculated to quantify each prolactin form, and compared with GFC. Clear separation of monomeric-, big- and macroprolactin forms was achieved. Quantification was comparable to GFC and precision was acceptable. Total time from injection to collection of the final fraction was 16 min. We have developed an HPLC method for quantification of macroprolactin, which is rapid and easy to perform and therefore can be used for routine measurement.

  19. Enhanced fluidity liquid chromatography of inulin fructans using ternary solvent strength and selectivity gradients.

    Science.gov (United States)

    Bennett, Raffeal; Olesik, Susan V

    2018-01-25

    The value of exploring selectivity and solvent strength ternary gradients in enhanced fluidity liquid chromatography (EFLC) is demonstrated for the separation of inulin-type fructans from chicory. Commercial binary pump systems for supercritical fluid chromatography only allow for the implementation of ternary solvent strength gradients which can be restrictive for the separation of polar polymeric analytes. In this work, a custom system was designed to extend the capability of EFLC to allow tuning of selectivity or solvent strength in ternary gradients. Gradient profiles were evaluated using the Berridge function (RF 1 ), normalized resolution product (NRP), and gradient peak capacity (P c ). Selectivity gradients provided the separation of more analytes over time. The RF 1 function showed favor to selectivity gradients with comparable P c to that of solvent strength gradients. NRP did not strongly correlate with P c or RF 1 score. EFLC with the hydrophilic interaction chromatography, HILIC, separation mode was successfully employed to separate up to 47 fructan analytes in less than 25 min using a selectivity gradient. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Gupta, V K; Jain, Rajeev; Lukram, Ojitkumar; Agarwal, Shilpi; Dwivedi, Ashish

    2011-01-15

    A rapid and sensitive liquid chromatography tandem mass spectrometry method has been developed and validated for the simultaneous determination of ramipril, ramiprilat and telmisartan in human plasma. The solid-phase extraction technique was used for the extraction of ramipril, ramiprilat and telmisartan from human plasma. Trandolaprilat and hydrochlorothiazide were used as the internal standards (ISs). Chromatography was performed on a Hypurity C18, 5 μm, 50 mm × 4.6mm column, with the mobile phase consisting of ammonium acetate and acetonitrile (in a 20:80 ratio), followed by detection using mass spectrometry. The method involves a simple reversed isocratic chromatography condition and mass spectrometry detection, which enables detection at sub-nanogram levels. The method was validated and the lower limit of quantification for ramipril, ramiprilat and telmisartan was found to be 0.1 ng mL(-1), 0.1 ng mL(-1) and 2 ng mL(-1), respectively. The mean recovery for ramipril, ramiprilat and telmisartan ranged from 90.1 to 104.1%. This method increased the sensitivity and selectivity; resulting in high-throughput analysis of ramipril, ramiprilat and telmisartan using two different ISs in a single experiment for bioequivalence studies, with a chromatographic run time of 1.5 min only. Copyright © 2010 Elsevier B.V. All rights reserved.

  1. High temperature interface superconductivity

    International Nuclear Information System (INIS)

    Gozar, A.; Bozovic, I.

    2016-01-01

    Highlight: • This review article covers the topic of high temperature interface superconductivity. • New materials and techniques used for achieving interface superconductivity are discussed. • We emphasize the role played by the differences in structure and electronic properties at the interface with respect to the bulk of the constituents. - Abstract: High-T_c superconductivity at interfaces has a history of more than a couple of decades. In this review we focus our attention on copper-oxide based heterostructures and multi-layers. We first discuss the technique, atomic layer-by-layer molecular beam epitaxy (ALL-MBE) engineering, that enabled High-T_c Interface Superconductivity (HT-IS), and the challenges associated with the realization of high quality interfaces. Then we turn our attention to the experiments which shed light on the structure and properties of interfacial layers, allowing comparison to those of single-phase films and bulk crystals. Both ‘passive’ hetero-structures as well as surface-induced effects by external gating are discussed. We conclude by comparing HT-IS in cuprates and in other classes of materials, especially Fe-based superconductors, and by examining the grand challenges currently laying ahead for the field.

  2. High-temperature uncertainty

    International Nuclear Information System (INIS)

    Timusk, T.

    2005-01-01

    Recent experiments reveal that the mechanism responsible for the superconducting properties of cuprate materials is even more mysterious than we thought. Two decades ago, Georg Bednorz and Alex Mueller of IBM's research laboratory in Zurich rocked the world of physics when they discovered a material that lost all resistance to electrical current at the record temperature of 36 K. Until then, superconductivity was thought to be a strictly low-temperature phenomenon that required costly refrigeration. Moreover, the IBM discovery - for which Bednorz and Mueller were awarded the 1987 Nobel Prize for Physics - was made in a ceramic copper-oxide material that nobody expected to be particularly special. Proposed applications for these 'cuprates' abounded. High-temperature superconductivity, particularly if it could be extended to room temperature, offered the promise of levitating trains, ultra-efficient power cables, and even supercomputers based on superconducting quantum interference devices. But these applications have been slow to materialize. Moreover, almost 20 years on, the physics behind this strange state of matter remains a mystery. (U.K.)

  3. State-of-the art of selective detection and identification of I-, Br-, Cl-, and F-containing compounds in gas chromatography and liquid chromatography.

    Science.gov (United States)

    Brede, Cato; Pedersen-Bjergaard, Stig

    2004-09-24

    This review article presents an overview of halogen-specific detection in gas chromatography (GC) and liquid chromatography (LC). Attention is primarily focused on the use of plasma emission spectroscopy and plasma mass spectrometry as detectors, but other halogen-selective detection principles are also mentioned. Different instrumental configurations are discussed both with respect to technical set-up and performance, the principal reasons for halogen-selective detection are highlighted, and recent applications are reviewed from areas such as environmental chemistry, petroleum characterization, and drug analysis.

  4. Determination of thiopurine S-methyltransferase activity by hydrophilic interaction liquid chromatography hyphenated with mass spectrometry.

    Science.gov (United States)

    Pecher, Daniel; Dokupilová, Svetlana; Zelinková, Zuzana; Peppelenbosch, Maikel; Mikušová, Veronika; Mikuš, Peter

    2017-08-05

    Thiopurine S-methyltransferase (TPMT) plays an important role in the metabolism of thiopurines used in the therapy of inflammatory bowel diseases (IBD). In this work a new progressive method for the determination of TPMT activity in red blood cells lysates was developed. Analysis was carried out by means of hydrophilic interaction liquid chromatography (HILIC) hyphenated with mass spectrometry (MS). In comparison with reversed-phase high-performance liquid chromatography (RP-HPLC), that has been typically applied in determination of TPMT activity, the HILIC significantly improved the analytical signal provided by MS, shortened analysis time, and improved chromatographic resolution. The HILIC-HPLC-MS method was optimized and validated, providing favorable parameters of detection and quantitation limits (5.5 and 16.5pmol/mL, respectively), linearity (coefficient of determination 0.9999 in the range of 0.01-1.0nmol/mL), recovery and precision (93.25-100.37% with RSD 1.06-1.32% in the whole concentration range of QC samples). Moreover, in contrast to the conventional RP-HPLC-UV approach, the complex phenotype TPMT profiles can be reliably and without interferences monitored using the HILIC-HPLC-MS method. Such advanced monitoring can provide valuable detail information on the thiopurines (e.g. evaluating ratio of methylated and non-methylated 6-mercaptopurine) and, by that, TPMT action in biological systems before and during the therapy of IBD. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. DETECTION AND QUANTIFICATION OF PHYTOCHEMICAL MARKERS OF Ilex paraguariensis BY LIQUID CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    Rodrigo M. C. Pinto

    2015-11-01

    Full Text Available Ilex paraguariensis (yerba-mate is used as a beverage, and its extract requires adequate quality control methods in order to guarantee quality and safe use. Strategies to develop and optimize a chromatographic method to quantify theobromine, caffeine, and chlorogenic acid in I. paraguariensis extracts were evaluated by applying a quality by design (QbD model and ultra high-performance liquid chromatography (UHPLC. The presence of these three phytochemical markers in the extracts was evaluated using UHPLC-MS and was confirmed by the chromatographic bands in the total ion current traces (m/z of 181.1 [M+H]+, 195.0 [M+H]+, and 353.0 [M−H]−, respectively. The developed method was then transferred to a high-performance liquid chromatography (HPLC platform, and the three phytochemical markers were used as external standards in the validation of a method for analyses of these compounds in extracts using a diode array detector (DAD. The validated method was applied to quantify the chlorogenic acid, caffeine, and theobromine in the samples. HPLC-DAD chromatographic fingerprinting was also used in a multivariate approach to process the entire data and to separate the I. paraguariensis extracts into two groups. The developed method is very useful for qualifying and quantifying I. paraguariensis extracts.

  6. Core-shell microspheres with porous nanostructured shells for liquid chromatography.

    Science.gov (United States)

    Ahmed, Adham; Skinley, Kevin; Herodotou, Stephanie; Zhang, Haifei

    2018-01-01

    The development of new stationary phases has been the key aspect for fast and efficient high-performance liquid chromatography separation with relatively low backpressure. Core-shell particles, with a solid core and porous shell, have been extensively investigated and commercially manufactured in the last decade. The excellent performance of core-shell particles columns has been recorded for a wide range of analytes, covering small and large molecules, neutral and ionic (acidic and basic), biomolecules and metabolites. In this review, we first introduce the advance and advantages of core-shell particles (or more widely known as superficially porous particles) against non-porous particles and fully porous particles. This is followed by the detailed description of various methods used to fabricate core-shell particles. We then discuss the applications of common silica core-shell particles (mostly commercially manufactured), spheres-on-sphere particles and core-shell particles with a non-silica shell. This review concludes with a summary and perspective on the development of stationary phase materials for high-performance liquid chromatography applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Analysis of glyphosate residues in cereals using liquid chromatography-mass spectrometry (LC-MS/MS)

    DEFF Research Database (Denmark)

    Granby, Kit; Johannesen, S.; Gabrielsen, Martin Vahl

    2003-01-01

    A fast and specific method for the determination of glyphosate in cereals is described. The method is based on extraction with water by ultrasonication. The samples are cleaned up and separated by high-performance liquid chromatography on a polystyrene-based reverse-phase column (clean-up) in ser......A fast and specific method for the determination of glyphosate in cereals is described. The method is based on extraction with water by ultrasonication. The samples are cleaned up and separated by high-performance liquid chromatography on a polystyrene-based reverse-phase column (clean...... monitored m/z 168--> 150 (glyphosate) and 170-->152 (internal standard 2- 13 (CN)-N-15-glyphosate) for quantification. The mean recovery was 85% ( n =32) at spiking levels from 0.03 to 0.33 mg kg(-1) . From 1998 to 2001, from the analysis of about 50 samples per annum, a reduction in the glyphosate residues...... was observed owing to a Danish trade decision not to use grain with glyphosate residues for milling or bread production....

  8. [Rapid determination of 8 urinary carbamate pesticides by liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Liu, Hualiang; Wang, Yuan; Zhu, Baoli

    2015-11-01

    To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides. After being purified by acetonitrile precipitation, urine samples were transferred to a liquid chromatography-tandem mass spectrometry system, and the concentrations of 8 carbamate pesticides were determined by external standard method. A C18 column was used for ultra-high-performance liquid chromatography; methanol/ammonium acetate solution was used as the mobile phase for gradient elution; the mass spectrometer was operated in a multi-reaction monitoring mode. The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20~800 µg/L, and the recovery rates were 61.0%~121% at spiked levels of 20, 200 and 800 µg/L, with a relative standard deviation of 1.7%~5.5%. This determination method meets the Guide for establishing occupational health standards-part 5: Determination methods of chemicals in biological materials, and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.

  9. High-throughput, Highly Sensitive Analyses of Bacterial Morphogenesis Using Ultra Performance Liquid Chromatography*

    Science.gov (United States)

    Desmarais, Samantha M.; Tropini, Carolina; Miguel, Amanda; Cava, Felipe; Monds, Russell D.; de Pedro, Miguel A.; Huang, Kerwyn Casey

    2015-01-01

    The bacterial cell wall is a network of glycan strands cross-linked by short peptides (peptidoglycan); it is responsible for the mechanical integrity of the cell and shape determination. Liquid chromatography can be used to measure the abundance of the muropeptide subunits composing the cell wall. Characteristics such as the degree of cross-linking and average glycan strand length are known to vary across species. However, a systematic comparison among strains of a given species has yet to be undertaken, making it difficult to assess the origins of variability in peptidoglycan composition. We present a protocol for muropeptide analysis using ultra performance liquid chromatography (UPLC) and demonstrate that UPLC achieves resolution comparable with that of HPLC while requiring orders of magnitude less injection volume and a fraction of the elution time. We also developed a software platform to automate the identification and quantification of chromatographic peaks, which we demonstrate has improved accuracy relative to other software. This combined experimental and computational methodology revealed that peptidoglycan composition was approximately maintained across strains from three Gram-negative species despite taxonomical and morphological differences. Peptidoglycan composition and density were maintained after we systematically altered cell size in Escherichia coli using the antibiotic A22, indicating that cell shape is largely decoupled from the biochemistry of peptidoglycan synthesis. High-throughput, sensitive UPLC combined with our automated software for chromatographic analysis will accelerate the discovery of peptidoglycan composition and the molecular mechanisms of cell wall structure determination. PMID:26468288

  10. Determination of Urine Albumin by New Simple High-Performance Liquid Chromatography Method.

    Science.gov (United States)

    Klapkova, Eva; Fortova, Magdalena; Prusa, Richard; Moravcova, Libuse; Kotaska, Karel

    2016-11-01

    A simple high-performance liquid chromatography (HPLC) method was developed for the determination of albumin in patients' urine samples without coeluting proteins and was compared with the immunoturbidimetric determination of albumin. Urine albumin is important biomarker in diabetic patients, but part of it is immuno-nonreactive. Albumin was determined by high-performance liquid chromatography (HPLC), UV detection at 280 nm, Zorbax 300SB-C3 column. Immunoturbidimetric analysis was performed using commercial kit on automatic biochemistry analyzer COBAS INTEGRA ® 400, Roche Diagnostics GmbH, Manheim, Germany. The HLPC method was fully validated. No significant interference with other proteins (transferrin, α-1-acid glycoprotein, α-1-antichymotrypsin, antitrypsin, hemopexin) was found. The results from 301 urine samples were compared with immunochemical determination. We found a statistically significant difference between these methods (P = 0.0001, Mann-Whitney test). New simple HPLC method was developed for the determination of urine albumin without coeluting proteins. Our data indicate that the HPLC method is highly specific and more sensitive than immunoturbidimetry. © 2016 Wiley Periodicals, Inc.

  11. Validation of a technique by high-performance liquid chromatography for the determination of total isoflavones

    Directory of Open Access Journals (Sweden)

    Pilar A. Soledispa Cañarte

    2017-04-01

    Full Text Available Context: Isoflavones may act as selective regulators in the prevention of various diseases. The most important source of isoflavones is the soy, from which different phytotherapeutics are elaborated of use in Ecuadorian population. However, its concentration varies depending on several factors, therefore quality assessment need to be carried out through out several analytical methods. Aims: To validate an analytical method by high precision liquid chromatography (HPLC to quantify total isoflavones in herbal medicine. Methods: To quantify isoflavones, it was used a brand liquid chromatography with UV/VIS detector at 260 nm, C-18 column using isocratic method. The mobile phase was composed of 2% acetic acid: acetonitrile (75:25. The quantification was performed against reference standard. The parameters for the validation followed the established in the USP 33. Results: The chromatogram presented six peaks with elution between 1.557 and 18.913 min. The linearity of the system and the method got r2 equal to 0.98 and 0.99 respectively. The coefficients of variation 1.5% in the study of repetitiveness and 2% in intermediate precision. The accuracy of the adjusted lineal model exhibited r=0.95 and intercept reliable interval (-0.921; 1.743. Conclusions: The validated method was specific, accurate, precise and linear. It can be used for quality control and stability studies of isoflavones present in herbal medicine.

  12. Targeted liquid chromatography tandem mass spectrometry to quantitate wheat gluten using well-defined reference proteins

    Science.gov (United States)

    Schalk, Kathrin; Koehler, Peter

    2018-01-01

    Celiac disease (CD) is an inflammatory disorder of the upper small intestine caused by the ingestion of storage proteins (prolamins and glutelins) from wheat, barley, rye, and, in rare cases, oats. CD patients need to follow a gluten-free diet by consuming gluten-free products with gluten contents of less than 20 mg/kg. Currently, the recommended method for the quantitative determination of gluten is an enzyme-linked immunosorbent assay (ELISA) based on the R5 monoclonal antibody. Because the R5 ELISA mostly detects the prolamin fraction of gluten, a new independent method is required to detect prolamins as well as glutelins. This paper presents the development of a method to quantitate 16 wheat marker peptides derived from all wheat gluten protein types by liquid chromatography tandem mass spectrometry (LC-MS/MS) in the multiple reaction monitoring mode. The quantitation of each marker peptide in the chymotryptic digest of a defined amount of the respective reference wheat protein type resulted in peptide-specific yields. This enabled the conversion of peptide into protein type concentrations. Gluten contents were expressed as sum of all determined protein type concentrations. This new method was applied to quantitate gluten in wheat starches and compared to R5 ELISA and gel-permeation high-performance liquid chromatography with fluorescence detection (GP-HPLC-FLD), which resulted in a strong correlation between LC-MS/MS and the other two methods. PMID:29425234

  13. Targeted liquid chromatography tandem mass spectrometry to quantitate wheat gluten using well-defined reference proteins.

    Directory of Open Access Journals (Sweden)

    Kathrin Schalk

    Full Text Available Celiac disease (CD is an inflammatory disorder of the upper small intestine caused by the ingestion of storage proteins (prolamins and glutelins from wheat, barley, rye, and, in rare cases, oats. CD patients need to follow a gluten-free diet by consuming gluten-free products with gluten contents of less than 20 mg/kg. Currently, the recommended method for the quantitative determination of gluten is an enzyme-linked immunosorbent assay (ELISA based on the R5 monoclonal antibody. Because the R5 ELISA mostly detects the prolamin fraction of gluten, a new independent method is required to detect prolamins as well as glutelins. This paper presents the development of a method to quantitate 16 wheat marker peptides derived from all wheat gluten protein types by liquid chromatography tandem mass spectrometry (LC-MS/MS in the multiple reaction monitoring mode. The quantitation of each marker peptide in the chymotryptic digest of a defined amount of the respective reference wheat protein type resulted in peptide-specific yields. This enabled the conversion of peptide into protein type concentrations. Gluten contents were expressed as sum of all determined protein type concentrations. This new method was applied to quantitate gluten in wheat starches and compared to R5 ELISA and gel-permeation high-performance liquid chromatography with fluorescence detection (GP-HPLC-FLD, which resulted in a strong correlation between LC-MS/MS and the other two methods.

  14. Separation of lanthanum from nuclear fuel solutions by high performance liquid chromatography

    International Nuclear Information System (INIS)

    Lazar, G. C.; Petre, M.; Androne, G.; Benga, A.

    2016-01-01

    This paper presents the separation of uranium, praseodymium and lanthanum from nuclear fuel solutions by high performance liquid chromatography (HPLC). The aim of this study is to establish a minimum concentration of lanthanum which can be analyzed by high performance liquid chromatography, and also to study the effect of uranium concentration on the separation of praseodymium and lanthanum. Optimum gradient mode was established for mixture standard stoc solutions with uranium in a concentration of 1 mg/ml, praseodymium and lanthanum in a concentration range of 1-5 μg/ml from each element. These conditions were applied for the separation of lanthanum from a nuclear fuel solution in which praseodymium and lanthanum were added in a concentration of 3 μg/ml from each element. The elution behavior of lanthanum as a function of the pH and the concentration of the mobile phase, using a mixture of 1-octanesulfonic acid sodium salt with a-hidroxyisobutiric acid is presented. (authors)

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

    Science.gov (United States)

    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: 15-40 ng). 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. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Isotope ratio mass spectrometry coupled to liquid and gas chromatography for wine ethanol characterization.

    Science.gov (United States)

    Cabañero, Ana I; Recio, Jose L; Rupérez, Mercedes

    2008-10-01

    Two new procedures for wine ethanol 13C/12C isotope ratio determination, using high-performance liquid chromatography and gas chromatography isotope ratio mass spectrometry (HPLC/IRMS and GC/IRMS), have been developed to improve isotopic methods dedicated to the study of wine authenticity. Parameters influencing separation of ethanol from wine matrix such as column, temperature, mobile phase, flow rates and injection mode were investigated. Twenty-three wine samples from various origins were analyzed for validation of the procedures. The analytical precision was better than 0.15 per thousand, and no significant isotopic fractionation was observed employing both separative techniques coupled to IRMS. No significant differences and a very strong correlation (r = 0.99) were observed between the 13C/12C ratios obtained by the official method (elemental analyzer/isotope ratio mass spectrometry) and the proposed new methodology. The potential advantages of the developed methods over the traditional one are speed (reducing time required from hours to minutes) and simplicity. In addition, these are the first isotopic methods that allow 13C/12C determination directly from a liquid sample with no previous ethanol isolation, overcoming technical difficulties associated with sample treatment.

  17. Hb A1c Separation by High Performance Liquid Chromatography in Hemoglobinopathies

    Directory of Open Access Journals (Sweden)

    Vani Chandrashekar

    2016-01-01

    Full Text Available Hb A1c measurement is subject to interference by hemoglobin traits and this is dependent on the method used for determination. In this paper we studied the difference between Hb A1c measured by HPLC in hemoglobin traits and normal chromatograms. We also studied the correlation of Hb A1c with age. Hemoglobin analysis was carried out by high performance liquid chromatography. Spearman’s rank correlation was used to study correlation between A1c levels and age. Mann-Whitney U test was used to study the difference in Hb A1c between patients with normal hemoglobin and hemoglobin traits. A total of 431 patients were studied. There was positive correlation with age in patients with normal chromatograms only. No correlation was seen in Hb E trait or beta thalassemia trait. No significant difference in Hb A1c of patients with normal chromatograms and patients with hemoglobin traits was seen. There is no interference by abnormal hemoglobin in the detection of A1c by high performance liquid chromatography. This method cannot be used for detection of A1c in compound heterozygous and homozygous disorders.

  18. Fast and Simple Forensic Red Pen Ink Analysis Using Ultra-Performance Liquid Chromatography (UPLC)

    International Nuclear Information System (INIS)

    Lee, L.C.; Ying, S.L.; Wan Nur Syazwani Wan Mohamad Fuad; Ab Aziz Ishak; Khairul Osman

    2016-01-01

    Ultra-performance liquid chromatography (UPLC) is more effective than high performance liquid chromatography in terms of analysis speed and sensitivity. This paper presents a feasibility study on forensic red pen inks analysis using UPLC. A total of 12 varieties of red ball point pen inks were purchased from selected stationary shop. For each variety, four different individual pens were sampled to provide intra-variability within a particular variety of pen. The proposed approach is very simple that it only involved limited analysis step and chemicals. A total of 144 chromatograms were obtained from red ink entries extracted with 1.5 mL 80 % (v/v) acetonitrile. Peaks originated from pen inks were determined by comparing the chromatograms of both blank paper and blank solvent against that of ink samples. Subsequently, one-way ANOVA was conducted to discriminate all 66 possible pairs for red pen inks. Results showed that the proposed approach giving discriminating power of 95.45 %. The outcome of the study indicates that UPLC could be a fast and simple approach to red ball point pen inks analysis. (author)

  19. A fast isocratic liquid chromatography method for the quantification of xanthophylls and their stereoisomers.

    Science.gov (United States)

    Nimalaratne, Chamila; Lopes-Lutz, Daise; Schieber, Andreas; Wu, Jianping

    2015-12-01

    A fast isocratic liquid chromatography method was developed for the simultaneous quantification of eight xanthophylls (13-Z-lutein, 13'-Z-lutein, 13-Z-zeaxanthin, all-E-lutein, all-E-zeaxanthin, all-E-canthaxanthin, all-E-β-apo-8'-carotenoic acid ethyl ester and all-E-β-apo-8'-carotenal) within 12 min, compared to 90 min by the conventional high-performance liquid chromatography method. The separation was achieved on a YMC C30 reversed-phase column (100 mm x 2.0 mm; 3 μm) operated at 20°C using a methanol/tert-butyl methyl ether/water solvent system at a flow rate of 0.8 mL/min. The method was successfully applied to quantify lutein and zeaxanthin stereoisomers in egg yolk, raw and cooked spinach, and a dietary supplement. The method can be used for the rapid analysis of xanthophyll isomers in different food products and for quality control purposes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. High-temperature phase transitions and domain structures of KLiSO{sub 4}. Studied by polarisation-optics, X-ray topography and liquid-crystal surface decoration

    Energy Technology Data Exchange (ETDEWEB)

    Scherf, Christian; Chung, Su Jin; Hahn, Theo; Klapper, Helmut [RWTH Aachen Univ. (Germany). Inst. fuer Kristallographie; Ivanov, Nicolay R. [Russian Academy of Sciences, Moscow (Russian Federation). Shubnikov Inst. of Crystallography

    2017-07-01

    The transitions between the room temperature phase III (space group P6{sub 3}) and the two high-temperature phases II (Pcmn) and I (P6{sub 3}/mmc) of KLiSO{sub 4} and the domain structures generated by them were investigated by high-temperature polarisation optics (birefringence) and room-temperature X-ray topography, optical activity and nematic-liquid-crystal (NLC) surface decoration. The transition from the polar hexagonal phase III into the centrosymmetric orthorhombic phase II at 708 K leads, due to the loss of the trigonal axis and the radial temperature gradient of the optical heating chamber used, to a roughly hexagonal arrangement of three sets of thin orthorhombic {110} lamelleae with angles of 60 (120 ) between them. The associated twin law ''reflection m{110}{sub orth}'' corresponds to the frequent growth twin m{10 anti 10}{sub hex} of phase III. The domains are easily ferroelastically switched. Upon further heating above 949 K into phase I (P6{sub 3}/mmc) all domains vanish. Upon cooling back into phase II the three domain states related by 60 (120 ) reflections m{110}{sub orth} re-appear, however (due to the higher thermal agitation at 949 K) with a completely different domain structure consisting of many small, irregularly arranged {110}{sub orth} domains. Particular attention is paid to the domain structure of the hexagonal room temperature phase III generated during the re-transition from the orthorhombic phase II. Curiously, from the expected three twin laws inversion anti 1, rotation 2 perpendicular to [001]{sub hex} and reflection m{10 anti 10}{sub hex} only the latter, which corresponds to the frequent growth twinning, has been found. Finally a short treatise of the structural relations of the KLiSO{sub 4} high-temperature polymorphs is given.