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Sample records for acid stationary phase

  1. Study of Stationary Phase Metabolism Via Isotopomer Analysis of Amino Acids from an Isolated Protein

    Energy Technology Data Exchange (ETDEWEB)

    Shaikh, AfshanS.; Tang, YinjieJ.; Mukhopadhyay, Aindrila; Martin, Hector Garcia; Gin, Jennifer; Benke, Peter; Keasling, Jay D.

    2009-09-14

    Microbial production of many commercially important secondary metabolites occurs during stationary phase, and methods to measure metabolic flux during this growth phase would be valuable. Metabolic flux analysis is often based on isotopomer information from proteinogenic amino acids. As such, flux analysis primarily reflects the metabolism pertinent to the growth phase during which most proteins are synthesized. To investigate central metabolism and amino acids synthesis activity during stationary phase, addition of fully 13C-labeled glucose followed by induction of green fluorescent protein (GFP) expression during stationary phase was used. Our results indicate that Escherichia coli was able to produce new proteins (i.e., GFP) in the stationary phase, and the amino acids in GFP were mostly from degraded proteins synthesized during the exponential growth phase. Among amino acid biosynthetic pathways, only those for serine, alanine, glutamate/glutamine, and aspartate/asparagine had significant activity during the stationary phase.

  2. Comparison of GC stationary phases for the separation of fatty acid methyl esters in biodiesel fuels.

    Science.gov (United States)

    Goding, Julian C; Ragon, Dorisanne Y; O'Connor, Jack B; Boehm, Sarah J; Hupp, Amber M

    2013-07-01

    The fatty acid methyl ester (FAME) content of biodiesel fuels has traditionally been determined using gas chromatography with a polar stationary phase. In this study, a direct comparison of the separation of FAMEs present in various biodiesel samples on three polar stationary phases and one moderately polar stationary phase (with comparable column dimensions) was performed. Retention on each column was based on solubility in and polarity of the phase. Quantitative metrics describing the resolution of important FAME pairs indicate high resolution on all polar columns, yet the best resolution, particularly of geometric isomers, is achieved on the cyanopropyl column. In addition, the separation of four C18 monounsaturated isomers was optimized and the elution order determined on each column. FAME composition of various biodiesel fuel types was determined on each column to illustrate (1) chemical differences in biodiesels produced from different feedstocks and (2) chemical similarities in biodiesels of the same feedstock type produced in different locations and harvest seasons.

  3. Ionic liquids as stationary phases for fatty acid analysis by gas chromatography.

    Science.gov (United States)

    Fanali, C; Micalizzi, G; Dugo, P; Mondello, L

    2017-12-04

    The present paper provides an overview of the application of ionic liquid (IL) columns for GC analysis of fatty acid methyl esters (FAMEs). Although their separation can be carried out utilizing GC columns containing polar stationary phases, some ILs have been employed as stationary phases, either commercial or laboratory made, in GC analysis. Monodimensional and bidimensional GC methods have been optimized in order to achieve the best separation especially considering the geometric and positional isomers of unsaturated fatty acids. Several methods for the analysis of trans-fatty acids have also been reported. The use of GC-GC, using either the same IL columns or different columns in the first and second dimensions, allowed the separation of a large number of FAMEs. The application of the IL columns for GC analysis of FAMEs in different types of real samples is described, e.g., oil of different nature (fish, flaxseed, and olive), margarine and butter, biodiesel, milk, bacteria etc.

  4. Enhanced dipicolinic acid production during the stationary phase in Bacillus subtilis by blocking acetoin synthesis.

    Science.gov (United States)

    Toya, Yoshihiro; Hirasawa, Takashi; Ishikawa, Shu; Chumsakul, Onuma; Morimoto, Takuya; Liu, Shenghao; Masuda, Kenta; Kageyama, Yasushi; Ozaki, Katsuya; Ogasawara, Naotake; Shimizu, Hiroshi

    2015-01-01

    Bacterial bio-production during the stationary phase is expected to lead to a high target yield because the cells do not consume the substrate for growth. Bacillus subtilis is widely used for bio-production, but little is known about the metabolism during the stationary phase. In this study, we focused on the dipicolinic acid (DPA) production by B. subtilis and investigated the metabolism. We found that DPA production competes with acetoin synthesis and that acetoin synthesis genes (alsSD) deletion increases DPA productivity by 1.4-fold. The mutant showed interesting features where the glucose uptake was inhibited, whereas the cell density increased by approximately 50%, resulting in similar volumetric glucose consumption to that of the parental strain. The metabolic profiles revealed accumulation of pyruvate, acetyl-CoA, and the TCA cycle intermediates in the alsSD mutant. Our results indicate that alsSD-deleted B. subtilis has potential as an effective host for stationary-phase production of compounds synthesized from these intermediates.

  5. Mutations Enhancing Amino Acid Catabolism Confer a Growth Advantage in Stationary Phase

    Science.gov (United States)

    Zinser, Erik R.; Kolter, Roberto

    1999-01-01

    Starved cultures of Escherichia coli undergo successive rounds of population takeovers by mutants of increasing fitness. These mutants express the growth advantage in stationary phase (GASP) phenotype. Previous work identified the rpoS819 allele as a GASP mutation allowing cells to take over stationary-phase cultures after growth in rich media (M. M. Zambrano, D. A. Siegele, M. A. Almirón, A. Tormo, and R. Kolter, Science 259:1757–1760, 1993). Here we have identified three new GASP loci from an aged rpoS819 strain: sgaA, sgaB, and sgaC. Each locus is capable of conferring GASP on the rpoS819 parent, and they can provide successively higher fitnesses for the bacteria in the starved cultures. All four GASP mutations isolated thus far allow for faster growth on both individual and mixtures of amino acids. Each mutation confers a growth advantage on a different subset of amino acids, and these mutations act in concert to increase the overall catabolic capacity of the cell. We present a model whereby this enhanced ability to catabolize amino acids is responsible for the fitness gain during carbon starvation, as it may allow GASP mutants to outcompete the parental cells when growing on the amino acids released by dying cells. PMID:10482523

  6. Synergistic effects on enantioselectivity of zwitterionic chiral stationary phases for separations of chiral acids, bases, and amino acids by HPLC.

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    Hoffmann, Christian V; Pell, Reinhard; Lämmerhofer, Michael; Lindner, Wolfgang

    2008-11-15

    In an attempt to overcome the limited applicability scope of earlier proposed Cinchona alkaloid-based chiral weak anion exchangers (WAX) and recently reported aminosulfonic acid-based chiral strong cation exchangers (SCX), which are conceptionally restricted to oppositely charged solutes, their individual chiral selector (SO) subunits have been fused in a combinatorial synthesis approach into single, now zwitterionic, chiral SO motifs. The corresponding zwitterionic ion-exchange-type chiral stationary phases (CSPs) in fact combined the applicability spectra of the parent chiral ion exchangers allowing for enantioseparations of chiral acids and amine-type solutes in liquid chromatography using polar organic mode with largely rivaling separation factors as compared to the parent WAX and SCX CSPs. Furthermore, the application spectrum could be remarkably expanded to various zwitterionic analytes such as alpha- and beta-amino acids and peptides. A set of structurally related yet different CSPs consisting of either a quinine or quinidine alkaloid moiety as anion-exchange subunit and various chiral or achiral amino acids as cation-exchange subunits enabled us to derive structure-enantioselectivity relationships, which clearly provided strong unequivocal evidence for synergistic effects of the two oppositely charged ion-exchange subunits being involved in molecular recognition of zwitterionic analytes by zwitterionic SOs driven by double ionic coordination.

  7. Preparation, characterization and application of N-methylene phosphonic acid chitosan grafted magnesia–zirconia stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qing; Chen, Jie; Huang, Kun; Zhang, Xin; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2015-01-07

    Highlights: • N-methylene phosphonic acid chitosan grafted MgO–ZrO{sub 2} was prepared. • It exhibited superior HILIC chromatographic performance to the bare MgO–ZrO{sub 2}. • Monosaccharides, phospholipids and peptides were successfully separated. • It was a promising HILIC stationary phase. - Abstract: A hydrophilic stationary phase (SP) was prepared through grafting N-methylene phosphonic acid chitosan on magnesia–zirconia particles (P-CTS-MgO–ZrO{sub 2}) via Lewis acid–base interaction. The resulting material was characterized by thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscope and nitrogen adsorption analysis. The chromatographic performance of P-CTS-MgO–ZrO{sub 2} was systemically evaluated by studying effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the novel SP provided hydrophilic, electrostatic-repulsion and ion-exchange interactions. Compared to the bare MgO–ZrO{sub 2}, P-CTS-MgO–ZrO{sub 2} exhibited superior peak shape, reasonable resolution and reduced analysis time in separation of basic analytes. Besides, remarkable resolving power of acids, i.e. six non-steroidal anti-inflammatory drugs which failed to be eluted from the bare MgO–ZrO{sub 2}, was obtained with the theoretical plate number (N/m) of 4653–31313, asymmetry factor <1.21 and the resolution of 1.6–3.4. Finally, P-CTS-MgO–ZrO{sub 2} SP was applied to separate monosaccharides, phospholipids and peptides. P-CTS-MgO–ZrO{sub 2} was a promising hydrophilic SP for wide applications.

  8. Increments to chiral recognition facilitating enantiomer separations of chiral acids, bases, and ampholytes using Cinchona-based zwitterion exchanger chiral stationary phases.

    Science.gov (United States)

    Wernisch, Stefanie; Pell, Reinhard; Lindner, Wolfgang

    2012-07-01

    The intramolecular distances of anion and cation exchanger sites of zwitterionic chiral stationary phases represent potential tuning sites for enantiomer selectivity. In this contribution, we investigate the influence of alkanesulfonic acid chain length and flexibility on enantiomer separations of chiral acids, bases, and amphoteric molecules for six Cinchona alkaloid-based chiral stationary phases in comparison with structurally related anion and cation exchangers. Employing polar-organic elution conditions, we observed an intramolecular counterion effect for acidic analytes which led to reduced retention times but did not impair enantiomer selectivities. Retention of amphoteric analytes is based on simultaneous double ion pairing of their charged functional groups with the acidic and basic sites of the zwitterionic selectors. A chiral center in the vicinity of the strong cation exchanger site is vital for chiral separations of bases. Sterically demanding side chains are beneficial for separations of free amino acids. Enantioseparations of free (un-derivatized) peptides were particularly successful in stationary phases with straight-chain alkanesulfonic acid sites, pointing to a beneficial influence of more flexible moieties. In addition, we observed pseudo-enantiomeric behavior of quinine and quinidine-derived chiral stationary phases facilitating reversal of elution orders for all analytes. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Optimising reversed-phase liquid chromatographic separation of an acidic mixture on a monolithic stationary phase with the aid of response surface methodology and experimental design.

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    Wang, Y; Harrison, M; Clark, B J

    2006-02-10

    An optimization strategy for the separation of an acidic mixture by employing a monolithic stationary phase is presented, with the aid of experimental design and response surface methodology (RSM). An orthogonal array design (OAD) OA(16) (2(15)) was used to choose the significant parameters for the optimization. The significant factors were optimized by using a central composite design (CCD) and the quadratic models between the dependent and the independent parameters were built. The mathematical models were tested on a number of simulated data set and had a coefficient of R(2) > 0.97 (n = 16). On applying the optimization strategy, the factor effects were visualized as three-dimensional (3D) response surfaces and contour plots. The optimal condition was achieved in less than 40 min by using the monolithic packing with the mobile phase of methanol/20 mM phosphate buffer pH 2.7 (25.5/74.5, v/v). The method showed good agreement between the experimental data and predictive value throughout the studied parameter space and were suitable for optimization studies on the monolithic stationary phase for acidic compounds.

  10. Separation of U and Pu be the method of liquid chromatography with free stationary phase in TBP - white spirit - nitric acid system

    International Nuclear Information System (INIS)

    Litvina, M.N.; Malikov, D.A.; Maryutina, T.A.; Kulyako, Yu.M.; Myasoedov, B.F.

    2006-01-01

    Possibility is studied of the use of liquid chromatography with free stationary phase for U and Pu separation from organic extract obtained by direct dissolution of MOX-fuel in supercritical CO 2 containing TBP·nHNO 3 complex. As stationary phase solutions of TBP in white-spirit of different concentrations are used. Effect of composition of stationary and mobile phases on separation efficiency is investigated. It is shown that use of liquid chromatography with free stationary phase permits to separate U and Pu in conditions of TBP concentration gradient in stationary phase and HNO 3 concentration gradient in mobile one [ru

  11. Design, preparation and application of a Pirkle-type chiral stationary phase for enantioseparation of some racemic organic acids and molecular dynamics studies

    Directory of Open Access Journals (Sweden)

    Reşit Çakmak

    2017-08-01

    Full Text Available This study consists of two parts. In the first part of the study; a Pirkle-type chiral stationary phase was prepared by synthesizing an aromatic amine derivative of (R-2-amino-1-butanol as a chiral selectorand binding to L- tyrosine -modified cyanogen bromide (CNBr-activated Sepharose 4B and then, packed into the separation column. T he chromatographic performance of the separation column was evaluated w ith racemic mandelic acid and 2-phenylpropionic acid by using phosphate buffers at three different pHs as mobile phase. In the resolution processes, t he prepared solutions were loaded onto the separation column at two different concentrations and at three different pHs for each racemic organic acid, separately. Enantiomeric excess (ee % of the eluates was determined on CHIRALPAK AD-H chiral analytical column by HPLC. The maximum ee% for mandelic acid and 2-phenylpropionic acid was determined to be 60.84 and 27.4, respectively. Separation factors (k 1 ’, k 2 ’, α, and Rs were calculated for each acid. The structures of the obtained compounds were characterized using the spectroscopic methods (NMR, and elemental analysis. In the second part of the study; enantioselective interactions between the prepared CSP and the analytes have been widely studied by docking, molecular dynamics simulation and quantum mechanical computation methods. The reason of column eluation of rac-2-phenylpropionic acid with lower enantiomeric yield was explained by these techniques.

  12. High-performance liquid chromatographic enantioseparation of unusual isoxazoline-fused 2-aminocyclopentanecarboxylic acids on macrocyclic glycopeptide-based chiral stationary phases.

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    Sipos, László; Ilisz, István; Nonn, Melinda; Fülöp, Ferenc; Pataj, Zoltán; Armstrong, Daniel W; Péter, Antal

    2012-04-06

    The enantiomers of four unusual isoxazoline-fused 2-aminocyclopentanecarboxylic acids were directly separated on chiral stationary phases containing macrocyclic glycopeptide antibiotics teicoplanin (Astec Chirobiotic T and T2), teicoplanin aglycone (Chirobiotic TAG), vancomycin (Chirobiotic V) and vancomycin aglycone (Chirobiotic VAG) as chiral selectors. The effects of the mobile phase composition, the structure of the analytes and temperature on the separations were investigated. Experiments were performed at constant mobile phase compositions in the temperature range 5-45 °C to study the effects of temperature, and thermodynamic parameters were calculated from plots of lnk or lnα versus 1/T. Some mechanistic aspects of the chiral recognition process are discussed with respect to the structures of the analytes. It was found that the enantiomeric separations were in most cases enthalpy-driven. The sequence of elution of the enantiomers was determined in all cases. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Diastereo- and enantioseparation of a Nα-Boc amino acid with a zwitterionic quinine-based stationary phase: Focus on the stereorecognition mechanism

    International Nuclear Information System (INIS)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria; Di Michele, Alessandro; Sardella, Roccaldo; Lindner, Wolfgang; Natalini, Benedetto

    2015-01-01

    Highlights: • The ZWIX(+) column allowed getting the Boc-Aph(Hor)-OH (1) isomeric peaks resolved. • ECD studies and molecular dynamic simulations allowed to assign the elution order. • Molecular descriptors revealed the active role of achiral elements of the CSP. - Abstract: A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N α -Boc-N 4 -(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water—49.7:49.7:0.6 (v/v/v) with formic acid (4.0 mM) and diethylamine (2.5 mM), allowed the successful separation of the four acid stereoisomers: α D,D-/D,L-1 = 1.08; α D,L-/L,D-1 = 1.08; α L,D-/L,L-1 = 1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: D,D-1 < D,L-1 < L,D-1 < L,L-1. With the aim of better understanding the molecular basis of the retention behaviour of the four stereoisomers in the employed chromatographic system and conditions, a computational protocol consisting in molecular dynamics simulations was applied. The use of the three descriptors INTER (in kcal mol −1 , encoding for the interaction energy between the selector SO unit and the whole system), INTER-SA (in kcal mol −1 , encoding for the interaction energy between SO and the sole selectand SA), and SELF (in kcal mol −1 , encoding for the conformational energy of SA relative to its minimum energy registered by the collected snapshots) revealed the active role of achiral sub-structural elements of the chiral stationary phase and eluent components in the overall stereorecognition mechanism

  14. Effect of pressure on the selectivity of polymeric C18 and C30 stationary phases in reversed-phase liquid chromatography. Increased separation of isomeric fatty acid methyl esters, triacylglycerols, and tocopherols at high pressure.

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    Okusa, Kensuke; Iwasaki, Yuki; Kuroda, Ikuma; Miwa, Shohei; Ohira, Masayoshi; Nagai, Toshiharu; Mizobe, Hoyo; Gotoh, Naohiro; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

    2014-04-25

    A high-density, polymeric C18 stationary phase (Inertsil ODS-P) or a polymeric C30 phase (Inertsil C30) provided improved resolution of the isomeric fatty acids (FAs), FA methyl esters (FAMEs), triacylglycerols (TAGs), and tocopherols with an increase in pressure of 20-70MPa in reversed-phase HPLC. With respect to isomeric C18 FAMEs with one cis-double bond, ODS-P phase was effective for recognizing the position of a double bond among petroselinic (methyl 6Z-octadecenoate), oleic (methyl 9Z-octadecenoate), and cis-vaccenic (methyl 11Z-octadecenoate), especially at high pressure, but the differentiation between oleic and cis-vaccenic was not achieved by C30 phase regardless of the pressure. A monomeric C18 phase (InertSustain C18) was not effective for recognizing the position of the double bond in monounsaturated FAME, while the separation of cis- and trans-isomers was achieved by any of the stationary phases. The ODS-P and C30 phases provided increased separation for TAGs and β- and γ-tocopherols at high pressure. The transfer of FA, FAME, or TAG molecules from the mobile phase to the ODS-P stationary phase was accompanied by large volume reduction (-30∼-90mL/mol) resulting in a large increase in retention (up to 100% for an increase of 50MPa) and improved isomer separation at high pressure. For some isomer pairs, the ODS-P and C30 provided the opposite elution order, and in each case higher pressure improved the separation. The two stationary phases showed selectivity for the isomers having rigid structures, but only the ODS-P was effective for differentiating the position of a double bond in monounsaturated FAMEs. The results indicate that the improved isomer separation was provided by the increased dispersion interactions between the solute and the binding site of the stationary phase at high pressure. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Equivalent chain lengths of all C4-C23 saturated monomethyl branched fatty acid methyl esters on methylsilicone OV-1 stationary phase.

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    Kubinec, Róbert; Blaško, Jaroslav; Górová, Renáta; Addová, Gabriela; Ostrovský, Ivan; Amann, Anton; Soják, Ladislav

    2011-04-01

    Isomer mixtures of monomethyl branched saturated C7-C23 fatty acid methyl esters (FAME) were prepared by performing a methylene insertion reaction to the straight chain FAME and this study model was completed by using commercially available standards of C4-C7 FAME. The equivalent chain lengths (ECL) of all 220 C4-C23 monomethyl branched FAME on OV-1 stationary phase were measured, achieving an average repeatability of ±0.0004 ECL units. The monomethyl branched FAME was identified by GC on the basis of regularity of the fractional chain lengths (FCL) dependence on the number of carbon atoms (C(z)) of individual homologous series of methyl 2-, 3-, …, 21-FAME. The prediction of retention of the first homologues, having the new position of methyl group beginning at higher carbon atoms number, and analogously for the second, third, fourth, and other members of the homologous series, allowed the dependence FCL=f(C(z)) for the first and subsequent members of beginning homologous of monomethyl derivatives of FAME. The identification was confirmed by mass spectrometry. All of the methyl isomers of FAME, which could not be completely separated by gas chromatography due to having a methyl group in surroundings of the middle of the carbon chain, were resolved by mass spectrometry using deconvolution in a SIM-mode. Measured gas chromatographic and mass spectrometric data were applied for identification of the monomethyl branched saturated FAME in tongue coating. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Localization and stationary phase approximation on supermanifolds

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    Zakharevich, Valentin

    2017-08-01

    Given an odd vector field Q on a supermanifold M and a Q-invariant density μ on M, under certain compactness conditions on Q, the value of the integral ∫Mμ is determined by the value of μ on any neighborhood of the vanishing locus N of Q. We present a formula for the integral in the case where N is a subsupermanifold which is appropriately non-degenerate with respect to Q. In the process, we discuss the linear algebra necessary to express our result in a coordinate independent way. We also extend the stationary phase approximation and the Morse-Bott lemma to supermanifolds.

  17. [[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

    Science.gov (United States)

    Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

    2014-09-01

    Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

  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. Stationary phases for superheated water chromatography

    International Nuclear Information System (INIS)

    Saha, Shikha

    2002-01-01

    This project focused on the comparison of conventional liquid chromatography and superheated water chromatography. It examined the differences in efficiency and retention of a range of different stationary phases. Alkyl aryl ketones and eight aromatic compounds were separated on PBD-zirconia, Xterra RP 18, Luna C 18 (2) and Oasis HLB columns using conventional LC and superheated water chromatography system. The retention indices were determined in the different eluents. On changing the organic component of the eluent from methanol to acetonitrile to superheated water considerable improvements were found in the peak shapes and column efficiencies on the PBD-zirconia and Oasis HLB columns. PS-DVB, PBD-zirconia and Xterra RP 18 columns have been used in efficiency studies. It was found that simply elevating the column temperature did not increase the efficiency of a separation in superheated water chromatography. The efficiency depended on flow rate, injection volume and also mobile phase preheating system. Although high efficiencies were not achieved with superheated water on PS-DVB and Xterra RP 18 columns, a higher efficiency was achieved on a PBD-zirconia column with superheated water than with 25-35% ACN at room temperature. The proposed theoretical increases in u opt were measured on three columns using superheated water as the mobile phase. The application of the superheated water chromatographic method to the separation of the pungent constituents of ginger by superheated water chromatography-NMR coupling system was studied. The coupling of superheated water chromatography using deuterium oxide to NMR spectroscopy for the separation of dry ginger extract was successful, although the NMR sensitivity in on-line mode coupling system was low. However, four compounds were identified in the ginger extract by stop-flow mode on superheated water chromatography-UV-NMR detection system. (author)

  20. Selectivity of some basic solutes on a poly(methyltetradecylsiloxane)-silica stationary phase.

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    Borges, Endler M; Collins, Carol H

    2011-11-01

    Complex analyses of polar compounds, especially basic ones, require more selective stationary phases. The present paper describes a stationary phase prepared by thermal immobilization of poly(methyltetradecylsiloxane) onto chromatographic silica (PMTDS-SiO(2)). This stationary phase presents hydrophobic and ion-exchange interactions that confer both high retention and unique selectivities for basic solutes. The influence of ion-exchange interactions is confirmed by the increase in retention factors of basic solutes when the mobile-phase pH changes from acidic to neutral and by the decrease in retention factors when the mobile-phase pH changes from neutral to alkaline. The ion-exchange properties of the stationary phase are enriched in neutral mobile phase (pH 7-7.5) using soft Lewis bases such as tricine and tris as buffers but are suppressed in both acidic (pH 2.5-6) and highly alkaline mobile phases (pH≤10). Increasing both temperature and flow rate permits more rapid separations while maintaining the selectivity. The stability of the stationary phase is evaluated with acid, neutral and alkaline mobile phases. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Enantioselective potential of polysaccharide-based chiral stationary phases in supercritical fluid chromatography.

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    Kucerova, Gabriela; Kalikova, Kveta; Tesarova, Eva

    2017-06-01

    The enantioselective potential of two polysaccharide-based chiral stationary phases for analysis of chiral structurally diverse biologically active compounds was evaluated in supercritical fluid chromatography using a set of 52 analytes. The chiral selectors immobilized on 2.5 μm silica particles were tris-(3,5-dimethylphenylcarmabate) derivatives of cellulose or amylose. The influence of the polysaccharide backbone, different organic modifiers, and different mobile phase additives on retention and enantioseparation was monitored. Conditions for fast baseline enantioseparation were found for the majority of the compounds. The success rate of baseline and partial enantioseparation with cellulose-based chiral stationary phase was 51.9% and 15.4%, respectively. Using amylose-based chiral stationary phase we obtained 76.9% of baseline enantioseparations and 9.6% of partial enantioseparations of the tested compounds. The best results on cellulose-based chiral stationary phase were achieved particularly with propane-2-ol and a mixture of isopropylamine and trifluoroacetic acid as organic modifier and additive to CO 2 , respectively. Methanol and basic additive isopropylamine were preferred on amylose-based chiral stationary phase. The complementary enantioselectivity of the cellulose- and amylose-based chiral stationary phases allows separation of the majority of the tested structurally different compounds. Separation systems were found to be directly applicable for analyses of biologically active compounds of interest. © 2017 Wiley Periodicals, Inc.

  2. Adsorptive removal of Methylene blue and Methyl orange from aqueous media by carboxylated diaminoethane sporopollenin: On the usability of an aminocarboxilic acid functionality-bearing solid-stationary phase in column techniques

    International Nuclear Information System (INIS)

    Ayar, Ahmet; Gezici, Orhan; Kuecuekosmanoglu, Muhittin

    2007-01-01

    The adsorption phenomena of Methylene blue (MB) and Methyl orange (MO) on a carboxylated diaminoethane sporopollenin (CDAE-S) solid phase were investigated in a column arrangement by using breakthrough technique. The adsorption phenomena were evaluated using some common adsorption isotherm models and Scatchard plot analysis, and obtained results were interpreted for evaluating the usability of CDAE-S for removal, recovery and preconcentration of the studied dyes both at the laboratory and industrial scales. On the basis of Scatchard plot analysis, the interaction types between the CDAE-S and the studied dyes were criticized in terms of affinity phenomena. Thus, the usability of a biomacromolecule-derived material, CDAE-S, as a cheap, environmentally-friendly and effective solid-stationary phase exhibiting both cation-exchange and anion-exchange characteristics at the same time, is discussed through the present study. Besides, from the obtained results, the protonated CDAE-S, which functionally resembles an amino acid structure, are presented as a two-in-one solid-stationary phase, and its adaptability to common processes performed under column conditions is also drawn in detail

  3. Retention of Halogenated Solutes on Stationary Phases Containing Heavy Atoms

    Directory of Open Access Journals (Sweden)

    Toshio Miwa

    2013-05-01

    Full Text Available To examine the effects of weak intermolecular interactions on solid-phase extraction (SPE and chromatographic separation, we synthesized some novel stationary phases with a heavy atom effect layer by immobilizing halogenated aromatic rings and hydroxyl groups onto the surface of a hydrophilic base polymer. Using SPE cartridges packed with the functionalized materials, we found that the heavy atom stationary phases could selectively retain halophenols in organic solvents, such as 1-propanol which blocks the hydrogen bonding, or acetonitrile which blocks the p-p interaction. The extraction efficiency of the materials toward the halophenols depended on the dipole moments of phenoxy groups present as functional groups. On the other hand, the extraction efficiency of solutes toward the functional group depended on their molar refractions, i.e., induced dipole moments. The retention of the solutes to the stationary phase ultimately depended on not only strong intermolecular interactions, but also the effects of weak interactions such as the dispersion force.

  4. 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.

  5. Natural terpene derivatives as new structural task-specific ionic liquids to enhance the enantiorecognition of acidic enantiomers on teicoplanin-based stationary phase by high-performance liquid chromatography.

    Science.gov (United States)

    Flieger, Jolanta; Feder-Kubis, Joanna; Tatarczak-Michalewska, Małgorzata; Płazińska, Anita; Madejska, Anna; Swatko-Ossor, Marta

    2017-06-01

    We present the specific cooperative effect of a semisynthetic glycopeptide antibiotic teicoplanin and chiral ionic liquids containing the (1R,2S,5R)-(-)-menthol moiety on the chiral recognition of enantiomers of mandelic acid, vanilmandelic acid, and phenyllactic acid. Experiments were performed chromatographically on an Astec Chirobiotic T chiral stationary phase applying the mobile phase with the addition of the chiral ionic liquids. The stereoselective binding of enantiomers to teicoplanin in presence of new chiral ionic liquids were evaluated applying thermodynamic measurements and the docking simulations. Both the experimental and theoretical methods revealed that the chiral recognition of enantiomers in the presence of new chiral ionic liquids was enthalpy driven. The changes of the teicoplanin conformation occurring upon binding of the chiral ionic liquids are responsible for the differences in the standard changes in Gibbs energy (ΔG 0 ) values obtained for complexes formed by the R and S enantiomers and teicoplanin. Docking simulations revealed the steric adjustment between the chiral ionic liquids cyclohexane ring (chair conformation) and the β-d-glucosamine ring of teicoplanin and additionally hydrophobic interactions between the decanoic aliphatic chain of teicoplanin and the alkyl group of the tested salts. The obtained terpene derivatives can be considered as "structural task-specific ionic liquids" responsible for enhancing the chiral resolution in synergistic systems with two chiral selectors. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Methylgroup interaction of hydrocarbon stationary phases and hydrocarbon solutes

    NARCIS (Netherlands)

    Kemenade, van A.W.C.; Groenendijk, H.

    1969-01-01

    The temperature dependency of the retention behaviour of some alkanes with squalane as stationary phase has been measured at a very high precision level, at temperatures from 30 to 90°C. Besides the retention index itself [1], its temperature dependency appears to be a source of information about

  7. Evaluation of hydrophilic interaction liquid chromatography stationary phases for analysis of opium alkaloids.

    Science.gov (United States)

    Bagheri, Mohsen; Taheri, Mohammadreza; Farhadpour, Mohsen; Rezadoost, Hassan; Ghassempour, Alireza; Aboul-Enein, Hassan Y

    2017-08-18

    The separation of a mixture containing five major opium alkaloids, namely morphine, codeine, thebaine, noscapine and papaverine has been investigated in hydrophilic interaction liquid chromatography (HILIC) mode using five different stationary phases: bare silica, zwitterion, aminopropyl, diol and cyanopropyl. In order to propose the appropriate column for separation and purification, retention behaviors of the five natural opioids have been studied on mentioned HILIC stationary phases. The mechanism of separation in diverse HILIC media, based on the formation of water-rich layer on surface of the HILIC stationary phases and the physicochemical properties of opium alkaloids, such as pKa (acidic pK) and the octanol-water distribution coefficient (log Do/w) are discussed. Chromatographic responses including modified limit of detection LOD m , signal to noise ratio (S/N) m , and defined modified R Sm have considered for suggestion of the suitable column for quantitative/qualitative and preparative purposes. According to the obtained results, diol stationary phase is best suited for analytical chromatography, whereas bare silica and zwitterionic stationary phases are appropriate for preparative applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Evaluation of ODS-AQ stationary phase for use in capillary electrochromatography.

    Science.gov (United States)

    Djordjevic, N M; Fitzpatrick, F; Houdiere, F

    2001-04-01

    The aim of this study was to evaluate the applicability of ODS-AQ packing material as a stationary phase in capillary electrochromatography (CEC). The electroosmotic flow created on an ODS-AQ stationary phase was measured at different mobile phase compositions and at different column temperatures. It was observed that the electroosmotic flow generated in the column increased by 50% when the temperature of the system was raised from 20 degrees C to 60 degrees C, while all other conditions were kept constant. The electroosmotic flow produced by the ODS-AQ stationary phase was found to be comparable to the flow generated in a column packed with Nucleosil bare-silica material. In addition, a set of polar compounds (D-lysergic acid diethylamide derivatives) was utilized to determine the influence of temperature and mobile phase composition on their chromatographic behavior on an ODS-AQ stationary phase in a CEC mode. A linear relationship between the solute retention factor and column temperatures was seen over the temperature range studied (20 degrees C to 60 degrees C). A quadratic function was used to describe the changes in the solute retention factors with variation of acetonitrile concentration in the mobile phase.

  9. Polar silica-based stationary phases. Part II- Neutral silica stationary phases with surface bound maltose and sorbitol for hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Rathnasekara, Renuka; El Rassi, Ziad

    2017-07-28

    Two neutral polyhydroxylated silica bonded stationary phases, namely maltose-silica (MALT-silica) and sorbitol-silica (SOR-silica), have been introduced and chromatographically characterized in hydrophilic interaction liquid chromatography (HILIC) for a wide range of polar compounds. The bonding of the maltose and sorbitol to the silica surface was brought about by first converting bare silica to an epoxy-activated silica surface via reaction with γ-glycidoxypropyltrimethoxysilane (GPTMS) followed by attaching maltose and sorbitol to the epoxy surface in the presence of the Lewis acid catalyst BF 3 .ethereate. Both silica based columns offered the expected retention characteristics usually encountered for neutral polar surface. The retention mechanism is majorly based on solute' differential partitioning between an organic rich hydro-organic mobile phase (e.g., ACN rich mobile phase) and an adsorbed water layer on the surface of the stationary phase although additional hydrogen bonding was also responsible in some cases for solute retention. The MALT-silica column proved to be more hydrophilic and offered higher retention, separation efficiency and resolution than the SOR-silica column among the tested polar solutes such as derivatized mono- and oligosaccharides, weak phenolic acids, cyclic nucleotide monophosphate and nucleotide-5'-monophosphates, and weak bases, e.g., nucleobases and nucleosides. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

    Science.gov (United States)

    Sato, Kosuke; Oaki, Yuya; Takahashi, Daisuke; Toshima, Kazunobu; Imai, Hiroaki

    2015-03-23

    In biomineralization, acidic macromolecules play important roles for the growth control of crystals through a specific interaction. Inspired by this interaction, we report on an application of the hierarchical structures in CaCO3 biominerals to a stationary phase of chromatography. The separation and purification of acidic small organic molecules are achieved by thin-layer chromatography and flash chromatography using the powder of biominerals as the stationary phase. The unit nanocrystals and their oriented assembly, the hierarchical structure, are suitable for the adsorption site of the target organic molecules and the flow path of the elution solvents, respectively. The separation mode is ascribed to the specific adsorption of the acidic molecules on the crystal face and the coordination of the functional groups to the calcium ions. The results imply that a new family of stationary phase of chromatography can be developed by the fine tuning of hierarchical structures in CaCO3 materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Selectivity differences of water-soluble vitamins separated on hydrophilic interaction stationary phases.

    Science.gov (United States)

    Yang, Yuanzhong; Boysen, Reinhard I; Hearn, Milton T W

    2013-06-01

    In this study, the retention behavior and selectivity differences of water-soluble vitamins were evaluated with three types of polar stationary phases (i.e. an underivatized silica phase, an amide phase, and an amino phase) operated in the hydrophilic interaction chromatographic mode with ESI mass spectrometric detection. The effects of mobile phase composition, including buffer pH and concentration, on the retention and selectivity of the vitamins were investigated. In all stationary phases, the neutral or weakly charged vitamins exhibited very weak retention under each of the pH conditions, while the acidic and more basic vitamins showed diverse retention behaviors. With the underivatized silica phase, increasing the salt concentration of the mobile phase resulted in enhanced retention of the acidic vitamins, but decreased retention of the basic vitamins. These observations thus signify the involvement of secondary mechanisms, such as electrostatic interaction in the retention of these analytes. Under optimized conditions, a baseline separation of all vitamins was achieved with excellent peak efficiency. In addition, the effects of water content in the sample on retention and peak efficiency were examined, with sample stacking effects observed when the injected sample contained a high amount of water. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Comparison of a polymeric pseudostationary phase in EKC with ODS stationary phase in RP-HPLC.

    Science.gov (United States)

    Ni, Xinjiong; Zhang, Min; Xing, Xiaoping; Cao, Yuhua; Cao, Guangqun

    2018-01-01

    Poly(stearyl methacrylate-co-methacrylic acid) (P(SMA-co-MAA)) was induced as pseudostationary phase (PSP) in electrokinetic chromatography (EKC). The n-octadecyl groups in SMA were the same as that in octadecylsilane (ODS) C18 column. Thus, the present work focused on the comparison of selectivity between polymeric PSP and ODS stationary phase (SP), and the effect of organic modifiers on the selectivity of polymeric PSP and ODS SP. 1-butanol could directly interacted with PSP as a Class I modifier, and improved both of the methylene selectivity and polar group selectivity. When the analysis times were similar, the polymeric PSP exhibited better methylene selectivity and polar group selectivity. Although the hydrophobic groups were similar, the substituted benzenes elution order was different between polymeric PSP and ODS SP. Linear solvation energy relationships (LSER) model analysis found that polymeric PSP and ODS SP exhibited two same key factors in selectivity: hydrophobic interaction and hydrogen bonding acidity. But polymeric PSP exhibited relatively strong n- and π-electrons interaction to the analytes. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Amino-modified diamond as a durable stationary phase for solid-phase extraction.

    Science.gov (United States)

    Saini, Gaurav; Yang, Li; Lee, Milton L; Dadson, Andrew; Vail, Michael A; Linford, Matthew R

    2008-08-15

    We report the formation of a highly stable amino stationary phase on diamond and demonstrate its use in solid-phase extraction (SPE). This process consists of spontaneous and self-limiting adsorption of polyallylamine (PAAm) from aqueous solution onto oxidized diamond. Thermal curing under reduced pressure or chemical cross-linking with a diepoxide was shown to fix the polymer to the particles. The resulting adsorbents are stable under even extreme pH conditions (from at least pH 0-14) and significantly more stable than a commercially available amino SPE adsorbent. Coated diamond particles were characterized by X-ray photoelectron spectroscopy (XPS) and diffuse reflectance Fourier transform-infrared spectroscopy (DRIFT). Model silicon surfaces were characterized by spectroscopic ellipsometry and wetting. Solid-phase extraction was demonstrated using cholesterol, hexadecanedioic acid, and palmitoyloleoylphosphatidylcholine as analytes, and these results were compared to those obtained with commercially available materials. Breakthrough curves indicate that, as expected, porous diamond particles have higher analyte capacity than nonporous solid particles.

  14. Nanostructured pillars based on vertically aligned carbon nanotubes as the stationary phase in micro-CEC.

    Science.gov (United States)

    Wu, Ren-Guei; Yang, Chung-Shi; Wang, Pen-Cheng; Tseng, Fan-Gang

    2009-06-01

    We present a micro-CEC chip carrying out a highly efficient separation of dsDNA fragments through vertically aligned multi-wall carbon nanotubes (MWCNTs) in a microchannel. The vertically aligned MWCNTs were grown directly in the microchannel to form straight nanopillar arrays as ordered and directional chromatographic supports. 1-Pyrenedodecanoic acid was employed for the surface modification of the MWCNTs' stationary phase to adsorb analytes by hydrophobic interactions. This device was used for separating dsDNA fragments of three different lengths (254, 360, and 572 bp), and fluorescence detection was employed to verify the electrokinetic transport in the MWCNT array. The micro-CEC separation of the three compounds was achieved in less than 300 s at a field strength of 66 V/cm due to superior laminar flow patterns and a lower flow resistance resulting from the vertically aligned MWCNTs being used as the stationary phase medium. In addition, a fivefold reduction of band broadening was obtained when the analyte was separated by the chromatographic MWCNT array channel instead of the CE channel. From all of the results, we suggest that an in situ grown and directional MWCNT array can potentially be useful for preparing more diversified forms of stationary phases for vertically efficient chip-based electrochromatography.

  15. The Proteome and Lipidome of Thermococcus kodakarensis across the Stationary Phase

    OpenAIRE

    Gagen, Emma J.; Yoshinaga, Marcos Y.; Garcia Prado, Franka; Hinrichs, Kai-Uwe; Thomm, Michael

    2016-01-01

    The majority of cells in nature probably exist in a stationary-phase-like state, due to nutrient limitation in most environments. Studies on bacteria and yeast reveal morphological and physiological changes throughout the stationary phase, which lead to an increased ability to survive prolonged nutrient limitation. However, there is little information on archaeal stationary phase responses. We investigated protein- and lipid-level changes in Thermococcus kodakarensis with extended time in the...

  16. Temporal transcriptomic analysis of Desulfovibrio vulgaris Hildenborough transition into stationary phase growth during electrondonor depletion

    Energy Technology Data Exchange (ETDEWEB)

    Clark, M.E.; He, Q.; He, Z.; Huang, K.H.; Alm, E.J.; Wan, X.-F.; Hazen, T.C.; Arkin, A.P.; Wall, J.D.; Zhou, J.-Z.; Fields, M.W.

    2006-08-01

    Desulfovibrio vulgaris was cultivated in a defined medium, and biomass was sampled for approximately 70 h to characterize the shifts in gene expression as cells transitioned from the exponential to the stationary phase during electron donor depletion. In addition to temporal transcriptomics, total protein, carbohydrate, lactate, acetate, and sulfate levels were measured. The microarray data were examined for statistically significant expression changes, hierarchical cluster analysis, and promoter element prediction and were validated by quantitative PCR. As the cells transitioned from the exponential phase to the stationary phase, a majority of the down-expressed genes were involved in translation and transcription, and this trend continued at the remaining times. There were general increases in relative expression for intracellular trafficking and secretion, ion transport, and coenzyme metabolism as the cells entered the stationary phase. As expected, the DNA replication machinery was down-expressed, and the expression of genes involved in DNA repair increased during the stationary phase. Genes involved in amino acid acquisition, carbohydrate metabolism, energy production, and cell envelope biogenesis did not exhibit uniform transcriptional responses. Interestingly, most phage-related genes were up-expressed at the onset of the stationary phase. This result suggested that nutrient depletion may affect community dynamics and DNA transfer mechanisms of sulfate-reducing bacteria via the phage cycle. The putative feoAB system (in addition to other presumptive iron metabolism genes) was significantly up-expressed, and this suggested the possible importance of Fe{sup 2+} acquisition under metal-reducing conditions. The expression of a large subset of carbohydrate-related genes was altered, and the total cellular carbohydrate levels declined during the growth phase transition. Interestingly, the D. vulgaris genome does not contain a putative rpoS gene, a common attribute

  17. Fundamental and practical studies on high-performance liquid affinity chromatography of biopolymers with novel stationary phases

    Energy Technology Data Exchange (ETDEWEB)

    Bacolod, M.D.

    1992-01-01

    Rigid microparticulate stationary phases having surface-bound metal chelating functions were developed and evaluated in high performance metal chelate affinity chromatography of proteins. Silica- and polystyrene-divinylbenzene-based metal chelate sorbents were produced in wide pore and in non-porous type of column packings. A major effort has been placed on development of non-porous highly crosslinked polystyrene-divinylbenzene (PSDVB). These PSDVB microparticles were produced by a two-step swelling polymerization, and exhibited excellent mechanical strength over a wide range of flow-rates and composition used in high performance liquid chromatography (HPLC). Simple and reproducible hydrophilic coatings were developed for the surface modification of hydrophobic PSDVB supports. A tetradentate metal chelating ligand, ethylenediamine-N, N[prime]-diacetic acid (EDDA), was covalently bound to the surface of the various supports. Sorbents having iminodiacetic acid (IDA) metal chelating functions were also evaluated. The hydrophilic character and surface coverage of various stationary phases were assessed chromatographically. Studies concerning the effects of eluent pH as well as the nature and concentration of salts on retention and selectivity with different metal chelate stationary phases having various immobilized metal ions were carried out. Elution schemes were developed for rapid separation of proteins in metal chelate affinity chromatography. EDDA stationary phases in metal forms can be viewed as complementary to IDA stationary phases since they afforded different selectivity and retentivity toward proteins. Hydrophilic PSDVB could be functionalized with IDA or EDDA metal chelating ligands or lectins. The non-porous metal chelate stationary phases afforded rapid separation of proteins by the development of multiple gradient systems, which permitted higher column peak capacity, enabling the separation of a greater number of proteins in a single chromatographic run.

  18. Prolonged Stationary-Phase Incubation Selects for lrp Mutations in Escherichia coli K-12

    Science.gov (United States)

    Zinser, Erik R.; Kolter, Roberto

    2000-01-01

    Evolution by natural selection occurs in cultures of Escherichia coli maintained under carbon starvation stress. Mutants of increased fitness express a growth advantage in stationary phase (GASP) phenotype, enabling them to grow and displace the parent as the majority population. The first GASP mutation was identified as a loss-of-function allele of rpoS, encoding the stationary-phase global regulator, ςS (M. M. Zambrano, D. A. Siegele, M. A. Almirón, A. Tormo, and R. Kolter, Science 259:1757–1760, 1993). We now report that a second global regulator, Lrp, can also play a role in stationary-phase competition. We found that a mutant that took over an aged culture of an rpoS strain had acquired a GASP mutation in lrp. This GASP allele, lrp-1141, encodes a mutant protein lacking the critical glycine in the turn of the helix-turn-helix DNA-binding domain. The lrp-1141 allele behaves as a null mutation when in single copy and is dominant negative when overexpressed. Hence, the mutant protein appears to retain stability and the ability to dimerize but lacks DNA-binding activity. We also demonstrated that a lrp null allele generated by a transposon insertion has a fitness gain identical to that of the lrp-1141 allele, verifying that cells lacking Lrp activity have a competitive advantage during prolonged starvation. Finally, we tested by genetic analysis the hypothesis that the lrp-1141 GASP mutation confers a fitness gain by enhancing amino acid catabolism during carbon starvation. We found that while amino acid catabolism may play a role, it is not necessary for the lrp GASP phenotype, and hence the lrp GASP phenotype is due to more global physiological changes. PMID:10894750

  19. Synthesis and characterization of mesoporous silica modified with chiral auxiliaries for their potential application as chiral stationary phase.

    Science.gov (United States)

    Mayani, Vishal J; Abdi, S H R; Kureshy, R I; Khan, N H; Agrawal, Santosh; Jasra, R V

    2008-05-16

    Novel chiral stationary phase (CSP) based on chiral aminoalcohol immobilized on ordered mesoporous silica SBA-15 1a and standard silica 1b and their copper complexes 1a' and 1b', respectively, was synthesized as potential material for chiral ligand exchange chromatography (CLEC). Microanalysis, inductively coupled plasma spectroscopy (ICP), thermo-gravimetric analysis (TGA), cross polarized magic angle spinning (CP-MAS) (13)C NMR, Powder X-ray diffraction (PXRD), FTIR, N(2) adsorption isotherm, scanning electron microscopy (SEM), transmitted electron microscope (TEM) and solid reflectance UV-vis spectroscopy were used to characterize these materials. All the chiral stationary phases thus synthesized were used for the separation of different racemic compounds such as mandelic acid, 2,2'-dihydroxy-1,1'-binaphthalene BINOL) and diethyl tartrate by simple medium-pressure column chromatography. Successful enantio-separation of racemic mandelic acid was achieved with all the stationary phases but 1a and 1b gave slightly better resolution than their copper complexes 1a' and 1b'. Remarkably these materials are stable under the given experimental conditions and can be used repeatedly for several cycles of enantioresolution. It was observed that the porosity and surface area of the stationary phase play an important role in the chiral separation.

  20. Modelling of Hydrophilic Interaction Liquid Chromatography Stationary Phases Using Chemometric Approaches

    Science.gov (United States)

    Ortiz-Villanueva, Elena; Tauler, Romà

    2017-01-01

    Metabolomics is a powerful and widely used approach that aims to screen endogenous small molecules (metabolites) of different families present in biological samples. The large variety of compounds to be determined and their wide diversity of physical and chemical properties have promoted the development of different types of hydrophilic interaction liquid chromatography (HILIC) stationary phases. However, the selection of the most suitable HILIC stationary phase is not straightforward. In this work, four different HILIC stationary phases have been compared to evaluate their potential application for the analysis of a complex mixture of metabolites, a situation similar to that found in non-targeted metabolomics studies. The obtained chromatographic data were analyzed by different chemometric methods to explore the behavior of the considered stationary phases. ANOVA-simultaneous component analysis (ASCA), principal component analysis (PCA) and partial least squares regression (PLS) were used to explore the experimental factors affecting the stationary phase performance, the main similarities and differences among chromatographic conditions used (stationary phase and pH) and the molecular descriptors most useful to understand the behavior of each stationary phase. PMID:29064436

  1. Bacteriophage T4 Infection of Stationary Phase E. coli: Life after Log from a Phage Perspective

    Directory of Open Access Journals (Sweden)

    Elizabeth Martin Kutter

    2016-09-01

    Full Text Available Virtually all studies of phage infections investigate bacteria growing exponentially in rich media. In nature, however, phages largely encounter non-growing cells. Bacteria entering stationary phase often activate well-studied stress defense mechanisms that drastically alter the cell, facilitating its long-term survival. An understanding of phage-host interactions in such conditions is of major importance from both an ecological and therapeutic standpoint. Here, we show that bacteriophage T4 can efficiently bind to, infect and kill E. coli in stationary phase, both in the presence and absence of a functional stationary-phase sigma factor, and explore the response of T4-infected stationary phase cells to the addition of fresh nutrients 5 or 24 hours after that infection. An unexpected new mode of response has been identified. Hibernation mode is a persistent but reversible dormant state in which the infected cells make at least some phage enzymes, but halt phage development until appropriate nutrients become available before producing phage particles. Our evidence indicates that the block in hibernation mode occurs after the middle-mode stage of phage development; host DNA breakdown and the incorporation of the released nucleotides into phage DNA indicate that the enzymes of the nucleotide synthesizing complex, under middle-mode control, have been made and assembled into a functional state. Once fresh glucose and amino acids become available, the standard lytic infection process rapidly resumes and concentrations of up to 1011 progeny phage (an average of about 40 phage per initially-present cell are produced. All evidence is consistent with the hibernation-mode control point lying between middle mode and late mode T4 gene expression. We have also observed a scavenger response, where the infecting phage takes advantage of whatever few nutrients are available to produce small quantities of progeny within 2 to 5 hours after infection. The scavenger

  2. Ceramic stationary gas turbine development. Final report, Phase 1

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-09-01

    This report summarizes work performed by Solar Turbines Inc. and its subcontractors during the period September 25, 1992 through April 30, 1993. The objective of the work is to improve the performance of stationary gas turbines in cogeneration through implementation of selected ceramic components.

  3. 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.

  4. Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

    Science.gov (United States)

    Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

    2016-01-01

    A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Haemophilus ducreyi Hfq contributes to virulence gene regulation as cells enter stationary phase.

    Science.gov (United States)

    Gangaiah, Dharanesh; Labandeira-Rey, Maria; Zhang, Xinjun; Fortney, Kate R; Ellinger, Sheila; Zwickl, Beth; Baker, Beth; Liu, Yunlong; Janowicz, Diane M; Katz, Barry P; Brautigam, Chad A; Munson, Robert S; Hansen, Eric J; Spinola, Stanley M

    2014-02-11

    To adapt to stresses encountered in stationary phase, Gram-negative bacteria utilize the alternative sigma factor RpoS. However, some species lack RpoS; thus, it is unclear how stationary-phase adaptation is regulated in these organisms. Here we defined the growth-phase-dependent transcriptomes of Haemophilus ducreyi, which lacks an RpoS homolog. Compared to mid-log-phase organisms, cells harvested from the stationary phase upregulated genes encoding several virulence determinants and a homolog of hfq. Insertional inactivation of hfq altered the expression of ~16% of the H. ducreyi genes. Importantly, there were a significant overlap and an inverse correlation in the transcript levels of genes differentially expressed in the hfq inactivation mutant relative to its parent and the genes differentially expressed in stationary phase relative to mid-log phase in the parent. Inactivation of hfq downregulated genes in the flp-tad and lspB-lspA2 operons, which encode several virulence determinants. To comply with FDA guidelines for human inoculation experiments, an unmarked hfq deletion mutant was constructed and was fully attenuated for virulence in humans. Inactivation or deletion of hfq downregulated Flp1 and impaired the ability of H. ducreyi to form microcolonies, downregulated DsrA and rendered H. ducreyi serum susceptible, and downregulated LspB and LspA2, which allow H. ducreyi to resist phagocytosis. We propose that, in the absence of an RpoS homolog, Hfq serves as a major contributor of H. ducreyi stationary-phase and virulence gene regulation. The contribution of Hfq to stationary-phase gene regulation may have broad implications for other organisms that lack an RpoS homolog. Pathogenic bacteria encounter a wide range of stresses in their hosts, including nutrient limitation; the ability to sense and respond to such stresses is crucial for bacterial pathogens to successfully establish an infection. Gram-negative bacteria frequently utilize the alternative sigma

  6. Evaluation of gamma radiation effects on stationary phases using gas chromatografy

    International Nuclear Information System (INIS)

    Basso, M.A.; Collins, K.E.; Collins, C.H.

    1988-01-01

    The overall objetive of this project is a thorough study of the effect of gamma radiation on supported stationary phases used in packed-column gas chromatography. The phases studied were SP-2100 on Supelcoport and SE-30 on Chromsorb W. The fases were irradiated with cobalt-60 gamma rays to various doses and subsequently subjected to tests of extractability, termal stability and efficiency as a chromatographic column packing. Extraction tests indicate that low doses of radiation are sufficient to produce significant immobilization of these polymethylsilicones; that is, to produce chemical bonds between different polymer chains or between the stationary phase and the support. Thermal stability is also increased. The values calculated for the number of theoretical plates (n) and resolution (Rsub (s)) after analysis of four synthetic mixtures of organic compounds also increase, in most cases, indicating that the gamma irradiation has positively altered the behavior of these stationary phases. (author) [pt

  7. The Proteome and Lipidome of Thermococcus kodakarensis across the Stationary Phase.

    Science.gov (United States)

    Gagen, Emma J; Yoshinaga, Marcos Y; Garcia Prado, Franka; Hinrichs, Kai-Uwe; Thomm, Michael

    2016-01-01

    The majority of cells in nature probably exist in a stationary-phase-like state, due to nutrient limitation in most environments. Studies on bacteria and yeast reveal morphological and physiological changes throughout the stationary phase, which lead to an increased ability to survive prolonged nutrient limitation. However, there is little information on archaeal stationary phase responses. We investigated protein- and lipid-level changes in Thermococcus kodakarensis with extended time in the stationary phase. Adaptations to time in stationary phase included increased proportion of membrane lipids with a tetraether backbone, synthesis of proteins that ensure translational fidelity, specific regulation of ABC transporters (upregulation of some, downregulation of others), and upregulation of proteins involved in coenzyme production. Given that the biological mechanism of tetraether synthesis is unknown, we also considered whether any of the protein-level changes in T. kodakarensis might shed light on the production of tetraether lipids across the same period. A putative carbon-nitrogen hydrolase, a TldE (a protease in Escherichia coli) homologue, and a membrane bound hydrogenase complex subunit were candidates for possible involvement in tetraether-related reactions, while upregulation of adenosylcobalamin synthesis proteins might lend support to a possible radical mechanism as a trigger for tetraether synthesis.

  8. The Proteome and Lipidome of Thermococcus kodakarensis across the Stationary Phase

    Directory of Open Access Journals (Sweden)

    Emma J. Gagen

    2016-01-01

    Full Text Available The majority of cells in nature probably exist in a stationary-phase-like state, due to nutrient limitation in most environments. Studies on bacteria and yeast reveal morphological and physiological changes throughout the stationary phase, which lead to an increased ability to survive prolonged nutrient limitation. However, there is little information on archaeal stationary phase responses. We investigated protein- and lipid-level changes in Thermococcus kodakarensis with extended time in the stationary phase. Adaptations to time in stationary phase included increased proportion of membrane lipids with a tetraether backbone, synthesis of proteins that ensure translational fidelity, specific regulation of ABC transporters (upregulation of some, downregulation of others, and upregulation of proteins involved in coenzyme production. Given that the biological mechanism of tetraether synthesis is unknown, we also considered whether any of the protein-level changes in T. kodakarensis might shed light on the production of tetraether lipids across the same period. A putative carbon-nitrogen hydrolase, a TldE (a protease in Escherichia coli homologue, and a membrane bound hydrogenase complex subunit were candidates for possible involvement in tetraether-related reactions, while upregulation of adenosylcobalamin synthesis proteins might lend support to a possible radical mechanism as a trigger for tetraether synthesis.

  9. Chelating agents as stationary phase in extraction chromatography, ch. 11

    International Nuclear Information System (INIS)

    Sebesta, F.

    1975-01-01

    Chelating agents have been used largely in extraction chromatography for separations related to activation analysis, for concentration of metals from dilute solutions, and for preparation of radiochemically pure or carrier-free radionuclides. This review deals with the theory of extraction by chelating agents, the experimental technique, and the chelating agents and systems used (β-diketones, oximes, hydroxamic acid, dithizone and diethyldithiocarbamic acid)

  10. The effect of charged groups on hydrophilic monolithic stationary phases on their chromatographic properties.

    Science.gov (United States)

    Li, Haibin; Liu, Chusheng; Wang, Qiqin; Zhou, Haibo; Jiang, Zhengjin

    2016-10-21

    In order to investigate the effect of charged groups present in hydrophilic monolithic stationary phases on their chromatographic properties, three charged hydrophilic monomers, i.e. N,N-dimethyl-N-acryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPDA), [2-(acryloyloxy)ethyl]trimethylammonium chloride (AETA), and 3-sulfopropyl acrylate potassium salt (SPA) were co-polymerized with the crosslinker N,N'-methylenebisacrylamide (MBA), respectively. The physicochemical properties of the three resulting charged hydrophilic monolithic columns were evaluated using scanning electron microscopy, ζ-potential analysis and micro-HPLC. High column efficiency was obtained on the three monolithic columns at a linear velocity of 1mm/s using thiourea as test compound. Comparative characterization of the three charged HILIC phases was then carried out using a set of model compounds, including nucleobases, nucleosides, benzoic acid derivatives, phenols, β-blockers and small peptides. Depending on the combination of stationary phase/mobile phase/solute, both hydrophilic interaction and other potential secondary interactions, including electrostatic interaction, hydrogen-bonding interaction, molecular shape selectivity, could contribute to the over-all retention of the analytes. Because of the strong electrostatic interaction provided by the quaternary ammonium groups in the poly (AETA-co-MBA) monolith, this cationic HILIC monolith exhibited the strongest retention for benzoic acid derivatives and small peptides with distorted peak shapes and the weakest retention for basic β-blockers. The sulfonyl groups on the poly (SPA-co-MBA) hydrophilic monolith could provide strong electrostatic attraction and hydrogen bonding for positively charged analytes and hydrogen-donor/acceptor containing analytes, respectively. Therefore, basic drugs, nucleobases and nucleotides exhibited the strongest retention on this anionic monolith. Because of the weak but distinct cation exchange properties of

  11. Molecular theory of chromatography for blocklike solutes in anisotropic stationary phases and its application

    International Nuclear Information System (INIS)

    Yan, Chao; Martire, D.E.

    1992-01-01

    DiMarzio's lattice model is successfully applied to describe the equilibrium partitioning of blocklike molecules between an isotropic mobile phase and an anisotropic stationary phase in various types of fluid chromatography to obtain a retention equation. A linear relationship between the logarithm of the solute distribution coefficient and minimum area is predicted. 44 refs., 8 figs., 2 tabs

  12. Recent progress of chiral stationary phases for separation of enantiomers in gas chromatography.

    Science.gov (United States)

    Xie, Sheng-Ming; Yuan, Li-Ming

    2017-01-01

    Chromatography techniques based on chiral stationary phases are widely used for the separation of enantiomers. In particular, gas chromatography has developed rapidly in recent years due to its merits such as fast analysis speed, lower consumption of stationary phases and analytes, higher column efficiency, making it a better choice for chiral separation in diverse industries. This article summarizes recent progress of novel chiral stationary phases based on cyclofructan derivatives and chiral porous materials including chiral metal-organic frameworks, chiral porous organic frameworks, chiral inorganic mesoporous materials, and chiral porous organic cages in gas chromatography, covering original research papers published since 2010. The chiral recognition properties and mechanisms of separation toward enantiomers are also introduced. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Modifying effect of caffeine on cell radiosensitivity in stationary and logarithmic phases of growth

    International Nuclear Information System (INIS)

    Plotnikova, E.D.; Kostenko, G.A.

    1978-01-01

    Studied was reproductive killing of cultivated fibroblasts of a Chinese hamster in stationary and exponential growth phases after gamma irradiation. After cell irradiation in a stationary phase at 1200 rad dose rate and postirradiation incubation in conditioned medium before resowing for 5 hrs the survival rate increased almost 5 times due to the reparation of potential-lethal injuries. Under sodium caffein-benzoate (4 mg/ml) effect on cells in a stationary growth phase for 5 hrs before irradiation the survival rate increased; protection level was almost the same as in case of reduction in a conditioned media. Modification factor of dose curve incline was 1.3. Caffein protective effect may be conjectured to relate to the inhibition of potentially-lethal injury fraction realization

  14. Metal-Organic Framework Thin Films as Stationary Phases in Microfabricated Gas-Chromatography Columns.

    Energy Technology Data Exchange (ETDEWEB)

    Read, Douglas [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sillerud, Colin Halliday [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-01-01

    The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

  15. Considerations of stationary-phase interactions in groundwater pollution studies

    International Nuclear Information System (INIS)

    Hall, E.S.

    1980-01-01

    Studies of groundwater pollution are complicated by retention of both pollutant and tracers as static phases associated with the rock matrix. Three types of static phase are considered: (1) immobile pore water, (2) equilibrium adsorbed layers and (3) bulk precipitates, including biological systems. A brief discussion of the systems is given with examples from the work of the Water Research Centre on the problems encountered in quantifying groundwater pollution where static contamination may occur. (author)

  16. 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.

  17. High-performance liquid chromatography using reversed-phase stationary phases dynamically modified with organophosphorus compound for the separation and determination of lanthanoid elements

    International Nuclear Information System (INIS)

    Tsuyoshi, Akira; Akiba, Kenichi

    2000-01-01

    An acidic organophosphorus compound, 2-ethylhexylphosphonic acid mono-2-ethlhexyl ester (EHPA), has been applied to reversed-phase high-performance liquid chromatography (RP-HPLC). The reversed-phase stationary phase was dynamically modified with EHPA by flowing the mobile phase of an acetone-water mixture containing the extracting regent. The retention of lanthanoid elements was widely varied by changing the conditions of the mobile phase, i.e., the pH, the EHPA concentration and the acetone content. The selectivity of EHPA is well reflected to the chromatographic systems, and a precise separation of lanthanoid elements was achieved with sufficient resolution. The determination of Sm was examined in the presence of a large amount of Nd. A linear calibration graph was obtained for Sm at the level of 10 -7 mol dm -3 , in the presence of 1x10 -4 mol dm -3 of Nd. (author)

  18. Peptidoglycan Recycling in Gram-Positive Bacteria Is Crucial for Survival in Stationary Phase

    Science.gov (United States)

    Borisova, Marina; Gaupp, Rosmarie; Duckworth, Amanda; Schneider, Alexander; Dalügge, Désirée; Mühleck, Maraike; Deubel, Denise; Unsleber, Sandra; Yu, Wenqi; Muth, Günther; Bischoff, Markus; Götz, Friedrich

    2016-01-01

    ABSTRACT Peptidoglycan recycling is a metabolic process by which Gram-negative bacteria reutilize up to half of their cell wall within one generation during vegetative growth. Whether peptidoglycan recycling also occurs in Gram-positive bacteria has so far remained unclear. We show here that three Gram-positive model organisms, Staphylococcus aureus, Bacillus subtilis, and Streptomyces coelicolor, all recycle the sugar N-acetylmuramic acid (MurNAc) of their peptidoglycan during growth in rich medium. They possess MurNAc-6-phosphate (MurNAc-6P) etherase (MurQ in E. coli) enzymes, which are responsible for the intracellular conversion of MurNAc-6P to N-acetylglucosamine-6-phosphate and d-lactate. By applying mass spectrometry, we observed accumulation of MurNAc-6P in MurNAc-6P etherase deletion mutants but not in either the isogenic parental strains or complemented strains, suggesting that MurQ orthologs are required for the recycling of cell wall-derived MurNAc in these bacteria. Quantification of MurNAc-6P in ΔmurQ cells of S. aureus and B. subtilis revealed small amounts during exponential growth phase (0.19 nmol and 0.03 nmol, respectively, per ml of cells at an optical density at 600 nm [OD600] of 1) but large amounts during transition (0.56 nmol and 0.52 nmol) and stationary (0.53 nmol and 1.36 nmol) phases. The addition of MurNAc to ΔmurQ cultures greatly increased the levels of intracellular MurNAc-6P in all growth phases. The ΔmurQ mutants of S. aureus and B. subtilis showed no growth deficiency in rich medium compared to the growth of the respective parental strains, but intriguingly, they had a severe survival disadvantage in late stationary phase. Thus, although peptidoglycan recycling is apparently not essential for the growth of Gram-positive bacteria, it provides a benefit for long-term survival. PMID:27729505

  19. Stationary two-phase flow evaluation by the dynamic slip model

    International Nuclear Information System (INIS)

    Stevanovic, D.

    1986-01-01

    The equations which describe a dynamic slip model for stationary conditions are given in the paper. The basic solving procedure by the code DVOF4 is briefly described. The results are verified on the experiment FRIGG 313014. besides the void fraction and the vapor and liquid phase temperatures, the following parameters are plotted and explained: vapor phase generation rate, vapor and liquid phase velocities, slip between the phases, interfacial surface, friction drag between each phase and the wall, two-phase flow friction multiplier and pressure drop along the channel. (author)

  20. 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.

  1. Assessment of the chromatographic lipophilicity of eight cephalosporins on different stationary phases.

    Science.gov (United States)

    Dąbrowska, Monika; Starek, Małgorzata; Komsta, Łukasz; Szafrański, Przemysław; Stasiewicz-Urban, Anna; Opoka, Włodzimierz

    2017-04-01

    The retention behaviors were investigated for a series of eight cephalosporins in thin-layer chromatography (TLC) using stationary phases of RP-2, RP-8, RP-18, NH 2 , DIOL, and CN chemically bonded silica gel. Additionally, various binary mobile phases (water/methanol and water/acetone) were used in different volume proportions. The retention behavior of the analyzed molecules was defined by R M0 constant. In addition, reversed phase high performance liquid chromatography (RP-HPLC) was performed in lipophilicity studies by using immobilized artificial membrane (IAM) stationary phase. Obtained chromatographic data (R M0 and logk' IAM ) were correlated with the lipophilicity, expressed as values of the log calculated (logP calc ) and experimental (logP exp(shake-flask) ) partition coefficient. Principal component analysis (PCA) was applied in order to obtain an overview of similarity or dissimilarity among the analyzed compounds. Hierarchical cluster analysis (HCA) was performed to compare the separation characteristics of the applied stationary phases. This study was undertaken to identify the best chromatographic system and chromatographic data processing method to enable the prediction of logP values. A comprehensive chromatographic investigation into the retention of the analyzed cephalosporins revealed a similar behavior on RP-18, RP-8 and CN stationary phases. The weak correlations obtained between experimental and certain computed lipophilicity indices revealed that R M0 and PC1/RM are relevant lipophilicity parameters and the RP-8, CN and RP-18 plates are appropriate stationary phases for lipophilicity investigation, whereas computational approaches still cannot fully replace experimentation. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Convergence to stationary solutions for a parabolic-hyperbolic phase-field system

    Czech Academy of Sciences Publication Activity Database

    Grasselli, M.; Petzeltová, Hana; Schimperna, G.

    2006-01-01

    Roč. 5, č. 4 (2006), s. 827-838 ISSN 1534-0392 R&D Projects: GA AV ČR(CZ) IAA1019302 Institutional research plan: CEZ:AV0Z10190503 Keywords : phase-field models * convergence to stationary solutions * Łojasiewicz-Simon inequality Subject RIV: BA - General Mathematics Impact factor: 0.857, year: 2006

  3. Carbon nanotube based stationary phases for microchip chromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Kutter, Jörg Peter

    2012-01-01

    already been demonstrated in more classical formats, for improved separation performance in gas and liquid chromatography, and for unique applications in solid phase extraction. Carbon nanotubes are now also entering the field of microfluidics, where there is a large potential to be able to provide......The objective of this article is to provide an overview and critical evaluation of the use of carbon nanotubes and related carbon-based nanomaterials for microchip chromatography. The unique properties of carbon nanotubes, such as a very high surface area and intriguing adsorptive behaviour, have...... integrated, tailor-made nanotube columns by means of catalytic growth of the nanotubes inside the fluidic channels. An evaluation of the different implementations of carbon nanotubes and related carbon-based nanomaterials for microfluidic chromatography devices is given in terms of separation performance...

  4. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    International Nuclear Information System (INIS)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m"−"1. The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  5. Synthesis and Purification of Iodoaziridines Involving Quantitative Selection of the Optimal Stationary Phase for Chromatography

    Science.gov (United States)

    Boultwood, Tom; Affron, Dominic P.; Bull, James A.

    2014-01-01

    The highly diastereoselective preparation of cis-N-Ts-iodoaziridines through reaction of diiodomethyllithium with N-Ts aldimines is described. Diiodomethyllithium is prepared by the deprotonation of diiodomethane with LiHMDS, in a THF/diethyl ether mixture, at -78 °Cin the dark. These conditions are essential for the stability of the LiCHI2 reagent generated. The subsequent dropwise addition of N-Ts aldimines to the preformed diiodomethyllithium solution affords an amino-diiodide intermediate, which is not isolated. Rapid warming of the reaction mixture to 0 °C promotes cyclization to afford iodoaziridines with exclusive cis-diastereoselectivity. The addition and cyclization stages of the reaction are mediated in one reaction flask by careful temperature control. Due to the sensitivity of the iodoaziridines to purification, assessment of suitable methods of purification is required. A protocol to assess the stability of sensitive compounds to stationary phases for column chromatography is described. This method is suitable to apply to new iodoaziridines, or other potentially sensitive novel compounds. Consequently this method may find application in range of synthetic projects. The procedure involves firstly the assessment of the reaction yield, prior to purification, by 1H NMR spectroscopy with comparison to an internal standard. Portions of impure product mixture are then exposed to slurries of various stationary phases appropriate for chromatography, in a solvent system suitable as the eluent in flash chromatography. After stirring for 30 min to mimic chromatography, followed by filtering, the samples are analyzed by 1H NMR spectroscopy. Calculated yields for each stationary phase are then compared to that initially obtained from the crude reaction mixture. The results obtained provide a quantitative assessment of the stability of the compound to the different stationary phases; hence the optimal can be selected. The choice of basic alumina, modified to

  6. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng, E-mail: cesoygf@mail.sysu.edu.cn

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m{sup −1}. The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  7. Tubing modifications for countercurrent chromatography (CCC): Stationary phase retention and separation efficiency.

    Science.gov (United States)

    Englert, Michael; Vetter, Walter

    2015-07-16

    Countercurrent chromatography (CCC) is a separation technique in which two immiscible liquid phases are used for the preparative purification of synthetic and natural products. In CCC the number of repetitive mixing and de-mixing processes, the retention of the stationary phase and the mass transfer between the liquid phases are significant parameters that influence the resolution and separation efficiency. Limited mass transfer is the main reason for peak broadening and a low number of theoretical plates along with impaired peak resolution in CCC. Hence, technical improvements with regard to column design and tubing modifications is an important aspect to enhance mixing and mass transfer. In this study we constructed a crimping tool which allowed us to make reproducible, semi-automated modifications of conventional round-shaped tubing. Six crimped tubing modifications were prepared, mounted onto multilayer coils which were subsequently installed in the CCC system. The stationary phase retention of the tubing modifications were compared to the conventional system with unmodified tubing in a hydrophobic, an intermediate and a hydrophilic two-phase solvent system. Generally, the tubing modifications provided higher capabilities to retain the stationary phase depending on the solvent system and flow rates. In the intermediate solvent system the separation efficiency was evaluated with a mixture of six alkyl p-hydroxybenzoates. The peak resolution could be increased up to 50% with one of the tubing modifications compared to the unmodified tubing. Using the most convincing tubing modification at fixed values for the stationary phase retention, a reasonable comparison to the unmodified tubing was achieved. The peak width could be reduced up to 49% and a strong positive impact at increased flow rates regarding peak resolution and theoretical plate number was observed compared to unmodified tubing. It could be concluded that the tubing modification enhanced the interphase

  8. Quantitation of anticonvulsant drugs in serum by gas-chromatography on the stationary phase SP-2510.

    Science.gov (United States)

    Godolphin, W; Thoma, J

    1978-03-01

    A new column packing, SP-2510 DA (Supelco, Inc., Bellefonte, Pa. 16823), is an excellent stationary phase for the determination of a wide variety of anticonvulsant drugs by gas--liquid chromatography without derivatization. However, when uncomplicated extraction procedures are used, serum cholesterol interferes with the determination of primidone. By the simple expedient of adding a short "pre-column" containing another phase (SP-2250 DA) the problem is overcome.

  9. Proteomic analysis of lactose-starved Lactobacillus casei during stationary growth phase.

    Science.gov (United States)

    Hussain, M A; Knight, M I; Britz, M L

    2009-03-01

    Starvation stress is a condition that nonstarter lactic acid bacteria (NSLAB) normally encounter. This study was aimed to investigate starvation-induced proteins in Lactobacillus casei during stationary growth phase. The impact of carbohydrate starvation on L. casei GCRL163 was investigated using two different media (a modified de Man, Rogosa and Sharpe broth and a semi-defined medium). Cells were grown in the presence of excess lactose (1%) or starvation (0%) and differences in the patterns of one-dimensional sodium dodecyl sulfate-polyacrylamide gel electrophoresis and two-dimensional electrophoresis of the cytosolic protein fractions were investigated. Differentially regulated proteins were identified by MALDI-TOF/TOF mass spectrometry. Many differentially regulated proteins were enzymes of various metabolic pathways involved in carbohydrate metabolism to yield energy. Differences in protein expression were also observed in the two culture conditions tested in this experiment. Numerous glycolytic enzymes were differentially regulated under lactose starvation. The differential expression of these glycolytic enzymes suggests a potential survival strategy under harsh growth conditions (i.e. lactose starvation). This paper reports improved understanding of stress responses and survival mechanism of NSLAB under lactose-depleted cheese-ripening condition. This knowledge of how NSLAB bacteria adapt to lactose starvation could be applied to predict the performances of bacteria in other industrial applications.

  10. Alkali Metal Modification of Silica Gel-Based Stationary Phase in Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

    Full Text Available Modification of the precipitated silica gel was done by treatment with alkali metal (NaCl before and after calcination. The silica surfaces before and after modification were confirmed by infrared spectroscopy in order to observe the strength and abundance of the acidic surface OH group bands which play an important role in the adsorption properties of polar and nonpolar solutes. The surface-modified silica gels were tested as GC solid stationary phases in terms of the separation efficiency for various groups of non-polar and polar solutes. Also, thermodynamic parameters (ΔH, ΔG, and ΔS were determined using n-hexane as a probe in order to show the adsorbate-adsorbent interaction. It was observed that the non-polar solutes could be separated Independent on the reactivity and porosity of the silica surfaces. The efficiency of the surface-modified silica gels to separate the aromatic hydrocarbons seemed to be strongly influenced by the density of the surface hydroxyls.

  11. Evaluation of an amide-based stationary phase for supercritical fluid chromatography

    Science.gov (United States)

    Borges-Muñoz, Amaris C.; Colón, Luis A.

    2017-01-01

    A relatively new stationary phase containing a polar group embedded in a hydrophobic backbone (i.e., ACE® C18-amide) was evaluated for use in supercritical fluid chromatography. The amide-based column was compared with columns packed with bare silica, C18 silica, and a terminal-amide silica phase. The system was held at supercritical pressure and temperature with a mobile phase composition of CO2 and methanol as cosolvent. The linear solvation energy relationship model was used to evaluate the behavior of these stationary phases, relating the retention factor of selected probes to specific chromatographic interactions. A five-component test mixture, consisting of a group of drug-like molecules was separated isocratically. The results show that the C18-amide stationary phase provided a combination of interactions contributing to the retention of the probe compounds. The hydrophobic interactions are favorable; however, the electron donating ability of the embedded amide group shows a large positive interaction. Under the chromatographic conditions used, the C18-amide column was able to provide baseline resolution of all the drug-like probe compounds in a text mixture, while the other columns tested did not. PMID:27396487

  12. A comparison of the radiosensitivity of stationary, exponential and G1 phase wild type and repair deficient yeast cultures: supporting evidence for stationary phase yeast cells being in G0

    International Nuclear Information System (INIS)

    Tippins, R.S.; Parry, J.M.

    1982-01-01

    The main points to emerge from this comparison of the radiosensitivity of stationary, exponential and G 1 phase yeast cultures were: (1) In wild type yeast cultures, G 1 cells were the most sensitive to the lethal effects of X-rays, exponential phase cells were the most resistant and stationary phase cells were intermediate in sensitivity. (2) With the excision-repair-defective strain D61-3 (rad 3) stationary phase cells were more resistant than exponential cells with G 1 cells again being most sensitive. (3) The rad 50 gene present in JD50 had a marked effect on the X-ray inactivation response of this strain. In the presence of the defective rad 50 allele, exponential phase cells were as sensitive as G 1 phase cells, with stationary phase cells being more resistant than either. (4) There were marked differences in sensitivity between stationary phase and G 1 phase cells. These differences, along with other physiological differences reported by other workers, lead the authors to suggest that stationary phase cells can be better described as being in G 0 phase, i.e. a stage which is outside the normal mitotic cell cycle of an exponential culture. (author)

  13. The extracellular proteome of Rhizobium etli CE3 in exponential and stationary growth phase

    Directory of Open Access Journals (Sweden)

    Mendoza-Hernández Guillermo

    2010-10-01

    Full Text Available Abstract Background The extracellular proteome or secretome of symbiotic bacteria like Rhizobium etli is presumed to be a key element of their infection strategy and survival. Rhizobia infect the roots of leguminous plants and establish a mutually beneficial symbiosis. To find out the possible role of secreted proteins we analyzed the extracellular proteome of R. etli CE3 in the exponential and stationary growth phases in minimal medium, supplemented with succinate-ammonium. Results The extracellular proteins were obtained by phenol extraction and identified by LC-ESI MS/MS. We identified 192 and 191 proteins for the exponential and stationary phases respectively. Using the software Signal P, we predicted signal peptides for 12.95% and 35.60% of the proteins identified in the exponential and stationary phases, respectively, which could therefore be secreted by the Sec pathway. For the exponential growth phase, we found in abundance proteins like the ribosomal proteins, toxins and proteins belonging to the group "defence mechanisms". For the stationary growth phase, we found that the most abundant proteins were those with unknown function, and in many of these we identified characteristic domains of proteases and peptidases. Conclusions Our study provided the first dataset of the secretome of R. etli and its modifications, which may lead to novel insights into the adaptive response of different stages of growth. In addition, we found a high number of proteins with unknown function; these proteins could be analyzed in future research to elucidate their role in the extracellular proteome of R. etli.

  14. Separation of piracetam derivatives on polysaccharide-based chiral stationary phases.

    Science.gov (United States)

    Kažoka, H; Koliškina, O; Veinberg, G; Vorona, M

    2013-03-15

    High-performance liquid chromatography was used for the enantiomeric separation of two chiral piracetam derivatives. The suitability of six commercially available polysaccharide-based chiral stationary phases (CSPs) under normal phase mode for direct enantioseparation has been investigated. The influence of the CSPs as well the nature and content of an alcoholic modifier in the mobile phase on separation and elution order was studied. It was established that CSP Lux Amylose-2 shows high chiral recognition ability towards 4-phenylsubstituted piracetam derivatives. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Hilbert and Blaschke phases in the temporal coherence function of stationary broadband light.

    Science.gov (United States)

    Fernández-Pousa, Carlos R; Maestre, Haroldo; Torregrosa, Adrián J; Capmany, Juan

    2008-10-27

    We show that the minimal phase of the temporal coherence function gamma (tau) of stationary light having a partially-coherent symmetric spectral peak can be computed as a relative logarithmic Hilbert transform of its amplitude with respect to its asymptotic behavior. The procedure is applied to experimental data from amplified spontaneous emission broadband sources in the 1.55 microm band with subpicosecond coherence times, providing examples of degrees of coherence with both minimal and non-minimal phase. In the latter case, the Blaschke phase is retrieved and the position of the Blaschke zeros determined.

  16. Strengthening of the DNA-protein complex during stationary phase aging of cell cultures

    International Nuclear Information System (INIS)

    Khokhlov, A.N.; Chirkova, E.Yu.; Gorin, A.I.

    1986-01-01

    The possibility of accumulation of cross-linkages in the DNA-protein complex was studied during stationary phase aging of cells in culture. Chinese hamster cells were used in the experiments, along with human fibroblasts. 3 H-thymidine, 14 C-valine, and 14 C-leucine were added to the medium. The quantity of protein firmly bound with DNA was judged from the value of the coefficient 14 C/ 3 H determined with allowance for penetration of counting from the 14 C-channel into the 3 H-channel. The authors maintain that the results presented in this paper provide further evidence of the value of stationary phase cell cultures for the study of the mechanisms of aging and also of some of the general principles underlying hereditary pathology

  17. Experimental comparison of chiral metal-organic framework used as stationary phase in chromatography.

    Science.gov (United States)

    Xie, Sheng-Ming; Zhang, Mei; Fei, Zhi-Xin; Yuan, Li-Ming

    2014-10-10

    Chiral metal-organic frameworks (MOFs) are a new class of multifunctional material, which possess diverse structures and unusual properties such as high surface area, uniform and permanent cavities, as well as good chemical and thermal stability. Their chiral functionality makes them attractive as novel enantioselective adsorbents and stationary phases in separation science. In this paper, the experimental comparison of a chiral MOF [In₃O(obb)₃(HCO₂)(H₂O)] solvent used as a stationary phase was investigated in gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC). The potential relationship between the structure and components of chiral MOFs with their chiral recognition ability and selectivity are presented. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Nutrient control for stationary phase cellulase production in Trichoderma reesei Rut C-30.

    Science.gov (United States)

    Callow, Nicholas V; Ray, Christopher S; Kelbly, Matthew A; Ju, Lu-Kwang

    2016-01-01

    This work describes the use of nutrient limitations with Trichoderma reesei Rut C-30 to obtain a prolonged stationary phase cellulase production. This period of non-growth may allow for dependable cellulase production, extended fermentation periods, and the possibility to use pellet morphology for easy product separation. Phosphorus limitation was successful in halting growth and had a corresponding specific cellulase production of 5±2 FPU/g-h. Combined with the addition of Triton X-100 for fungal pellet formation and low shear conditions, a stationary phase cellulase production period in excess of 300 h was achieved, with a constant enzyme production rate of 7±1 FPU/g-h. While nitrogen limitation was also effective as a growth limiter, it, however, also prevented cellulase production. Copyright © 2015 Elsevier Inc. All rights reserved.

  19. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Qifeng, E-mail: fuqifeng1990@163.com [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Zhang, Kailian; Gao, Die; Wang, Lujun [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Yang, Fengqing; Liu, Yao [School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China); Xia, Zhining, E-mail: tcm_anal_cqu@163.com [Innovative Drug Research Centre and School of Pharmaceutical Sciences, Chongqing University, Chongqing 400030 (China); School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China)

    2017-05-29

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  20. Copolymerization preparation of cationic cyclodextrin chiral stationary phases for drug enantioseparation in chromatography

    OpenAIRE

    sprotocols

    2015-01-01

    Authors: Ren-Qi Wang, Teng-Teng Ong, Ke Huang, Weihua Tang & Siu-Choon Ng ### Abstract We described a facile and effective protocol wherein radical copolymerization is employed to covalently bond cationic β-cyclodextrin (β-CD) onto silica particles with extended linkage, resulting in a chiral stationary phase (IMPCSP) that can be used for the enantioseparation of racemic drugs in both high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). Starting ...

  1. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    International Nuclear Information System (INIS)

    Fu, Qifeng; Zhang, Kailian; Gao, Die; Wang, Lujun; Yang, Fengqing; Liu, Yao; Xia, Zhining

    2017-01-01

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  2. Growth potential of exponential- and stationary-phase Salmonella Typhimurium during sausage fermentation

    DEFF Research Database (Denmark)

    Birk, Tina; Henriksen, Sidsel; Müller, K.

    2016-01-01

    - and stationary-phase Salmonella Typhimurium (DT12 and DTU292) during freezing at − 18 °C and their subsequent growth potential during 72 h sausage fermentation at 25 °C. After 0, 7 and > 35 d of frozen storage, sausage batters were prepared with NaCl (3%) and NaNO2 (0, 100 ppm) and fermented with and without...

  3. A 3-D open-framework material with intrinsic chiral topology used as a stationary phase in gas chromatography.

    Science.gov (United States)

    Xie, Sheng-Ming; Zhang, Xin-Huan; Zhang, Ze-Jun; Zhang, Mei; Jia, Jia; Yuan, Li-Ming

    2013-04-01

    Compared with liquid chromatography and capillary electrophoresis, the diversity of gas chromatography chiral stationary phases is rather limited. Here, we report the fabrication of Co(D-Cam)1/2(bdc)1/2(tmdpy) (D-Cam = D-camphoric acid; bdc = 1,4-benzenedicarboxylate; tmdpy = 4,4'-trimethylenedipyridine)-coated open tubular columns for high-resolution gas chromatographic separation of compounds. The Co(D-Cam)1/2(bdc)1/2(tmdpy) compound possesses a 3-D framework containing enantiopure building blocks embedded in intrinsically chiral topological nets. In this study, two fused-silica open tubular columns with different inner diameters and lengths, including column A (30 m × 530 μm i.d.) and column B (2 m × 75 μm i.d.), were prepared by a dynamic coating method using Co-(D-Cam)1/2(bdc)1/2(tmdpy) as the stationary phase. The chromatographic properties of the two columns were investigated using n-dodecane as the test compound at 120 °C. The number of theoretical plates (plates/m) of the two metal-organic framework columns was 1,450 and 3,100, respectively. The separation properties were evaluated using racemates, isomers, alkanes, alcohols, and Grob's test mixture. The limit of detection and limit of quantification were found to be 0.125 and 0.417 ng for citronellal enantiomers, respectively. Repeatability (n = 6) showed lower than 0.25 % relative standard deviation (RSD) for retention times and lower than 2.2 % RSD for corrected peak areas. The experimental results showed that the stationary phase has excellent selectivity and also possesses good recognition ability toward these organic compounds, especially chiral compounds.

  4. Preparation and characterization of a new microwave immobilized poly(2-phenylpropyl)methylsiloxane stationary phase for reversed phase high-performance liquid chromatography.

    Science.gov (United States)

    Begnini, Fernanda R; Jardim, Isabel C S F

    2013-07-05

    A new reversed phase high-performance liquid chromatography (RP-HPLC) stationary phase was prepared and its chromatographic and physical-chemical properties were evaluated. The new stationary phase was prepared with a silica support and poly(2-phenylpropyl)methylsiloxane (PPPMS), a phenyl type polysiloxane copolymer. Since this is a new copolymer and there is little information in the literature, it was submitted to physical-chemical characterization by infrared spectroscopy and thermogravimetry. The chromatographic phase was prepared through sorption and microwave immobilization of the copolymer onto a silica support. The chromatographic performance was evaluated by employing test procedures suggested by Engelhardt and Jungheim, Tanaka and co-workers, Neue, and Szabó and Csató. These test mixtures provide information about the hydrophobic selectivity, silanophilic activity, ion-exchange capacity, shape selectivity and interaction with polar analytes of the new Si-PPPMS reversed phase. Stability tests were developed using accelerated aging tests under both basic and acidic conditions to provide information about the lifetime of the packed columns. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Liquid chromatographic studies on the behaviour of Pu(III), Pu(IV) and Pu(VI) on a RP stationary phase in presence of α-hydroxyisobutyric acid as a chelating agent

    Energy Technology Data Exchange (ETDEWEB)

    Jaison, P.G.; Kumar, Pranaw; Telmore, Vijay M. [Bhabha Atomic Research Centre, Mumbai (India). Fuel Chemistry Division

    2017-06-01

    Since plutonium possesses multiple oxidation states which can coexist in solution, a method for the identification of these oxidation states is important to understand its chemical processes. Liquid chromatographic studies were carried out to compare the chromatographic behaviour of different oxidation states of Pu in presence of the eluent, α-hydroxyisobutyric acid (HIBA). The three oxidation states of Pu viz. Pu(III), Pu(IV) and Pu(VI) were separated under optimised conditions. It was seen that the presence of the complexing agent influences the equilibrium of Pu(III)/(IV) as well as Pu(IV)/(VI) systems. Pu(III) to Pu(IV) conversion was found to be enhanced by high pH and concentration of HIBA whereas a relatively low pH and high concentration of HIBA promotes the conversion of Pu(VI) to Pu(IV).

  6. Capillary electrochromatography of inorganic cations in open tubular columns with a controllable capacity multilayered stationary phase architecture.

    Science.gov (United States)

    Kubán, Pavel; Kubán, Petr; Kubán, Vlastimil; Hauser, Peter C; Bocek, Petr

    2008-05-09

    In this paper capillary electrochromatography of alkali and alkaline-earth metal cations in open tubular capillary columns is described. Capillary columns are prepared by coating fused silica capillaries of 75 microm I.D. with poly(butadiene-maleic acid) copolymer (PBMA) in multiple layers. Thermally initiated radical polymerization is used to crosslink the stationary phase. Capillary columns with different number of stationary phase layers can be prepared and allow for the adjustment of separation selectivity in the electrochromatographic mode. Fast and sensitive separations of common inorganic cations are achieved in less than 6 min in a 60 cm capillary column with on-column capacitively coupled contactless conductivity detector. Limits of detection (S/N=3) for the determination of alkali and alkaline-earth metal cations range from 0.3 to 2.5 microM and repeatability is better than 0.5, 4.5 and 6.1% for migration times, peak heights and peak areas, respectively.

  7. Characterizing the selectivity of stationary phases and organic modifiers in reversed-phase high-performance liquid chromatographic systems by a general solvation equation using gradient elution.

    Science.gov (United States)

    Du, C M; Valko, K; Bevan, C; Reynolds, D; Abraham, M H

    2000-11-01

    Retention data for a set of 69 compounds using rapid gradient elution are obtained on a wide range of reversed-phase stationary phases and organic modifiers. The chromatographic stationary phases studied are Inertsil (IN)-ODS, pentafluorophenyl, fluoro-octyl, n-propylcyano, Polymer (PLRP-S 100), and hexylphenyl. The organic solvent modifiers are 2,2,2-trifluoroethanol (TFE); 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP); isopropanol; methanol (MeOH); acetonitrile (AcN); tetrahydrofuran; 1,4-dioxane; N,N-dimethylformamide; and mixed solvents of dimethylsulfoxide (DMSO) with AcN and DMSO with MeOH (1:1). A total of 25 chromatographic systems are analyzed using a solvation equation. In general, most of the systems give reasonable statistics. The selectivity of the reversed phase-high-performance liquid chromatographic (HPLC) systems with respect to the solute's dipolarity-polarity, hydrogen-bond acidity, and basicity are reflected in correspondingly large coefficients in the solvation equation. We wanted to find the most orthogonal HPLC systems, showing the highest possible selectivity difference in order to derive molecular descriptors using the gradient retention times of a compound. We selected eight chromatographic systems that have a large range of coefficients of interest (s, a, and b) similar to those found in water-solvent partitions used previously to derive molecular descriptors. The systems selected are IN-ODS phases with AcN, MeOH, TFE, and HFIP as mobile phase, PLRP-S 100 phase with AcN, propylcyano phase with AcN and MeOH, and fluorooctyl phase with TFE. Using the retention data obtained for a compound in the selected chromatographic systems, we can estimate the molecular descriptors with the faster and simpler gradient elution method.

  8. Thiol-ene click chemistry derived cationic cyclodextrin chiral stationary phase and its enhanced separation performance in liquid chromatography.

    Science.gov (United States)

    Yao, Xiaobin; Tan, Timothy Thatt Yang; Wang, Yong

    2014-01-24

    This work is the first demonstration of a simple thiol-ene click chemistry to anchor vinyl imidazolium β-CD onto thiol silica to form a novel cationic native cyclodextrin (CD) chiral stationary phase (CSP). The CSP afforded high enantioseparation ability towards dansyl (Dns) amino acids, carboxylic aryl compounds and flavonoids in chiral HPLC. The current CSP demonstrates the highest resolving ability (selectivity >1.1, resolution >1.5) towards Dns amino acids in a mobile phase buffered at pH=6.5, with the resolution of Dns-dl-leucine as high as 6.97. 2,4-dichloride propionic acid (2,4-ClPOPA) was well resolved with the selectivity and resolution of 1.37 and 4.88, respectively. Compared to a previously reported native CD-CSP based on a triazole linkage, the current cationic CD-CSP shows a stronger retention and higher resolution towards acidic chiral compounds, ascribed to the propitious strong electrostatic attraction. Stability evaluation results indicated that thiol-ene reaction can provide a facile and robust approach for the preparation of positively charged CD CSPs. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. 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.

  10. Argentation gas chromatography revisited: Separation of light olefin/paraffin mixtures using silver-based ionic liquid stationary phases.

    Science.gov (United States)

    Nan, He; Zhang, Cheng; Venkatesh, Amrit; Rossini, Aaron J; Anderson, Jared L

    2017-11-10

    Silver ion or argentation chromatography utilizes stationary phases containing silver ions for the separation of unsaturated compounds. In this study, a mixed-ligand silver-based ionic liquid (IL) was evaluated for the first time as a gas chromatographic (GC) stationary phase for the separation of light olefin/paraffin mixtures. The selectivity of the stationary phase toward olefins can be tuned by adjusting the ratio of silver ion and the mixed ligands. The maximum allowable operating temperature of these stationary phases was determined to be between 125°C and 150°C. Nuclear magnetic resonance (NMR) spectroscopy was used to characterize the coordination behavior of the silver-based IL as well as provide an understanding into the retention mechanism of light olefins. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Chiral chromatography studies of chemical behavior of cinacalcet on polysaccharide chiral reversed-phase HPLC stationary phases.

    Science.gov (United States)

    Dousa, Michal; Brichác, Jirí

    2012-01-01

    A rapid HPLC method for the analytical resolution of cinacalcet enantiomers was developed. Four chiral columns (two amylose and two cellulose type) were evaluated in RP systems. Excellent enantioseparation with a resolution of more than 6 was achieved on Chiralpak AY (amylose 5-chloro-2-methylphenylcarbamate chiral stationary phase) using 10 mM triethylamine (pH 8.0)-acetonitrile (40 + 60, v/v) mobile phase. Validation of the HPLC method, including linearity, LOD, LOQ, precision, accuracy, and selectivity, was performed according to the International Conference on Harmonization guidelines. The method was successfully applied for the determination of (S)-cinacalcet in enantiopure active pharmaceutical ingredient (R)-cinacalcet.

  12. Proteomic Analysis of Stationary Phase in the Marine Bacterium "Candidatus Pelagibacter ubique"

    Energy Technology Data Exchange (ETDEWEB)

    Sowell, S. M.; Norbeck, A. D.; Lipton, M. S.; Nicora, C. D.; Callister, S. J.; Smith, R. D.; Barofsky, D. F.; Giovannoni, S. J.

    2008-05-09

    The α-proteobacterium ‘Candidatus Pelagibacter ubique’ str. HTCC1062, and most other members of the SAR11 clade, lack genes for assimilatory sulfate reduction, making them dependent on organosulfur compounds that occur naturally in seawater. To investigate how these cells adapt to sulfur limitation, batch cultures were grown in defined media containing either limiting or non-limiting amounts of dimethylsulfoniopropionate (DMSP) as the sole sulfur source. Protein and mRNA expression were measured during exponential growth, immediately prior to stationary phase, and in late stationary phase. Two distinct responses were observed: one as DMSP became exhausted, and another as cells acclimated to a sulfur-limited environment. The first response was characterized by increased transcription and translation of all Ca. P. ubique genes downstream of previously confirmed S-adenosyl methionine (SAM) riboswitches: bhmT, mmuM, and metY. Proteins encoded by these genes were up to 33 times more abundant as DMSP became limiting. Their predicted function is to shunt all available sulfur to methionine. The secondary response, observed during sulfur-depleted stationary phase, was a 6-10 fold increase in transcription of the heme c shuttle ccmC and two small genes of unknown function (SAR11_1163 and SAR11_1164). This bacterium's strategy for coping with sulfur stress appears to be intracellular redistribution to support methionine biosynthesis, rather than increasing organosulfur import. Many of the genes and SAM riboswitches involved in this response are located in a hypervariable genome region (HVR). One of these HVR genes, ordL, is located downstream of a conserved motif that evidence suggests is a novel riboswitch.

  13. Stationary phase expression of the arginine biosynthetic operon argCBH in Escherichia coli

    Directory of Open Access Journals (Sweden)

    Sun Yuan

    2006-02-01

    Full Text Available Abstract Background Arginine biosynthesis in Escherichia coli is elevated in response to nutrient limitation, stress or arginine restriction. Though control of the pathway in response to arginine limitation is largely modulated by the ArgR repressor, other factors may be involved in increased stationary phase and stress expression. Results In this study, we report that expression of the argCBH operon is induced in stationary phase cultures and is reduced in strains possessing a mutation in rpoS, which encodes an alternative sigma factor. Using strains carrying defined argR, and rpoS mutations, we evaluated the relative contributions of these two regulators to the expression of argH using operon-lacZ fusions. While ArgR was the main factor responsible for modulating expression of argCBH, RpoS was also required for full expression of this biosynthetic operon at low arginine concentrations (below 60 μM L-arginine, a level at which growth of an arginine auxotroph was limited by arginine. When the argCBH operon was fully de-repressed (arginine limited, levels of expression were only one third of those observed in ΔargR mutants, indicating that the argCBH operon is partially repressed by ArgR even in the absence of arginine. In addition, argCBH expression was 30-fold higher in ΔargR mutants relative to levels found in wild type, fully-repressed strains, and this expression was independent of RpoS. Conclusion The results of this study indicate that both derepression and positive control by RpoS are required for full control of arginine biosynthesis in stationary phase cultures of E. coli.

  14. Stereoelectronic model to explain the resolution of enantiomeric ibuprofen amides on the Pirkle chiral stationary phase.

    Science.gov (United States)

    Nicoll-Griffith, D A

    1987-07-31

    A chiral recognition model is proposed which incorporates the electronic and steric interactions between amide derivatives of ibuprofen and the (R)-N-(3,5-dinitrobenzoyl)phenylglycine-derived Pirkle chiral stationary phase during high-performance liquid chromatography. Based on this rationale, amide derivatives of ibuprofen were prepared using 4-chloroaniline, 4-bromoaniline, aniline, 4-methoxyaniline and 1-aminonaphthylene to improve the enantiomer separation over previously reported results with this column. The amides prepared gave separation values of 1.16, 1.16, 1.19, 1.21 and 1.23, respectively. These high separation values are consistent with the proposed model.

  15. 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)

  16. Poly(butylene terephthalate) based novel achiral stationary phase investigated under supercritical fluid chromatography conditions.

    Science.gov (United States)

    Nagai, Kanji; Shibata, Tohru; Shinkura, Satoshi; Ohnishi, Atsushi

    2018-05-11

    Poly(butylene terephthalate) based novel stationary phase (SP), composed of planar aromatic phenyl group together with ester group monomer units, was designed for supercritical fluid chromatography (SFC) use. As expected from its structure, this phase shows planarity recognition of isomeric aromatics and closely similar compounds. Interestingly, for most analytes, the retention behavior of this SP is significantly distinct from that of the 2-ethylpyridine based SPs which is among the most well-known SFC dedicated phases. Although the poly(butylene terephthalate) is coated on silica gel, the performance of the column did not change by using extended range modifiers such as THF, dichloromethane or ethyl acetate and column robustness was confirmed by cycle durability testing. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

  17. Transcriptional Characterization of Salmonella TAl00 in Growth and Stationary Phase: Mutagenesis of MX in Both Types of Cells

    Science.gov (United States)

    The Salmonella (Ames) mutagenicity assay can be performed using cells that are in different growth phases. Thus, the plate-incorporation assay involves plating stationary-phase cells with the mutagen, after which the cells undergo a brief lag phase and, consequently, are exposed ...

  18. [Preparation and evaluation of stationary phase of high performance liquid chromatography for the separation of basic solutes].

    Science.gov (United States)

    Wang, P; Wang, J; Cong, R; Dong, B

    1997-05-01

    A bonded phase for high performance liquid chromatography (HPLC) has been prepared by the new reaction between silica and silicon ether. The ether was synthesized from alkylchlorosilane and pentane-2,4-dione in the presence of imidazole under inert conditions by using anhydrous tetrahydrofuran as solvent. The bonded phase thus obtained was characterized by elemental analysis, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and HPLC evaluation. The carbon content was 9.4% and the surface coverage almost attained 3.0micromol/m2 without end-capping. The silanol absorption peaks of the product cannot be observed from the DRIFT spectrum, which revealed that the silanization reaction proceeded thoroughly. The basic solutes, such as aniline, o-toluidine, p-toluidine, N,N-dimethylaniline and pyridine were used as the probe solutes to examine their interaction with the residual silanols on the surface of the products. No buffer or salt was used in the mobile phase for these experiments. In comparison with an acidic solute, such as, phenol, basic aniline eluted in front of phenol, and the ratio of asymmetry of aniline peak to that of the phenol peak was 1.1. Furthermore the relative k' value of p-toluidine to that of o-toluidine was also 1.1. All the results showed that the stationary phase has better quality and reproducibility and can be used for the separation of basic solutes efficiently.

  19. Retention behavior of resorcinarene-based cavitands on C8 and C18 stationary phases.

    Science.gov (United States)

    Bartó, Endre; Prauda, Ibolya; Kilár, Ferenc; Kiss, Ibolya; Felinger, Attila

    2015-09-01

    The understanding of the retention behavior of large molecules is an area of interest in liquid chromatography. Resorcinarene-based cavitands are cavity-shaped cyclic oligomers that can create host-guest interactions. We have investigated the chromatographic behavior of two types of cyclic tetramers as analytes in high-performance liquid chromatography. The experiments were performed at four different temperatures (15, 25, 35, 45°C) on two types of reversed stationary phases (C8 and C18 ) from two different manufacturers. We have found a huge difference between the retention of resorcinarenes and cavitands. In some cases, the retention factor of cavitands was even a hundred times larger than the retention factor of resorcinarenes. The retention of methylated derivates was two to four times larger compared to that of demethylated compounds on every column. The opposite retention behavior of the resorcinarenes and cavitands on the two types of stationary phases showed well the difference of the selectivity of the XTerra and BDS Hypersil columns. The retention mechanism was studied by the thermodynamic parameters calculated from the van't Hoff equation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. The Trypanosoma cruzi nucleolus: a morphometrical analysis of cultured epimastigotes in the exponential and stationary phases.

    Science.gov (United States)

    Nepomuceno-Mejía, Tomás; Lara-Martínez, Reyna; Cevallos, Ana María; López-Villaseñor, Imelda; Jiménez-García, Luis Felipe; Hernández, Roberto

    2010-12-01

    Our group is interested in rRNA and ribosome biogenesis in the parasitic protozoan Trypanosoma cruzi. Epimastigotes represent an extracellular replicative stage of T. cruzi and can be cultured in axenic media. The growth curve of epimastigotes allows assessment of potential differences in the nucleoli of cells undergoing growth-rate transitions. To establish cellular parameters for studying ribosome biogenesis in T. cruzi, a morphometric analysis of the nucleoli of cultured cells in the exponential and stationary phases was conducted. Electron micrograph-based measurements of nuclear sections from independent cells demonstrated that the nucleolar area is over twofold higher in exponentially growing cells, as compared with epimastigotes in the stationary phase. The granular component of the nucleoli of actively growing cells was the main structural element. Cycloheximide moderately reduced the apparent size of the nucleoli without an apparent disruption of their architecture. Our results provide a firm basis for the establishment of an experimental model to study the organization of the nucleolus during the growth and development of T. cruzi. © 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved.

  1. An immobilized graphene oxide stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Wang, Chun; de Rooy, Sergio; Lu, Cheng-Fei; Fernand, Vivian; Moore, Leonard; Berton, Paula; Warner, Isiah M

    2013-04-01

    The research literature currently abounds with studies of graphene-related materials as a result of the extraordinary properties of such materials. On the basis of these citations, it is clear that the range of applications for such materials is substantial. In this manuscript, we report the immobilization of graphene oxide (GO) onto a fused-silica capillary to form a potential stationary phase for use in open-tubular CEC. We successfully incorporated GO through an in situ condensation reaction with (3-aminopropyl)triethoxysilane after silanization with (3-aminopropyl)triethoxysilane on the inner surface of the capillary. This GO-incorporated capillary was then characterized by use of SEM, infrared spectroscopy, and measurements of EOF. The electrochromatographic features of this stationary phase have also been investigated. Evaluation of acquired data indicates high electrochromatographic resolution and good capillary efficiency. Highly reproducible results between runs, days, and capillaries were also obtained. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Chiral stationary phase optimized selectivity liquid chromatography: A strategy for the separation of chiral isomers.

    Science.gov (United States)

    Hegade, Ravindra Suryakant; De Beer, Maarten; Lynen, Frederic

    2017-09-15

    Chiral Stationary-Phase Optimized Selectivity Liquid Chromatography (SOSLC) is proposed as a tool to optimally separate mixtures of enantiomers on a set of commercially available coupled chiral columns. This approach allows for the prediction of the separation profiles on any possible combination of the chiral stationary phases based on a limited number of preliminary analyses, followed by automated selection of the optimal column combination. Both the isocratic and gradient SOSLC approach were implemented for prediction of the retention times for a mixture of 4 chiral pairs on all possible combinations of the 5 commercial chiral columns. Predictions in isocratic and gradient mode were performed with a commercially available and with an in-house developed Microsoft visual basic algorithm, respectively. Optimal predictions in the isocratic mode required the coupling of 4 columns whereby relative deviations between the predicted and experimental retention times ranged between 2 and 7%. Gradient predictions led to the coupling of 3 chiral columns allowing baseline separation of all solutes, whereby differences between predictions and experiments ranged between 0 and 12%. The methodology is a novel tool allowing optimizing the separation of mixtures of optical isomers. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Rapid purification of diastereoisomers from Piper kadsura using supercritical fluid chromatography with chiral stationary phases.

    Science.gov (United States)

    Xin, Huaxia; Dai, Zhuoshun; Cai, Jianfeng; Ke, Yanxiong; Shi, Hui; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-08-04

    Supercritical fluid chromatography (SFC) with chiral stationary phases (CSPs) is an advanced solution for the separation of achiral compounds in Piper kadsura. Analogues and stereoisomers are abundant in natural products, but there are obstacles in separation using conventional method. In this paper, four lignan diastereoisomers, (-)-Galbelgin, (-)-Ganschisandrin, Galgravin and (-)-Veraguensin, from Piper kadsura were separated and purified by chiral SFC. Purification strategy was designed, considering of the compound enrichment, sample purity and purification throughput. Two-step achiral purification method on chiral preparative columns with stacked automated injections was developed. Unconventional mobile phase modifier dichloromethane (DCM) was applied to improve the sample solubility. Four diastereoisomers was prepared at the respective weight of 103.1mg, 10.0mg, 152.3mg and 178.6mg from 710mg extract with the purity of greater than 98%. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Ion chromatography of transition metals: specific alteration of retention by complexation reactions in the mobile and on the stationary phase

    International Nuclear Information System (INIS)

    Baumgartner, S.

    1992-05-01

    Ion chromatography of mono- and bivalent cations was performed on a conventional cation exchanger. The pH influence of an ethylene-diamine/citrate eluent was significant for the retention of alkaline earth and transition metals, but negligible for alkali ions. This was dealt with from a mechanistic point of view. Mobile phase optimization allowed fast isocratic analysis of mono- and bivalent cations and the separation of the radionuclides Cs-137 and Sr-90. A newly synthesized stationary phase containing iminodiacetate (IDA) function was investigated for cation chromatography using ethylenediamine/citrate eluents, polyhydroxy acid and dipicolinic acid. The column's high selectivity for transition metal ions in comparison to alkali and alkaline earth metals may be governed by the choice of complexing ability and pH of the eluent. Applications verified by atomic absorption spectroscopy include alkaline earth metals in beverages and the determination of Co, Cd and Zn in solutions containing more than 10 14 -fold excess of Na and Mg, such as sea water

  5. The Stationary-Phase Cells of Saccharomyces cerevisiae Display Dynamic Actin Filaments Required for Processes Extending Chronological Life Span.

    Science.gov (United States)

    Vasicova, Pavla; Lejskova, Renata; Malcova, Ivana; Hasek, Jiri

    2015-11-01

    Stationary-growth-phase Saccharomyces cerevisiae yeast cultures consist of nondividing cells that undergo chronological aging. For their successful survival, the turnover of proteins and organelles, ensured by autophagy and the activation of mitochondria, is performed. Some of these processes are engaged in by the actin cytoskeleton. In S. cerevisiae stationary-phase cells, F actin has been shown to form static aggregates named actin bodies, subsequently cited to be markers of quiescence. Our in vivo analyses revealed that stationary-phase cultures contain cells with dynamic actin filaments, besides the cells with static actin bodies. The cells with dynamic actin displayed active endocytosis and autophagy and well-developed mitochondrial networks. Even more, stationary-phase cell cultures grown under calorie restriction predominantly contained cells with actin cables, confirming that the presence of actin cables is linked to successful adaptation to stationary phase. Cells with actin bodies were inactive in endocytosis and autophagy and displayed aberrations in mitochondrial networks. Notably, cells of the respiratory activity-deficient cox4Δ strain displayed the same mitochondrial aberrations and actin bodies only. Additionally, our results indicate that mitochondrial dysfunction precedes the formation of actin bodies and the appearance of actin bodies corresponds to decreased cell fitness. We conclude that the F-actin status reflects the extent of damage that arises from exponential growth. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

  6. Integrated Time and Phase Synchronization Strategy for a Multichannel Spaceborne-Stationary Bistatic SAR System

    Directory of Open Access Journals (Sweden)

    Feng Hong

    2016-07-01

    Full Text Available The spatial separation of the transmitter and receiver in Bistatic Synthetic Aperture Radar (BiSAR makes it a promising and useful supplement to a classical Monostatic SAR system (MonoSAR. This paper proposes a novel integrated time and phase synchronization strategy for a multichannel spaceborne-stationary BiSAR system. Firstly, the time synchronization strategy is proposed, which includes Pulse Repetition Frequency (PRF generation under noisy conditions, multichannel calibration and the alignment of the recorded data with the orbital data. Furthermore, the phase synchronization strategy, which fully considers the deteriorative factors in the BiSAR configuration, is well studied. The contribution of the phase synchronization strategy includes two aspects: it not only compensates the phase error, but also improves the Signal to Noise Ratio (SNR of the obtained signals. Specifically, all direct signals on different PRF time can be reconstructed with the shift and phase compensation operation using a reference signal. Besides, since the parameters of the reference signal can be estimated only once using the selected practical direct signal and a priori information, the processing complexity is well reduced. Final imaging results with and without compensation for real data are presented to validate the proposed synchronization strategy.

  7. Strong cation exchange-type chiral stationary phase for enantioseparation of chiral amines in subcritical fluid chromatography.

    Science.gov (United States)

    Wolrab, Denise; Kohout, Michal; Boras, Mario; Lindner, Wolfgang

    2013-05-10

    A new strong cation exchange type chiral stationary phase (SCX CSP) based on a syringic acid amide derivative of trans-(R, R)-2-aminocyclohexanesulfonic acid was applied to subcritical fluid chromatography (SFC) for separation of various chiral basic drugs and their analogues. Mobile phase systems consisting of aliphatic alcohols as polar modifiers and a broad range of amines with different substitution patterns and lipophilicity were employed to evaluate the impact on the SFC retention and selectivity characteristics. The observed results point to the existence of carbonic and carbamic acid salts formed as a consequence of reactions occurring between carbon dioxide, the alcoholic modifiers and the amine species present in the sub/supercritical fluid medium, respectively. Evidence is provided that these species are essential for affecting ion exchange between the strongly acidic chiral selector units and the basic analytes, following the well-established stoichiometric displacement mechanisms. Specific trends were observed when different types of amines were used as basic additives. While ammonia gave rise to the formation of the most strongly eluting carbonic and carbamic salt species, simple tertiary amines consistently provided superior levels of enantioselectivity. Furthermore, trends in the chiral SFC separation characteristics were investigated by the systematic variation of the modifier content and temperature. Different effects of additives are interpreted in terms of changes in the relative concentration of the transient ionic species contributing to analyte elution, with ammonia-derived carbamic salts being depleted at elevated temperatures by decomposition. Additionally, in an effort to optimize SFC enantiomer separation conditions for selected analytes, the impact of the type of the organic modifier, temperature, flow rate and active back pressure were also investigated. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. New method for evaluating irreversible adsorption and stationary phase bleed in gas chromatographic capillary columns.

    Science.gov (United States)

    Wright, Bob W; Wright, Cherylyn W

    2012-10-26

    A novel method is described for the evaluation of irreversible adsorption and column bleed in gas chromatographic (GC) columns using a tandem GC approach. This work specifically determined the degree of irreversible adsorption behavior of specific sulfur and phosphorous containing test probe compounds at levels ranging from approximately 50 picograms (pg) to 1 nanogram (ng) on selected gas chromatographic columns. This method does not replace existing evaluation methods that characterize reversible adsorption but provides an additional tool. The test compounds were selected due to their ease of adsorption and their importance in the specific trace analytical detection methodology being developed. Replicate chromatographic columns with 5% phenylmethylpolysiloxane (PMS), polyethylene glycol (wax), trifluoropropylpolysiloxane (TFP), or 78% cyanopropylpolysiloxane stationary phases from a variety of vendors were evaluated. As expected, the results demonstrate that the different chromatographic phases exhibit differing degrees of irreversible adsorption behavior. The results also indicate that all manufacturers do not produce equally inert columns nor are columns from a given manufacturer identical. The wax-coated columns for the test probes used were more inert as a group than 5% PMS coated columns, and they were more reproducibly manufactured. Both TFP and 78% cyanopropylpolysiloxane columns displayed superior inertness to the test compounds compared to either 5% PMS- or wax-coated columns. Irreversible adsorption behavior was characterized for a limited range of stationary phase film thicknesses. In addition, the method was shown effective for characterizing column bleed and methods to remove bleed components. This method is useful in screening columns for demanding applications and to obtain diagnostic information related to improved preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. New poly(styrene/divinylbenzene) based stationary phases for the solid phase extraction of pesticides and the chromatography of carbohydrates

    International Nuclear Information System (INIS)

    Wartusch, I.

    2002-02-01

    The introduced sorbents based on poly(styrene/divinylbenzene) are studied regarding their extraction behavior of pesticides out of water. The sorbents are prepared with different porogens like n-octanol, n-decanol, n-dodecanol and acetone. The comparison of the extraction properties of these substances shows that the use of n-octanol as a porogen leads to the best recoveries. Furthermore this sorbent is compared to a stationary phase prepared via ring opening metathesis polymerization (ROMP) and to commercially available silica-C18. It is shown that the poly(styrene/divinylbenzene) based material on average yields higher recoveries as the other materials. Only the extraction of relatively polar pesticides works better with the ROMP based sorbent. For the chromatography of carbohydrates nonporous particles with diameters of about 3 μm were synthesized via poly(styrene/divinylbenzene) using the activated swelling method. Quaternary ammonia functional groups were introduced into the poly(styrene/divinylbenzene) particles via their nitration, reduction and quaternization. The applicability of these stationary phases for anion exchange chromatography is shown by separation of different kinds of sugars using a pulsed amperometric detection system. Monosaccharides are isocratically separated using an eluent containing sodium hydroxide, separations of disaccharides and oligosaccharides are performed using sodium acetate gradients. Linearity, detection limits and reproducibility of the system are investigated by the analysis of glucose, sucrose and fructose out of the real samples Coca Cola and apple juice. (author)

  10. Enantioseparation of novel chiral sulfoxides on chlorinated polysaccharide stationary phases in supercritical fluid chromatography.

    Science.gov (United States)

    West, Caroline; Konjaria, Mari-Luiza; Shashviashvili, Natia; Lemasson, Elise; Bonnet, Pascal; Kakava, Rusudan; Volonterio, Alessandro; Chankvetadze, Bezhan

    2017-05-26

    Asymmetric sulfoxides is a particular case of chirality that may be found in natural as well as synthetic products. Twenty-four original molecules containing a sulfur atom as a centre of chirality were analyzed in supercritical fluid chromatography on seven polysaccharide-based chiral stationary phases (CSP) with carbon dioxide - methanol mobile phases. While all the tested CSP provided enantioseparation for a large part of the racemates, chlorinated cellulosic phases proved to be both highly retentive and highly enantioselective towards these species. Favourable structural features were determined by careful comparison of the enantioseparation of the probe molecules. Molecular modelling studies indicate that U-shaped (folded) conformations were most favorable to achieve high enantioresolution on these CSP, while linear (extended) conformations were not so clearly discriminated. For a subset of these species adopting different conformations, a broad range of mobile phase compositions, ranging from 20 to 100% methanol in carbon dioxide, were investigated. While retention decreased continuously in this range, enantioseparation varied in a non-monotonous fashion. Abrupt changes in the tendency curves of retention and selectivity were observed when methanol proportion reaches about 60%, suggesting that a change in the conformation of the analytes and/or chiral selector is occurring at this point. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Thermal and Hydrothermal Treatment of Silica Gels as Solid Stationary Phases in Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

    Full Text Available Silica gel was prepared and treated thermally and hydrothermally and was characterized as solid stationary phase in gas chromatography. The characteristics have been evaluated in terms of polarity, selectivity, and separation efficiencies. These parameters were used to assess the outer silica surface contributions and the degree of surface deactivation brought about by different treatment techniques. The parent silica elutes the paraffinic hydrocarbons with high efficiency of separation and elutes aromatic hydrocarbons with nearly good separation and has bad separation of alcohols. The calcined silica at 500°C and 1000°C has a pronounced effect on the separation of aromatic hydrocarbons compared with the parent silica and hydrothermal treatment of silica. With respect to alcohols separation, the obtained bad separations using treated and untreated silica reflect the little effect of the thermal and hydrothermal treatment on the silica surface deactivation.

  12. Improved Procedure for Preparation of Covalently Bonded Cellulose Tris-phenylcarbamate Chiral Stationary Phases

    Institute of Scientific and Technical Information of China (English)

    秦峰; 陈小明; 刘月启; 邹汉法; 王俊德

    2005-01-01

    The classical method for preparation of covalently boned cellulose derivative chiral stationary phases (CSP) with diisocyanate as spacer was improved. Diisocyanate was firstly allowed to react with 3-aminopropyltriethoxysilane, and the resulting product was then applied as the spacer reagent to immobilize cellulose derivatives onto silica gel. Influences of the amount and the length of the spacer on the optical resolution ability of the CSP were investigated. Comparing improved procedure to classical diisocyanate method, the cross-linking between the glucose units of the cellulose derivatives was avoided to the most extent. With the improved procedure, regio-nonselective ways could be adooted to prepare covalently bonded CSP, which showed an advantage for the rapid preparation.

  13. Application of the zeta potential for stationary phase characterization in ion chromatography.

    Science.gov (United States)

    Buszewski, Bogusław; Jaćkowska, Magdalena; Bocian, Szymon; Dziubakiewicz, Ewelina

    2013-01-01

    Two series of homemade stationary bonded phases for ion chromatography were investigated according to their zeta potential. One set of dendrimer anion exchanger was synthesized on the polymer support whereas the second material was prepared on the silica gel. The zeta potential data in water environment as well as buffered water solution were obtained. The influence of the length of anion-exchanger chains, the type of the support of the modified surface, and charge distribution on these data was investigated. Additionally, the zeta potential was correlated with retention factor of inorganic ions to describe their influence on the retention mechanism in ion chromatography. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Versatile ligands for high-performance liquid chromatography: An overview of ionic liquid-functionalized stationary phases.

    Science.gov (United States)

    Zhang, Mingliang; Mallik, Abul K; Takafuji, Makoto; Ihara, Hirotaka; Qiu, Hongdeng

    2015-08-05

    Ionic liquids (ILs), a class of unique substances composed purely by cation and anions, are renowned for their fascinating physical and chemical properties, such as negligible volatility, high dissolution power, high thermal stability, tunable structure and miscibility. They are enjoying ever-growing applications in a great diversity of disciplines. IL-modified silica, transforming the merits of ILs into chromatographic advantages, has endowed the development of high-performance liquid chromatography (HPLC) stationary phase with considerable vitality. In the last decade, IL-functionalized silica stationary phases have evolved into a series of branches to accommodate to different HPLC modes. An up-to-date overview of IL-immobilized stationary phases is presented in this review, and divided into five parts according to application mode, i.e., ion-exchange, normal-phase, reversed-phase, hydrophilic interaction and chiral recognition. Specific attention is channeled to synthetic strategies, chromatographic behavior and separation performance of IL-functionalized silica stationary phases. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Modified performance test of vented lead acid batteries for stationary applications

    International Nuclear Information System (INIS)

    Uhlir, K.W.; Fletcher, R.J.

    1995-01-01

    The concept of a modified performance test for vented lead acid batteries in stationary applications has been developed by the IEEE Battery Working Group. The modified performance test is defined as a test in the ''as found'' condition of the battery capacity and its ability to provide a high rate, short duration load (usually the highest rate of the duty cycle) that will confirm the battery's ability to meet the critical period of the load duty cycle, in addition to determining its percentage of rated capacity. This paper will begin by reviewing performance and service test requirements and concerns associated with both types of tests. The paper will then discuss the rationale for developing a modified performance test along with the benefits that can be derived from performing a modified performance test in lieu of a capacity test and/or a service test. The paper will conclude with an example on how to apply a modified performance test and test acceptance criteria

  16. Preparation and evaluation of a hydrophilic interaction and cation-exchange chromatography stationary phase modified with 2-methacryloyloxyethyl phosphorylcholine.

    Science.gov (United States)

    Xiong, Caifeng; Yuan, Jie; Wang, Zhiying; Wang, Siyao; Yuan, Chenchen; Wang, Lili

    2018-04-20

    In this work, 2-methacryloyloxyethyl phosphorylcholine (MPC) was used as a ligand to prepare a novel mixed-mode chromatography (MMC) stationary phase by the thiol-ene click reaction onto silica (MPC-silica). It was found that this MPC-silica showed the retention characteristics of hydrophilic interaction chromatography (HILIC) and weak cation exchange chromatography (WCX) under suitable mobile phase conditions. In detail, acidic and basic hydrophilic compounds and puerarin from pueraria were separated quickly with HILIC mode. Meanwhile, six standard proteins were allowed to reach baseline separation in WCX mode, and protein separation from egg white was also achieved with this mode. In addition, reduced/denatured lysozyme could be refolded with the MPC-silica column. In the meantime, the MPC-silica has been applied for refolding with simultaneous purification of recombinant human Delta-like1-RGD (rhDll1-RGD) expressed in Escherichia coli. The results show that the mass recovery and purity of rhDll1-RGD could reach 63.4% and 97% by one step, respectively. Furthermore, the reporter assay results demonstrated that refolded with simultaneously purified rhDll1-RGD could efficiently activate the signalling pathway in a dose-dependent manner. In general, this MPC-silica has good resolution and selectivity in the separation of polar compounds and protein samples in different high-performance liquid chromatography (HPLC) modes, and it successfully achieved refolding with simultaneous purification of denatured protein. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance

    Directory of Open Access Journals (Sweden)

    Xiaoli Zhang

    2016-05-01

    Full Text Available Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  18. Enantioseparation and chiral recognition mechanism of new chiral derivatives of xanthones on macrocyclic antibiotic stationary phases.

    Science.gov (United States)

    Fernandes, Carla; Tiritan, Maria Elizabeth; Cass, Quezia; Kairys, Visvaldas; Fernandes, Miguel Xavier; Pinto, Madalena

    2012-06-08

    A chiral HPLC method using four macrocyclic antibiotic chiral stationary phases (CSPs) has been investigated for determination of the enantiomeric purity of fourteen new chiral derivatives of xanthones (CDXs). The separations were performed with the CSPs Chirobiotic T, Chirobiotic TAG, Chirobiotic V and Chirobiotic R under multimodal elution conditions (normal-phase, reversed-phase and polar ionic mode). The analyses were performed at room temperature in isocratic mode and UV and CD detection at a wavelength of 254 nm. The best enantioselectivity and resolution were achieved on Chirobiotic R and Chirobiotic T CSPs, under normal elution conditions, with R(S) ranging from 1.25 to 2.50 and from 0.78 to 2.06, respectively. The optimized chromatographic conditions allowed the determination of the enantiomeric ratio of eight CDXs, always higher than 99%. In order to better understand the chromatographic behavior at a molecular level, and the structural features associated with the chiral recognition mechanism, computational studies by molecular docking were carried out using VDock. These studies shed light on the mechanisms involved in the enantioseparation for this important class of chiral compounds. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Reversed phase liquid chromatography with UV absorbance and flame ionization detection using a water mobile phase and a cyano propyl stationary phase Analysis of alcohols and chlorinated hydrocarbons.

    Science.gov (United States)

    Quigley, W W; Ecker, S T; Vahey, P G; Synovec, R E

    1999-10-01

    The development of liquid chromatography with a commercially available cyano propyl stationary phase and a 100% water mobile phase is reported. Separations were performed at ambient temperature, simplifying instrumental requirements. Excellent separation efficiency using a water mobile phase was achieved, for example N=18 800, or 75 200 m(-1), was obtained for resorcinol, at a retention factor of k'=4.88 (retention time of 9.55 min at 1 ml min(-1) for a 25 cmx4.6 mm i.d. column, packed with 5 mum diameter particles with the cyano propyl stationary phase). A separation via reversed phase liquid chromatography (RP-LC) with a 100% water mobile phase of six phenols and related compounds was compared to a separation of the same compounds by traditional RP-LC, using octadecylsilane (ODS), i.e. C18, bound to silica and an aqueous mobile phase modified with acetonitrile. Nearly identical analysis time was achieved for the separation of six phenols and related compounds using the cyano propyl stationary phase with a 100% water mobile phase, as compared to traditional RP-LC requiring a relatively large fraction of organic solvent modifier in the mobile phase (25% acetonitrile:75% water). Additional understanding of the retention mechanism with the 100% water mobile phase was obtained by relating measured retention factors of aliphatic alcohols, phenols and related compounds, and chlorinated hydrocarbons to their octanol:water partition coefficients. The retention mechanism is found to be consistent with a RP-LC mechanism coupled with an additional retention effect due to residual hydroxyl groups on the cyano propyl stationary phase. Advantages due to a 100% water mobile phase for the chemical analysis of alcohol mixtures and chlorinated hydrocarbons are reported. By placing an absorbance detector in-series and preceding a novel drop interface to a flame ionization detector (FID), selective detection of a separated mixture of phenols and related compounds and aliphatic

  20. Retention prediction of highly polar ionizable solutes under gradient conditions on a mixed-mode reversed-phase and weak anion-exchange stationary phase.

    Science.gov (United States)

    Balkatzopoulou, P; Fasoula, S; Gika, H; Nikitas, P; Pappa-Louisi, A

    2015-05-29

    In the present work the retention of three highly polar and ionizable solutes - uric acid, nicotinic acid and ascorbic acid - was investigated on a mixed-mode reversed-phase and weak anion-exchange (RP/WAX) stationary phase in buffered aqueous acetonitrile (ACN) mobile phases. A U-shaped retention behavior was observed for all solutes with respect to the eluent organic modifier content studied in a range of 5-95% (v/v). This retention behavior clearly demonstrates the presence of a HILIC-type retention mechanism at ACN-rich hydro-organic eluents and an RP-like retention at aqueous-rich hydro-organic eluents. Hence, this column should be promising for application under both RP and HILIC gradient elution modes. For this reason, a series of programmed elution runs were carried out with increasing (RP) and decreasing (HILIC) organic solvent concentration in the mobile phase. This dual gradient process was successfully modeled by two retention models exhibiting a quadratic or a cubic dependence of the logarithm of the solute retention factor (lnk) upon the organic modifier volume fraction (φ). It was found that both models produced by gradient retention data allow the prediction of solute retention times for both types of programmed elution on the mixed-mode column. Four, in the case of the quadratic model, or five, in the case of the cubic model, initial HILIC- and RP-type gradient runs gave satisfactory retention predictions of any similar kind elution program, even with different flow rate, with an overall error of only 2.5 or 1.7%, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. A new imidazolium-embedded C{sub 18} stationary phase with enhanced performance in reversed-phase liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Qiu Hongdeng [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou 730000 (China); Mallik, Abul K. [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Takafuji, Makoto [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Kumamoto Institute for Photo-Electro Organics (Phoenics), Kumamoto 862-0901 (Japan); Liu Xia; Jiang Shengxiang [Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou 730000 (China); Ihara, Hirotaka, E-mail: ihara@kumamoto-u.ac.jp [Department of Applied Chemistry and Biochemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555 (Japan); Kumamoto Institute for Photo-Electro Organics (Phoenics), Kumamoto 862-0901 (Japan)

    2012-08-13

    Highlights: Black-Right-Pointing-Pointer Imidazolium-embedded C{sub 18} stationary phase was prepared and characterized. Black-Right-Pointing-Pointer Enhanced chromatographic selectivity was observed in SiImC{sub 18} column. Black-Right-Pointing-Pointer Seven nucleosides and bases were separated using only water as eluent within 8 min. Black-Right-Pointing-Pointer Multiple-interactions induced by embedded polar imidazolium was investigated. - Abstract: In this paper, a new imidazolium-embedded C{sub 18} stationary phase (SiImC{sub 18}) for reversed-phase high-performance liquid chromatography is described. 1-Allyl-3-octadecylimidazolium bromide ionic liquid compound having a long alkyl chain and reactive groups was newly prepared and grafted onto 3-mercaptopropyltrimethoxysilane-modified silica via a surface-initiated radical-chain transfer addition reaction. The SiImC{sub 18} obtained was characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, diffuse reflectance infrared Fourier transform, and solid-state {sup 13}C and {sup 29}Si cross-polarization/magic angle spinning nuclear magnetic resonance spectroscopy. The selectivity toward polycyclic aromatic hydrocarbons relative to that toward alkylbenzenes exhibited by SiImC{sub 18} was higher than the corresponding selectivity exhibited by a conventional octadecyl silica (ODS) column, which could be explained by electrostatic {pi}-{pi} interaction cationic imidazolium and electron-rich aromatic rings. On the other hand, SiImC{sub 18} also showed high selectivity for polar compounds, which was based on the multiple interaction and retention mechanisms of this phase with different analytes. 1,6-Dinitropyrene and 1,8-dinitropyrene, which form a positional isomer pair of dipolar compounds, were separated successfully with the SiImC{sub 18} phase. Seven nucleosides and bases (i.e. cytidine, uracil, uridine, thymine, guanosine, xanthosine, and adenosine) were separated using only water as

  2. Response surface methodology for the determination of the design space of enantiomeric separations on cinchona-based zwitterionic chiral stationary phases by high performance liquid chromatography.

    Science.gov (United States)

    Hanafi, Rasha Sayed; Lämmerhofer, Michael

    2018-01-26

    Quality-by-Design approach for enantioselective HPLC method development surpasses Quality-by-Testing in offering the optimal separation conditions with the least number of experiments and in its ability to describe the method's Design Space visually which helps to determine enantiorecognition to a significant extent. Although some schemes exist for enantiomeric separations on Cinchona-based zwitterionic stationary phases, the exact design space and the weights by which each of the chromatographic parameters influences the separation have not yet been statistically studied. In the current work, a screening design followed by a Response Surface Methodology optimization design were adopted for enantioseparation optimization of 3 model drugs namely the acidic Fmoc leucine, the amphoteric tryptophan and the basic salbutamol. The screening design proved that the acid/base additives are of utmost importance for the 3 chiral drugs, and that among 3 different pairs of acids and bases, acetic acid and diethylamine is the couple able to provide acceptable resolution at variable conditions. Visualization of the response surface of the retention factor, separation factor and resolution helped describe accurately the magnitude by which each chromatographic factor (% MeOH, concentration and ratio of acid base modifiers) affects the separation while interacting with other parameters. The global optima compromising highest enantioresolution with the least run time for the 3 chiral model drugs varied extremely, where it was best to set low % methanol with equal ratio of acid-base modifiers for the acidic drug, very high % methanol and 10-fold higher concentration of the acid for the amphoteric drug while 20 folds of the base modifier with moderate %methanol were needed for the basic drug. Considering the selected drugs as models for many series of structurally related compounds, the design space defined and the optimum conditions computed are the key for method development on

  3. Effect of benzalkonium chloride on viability and energy metabolism in exponential- and stationary-growth-phase cells of Listeria monocytogenes

    NARCIS (Netherlands)

    Luppens, S.B.I.; Abee, T.; Oosterom, J.

    2001-01-01

    The difference in killing exponential- and stationary-phase cells of Listeria monocytogenes by benzalkonium chloride (BAC) was investigated by plate counting and linked to relevant bioenergetic parameters. At a low concentration of BAC (8 mg liter-1), a similar reduction in viable cell numbers was

  4. One-Pot Click Access to a Cyclodextrin Dimer-Based Novel Aggregation Induced Emission Sensor and Monomer-Based Chiral Stationary Phase

    Directory of Open Access Journals (Sweden)

    Xiaoli Li

    2016-11-01

    Full Text Available A ‘two birds, one stone’ strategy was developed via a one-pot click reaction to simultaneously prepare a novel cyclodextrin (CD dimer based aggregation induced emission (AIE sensor (AIE-DCD and a monomer based chiral stationary phase (CSP-MCD for chiral high performance liquid chromatography (CHPLC. AIE-DCD was found to afford satisfactory AIE response for specific detection of Zn2+ with a detection limit of 50 nM. CSP-MCD exhibits excellent enantioseparation ability toward dansyl amino acids, where the resolution of dansyl amino leucine reaches 5.43.

  5. Cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase for the enantioseparation of drugs in supercritical fluid chromatography: comparison with HPLC.

    Science.gov (United States)

    Kalíková, Květa; Martínková, Monika; Schmid, Martin G; Tesařová, Eva

    2018-03-01

    A cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase was studied as a tool for the enantioselective separation of 21 selected analytes with different pharmaceutical and physicochemical properties. The enantioseparations were performed using supercritical fluid chromatography. The effect of the mobile phase composition was studied. Four different additives (diethylamine, triethylamine, isopropylamine, and trifluoroacetic acid) and isopropylamine combined with trifluoroacetic acid were tested and their influence on enantioseparation was compared. The influence of two different mobile phase co-solvents (methanol and propan-2-ol) combined with all the additives was also evaluated. The best mobile phase compositions for the separation of the majority of enantiomers were CO 2 /methanol/isopropylamine 80:20:0.1 v/v/v or CO 2 /propan-2-ol/isopropylamine/trifluoroacetic acid 80:20:0.05:0.05 v/v/v/v. The best results were obtained from the group of basic β-blockers. A high-performance liquid chromatography separation system composed of the same stationary phase and mobile phase of similar properties prepared as a mixture of hexane/propan-2-ol/additive 80:20:0.1 v/v/v was considered for comparison. Supercritical fluid chromatography was found to yield better results, i.e. better enantioresolution for shorter analysis times than high-performance liquid chromatography. However, examples of enantiomers better resolved under the optimized conditions in high-performance liquid chromatography were also found. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. A polyacrylamide-based silica stationary phase for the separation of carbohydrates using alcohols as the weak eluent in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Cai, Jianfeng; Cheng, Lingping; Zhao, Jianchao; Fu, Qing; Jin, Yu; Ke, Yanxiong; Liang, Xinmiao

    2017-11-17

    A hydrophilic interaction liquid chromatography (HILIC) stationary phase was prepared by a two-step synthesis method, immobilizing polyacrylamide on silica sphere particles. The stationary phase (named PA, 5μm dia) was evaluated using a mixture of carbohydrates in HILIC mode and the column efficiency reached 121,000Nm -1 . The retention behavior of carbohydrates on PA stationary phase was investigated with three different organic solvents (acetonitrile, ethanol and methanol) employed as the weak eluent. The strongest hydrophilicity of PA stationary phase was observed in both acetonitrile and methanol as the weak eluent, when compared with another two amide stationary phases. Attributing to its high hydrophilicity, three oligosaccharides (xylooligosaccharide, fructooligosaccharide and chitooligosaccharides) presented good retention on PA stationary phase using alcohols/water as mobile phase. Finally, PA stationary phase was successfully applied for the purification of galactooligosaccharides and saponins of Paris polyphylla. It is feasible to use safer and cheaper alcohols to replace acetonitrile as the weak eluent for green analysis and purification of polar compounds on PA stationary phase. Copyright © 2017. Published by Elsevier B.V.

  7. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Enantiomeric Separation of 1-(Benzofuran-2-yl)alkylamines on Chiral Stationary Phases Based on Chiral Crown Ethers

    International Nuclear Information System (INIS)

    Park, Soohyun; Kim, Sang Jun; Hyun, Myung Ho

    2012-01-01

    Optically active chiral amines are important as building blocks for pharmaceuticals and as scaffolds for chiral ligands and, consequently, many efforts have been devoted to the development of efficient methods for their preparation. For example, reduction of amine precursors with chiral catalysts, enzymatic kinetic resolution or dynamic kinetic resolution of racemic amines and the direct amination of ketones with transaminases have been developed as the efficient methods for the preparation of optically active chiral amines. During the process of developing or utilizing optically active chiral amines, the methods for the determination of their enantiomeric composition are essential. Among various methods, liquid chromatographic resolution of enantiomers on chiral stationary phases (CSPs) have been known to be one of the most accurate and economic means for the determination of the enantiomeric composition of optically active chiral compounds. Especially, CSPs based on chiral crown ethers have been successfully used for the resolution of racemic primary amines. For example, CSPs based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (CSP 1, Figure 1) or (3,3'-diphenyl-1,1'-binaphthyl)-20-crown-6 (CSP 2 and CSP 3, Figure 1) have been known to be quite effective for the resolution of cyclic and non-cyclic amines, various fluoroquinolone antibacterials containing a primary amino group, tocainide (antiarrhythmic agent) and its analogues, aryl-a-amino ketones and 3-amino-1,4-benzodiazepin-2-ones

  9. Effect of benzalkonium chloride on viability and energy metabolism in exponential- and stationary-growth-phase cells of Listeria monocytogenes.

    Science.gov (United States)

    Luppens, S B; Abee, T; Oosterom, J

    2001-04-01

    The difference in killing exponential- and stationary-phase cells of Listeria monocytogenes by benzalkonium chloride (BAC) was investigated by plate counting and linked to relevant bioenergetic parameters. At a low concentration of BAC (8 mg liter(-1)), a similar reduction in viable cell numbers was observed for stationary-phase cells and exponential-phase cells (an approximately 0.22-log unit reduction), although their membrane potential and pH gradient were dissipated. However, at higher concentrations of BAC, exponential-phase cells were more susceptible than stationary-phase cells. At 25 mg liter(-1), the difference in survival on plates was more than 3 log units. For both types of cells, killing, i.e., more than 1-log unit reduction in survival on plates, coincided with complete inhibition of acidification and respiration and total depletion of ATP pools. Killing efficiency was not influenced by the presence of glucose, brain heart infusion medium, or oxygen. Our results suggest that growth phase is one of the major factors that determine the susceptibility of L. monocytogenes to BAC.

  10. Impact of column and stationary phase properties on the productivity in chiral preparative LC.

    Science.gov (United States)

    Forssén, Patrik; Fornstedt, Torgny

    2018-03-01

    By generating 1500 random chiral separation systems, assuming two-site Langmuir interactions, we investigated numerically how the maximal productivity (P R,max ) was affected by changes in stationary phase adsorption properties. The relative change in P R,max , when one adsorption property changed 10%, was determined for each system and for each studied parameter the corresponding productivity change distribution of the systems was analyzed. We could conclude that there is no reason to have columns with more than 500 theoretical plates and larger selectivity than 3. More specifically, we found that changes in selectivity have a major impact on P R,max if it is below ∼2 and, interestingly, increasing selectivity when it is above ∼3 decreases P R,max . Increase in relative saturation capacity will have a major impact on P R,max if it is below ∼40%, but only modest above this percent. Increasing total monolayer saturation capacity, or decreasing the first eluting enantiomer's retention factor, will have a modest effect on P R,max and increased efficiency will have almost no effect at all on P R,max unless it is below ∼500 theoretical plates. Finally, we showed that chiral columns with superior analytic performance might have inferior preparative performance, or vice versa. It is, therefore, not possible to assess columns based on their analytical performance alone. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Silica, alumina and aluminosilicates as solid stationary phases in gas chromatography

    Directory of Open Access Journals (Sweden)

    S. Faramawy

    2016-09-01

    Full Text Available Silica, alumina and Aluminosilicates of different Si/Al ratios were prepared by conventional precipitation or co-precipitation methods and then subjected to thermal treatment at 800 °C. The parent and thermally treated materials were characterized by means of FTIR, SEM and thermal analysis (DTA and TGA in order to elucidate the main structural properties. Surface textural characteristics were investigated by means of nitrogen adsorption–desorption isotherms at −196 °C. Pore size distribution curves indicated the presence of mesopores (10–150 Å exhibiting maxima at 35 Å. The maxima were shifted toward higher values by increasing the alumina content. Thermodynamic parameters, ΔH, ΔG and ΔS, were determined by means of inverse gas chromatography using n-hexane as a probe. The untreated and thermally treated materials were tested as solid stationary phases in gas chromatography. The separation efficiency of various non polar and polar compounds was explained in terms of surface texture and thermodynamic parameters.

  12. Molecular theory of chromatography for blocklike solutes in isotropic stationary phases and its application to supercritical fluid chromatographic retention of PAHs

    International Nuclear Information System (INIS)

    Chao Yan; Martire, D.E.

    1992-01-01

    This report discusses a molecular theory of chromatography for blocklike solutes in isotropic stationary phases as an extension to the anisotopic phase approach. Its it applied to gas, liquid, and supercritical fluid chromatography

  13. Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications.

    Science.gov (United States)

    Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, Recep

    2015-01-01

    A novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 µm, 60 Å). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20°C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 230 or 278 nm. The best separation

  14. Microstructure-based analysis and simulation of flow and mass transfer in chromatographic stationary phases

    Science.gov (United States)

    Koku, Harun

    Limitations of mass transfer in chromatographic bioseparations employing traditional packed particles have fuelled the inception and development of alternative stationary phases with improved performance characteristics. This work investigates case studies in two categories of these alternative media, namely polymer-modified packed particles and continuous monolithic phases, for insight into their enhanced properties. Specifically, high-resolution microscopy techniques and image-based analysis algorithms were implemented to extract morphology information for these materials, in an attempt to elucidate the relation between microstructure and performance. For the monolith, mesoscopic simulation methods were also employed for a more rigorous analysis of the flow and dispersion behavior. Scanning and transmission electron microscopy images of the commercial polymer-modified, agarose-based particle Sepharose XL were compared to those for its unmodified counterpart, Sepharose FF. Local regions in the composite dextran-agarose Sepharose XL particles were noted to exhibit a denser network of fibers and smaller pore sizes overall, compared to those in the traditional Sepharose FF particles. Images of particles equilibrated with high concentrations of protein revealed a significant difference in protein localization patterns, with the stained protein in XL occupying a markedly higher area fraction of the images. This suggests a higher volume available for adsorption and provides visual clues into how the consistently higher static capacity of these polymer-modified particles is manifested. Treatment of the XL particles with dextranase, an enzyme that breaks down dextran, resulted in a reduction of protein coverage, providing evidence that it is indeed the dextran that is responsible for the improved static capacity in this polymer-modified stationary phase. Imaging and image analysis techniques were also used to analyze the commercial CIM(TM) disk monolith. Two- and three

  15. Immunoassay of paralytic shellfish toxins by moving magnetic particles in a stationary liquid-phase lab-on-a-chip.

    Science.gov (United States)

    Kim, Myoung-Ho; Choi, Suk-Jung

    2015-04-15

    In this study, we devised a stationary liquid-phase lab-on-a-chip (SLP LOC), which was operated by moving solid-phase magnetic particles in the stationary liquid phase. The SLP LOC consisted of a sample chamber to which a sample and reactants were added, a detection chamber containing enzyme substrate solution, and a narrow channel connecting the two chambers and filled with buffer. As a model system, competitive immunoassays of saxitoxin (STX), a paralytic shellfish toxin, were conducted in the SLP LOC using protein G-coupled magnetic particles (G-MPs) as the solid phase. Anti-STX antibodies, STX-horseradish peroxidase conjugate, G-MPs, and a STX sample were added to the sample chamber and reacted by shaking. While liquids were in the stationary state, G-MPs were transported from the sample chamber to the detection chamber by moving a magnet below the LOC. After incubation to allow the enzymatic reaction to occur, the absorbance of the detection chamber solution was found to be reciprocally related to the STX concentration of the sample. Thus, the SLP LOC may represent a novel, simple format for point-of-care testing applications of enzyme-linked immunosorbent assays by eliminating complicated liquid handling steps. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Non-stationary filtration mode during chemical reactions with the gas phase

    Science.gov (United States)

    Zavialov, Ivan; Konyukhov, Andrey; Negodyaev, Sergey

    2015-04-01

    An experimental and numerical study of filtration accompanied by chemical reactions between displacing fluid and solid skeleton is considered. Glass balls (400-500 μm in diameter) were placed in 1 cm gap between two glass sheets and were used as model porous medium. The baking soda was added to the glass balls. The 70% solution of acetic acid was used as the displacer. The modeling porous medium was saturated with a mineral oil, and then 70% solution of colored acetic acid was pumped through the medium. The glass balls and a mineral oil have a similar refractive index, so the model porous medium was optically transparent. During the filtration, the gas phase was generated by the chemical reactions between the baking soda and acetic acid, and time-dependent displacement of the chemical reaction front was observed. The front of the chemical reaction was associated with the most intensive gas separation. The front moved, stopped, and then moved again to the area where it had been already. We called this process a secondary oxidation wave. To describe this effect, we added to the balance equations a term associated with the formation and disappearance of phases due to chemical reactions. The equations were supplemented by Darcy's law for multiphase filtration. Nonstationarity front propagation of the chemical reaction in the numerical experiment was observed at Damköhler numbers greater than 100. The mathematical modelling was agreed well with the experimental results.

  17. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

    International Nuclear Information System (INIS)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny

    2015-01-01

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r 2 =0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel

  18. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    International Nuclear Information System (INIS)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho

    2016-01-01

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic

  19. [Preparation and performance characterization of gold nanoparticles modified chiral capillary electrochromatography stationary phase].

    Science.gov (United States)

    Xiong, Lele; Li, Ruijun; Ji, Yibing

    2017-07-08

    Gold nanoparticles (GNPs, 15 nm) were prepared and introduced to amino groups derived silica monolithic column. Bovine serum albumin (BSA) was immobilized via covalent modification method onto the carboxylic functionalized GNPs to afford chiral stationary phase (CSP) for enantioseparation. GNPs were well dispersed and successfully incorporated onto the columns with the contents as high as 17.18% by characterization method such as transmission electron microscopy (TEM), ultraviolet (UV)-visible absorption spectra and scanning electron microscopy (SEM). The preparation conditions of the BSA modified CSP were optimized and 10% (v/v) 3-aminopropyltriethoxysilane (APTES) and 15 g/L BSA were selected as appropriate reaction conditions. The enantioseparation performance of the BSA modified CSP has been investigated by capillary electrochromatography (CEC). Enantiomers of tryptophan, ephedrine and atenolol were resolved, and the baseline separation of tryptophan was achieved. Meanwhile, the influences of pH value, buffer concentrations and applied voltages used on the chiral separation were studied, and the optimal separation conditions were 10 mmol/L phosphate buffer at pH 7.4 and 15 kV applied voltages. In comparison with the BSA modified CSP prepared by physical adsorption, the CSP prepared by covalent modification method had better separation results, and the analytes could be separated directly without pre-column derivatization. In addition, the prepared BSA modified CSP exhibited good run to run repeatability with relative standard deviations (RSDs) of the migration times and selectivity factors not more than 2.3% and 0.96%, respectively. This work offers a good thinking for modification with other proteins or other types of chiral selectors.

  20. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

    Energy Technology Data Exchange (ETDEWEB)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny [Organic Chemistry Laboratory, Departement of Chemistry, Diponegoro University Jln Prof. Soedharto SH, Tembalang, Semarang 50275, Indonesia Tel / Fax: (024) 7460058 (Indonesia)

    2015-12-29

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r{sup 2}=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

  1. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho [Dept. of Chemistry and Chemistry Institute for Functional Materials, Pusan National University, Busan (Korea, Republic of)

    2016-12-15

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic.

  2. Role of nutrient limitation and stationary-phase existence in Klebsiella pneumoniae biofilm resistance to ampicillin and ciprofloxacin.

    Science.gov (United States)

    Anderl, Jeff N; Zahller, Jeff; Roe, Frank; Stewart, Philip S

    2003-04-01

    Biofilms formed by Klebsiella pneumoniae resisted killing during prolonged exposure to ampicillin or ciprofloxacin even though these agents have been shown to penetrate bacterial aggregates. Bacteria dispersed from biofilms into medium quickly regained most of their susceptibility. Experiments with free-floating bacteria showed that stationary-phase bacteria were protected from killing by either antibiotic, especially when the test was performed in medium lacking carbon and nitrogen sources. These results suggested that the antibiotic tolerance of biofilm bacteria could be explained by nutrient limitation in the biofilm leading to stationary-phase existence of at least some of the cells in the biofilm. This mechanism was supported by experimental characterization of nutrient availability and growth status in biofilms. The average specific growth rate of bacteria in biofilms was only 0.032 h(-1) compared to the specific growth rate of planktonic bacteria of 0.59 h(-1) measured in the same medium. Glucose did not penetrate all the way through the biofilm, and oxygen was shown to penetrate only into the upper 100 micro m. The specific catalase activity was elevated in biofilm bacteria to a level similar to that of stationary-phase planktonic cells. Transmission electron microscopy revealed that bacteria were affected by ampicillin near the periphery of the biofilm but were not affected in the interior. Taken together, these results indicate that K. pneumoniae in this system experience nutrient limitation locally within the biofilm, leading to zones in which the bacteria enter stationary phase and are growing slowly or not at all. In these inactive regions, bacteria are less susceptible to killing by antibiotics.

  3. Schizosaccharomyces pombe Homologs of Human DJ-1 Are Stationary Phase-Associated Proteins That Are Involved in Autophagy and Oxidative Stress Resistance.

    Directory of Open Access Journals (Sweden)

    Yang Su

    Full Text Available The Parkinson's disease protein DJ-1 is involved in various cellular functions including detoxification of dicarbonyl compounds, autophagy and oxidative stress response. DJ-1 homologs are widely found in both prokaryotes and eukaryotes, constituting a superfamily of proteins that appear to be involved in stress response. Schizosaccharomyces pombe contains six DJ-1 homologs, designated Hsp3101-Hsp3105 and Sdj1 (previously named SpDJ-1. Here we show that deletion of any one of these six genes somehow affects autophagy during prolonged stationary phase. Furthermore, deletions of each of these DJ-1 homologs result in reduced stationary phase survival. Deletion of sdj1 also increases the sensitivity of stationary-phase cells to oxidative stress induced by hydrogen peroxide (H2O2 whereas overexpression of sdj1 has the opposite effect. Consistent with their role in stationary phase, expression of hsp3101, hsp3102, hsp3105 and sdj1, and to a lesser extent hsp3103 and hsp3104, is increased in stationary phase. The induction of hsp3101, hsp3102, hsp3105 and sdj1 involves the Sty1-regulated transcription factor Atf1 but not the transcription factor Pap1. Our results firmly establish that S. pombe homologs of DJ-1 are stationary-phase associated proteins and are likely involved in autophagy and antioxidant defense in stationary phase of S. pombe cells.

  4. Micro-fabricated semi-packed column for gas chromatography by using functionalized parylene as a stationary phase

    International Nuclear Information System (INIS)

    Nakai, T; Nishiyama, S; Shuzo, M; Delaunay, J-J; Yamada, I

    2009-01-01

    The conformal coating of effective stationary phases onto micro-fabricated columns having complex geometries such as semi-packed columns poses a real challenge. Here, we report for the first time the conformal coating of a semi-packed column with amino-functionalized parylene diX-AM (poly-aminomethyl-[2,2]-paracyclophane), which was found to be an effective stationary-phase material for the chromatography of short-retention-time compounds. A semi-packed column (consisting of a zigzag array of 30 µm square micro-pillars in a 1.0 m long, 180 µm wide and 230 µm deep channel) and an open tubular column (1.0 m long, 160 µm wide and 230 µm deep channel) used for comparison purposes were micro-fabricated on silicon that was subsequently coated with diX-AM parylene and thermally bonded. The chromatograms recorded on a commercial gas chromatograph demonstrated the usefulness of the conformal diX-AM coating as a stationary phase for semi-packed columns. The separation efficiency of the semi-packed column was found to be more than ten times that of the open tubular column

  5. A stationary phase solution for mountain waves with application to mesospheric mountain waves generated by Auckland Island

    Science.gov (United States)

    Broutman, Dave; Eckermann, Stephen D.; Knight, Harold; Ma, Jun

    2017-01-01

    A relatively general stationary phase solution is derived for mountain waves from localized topography. It applies to hydrostatic, nonhydrostatic, or anelastic dispersion relations, to arbitrary localized topography, and to arbitrary smooth vertically varying background temperature and vector wind profiles. A simple method is introduced to compute the ray Jacobian that quantifies the effects of horizontal geometrical spreading in the stationary phase solution. The stationary phase solution is applied to mesospheric mountain waves generated by Auckland Island during the Deep Propagating Gravity Wave Experiment. The results are compared to a Fourier solution. The emphasis is on interpretations involving horizontal geometrical spreading. The results show larger horizontal geometrical spreading for nonhydrostatic waves than for hydrostatic waves in the region directly above the island; the dominant effect of horizontal geometrical spreading in the lower ˜30 km of the atmosphere, compared to the effects of refraction and background density variation; and the enhanced geometrical spreading due to directional wind in the approach to a critical layer in the mesosphere.

  6. Multi-mode application of graphene quantum dots bonded silica stationary phase for high performance liquid chromatography.

    Science.gov (United States)

    Wu, Qi; Sun, Yaming; Zhang, Xiaoli; Zhang, Xia; Dong, Shuqing; Qiu, Hongdeng; Wang, Litao; Zhao, Liang

    2017-04-07

    Graphene quantum dots (GQDs), which possess hydrophobic, hydrophilic, π-π stacking and hydrogen bonding properties, have great prospect in HPLC. In this study, a novel GQDs bonded silica stationary phase was prepared and applied in multiple separation modes including normal phase, reversed phase and hydrophilic chromatography mode. Alkaloids, nucleosides and nucleobases were chosen as test compounds to evaluate the separation performance of this column in hydrophilic chromatographic mode. The tested polar compounds achieved baseline separation and the resolutions reached 2.32, 4.62, 7.79, 1.68 for thymidine, uridine, adenosine, cytidine and guanosine. This new column showed satisfactory chromatographic performance for anilines, phenols and polycyclic aromatic hydrocarbons in normal and reversed phase mode. Five anilines were completely separated within 10min under the condition of mobile phase containing only 10% methanol. The effect of water content, buffer concentration and pH on chromatographic separation was further investigated, founding that this new stationary phase showed a complex retention mechanism of partitioning, adsorption and electrostatic interaction in hydrophilic chromatography mode, and the multiple retention interactions such as π-π stacking and π-π electron-donor-acceptor interaction played an important role during the separation process. This GQDs bonded column, which allows us to adjust appropriate chromatography mode according to the properties of analytes, has possibility in actual application after further research. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

    Science.gov (United States)

    Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

    2016-06-01

    In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A phase angle based diagnostic scheme to planetary gear faults diagnostics under non-stationary operational conditions

    Science.gov (United States)

    Feng, Ke; Wang, Kesheng; Ni, Qing; Zuo, Ming J.; Wei, Dongdong

    2017-11-01

    Planetary gearbox is a critical component for rotating machinery. It is widely used in wind turbines, aerospace and transmission systems in heavy industry. Thus, it is important to monitor planetary gearboxes, especially for fault diagnostics, during its operational conditions. However, in practice, operational conditions of planetary gearbox are often characterized by variations of rotational speeds and loads, which may bring difficulties for fault diagnosis through the measured vibrations. In this paper, phase angle data extracted from measured planetary gearbox vibrations is used for fault detection under non-stationary operational conditions. Together with sample entropy, fault diagnosis on planetary gearbox is implemented. The proposed scheme is explained and demonstrated in both simulation and experimental studies. The scheme proves to be effective and features advantages on fault diagnosis of planetary gearboxes under non-stationary operational conditions.

  9. Preparation of a novel dual-function strong cation exchange/hydrophobic interaction chromatography stationary phase for protein separation.

    Science.gov (United States)

    Zhao, Kailou; Yang, Li; Wang, Xuejiao; Bai, Quan; Yang, Fan; Wang, Fei

    2012-08-30

    We have explored a novel dual-function stationary phase which combines both strong cation exchange (SCX) and hydrophobic interaction chromatography (HIC) characteristics. The novel dual-function stationary phase is based on porous and spherical silica gel functionalized with ligand containing sulfonic and benzyl groups capable of electrostatic and hydrophobic interaction functionalities, which displays HIC character in a high salt concentration, and IEC character in a low salt concentration in mobile phase employed. As a result, it can be employed to separate proteins with SCX and HIC modes, respectively. The resolution and selectivity of the dual-function stationary phase were evaluated under both HIC and SCX modes with standard proteins and can be comparable to that of conventional IEC and HIC columns. More than 96% of mass and bioactivity recoveries of proteins can be achieved in both HIC and SCX modes, respectively. The results indicated that the novel dual-function column could replace two individual SCX and HIC columns for protein separation. Mixed retention mechanism of proteins on this dual-function column based on stoichiometric displacement theory (SDT) in LC was investigated to find the optimal balance of the magnitude of electrostatic and hydrophobic interactions between protein and the ligand on the silica surface in order to obtain high resolution and selectivity for protein separation. In addition, the effects of the hydrophobicity of the ligand of the dual-function packings and pH of the mobile phase used on protein separation were also investigated in detail. The results show that the ligand with suitable hydrophobicity to match the electrostatic interaction is very important to prepare the dual-function stationary phase, and a better resolution and selectivity can be obtained at pH 6.5 in SCX mode. Therefore, the dual-function column can replace two individual SCX and HIC columns for protein separation and be used to set up two-dimensional liquid

  10. 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.

  11. Evaluation of innovative stationary phase ligand chemistries and analytical conditions for the analysis of basic drugs by supercritical fluid chromatography.

    Science.gov (United States)

    Desfontaine, Vincent; Veuthey, Jean-Luc; Guillarme, Davy

    2016-03-18

    Similar to reversed phase liquid chromatography, basic compounds can be highly challenging to analyze by supercritical fluid chromatography (SFC), as they tend to exhibit poor peak shape, especially those with high pKa values. In this study, three new stationary phase ligand chemistries available in sub -2 μm particle sizes, namely 2-picolylamine (2-PIC), 1-aminoanthracene (1-AA) and diethylamine (DEA), were tested in SFC conditions for the analysis of basic drugs. Due to the basic properties of these ligands, it is expected that the repulsive forces may improve peak shape of basic substances, similarly to the widely used 2-ethypyridine (2-EP) phase. However, among the 38 tested basic drugs, less of 10% displayed Gaussian peaks (asymmetry between 0.8 and 1.4) using pure CO2/methanol on these phases. The addition of 10mM ammonium formate as mobile phase additive, drastically improved peak shapes and increased this proportion to 67% on 2-PIC. Introducing the additive in the injection solvent rather than in the organic modifier, gave acceptable results for 2-PIC only, with 31% of Gaussian peaks with an average asymmetry of 1.89 for the 38 selected basic drugs. These columns were also compared to hybrid silica (BEH), DIOL and 2-EP stationary phases, commonly employed in SFC. These phases commonly exhibit alternative retention and selectivity. In the end, the two most interesting ligands used as complementary columns were 2-PIC and BEH, as they provided suitable peak shapes for the basic drugs and almost orthogonal selectivities. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi.

    Science.gov (United States)

    Feng, Jie; Zhang, Shuo; Shi, Wanliang; Zubcevik, Nevena; Miklossy, Judith; Zhang, Ying

    2017-01-01

    Although the majority of patients with acute Lyme disease can be cured with the standard 2-4 week antibiotic treatment, about 10-20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi ( B. burgdorferi ) has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen) at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be considered as a

  13. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi

    Science.gov (United States)

    Feng, Jie; Zhang, Shuo; Shi, Wanliang; Zubcevik, Nevena; Miklossy, Judith; Zhang, Ying

    2017-01-01

    Although the majority of patients with acute Lyme disease can be cured with the standard 2–4 week antibiotic treatment, about 10–20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi (B. burgdorferi) has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen) at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be considered as a

  14. A Stationary Reference Frame Grid Synchronization System for Three-Phase Grid-Connected Power Converters Under Adverse Grid Conditions

    DEFF Research Database (Denmark)

    Rodríguez, P.; Luna, A.; Muñoz-Aguilar, R. S.

    2012-01-01

    synchronization method for three-phase three-wire networks, namely dual second-order generalized integrator (SOGI) frequency-locked loop. The method is based on two adaptive filters, implemented by using a SOGI on the stationary αβ reference frame, and it is able to perform an excellent estimation......Grid synchronization algorithms are of great importance in the control of grid-connected power converters, as fast and accurate detection of the grid voltage parameters is crucial in order to implement stable control strategies under generic grid conditions. This paper presents a new grid...

  15. Thin-layer chromatography with stationary phase gradient as a method for separation of water-soluble vitamins.

    Science.gov (United States)

    Cimpoiu, Claudia; Hosu, Anamaria; Puscas, Anitta

    2012-02-03

    The group of hydrophilic vitamins play an important role in human health, and their lack or excess produces specific diseases. Therefore, the analysis of these compounds is indispensable for monitoring their content in pharmaceuticals and food in order to prevent some human diseases. TLC was successfully applied in the analysis of hydrophilic vitamins, but the most difficult problem in the simultaneous analysis of all these compounds is to find an optimum stationary phase-mobile phase system due to different chemical characteristics of analytes. Unfortunately structural analogues are difficult to separate in one chromatographic run, and this is the case in hydrophilic vitamins investigations. TLC gives the possibility to perform two-dimensional separations by using stationary phase gradient achieving the highest resolution by combining two systems with different selectivity. The goal of this work was to develop a method of analysis enabling separation of hydrophilic vitamins using TLC with adsorbent gradient. The developed method was used for identifying the water-soluble vitamins in alcoholic extracts of Hippophae rhamnoides and of Ribes nigrum. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Heat-shock induction of ionizing radiation resistance in Saccharomyces cerevisiae, and the correlation with stationary growth phase

    International Nuclear Information System (INIS)

    Mitchel, R.E.J.; Morrison, D.P.

    1982-01-01

    Radiation resistance and thermal resistance vary as a function of culture temperature in logarithmically growing Saccharomyces cerevisiae and are related to the optimum temperature for growth. Radiation resistance and thermal resistance were also induced when cells grown at low temperatures were subjected to a heat shock at or above the optimum growth temperature. Exposure to ionizing radiation followed by a short incubation at low temperature also induced resistance to killing by heat. Heat-shocked cells are induced to a level of thermal and radioresistance much greater than the characteristic resistance level of cells grown continuously at the shock temperature. This high level of resistance, which resembles that of stationary-phase cells, decays to the characteristic log-phase level within one doubling of cell number after the heat shock. Both induction of resistance and decay of that induction require protein synthesis. It is postulated that induction of resistance by heat shock or ionizing radiation is a response of the cells to stress and represents a preparation to enter stationary phase

  17. Diversity oriented high-throughput screening of 1,3,4-oxadiazole modified chlorophenylureas and halogenobenzamides by HPLC with peptidomimetic calixarene-bonded stationary phases.

    Science.gov (United States)

    Bazylak, Grzegorz; Malak, Anna; Ali, Imran; Borowiak, Teresa; Dutkiewicz, Grzegorz

    2008-06-01

    Retention profiles in series of the neutral and highly hydrophobic 1,3,4-oxadiazoles containing chlorophenylurea and halogenobenzamide moiety and indicating analgesic activity were determined in the isocratic standard- and narrow-bore HPLC systems employing, respectively, various octadecylsilica and different calixarene bonded stationary phases. When acetonitrile - 2.65 mM phosphoric acid (55 : 45, %, v/v), pH* 3.25, mobile phase was applied retention of these compounds increased with decline of their overall hydrophobicity according to the general preference of more polar compounds by calixarene cavity in time of its non-specific host-guest supramolecular interactions with halogenated substances. The size of calixarene nanocavity and its upper-rim substitution did not change the observed retention order, resolution and selectivity of separation for oxadiazoles. Compared to the retention on the non-end-capped and the highly-end-capped octadecylsilica HPLC column a most improved separation of some regioisomers of halogenated 1,3,4-oxadiazoles were observed on both used calixarene-type HPLC supports. In addition, preliminary data on the self-assembled supramolecular crystal structure of exemplary 1,3,4-oxadiazolchlorophenylurea with cis-elongated conformation was reported and formation of the monovalent inclusion host-guest complexes between 1,3,4-oxadiazoles and each calixarene-type stationary phase was studied with molecular modelling MM+ and AM1 methods. The structural, isomeric and energetic factors leading to the hydrogen bond stabilized inclusion complexes between these species were considered and used for explanation of observed retention sequence and selectivity of 1,3,4-oxadiazoles separation in applied calixarene-based HPLC systems. All these data would be useful in future development of optimized procedures enabling encapsulation of 1,3,4-oxadiazolurea-type drugs with calixarenes.

  18. Determination of nitrosamines and caffeine metabolites in wastewaters using gas chromatography mass spectrometry and ionic liquid stationary phases.

    Science.gov (United States)

    Reyes-Contreras, Carolina; Domínguez, Carmen; Bayona, Josep M

    2012-10-26

    Recently, the interest to assess the environmental and human health effects of a wide group of emerging contaminants is growing worldwide. However, one of the main problems associated to their exposure is their determination in environmental matrices. It is hindered by the high polarity of most of these analytes, the poor selectivity obtained with low polarity stationary phases and the high background obtained with polar columns commonly used in GC-MS. Accordingly, this study examines the suitability of ionic liquid (IL) (e.g. SLB-IL59, SLB-IL61, SLB-IL82 and SLB-IL111) as stationary phases for GC-MS and their application to the determination of nitrosamines and caffeine metabolites in wastewater samples. Different chromatographic conditions were evaluated and results discussed in terms of resolution and peak symmetry. The SLB-IL111 column enabled the baseline separation and quantification of 7 nitrosamines in a shorter analysis time compared with cyanopropylphenyl polysiloxane commonly used. On the other hand, the SLB-IL59 column provided the best results for caffeine metabolites. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Effect of Secondary Equilibria on the Adsorption of Ibuprofen Enantiomers on a Chiral Stationary Phase with a Grafted Antibiotic Eremomycin

    Science.gov (United States)

    Reshetova, E. N.; Asnin, L. D.; Kachmarsky, K.

    2018-02-01

    The chromatographic separation of ibuprofen enantiomers on a Nautilus-E chiral stationary phase with a grafted eremomycin antibiotic at high column loading is accompanied by distortion of the shape of chromatographic peaks. A model is proposed to explain this phenomenon. A number of factors are considered in the model: the ionization of ibuprofen in the mobile phase, the pH change in the mass transfer zone caused by ionization, and competitive adsorption involving buffer components. Simulations performed using this model within the theory of nonequilibrium chromatography allow the shape of chromatograms for large amounts of S- and R-ibuprofen samples to be predicted. The adsorption mechanism is found to be mainly ion-exchange. The contribution from the molecular adsorption of ibuprofen to the total retention is shown to be several percent.

  20. Optimization of o-phtaldialdehyde/2-mercaptoethanol postcolumn reaction for the hydrophilic interaction liquid chromatography determination of memantine utilizing a silica hydride stationary phase.

    Science.gov (United States)

    Douša, Michal; Pivoňková, Veronika; Sýkora, David

    2016-08-01

    A rapid procedure for the determination of memantine based on hydrophilic interaction chromatography with fluorescence detection was developed. Fluorescence detection after postcolumn derivatization with o-phtaldialdehyde/2-mercaptoethanol was performed at excitation and emission wavelengths of 345 and 450 nm, respectively. The postcolumn reaction conditions such as reaction temperature, derivatization reagent flow rate, and reagents concentration were studied due to steric hindrance of amino group of memantine. The derivatization reaction was applied for the hydrophilic interaction liquid chromatography method which was based on Cogent Silica-C stationary phase with a mobile phase consisting of a mixture of 10 mmol/L citric acid and 10 mmol/L o-phosphoric acid (pH 6.0) with acetonitrile using an isocratic composition of 2:8 v/v. The benefit of the reported approach consists in a simple sample pretreatment and a quick and sensitive hydrophilic interaction chromatography method. The developed method was validated in terms of linearity, accuracy, precision, and selectivity according to the International Conference on Harmonisation guidelines. The developed method was successfully applied for the analysis of commercial memantine tablets. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. A Model for Solving the Maxwell Quasi Stationary Equations in a 3-Phase Electric Reduction Furnace

    Directory of Open Access Journals (Sweden)

    S. Ekrann

    1982-10-01

    Full Text Available A computer code has been developed for the approximate computation of electric and magnetic fields within an electric reduction furnace. The paper describes the numerical methods used to solve Maxwell's quasi-stationary equations, which are the governing equations for this problem. The equations are discretized by a staggered grid finite difference technique. The resulting algebraic equations are solved by iterating between computations of electric and magnetic quantities. This 'outer' iteration converges only when the skin depth is larger or of about the same magnitude as the linear dimensions of the computational domain. In solving for electric quantities with magnetic quantities being regarded as known, and vice versa, the central computational task is the solution of a Poisson equation for a scalar potential. These equations are solved by line successive overrelaxation combined with a rebalancing technique.

  2. Iptycene-based stationary phase with three-dimensional aromatic structure for highly selective separation of H-bonding analytes and aromatic isomers.

    Science.gov (United States)

    Yang, Xiaohong; Han, Ying; Qi, Meiling; Chen, Chuanfeng

    2016-05-06

    Unique structures and molecular recognition ability endow iptycene derivatives with great potential as stationary phases in chromatography, which, however, has not been explored yet. Herein, we report the first example of utilizing a pentiptycene quinone (PQ) for gas chromatographic (GC) separations. Remarkably, the statically coated capillary column with the stationary phase achieved extremely high column efficiency of 4800 plates/m. It exhibited preferential retention and high resolving capability for H-bonding and aromatic analytes and positional isomers, showing advantages over the ordinary polysiloxane phase. Moreover, the fabricated iptycene column showed excellent separation repeatability with RSD values of 0.02-0.06% for intra-day, 0.20-0.35% for inter-day and 3.1-5.5% for between-column, respectively. In conclusion, iptycene derivatives as a new class of stationary phases show promising future for their use in GC separations. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. In situ synthesis of metal-organic frameworks in a porous polymer monolith as the stationary phase for capillary liquid chromatography.

    Science.gov (United States)

    Yang, Shengchao; Ye, Fanggui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

    2015-04-21

    In this study, HKUST-1 was synthesized in situ on the porous polymer monolith as the stationary phase for capillary liquid chromatography (cLC). The unique carboxyl functionalized poly(methacrylic acid-co-ethylene dimethacrylate) (poly(MAA-co-EDMA)) monolith was used as a support to directly grow HKUST-1 by a controlled layer-by-layer self-assembly strategy. X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry, and Fourier transform infrared spectroscopy of the resulting HKUST-1-poly(MAA-co-EDMA) monoliths indicated that HKUST-1 was successfully grafted onto the pore surface of the poly(MAA-co-EDMA) monolith. The column performance of HKUST-1-poly(MAA-co-EDMA) monoliths for the separation of various small molecules, such as benzenediols, xylenes, ethylbenzenes, and styrenes, was evaluated. The chromatographic performance was found to improve with increasing HKUST-1 density, and the column efficiencies and resolutions of HKUST-1-poly(MAA-co-EDMA) monoliths were 18 320-19 890 plates m(-1) and 1.62-6.42, respectively, for benzenediols. The HKUST-1-poly(MAA-co-EDMA) monolith displayed enhanced resolution for the separation of positional isomers when compared to the traditional C18 and HKUST-1 incorporated polymer monoliths. Hydrophobic, π-π, and hydrogen bonding interactions within the HKUST-1-poly(MAA-co-EDMA) monolith were observed in the separation of small molecules. The results showed that the HKUST-1-poly(MAA-co-EDMA) monoliths are promising stationary phases for cLC.

  4. Gaseous phase heat capacity of benzoic acid

    NARCIS (Netherlands)

    Santos, L.M.N.B.F.; Alves da Rocha, M.A.; Gomes, L.R.; Schröder, B.; Coutinho, J.A.P.

    2010-01-01

    The gaseous phase heat capacity of benzoic acid (BA) was proven using the experimental technique called the "in vacuum sublimation/vaporization Calvet microcalorimetry drop method". To overcome known experimental shortfalls, the gaseous phase heat capacity of BA monomer was estimated by ab initio

  5. Synthesis of a stationary phase based on silica modified with branched octadecyl groups by Michael addition and photoinduced thiol-yne click chemistry for the separation of basic compounds.

    Science.gov (United States)

    Huang, Guang; Ou, Junjie; Wang, Hongwei; Ji, Yongsheng; Wan, Hao; Zhang, Zhang; Peng, Xiaojun; Zou, Hanfa

    2016-04-01

    A novel silica-based stationary phase with branched octadecyl groups was prepared by the sequential employment of the Michael addition reaction and photoinduced thiol-yne click chemistry with 3-aminopropyl-functionalized silica microspheres as the initial material. The resulting stationary phase denoted as SiO2 -N(C18)4 was characterized by elemental analysis, FTIR spectroscopy and Raman spectroscopy, demonstrating the existence of branched octadecyl groups in silica microspheres. The separations of benzene homologous compounds, acid compounds and amine analogues were conducted, demonstrating mixed-mode separation mechanism on SiO2 -N(C18)4 . Baseline separation of basic drugs mixture was acquired with the mobile phase of acetonitrile/H2 O (5%, v/v). SiO2 -N(C18)4 was further applied to separate Corydalis yanhusuo Wang water extracts, and more baseline separation peaks were obtained for SiO2 -N(C18)4 than those on Atlantis dC18 column. It can be expected that this new silica-based stationary phase will exhibit great potential in the analysis of basic compounds. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. The Optical Resolution of Chiral Tetrahedrone-type Clusters Contai- ning SCoFeM (M=Mo or W) Using High Performance Liquid Chromatography Chiral Stationary Phase

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Amylose tris (phenylcarbamate) chiral stationary phase (ATPC-CSP) was prepared and used for optical resolution of clusters 1 and 2. n-Hexane/2-propanol ( 99/1; v/v) were found to be the most suitable mobile phase on ATPC-CSP.

  7. Enantioseparation and impurity determination of the enantiomers of novel phenylethanolamine derivatives by high performance liquid chromatography on amylose stationary phase

    International Nuclear Information System (INIS)

    Yang Jing; Guan Jin; Pan Li; Jiang Kun; Cheng Maosheng; Li Famei

    2008-01-01

    Simple and efficient analytical HPLC methods using Chiralpak AS-H as chiral stationary phase were developed for direct enantioseparation of 11 novel phenylethanolamine derivatives. The chromatographic experiments were performed in normal phase mode with n-hexane-ethanol-triethylamine (TEA) as mobile phase. Excellent baseline enantioseparation was obtained for most of compounds. The effects of the concentration of organic modifiers and column temperature were studied for the enantiomeric separation. The mechanism of chiral recognition was discussed based on the relationship between the thermodynamic parameters and structures of compounds. It was found that the enantioseparations were all enthalpy driven, and the tert-butyl groups of compounds had significant influence on the chiral recognition. Trantinterol enantiomers were resolved (R s = 2.73) within 14 min using n-hexane-ethanol-TEA (98:2:0.1, v/v/v) as mobile phase with a flow rate of 0.8 mL min -1 at 30 deg. C. The optimized method was validated for linearity, precision, accuracy and stability in solution and proved to be robust. The limits of detection (LOD) and quantification (LOQ) for (+)-trantinterol were 0.15 and 0.46 μg mL -1 . The method was applied for enantiomeric impurity determination of (-)-trantinterol bulk samples

  8. Morphological and quantitative changes in mitochondria, plastids, and peroxisomes during the log-to-stationary transition of the growth phase in cultured tobacco BY-2 cells.

    Science.gov (United States)

    Toyooka, Kiminori; Sato, Mayuko; Wakazaki, Mayumi; Matsuoka, Ken

    2016-01-01

    We developed a wide-range and high-resolution transmission electron microscope acquisition system and obtained giga-pixel images of tobacco BY-2 cells during the log and stationary phases of cell growth. We demonstrated that the distribution and ultrastructure of compartments involved in membrane traffic (i.e., Golgi apparatus, multivesicular body, and vesicle cluster) change during the log-to-stationary transition. Mitochondria, peroxisomes, and plastids were also enumerated. Electron densities of mitochondria and peroxisomes were altered during the growth-phase shift, while their numbers were reduced by nearly half. Plastid structure dramatically changed from atypical to spherical with starch granules. Nearly the same number of plastids was observed in both log and stationary phases. These results indicate that mechanisms regulating organelle populations differ from organelle to organelle.

  9. Kinetic modeling of sporulation and product formation in stationary phase by Bacillus coagulans RK-02 vis-à-vis other Bacilli.

    Science.gov (United States)

    Das, Subhasish; Sen, Ramkrishna

    2011-10-01

    A logistic kinetic model was derived and validated to characterize the dynamics of a sporogenous bacterium in stationary phase with respect to sporulation and product formation. The kinetic constants as determined using this model are particularly important for describing intrinsic properties of a sporogenous bacterial culture in stationary phase. Non-linear curve fitting of the experimental data into the mathematical model showed very good correlation with the predicted values for sporulation and lipase production by Bacillus coagulans RK-02 culture in minimal media. Model fitting of literature data of sporulation and product (protease and amylase) formation in the stationary phase by some other Bacilli and comparison of the results of model fitting with those of Bacillus coagulans helped validate the significance and robustness of the developed kinetic model. Copyright © 2011 Elsevier Ltd. All rights reserved.

  10. Two-dimensional high-performance thin-layer chromatography of tryptic bovine albumin digest using normal- and reverse-phase systems with silanized silica stationary phase.

    Science.gov (United States)

    Gwarda, Radosław Łukasz; Dzido, Tadeusz Henryk

    2013-10-18

    Among many advantages of planar techniques, two-dimensional (2D) separation seems to be the most important for analysis of complex samples. Here we present quick, simple and efficient two-dimensional high-performance thin-layer chromatography (2D HPTLC) of bovine albumin digest using commercial HPTLC RP-18W plates (silica based stationary phase with chemically bonded octadecyl ligands of coverage density 0.5μmol/m(2) from Merck, Darmstadt). We show, that at low or high concentration of water in the mobile phase comprised methanol and some additives the chromatographic systems with the plates mentioned demonstrate normal- or reversed-phase liquid chromatography properties, respectively, for separation of peptides obtained. These two systems show quite different separation selectivity and their combination into 2D HPTLC process provides excellent separation of peptides of the bovine albumin digest. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Comparison of Separation of Seed Oil Triglycerides Containing Isomeric Conjugated Octadecatrienoic Acid Moieties by Reversed-Phase HPLC

    OpenAIRE

    Anh Van Nguyen; Victor Deineka; Lumila Deineka; Anh Vu Thi Ngoc

    2017-01-01

    Relative retention analysis and increment approach were applied for the comparison of triglycerides (TGs) retention of a broad set of plant seed oils with isomeric conjugated octadecatrienoic acids (CLnA) by reversed-phase HPLC for “propanol-2-acetonitrile” mobile phases and Kromasil 100-5C18 stationary phase with diode array detection (DAD) and mass spectrometric (MS) detection. The subjects of investigation were TGs of seed oils: Calendula officinalis, Catalpa ovata, Jacaranda mimosifolia, ...

  12. Evaluation of different hydrophilic stationary phases for the simultaneous determination of iminosugars and other low molecular weight carbohydrates in vegetable extracts by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Rodríguez-Sánchez, S; Quintanilla-López, J E; Soria, A C; Sanz, M L

    2014-11-01

    Iminosugars are considered potential drug candidates for the treatment of several diseases, mainly as a result of their α-glycosidase inhibition properties. A method by hydrophilic interaction liquid chromatography tandem mass spectrometry has been optimized for the first time for the simultaneous determination of complex mixtures of bioactive iminosugars and other low molecular weight carbohydrates (LMWC) in vegetable extracts. Three hydrophilic stationary phases (sulfoalkylbetaine zwitterionic, polyhydroxyethyl aspartamide and ethylene bridge hybrid (BEH) with trifunctionally bonded amide) were compared under both basic and acidic conditions. The best sensitivity (limits of detection between 0.025 and 0.28ngmL -1 ) and overall chromatographic performance in terms of resolution, peak width and analysis time were obtained with the BEH amide column using 0.1% ammonium hydroxide as a mobile phase additive. The optimized method was applied to the analysis of extracts of hyacinth bulbs, buckwheat seeds and mulberry leaves. Iminosugar and other LMWC structures were tentatively assigned by their high resolution daughter ions mass spectra. Several iminosugars such as glycosyl-fagomine in mulberry extract were also described for the first time. Among the extracts analysed, mulberry showed the widest diversity of iminosugars, whereas the highest content of them was found in hyacinth bulb (2.5mgg -1 ) followed by mulberry (1.95 mgg -1 ). Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Contaminants migration in the soil: the influence of transfer between the mobile and stationary phases

    International Nuclear Information System (INIS)

    Moreira, R.M.; Sabino, C.S.V.; Macedo, W.A.

    1996-01-01

    Three transport mechanisms control the contaminant migration in saturated soils: advection, diffusion and interchanges between liquid and solid phases. These interchanges define the retention by the soil and the contaminant delay related to the liquid phase flow. Therefore, the knowledge of the adsorption/desorption characteristics of the solute in solid surfaces is fundamental for the evaluation of toxic agent releases to the compartment soil. This communication reports the study which is being performed by the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) in this area, particularly with cesium and mercury by using X-ray absorption spectroscopy for contaminants migration

  14. Antimicrobial efficacy of chlorine dioxide against Candida albicans in stationary and starvation phases in human root canal: An in-vitro study

    Directory of Open Access Journals (Sweden)

    Shirur Krishnaraj Somayaji

    2014-01-01

    Full Text Available Introduction: Candida albicans (C. albicans is the most commonly isolated fungal pathogen from dental root canal. C. albicans forms biofilm and develops resistance against root canal irrigants . This study determines the fungicidal efficacy of 13.8% chlorine dioxide in extracted human teeth at stationary and starvation phases of C. albicans. Materials and Methods: Teeth were decoronated and coronal portion of the roots were prepared into blocks, which were incubated at 37°C with C. albicans for five days. The samples were treated with chlorine dioxide for 12 and 20 minutes. Total of fifty blocks were taken in the study. Colony-forming units were counted in Sabourauds dextrose agar and scanning electron microscopic observation was done. Data were analyzed by one-way ANOVA and Bonferoni′s post hoc test. Results: Teeth at stationary phase (12 min showed mean colony count of 28,000 ± 1814 which is significantly (P < 0.001 less than control group. Teeth at starvation phase (12 min showed colony count of 65,600 ± 1912 which is also significantly (P < 0.001 less than control group. Teeth irrigated at stationary phase (20 min showed mean colony count of 23,400 ± 1776 (P < 0.001. Teeth irrigated at starvation phase (20 min showed mean colony count of 48,100 ± 1663 which is also significantly (P < 0.001 less than that of control group. Conclusion: Treatment of chlorine dioxide reduces the C. albicans count in root canals of extracted human teeth at stationary and starvation phases. Efficacy of chlorine dioxide against C. albicans is relatively higher in stationary phase than that of starvation phase.

  15. Characterization of bonded stationary phase performance as a function of qualitative and quantitative chromatographic factors in chaotropic chromatography with risperidone and its impurities as model substances.

    Science.gov (United States)

    Čolović, Jelena; Rmandić, Milena; Malenović, Anđelija

    2018-05-17

    Numerous stationary phases have been developed with the aim to provide desired performances during chromatographic analysis of the basic solutes in their protonated form. In this work, the procedure for the characterization of bonded stationary phase performance, when both qualitative and quantitative chromatographic factors were varied in chaotropic chromatography, was proposed. Risperidone and its three impurities were selected as model substances, while acetonitrile content in the mobile phase (20-30%), the pH of the aqueous phase (3.00-5.00), the content of chaotropic agents in the aqueous phase (10-100 mM), type of chaotropic agent (NaClO 4 , CF 3 COONa), and stationary phase type (Zorbax Eclipse XDB, Zorbax Extend) were studied as chromatographic factors. The proposed procedure implies the combination of D-optimal experimental design, indirect modeling, and polynomial-modified Gaussian model, while grid point search method was selected for the final choice of the experimental conditions which lead to the best possible stationary phase performance for basic solutes. Good agreement between experimentally obtained chromatogram and simulated chromatogram for chosen experimental conditions (25% acetonitrile, 75 mM of NaClO 4 , pH 4.00 on Zorbax Eclipse XDB column) confirmed the applicability of the proposed procedure. The additional point was selected for the verification of proposed procedure ability to distinguish changes in solutes' elution order. Simulated chromatogram for 21.5% acetonitrile, 85 mM of NaClO 4 , pH 5.00 on Zorbax Eclipse XDB column was in line with experimental data. Furthermore, the values of left and right peak half-widths obtained from indirect modeling were used in order to evaluate performances of differently modified stationary phases applying a half-width plots approach. The results from half-width plot approach as well as from the proposed procedure indicate higher efficiency and better separation performance of the stationary phase

  16. Analytical and semipreparative chiral separation of cis-itraconazole on cellulose stationary phases by high-performance liquid chromatography.

    Science.gov (United States)

    Kurka, Ondřej; Kučera, Lukáš; Bednář, Petr

    2016-07-01

    cis-Itraconazole is a chiral antifungal drug administered as a racemate. The knowledge of properties of individual cis-itraconazole stereoisomers is vital information for medicine and biosciences as different stereoisomers of cis-itraconazole may possess different affinity to certain biological pathways in the human body. For this purpose, either chiral synthesis of enantiomers or chiral separation of racemate can be used. This paper presents a two-step high-performance liquid chromatography approach for the semipreparative isolation of four stereoisomers (two enantiomeric pairs) of itraconazole using polysaccharide stationary phases and volatile organic mobile phases without additives in isocratic mode. The approach used involves the separation of the racemate into three fractions (i.e. two pure stereoisomers and one mixed fraction containing the remaining two stereoisomers) in the first run and consequent separation of the collected mixed fraction in the second one. For this purpose, combination of cellulose tris-(4-methylbenzoate) and cellulose tris-(3,5-dimehylphenylcarbamate) columns with complementary selectivity for cis-itraconazole provided full separation of all four stereoisomers (with purity of each isomer > 97%). The stereoisomers were collected, their optical rotation determined and their identity confirmed based on the results of a previously published study. Pure separated stereoisomers are subjected to further biological studies. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Capillary gas chromatographic separation of organic bases using a pH-adjusted basic water stationary phase.

    Science.gov (United States)

    Darko, Ernest; Thurbide, Kevin B

    2016-09-23

    The use of a pH-adjusted water stationary phase for analyzing organic bases in capillary gas chromatography (GC) is demonstrated. Through modifying the phase to typical values near pH 11.5, it is found that various organic bases are readily eluted and separated. Conversely, at the normal pH 7 operating level, they are not. Sodium hydroxide is found to be a much more stable base than ammonium hydroxide for altering the pH due to the higher volatility and evaporation of the latter. In the basic condition, such analytes are not ionized and are observed to produce good peak shapes even for injected masses down to about 20ng. By comparison, analyses on a conventional non-polar capillary GC column yield more peak tailing and only analyte masses of 1μg or higher are normally observed. Through carefully altering the pH, it is also found that the selectivity between analytes can be potentially further enhanced if their respective pKa values differ sufficiently. The analysis of different pharmaceutical and petroleum samples containing organic bases is demonstrated. Results indicate that this approach can potentially offer unique and beneficial selectivity in such analyses. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Comparison of core-shell and totally porous ultra high performance liquid chromatographic stationary phases based on their selectivity towards alfuzosin compounds.

    Science.gov (United States)

    Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

    2014-06-13

    This paper focuses on the application of a column classification system based on the Katholieke Universiteit Leuven for the characterization of physicochemical properties of core-shell and ultra-high performance liquid chromatographic stationary phases, followed by the verification of the reliability of the obtained column classification in pharmaceutical practice. In the study, 7 stationary phases produced in core-shell technology and 18 ultra-high performance liquid chromatographic columns were chromatographically tested, and ranking lists were built on the FKUL-values calculated against two selected reference columns. In the column performance test, an analysis of alfuzosin in the presence of related substances was carried out using the brands of the stationary phases with the highest ranking positions. Next, a system suitability test as described by the European Pharmacopoeia monograph was performed. Moreover, a study was also performed to achieve a purposeful shortening of the analysis time of the compounds of interest using the selected stationary phases. Finally, it was checked whether methods using core-shell and ultra-high performance liquid chromatographic columns can be an interesting alternative to the high-performance liquid chromatographic method for the analysis of alfuzosin in pharmaceutical practice. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Enantiomeric separation of type I and type II pyrethroid insecticides with different chiral stationary phases by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Zhang, Ping; Yu, Qian; He, Xiulong; Qian, Kun; Xiao, Wei; Xu, Zhifeng; Li, Tian; He, Lin

    2018-04-01

    The enantiomeric separation of type I (bifenthrin, BF) and type II (lambda-cyhalothrin, LCT) pyrethroid insecticides on Lux Cellulose-1, Lux Cellulose-3, and Chiralpak IC chiral columns was investigated by reversed-phase high-performance liquid chromatography. Methanol/water or acetonitrile/water was used as mobile phase at a flow rate of 0.8 mL/min. The effects of chiral stationary phase, mobile phase composition, column temperature, and thermodynamic parameters on enantiomer separation were carefully studied. Bifenthrin got a partial separation on Lux Cellulose-1 column and baseline separation on Lux Cellulose-3 column, while LCT enantiomers could be completely separated on both Lux Cellulose-1 and Lux Cellulose-3 columns. Chiralpak IC provided no separation ability for both BF and LCT. Retention factor (k) and selectivity factor (α) decreased with the column temperature increasing from 10°C to 40°C for both BF and LCT enantiomers. Thermodynamic parameters including ∆H and ∆S were also calculated, and the maximum R s were not always obtained at lowest temperature. Furthermore, the quantitative analysis methods for BF and LCT enantiomers in soil and water were also established. Such results provide a new approach for pyrethroid separation under reversed-phase condition and contribute to environmental risk assessment of pyrethroids at enantiomer level. © 2017 Wiley Periodicals, Inc.

  20. Polymethacrylate-based monoliths as stationary phases for separation of biopolymers and immobilization of enzymes.

    Science.gov (United States)

    Martinović, Tamara; Josić, Djuro

    2017-11-01

    The experiences in the production and application of polymethacrylate-based monolithic supports, since their development almost thirty years ago, are presented. The main driving force for the development of new chromatographic supports was the necessity for the isolation and separation of physiologically active biopolymers and their use for therapeutic purposes. For this sake, a development of a method for fast separation, preventing denaturation and preserving their biological activity was necessary. Development of polysaccharide-based supports, followed by the introduction of polymer-based chromatographic media, is shortly described. This development was followed by the advances in monolithic media that are now used for both large- and small-scale separation of biopolymers and nanoparticles. Finally, a short overview is given about the applications of monoliths for sample displacement chromatography, resulting in isolation of physiologically active biomolecules, such as proteins, protein complexes, and nucleic acid, as well as high-throughput sample preparation for proteomic investigations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Sinorhizobium meliloti sigma factors RpoE1 and RpoE4 are activated in stationary phase in response to sulfite.

    Directory of Open Access Journals (Sweden)

    Bénédicte Bastiat

    Full Text Available Rhizobia are soil bacteria able to establish a nitrogen-fixing symbiosis with legume plants. Both in soil and in planta, rhizobia spend non-growing periods resembling the stationary phase of in vitro-cultured bacteria. The primary objective of this work was to better characterize gene regulation in this biologically relevant growth stage in Sinorhizobium meliloti. By a tap-tag/mass spectrometry approach, we identified five sigma factors co-purifying with the RNA polymerase in stationary phase: the general stress response regulator RpoE2, the heat shock sigma factor RpoH2, and three extra-cytoplasmic function sigma factors (RpoE1, RpoE3 and RpoE4 belonging to the poorly characterized ECF26 subgroup. We then showed that RpoE1 and RpoE4 i are activated upon metabolism of sulfite-generating compounds (thiosulfate and taurine, ii display overlapping regulatory activities, iii govern a dedicated sulfite response by controlling expression of the sulfite dehydrogenase SorT, iv are activated in stationary phase, likely as a result of endogenous sulfite generation during bacterial growth. We showed that SorT is required for optimal growth of S. meliloti in the presence of sulfite, suggesting that the response governed by RpoE1 and RpoE4 may be advantageous for bacteria in stationary phase either by providing a sulfite detoxification function or by contributing to energy production through sulfite respiration. This paper therefore reports the first characterization of ECF26 sigma factors, the first description of sigma factors involved in control of sulphur metabolism, and the first indication that endogenous sulfite may act as a signal for regulation of gene expression upon entry of bacteria in stationary phase.

  2. [Separation of purines, pyrimidines, pterins and flavonoids on magnolol-bonded silica gel stationary phase by high performance liquid chromatography].

    Science.gov (United States)

    Chen, Hong; Li, Laishen; Zhang, Yang; Zhou, Rendan

    2012-10-01

    A new magnolol-bonded silica gel stationary phase (MSP) was used to separate the basic drugs including four purines, eight pyrimidines, four pterins and five flavonoids as polar representative samples by high performance liquid chromatography (HPLC). To clarify the separation mechanism, a commercial ODS column was also tested under the same chromatographic conditions. The high selectivities and fast baseline separations of the above drugs were achieved by using simple mobile phases on MSP. Although there is no end-caped treatment, the peak shapes of basic drugs containing nitrogen such as purines, pyrimidines and pterins were rather symmetrical on MSP, which indicated the the magnolol as ligand with multi-sites could shield the side effect of residual silanol groups on the surface of silica gel. Although somewhat different in the separation resolution, it was found that the elution orders of some drugs were generally similar on both MSP and ODS. The hydrophobic interaction should play a significant role in the separations of the above basic drugs, which was attributed to their reversed-phase property in the nature. However, MSP could provide the additional sites for many polar solutes, which was a rational explanation for the high selectivity of MSP. For example, in the separation of purines, pyrimidines and pterins on MSP, hydrogen-bonding and dipole-dipole interactions played leading roles besides hydrophobic interaction. Some solute molecules (such as mercaptopurine, vitexicarpin) and MSP can form the strong pi-pi stacking in the separation process. All enhanced the retention and improved the separation selectivity of MSP, which facilitated the separation of the basic drugs.

  3. Synthesis and characterization of nanometric zinc oxide for a stationary phase in liquid chromatography

    International Nuclear Information System (INIS)

    Gordillo-Delgado, F; Soto-Barrera, C C; Plazas-Saldaña, J

    2017-01-01

    The increasing demand for equipment to remove organic compounds in industry and research activity has led to evaluate nanometric zinc oxide (ZnO). In this work, we present the ZnO nanoparticles synthesis for reusing of discarded columns, as a low-cost alternative. The compound was obtained by sol-gel technique using zinc chloride and sodium hydroxide as precursors and a drying temperature of 169°C. An X-ray diffractometer was used to estimate the average particle size at 20.3±0.2nm; the adsorption capacity was 0.0144L/g and the chemical resistance was tested with HCl and NaOH. The ZnO nanopowder was packed with 100psi pressure in an empty C-18 column cavity. The column packing resolution was evaluated using a high performance liquid chromatographer (HPLC-Thermo Scientific Dionex UltiMate 3000); using a caffeine standard, the following parameters were established: solvent flow: 1.2mL/min, average column temperature: 40°C, running time: 10 minutes, mobile phase acetonitrile-water composition (9:1). These results validate the potential of ZnO nanopowder as a column packing material in HPLC technique. (paper)

  4. Dose-rate evidence for two kinds of radiation damage in stationary-phase mammalian cells

    International Nuclear Information System (INIS)

    Metting, N.F.; Braby, L.A.; Roesch, W.C.; Nelson, J.M.

    1985-01-01

    Survival based on colony formation was measured for starved plateau-phase Chinese hamster ovary (CHO) cells exposed to 250 kVp X rays at dose rates of 0.0031, 0.025, 0.18, 0.31, and 1.00 Gy/min. A large dose-rate effect was demonstrated. Delayed plating experiments and dose response experiments following a conditioning dose, both using a dose rate of 1.00 Gy/min and plating delays of up to 48 hr, were also used to investigate the alternative repair hypotheses. There is clearly a greater change in survival in dose-rate experiments than in the other experiments. Thus the authors believe that a process which depends on the square of the concentration of initial damage, and which alters the effect of initial damage on cell survival is being observed. They have applied the damage accumulation model to separate the single-event damage from this concentration-dependent form and estimate the repair rate for the latter type to be 70 min for their CHO cells

  5. Synthesis and characterization of nanometric zinc oxide for a stationary phase in liquid chromatography

    Science.gov (United States)

    Gordillo-Delgado, F.; Soto-Barrera, C. C.; Plazas-Saldaña, J.

    2017-01-01

    The increasing demand for equipment to remove organic compounds in industry and research activity has led to evaluate nanometric zinc oxide (ZnO). In this work, we present the ZnO nanoparticles synthesis for reusing of discarded columns, as a low-cost alternative. The compound was obtained by sol-gel technique using zinc chloride and sodium hydroxide as precursors and a drying temperature of 169°C. An X-ray diffractometer was used to estimate the average particle size at 20.3±0.2nm the adsorption capacity was 0.0144L/g and the chemical resistance was tested with HCl and NaOH. The ZnO nanopowder was packed with 100psi pressure in an empty C-18 column cavity. The column packing resolution was evaluated using a high performance liquid chromatographer (HPLC-Thermo Scientific Dionex UltiMate 3000); using a caffeine standard, the following parameters were established: solvent flow: 1.2mL/min, average column temperature: 40°C, running time: 10 minutes, mobile phase acetonitrile-water composition (9:1). These results validate the potential of ZnO nanopowder as a column packing material in HPLC technique.

  6. Normal-phase liquid chromatography retention behavior of polycyclic aromatic sulfur heterocycles and alkyl-substituted polycyclic aromatic sulfur heterocycle isomers on an aminopropyl stationary phase.

    Science.gov (United States)

    Wilson, Walter B; Hayes, Hugh V; Sander, Lane C; Campiglia, Andres D; Wise, Stephen A

    2018-02-01

    Retention indices for 67 polycyclic aromatic sulfur heterocycles (PASHs) and 80 alkyl-substituted PASHs were determined using normal-phase liquid chromatography (NPLC) on an aminopropyl (NH 2 ) stationary phase. The retention behavior of PASH on the NH 2 phase is correlated with the number of aromatic carbon atoms and two structural characteristics have a significant influence on their retention: non-planarity (thickness, T) and the position of the sulfur atom in the bay-region of the structure. Correlations between solute retention on the NH 2 phase and T of PASHs were investigated for three cata-condensed (cata-) PASH isomer groups: (a) 13 four-ring molecular mass (MM) 234 Da cata-PASHs, (b) 20 five-ring MM 284 Da cata-PASHs, and (c) 12 six-ring MM 334 Da cata-PASHs. Correlation coefficients ranged from r = -0.49 (MM 234 Da) to r = -0.65 (MM 334 Da), which were significantly lower than structurally similar PAH isomer groups (r = -0.70 to r = -0.99). The NPLC retention behavior of the PASHs are compared to similar results for PAHs.

  7. Kinetics of oxidic phase dissolution in acids

    International Nuclear Information System (INIS)

    Gorichev, I.G.; Kipriyanov, N.A.

    1981-01-01

    The critical analysis of the experimental data on dissolution kinetics of metal oxides (BeO, V 2 O 5 , UO 2 , Nb 2 O 5 , Ta 2 O 5 etc.) in acid media is carried out. Kinetic peculiarities of oxide dissolution are explained on the basis of the notions of electron- proton theory. It is established that the surface nonstoichiometric ccomposition of oxide phase and potential jump, appearing on the interface of the oxide-electrolyte phase are the important factors, determining the dissolution rate of a solid phase. The dissolution rate of metal oxides is limited by the transition of protons into the solid oxide phase. Morphological models of heterogeneous kinetics are used when explaining kinetic regularities of oxide dissolution process [ru

  8. Calcium and Magnesium Ions Are Membrane-Active against Stationary-Phase Staphylococcus aureus with High Specificity

    Science.gov (United States)

    Xie, Yuntao; Yang, Lihua

    2016-02-01

    Staphylococcus aureus (S. aureus) is notorious for its ability to acquire antibiotic-resistance, and antibiotic-resistant S. aureus has become a wide-spread cause of high mortality rate. Novel antimicrobials capable of eradicating S. aureus cells including antibiotic-resistant ones are thus highly desired. Membrane-active bactericides and species-specific antimicrobials are two promising sources of novel anti-infective agents for fighting against bacterial antibiotic-resistance. We herein show that Ca2+ and Mg2+, two alkaline-earth-metal ions physiologically essential for diverse living organisms, both disrupt model S. aureus membranes and kill stationary-phase S. aureus cells, indicative of membrane-activity. In contrast to S. aureus, Escherichia coli and Bacillus subtilis exhibit unaffected survival after similar treatment with these two cations, indicative of species-specific activity against S. aureus. Moreover, neither Ca2+ nor Mg2+ lyses mouse red blood cells, indicative of hemo-compatibility. This works suggests that Ca2+ and Mg2+ may have implications in targeted eradication of S. aureus pathogen including the antibiotic-resistant ones.

  9. High enantioselective Novozym 435-catalyzed esterification of (R,S)-flurbiprofen monitored with a chiral stationary phase.

    Science.gov (United States)

    Siódmiak, Tomasz; Mangelings, Debby; Vander Heyden, Yvan; Ziegler-Borowska, Marta; Marszałł, Michał Piotr

    2015-03-01

    Lipases form Candida rugosa and Candida antarctica were tested for their application in the enzymatic kinetic resolution of (R,S)-flurbiprofen by enantioselective esterification. Successful chromatographic separation with well-resolved peaks of (R)- and (S)-flurbiprofen and their esters was achieved in one run on chiral stationary phases by high-performance liquid chromatography (HPLC). In this study screening of enzymes was performed, and Novozym 435 was selected as an optimal catalyst for obtaining products with high enantiopurity. Additionally, the influence of organic solvents (dichloromethane, dichloroethane, dichloropropane, and methyl tert-butyl ether), primary alcohols (methanol, ethanol, n-propanol, and n-butanol), reaction time, and temperature on the enantiomeric ratio and conversion was tested. The high values of enantiomeric ratio (E in the range of 51.3-90.5) of the esterification of (R,S)-flurbiprofen were obtained for all tested alcohols using Novozym 435, which have a great significance in the field of biotechnological synthesis of drugs. The optimal temperature range for the performed reactions was from 37 to 45 °C. As a result of the optimization, (R)-flurbiprofen methyl ester was obtained with a high optical purity, eep = 96.3 %, after 96 h of incubation. The enantiomeric ratio of the reaction was E = 90.5 and conversion was C = 35.7 %.

  10. Heterodyne laser Doppler distance sensor with phase coding measuring stationary as well as laterally and axially moving objects

    International Nuclear Information System (INIS)

    Pfister, T; Günther, P; Nöthen, M; Czarske, J

    2010-01-01

    Both in production engineering and process control, multidirectional displacements, deformations and vibrations of moving or rotating components have to be measured dynamically, contactlessly and with high precision. Optical sensors would be predestined for this task, but their measurement rate is often fundamentally limited. Furthermore, almost all conventional sensors measure only one measurand, i.e. either out-of-plane or in-plane distance or velocity. To solve this problem, we present a novel phase coded heterodyne laser Doppler distance sensor (PH-LDDS), which is able to determine out-of-plane (axial) position and in-plane (lateral) velocity of rough solid-state objects simultaneously and independently with a single sensor. Due to the applied heterodyne technique, stationary or purely axially moving objects can also be measured. In addition, it is shown theoretically as well as experimentally that this sensor offers concurrently high temporal resolution and high position resolution since its position uncertainty is in principle independent of the lateral object velocity in contrast to conventional distance sensors. This is a unique feature of the PH-LDDS enabling precise and dynamic position and shape measurements also of fast moving objects. With an optimized sensor setup, an average position resolution of 240 nm was obtained

  11. Application of Homochiral Alkylated Organic Cages as Chiral Stationary Phases for Molecular Separations by Capillary Gas Chromatography.

    Science.gov (United States)

    Xie, Shengming; Zhang, Junhui; Fu, Nan; Wang, Bangjin; Hu, Cong; Yuan, Liming

    2016-11-08

    Molecular organic cage compounds have attracted considerable attention due to their potential applications in gas storage, catalysis, chemical sensing, molecular separations, etc. In this study, a homochiral pentyl cage compound was synthesized from a condensation reaction of ( S , S )-1,2-pentyl-1,2-diaminoethane and 1,3,5-triformylbenzene. The imine-linked pentyl cage diluted with a polysiloxane (OV-1701) was explored as a novel stationary phase for high-resolution gas chromatographic separation of organic compounds. Some positional isomers were baseline separated on the pentyl cage-coated capillary column. In particular, various types of enantiomers including chiral alcohols, esters, ethers and epoxides can be resolved without derivatization on the pentyl cage-coated capillary column. The reproducibility of the pentyl cage-coated capillary column for separation was investigated using nitrochlorobenzene and styrene oxide as analytes. The results indicate that the column has good stability and separation reproducibility after being repeatedly used. This work demonstrates that molecular organic cage compounds could become a novel class of chiral separation media in the near future.

  12. Application of Homochiral Alkylated Organic Cages as Chiral Stationary Phases for Molecular Separations by Capillary Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Shengming Xie

    2016-11-01

    Full Text Available Molecular organic cage compounds have attracted considerable attention due to their potential applications in gas storage, catalysis, chemical sensing, molecular separations, etc. In this study, a homochiral pentyl cage compound was synthesized from a condensation reaction of (S,S-1,2-pentyl-1,2-diaminoethane and 1,3,5-triformylbenzene. The imine-linked pentyl cage diluted with a polysiloxane (OV-1701 was explored as a novel stationary phase for high-resolution gas chromatographic separation of organic compounds. Some positional isomers were baseline separated on the pentyl cage-coated capillary column. In particular, various types of enantiomers including chiral alcohols, esters, ethers and epoxides can be resolved without derivatization on the pentyl cage-coated capillary column. The reproducibility of the pentyl cage-coated capillary column for separation was investigated using nitrochlorobenzene and styrene oxide as analytes. The results indicate that the column has good stability and separation reproducibility after being repeatedly used. This work demonstrates that molecular organic cage compounds could become a novel class of chiral separation media in the near future.

  13. Behavior of neutral solutes in pressurized flow driven electrochromatography using a mixed stationary phase of ODS and anion-exchange.

    Science.gov (United States)

    Kitagawa, Shinya; Tsuda, Takao

    2003-05-02

    The behavior of neutral sample solutes in pressurized flow driven electrochromatography using a mixed stationary phase, which consisted of ODS and anion-exchange (ODS-SAX), was studied. Applications of both positive and negative voltage on a column induced increases in retention factors of sample solutes. The direction of an electroosmotic flow under applications of positive and negative voltage were the same, therefore, the sign of the surface charge density under positive and negative voltage was opposite. We proposed a new equation for the relationship between applied voltage and surface charge density, and the practical electroosmotic flow conformed to this equation. Studying the electroosmotic flow using our proposed equation revealed that the applied negative voltage accelerates the protonation of the quaternary ammonium group and dissociation of the silanol group on packing materials. The retention behavior of a neutral solute was affected by the existence of the charged functional groups. We propose that this phenomenon is applicable to the control of the retention behavior of a sample solute using an electric field.

  14. Synthesis and characterization of a novel stationary phase, Si-Zr/Ti(PMTDS), based upon ternary oxide support for high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Amparo, Maura R.; Marques, Fabiana A.; Faria, Anizio M., E-mail: anizio@pontal.ufu.br [Universidade Federal de Uberlandia (FACIP/UFU), Ituiutaba, MG (Brazil). Faculdade de Ciencias Integradas do Pontal

    2013-09-15

    A new stationary phase based on the thermal immobilization of poly(methyltetradecylsiloxane) (PMTDS) on silica particles coated with a mixture of zirconia and titania was prepared and evaluated for the chromatographic separation of test mixtures. The spherical particles were characterized by elemental analysis, SEM, FTIR and {sup 29}Si NMR. The physicochemical properties of PMTDS phase supported on Si-Zr/Ti were intermediate between PMTDS phases supported on titanized silica and zirconized silica. The chromatographic performance of Si-Zr/Ti(PMTDS) phase was similar to PMTDS phases based on metal oxide coated silica having only one metal oxide and the preparation of a Si-Zr/Ti(PMTDS) phase allowed evaluation of the effect of each oxide, zirconia and titania, on the separation process and on the stability of the immobilized polymer phase. The hydrolytic stability of Si-Zr/Ti(PMTDS) stationary phase was similar to the Si-Ti(PMTDS) phase, improving the chemical stability of the silica-based PMTDS phase by about 100%. (author)

  15. Silica particles encapsulated poly(styrene-divinylbenzene) monolithic stationary phases for micro-high performance liquid chromatography.

    Science.gov (United States)

    Bakry, R; Stöggl, W M; Hochleitner, E O; Stecher, G; Huck, C W; Bonn, G K

    2006-11-03

    In the paper we demonstrate a new approach for the preparation and application of continuous silica bed columns that involve encapsulation (entrapment) of functionalized silica microparticles, which can be used as packing material in micro high performance liquid chromatography (micro-HPLC) and capillary electrochromatography (CEC). Like traditional packed columns, these capillaries possess characterized silica particles that offer high phase ratio and narrow pore size distribution leading to high retention and separation efficiency, respectively. More importantly, immobilization of the microparticles stabilizes the separation bed and eliminates the need for retaining frits. The developed capillary columns were fabricated in exactly the same way as a packed capillary column (slurry packing) but with an additional entrapment step. This immobilization of the packed bed was achieved by in situ polymerization of styrene and divinylbenzene in presence of decanol as a porogen and azobisisobutyronitrile as thermal initiator. Silica particles with different particle sizes and pore sizes ranging from 60 to 4000 A were studied. In addition different modified silica was used, including C-18 reversed phase, anion exchange and chiral stationary phases. Efficient separation of polyphenolic compounds, peptides, proteins and even DNA mutation were achieved using the developed technique depending on the properties of the silica particles used (particles pore size). For example, using 3 microm ProntoSIL C-18 particles with 300 A pore size, separation efficiencies in the range of 120,000-200,000 plates/m were obtained for protein separation, in a 6 cm x 200 microm i.d. capillary column. Using encapsulated silica C-18 with 1000 A pore size, separation of DNA homo and hetero duplexes were achieved under denaturing HPLC conditions for mutation detection. In addition, nucleotides were separated using anion exchange material encapsulated with poly(styrene-divinylbenzene) (PS/DVB), which

  16. Distinction of synthetic dl-α-tocopherol from natural vitamin E (d-α-tocopherol) by reversed-phase liquid chromatography. Enhanced selectivity of a polymeric C18 stationary phase at low temperature and/or at high pressure.

    Science.gov (United States)

    Yui, Yuko; Miyazaki, Shota; Ma, Yan; Ohira, Masayoshi; Fiehn, Oliver; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

    2016-06-10

    Separation of diastereomers of dl-α-tocopherol was studied by reversed-phase liquid chromatography using three types of stationary phases, polymeric ODS, polymeric C30, and monomeric ODS. Polymeric ODS stationary phase (Inertsil ODS-P, 3mmID, 20cm) was effective for the separation of the isomers created by the presence of three chiral centers on the alkyl chain of synthetic dl-α-tocopherol. Considerable improvement of the separation of isomers was observed on ODS-P phase at high pressure and at low temperature. Complete separation of four pairs of diastereomers was achieved at 12.0°C, 536bar, while three peaks were observed when the separation was carried out either at 12.0°C at low pressure or at 20°C at 488bar. Higher temperature (30.0°C) with the ODS-P phase resulted in only partial separation of the diastereomers even at high pressure. Only slight resolution was observed for the mixture of diastereomers with the C30 stationary phase (Inertsil C30) at 12.0°C and 441bar, although the stationary phase afforded greater resolution for β- and γ-tocopherol than ODS-P. A monomeric C18 stationary phase did not show any separation at 12.0°C and 463bar. The results suggest that the binding site of the polymeric ODS-P phase is selective for flexible alkyl chains that provided the longest retention for the natural form, (R,R,R) form, and the enantiomer, (S,S,S) form, of dl-α-tocopherol. Copyright © 2016. Published by Elsevier B.V.

  17. Normal-phase liquid chromatography retention behavior of polycyclic aromatic hydrocarbon and their methyl-substituted derivatives on an aminopropyl stationary phase.

    Science.gov (United States)

    Wilson, Walter B; Hayes, Hugh V; Sander, Lane C; Campiglia, Andres D; Wise, Stephen A

    2017-09-01

    Retention indices for 124 polycyclic aromatic hydrocarbons (PAHs) and 62 methyl-substituted (Me-) PAHs were determined using normal-phase liquid chromatography (NPLC) on a aminopropyl (NH 2 ) stationary phase. PAH retention behavior on the NH 2 phase is correlated to the total number of aromatic carbons in the PAH structure. Within an isomer group, non-planar isomers generally elute earlier than planar isomers. MePAHs generally elute slightly later but in the same region as the parent PAHs. Correlations between PAH retention behavior on the NH 2 phase and PAH thickness (T) values were investigated to determine the influence of non-planarity for isomeric PAHs with four to seven aromatic rings. Correlation coefficients ranged from r = 0.19 (five-ring peri-condensed molecular mass (MM) 252 Da) to r = -0.99 (five-ring cata-condensed MM 278 Da). In the case of the smaller PAHs (MM ≤ 252 Da), most of the PAHs had a planar structure and provided a low correlation. In the case of larger PAHs (MM ≥ 278 Da), nonplanarity had a significant influence on the retention behavior and good correlation between retention and T was obtained for the MM 278 Da, MM 302 Da, MM 328 Da, and MM 378 Da isomer sets. Graphical abstract NPLC separation of the three-, four-, five-, and six-ring PAH isomers with different number of aromatic carbon atoms and degrees of non-planarity (Thickness, T). The inserted figure plots the number of aromatic carbon atoms vs. the log I value for the 124 parent PAHs.

  18. Deteriorated stress response in stationary-phase yeast: Sir2 and Yap1 are essential for Hsf1 activation by heat shock and oxidative stress, respectively.

    Directory of Open Access Journals (Sweden)

    Inbal Nussbaum

    Full Text Available Stationary-phase cultures have been used as an important model of aging, a complex process involving multiple pathways and signaling networks. However, the molecular processes underlying stress response of non-dividing cells are poorly understood, although deteriorated stress response is one of the hallmarks of aging. The budding yeast Saccharomyces cerevisiae is a valuable model organism to study the genetics of aging, because yeast ages within days and are amenable to genetic manipulations. As a unicellular organism, yeast has evolved robust systems to respond to environmental challenges. This response is orchestrated largely by the conserved transcription factor Hsf1, which in S. cerevisiae regulates expression of multiple genes in response to diverse stresses. Here we demonstrate that Hsf1 response to heat shock and oxidative stress deteriorates during yeast transition from exponential growth to stationary-phase, whereas Hsf1 activation by glucose starvation is maintained. Overexpressing Hsf1 does not significantly improve heat shock response, indicating that Hsf1 dwindling is not the major cause for Hsf1 attenuated response in stationary-phase yeast. Rather, factors that participate in Hsf1 activation appear to be compromised. We uncover two factors, Yap1 and Sir2, which discretely function in Hsf1 activation by oxidative stress and heat shock. In Δyap1 mutant, Hsf1 does not respond to oxidative stress, while in Δsir2 mutant, Hsf1 does not respond to heat shock. Moreover, excess Sir2 mimics the heat shock response. This role of the NAD+-dependent Sir2 is supported by our finding that supplementing NAD+ precursors improves Hsf1 heat shock response in stationary-phase yeast, especially when combined with expression of excess Sir2. Finally, the combination of excess Hsf1, excess Sir2 and NAD+ precursors rejuvenates the heat shock response.

  19. Fases estacionárias quirais para cromatografia líquida de alta eficiência Chiral stationary phases for high-performance liquid chromatography

    OpenAIRE

    Tiago de Campos Lourenço; Neila Maria Cassiano; Quezia B. Cass

    2010-01-01

    The development of Chiral Stationary Phases (CSPs) for high performance liquid chromatography has been studied by various researches around the world, especially, since 1980. This simple interest has been transformed into a tool of great technological value for the industrial community and scholars in general providing the existence of several CSPs, which act through different mechanisms of chiral discrimination. This paper describes the main types of CSPs that are used for the resolution of ...

  20. Deteriorated stress response in stationary-phase yeast: Sir2 and Yap1 are essential for Hsf1 activation by heat shock and oxidative stress, respectively.

    Science.gov (United States)

    Nussbaum, Inbal; Weindling, Esther; Jubran, Ritta; Cohen, Aviv; Bar-Nun, Shoshana

    2014-01-01

    Stationary-phase cultures have been used as an important model of aging, a complex process involving multiple pathways and signaling networks. However, the molecular processes underlying stress response of non-dividing cells are poorly understood, although deteriorated stress response is one of the hallmarks of aging. The budding yeast Saccharomyces cerevisiae is a valuable model organism to study the genetics of aging, because yeast ages within days and are amenable to genetic manipulations. As a unicellular organism, yeast has evolved robust systems to respond to environmental challenges. This response is orchestrated largely by the conserved transcription factor Hsf1, which in S. cerevisiae regulates expression of multiple genes in response to diverse stresses. Here we demonstrate that Hsf1 response to heat shock and oxidative stress deteriorates during yeast transition from exponential growth to stationary-phase, whereas Hsf1 activation by glucose starvation is maintained. Overexpressing Hsf1 does not significantly improve heat shock response, indicating that Hsf1 dwindling is not the major cause for Hsf1 attenuated response in stationary-phase yeast. Rather, factors that participate in Hsf1 activation appear to be compromised. We uncover two factors, Yap1 and Sir2, which discretely function in Hsf1 activation by oxidative stress and heat shock. In Δyap1 mutant, Hsf1 does not respond to oxidative stress, while in Δsir2 mutant, Hsf1 does not respond to heat shock. Moreover, excess Sir2 mimics the heat shock response. This role of the NAD+-dependent Sir2 is supported by our finding that supplementing NAD+ precursors improves Hsf1 heat shock response in stationary-phase yeast, especially when combined with expression of excess Sir2. Finally, the combination of excess Hsf1, excess Sir2 and NAD+ precursors rejuvenates the heat shock response.

  1. Azithromycin blocks quorum sensing and alginate polymer formation and increases the sensitivity to serum and stationary growth phase killing of P. aeruginosa and attenuates chronic P. aeruginosa lung infection in Cftr -/--mice

    DEFF Research Database (Denmark)

    Hoffmann, N.; Lee, Bao le ri; Hentzer, Morten

    2007-01-01

    The consequences of O-acetylated alginate-producing Pseudomonas aeruginosa biofilms in the lungs of chronically infected cystic fibrosis (CF) patients are tolerance to both antibiotic treatments and effects on the innate and the adaptive defense mechanisms. In clinical trials, azithromycin (AZM...... and the complement system. Moreover, we show that AZM may affect the polymerization of P. aeruginosa alginate by the incomplete precipitation of polymerized alginate and high levels of readily dialyzable uronic acids. In addition, we find that mucoid bacteria in the stationary growth phase became sensitive to AZM......, whereas cells in the exponential phase did not. Interestingly, AZM-treated P. aeruginosa lasI mutants appeared to be particularly resistant to serum, whereas bacteria with a functional QS system did not. We show in a CF mouse model of chronic P. aeruginosa lung infection that AZM treatment results...

  2. High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010 on cellulose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Ying Zhou

    2012-02-01

    Full Text Available The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ by high performance liquid chromatographic (HPLC methods, which included ibuprofen (C1, ketoprofen (C2, nitrendipine (C3, nimodipine (C4, felodipine (C5, omeprazole (C6, praziquantel (C7, propranolol hydrochloride (C8, atenolol (C9, sulpiride (C10, clenbuterol hydrochloride (C11, verapamil hydrochloride (C12, and chlorphenamine maleate (C13. The mobile phase consisted of isopropanol and n-hexane. The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min. The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied, while the effects of proportion of organic additives, alcohol displacer and temperature on the separation were studied. And the mechanism of some of racemates was discussed. The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When concentration of organic alkaline modifier was 0.2% (v/v, the resolution and the peak shape were fairly good. Most racemates mentioned above had better resolution at column temperature of 25 °C. When racemates were separated, the temperature should be kept so as to obtain stable separation results. Keywords: HPLC, Chiral stationary phase, Optical enantiomers, Cellulose ramification

  3. Comparison of Various Types of Stationary Phases in Non-Aqueous Reversed-Phase High-Performance Liquid Chromatography–Mass Spectrometry of Glycerolipids in Blackcurrant Oil and Its Enzymatic Hydrolysis Mixture

    Czech Academy of Sciences Publication Activity Database

    Lísa, M.; Holčapek, M.; Sovová, Helena

    2009-01-01

    Roč. 1216, č. 47 (2009), s. 8371-8378 ISSN 0021-9673 Institutional research plan: CEZ:AV0Z40720504 Keywords : ultra high-performance liquid chromatography * C30 stationary phase * triacylglycerols Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.101, year: 2009

  4. Application of a cholesterol stationary phase in the analysis of phosphorothioate oligonucleotides by means of ion pair chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Studzińska, Sylwia; Krzemińska, Katarzyna; Szumski, Michał; Buszewski, Bogusław

    2016-07-01

    The main aim of this study was the investigation of the influence of several ion pair reagents towards both the retention and the mass spectrometry sensitivity of phosphorothioate oligonucleotides. A cholesterol stationary phase was applied for the first time in the analysis of this group of compounds. The mobile phase composition was modified by changing the concentration and the type of amines and acetates or 1,1,1,3,3,3-hexafluoroisopropanol. It has been shown that the increase of amines concentration results in the retention factor increase for each oligonucleotide, on each adsorbent. The only exception was the mobile phase composed of triethylamine and 1,1,1,3,3,3-hexafluoroisopropanol. This is a consequence of interactions taking place between a cholesterol molecule and an alcohol. This effect was convenient when the mass spectrometry detection was applied, since it allowed an increase in the sensitivity. Moreover, optimization of the mobile phase composition and its impact on the efficiency of ionization process and on the sensitivity in mass spectrometry were also presented. The optimization of this new method, based on cholesterol stationary phase coupled with mass spectrometry detection, was finally applied for the determination of phosphorothioate oligonucleotides impurity in a real sample. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Solvation molar enthalpies and heat capacities of n-alkanes and n-alkylbenzenes on stationary phases of wide-ranging polarity.

    Science.gov (United States)

    Lebrón-Aguilar, Rosa; Quintanilla-López, Jesús Eduardo; Santiuste, José María

    2010-12-03

    A comparison of the most usual gas chromatographic methods for the calculation of partial molar enthalpies of solvation (Δ(sol)H(o)) has been carried out. Those methods based on the fitting of lnV(g) or ln(k/T) vs. 1/T and ln(k/T) vs. (1/T and the temperature arrangement, T(a)) are the most adequate ones for obtaining Δ(sol)H(o) values. However, the latter is the only reliable option for Δ(sol)H(o) estimation when commercial WCOT capillary columns are used, since in this case the estimation of some variables involved in the V(g) determination is less accurate or even impossible. Consequently, in this paper, Δ(sol)H(o) obtained from ln(k/T) vs. (1/T+T(a)) fitting at 373.15 and 298.15K for n-alkanes and n-alkylbenzenes on 12 commercial capillary columns coated with stationary phases covering the 203-3608 McReynolds polarity range are reported. Moreover, molar heat capacities of solvation at constant pressure (Δ(sol)C(p)(o)) have also been calculated using this method. A clear influence on Δ(sol)H(o) of the type and content of the substitution group in the stationary phase was observed. In addition, a linear relationship of Δ(sol)C(p)(o) with the van der Waals volume of the n-alkanes and the temperature gradient of density of the stationary phase was found. The effect of the size of the hydrocarbon on both thermodynamic variables was also investigated. Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Attempted - to -Phase Conversion of Croconic Acid via Ball Milling

    Science.gov (United States)

    2017-05-18

    ARL-TN-0824 MAY 2017 US Army Research Laboratory Attempted α- to β-Phase Conversion of Croconic Acid via Ball Milling by...Laboratory Attempted α- to β-Phase Conversion of Croconic Acid via Ball Milling by Steven W Dean, Rose A Pesce-Rodriguez, and Jennifer A Ciezak...

  7. Theory and applications of a novel ion exchange chromatographic technology using controlled pH gradients for separating proteins on anionic and cationic stationary phases.

    Science.gov (United States)

    Tsonev, Latchezar I; Hirsh, Allen G

    2008-07-25

    pISep is a major new advance in low ionic strength ion exchange chromatography. It enables the formation of externally controlled pH gradients over the very broad pH range from 2 to 12. The gradients can be generated on either cationic or anionic exchangers over arbitrary pH ranges wherein the stationary phases remain totally charged. Associated pISep software makes possible the calculation of either linear, nonlinear or combined, multi-step, multi-slope pH gradients. These highly reproducible pH gradients, while separating proteins and glycoproteins in the order of their electrophoretic pIs, provide superior chromatographic resolution compared to salt. This paper also presents a statistical mechanical model for protein binding to ion exchange stationary phases enhancing the electrostatic interaction theory for the general dependence of retention factor k, on both salt and pH simultaneously. It is shown that the retention factors computed from short time isocratic salt elution data of a model protein can be used to accurately predict its salt elution concentration in varying slope salt elution gradients formed at varying isocratic pH as well as the pH at which it will be eluted from an anionic exchange column by a pISep pH gradient in the absence of salt.

  8. Fragment-based approach to calculate hydrophobicity of anionic and nonionic surfactants derived from chromatographic retention on a C18 stationary phase.

    Science.gov (United States)

    Hammer, Jort; Haftka, Joris J-H; Scherpenisse, Peter; Hermens, Joop L M; de Voogt, Pim W P

    2017-02-01

    To predict the fate and potential effects of organic contaminants, information about their hydrophobicity is required. However, common parameters to describe the hydrophobicity of organic compounds (e.g., octanol-water partition constant [K OW ]) proved to be inadequate for ionic and nonionic surfactants because of their surface-active properties. As an alternative approach to determine their hydrophobicity, the aim of the present study was therefore to measure the retention of a wide range of surfactants on a C 18 stationary phase. Capacity factors in pure water (k' 0 ) increased linearly with increasing number of carbon atoms in the surfactant structure. Fragment contribution values were determined for each structural unit with multilinear regression, and the results were consistent with the expected influence of these fragments on the hydrophobicity of surfactants. Capacity factors of reference compounds and log K OW values from the literature were used to estimate log K OW values for surfactants (log KOWHPLC). These log KOWHPLC values were also compared to log K OW values calculated with 4 computational programs: KOWWIN, Marvin calculator, SPARC, and COSMOThermX. In conclusion, capacity factors from a C 18 stationary phase are found to better reflect hydrophobicity of surfactants than their K OW values. Environ Toxicol Chem 2017;36:329-336. © 2016 The Authors. Environmental Toxicology and Chemistry Published by Wiley Periodicals, Inc. on behalf of SETAC. © 2016 The Authors. Environmental Toxicology and Chemistry Published by Wiley Periodicals, Inc. on behalf of SETAC.

  9. The use of Stationary Phase Optimized Selectivity Liquid Chromatography for the development of herbal fingerprints to detect targeted plants in plant food supplements.

    Science.gov (United States)

    Deconinck, E; Djiogo, C A Sokeng; Kamugisha, A; Courselle, P

    2017-08-01

    The consumption of plant food supplements is increasing steadily and more and more, these products are bought through internet. Often the products sold through internet are not registered or declared with a national authority, meaning that no or minimal quality control is performed and that they could contain herbs or plants that are regulated. Stationary Phase Optimized Selectivity Liquid Chromatography (SOS-LC) was evaluated for the development of specific fingerprints, to be used for the detection of targeted plants in plant food supplements. Three commonly used plants in plant food supplements and two regulated plants were used to develop fingerprints with SOS-LC. It was shown that for all plants specific fingerprints could be obtained, allowing the detection of these targeted plants in triturations with different herbal matrices as well as in real samples of suspicious supplements seized by the authorities. For three of the five plants a more specific fingerprint was obtained, compared to the ones developed on traditional columns described in literature. It could therefore be concluded that the combination of segments of different types of stationary phases, as used in SOS-LC, has the potential of becoming a valuable tool in the quality control and the identification of crude herbal or plant material and in the detection of regulated plants in plant food supplements or other herbal preparations. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Enantioseparation of angiotensin II receptor type 1 blockers: evaluation of 6-substituted carbamoyl benzimidazoles on immobilized polysaccharide-based chiral stationary phases. Unusual temperature behavior.

    Science.gov (United States)

    Su, Ran; Hou, Zhun; Sang, Lihong; Zhou, Zhi-Ming; Fang, Hao; Yang, Xinying

    2017-09-15

    Enantioseparation of thirteen 6-substituted carbamoyl benzimidazoles by high-performance liquid chromatography (HPLC) was investigated using two immobilized polysaccharide-based chiral stationary phases (CSPs), Chiralpak IC and Chiralpak IA, in normal-phase mode. Most of the examined compounds were completely resolved. The effects of a polar alcohol modifier, analyte structure, and column temperature on the chiral recognition were investigated. Furthermore, the structure-retention relationship was evaluated, and thermodynamic parameters were calculated from plots of ln k' or ln α versus 1/T. The thermodynamic parameters indicated that the separations were enthalpy-driven. Moreover, nonlinear van't Hoff plots were obtained on Chiralpak IA. However, two unusual phenomena were observed: (1) an unusual increase in retention with increasing temperature with linear van't Hoff plots on Chiralpak IC and (2) an extremely high T iso value (i.e., several thousand degrees centigrade). Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

    Science.gov (United States)

    Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

    2018-01-26

    The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Comparison of the peak resolution and the stationary phase retention between the satellite and the planetary motions using the coil satellite centrifuge with counter-current chromatographic separation of 4-methylumbelliferyl sugar derivatives.

    Science.gov (United States)

    Shinomiya, Kazufusa; Zaima, Kazumasa; Harada, Yukina; Yasue, Miho; Harikai, Naoki; Tokura, Koji; Ito, Yoichiro

    2017-01-20

    Coil satellite centrifuge (CSC) produces the complex satellite motion consisting of the triplicate rotation of the coiled column around three axes including the sun axis (the angular velocity, ω 1 ), the planet axis (ω 2 ) and the satellite axis (the central axis of the column) (ω 3 ) according to the following formula: ω 1 =ω 2 +ω 3 . Improved peak resolution in the separation of 4-methylumbelliferyl sugar derivatives was achieved using the conventional multilayer coiled columns with ethyl acetate/1-butanol/water (3: 2: 5, v/v) for the lower mobile phase at the combination of the rotation speeds (ω 1 , ω 2 , ω 3 )=(300, 150, 150rpm), and (1:4:5, v/v) for the upper mobile phase at (300:100:200rpm). The effect of the satellite motion on the peak resolution and the stationary phase retention was evaluated by each CSC separation with the different rotation speeds of ω 2 and ω 3 under the constant revolution speed at ω 1 =300rpm. With the lower mobile phase, almost constant peak resolution and stationary phase retention were yielded regardless of the change of ω 2 and ω 3 , while with the upper mobile phase these two values were sensitively varied according to the different combination of ω 2 and ω 3 . For example, when ω 2 =147 or 200rpm is used, no stationary phase was retained in the coiled column while ω 2 =150rpm could retain enough volume of stationary phase for separation. On the other hand, the combined rotation speeds at (ω 1 , ω 2 , ω 3 )=(300, 300, 0rpm) or (300, 0, 300rpm) produced insufficient peak resolution regardless of the choice of the mobile phase apparently due to the lack of rotation speed except at (300, 0, 300rpm) with the upper mobile phase. At lower rotation speed of ω 1 =300rpm, better peak resolution and stationary phase retention were obtained by the satellite motion (ω 3 ) than by the planetary motion (ω 2 ), or ω 3 >ω 2 . The effect of the hydrophobicity of the two-phase solvent systems on the stationary phase

  13. Ionic liquid phases with comprehensive two-dimensional gas chromatography of fatty acid methyl esters.

    Science.gov (United States)

    Pojjanapornpun, Siriluck; Nolvachai, Yada; Aryusuk, Kornkanok; Kulsing, Chadin; Krisnangkura, Kanit; Marriott, Philip J

    2018-02-17

    New generation inert ionic liquid (iIL) GC columns IL60i, IL76i and IL111i, comprising phosphonium or imidazolium cationic species, were investigated for separation of fatty acid methyl esters (FAME). In general, the iIL phases provide comparable retention times to their corresponding conventional columns, with only minor selectivity differences. The average tailing factors and peak widths were noticeably improved (reduced) for IL60i and IL76i, while they were slightly improved for IL111i. Inert IL phase columns were coupled with conventional IL columns in comprehensive two-dimensional GC (GC × GC) with a solid-state modulator which offers variable modulation temperature (T M ), programmable T M during analysis and trapping stationary phase material during the trap/release (modulation) process, independent of oven T and column sets. Although IL phases are classified as polar, relative polarity of the two phases comprising individual GC × GC column sets permits combination of less-polar IL/polar IL and polar IL/less-polar IL column sets; it was observed that a polar/less-polar column set provided better separation of FAME. A higher first dimension ( 1 D) phase polarity combined with a lower 2 D phase polarity, for instance 1 D IL111i with 2 D IL59 gave the best result; the greater difference in 1 D/ 2 D phase polarity results in increasing occupancy of peak area in the 2D space. The IL111i/IL59 column set was selected for analysis of fatty acids in fat and oil products (butter, margarine, fish oil and canola oil). Compared with the conventional IL111, IL111i showed reduced column bleed which makes this more suited to GC × GC analysis of FAME. The proposed method offers a fast profiling approach with good repeatability of analysis of FAME.

  14. The PaPsr1 and PaWhi2 genes are members of the regulatory network that connect stationary phase to mycelium differentiation and reproduction in Podospora anserina.

    Science.gov (United States)

    Timpano, Hélène; Chan Ho Tong, Laetitia; Gautier, Valérie; Lalucque, Hervé; Silar, Philippe

    2016-09-01

    In filamentous fungi, entrance into stationary phase is complex as it is accompanied by several differentiation and developmental processes, including the synthesis of pigments, aerial hyphae, anastomoses and sporophores. The regulatory networks that control these processes are still incompletely known. The analysis of the "Impaired in the development of Crippled Growth (IDC)" mutants of the model filamentous ascomycete Podospora anserina has already yielded important information regarding the pathway regulating entrance into stationary phase. Here, the genes affected in two additional IDC mutants are identified as orthologues of the Saccharomyces cerevisiae WHI2 and PSR1 genes, known to regulate stationary phase in this yeast, arguing for a conserved role of these proteins throughout the evolution of ascomycetes. Copyright © 2016 Elsevier Inc. All rights reserved.

  15. Synthesis and Evaluation of Molecularly Imprinted Polymeric Microspheres for Chloramphenicol by Aqueous Suspension Polymerization as a High Performance Liquid Chromatography Stationary Phase

    International Nuclear Information System (INIS)

    Zhang, Yan; Lei, Jiandu

    2013-01-01

    Molecularly imprinted microsphere for chloramphenicol (CAP) with high adsorption capacity and excellent selectivity is prepared by aqueous suspension polymerization, in which chloramphenicol is used as template molecule and ethyl acetate as porogen. The CAP-imprinted microspheres are used as high performance liquid chromatography (HPLC) stationary phase and packed into stainless steel column (150 mm Χ 4.6 mm i. d.) for selective separation of chloramphenicol. HPLC analysis suggests that chloramphenicol can be distinguished from not only its structural analogs but also other broad-spectrum antibiotic such as erythromycin and tetracycline. In addition, the binding experiments of CAP-imprinted microspheres are carried out in ethanol/water (1:4, V:V), the results indicate that the maximum apparent static binding capacity of molecularly imprinted microspheres is up to 66.64 mg g -1 according to scatchard model

  16. Determination of melatonin in wine and plant extracts by capillary electrochromatography with immobilized carboxylic multi-walled carbon nanotubes as stationary phase.

    Science.gov (United States)

    Stege, Patricia W; Sombra, Lorena L; Messina, Germán; Martinez, Luis D; Silva, María F

    2010-07-01

    The finding of melatonin, the often called "hormone of darkness" in plants opens an interesting perspective associated to the plethora of health benefits related to the moderate consumption of red wine. In this study, the implementation of a new method for the determination of melatonin in complex food matrices by CEC with immobilized carboxylic multi-walled carbon nanotubes as stationary phase is demonstrated. The results indicated high electrochromatographic resolution, good capillary efficiencies and improved sensitivity respect to those obtained with conventional capillaries. In addition, it was demonstrated highly reproducible results between runs, days and columns. The LOD for melatonin was 0.01 ng/mL. The method was successfully applied to the determination of melatonin in red and white wine, grape skin and plant extracts of Salvia officinalis L.

  17. Evaluation of the chiral recognition properties as well as the column performance of four chiral stationary phases based on cellulose (3,5-dimethylphenylcarbamate) by parallel HPLC and SFC.

    Science.gov (United States)

    Nelander, Hanna; Andersson, Shalini; Ohlén, Kristina

    2011-12-30

    The performance of four commercially available cellulose tris(3,5-dimethylphenylcarbamate) based chiral stationary phases (CSPs) was evaluated with parallel high performance liquid chromatography (HPLC) and super critical fluid chromatography (SFC). Retention, enantioselectivity, resolution and efficiency were compared for a set of neutral, basic and acidic compounds having different physico-chemical properties by using different mobile phase conditions. Although the chiral selector is the same in all the four CSPs, a large difference in the ability to retain and resolve enantiomers was observed under the same chromatographic conditions. We believe that this is mainly due to differences in the silica matrix and immobilization techniques used by the different vendors. An extended study of metoprolol and structure analogues gave a deeper understanding of the accessibility of the chiral discriminating interactions and its impact on the resolution of the racemic compounds on the four CSPs studied. Also, a clear difference in enantioselectivity is observed between SFC and LC mode, hydrogen bonding was found to play an important role in the differential binding of the enantiomers to the CSPs. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. A direct HPLC method for the resolution and quantitation of the R-(-)- and S-(+)-enantiomers of vigabatrin (gamma-vinyl-GABA) in pharmaceutical dosage forms using teicoplanin aglycone chiral stationary phase.

    Science.gov (United States)

    Al-Majed, Abdulrahman A

    2009-08-15

    A direct chiral high-performance liquid chromatography (HPLC) method was developed and validated for the resolution and quantification of antiepileptic drug enantiomers, R-(-)- and S-(+)-vigabatrin (gamma-vinyl-gamma-aminobutyric acid) in pharmaceutical products. The separation was optimized on a macrocyclic glycopeptide antibiotic chiral stationary phase (CSP) based on teicoplanin aglycone, chirobiotic (TAG), using a mobile phase system containing ethanol-water (80:20, v/v), at a flow rate of 0.4ml/min and UV detection set at 210nm. The stability of vigabatrin enantiomers under different degrees of temperature was also studied. The enantiomers of vigabatrin were separated from each other. The calibration curves were linear over a range of 100-1600microg/ml (r=0.999) for both enantiomers. The overall recoveries of R-(-)- and S-(+)-vigabatrin enantiomers from pharmaceutical products were in the range of 98.3-99.8% with %RSD ranged from 0.48 to 0.52%. The limit of quantification (LOQ) and limit of detection (LOD) for each enantiomer were 100 and 25microg/ml, respectively. No interferences were found from commonly co-formulated excipients.

  19. Extraterrestrial material analysis: loss of amino acids during liquid-phase acid hydrolysis

    Science.gov (United States)

    Buch, Arnaud; Brault, Amaury; Szopa, Cyril; Freissinet, Caroline

    2015-04-01

    Searching for building blocks of life in extraterrestrial material is a way to learn more about how life could have appeared on Earth. With this aim, liquid-phase acid hydrolysis has been used, since at least 1970 , in order to extract amino acids and other organic molecules from extraterrestrial materials (e.g. meteorites, lunar fines) or Earth analogues (e.g. Atacama desert soil). This procedure involves drastic conditions such as heating samples in 6N HCl for 24 h, either under inert atmosphere/vacuum, or air. Analysis of the hydrolyzed part of the sample should give its total (free plus bound) amino acid content. The present work deals with the influence of the 6N HCl hydrolysis on amino acid degradation. Our experiments have been performed on a standard solution of 17 amino acids. After liquid-phase acid hydrolysis (6N HCl) under argon atmosphere (24 h at 100°C), the liquid phase was evaporated and the dry residue was derivatized with N-Methyl-N-(t-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) and dimethylformamide (DMF), followed by gas chromatography-mass spectrometry analysis. After comparison with derivatized amino acids from the standard solution, a significant reduction of the chromatographic peak areas was observed for most of the amino acids after liquid-phase acid hydrolysis. Furthermore, the same loss pattern was observed when the amino acids were exposed to cold 6N HCl for a short amount of time. The least affected amino acid, i.e. glycine, was found to be 73,93% percent less abundant compared to the non-hydrolyzed standard, while the most affected, i.e. histidine, was not found in the chromatograms after hydrolysis. Our experiments thereby indicate that liquid-phase acid hydrolysis, even under inert atmosphere, leads to a partial or total loss of all of the 17 amino acids present in the standard solution, and that a quick cold contact with 6N HCl is sufficient to lead to a loss of amino acids. Therefore, in the literature, the reported increase

  20. Novas fases estacionárias à base de sílica para cromatografia líquida de alta eficiência New stationary phases based on silica for high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    César R. Silva

    2004-04-01

    Full Text Available The present work reviews recent advances in the preparation of new reversed phase packing materials such as sterically protected, bidentate, hybrid organic-inorganic and monolithic phases and phases containing embedded polar groups. The bonding chemistry involved in the preparation of these phases as well as their advantages over conventional C8 and C18 reversed phases are discussed. Understanding the reasons behind the development of these newer column packings helps analysts select the best stationary phase for a given application.

  1. High-performance liquid chromatographic enantioseparation of 2-aminomono- and dihydroxycyclopentanecarboxylic and 2-aminodihydroxycyclohexanecarboxylic acids on macrocyclic glycopeptide-based phases.

    Science.gov (United States)

    Berkecz, Róbert; Ilisz, István; Benedek, Gabriella; Fülöp, Ferenc; Armstrong, Daniel W; Péter, Antal

    2009-02-06

    The direct separation of the enantiomers of four 2-aminomono- or dihydroxycyclopentanecarboxylic acids and four 2-aminodihydroxycyclohexanecarboxylic acids was performed on chiral stationary phases containing macrocyclic glycopeptide antibiotics such as teicoplanin (Astec Chirobiotic T and T2), teicoplanin aglycone (Chirobiotic TAG) or ristocetin A (Chirobiotic R) as chiral selectors. The effects of the nature of organic modifiers, the pH, the mobile phase composition and the structures of the analytes on the separation were investigated. Chirobiotic TAG, and in some cases Chirobiotic T, proved to be the most useful of these columns. The elution sequence was determined in most cases.

  2. A 2H nuclear magnetic resonance study of the state of water in neat silica and zwitterionic stationary phases and its influence on the chromatographic retention characteristics in hydrophilic interaction high-performance liquid chromatography.

    Science.gov (United States)

    Wikberg, Erika; Sparrman, Tobias; Viklund, Camilla; Jonsson, Tobias; Irgum, Knut

    2011-09-23

    2H NMR has been used as a tool for probing the state of water in hydrophilic stationary phases for liquid chromatography at temperatures between -80 and +4 °C. The fraction of water that remained unfrozen in four different neat silicas with nominal pore sizes between 60 and 300 Å, and in silicas with polymeric sulfobetaine zwitterionic functionalities prepared in different ways, could be determined by measurements of the line widths and temperature-corrected integrals of the 2H signals. The phase transitions detected during thawing made it possible to estimate the amount of non-freezable water in each phase. A distinct difference was seen between the neat and modified silicas tested. For the neat silicas, the relationship between the freezing point depression and their pore size followed the expected Gibbs-Thomson relationship. The polymeric stationary phases were found to contain considerably higher amounts of non-freezable water compared to the neat silica, which is attributed to the structural effect that the sulfobetaine polymers have on the water layer close to the stationary phase surface. The sulfobetaine stationary phases were used alongside the 100 Å silica to separate a number of polar compounds in hydrophilic interaction (HILIC) mode, and the retention characteristics could be explained in terms of the surface water structure, as well as by the porous properties of the stationary phases. This provides solid evidence supporting a partitioning mechanism, or at least of the existence of an immobilized layer of water into which partitioning could be occurring. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Modeling, analysis, and design of stationary reference frame droop controlled parallel three-phase voltage source inverters

    DEFF Research Database (Denmark)

    Vasquez, Juan Carlos; Guerrero, Josep M.; Savaghebi, Mehdi

    2013-01-01

    Power electronics based MicroGrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of parallel connected three-phase VSIs are derived. The proposed voltage and current inner control loops and the mat......Power electronics based MicroGrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of parallel connected three-phase VSIs are derived. The proposed voltage and current inner control loops...... control restores the frequency and amplitude deviations produced by the primary control. Also, a synchronization algorithm is presented in order to connect the MicroGrid to the grid. Experimental results are provided to validate the performance and robustness of the parallel VSI system control...

  4. Two-phase air-solid stationary turbulent flow in a cylindrical tube, with a high massive concentration

    International Nuclear Information System (INIS)

    Fortier, Andre; Chen, Che Pen

    1976-01-01

    The momentum theorem, applied separately to the two phases (fluid and solid particles), together with the equations of continuity, gives two differential equations by which the pressure and the concentration along the longitudinal profile x can be computed. These equations can be obtained by introduction of several averaging procedures of physical significance. These quantities are defined in a simple manner for the general case. Using experimental measurements of solid particle velocities in a horizontal tube by radio-tracers, it is shown how to determine the three average coefficients: Λsub(g) friction coefficient of gas, Λsub(s) momentum loss coefficient of solid particles by impacts, against the wall, and Csub(D) drag coefficient due to the velocity difference between the two phases. This determination is based on the numerical solution of the two differential equations conveniently simplified [fr

  5. Thin Layer Chromatographic Resolution of Some β-adrenolytics and a β2-Agonist Using Bovine Serum Albumin as Chiral Additive in Stationary Phase.

    Science.gov (United States)

    Malik, Poonam; Bhushan, Ravi

    2018-01-01

    Direct enantiomeric resolution of commonly used five racemic β-adrenolytics, namely, bisoprolol, atenolol, propranolol, salbutamol and carvedilol has been achieved by thin layer chromatography using bovine serum albumin (BSA) as chiral additive in stationary phase. Successful resolution of the enantiomers of all racemic β-adrenolytics was achieved by use of different composition of simple organic solvents having no buffer or inorganic ions. The effect of variation in pH, temperature, amount of BSA as the additive, and composition of mobile phase on resolution was systematically studied. Spots were visualized in iodine vapors. Native enantiomers for each of the five analytes were isolated and identified and their elution order was determined. The limit of detection was found to be 0.7, 1.2, 0.84, 1.6 and 0.9 μg (per spot) for each enantiomer of bisoprolol, atenolol, propranolol, salbutamol and carvedilol, respectively. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Supercritical fluid chromatography versus high performance liquid chromatography for enantiomeric and diastereoisomeric separations on coated polysaccharides-based stationary phases: Application to dihydropyridone derivatives.

    Science.gov (United States)

    Hoguet, Vanessa; Charton, Julie; Hecquet, Paul-Emile; Lakhmi, Chahinaze; Lipka, Emmanuelle

    2018-05-11

    For analytical applications, SFC has always remained in the shadow of LC. Analytical enantioseparation of eight dihydropyridone derivatives, was run in both High Performance Liquid Chromatography and Supercritical Fluid Chromatography. Four polysaccharide based chiral stationary phases namely amylose and cellulose tris(3, 5-dimethylphenylcarbamate), amylose tris((S)-α-phenylethylcarbamate) and cellulose tris(4-methylbenzoate) with four mobile phases consisted of either n-hexane/ethanol or propan-2-ol (80:20 v:v) or carbon dioxide/ethanol or propan-2-ol (80:20 v:v) mixtures were investigated under same operatory conditions (temperature and flow-rate). The elution strength, enantioselectivity and resolution were compared in the two methodologies. For these compounds, for most of the conditions, HPLC afforded shorter retention times and a higher resolution than SFC. HPLC appears particularly suitable for the separation of the compounds bearing two chiral centers. For instance compound 7 was baseline resolved on OD-H CSP under n-Hex/EtOH 80/20, with resolution values equal to 2.98, 1.55, 4.52, between the four stereoisomers in less than 17 min, whereas in SFC, this latter is not fully separated in 23 min under similar eluting conditions. After analytical screenings, the best conditions were transposed to semi-preparative scale. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. Modeling, analysis, and design of stationary reference frame droop controlled parallel three-phase voltage source inverters

    DEFF Research Database (Denmark)

    Vasquez, Juan Carlos; Guerrero, Josep M.; Savaghebi, Mehdi

    2011-01-01

    and discussed. Experimental results are provided to validate the performance and robustness of the VSIs functionality during Islanded and grid-connected operations, allowing a seamless transition between these modes through control hierarchies by regulating frequency and voltage, main-grid interactivity......Power electronics based microgrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of three-phase VSIs are derived. The proposed voltage and current inner control loops and the mathematical models...

  8. Correlations between retention indices and molecular structure of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    Pias, J.B.; Gasco, L.

    1976-01-01

    The retention indices of aliphaticalcohols of carbon number up to Csub(g), and of their benzoyl derivatives up to C 7 , were determined in columns packed with Chromosorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, OV-3, OV-7; OV-11, OV-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1, on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 0 C. In alcohols, a -CH 2 - group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices ΔI, and positional and structural increments of I were evaluated for -OH and benzoyl groups in terms for phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (author)

  9. Phase behavior of (CO2 + methanol + lauric acid) system

    International Nuclear Information System (INIS)

    Ferreira, Franciele M.; Ramos, Luiz P.; Ndiaye, Papa M.; Corazza, Marcos L.

    2011-01-01

    Highlights: → We measured SVL, LLE and VLE for the binary system {lauric acid + methanol + CO 2 }. → Bubble point and dew point were measured at high pressures. → The experimental data were modeled using the Peng-Robinson equation of state with the classical van der Waals mixing rule. - Abstract: In this study the phase equilibrium behaviors of the binary system (CO 2 + lauric acid) and the ternary system (CO 2 + methanol + lauric acid) were determined. The static synthetic method, using a variable-volume view cell, was employed to obtain the experimental data in the temperature range of (293 to 343) K and pressures up to 24 MPa. The mole fractions of carbon dioxide were varied according to the systems as follows: (0.7524 to 0.9955) for the binary system (CO 2 + lauric acid); (0.4616 to 0.9895) for the ternary system (CO 2 + methanol + lauric acid) with a methanol to lauric acid molar ratio of (2:1); and (0.3414 to 0.9182) for the system (CO 2 + methanol + lauric acid) with a methanol to lauric acid molar ratio of (6:1). For these systems (vapor + liquid), (liquid + liquid), (vapor + liquid + liquid), and (solid + fluid) transitions were observed. The phase equilibrium data obtained for the systems were modeled using the Peng-Robinson equation of state with the classical van der Waals mixing rule with a satisfactory correlation between experimental and calculated values.

  10. High-performance liquid chromatographic enantioseparation of monoterpene-based 2-amino carboxylic acids on macrocyclic glycopeptide-based phases.

    Science.gov (United States)

    Sipos, László; Ilisz, István; Pataj, Zoltán; Szakonyi, Zsolt; Fülöp, Ferenc; Armstrong, Daniel W; Péter, Antal

    2010-10-29

    The enantiomers of five monoterpene-based 2-amino carboxylic acids were directly separated on chiral stationary phases containing macrocyclic glycopeptide antibiotics such as teicoplanin (Astec Chirobiotic T and T2) and teicoplanin aglycone (Chirobiotic TAG) as chiral selectors. The effects of pH, the mobile phase composition, the structure of the analyte and temperature on the separations were investigated. Experiments were performed at constant mobile phase compositions in the temperature range 10-40°C to study the effects of temperature and thermodynamic parameters on separations. Apparent thermodynamic parameters and T(iso) values were calculated from plots of ln k or ln α versus 1/T. Some mechanistic aspects of the chiral recognition process are discussed with respect to the structures of the analytes. It was found that the enantioseparations were in most cases enthalpy driven. The sequence of elution of the enantiomers was determined in all cases. Copyright © 2010 Elsevier B.V. All rights reserved.

  11. Microencapsulated acids associated with essential oils and acid salts for piglets in the nursery phase

    Directory of Open Access Journals (Sweden)

    Marco Aurelio Callegari

    2016-08-01

    Full Text Available The objective of this study was to evaluate the use of commercial blends of organic and inorganic acids combined with essential oils for piglets in the nursery phase. The formulations were administered as microcapsules or as acid salts. Ninety-six, Pen Ar Lan, barrow and female piglets, weaned at a body weight of 600 kg ± 12 kg and age of 23 days were subjected to four treatments. The animals were distributed in randomized blocks of three animals per pen and 8 replicates per treatment. The treatments consisted of four different diets: control (free of organic acids; acid and essential oil blends (fumaric acid 10,5%, malic acid 8.0%, essential oils; in microencapsulated form; microencapsulated acid blend (phosphoric acid 10%, citric acid 10%, malic acid 10%, fumaric acid 20%; in microencapsulated form; and acid salt blend (formic acid 40.5%, phosphoric acid 13.6%, propionic acid 4.9% and salts (23.2% calcium and 4.4% phosphorus available. The performance parameters, digestive transit time, weights of organs of the digestive tract, bacterial count of feces (Lactobacillus, E coli and Salmonella ssp and Clostridium, pH of the stomach and duodenal content did not differ between treatment groups (P > 005. All treatments containing organic acids exhibited positive effects on diarrhea control (P < 005. The cecal contents of volatile fatty acids (VFA were higher in piglets fed diets containing acids than in animals that received the control diet (P < 005, and blends containing essential oils improved the jejunum villus height compared with the control group. The use of diets containing acids improved diarrhea control and VFA production in the cecum, and specifically the diets containing microencapsulated acid blends required the lowest doses to be effective.

  12. Aqueous-Phase Acetic Acid Ketonization over Monoclinic Zirconia

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Qiuxia [Institute for Integrated Catalysis, Pacific Northwest; College; Lopez-Ruiz, Juan A. [Institute for Integrated Catalysis, Pacific Northwest; Cooper, Alan R. [Institute for Integrated Catalysis, Pacific Northwest; Wang, Jian-guo [College; Albrecht, Karl O. [Institute for Integrated Catalysis, Pacific Northwest; Mei, Donghai [Institute for Integrated Catalysis, Pacific Northwest

    2017-12-13

    The effect of aqueous phase on the acetic acid ketonization over monoclinic zirconia has been investigated using first-principles based density functional theory (DFT) calculations. To capture the aqueous phase chemistry over the solid zirconia catalyst surface, the aqueous phase is represented by 111 explicit water molecules with a liquid water density of 0.93 g/cm3 and the monoclinic zirconia is modeled by the most stable surface structure . The dynamic nature of aqueous phase/ interface was studied using ab initio molecular dynamics simulation, indicating that nearly half of the surface Zr sites are occupied by either adsorbed water molecules or hydroxyl groups at 550 K. DFT calculations show that the adsorption process of acetic acid from the liquid water phase to the surface is nearly thermodynamically neutral with a Gibbs free energy of -2.3 kJ/mol although the adsorption strength of acetic acid on the surface in aqueous phase is much stronger than in vapor phase. Therefore it is expected that the adsorption of acetic acid will dramatically affects aqueous phase ketonization reactivity over the monoclinic zirconia catalyst. Using the same ketonization mechanism via the β-keto acid intermediate, we have compared acetic acid ketonization to acetone in both vapor and aqueous phases. Our DFT calculation results show although the rate-determining step of the β-keto acid formation via the C-C coupling is not pronouncedly affected, the presence of liquid water molecules will dramatically affect dehydrogenation and hydrogenation steps via proton transfer mechanism. This work was financially supported by the United States Department of Energy (DOE)’s Bioenergy Technologies Office (BETO) and performed at the Pacific Northwest National Laboratory (PNNL). PNNL is a multi-program national laboratory operated for DOE by Battelle Memorial Institute. Computing time and advanced catalyst characterization use was granted by a user proposal at the William R. Wiley

  13. The stationary phase sigma factor, RpoS, regulates the production of a carbapenem antibiotic, a bioactive prodigiosin and virulence in the enterobacterial pathogen Serratia sp. ATCC 39006.

    Science.gov (United States)

    Wilf, Nabil M; Salmond, George P C

    2012-03-01

    Serratia sp. ATCC 39006 (S39006) is a Gram-negative bacterium that is virulent in plant (potato) and invertebrate animal (Caenorhabditis elegans) models. It produces two secondary metabolite antibiotics, a prodigiosin and a carbapenem, and the exoenzymes pectate lyase and cellulase. We showed previously that deletion of the RNA chaperone Hfq abolished antibiotic production and attenuated virulence in both animal and plant hosts. Hfq and dependent small RNAs (sRNAs) are known to regulate the post-transcriptional expression of rpoS, which encodes σ(S), the stationary phase sigma factor subunit of RNA polymerase. An S39006 hfq deletion mutant showed decreased transcript levels of rpoS. Therefore, in this study we investigated whether the phenotypes regulated by Hfq were mediated through its control of rpoS. Whereas loss of Hfq abolished prodigiosin and carbapenem production and attenuated virulence in both C. elegans and potato, characterization of an S39006 rpoS mutant showed unexpectedly elevated prodigiosin and carbapenem production. Furthermore, the rpoS mutant exhibited attenuated animal pathogenesis, but not plant pathogenesis. Additionally, a homologue of the Hfq-dependent sRNA, RprA, was identified and shown to regulate prodigiosin production in a manner consistent with its role in positively regulating translation of rpoS mRNA. Combined, these results demonstrate that Hfq regulation of secondary metabolism and plant pathogenesis is independent of RpoS and establishes RpoS and RprA as regulators of antibiotic production.

  14. Comparison of high-accuracy numerical simulations of black-hole binaries with stationary-phase post-Newtonian template waveforms for initial and advanced LIGO

    International Nuclear Information System (INIS)

    Boyle, Michael; Brown, Duncan A; Pekowsky, Larne

    2009-01-01

    We study the effectiveness of stationary-phase approximated post-Newtonian waveforms currently used by ground-based gravitational-wave detectors to search for the coalescence of binary black holes by comparing them to an accurate waveform obtained from numerical simulation of an equal-mass non-spinning binary black hole inspiral, merger and ringdown. We perform this study for the initial- and advanced-LIGO detectors. We find that overlaps between the templates and signal can be improved by integrating the match filter to higher frequencies than used currently. We propose simple analytic frequency cutoffs for both initial and advanced LIGO, which achieve nearly optimal matches, and can easily be extended to unequal-mass, spinning systems. We also find that templates that include terms in the phase evolution up to 3.5 post-Newtonian (pN) order are nearly always better, and rarely significantly worse, than 2.0 pN templates currently in use. For initial LIGO we recommend a strategy using templates that include a recently introduced pseudo-4.0 pN term in the low-mass (M ≤ 35 M o-dot ) region, and 3.5 pN templates allowing unphysical values of the symmetric reduced mass η above this. This strategy always achieves overlaps within 0.3% of the optimum, for the data used here. For advanced LIGO we recommend a strategy using 3.5 pN templates up to M = 12 M o-dot , 2.0 pN templates up to M = 21 M o-dot , pseudo-4.0 pN templates up to 65 M o-dot , and 3.5 pN templates with unphysical η for higher masses. This strategy always achieves overlaps within 0.7% of the optimum for advanced LIGO.

  15. A molecular dynamics calculation of solid phase of malonic acid

    Indian Academy of Sciences (India)

    Recent studies suggest that hydrogen bonds, in particular, hydrogen bond chains play an important role in determining the properties of a substance.We report an investigation into the triclinic phase of crystalline malonic acid. One of two intermolecular interaction potentials proposed here is seen to predict the lattice ...

  16. Gas-Phase IR Spectroscopy of Deprotonated Amino Acids

    NARCIS (Netherlands)

    Oomens, J.; Steill, J. D.; Redlich, B.

    2009-01-01

    Gas-phase infrared multiple photon dissociation (IRMPD) spectra have been recorded for the conjugate bases of a series of amino acids (Asp, Cys, Glu, Phe, Set, Trp, Tyr). The spectra are dominated by strong symmetric and antisymmetric carboxylate stretching modes around 1300 and 1600 cm(-1),

  17. Equivariant cohomology and stationary phase

    NARCIS (Netherlands)

    Duistermaat, J.J.

    1993-01-01

    This is the text of a survey lecture given at the conference on \\Symplectic Geometry and its Applications", Keio University, Yokohama, July 21, 1993. I have been stimulated by many people, but I would like to thank especially L. Jerey for her helpful explanations to me of [17].

  18. Predicted Gas-Phase and Liquid-Phase Acidities of Carborane Carboxylic and Dicarboxylic Acids

    Czech Academy of Sciences Publication Activity Database

    Oliva-Enrich, J. M.; Humbel, S.; Santaballa, J.A.; Alkorta, I.; Notario, R.; Dávalos, J. Z.; Canle-L., M.; Bernhardt, E.; Holub, Josef; Hnyk, Drahomír

    2018-01-01

    Roč. 3, č. 16 (2018), s. 4344-4353 ISSN 2365-6549 Institutional support: RVO:61388980 Keywords : Acidity * Carboranes * Computational Chemistry * Delocalization Energy * Electronic Structure Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry

  19. Wide-range high-resolution transmission electron microscopy reveals morphological and distributional changes of endomembrane compartments during log to stationary transition of growth phase in tobacco BY-2 cells.

    Science.gov (United States)

    Toyooka, Kiminori; Sato, Mayuko; Kutsuna, Natsumaro; Higaki, Takumi; Sawaki, Fumie; Wakazaki, Mayumi; Goto, Yumi; Hasezawa, Seiichiro; Nagata, Noriko; Matsuoka, Ken

    2014-09-01

    Rapid growth of plant cells by cell division and expansion requires an endomembrane trafficking system. The endomembrane compartments, such as the Golgi stacks, endosome and vesicles, are important in the synthesis and trafficking of cell wall materials during cell elongation. However, changes in the morphology, distribution and number of these compartments during the different stages of cell proliferation and differentiation have not yet been clarified. In this study, we examined these changes at the ultrastructural level in tobacco Bright yellow 2 (BY-2) cells during the log and stationary phases of growth. We analyzed images of the BY-2 cells prepared by the high-pressure freezing/freeze substitution technique with the aid of an auto-acquisition transmission electron microscope system. We quantified the distribution of secretory and endosomal compartments in longitudinal sections of whole cells by using wide-range gigapixel-class images obtained by merging thousands of transmission electron micrographs. During the log phase, all Golgi stacks were composed of several thick cisternae. Approximately 20 vesicle clusters (VCs), including the trans-Golgi network and secretory vesicle cluster, were observed throughout the cell. In the stationary-phase cells, Golgi stacks were thin with small cisternae, and only a few VCs were observed. Nearly the same number of multivesicular body and small high-density vesicles were observed in both the stationary and log phases. Results from electron microscopy and live fluorescence imaging indicate that the morphology and distribution of secretory-related compartments dramatically change when cells transition from log to stationary phases of growth. © The Author 2014. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

  20. The Genealogical Tree of Ethanol: Gas-phase Formation of Glycolaldehyde, Acetic Acid, and Formic Acid

    Science.gov (United States)

    Skouteris, Dimitrios; Balucani, Nadia; Ceccarelli, Cecilia; Vazart, Fanny; Puzzarini, Cristina; Barone, Vincenzo; Codella, Claudio; Lefloch, Bertrand

    2018-02-01

    Despite the harsh conditions of the interstellar medium, chemistry thrives in it, especially in star-forming regions where several interstellar complex organic molecules (iCOMs) have been detected. Yet, how these species are synthesized is a mystery. The majority of current models claim that this happens on interstellar grain surfaces. Nevertheless, evidence is mounting that neutral gas-phase chemistry plays an important role. In this paper, we propose a new scheme for the gas-phase synthesis of glycolaldehyde, a species with a prebiotic potential and for which no gas-phase formation route was previously known. In the proposed scheme, the ancestor is ethanol and the glycolaldehyde sister species are acetic acid (another iCOM with unknown gas-phase formation routes) and formic acid. For the reactions of the new scheme with no available data, we have performed electronic structure and kinetics calculations deriving rate coefficients and branching ratios. Furthermore, after a careful review of the chemistry literature, we revised the available chemical networks, adding and correcting several reactions related to glycolaldehyde, acetic acid, and formic acid. The new chemical network has been used in an astrochemical model to predict the abundance of glycolaldehyde, acetic acid, and formic acid. The predicted abundance of glycolaldehyde depends on the ethanol abundance in the gas phase and is in excellent agreement with the measured one in hot corinos and shock sites. Our new model overpredicts the abundance of acetic acid and formic acid by about a factor of 10, which might imply a yet incomplete reaction network.

  1. Gene encoding gamma-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7.

    Science.gov (United States)

    Kaur, Simarjot; Mishra, Mukti N; Tripathi, Anil K

    2010-07-04

    Carbonic anhydrase (CA) is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (gamma-CAs) are widespread in prokaryotes but their physiological roles remain elusive. At present, only gamma-CA of Methanosarcina thermophila (Cam) has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one beta-CA and two gamma-CAs. One of the putative gamma-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-gamma-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1). Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a gamma-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized gamma-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration.

  2. Characterization of condensed phase nitric acid particles formed in the gas phase

    Institute of Scientific and Technical Information of China (English)

    Long Jia; Yongfu Xu

    2011-01-01

    The formation of nitric acid hydrates has been observed in a chamber during the dark reaction of NO2 with O3 in the presence of air.The size of condensed phase nitric acid was measured to be 40-100 nm and 20-65 nm at relative humidity (RH) ≤ 5% and RH = 67% under our experimental conditions, respectively.The nitric acid particles were collected on the glass fiber membrane and their chemical compositions were analyzed by infrared spectrum.The main components of nitric acid hydrates in particles are HNO3·3H2O and NO3-·xH2O (x≥ 4) at low RH, whereas at high RH HNO3·H2O, HNO3·2H2O, HNO3·3H2O and NO3-·xH2O (x≥ 4) all exist in the condensed phase.At high RH HNO3·xH2O (x ≤ 3) collected on the glass fiber membrane is greatly increased, while NO3-·xH2O (x ≥4) decreased, compared with low RH.To the best of our knowledge, this is the first time to report that condensed phase nitric acid can be generated in the gas phase at room temperature.

  3. Fundamental thermochemical properties of amino acids: gas-phase and aqueous acidities and gas-phase heats of formation.

    Science.gov (United States)

    Stover, Michele L; Jackson, Virgil E; Matus, Myrna H; Adams, Margaret A; Cassady, Carolyn J; Dixon, David A

    2012-03-08

    The gas-phase acidities of the 20 L-amino acids have been predicted at the composite G3(MP2) level. A broad range of structures of the neutral and anion were studied to determine the lowest energy conformer. Excellent agreement is found with the available experimental gas-phase deprotonation enthalpies, and the calculated values are within experimental error. We predict that tyrosine is deprotonated at the CO(2)H site. Cysteine is predicted to be deprotonated at the SH but the proton on the CO(2)H is shared with the S(-) site. Self-consistent reaction field (SCRF) calculations with the COSMO parametrization were used to predict the pK(a)'s of the non-zwitterion form in aqueous solution. The differences in the non-zwitterion pK(a) values were used to estimate the free energy difference between the zwitterion and nonzwitterion forms in solution. The heats of formation of the neutral compounds were calculated from atomization energies and isodesmic reactions to provide the first reliable set of these values in the gas phase. Further calculations were performed on five rare amino acids to predict their heats of formation, acidities, and pK(a) values.

  4. Preferential Ty1 retromobility in mother cells and nonquiescent stationary phase cells is associated with increased concentrations of total Gag or processed Gag and is inhibited by exposure to a high concentration of calcium.

    Science.gov (United States)

    Peifer, Andrew C; Maxwell, Patrick H

    2018-03-21

    Retrotransposons are abundant mobile DNA elements in eukaryotic genomes that are more active with age in diverse species. Details of the regulation and consequences of retrotransposon activity during aging remain to be determined. Ty1 retromobility in Saccharomyces cerevisiae is more frequent in mother cells compared to daughter cells, and we found that Ty1 was more mobile in nonquiescent compared to quiescent subpopulations of stationary phase cells. This retromobility asymmetry was absent in mutant strains lacking BRP1 that have reduced expression of the essential Pma1p plasma membrane proton pump, lacking the mRNA decay gene LSM1 , and in cells exposed to a high concentration of calcium. Mother cells had higher levels of Ty1 Gag protein than daughters. The proportion of protease-processed Gag decreased as cells transitioned to stationary phase, processed Gag was the dominant form in nonquiescent cells, but was virtually absent from quiescent cells. Treatment with calcium reduced total Gag levels and the proportion of processed Gag, particularly in mother cells. We also found that Ty1 reduced the fitness of proliferating but not stationary phase cells. These findings may be relevant to understanding regulation and consequences of retrotransposons during aging in other organisms, due to conserved impacts and regulation of retrotransposons.

  5. Gas Phase Hydrogenation of Levulinic Acid to gamma-Valerolactone

    NARCIS (Netherlands)

    Bonrath, Werner; Castelijns, Anna Maria Cornelia Francisca; de Vries, Johannes Gerardus; Guit, Rudolf Philippus Maria; Schuetz, Jan; Sereinig, Natascha; Vaessen, Henricus Wilhelmus Leonardus Marie

    The gas phase hydrogenation of levulinic acid to gamma-valerolactone over copper and ruthenium based catalysts in a continuous fixed-bed reactor system was investigated. Among the catalysts a copper oxide based one [50-75 % CuO, 20-25 % SiO2, 1-5 % graphite, 0.1-1 % CuCO3/Cu(OH)(2)] gave

  6. Retention of nucleic acids in ion-pair reversed-phase high-performance liquid chromatography depends not only on base composition but also on base sequence.

    Science.gov (United States)

    Qiao, Jun-Qin; Liang, Chao; Wei, Lan-Chun; Cao, Zhao-Ming; Lian, Hong-Zhen

    2016-12-01

    The study on nucleic acid retention in ion-pair reversed-phase high-performance liquid chromatography mainly focuses on size-dependence, however, other factors influencing retention behaviors have not been comprehensively clarified up to date. In this present work, the retention behaviors of oligonucleotides and double-stranded DNAs were investigated on silica-based C 18 stationary phase by ion-pair reversed-phase high-performance liquid chromatography. It is found that the retention of oligonucleotides was influenced by base composition and base sequence as well as size, and oligonucleotides prone to self-dimerization have weaker retention than those not prone to self-dimerization but with the same base composition. However, homo-oligonucleotides are suitable for the size-dependent separation as a special case of oligonucleotides. For double-stranded DNAs, the retention is also influenced by base composition and base sequence, as well as size. This may be attributed to the interaction of exposed bases in major or minor grooves with the hydrophobic alky chains of stationary phase. In addition, no specific influence of guanine and cytosine content was confirmed on retention of double-stranded DNAs. Notably, the space effect resulted from the stereostructure of nucleic acids also influences the retention behavior in ion-pair reversed-phase high-performance liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Gene encoding γ-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7

    Science.gov (United States)

    2010-01-01

    Background Carbonic anhydrase (CA) is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (γ-CAs) are widespread in prokaryotes but their physiological roles remain elusive. At present, only γ-CA of Methanosarcina thermophila (Cam) has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one β-CA and two γ-CAs. Results One of the putative γ-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-γ-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1). Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. Conclusions This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a γ-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized γ-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration. PMID:20598158

  8. Gene encoding γ-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7

    Directory of Open Access Journals (Sweden)

    Mishra Mukti N

    2010-07-01

    Full Text Available Abstract Background Carbonic anhydrase (CA is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (γ-CAs are widespread in prokaryotes but their physiological roles remain elusive. At present, only γ-CA of Methanosarcina thermophila (Cam has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one β-CA and two γ-CAs. Results One of the putative γ-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-γ-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1. Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. Conclusions This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a γ-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized γ-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration.

  9. Carbon nanotube-based benzyl polymethacrylate composite monolith as a solid phase extraction adsorbent and a stationary phase material for simultaneous extraction and analysis of polycyclic aromatic hydrocarbon in water.

    Science.gov (United States)

    Al-Rifai, Asma'a; Aqel, Ahmad; Wahibi, Lamya Al; ALOthman, Zeid A; Badjah-Hadj-Ahmed, Ahmed-Yacine

    2018-02-02

    A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m -1 for chrysene at flow rate of 0.5 μL min -1 . The method showed a wide linear range (1-500 μg L -1 with R 2 more than 0.9938), acceptable extraction repeatability (RSDs extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L -1 ). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges. Copyright © 2018. Published by Elsevier B.V.

  10. [Separation of p-aminobenzenearsonic acid and its oxide by ion-pair reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Kang, J; Ma, X; Meng, L; Ma, D

    1999-05-01

    To study the separation of p-aminobenzenearsonic acid (PABAA) and its oxide, p-aminophenylarsine oxide (PAPAO), both the absorption spectra were scanned at the wavelengths from 200 nm to 380 nm. PABAA had absorption maximum at 254 nm and PAPAO 258 nm. The effects of salt concentration, column temperature, methanol and ion-pair agent concentrations on the capacity factor were investigated. Compounds of high polarity showed almost no retention on reversed-phase column; as the volume fraction of the methanol decreased from 90% to 10%, the retention time of PABAA gradually increased with broad peak, and partially eluted when methanol volume fraction being below 20%. With temperature rising, the retention time of PABAA was decreased. But PABAA capacity factor can be increased by selecting an appropriate salt concentration for the mobile phase. The cetyltrimethyl and tetrabutyl ammonium ions were separately added as ion-pair agents to the mobile phase containing methanol in phosphate buffer of 10 mmol/L, the changes of retention time were observed. The mechanism of retention based on reversed phase ion-pair model is proposed. Besides, the retention behaviour is also influenced by size exclusion in stationary phase as well as polar interactions with residual silanol group on the silica surface.

  11. Comparison of Separation of Seed Oil Triglycerides Containing Isomeric Conjugated Octadecatrienoic Acid Moieties by Reversed-Phase HPLC

    Directory of Open Access Journals (Sweden)

    Anh Van Nguyen

    2017-12-01

    Full Text Available Relative retention analysis and increment approach were applied for the comparison of triglycerides (TGs retention of a broad set of plant seed oils with isomeric conjugated octadecatrienoic acids (CLnA by reversed-phase HPLC for “propanol-2-acetonitrile” mobile phases and Kromasil 100-5C18 stationary phase with diode array detection (DAD and mass spectrometric (MS detection. The subjects of investigation were TGs of seed oils: Calendula officinalis, Catalpa ovata, Jacaranda mimosifolia, Centranthus ruber, Momordica charantia, Trichosanthes anguina, Punica granatum, Thladiantha dubia, Valeriana officinalis, and Vernicia montana. It was found that a sequence of elution of TGs of the same types is the same without any inversions for full range of mobile phase compositions: punicic (C18:39Z11E13Z < jacaric (C18:38Z10E12Z < catalpic (C18:39E11E13Z < α-eleostearic (C18:39Z11E13E < calendic (C18:38E10E12Z < β-eleostearic (C18:39E11E13E < all-E calendic (C18:38E10E12E acids. TGs and fatty acid compositions were calculated for all oil samples. Regularities of solute retentions as a function of isomeric conjugated octadecatrienoic acid moiety structure are discussed. Thus, it was proven that it is possible to differentiate TGs of complex composition with moieties of all natural CLnA by retention control accomplished by electronic spectra comparison, even though there are only three types of electronic-vibration spectra for seven isomeric CLnA.

  12. Separation of Transfer Ribonucleic Acids by Reverse Phase Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Kelmers, A. D.; Novelli, G. David; Stulberg, M. P.

    1965-10-01

    Numerous experimental techniques for the separation of transfer ribonucleic acids have been successful in preparing partially purified fractions of several specific t-RNAs. Many of the existing methods have depended upon the differential solubility of specific t-RNAs in complex two-phase systems (1-6) and the separation was achieved by means of counter-current extraction techniques. Column chromatography experiments using cellulose exchangers, (7,8) methylated albumin (9,10) or with solvent phases supported on inert material (11-13) have also shown partial separation of specific t-RNAs. Paper chromatographic procedures have produced partial resolutions of t-RNA.14 Methods involving chemical treatment of specific t-RNAs have been reported (15-19).

  13. Synthesis and HPLC evaluation of carboxylic acid phases on a hydride surface.

    Science.gov (United States)

    Pesek, Joseph J; Matyska, Maria T; Gangakhedkar, Surekha; Siddiq, Rukhsana

    2006-04-01

    Three organic moieties containing carboxylic acid functional groups are attached to a particulate silica surface through silanization/hydrosilation. Two compounds (undecylenic acid and 10-undecynoic acid) have 11 carbon chains and the other is a five-carbon acid (pentenoic acid). Bonding is confirmed through carbon elemental analysis, diffuse reflectance infrared fourier transform spectroscopy, and carbon-13 and silicon-29 CP-MAS NMR spectroscopy. The bonded phases are tested by HPLC using PTH amino acids, nucleic acids, theophylline-related compounds, anilines, benzoic acid compounds, choline, and tobramycin. The latter two compounds are used to investigate the aqueous normal phase properties of the three bonded materials.

  14. Stationary nonlinear Airy beams

    International Nuclear Information System (INIS)

    Lotti, A.; Faccio, D.; Couairon, A.; Papazoglou, D. G.; Panagiotopoulos, P.; Tzortzakis, S.; Abdollahpour, D.

    2011-01-01

    We demonstrate the existence of an additional class of stationary accelerating Airy wave forms that exist in the presence of third-order (Kerr) nonlinearity and nonlinear losses. Numerical simulations and experiments, in agreement with the analytical model, highlight how these stationary solutions sustain the nonlinear evolution of Airy beams. The generic nature of the Airy solution allows extension of these results to other settings, and a variety of applications are suggested.

  15. Plasma homovanillic acid in the prodromal phase of schizophrenia.

    Science.gov (United States)

    Sumiyoshi, T; Kurachi, M; Kurokawa, K; Yotsutsuji, T; Uehara, T; Itoh, H; Saitoh, O

    2000-03-01

    Plasma levels of homovanillic acid (pHVA) have been used as a peripheral measure of central dopaminergic activity. Despite a large body of studies investigating pHVA in schizophrenia, little is known about pHVA in patients in the prodromal phase of the illness. Plasma HVA levels of 12 male outpatients meeting DSM-III-R criteria for the prodromal phase of schizophrenia at the time of blood sampling (who later developed psychotic symptoms) were compared with those of 12 normal male healthy volunteers. Task amounts in the Kraepelin arithmetic test at the time of blood sampling were compared between the prodromal patients and normal controls and were correlated with pHVA levels. The prodromal patients had significantly higher pHVA levels compared with normal control subjects. The mean amount of the arithmetic task for the prodromal patients was significantly less than that for controls. In the patient group, a significant negative correlation was observed between pHVA levels and the task amounts. Data from the present study indicate the presence of dopaminergic dysfunction in the prodromal stage of schizophrenia that is associated with neuropsychological impairment. Increased pHVA levels in the prodromal patients may have implications for early detection of schizophrenia.

  16. Development of an achiral supercritical fluid chromatography method with ultraviolet absorbance and mass spectrometric detection for impurity profiling of drug candidates. Part II. Selection of an orthogonal set of stationary phases.

    Science.gov (United States)

    Lemasson, Elise; Bertin, Sophie; Hennig, Philippe; Boiteux, Hélène; Lesellier, Eric; West, Caroline

    2015-08-21

    Impurity profiling of organic products that are synthesized as possible drug candidates requires complementary analytical methods to ensure that all impurities are identified. Supercritical fluid chromatography (SFC) is a very useful tool to achieve this objective, as an adequate selection of stationary phases can provide orthogonal separations so as to maximize the chances to see all impurities. In this series of papers, we have developed a method for achiral SFC-MS profiling of drug candidates, based on a selection of 160 analytes issued from Servier Research Laboratories. In the first part of this study, focusing on mobile phase selection, a gradient elution with carbon dioxide and methanol comprising 2% water and 20mM ammonium acetate proved to be the best in terms of chromatographic performance, while also providing good MS response [1]. The objective of this second part was the selection of an orthogonal set of ultra-high performance stationary phases, that was carried out in two steps. Firstly, a reduced set of analytes (20) was used to screen 23 columns. The columns selected were all 1.7-2.5μm fully porous or 2.6-2.7μm superficially porous particles, with a variety of stationary phase chemistries. Derringer desirability functions were used to rank the columns according to retention window, column efficiency evaluated with peak width of selected analytes, and the proportion of analytes successfully eluted with good peak shapes. The columns providing the worst performances were thus eliminated and a shorter selection of columns (11) was obtained. Secondly, based on 160 tested analytes, the 11 columns were ranked again. The retention data obtained on these columns were then compared to define a reduced set of the best columns providing the greatest orthogonality, to maximize the chances to see all impurities within a limited number of runs. Two high-performance columns were thus selected: ACQUITY UPC(2) HSS C18 SB and Nucleoshell HILIC. Copyright © 2015

  17. Determinação da espessura da camada polimérica de fases estacionárias imobilizadas para cromatografia líquida de alta eficiência por termogravimetria Determination of polymeric layer thickness on immobilized stationary phases for high-performance liquid chromatography using thermogravimetric analyses

    Directory of Open Access Journals (Sweden)

    Anizio M. Faria

    2008-01-01

    Full Text Available This paper presents a simple and practical thermogravimetric method for determining the layer thickness of immobilized polymer stationary phases used in reversed-phase high-performance liquid chromatography. In this method, the weight loss of different polysiloxanes immobilized onto chromatographic supports, determined over the temperature range 150-650 ºC, demonstrated excellent agreement with the sum of carbon and hydrogen content obtained by elemental analysis. The results presented here suggest that the thermogravimetric procedure is an accurate and precise method to determine the polymeric material content on polymer-coated stationary phases.

  18. Chirality, phase transitions and their induction in amino acids

    International Nuclear Information System (INIS)

    Salam, A.

    1991-04-01

    ''Atoms such as carbon, oxygen, nitrogen and hydrogen, the major constituents of biological molecules, are less than 0.4 nm in diameter... The behaviour of small molecules is a reflection of the intrinsic properties of the constituent atoms. Hence it might be expected that the behaviour of large macromolecules can be explained by a knowledge of atomic properties. Since organelles, whole cells and organisms are essentially macromolecular assemblies, it may be possible in time to derive an atomic theory of life'' (Rees and Sternberg). It has been suggested that chirality among the twenty amino acids which make up the proteins may be a consequence of a phase transition which is analogous to that due to BCS superconductivity. We explore these ideas in this paper and show, following Lee and Drell, that a crucial form for the transition temperature T c involves dynamical symmetry breaking. The t-quarks or supersymmetry (or something similar which ensures a heavy mass) appear to be essential if such mechanisms are to hold. (author). 12 refs, 1 fig., 1 tab

  19. Conformational variability of the stationary phase survival protein E from Xylella fastidiosa revealed by X-ray crystallography, small-angle X-ray scattering studies, and normal mode analysis.

    Science.gov (United States)

    Machado, Agnes Thiane Pereira; Fonseca, Emanuella Maria Barreto; Reis, Marcelo Augusto Dos; Saraiva, Antonio Marcos; Santos, Clelton Aparecido Dos; de Toledo, Marcelo Augusto Szymanski; Polikarpov, Igor; de Souza, Anete Pereira; Aparicio, Ricardo; Iulek, Jorge

    2017-10-01

    Xylella fastidiosa is a xylem-limited bacterium that infects a wide variety of plants. Stationary phase survival protein E is classified as a nucleotidase, which is expressed when bacterial cells are in the stationary growth phase and subjected to environmental stresses. Here, we report four refined X-ray structures of this protein from X. fastidiosa in four different crystal forms in the presence and/or absence of the substrate 3'-AMP. In all chains, the conserved loop verified in family members assumes a closed conformation in either condition. Therefore, the enzymatic mechanism for the target protein might be different of its homologs. Two crystal forms exhibit two monomers whereas the other two show four monomers in the asymmetric unit. While the biological unit has been characterized as a tetramer, differences of their sizes and symmetry are remarkable. Four conformers identified by Small-Angle X-ray Scattering (SAXS) in a ligand-free solution are related to the low frequency normal modes of the crystallographic structures associated with rigid body-like protomer arrangements responsible for the longitudinal and symmetric adjustments between tetramers. When the substrate is present in solution, only two conformers are selected. The most prominent conformer for each case is associated to a normal mode able to elongate the protein by moving apart two dimers. To our knowledge, this work was the first investigation based on the normal modes that analyzed the quaternary structure variability for an enzyme of the SurE family followed by crystallography and SAXS validation. The combined results raise new directions to study allosteric features of XfSurE protein. © 2017 Wiley Periodicals, Inc.

  20. Relationship between Acute Phase Proteins and Serum Fatty Acid Composition in Morbidly Obese Patients

    Science.gov (United States)

    Fernandes, Ricardo; Beserra, Bruna Teles Soares; Cunha, Raphael Salles Granato; Hillesheim, Elaine; Camargo, Carolina de Quadros; Pequito, Danielle Cristina Tonello; de Castro, Isabela Coelho; Fernandes, Luiz Cláudio; Nunes, Everson Araújo; Trindade, Erasmo Benício Santos de Moraes

    2013-01-01

    Background. Obesity is considered a low-grade inflammatory state and has been associated with increased acute phase proteins as well as changes in serum fatty acids. Few studies have assessed associations between acute phase proteins and serum fatty acids in morbidly obese patients. Objective. To investigate the relationship between acute phase proteins (C-Reactive Protein, Orosomucoid, and Albumin) and serum fatty acids in morbidly obese patients. Methods. Twenty-two morbidly obese patients were enrolled in this study. Biochemical and clinical data were obtained before bariatric surgery, and fatty acids measured in preoperative serum. Results. Orosomucoid was negatively correlated with lauric acid (P = 0.027) and eicosapentaenoic acid (EPA) (P = 0.037) and positively with arachidonic acid (AA) (P = 0.035), AA/EPA ratio (P = 0.005), and n-6/n-3 polyunsaturated fatty acids ratio (P = 0.035). C-Reactive Protein (CRP) was negatively correlated with lauric acid (P = 0.048), and both CRP and CRP/Albumin ratio were negatively correlated with margaric acid (P = 0.010, P = 0.008, resp.). Albumin was positively correlated with EPA (P = 0.027) and margaric acid (P = 0.008). Other correlations were not statistically significant. Conclusion. Our findings suggest that serum fatty acids are linked to acute phase proteins in morbidly obese patients. PMID:24167354

  1. Stationary scattering theory

    International Nuclear Information System (INIS)

    Combes, J.M.

    1980-10-01

    A complementary approach to the time dependent scattering theory for one-body Schroedinger operators is presented. The stationary theory is concerned with objects of quantum theory like scattering waves and amplitudes. In the more recent abstract stationary theory some generalized form of the Lippman-Schwinger equation plays the basic role. Solving this equation leads to a linear map between generalized eigenfunctions of the perturbed and unperturbed operators. This map is the section at fixed energy of the wave-operator from the time dependent theory. Although the radiation condition does not appears explicitely in this formulation it can be shown to hold a posteriori in a variety of situations thus restoring the link with physical theories

  2. Stationary theory of scattering

    International Nuclear Information System (INIS)

    Kato, T.

    1977-01-01

    A variant of the stationary methods is described, and it is shown that it is useful in a wide range of problems, including scattering, by long-range potentials, two-space scattering, and multichannel scattering. The method is based on the notion of spectral forms. The paper is restricted to the simplest case of continuous spectral forms defined on a Banach space embedded in the basic Hilbert space. (P.D.)

  3. Evaluation of the chiral recognition properties and the column performances of three chiral stationary phases based on cellulose for the enantioseparation of six dihydropyridines by high-performance liquid chromatography.

    Science.gov (United States)

    Yu, Jia; Tang, Jing; Yuan, Xiaowei; Guo, Xingjie; Zhao, Longshan

    2017-03-01

    Separations of six dihydropyridine enantiomers on three commercially available cellulose-based chiral stationary phases (Chiralcel OD-RH, Chiralpak IB, and Chiralpak IC) were evaluated with high-performance liquid chromatography (HPLC). The best enantioseparation of the six chiral drugs was obtained with a Chiralpak IC (250 × 4.6 mm i.d., 5 μm) column. Then the influence of the mobile phase including an alcohol-modifying agent and alkaline additive on the enantioseparation were investigated and optimized. The optimal mobile phase conditions and maximum resolution for every analyte were as follows respectively: n-hexane/isopropanol (85:15, v/v) for nimodipine (R = 5.80) and cinildilpine (R = 5.65); n-hexane/isopropanol (92:8, v/v) for nicardipine (R = 1.76) and nisoldipine (R = 1.92); and n-hexane/isopropanol/ethanol (97:2:1, v/v/v) for felodipine (R = 1.84) and lercanidipine (R = 1.47). Relative separation mechanisms are discussed based on the separation results, and indicate that the achiral parts in the analytes' structure showed an important influence on the separation of the chiral column. © 2017 Wiley Periodicals, Inc.

  4. The staphylococcal accessory regulator, SarA, is an RNA-binding protein that modulates the mRNA turnover properties of late-exponential and stationary phase Staphylococcus aureus cells

    Directory of Open Access Journals (Sweden)

    John M Morrison

    2012-03-01

    Full Text Available The modulation of mRNA turnover is gaining recognition as a mechanism by which Staphylococcus aureus regulates gene expression, but the factors that orchestrate alterations in transcript degradation are poorly understood. In that regard, we previously found that 138 mRNA species, including the virulence factors protein A (spa and collagen binding protein (cna, are stabilized in a sarA-dependent manner during exponential phase growth, suggesting that SarA protein may directly or indirectly effect the RNA turnover properties of these transcripts. Herein, we expanded our characterization of the effects of sarA on mRNA turnover during late exponential and stationary phases of growth. Results revealed that the locus affects the RNA degradation properties of cells during both growth phases. Further, using gel mobility shift assays and RIP-ChIP, it was found that SarA protein is capable of binding mRNA species that it stabilizes both in vitro and within bacterial cells. Taken together, these results suggest that SarA post-transcriptionally regulates S. aureus gene expression in a manner that involves binding to and consequently altering the mRNA turnover properties of target transcripts.

  5. The effect of growth phase on the lipid class, fatty acid and sterol composition in the marine dinoflagellate, Gymnodinium sp. in batch culture.

    Science.gov (United States)

    Mansour, Maged P; Volkman, John K; Blackburn, Susan I

    2003-05-01

    We have studied the effects of growth phase on the lipid composition in batch cultures of Gymnodinium sp. CS-380/3 over 43 days of culturing. The lipid content increased two fold, from late logarithmic (day 6) to linear growth phase (day 22) then decreased at stationary phase (day 43) while the lipid yield (mg l(-1)) increased 30-fold from day 6 to 30 mg l(-1) at day 43. Changes in fatty acid content mirrored those observed for the total lipid, while the sterol content continued to increase with culture age through to stationary phase. The largest changes occurred in the lipid classes, especially the polar lipids and triacylglycerols (oil). The proportion of triacylglycerols increased from 8% (of total lipids) at day 6 to 30% at day 43, with a concomitant decrease in the polar lipid fraction. The proportions of 16:0 and DHA [22:6(n-3)] increased while those of 18:5(n-3) and EPA [20:5(n-3)] decreased with increasing culture age. The proportion of the major sterol, dinosterol, decreased from 41% (day 6) to 29% (day 43), while the major dinostanol epimer (23R,24R) increased from 33% (day 6) to 38% (day 22). Despite small changes in the proportion of the main sterols, the same sterols were present at all stages of growth, indicating their value as a chemotaxonomic tool for distinguishing between strains within the same genus. Growth phase could be a useful variable for optimising the oil and DHA content with potential for aquaculture feeds and a source of DHA-rich oils for nutraceuticals.

  6. Acid-base equilibrium. A thermodynamic study of formation and stability of the Bi-2223 phase

    International Nuclear Information System (INIS)

    Xi, Z.; Zhou, L.

    1993-01-01

    A general acid-base equilibrium theory was proposed to explain the formation and stability of the Bi-2223 phase based on the Lewis acid base theory and principle of metallurgical physical chemistry. The acid-base nature of oxide was defined according to the electrostatic force between cation and oxygen anion. A series of experimental facts were systematically explained based on the theory: substitution of Bi for Ca in the Pb-free 2223 phase, and the effect of substitution of the high-valent cation for Bi 3+ ; oxygen-pressure atmosphere, and the heat-schocking technique on the formation and stability of the 2223 phase. 14 refs., 2 tabs

  7. Effect of the water content on the retention and enantioselectivity of albendazole and fenbendazole sulfoxides using amylose-based chiral stationary phases in organic-aqueous conditions.

    Science.gov (United States)

    Materazzo, Sabrina; Carradori, Simone; Ferretti, Rosella; Gallinella, Bruno; Secci, Daniela; Cirilli, Roberto

    2014-01-31

    Four commercially available immobilized amylose-derived CSPs (Chiralpak IA-3, Chiralpak ID-3, Chiralpak IE-3 and Chiralpak IF-3) were used in the HPLC analysis of the chiral sulfoxides albendazole (ABZ-SO) and fenbendazole (FBZ-SO) and their in vivo sulfide precursor (ABZ and FBZ) and sulfone metabolite (ABZ-SO2 and FBZ-SO2) under organic-aqueous mode. U-shape retention maps, established by varying the water content in the acetonitrile- and ethanol-water mobile phases, were indicative of two retention mechanisms operating on the same CSP. The dual retention behavior of polysaccharide-based CSPs was exploited to design greener enantioselective and chemoselective separations in a short time frame. The enantiomers of ABZ-SO and FBZ-SO were baseline resolved with water-rich mobile phases (with the main component usually being 50-65% water in acetonitrile) on the IF-3 CSP and ethanol-water 100:5 mixture on the IA-3 and IE-3 CSPs. A simultaneous separation of ABZ (or FBZ), enantiomers of the corresponding sulfoxide and sulfone was achieved on the IA-3 using ethanol-water 100:60 (acetonitrile-water 100:100 for FBZ) as a mobile phase. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Stationary flow near fronts

    Directory of Open Access Journals (Sweden)

    Reinhold Steinacker

    2016-12-01

    Full Text Available In 1906, the Austrian scientist Max Margules published a paper on temperature stratification in resting and non-accelerated moving air. The paper derives conditions for stationary slopes of air mass boundaries and was an important forerunner of frontal theories. Its formulation of relations between changes in density and geostrophic wind across the front is basically a discrete version of the thermal wind balance equation. The paper was highly influential and is still being cited to the present day. This paper accompanies an English translation of Margules’ seminal paper. We conclude here our “Classic Papers” series of the Meteorologische Zeitschrift.

  9. Are carboxyl groups the most acidic sites in amino acids? Gas-phase acidities, photoelectron spectra, and computations on tyrosine, p-hydroxybenzoic acid, and their conjugate bases.

    Science.gov (United States)

    Tian, Zhixin; Wang, Xue-Bin; Wang, Lai-Sheng; Kass, Steven R

    2009-01-28

    Deprotonation of tyrosine in the gas phase was found to occur preferentially at the phenolic site, and the conjugate base consists of a 70:30 mixture of phenoxide and carboxylate anions at equilibrium. This result was established by developing a chemical probe for differentiating these two isomers, and the presence of both ions was confirmed by photoelectron spectroscopy. Equilibrium acidity measurements on tyrosine indicated that deltaG(acid)(o) = 332.5 +/- 1.5 kcal mol(-1) and deltaH(acid)(o) = 340.7 +/- 1.5 kcal mol(-1). Photoelectron spectra yielded adiabatic electron detachment energies of 2.70 +/- 0.05 and 3.55 +/- 0.10 eV for the phenoxide and carboxylate anions, respectively. The H/D exchange behavior of deprotonated tyrosine was examined using three different alcohols (CF3CH2OD, C6H5CH2OD, and CH3CH2OD), and incorporation of up to three deuterium atoms was observed. Two pathways are proposed to account for these results, and all of the experimental findings are supplemented with B3LYP/aug-cc-pVDZ and G3B3 calculations. In addition, it was found that electrospray ionization of tyrosine from a 3:1 (v/v) CH3OH/H2O solution using a commercial source produces a deprotonated [M-H]- anion with the gas-phase equilibrium composition rather than the structure of the ion that exists in aqueous media. Electrospray ionization from acetonitrile, however, leads largely to the liquid-phase (carboxylate) structure. A control molecule, p-hydroxybenzoic acid, was found to behave in a similar manner. Thus, the electrospray conditions that are employed for the analysis of a compound can alter the isomeric composition of the resulting anion.

  10. An Experimental and Computational Study of the Gas-Phase Acidities of the Common Amino Acid Amides.

    Science.gov (United States)

    Plummer, Chelsea E; Stover, Michele L; Bokatzian, Samantha S; Davis, John T M; Dixon, David A; Cassady, Carolyn J

    2015-07-30

    Using proton-transfer reactions in a Fourier transform ion cyclotron resonance mass spectrometer and correlated molecular orbital theory at the G3(MP2) level, gas-phase acidities (GAs) and the associated structures for amides corresponding to the common amino acids have been determined for the first time. These values are important because amino acid amides are models for residues in peptides and proteins. For compounds whose most acidic site is the C-terminal amide nitrogen, two ions populations were observed experimentally with GAs that differ by 4-7 kcal/mol. The lower energy, more acidic structure accounts for the majority of the ions formed by electrospray ionization. G3(MP2) calculations predict that the lowest energy anionic conformer has a cis-like orientation of the [-C(═O)NH](-) group whereas the higher energy, less acidic conformer has a trans-like orientation of this group. These two distinct conformers were predicted for compounds with aliphatic, amide, basic, hydroxyl, and thioether side chains. For the most acidic amino acid amides (tyrosine, cysteine, tryptophan, histidine, aspartic acid, and glutamic acid amides) only one conformer was observed experimentally, and its experimental GA correlates with the theoretical GA related to side chain deprotonation.

  11. Ortho-substituent correlated retention of polychlorinated biphenyls on a 50% n-octyl-methylpolysiloxane stationary phase by HRGC/MSD

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, R.; Ballschmiter, K.

    1988-11-01

    Polychlorinated biphenyls (PCB) have been known as ubiquitous environmental pollutants since the late 60s. They are found partitioned between all environmental compartments according to their physico-chemical properties. Investigation of their partitioning, degradation, and transport behaviour demands sensitive and selective analytical methods for this complex mixture of up to 209 theoretically possible compounds. Congener-specific separation by high-resolution gas chromatography coupled with mass-selective detection would be a suitable approach to this multi-compound problem. In this paper, the separation of PCB congeners by capillary gas chromatography (HRGC) on a 50% n-octyl-methylpolysiloxane phase is presented.

  12. The synthesis and characterization of novel brush-type chiral stationary phase based on terpenoid selector for resolution of chiral drugs

    Directory of Open Access Journals (Sweden)

    Wang Dao-Cai

    2016-01-01

    Full Text Available In the light of the chiral resolution mechanism and structures of brush-type CSP, a new chiral selector 4′-carboxyl-1′-ursolic methyl ester-3β-yl-benzoate has been prepared. Then the terpenoid chiral selector was covalently linked to 3-aminopropyl silica gel. Its structure identification data are provided by 1H NMR, MS and elementary analysis. The enantiodiscriminating capability of the brush-type CSP was evaluated by static adsorption experiment with methyl mandelate, aniline derivative of mandelic acid, benzoin and ibuprofen. Experimental results demonstrated that the chiral selector has selectivity, and the enantiomers of methyl mandelate and ibuprofen could be separated on the CSP, which indicated that the novel brush-type CSP possess a bright prospects for chiral separation potentially.

  13. The Stationary SQUID

    Science.gov (United States)

    Berger, Jorge

    2018-06-01

    In the customary mode of operation of a SQUID, the electromagnetic field in the SQUID is an oscillatory function of time. In this situation, electromagnetic radiation is emitted and couples to the sample. This is a back action that can alter the state that we intend to measure. A circuit that could perform as a stationary SQUID consists of a loop of superconducting material that encloses the magnetic flux, connected to a superconducting and to a normal electrode. This circuit does not contain Josephson junctions, or any other miniature feature. We study the evolution of the order parameter and of the electrochemical potential in this circuit; they converge to a stationary regime, and the voltage between the electrodes depends on the enclosed flux. We obtain expressions for the power dissipation and for the heat transported by the electric current; the validity of these expressions does not rely on a particular evolution model for the order parameter. We evaluate the influence of fluctuations. For a SQUID perimeter of the order of 1μ m and temperature 0.9T_c, we obtain a flux resolution of the order of 10^{-5}Φ _0/Hz^{1/2}; the resolution is expected to improve as the temperature is lowered.

  14. Stationary flywheel energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Gilhaus, A; Hau, E; Gassner, G; Huss, G; Schauberger, H

    1981-01-01

    The aim of this system study is to find out industrial applications of stationary flywheel energy accumulators. The economic value for the consumer and the effects on the power supply grid are investigated. Up to now, stationary flywheel energy accumulators have only been used in a small range. The main reason for thinking of the application in a wider range was the hope that those could be used economically for lowering the maximum output demand of the power supply grid. The possible savings in energy costs, however, proved to be too small for paying back the investment costs. Further benefits are necessary for advantageous application. As to overall economy, compensation of short time maximum power output seems to be more favorable at the power stations. An additional possibility for energy storage by flywheels is given where otherwise lost energy can be used effectively, according to the successful brake energy storage in vehicles. Under this aspect the future use of flywheels in wind-power-plants seems to be promising. Attractive savings of energy can be obtained by introducing modern flywheel technology for emergency power supply units which are employed for instance in telecommunication systems. Especially the application for emergency power supply, in power stations and in combustion with wind energy converters need further investigation.

  15. Vapour phase synthesis of salol over solid acids via transesterification

    Indian Academy of Sciences (India)

    Administrator

    rate of reactants, WHSV and time-on-stream on the conversion (%) of phenol and selectivity (%) of salol ... Possible reaction mechanisms for the formation of salol and diphenyl ether over ... Hence, vapour-phase conditions of the experiment.

  16. Bleeding evaluation of the stationary phase from a few novel macroporous silica-substrate polymeric materials used for radionuclide partitioning from HLLW in MAREC process

    International Nuclear Information System (INIS)

    Zhang, A.; Wei, Y.; Kumagai, M.

    2005-01-01

    To separate minor actinides from HLLW by extraction chromatography, a few novel silica-based di(2-ethylhexyl)phosphoric acid (HDEHP), 4,4',(5')-di(tert-butylcyclohexano)-18-crown-6 (DtBuCH18C6), octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO), and N,N,N',N'-tetraoctyl-3-oxapentane-1,5-diamide (TODGA) polymeric adsorption materials (HDEHP/SiO 2 -P, DtBuCH18C6/SiO 2 -P, CMPO/SiO 2 -P, and TODGA/SiO 2 -P) were synthesized by impregnating HDEHP, DtBuCH18C6, CMPO, and TODGA into the pores of porous SiO 2 -P particles, which were the new kind of inorganic/organic composites consisted of macroporous SiO 2 and copolymer. The bleeding behavior of these composites was investigated by examining the effect of contact time and HNO 3 concentration. It was found that in the tested HNO 3 concentration range, a noticeable quantity of DtBuCH18C6, at least 600 ppm, leaked out from DtBuCH18C6/SiO 2 -P because of the protonation of DtBuCH18C6 with hydrogen ion, while the others were lower and basically equivalent to the solubility of HDEHP, CMPO, or TODGA in corresponding acidities solutions. Based on the batch experiment, the bleeding of CMPO/SiO 2 -P and TODGA/SiO 2 -P, the main adsorbents used in MAREC process for HLLW partitioning, was evaluated by column operation in 0.01M HNO 3 and 3M HNO 3 . The quantity of CMPO leaked was ∼48 ppm in 0.01M HNO 3 and ∼37 ppm in 3.0M HNO 3 . The bleeding of TODGA decreased from 23.2 ppm to 7.27 ppm at the initial stage and then basically kept constant. An actual bleeding of TODGA was evaluated by the separation of Sr(II) from a 2.0M HNO 3 solution containing 5.0 x 10 -3 M of 6 typically simulated elements. (author)

  17. Phase equilibrium modelling for mixtures with acetic acid using an association equation of state

    DEFF Research Database (Denmark)

    Muro Sunè, Nuria; Kontogeorgis, Georgios; von Solms, Nicolas

    2008-01-01

    Acetic acid is a very important compound in the chemical industry with applications both as solvent and intermediate in the production of, e.g., polyesters. The design of these processes requires knowledge of the phase equilibria of mixtures containing acetic acid and a wide variety of compounds ...

  18. Experimental study and phase equilibrium modeling of systems containing acid gas and glycol

    DEFF Research Database (Denmark)

    Afzal, Waheed; Breil, Martin P.; Tsivintzelis, Ioannis

    2012-01-01

    In this work, we study phase equilibria of systems containing acid gases and glycols. The acid gases include carbonyl sulfide (COS), hydrogen sulfide (H2S), and carbon dioxide (CO2) while glycols include monoethylene glycol (MEG), diethylene glycol (DEG), and triethylene glycol (TEG). A brief lit...

  19. High Pressure Size Exclusion Chromatography (HPSEC) Determination of Dissolved Organic Matter Molecular Weight Revisited: Accounting for Changes in Stationary Phases, Analytical Standards, and Isolation Methods.

    Science.gov (United States)

    McAdams, Brandon C; Aiken, George R; McKnight, Diane M; Arnold, William A; Chin, Yu-Ping

    2018-01-16

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA 280 ) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA 280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA 280 .

  20. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    Pias, J. B.; Gasco, L.

    1976-01-01

    The retention indices of aliphatic alcohols of carbon number up to C g , and of their benzoyl derivatives up to C 7 , were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH 2 - group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices Δl , and positional and structural increments δI, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs

  1. High pressure size exclusion chromatography (HPSEC) determination of dissolved organic matter molecular weight revisited: Accounting for changes in stationary phases, analytical standards, and isolation methods

    Science.gov (United States)

    McAdams, Brandon C.; Aiken, George R.; McKnight, Diane M.; Arnold, William A.; Chin, Yu-Ping

    2018-01-01

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA280) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA280.

  2. Gas Phase Structure of Amino Acids: La-Mb Studies

    Science.gov (United States)

    Mata, I. Pena S.; Sanz, M. E.; Vaquero, V.; Cabezas, C.; Perez, C.; Blanco, S.; López, J. C.; Alonso, J. L.

    2009-06-01

    Recent improvements in our laser ablation molecular beam Fourier transform microwave (LA-MB-FTMW) spectrometer such as using Laval-type nozzles and picoseconds Nd:YAG lasers (30 to 150 ps) have allowed a major step forward in the capabilities of this experimental technique as demonstrated by the last results in serine cysteine and threonine^a for which seven, six and seven conformers have been respectively identified. Taking advantage of these improvements we have investigated the natural amino acids metionine, aspartic and glutamic acids and the γ-aminobutyric acid (GABA) with the aim of identify and characterize their lower energy conformers. Searches in the rotational spectra have lead to the identification of seven conformers of metionine, six and five of aspartic and glutamic acids, respectively, and seven for the γ-aminobutyric. These conformers have been unambiguously identified by their spectroscopic constants. In particular the ^{14}N nuclear quadrupole coupling constants, that depend heavily on the orientation of the amino group with respect to the principal inertial axes of the molecule, prove to be a unique tool to distinguish unambigously between conformations with similar rotational constants. For the γ-aminobutyric acid two of the seven observed structures are stablized by an intramolecular interaction n-π*. Two new conformers of proline have been identified together with the two previously observed. J. L. Alonso, C. Pérez, M. E. Sanz, J. C. López, S. Blanco, Phys.Chem.Chem.Phys., 2009, 11, 617. D. B. Atkinson, M. A. Smith, Rev. Sci. Instrum. 1995, 66, 4434 S. Blanco, M. E. Sanz, J. C. López, J. L. Alonso, Proc. Natl. Acad. Sci. USA2007, 104, 20183. M. E. Sanz, S. Blanco, J. C. López, J. L. Alonso, Angew. Chem. Int. Ed.,2008, 120, 6312. A. Lesarri, S. Mata, E. J. Cocinero, S. Blanco, J.C. López, J. L. Alonso, Angew. Chem. Int. Ed. , 2002, 41, 4673

  3. Phase transformations of 4,4'-biphenyldicarboxylic acid on Cu(001)

    NARCIS (Netherlands)

    Schwarz, Daniel; van Gastel, Raoul; Zandvliet, Henricus J.W.; Poelsema, Bene

    2012-01-01

    The growth and structure of 4,4′-biphenyldicarboxylic-acid (BDA) on Cu(001) at temperatures between 300 and 400 K was studied by low energy electron microscopy and μ-LEED. First, the adsorbed BDA molecules form a disordered dilute phase. Once this phase reaches a sufficiently high density, a

  4. Phase Behavior of a Phospholipid/Fatty Acid/Water Mixture Studied in Atomic Detail

    NARCIS (Netherlands)

    Knecht, Volker; Mark, Alan E.; Marrink, Siewert-Jan

    2006-01-01

    Molecular dynamics simulations have been used to study the phase behavior of a dipalmitoylphosphatidylcholine (DPPC)/palmitic acid (PA)/water 1:2:20 mixture in atomic detail. Starting from a random solution of DPPC and PA in water, the system adopts either a gel phase at temperatures below similar

  5. New high-performance liquid chromatography method for the determination of (R)-warfarin and (S)-warfarin using chiral separation on a glycopeptide-based stationary phase.

    Science.gov (United States)

    Malakova, Jana; Pavek, Petr; Svecova, Lucie; Jokesova, Iveta; Zivny, Pavel; Palicka, Vladimir

    2009-10-01

    Warfarin is a well-known anticoagulant agent that occurs in two enantiomers, (R)-(+)-warfarin and (S)-(-)-warfarin. A new liquid chromatography method for the determination of both enantiomers was developed, validated and applied in in vitro studies with the aim of evaluating the accumulation of (R)-warfarin and (S)-warfarin in the hepatoma HepG2 cell line. OptiMEM cell cultivation medium samples and cellular lysates were purified using Waters Oasis MAX extraction cartridges. The chiral separation of warfarin and the internal standard p-chlorowarfarin enantiomers was performed on an Astec Chirobiotic V2 column at a flow rate of 1.2mL/min. The mobile phase was composed of 31% acetonitrile, 5% of methanol and 64% of ammonium acetate buffer (10mmol/L, pH 4.1). The enantiomers were quantified using a fluorescence detector (lambda(excit)=320nm, lambda(emiss)=415nm). The limit of detection was found to be 0.121micromol/L of (S)-warfarin and 0.109micromol/L of (R)-warfarin. The range of applicability and linearity was estimated from 0.25 to 100micromol/L. The precision ranged from 1.3% to 12.2% of the relative standard deviation, and the accuracy reached acceptable values from 95.5% to 108.4%. The new bioanalytical method confirmed the same accumulation of (R)-warfarin and (S)-warfarin in the hepatoma HepG2 cell line.

  6. Determination of complex formation constants by phase sensitive alternating current polarography: Cadmium-polymethacrylic acid and cadmium-polygalacturonic acid.

    Science.gov (United States)

    Garrigosa, Anna Maria; Gusmão, Rui; Ariño, Cristina; Díaz-Cruz, José Manuel; Esteban, Miquel

    2007-10-15

    The use of phase sensitive alternating current polarography (ACP) for the evaluation of complex formation constants of systems where electrodic adsorption is present has been proposed. The applicability of the technique implies the previous selection of the phase angle where contribution of capacitive current is minimized. This is made using Multivariate Curve Resolution by Alternating Least Squares (MCR-ALS) in the analysis of ACP measurements at different phase angles. The method is checked by the study of the complexation of Cd by polymethacrylic (PMA) and polygalacturonic (PGA) acids, and the optimal phase angles have been ca. -10 degrees for Cd-PMA and ca. -15 degrees for Cd-PGA systems. The goodness of phase sensitive ACP has been demonstrated comparing the determined complex formation constants with those obtained by reverse pulse polarography, a technique that minimizes the electrode adsorption effects on the measured currents.

  7. Frustrated smectic liquid crystalline phases in lactic acid derivatives

    Czech Academy of Sciences Publication Activity Database

    Glogarová, Milada; Novotná, Vladimíra

    2016-01-01

    Roč. 89, č. 7-8 (2016), s. 829-839 ISSN 0141-1594 R&D Projects: GA ČR GA15-02843S Institutional support: RVO:68378271 Keywords : field * liquid crystals * TGB phases Subject RIV: JJ - Other Materials Impact factor: 1.060, year: 2016

  8. Determination of medronic acid by reversed-phase high-performance liquid chromatography

    International Nuclear Information System (INIS)

    Zhao Xiuyan; Wang Xiaojing; Fu Bo; Ye Zhaoyun; Liu Yinli

    2012-01-01

    An isocratic liquid chromatographic method with evaporative light scattering detection (ELSD) was developed for the determination of medronic acid and its related sub- stances. Volatile pentylamine was used as the ion-pairing agent. Separations were performed on a Symmetry C8 column with an mobile phase of 98 : 2 (V : V) 30 mmol/L pentylamine (pH 5.0, adjusted with acetic acid)-methanol. The mobile phase was delivered at a flow-rate 1.0 mL/min. The method is applicable to the routine analysis and the quality con- trol of medronic acid. (authors)

  9. The chromatographic behavior of arsenic compounds on anion exchange columns with binary organic acids as mobile phases

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, J.; Goessler, W.; Kosmus, W. [Graz Univ. (Austria). Inst. fuer Analytische Chemie

    1998-03-01

    Identification and quantification of arsenic compounds was performed with high-performance liquid chromatography (HPLC) and flame atomic absorption spectrometry (FAAS) as element-specific detector. Arsenous acid, methylarsonic acid, dimethylarsinic acid, arsenic acid, arsenobetaine, and arsenocholine were separated on two anion-exchange columns (Synchropak Q 300 and PRP-X 100) with different binary organic acids as mobile phases. The influence of chromatographic parameters, such as pH and the concentration of the mobile phase were investigated. An unusual chromatographic behavior of arsenous acid was observed when tartaric acid was used as mobile phase. (orig.)

  10. Employment of a novel ultrasonic method to investigate high pressure phase transitions in oleic acid

    Science.gov (United States)

    Rostocki, A. J.; Siegoczyński, R. M.; Kiełczyński, P.; Szalewski, M.; Balcerzak, A.; Zduniak, M.

    2011-06-01

    In this work, the variation of sound velocity with hydrostatic pressure for oleic acid is evaluated up to 350 MPa. During the measurement, we identified the phase transformation of oleic acid and the presence of the hysteresis of the dependence of sound velocity on pressure. From the performed measurements, it can be seen that the dependence of sound velocity on pressure can be used to investigate phase transformations in natural oils. Ultrasonic waves were excited and detected using piezoelectric LiNbO3(Y-36 cut) 5 MHz transducers. The phase velocity of the longitudinal ultrasonic waves was measured using a cross-correlation method to evaluate the time of flight.

  11. A Novel Two-Step Liquid-Liquid Extraction Procedure Combined with Stationary Phase Immobilized Human Serum Albumin for the Chiral Separation of Cetirizine Enantiomers along with M and P Parabens

    Directory of Open Access Journals (Sweden)

    Aleksandra Chmielewska

    2016-12-01

    Full Text Available The research into the separation of drug enantiomers is closely related to the safety and efficiency of the drugs. The aim of this study was to develop a simple and validated HPLC method to analyze cetirizine enantiomers. In the case of liquid dosage forms, besides the active substance in large amounts there are usually also inactive ingredients such as methyl- and propylparaben. Unfortunately, these compounds can interfere with the analyte, inter alia during chiral separation of the analyte enantiomers. The proposed innovative two-step liquid-liquid extraction procedure allowed for the determination of cetirizine enantiomers (along with M and P parabens also in liquid dosage forms. The main focus of this study was the chromatographic activity of cetirizine dihydrochloride on the proteinate-based chiral stationary phase. The chromatographic separation of cetirizine enantiomers was performed on an immobilized human serum albumin (HSA column for the first time. Measurements were performed at a wavelength of 227 nm. Under optimal conditions, baseline separation of two enantiomers was obtained with 1.43 enantioseparation factor (α and 1.82 resolution (Rs. Finally, the proposed method was successfully applied to the selected pharmaceutical formulations.

  12. Solid-phase route to Fmoc-protected cationic amino acid building blocks

    DEFF Research Database (Denmark)

    Clausen, Jacob Dahlqvist; Linderoth, Lars; Nielsen, Hanne Mørck

    2012-01-01

    Diamino acids are commonly found in bioactive compounds, yet only few are commercially available as building blocks for solid-phase peptide synthesis. In the present work a convenient, inexpensive route to multiple-charged amino acid building blocks with varying degree of hydrophobicity...... was developed. A versatile solid-phase protocol leading to selectively protected amino alcohol intermediates was followed by oxidation to yield the desired di- or polycationic amino acid building blocks in gram-scale amounts. The synthetic sequence comprises loading of (S)-1-(p-nosyl)aziridine-2-methanol onto...... of simple neutral amino acids as well as analogs displaying high bulkiness or polycationic side chains was prepared. Two building blocks were incorporated into peptide sequences using microwave-assisted solid-phase peptide synthesis confirming their general utility....

  13. Purification and H-1 NMR spectroscopic characterization of phase II metabolites of tolfenamic acid

    DEFF Research Database (Denmark)

    Sidelmann, U. G.; Christiansen, E.; Krogh, L.

    1997-01-01

    samples obtained on days 7 to 10 from a human volunteer after oral administration of 200 mg of the drug three times per day (steady-state plasma concentration). The metabolites of tolfenamic acid were initially concentrated by preparative solid phase extraction (PSPE) chromatography, thereby removing...... the endogenous polar compounds that are present in the urine. The individual metabolites were purified by preparative high performance liquid chromatography (HPLC) and then identified using H-1 NMR, Both one- and two-dimensional NMR experiments were performed to identify the phase II metabolites of tolfenamic......), and N-(2-methyl-4-hydroxyphenyl)-anthranilic acid (11) were identified. The phase II metabolites (5-11) had not previously been identified in urine from humans administered tolfenamic acid. The phase I metabolites of the glucuronides 7, 8, 10, and 11 were identified here for the first time. An HPLC...

  14. Ferroelectric, antiferroelectric and TGB phases in lactic acid derivatives

    Czech Academy of Sciences Publication Activity Database

    Novotná, Vladimíra; Kašpar, Miroslav; Hamplová, Věra; Podoliak, Natalia; Glogarová, Milada; Pociecha, D.

    2012-01-01

    Roč. 39, č. 4 (2012), s. 477-486 ISSN 0267-8292 R&D Projects: GA ČR(CZ) GAP204/11/0723 Institutional research plan: CEZ:AV0Z10100520 Keywords : liquid crystals * lactate derivatives * TGB phases Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.959, year: 2012 http://www.tandfonline.com/doi/abs/10.1080/02678292.2011.653411

  15. Stationary and Transient Response Statistics

    DEFF Research Database (Denmark)

    Madsen, Peter Hauge; Krenk, Steen

    1982-01-01

    The covariance functions for the transient response of a linear MDOF-system due to stationary time limited excitation with an arbitrary frequency content are related directly to the covariance functions of the stationary response. For rational spectral density functions closed form expressions fo...

  16. Chaotic Bohmian trajectories for stationary states

    International Nuclear Information System (INIS)

    Cesa, Alexandre; Martin, John; Struyve, Ward

    2016-01-01

    In Bohmian mechanics, the nodes of the wave function play an important role in the generation of chaos. However, so far, most of the attention has been on moving nodes; little is known about the possibility of chaos in the case of stationary nodes. We address this question by considering stationary states, which provide the simplest examples of wave functions with stationary nodes. We provide examples of stationary wave functions for which there is chaos, as demonstrated by numerical computations, for one particle moving in three spatial dimensions and for two and three entangled particles in two dimensions. Our conclusion is that the motion of the nodes is not necessary for the generation of chaos. What is important is the overall complexity of the wave function. That is, if the wave function, or rather its phase, has a complex spatial variation, it will lead to complex Bohmian trajectories and hence to chaos. Another aspect of our work concerns the average Lyapunov exponent, which quantifies the overall amount of chaos. Since it is very hard to evaluate the average Lyapunov exponent analytically, which is often computed numerically, it is useful to have simple quantities that agree well with the average Lyapunov exponent. We investigate possible correlations with quantities such as the participation ratio and different measures of entanglement, for different systems and different families of stationary wave functions. We find that these quantities often tend to correlate to the amount of chaos. However, the correlation is not perfect, because, in particular, these measures do not depend on the form of the basis states used to expand the wave function, while the amount of chaos does. (paper)

  17. CCN activation experiments with adipic acid: effect of particle phase and adipic acid coatings on soluble and insoluble particles

    Directory of Open Access Journals (Sweden)

    S. S. Hings

    2008-07-01

    Full Text Available Slightly soluble atmospherically relevant organic compounds may influence particle CCN activity and therefore cloud formation. Adipic acid is a frequently employed surrogate for such slightly soluble organic materials. The 11 published experimental studies on the CCN activity of adipic acid particles are not consistent with each other nor do they, in most cases, agree with the Köhler theory. The CCN activity of adipic acid aerosol particles was studied over a significantly wider range of conditions than in any previous single study. The work spans the conditions of the previous studies and also provides alternate methods for producing "wet" (deliquesced solution droplets and dry adipic acid particles without the need to produce them by atomization of aqueous solutions. The experiments suggest that the scatter in the previously published CCN measurements is most likely due to the difficulty of producing uncontaminated adipic acid particles by atomization of solutions and possibly also due to uncertainties in the calibration of the instruments. The CCN activation of the small (dm<150 nm initially dry particles is subject to a deliquescence barrier, while for the larger particles the activation follows the Köhler curve. Wet adipic acid particles follow the Köhler curve over the full range of particle diameters studied. In addition, the effect of adipic acid coatings on the CCN activity of both soluble and insoluble particles has also been studied. When a water-soluble core is coated by adipic acid, the CCN-hindering effect of particle phase is eliminated. An adipic acid coating on hydrophobic soot yields a CCN active particle. If the soot particle is relatively small (dcore≤102 nm, the CCN activity of the coated particles approaches the deliquescence line of adipic acid, suggesting that the total size of the particle determines CCN activation and the soot core acts as a scaffold.

  18. Unravelling the effects of mobile phase additives in supercritical fluid chromatography. Part I: Polarity and acidity of the mobile phase.

    Science.gov (United States)

    West, Caroline; Melin, Jodie; Ansouri, Hassna; Mengue Metogo, Maïly

    2017-04-07

    The mobile phases employed in current supercritical fluid chromatography (SFC) are usually composed of a mixture of pressurized carbon dioxide and a co-solvent. The co-solvent is most often an alcohol and may contain a third component in small proportions, called an additive (acid, base or salt). The polarity of such mobile phase compositions is here re-evaluated with a solvatochromic dye (Nile Red), particularly to assess the contribution of additives. It appears that additives, when employed in usual concentration range (0.1% or 20mM) do not modify the polarity in the immediate environment of the probe. In addition, the combination of carbon dioxide and an alcohol is known to form alkoxylcarbonic acid, supposedly conferring some acidic character to SFC mobile phases. Direct measurements of the apparent pH are impossible, but colour indicators of pH can be used to define the range of apparent pH provided by carbon dioxide-alcohol mixtures, with or without additives. Five colour indicators (Thymol Blue, Bromocresol Green, Methyl Red, Bromocresol Purple, and Bromothymol Blue) were selected to provide a wide range of aqueous pK a values (from 1.7 to 8.9). UV-vis absorption spectra measured in liquid phases of controlled pH were compared to those measured with a diode-array detector employed in SFC, with the help of chemometric methods. Based on these observations, it is concluded that the apparent pH range in carbon dioxide-methanol mobile phases is close to 5. Increasing the proportion of methanol (in the course of a gradient elution for instance) causes decreasing apparent pH. Strong acids can further decrease the apparent pH below 1.7; strong bases have little influence on the apparent pH, probably because, in this range of concentrations, they are titrated by alkoxylcarbonic acid or form ion pairs with alkoxycarbonate. However, bases and salts could stabilize the acidity in the course of gradient runs. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Extraction Equilibrium of Acrylic Acid by Aqueous Two-Phase Systems Using Hydrophilic Ionic Liquids

    International Nuclear Information System (INIS)

    Lee, Yong Hwa; Lee, Woo Youn; Kim, Ki-Sub; Hong, Yeon Ki

    2014-01-01

    As an effective method for extraction of acrylic acid, aqueous two-phase systems based on morpholinium ionic liquids were used in this study. Effects of the alkyl chain length of cation in morpholinium ionic liquids on phase diagram and extraction efficiencies were investigated. Experimental results show that aqueous two phase systems can be formed by adding appropriate amount of morpholinium ionic liquids to aqueous K 2 HPO 4 solutions. It can be found that the ability of morpholinium ionic liquids for phase separation followed the order [HMMor][Br]>[OMMor][Br]>[BMMor][Br]>[EMMor][Br]. There was little difference between binodal curves of imidazolium ionic liquids and those of morpholinium ionic liquids. 50-90% of the extraction efficiency was observed for acrylic acid by aqueous two phase extraction of acrylic acid with morpholinium ionic liquids. It can be concluded that morpholinium ionic liquids/K 2 HPO 4 were effective for aqueous two phases extraction of acrylic acid comparing to imidazolium ionic liquids/K 2 HPO 4 systems because of their lower cost

  20. The binary (solid + liquid) phase diagrams of (caprylic or capric acid) + (1-octanol or 1-decanol)

    International Nuclear Information System (INIS)

    Carareto, Natália D.D.; Castagnaro, Thamires; Costa, Mariana C.; Meirelles, Antonio J.A.

    2014-01-01

    Highlights: • SLE of mixtures of caprylic acid, (capric acid + 1-octanol), 1-decanol were studied. • Experimental data were obtained through DSC and Stepscan DSC. • Systems presented eutectic and peritectic points. • Liquidus line was modeled using Margules and NRTL models. • Solid phase was modeled using the Slaughter and Doherty approach. - Abstract: In the present study the phase diagrams of four (fatty acid + fatty alcohol) binary mixtures composed of caprylic (C8O2) or capric acid (C10O2) + 1-octanol (C8OH) or 1-decanol (C10OH) were obtained by differential scanning calorimetry (DSC). Eutectic and peritectic reactions occurred in the systems. In standard DSC analyses of the (C8O2 + C10OH) and (C10O2 + C8OH) systems, an exothermic transition occurs in association with the melting of a metastable phase. A Stepscan DSC method was used in order to avoid the formation of this metastable phase during the heating of the mixtures. The approach suggested by Slaughter and Doherty (1995) [24] was used for modeling the solid phase, and the Margules 2-suffix, Margules 3-suffix and NRTL models were applied for calculating the activity coefficients of the liquid phase. The best modeling results were obtained using the Margules-3-suffix with an average deviation between experimental and calculated values ranging from T = (0.3 to 0.9) K

  1. Learning Markov models for stationary system behaviors

    DEFF Research Database (Denmark)

    Chen, Yingke; Mao, Hua; Jaeger, Manfred

    2012-01-01

    to a single long observation sequence, and in these situations existing automatic learning methods cannot be applied. In this paper, we adapt algorithms for learning variable order Markov chains from a single observation sequence of a target system, so that stationary system properties can be verified using......Establishing an accurate model for formal verification of an existing hardware or software system is often a manual process that is both time consuming and resource demanding. In order to ease the model construction phase, methods have recently been proposed for automatically learning accurate...... the learned model. Experiments demonstrate that system properties (formulated as stationary probabilities of LTL formulas) can be reliably identified using the learned model....

  2. UPS and DFT investigation of the electronic structure of gas-phase trimesic acid

    Energy Technology Data Exchange (ETDEWEB)

    Reisberg, L., E-mail: rebban@ut.ee [Institute of Physics, University of Tartu, W. Oswaldi 1, EE-50411 Tartu (Estonia); Pärna, R. [Institute of Physics, University of Tartu, W. Oswaldi 1, EE-50411 Tartu (Estonia); MAX IV Laboratory, Lund University, Fotongatan 2, 225 94 Lund (Sweden); Kikas, A.; Kuusik, I.; Kisand, V. [Institute of Physics, University of Tartu, W. Oswaldi 1, EE-50411 Tartu (Estonia); Hirsimäki, M.; Valden, M. [Surface Science Laboratory, Optoelectronics Research Centre, Tampere University of Technology, FIN-33101 Tampere (Finland); Nõmmiste, E. [Institute of Physics, University of Tartu, W. Oswaldi 1, EE-50411 Tartu (Estonia)

    2016-11-15

    Highlights: • In the current study outer valence band electronic structure of benzene-1,3,5-tricarboxylic acid was interpreted. • Experimental and calculated trimesic acid (TMA) spectrum were compared to ones of benzene and benzoic acid. • It is shown that similarities between MO energies and shapes for benzene and TMA exists. • Addition of carboxyl groups to the benzene ring clearly correlates with increasing binding energy of HOMO. - Abstract: Benzene-1,3,5-tricarboxylic acid (trimesic acid, TMA) molecules in gas-phase have been investigated by using valence band photoemission. The photoelectron spectrum in the binding energy region from 9 to 22 eV is interpreted by using density functional theory calculations. The electronic structure of TMA is compared with benzene and benzoic acid in order to demonstrate changes in molecular orbital energies induced by addition of carboxyl groups to benzene ring.

  3. Carbon nanotube stationary phases for microchip electrochromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Bøggild, Peter; Kutter, Jörg Peter

    , microfluidic devices with microfabricated carbon nanotube columns for electrochromatographic separations will be presented. The electrically conductive carbon nanotube layer has been patterned into hexoganol micropillars in order to support electroosmotic flow without forming gas bubbles from electrolysis......The use of nanomaterials in separation science has increased rapidly in the last decade. The reason for this is to take advantage of the unique properties of these materials, such as a very high surface-to-volume ratio and favourable sorbent behaviour. Carbon nanostructures, such as carbon...

  4. Investigation of solid-phase hydrogenation of amino acids and peptides

    International Nuclear Information System (INIS)

    Zolotarev, Yu.A.; Myasoedov, N.F.; Zajtsev, D.A.; Lubnin, M.Yu.; Tatur, V.Yu.; Kozik, V.S.; Dorokhova, E.M.; Rozenberg, S.N.

    1990-01-01

    The possibility of synthesizing amino acids and peptides multiply labelled with tritium or deuterium by the method of solid-phase isotopic exchange with gaseous hydrogen isotopes was verified. Establishment of the isotopic hydrogen equilibrium between the gaseous phase and the solid phase formed by the amino acid molecules was found experimentally. The activation energy of the isotopic exchange is 13 kcal/mol. A mathematical model was set up for the isotopic exchange with a probable substitution of hydrogen atoms. Uniformly labelled amino acids were obtained in a high optical purity and with 80 to 90% hydrogen substitution by deuterium and tritium. Tritiated peptides were prepared in high yields at molar activities of 1.5 to 3.7 TBq/mmol. (author). 4 tabs

  5. Impact of metabolism and growth phase on the hydrogen isotopic composition of microbial fatty acids

    Science.gov (United States)

    Heinzelmann, Sandra M.; Villanueva, Laura; Sinke-Schoen, Danielle; Sinninghe Damsté, Jaap S.; Schouten, Stefan; van der Meer, Marcel T. J.

    2015-01-01

    Microorganisms are involved in all elemental cycles and therefore it is important to study their metabolism in the natural environment. A recent technique to investigate this is the hydrogen isotopic composition of microbial fatty acids, i.e., heterotrophic microorganisms produce fatty acids enriched in deuterium (D) while photoautotrophic and chemoautotrophic microorganisms produce fatty acids depleted in D compared to the water in the culture medium (growth water). However, the impact of factors other than metabolism have not been investigated. Here, we evaluate the impact of growth phase compared to metabolism on the hydrogen isotopic composition of fatty acids of different environmentally relevant microorganisms with heterotrophic, photoautotrophic and chemoautotrophic metabolisms. Fatty acids produced by heterotrophs are enriched in D compared to growth water with εlipid/water between 82 and 359‰ when grown on glucose or acetate, respectively. Photoautotrophs (εlipid/water between −149 and −264‰) and chemoautotrophs (εlipid/water between −217 and −275‰) produce fatty acids depleted in D. Fatty acids become, in general, enriched by between 4 and 46‰ with growth phase which is minor compared to the influence of metabolisms. Therefore, the D/H ratio of fatty acids is a promising tool to investigate community metabolisms in nature. PMID:26005437

  6. [Determination of glycyrrhizinic acid in biotransformation system by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Li, Hui; Lu, Dingqiang; Liu, Weimin

    2004-05-01

    A method for determining glycyrrhizinic acid in the biotransformation system by reversed-phase high performance liquid chromatography (RP-HPLC) was developed. The HPLC conditions were as follows: Hypersil C18 column (4.6 mm i.d. x 250 mm, 5 microm) with a mixture of methanol-water-acetic acid (70:30:1, v/v) as the mobile phase; flow rate at 1.0 mL/min; and UV detection at 254 nm. The linear range of glycyrrhizinic acid was 0.2-20 microg. The recoveries were 98%-103% with relative standard deviations between 0.16% and 1.58% (n = 3). The method is simple, rapid and accurate for determining glycyrrhizinic acid.

  7. Identification of IbeR as a Stationary-Phase Regulator in Meningitic Escherichia coli K1 that Carries a Loss-of-Function Mutation in rpoS

    Directory of Open Access Journals (Sweden)

    Feng Chi

    2009-01-01

    Full Text Available IbeR is a regulator present in meningitic Escherichia coli strain E44 that carries a loss-of-function mutation in the stationary-phase (SP regulatory gene rpoS. In order to determine whether IbeR is an SP regulator in E44, two-dimensional gel electrophoresis and LC-MS were used to compare the proteomes of a noninvasive ibeR deletion mutant BR2 and its parent strain E44 in the SP. Four up-regulated (TufB, GapA, OmpA, AhpC and three down-regulated (LpdA, TnaA, OpmC proteins in BR2 were identified when compared to E44. All these proteins contribute to energy metabolism or stress resistance, which is related to SP regulation. One of the down-regulated proteins, tryptophanase (TnaA, which is regulated by RpoS in other E. coli strains, is associated with SP regulation via production of a signal molecule indole. Our studies demonstrated that TnaA was required for E44 invasion, and that indole was able to restore the noninvasive phenotype of the tnaA mutant. The production of indole was significantly reduced in BR2, indicating that ibeR is required for the indole production via tnaA. Survival studies under different stress conditions indicated that IbeR contributed to bacteria stress resistance in the SP. Taken together, IbeR is a novel regulator contributing to the SP regulation.

  8. An exceptional series of phase transitions in hydrophobic amino acids with linear side chains

    Directory of Open Access Journals (Sweden)

    Carl Henrik Görbitz

    2016-09-01

    Full Text Available The solid-state phase transitions and intermediate structures of S-2-aminobutanoic acid (l-2-aminobutyric acid, S-2-aminopentanoic acid (l-norvaline, S-2-aminohexanoic acid (l-norleucine and l-methionine between 100 and 470 K, identified by differential scanning calorimetry, have been characterized in a comprehensive single-crystal X-ray diffraction investigation. Unlike other enantiomeric amino acids investigated until now, this group featuring linear side chains displays up to five distinct phases. The multiple transitions between them involve a number of different processes: alteration of the hydrogen-bond pattern, to our knowledge the first example of this observed for an amino acid, sliding of molecular bilayers, seen previously only for racemates and quasiracemates, concerted side-chain rearrangements and abrupt as well as gradual modifications of the side-chain disorder. Ordering of l-norleucine upon cooling even proceeds via an incommensurately modulated structure. l-Methionine has previously been described as being fully ordered at room temperature. An accurate refinement now reveals extensive disorder for both molecules in the asymmetric unit, while two previously unknown phases occur above room temperature.

  9. Enhancement in extraction rates by addition of organic acids to aqueous phase in solvent extraction of rare earth metals in presence of diethylenetriaminepentaacetic acid

    International Nuclear Information System (INIS)

    Matsuyama, Hideto; Azis, A.; Fujita, Mamoru; Teramoto, Masaaki.

    1996-01-01

    It is well known that the selectivity of rare earth metals by solvent extraction is increased by the addition of a chelating agent such as diethylenetriaminepentaacetic acid (DTPA) in the aqueous phase. One of the disadvantages of this method is the decrease in extraction rates due to complexation in the aqueous phase. In this paper, further addition of organic acids to the aqueous phase was examined for the purpose of enhancing the extraction rates in solvent extraction with DTPA. The addition of several kind of organic acids such as formic acid, acetic acid, malonic acid, lactic acid and citric acid was investigated for a Er/Y separation system. A remarkable enhancement in extraction rates was observed with a slight decrease in the selectivity by the addition of citric acid or lactic acid. Extraction rates in the presence of both DTPA and citric acid increased with the increase in citric acid concentration and with the increase in proton concentration. A 150 times enhancement in extraction rates was found in the low proton concentration condition. In order to analyze the extraction rates and selectivities obtained, mass transfer equations were presented by considering both the dissociation reaction of rare earth metal-DTPA complexes and the complex formation between rare earth metal and organic acid in the aqueous phase. The experimental data were analyzed by these equations. (author)

  10. An exceptional series of phase transitions in hydrophobic amino acids with linear side chains

    Czech Academy of Sciences Publication Activity Database

    Görbitz, C.H.; Karen, P.; Dušek, Michal; Petříček, Václav

    2016-01-01

    Roč. 3, Sep (2016), s. 341-353 ISSN 2052-2525 R&D Projects: GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : amino acids * disorder * hydrogen bonding * modulated phases * phase transitions * side-chain stacking * polymorphism * molecular crystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 5.793, year: 2016

  11. Study on preparation and thermal property of binary fatty acid and the binary fatty acids/diatomite composite phase change materials

    International Nuclear Information System (INIS)

    Li, Min; Kao, Hongtao; Wu, Zhishen; Tan, Jinmiao

    2011-01-01

    This study prepared a series of binary phase change materials by mixing decanoic acid, dodecanoic acid, hexadecanoic acid and octadecanoic acid each other. The phase-transition temperature of binary fatty acid and its corresponding mixing proportion are calculated with phase diagram thermodynamic method. The results are verified by the experimental result of the heat absorption curve and the Differential Scanning Calorimetry (DSC) analysis curve. The results show that the calculation method of phase diagram thermodynamic calculation can be taken as a basis for mixing proportion of binary fatty acid phase change materials. In addition, the decanoic-dodecanoic acid/diatomite composite phase change material (PCM) are prepared and its microstructure, thermal property and thermal reliability are characterized. The result shows that the decanoic-dodecanoic acid is uniformly adsorbed into diatomite and the form-stable PCM are formed. The phase-transition temperature and the latent heat of the decanoic-dodecanoic acid/diatomite composite PCMs is 16.74 o C and 66.8114 J/g, respectively.

  12. Stable, low-cost phase change material for building applications: The eutectic mixture of decanoic acid and tetradecanoic acid

    International Nuclear Information System (INIS)

    Kahwaji, Samer; Johnson, Michel B.; Kheirabadi, Ali C.; Groulx, Dominic; White, Mary Anne

    2016-01-01

    Highlights: • Decanoic/tetradecanoic acid eutectic at 0.82 ± 0.02 mole fraction (78 ± 2 mass%) decanoic acid. • Melting of eutectic at 20.5 ± 1.5 °C, useful for building applications. • High enthalpy change, 153 ± 15 J g"−"1, is promising. • Negligible change in stability after 3000 melt–freeze cycles. - Abstract: We present a thorough characterization of the thermal properties and thermal reliability of the eutectic mixture of decanoic acid with tetradecanoic acid, as a phase change material (PCM) of potential interest for passive temperature control in buildings. From the temperature-composition binary phase diagram we found that the eutectic composition is 0.82 ± 0.02 mole fraction (78 ± 2 mass%) decanoic acid. We thoroughly characterized the thermal properties of the eutectic mixture. The eutectic composition has a high latent heat of fusion Δ_f_u_sH = 153 ± 15 J g"−"1 and a melting temperature T_o_n_s_e_t = 20.5 ± 1.5 °C. The heat capacity measured as a function of temperature for the solid and liquid phases just below and above the melting point is 1.9 and 2.1 ± 0.2 J K"−"1 g"−"1, respectively. The average value of the thermal conductivity of the solid phase measured between −33 and 9 °C is κ_s = 0.20 ± 0.02 W m"−"1 K"−"1 and for the liquid phase, the thermal conductivity is κ_l = 0.23 ± 0.03 W m"−"1 K"−"1 for 28 and 38 °C. The mixture has a good long-term thermal stability as indicated by negligible changes in Δ_f_u_sH and T_o_n_s_e_t after 3000 melt–freeze cycles. The parameters determined in this work allow more accurate modeling and optimization of the behavior of the eutectic mixture in preparation for implementation as a thermal energy storage PCM.

  13. Decontamination and inspection plan for Phase 3 closure of the 300 area waste acid treatment system

    International Nuclear Information System (INIS)

    LUKE, S.N.

    1999-01-01

    This decontamination and inspection plan (DIP) describes decontamination and verification activities in support of Phase 3 closure of the 300 Area Waste Acid Treatment System (WATS). Phase 3 is the third phase of three WATS closure phases. Phase 3 attains clean closure conditions for WATS portions of the 334 and 311 Tank Farms (TF) and the 333 and 303-F Buildings. This DIP also describes designation and management of waste and debris generated during Phase 3 closure activities. Information regarding Phase 1 and Phase 2 for decontamination and verification activities closure can be found in WHC-SD-ENV-AP-001 and HNF-1784, respectively. This DIP is provided as a supplement to the closure plan (DOE/RL-90-11). This DIP provides the documentation for Ecology concurrence with Phase 3 closure methods and activities. This DIP is intended to provide greater detail than is contained in the closure plan to satisfy Ecology Dangerous Waste Regulations, Washington Administrative Code (WAC) 173-303-610 requirement that closure documents describe the methods for removing, transporting, storing, and disposing of all dangerous waste at the unit. The decontamination and verification activities described in this DIP are based on the closure plan and on agreements reached between Ecology and the U.S. Department of Energy, Richland Operations Office (DOE-RL) during Phase 3 closure activity workshops and/or project manager meetings (PMMs)

  14. Highly Selective Liquid-Phase Benzylation of Anisole with Solid-Acid Zeolite Catalysts

    DEFF Research Database (Denmark)

    Poreddy, Raju; Shunmugavel, Saravanamurugan; Riisager, Anders

    2015-01-01

    Zeolites were evaluated as solid acid catalysts for the liquid-phase benzylation of anisole with benzyl alcohol, benzyl bromide, and benzyl chloride at 80 °C. Among the examined zeolites, H-mordenite-10 (H-MOR-10) demonstrated particular high activity (>99 %) and excellent selectivity (>96...

  15. A convenient procedure for the solid-phase synthesis of hydroxamic acids on PEGA resins

    DEFF Research Database (Denmark)

    Nandurkar, Nitin Subhash; Petersen, Rico; Qvortrup, Katrine

    2011-01-01

    An efficient method for the solid-phase synthesis of hydroxamic acids is described. The method comprises the nucleophilic displacement of esters immobilized on PEGA resins with hydroxylamine/sodium hydroxide in isopropanol. The hydroxyaminolysis protocol is compatible with a broad range of PEGA...

  16. Gas-phase salt bridge interactions between glutamic acid and arginine

    NARCIS (Netherlands)

    Jaeqx, S.; Oomens, J.; Rijs, A.M.

    2013-01-01

    The gas-phase side chain-side chain (SC-SC) interaction and possible proton transfer between glutamic acid (Glu) and arginine (Arg) residues are studied under low-temperature conditions in an overall neutral peptide. Conformation-specific IR spectra, obtained with the free electron laser FELIX, in

  17. Hydrocarbon fuels from gas phase decarboxylation of hydrolyzed free fatty acid

    KAUST Repository

    Wang, Weicheng; Roberts, William L.; Stikeleather, Larry F.

    2012-01-01

    Gas phase decarboxylation of hydrolyzed free fatty acid (FFA) from canola oil has beeninvestigated in two fix-bed reactors by changing reaction parameters such as temperatures,FFA feed rates, and H 2-to-FFA molar ratios. FFA, which contains mostly C

  18. Phase Transformation of Adefovir Dipivoxil/Succinic Acid Cocrystals Regulated by Polymeric Additives

    Directory of Open Access Journals (Sweden)

    Sungyup Jung

    2013-12-01

    Full Text Available The polymorphic phase transformation in the cocrystallization of adefovir dipivoxil (AD and succinic acid (SUC was investigated. Inspired by biological and biomimetic crystallization, polymeric additives were utilized to control the phase transformation. With addition of poly(acrylic acid, the metastable phase newly identified through the analysis of X-ray diffraction was clearly isolated from the previously reported stable form. Without additives, mixed phases were obtained even at the early stage of cocrystallization. Also, infrared spectroscopy analysis verified the alteration of the hydrogen bonding that was mainly responsible for the cocrystal formation between AD and SUC. The hydrogen bonding in the metastable phase was relatively stronger than that in the stable form, which indicated the locally strong AD/SUC coupling in the initial stage of cocrystallization followed by the overall stabilization during the phase transformation. The stronger hydrogen bonding could be responsible for the faster nucleation of the initially observed metastable phase. The present study demonstrated that the polymeric additives could function as effective regulators for the polymorph-selective cocrystallization.

  19. Selenium Derivatization of Nucleic Acids for Phase and Structure Determination in Nucleic Acid X-ray Crystallography

    Directory of Open Access Journals (Sweden)

    Zhen Huang

    2008-03-01

    Full Text Available Selenium derivatization (via selenomethionine of proteins for crystal structure determination via MAD phasing has revolutionized protein X-ray crystallography. It is estimated that over two thirds of all new crystal structures of proteins have been determined via Se-Met derivatization. Similarly, selenium functionalities have also been successfully incorporated into nucleic acids to facilitate their structure studies and it has been proved that this Se-derivatization has advantages over halogen strategy, which was usually used as a traditional method in this field. This review reports the development of site-specific selenium derivatization of nucleic acids for phase determination since the year of 2001 (mainly focus on the 2’-position of the ribose. All the synthesis of 2’-SeMe modified phosphoramidite building blocks (U, C, T, A, G and the according oligonucleotides are included. In addition, several structures of selenium contained nucleic acid are also described in this paper.

  20. Aqueous Microwave-Assisted Solid-Phase Synthesis Using Boc-Amino Acid Nanoparticles

    Directory of Open Access Journals (Sweden)

    Yoshinobu Fukumori

    2013-07-01

    Full Text Available We have previously developed water-based microwave (MW-assisted peptide synthesis using Fmoc-amino acid nanopaticles. It is an organic solvent-free, environmentally friendly method for peptide synthesis. Here we describe water-based MW-assisted solid-phase synthesis using Boc-amino acid nanoparticles. The microwave irradiation allowed rapid solid-phase reaction of nanoparticle reactants on the resin in water. We also demonstrated the syntheses of Leu-enkephalin, Tyr-Gly-Gly-Phe-Leu-OH, and difficult sequence model peptide, Val-Ala-Val-Ala-Gly-OH, using our water-based MW-assisted protocol with Boc-amino acid nanoparticles.

  1. Noise Diagnostics of Stationary and Non-Stationary Reactor Processes

    Energy Technology Data Exchange (ETDEWEB)

    Sunde, Carl

    2007-04-15

    This thesis concerns the application of noise diagnostics on different problems in the area of reactor physics involving both stationary and non-stationary core processes. Five different problems are treated, divided into three different parts. The first problem treated in the first part is the classification of two-phase flow regimes from neutron radiographic and visible light images with a neuro-wavelet algorithm. The algorithm consists of wavelet pre-processing and of an artificial neural network. The result indicates that the wavelet pre-processing is improving the training of the neural network. Next, detector tubes which are suspected of impacting on nearby fuel-assemblies in a boiling water reactor (BWR) are identified by both a classical spectral method and wavelet-based methods. It was found that there is good agreement between the different methods as well as with visual inspections of detector tube and fuel assembly damage made during the outage at the plant. The third problem addresses the determination of the decay ratio of a BWR from the auto-correlation function (ACF). Here wavelets are used, with some success, both for de-trending and de-nosing of the ACF and also for direct estimation of the decay ratio from the ACF. The second part deals with the analysis of beam-mode and shell-mode core-barrel vibrations in pressurised water reactors (PWRs). The beam-mode vibrations are analysed by using parameters of the vibration peaks, in spectra from ex core detectors. A trend analysis of the peak amplitude shows that the peak amplitude is changing during the fuel cycle. When it comes to the analysis of the shell-mode vibration, 1-D analytical and numerical calculations are performed in order to calculate the neutron noise induced in the core. The two calculations are in agreement and show that a large local noise component is present in the core which could be used to classify the shell-mode vibrations. However, a measurement made in the PWR Ringhals-3 shows

  2. Noise Diagnostics of Stationary and Non-Stationary Reactor Processes

    International Nuclear Information System (INIS)

    Sunde, Carl

    2007-01-01

    This thesis concerns the application of noise diagnostics on different problems in the area of reactor physics involving both stationary and non-stationary core processes. Five different problems are treated, divided into three different parts. The first problem treated in the first part is the classification of two-phase flow regimes from neutron radiographic and visible light images with a neuro-wavelet algorithm. The algorithm consists of wavelet pre-processing and of an artificial neural network. The result indicates that the wavelet pre-processing is improving the training of the neural network. Next, detector tubes which are suspected of impacting on nearby fuel-assemblies in a boiling water reactor (BWR) are identified by both a classical spectral method and wavelet-based methods. It was found that there is good agreement between the different methods as well as with visual inspections of detector tube and fuel assembly damage made during the outage at the plant. The third problem addresses the determination of the decay ratio of a BWR from the auto-correlation function (ACF). Here wavelets are used, with some success, both for de-trending and de-nosing of the ACF and also for direct estimation of the decay ratio from the ACF. The second part deals with the analysis of beam-mode and shell-mode core-barrel vibrations in pressurised water reactors (PWRs). The beam-mode vibrations are analysed by using parameters of the vibration peaks, in spectra from ex core detectors. A trend analysis of the peak amplitude shows that the peak amplitude is changing during the fuel cycle. When it comes to the analysis of the shell-mode vibration, 1-D analytical and numerical calculations are performed in order to calculate the neutron noise induced in the core. The two calculations are in agreement and show that a large local noise component is present in the core which could be used to classify the shell-mode vibrations. However, a measurement made in the PWR Ringhals-3 shows

  3. Solid-phase extraction of galloyl- and caffeoylquinic acids from natural sources (Galphimia glauca and Arnicae flos) using pure zirconium silicate and bismuth citrate powders as sorbents inside micro spin columns.

    Science.gov (United States)

    Hussain, Shah; Schönbichler, Stefan A; Güzel, Yüksel; Sonderegger, Harald; Abel, Gudrun; Rainer, Matthias; Huck, Christian W; Bonn, Günther K

    2013-10-01

    Galloyl- and caffeoylquinic acids are among the most important pharmacological active groups of natural compounds. This study describes a pre-step in isolation of some selected representatives of these groups from biological samples. A selective solid-phase extraction (SPE) method for these compounds may help assign classes and isomer designations within complex mixtures. Pure zirconium silicate and bismuth citrate powders (325 mesh) were employed as two new sorbents for optimized SPE of phenolic acids. These sorbents possess electrostatic interaction sites which accounts for additional interactions for carbon acid moieties as compared to hydrophilic and hydrophobic sorbents alone. Based on this principle, a selective SPE method for 1,3,4,5-tetragalloylquinic acid (an anti-HIV and anti-asthamatic agent) as a starting compound was developed and then deployed upon other phenolic acids with success. The recoveries and selectivities of both sorbents were compared to most commonly applied and commercially available sorbents by using high performance liquid chromatography. The nature of interaction between the carrier sorbent and the acidic target molecules was investigated by studying hydrophilic (silica), hydrophobic (C18), mixed-mode (ionic and hydrophobic: Oasis(®) MAX) and predominantly electrostatic (zirconium silicate) materials. The newly developed zirconium silicate and bismuth citrate stationary phases revealed promising results for the selective extraction of galloyl- and caffeoylquinic acids from natural sources. It was observed that zirconium silicate exhibited maximum recovery and selectivity for tetragalloylquinic acid (84%), chlorogenic acid (82%) and dicaffeoylquinic acid (94%) among all the tested sorbents. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Graphene oxide for solid-phase extraction of bioactive phenolic acids.

    Science.gov (United States)

    Hou, Xiudan; Wang, Xusheng; Sun, Yingxin; Wang, Licheng; Guo, Yong

    2017-05-01

    A solid-phase extraction (SPE) method for the efficient analysis of trace phenolic acids (PAs, caffeic acid, ferulic acid, protocatechuic acid, cinnamic acid) in urine was established. In this work, a graphene oxide (GO) coating was grafted onto pure silica to be investigated as SPE material. The prepared GO surface had a layered and wrinkled structure that was rough and well organized, which could provide more open adsorption sites. Owing to its hydrophilicity and polarity, GO showed higher extraction efficiency toward PAs than reduced GO did, in agreement with the theoretical calculation results performed by Gaussian 09 software. The adsorption mechanism of PAs on GO@Sil was also investigated through static state and kinetic state adsorption experiments, which showed a monolayer surface adsorption. Extraction capacity of the as-prepared material was optimized using the response surface methodology. Under the optimized conditions, the as-established method provided wide linearity range (2-50 μg L -1 for protocatechuic acid and 1-50 μg L -1 for caffeic acid, ferulic acid, and cinnamic acid) and low limits of detection (0.25-1 μg L -1 ). Finally, the established method was applied for the analysis of urine from two healthy volunteers. The results indicate that the prepared material is a practical, cost-effective medium for the extraction and determination of phenolic acids in complex matrices. Graphical Abstract A graphene oxide coating was grafted onto pure silica as the SPE material for the extraction of phenolic acids in urines and the extraction mechanism was also mainly investigated.

  5. Liquid-liquid phase separation in internally mixed magnesium sulfate/glutaric acid particles

    Science.gov (United States)

    Wu, Feng-Min; Wang, Xiao-Wei; Jing, Bo; Zhang, Yun-Hong; Ge, Mao-Fa

    2018-04-01

    The confocal Raman microscopy is utilized to investigate the liquid-liquid phase separation (LLPS) of mixed magnesium sulfate/glutaric acid (MgSO4/GA) droplets deposited on a hydrophobic polytetrafluoroethylene (PTFE) substrate and a hydrophilic quartz substrate. Raman spectra collected from different regions of the mixed droplets provide detailed information of component distributions for MgSO4 and GA. During the dehydration process, the MgSO4/GA mixed particles show the initial liquid-liquid phase separation between 85% and 80% relative humidity (RH) on both the hydrophobic and hydrophilic substrates. For the droplets deposited on the two substrates, the inner phase of droplets is dominated by aqueous MgSO4, which is surrounded by a rich GA organic layer due to the surface tension effects. In addition, the crystallization of GA could be observed in the organic aqueous phase while it is inhibited in the inner MgSO4 phase due to the effects of gel formation of MgSO4 at low RH. The Raman spectra reveal that with decreasing RH the morphology of the mixed droplet evolves from a uniform droplet to the structure of LLPS with the GA crystallizing in the outer layer and MgSO4 gel formed in the inner phase. These findings contribute to the further understanding of the role of interactions between inorganic salts and organic acids on the morphological evolution and environmental effects of atmospheric aerosols under ambient RH conditions.

  6. Determination and modeling of binary and ternary solid-liquid phase equilibrium for the systems formed by 3,5-dinitrobenzoic acid, m-nitrobenzoic acid and acetone

    International Nuclear Information System (INIS)

    Li, Xinbao; Du, Cunbin; Zhao, Hongkun

    2017-01-01

    Highlights: • The solubility of 3,5-dinitrobenzoic acid in acetone was determined. • Solubility of m-nitrobenzoic acid + 3,5-dinitrobenzoic acid + acetone was determined. • Three ternary phase diagrams were constructed for the ternary system. • The ternary phase diagrams were calculated by Wilson model and NRTL model. - Abstract: The solubility of 3,5-dinitrobenzoic acid in acetone at the temperatures ranging from (283.15 to 318.15) K and the mutual solubility of the ternary m-nitrobenzoic acid + 3,5-dinitrobenzoic acid + acetone system at (283.15, 298.15 and 313.15) K were determined experimentally by using the isothermal saturation method under atmosphere pressure (101.2 kPa). Three isothermal ternary phase diagrams were constructed according to the measured mutual solubility data. In each ternary phase diagram, there was one co-saturated point, two boundary curves, and three crystalline regions. The modified Apelblat equation, λh equation, NRTL model and Wilson model were used to correlate the solubility of 3,5-dinitrobenzoic acid in acetone; and the NRTL and Wilson models, the mutual solubility for the ternary m-nitrobenzoic acid + 3,5-dinitrobenzoic acid + acetone system. The value of root-mean-square deviation (RMSD) was 8.53 × 10 −4 for the binary system of 3,5-dinitrobenzoic acid + acetone; and the largest value of RMSD was 81.08 × 10 −4 for the ternary system.

  7. In-house SIRAS phasing of the polyunsaturated fatty-acid isomerase from Propionibacterium acnes

    International Nuclear Information System (INIS)

    Liavonchanka, Alena; Hornung, Ellen; Feussner, Ivo; Rudolph, Markus

    2006-01-01

    Low iodide concentrations were sufficient to allow SAD and SIRAS phasing of cubic crystals of a novel fatty acid isomerase using Cu Kα radiation. The polyenoic fatty-acid isomerase from Propionibacterium acnes (PAI) catalyzes the double-bond isomerization of linoleic acid to conjugated linoleic acid, which is a dairy- or meat-derived fatty acid in the human diet. PAI was overproduced in Escherichia coli and purified to homogeneity as a yellow-coloured protein. The nature of the bound cofactor was analyzed by absorption and fluorescence spectroscopy. Single crystals of PAI were obtained in two crystal forms. Cubic shaped crystals belong to space group I2 1 3, with a unit-cell parameter of 160.4 Å, and plate-like crystals belong to the monoclinic space group C2, with unit-cell parameters a = 133.7, b = 60.8, c = 72.2 Å, β = 115.8°. Both crystal forms contain one molecule per asymmetric unit and diffract to a resolution of better than 2.0 Å. Initial phases were obtained by SIRAS from in-house data from a cubic crystal that was soaked with an unusually low KI concentration of 0.25 M

  8. Effect of dimethylamine on the gas phase sulfuric acid concentration measured by Chemical Ionization Mass Spectrometry

    CERN Document Server

    Rondo, L.; Kürten, A.; Adamov, A.; Bianchi, F.; Breitenlechner, M.; Duplissy, J.; Franchin, A.; Dommen, J.; Donahue, N. M.; Dunne, E. M.; Flagan, R. C.; Hakala, J.; Hansel, A.; Keskinen, H.; Kim, J.; Jokinen, T.; Lehtipalo, K.; Leiminger, M.; Praplan, A.; Riccobono, F.; Rissanen, M. P.; Sarnela, N.; Schobesberger, S.; Simon, M.; Sipilä, M.; Smith, J. N.; Tomé, A.; Tröstl, J.; Tsagkogeorgas, G.; Vaattovaara, P.; Winkler, P. M.; Williamson, C.; Wimmer, D.; Baltensperger, U.; Kirkby, J.; Kulmala, M.; Petäjä, T.; Worsnop, D. R.; Curtius, J.

    2016-01-01

    Sulfuric acid is widely recognized as a very important substance driving atmospheric aerosolnucleation. Based on quantum chemical calculations it has been suggested that the quantitative detectionof gas phase sulfuric acid (H2SO4) by use of Chemical Ionization Mass Spectrometry (CIMS) could be biased inthe presence of gas phase amines such as dimethylamine (DMA). An experiment (CLOUD7 campaign) was setup at the CLOUD (Cosmics Leaving OUtdoor Droplets) chamber to investigate the quantitative detection ofH2SO4in the presence of dimethylamine by CIMS at atmospherically relevant concentrations. For the first time inthe CLOUD experiment, the monomer sulfuric acid concentration was measured by a CIMS and by two CI-APi-TOF(Chemical Ionization-Atmospheric Pressure interface-Time Of Flight) mass spectrometers. In addition, neutralsulfuric acid clusters were measured with the CI-APi-TOFs. The CLOUD7 measurements show that in the presenceof dimethylamine (<5 to 70 pptv) the sulfuric acid monomer measured by the CIMS...

  9. Impact of the updating scheme on stationary states of networks

    International Nuclear Information System (INIS)

    Radicchi, F; Ahn, Y Y; Meyer-Ortmanns, H

    2008-01-01

    From Boolean networks it is well known that the number of attractors as a function of the system size depends on the updating scheme which is chosen either synchronously or asynchronously. In this contribution, we report on a systematic interpolation between synchronous and asynchronous updating in a one-dimensional chain of Ising spins. The stationary state for fully synchronous updating is antiferromagnetic. The interpolation allows us to locate a phase transition between phases with an absorbing and a fluctuating stationary state. The associated universality class is that of parity conservation. We also report on a more recent study of asynchronous updates applied to the yeast cell-cycle network. Compared to the synchronous update, the basin of attraction of the largest attractor considerably shrinks and the convergence to the biological pathway slows down and is less dominant. Both examples illustrate how sensitively the stationary states and the properties of attractors can depend on the updating mode of the algorithm

  10. Phase equilibria in a system of aqueous arginine with an octane solution of sulfonic acid

    Science.gov (United States)

    Kuvaeva, Z. I.; Koval'chuk, I. V.; Vodop'yanova, L. A.; Soldatov, V. S.

    2013-05-01

    The extraction of arginine (Arg) from aqueous salt (0.1 M NaCl) solutions with a sulfo extractant in a wide range of pH values and amino acid concentrations was studied. The 0.1 M solution of dinonylnaphthalenesulfonic acid (HD) in octane was used as an extractant. The degree of extraction was found to be high at pH 0.8-9.0. This can be explained by the effect of additional intermolecular interactions in the extractant phase involving the guanidine group of Arg.

  11. The stationary neutron radiography system

    International Nuclear Information System (INIS)

    Weeks, A.A.; Newell, D.L.; Heidel, C.C.

    1990-01-01

    To provide the high intensity neutron beam and support systems necessary for radiography, the Stationary Neutron Radiography System was constructed at McClellan Air Force Base. The Stationary Neutron Radiography System utilizes a one megawatt TRIGA reactor contained in an Aluminium tank surrounded by eight foot thick concrete walls. There are four neutron beam tubes at inclined angles from the reactor core to separate radiography bays. In three of the bays, robotic systems manipulate aircraft components in the neutron beam, while real-time imaging systems provide images concurrent with the irradiation. Film radiography of smaller components is performed in the remaining bay

  12. Fatty acid synthase inhibition triggers apoptosis during S phase in human cancer cells.

    Science.gov (United States)

    Zhou, Weibo; Simpson, P Jeanette; McFadden, Jill M; Townsend, Craig A; Medghalchi, Susan M; Vadlamudi, Aravinda; Pinn, Michael L; Ronnett, Gabriele V; Kuhajda, Francis P

    2003-11-01

    C75, an inhibitor of fatty acid synthase (FAS), induces apoptosis in cultured human cancer cells. Its proposed mechanism of action linked high levels of malonyl-CoA after FAS inhibition to potential downstream effects including inhibition of carnitine palmitoyltransferase-1 (CPT-1) with resultant inhibition of fatty acid oxidation. Recent data has shown that C75 directly stimulates CPT-1 increasing fatty acid oxidation in MCF-7 human breast cancer cells despite inhibitory concentrations of malonyl-CoA. In light of these findings, we have studied fatty acid metabolism in MCF7 human breast cancer cells to elucidate the mechanism of action of C75. We now report that: (a) in the setting of increased fatty acid oxidation, C75 inhibits fatty acid synthesis; (b) C273, a reduced form of C75, is unable to inhibit fatty acid synthesis and is nontoxic to MCF7 cells; (c) C75 and 5-(tetradecyloxy)-2-furoic acid (TOFA), an inhibitor of acetyl-CoA carboxylase, both cause a significant reduction of fatty acid incorporation into phosphatidylcholine, the major membrane phospholipid, within 2 h; (d) pulse chase studies with [(14)C]acetate labeling of membrane lipids show that both C75 and TOFA accelerate the decay of (14)C-labeled lipid from membranes within 2 h; (e) C75 also promotes a 2-3-fold increase in oxidation of membrane lipids within 2 h; and (f) because interference with phospholipid synthesis during S phase is known to trigger apoptosis in cycling cells, we performed double-labeled terminal deoxynucleotidyltransferase-mediated nick end labeling and BrdUrd analysis with both TOFA and C75. C75 triggered apoptosis during S phase, whereas TOFA did not. Moreover, application of TOFA 2 h before C75 blocked the C75 induced apoptosis, whereas etomoxir did not. Taken together these data indicate that FAS inhibition and its downstream inhibition of phospholipid production is a necessary part of the mechanism of action of C75. CPT-1 stimulation does not likely play a role in the

  13. Ammonium fluoride as a mobile phase additive in aqueous normal phase chromatography.

    Science.gov (United States)

    Pesek, Joseph J; Matyska, Maria T

    2015-07-03

    The use of ammonium fluoride as a mobile phase additive in aqueous normal phase chromatography with silica hydride-based stationary phases and mass spectrometry detection is evaluated. Retention times, peak shape, efficiency and peak intensity are compared to the more standard additives formic acid and ammonium formate. The test solutes were NAD, 3-hydroxyglutaric acid, α-ketoglutaric acid, p-aminohippuric acid, AMP, ATP, aconitic acid, threonine, N-acetyl carnitine, and 3-methyladipic acid. The column parameters are assessed in both the positive and negative ion detection modes. Ammonium fluoride is potentially an aggressive mobile phase additive that could have detrimental effects on column lifetime. Column reproducibility is measured and the effects of switching between different additives are also tested. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Quantification and speciation of volatile fatty acids in the aqueous phase.

    Science.gov (United States)

    Lee, Jechan; Kim, Jieun; Oh, Jeong-Ik; Lee, Sang-Ryong; Kwon, Eilhann E

    2017-11-01

    This study lays great emphasis on establishing a reliable analytical platform to quantify and specify volatile fatty acids (VFAs) in the aqueous phase by derivatizing VFAs into their corresponding alkyl esters via thermally-induced rapid esterification (only 10 s reaction time). To this end, reaction conditions for the thermally-induced rapid esterification are optimized. A volumetric ratio of 0.5 at 400 °C for VFA/methanol is identified as the optimal reaction conditions to give ∼90% volatile fatty acid methyl ester (VFAME) yield. To maintain a high yield of VFAMEs, this study suggests that dilution of the sample to an optimum concentration (∼500 ppm for each VFA) is required. Derivatization of VFAs into VFAMEs via the thermally-induced rapid esterification is more reliable to quantify and specify VFAs in the aqueous phase than conventional colorimetric method. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Tritium distribution ratios between the 30 % tributyl phosphate(TBP)-normal dodecane(nDD) organic phase and uranyl nitrate-nitric acid aqueous phase

    International Nuclear Information System (INIS)

    Fujine, Sachio; Uchiyama, Gunzou; Sugikawa, Susumu; Maeda, Mitsuru; Tsujino, Takeshi.

    1989-10-01

    Tritium distribution ratios between the organic and aqueous phases were measured for the system of 30 % tributyl phosphate(TBP)-normal dodecane(nDD)/uranyl nitrate-nitric acid water. It was confirmed that tritium is extracted by TBP into the organic phase in both chemical forms of tritiated water (HTO) and tritiated nitric acid (TNO 3 ). The value of tritium distribution ratio ranged from 0.002 to 0.005 for the conditions of 0-6 mol/L nitric acid, 0.5-800 mCi/L tritium in aqueous phase, and 0-125 g-U/L uranium in organic phase. Isotopic distribution coefficient of tritium between the organic and aqueous phases was observed to be about 0.95. (author)

  16. Thermodynamic study of phase transitions in methyl esters of ortho- meta- and para-aminobenzoic acids

    International Nuclear Information System (INIS)

    Almeida, Ana R.R.P.; Monte, Manuel J.S.

    2012-01-01

    Highlights: ► Vapor pressures of liquid and crystalline phases of methyl esters of the aminobenzoic acids were measured. ► Accurate values of enthalpies of sublimation, vaporization, and fusion were derived. ► The enthalpy of intermolecular NH–O hydrogen bonds in methyl p-aminobenzoate was determined. ► The volatility of the methyl benzoates was compared with the volatility of the parent acids. - Abstract: A static method based on capacitance gauges was used to measure the vapor pressures of the condensed phases of the methyl esters of the three aminobenzoic acids. For methyl o-aminobenzoate the vapor pressures of the liquid phase were measured in the range (285.4 to 369.5) K. For the meta and para isomers vapor pressures of both crystalline and liquid phases were measured in the ranges (308.9 to 376.6) K, and (332.9 to 428.0) K, respectively. Vapor pressures of the latter compound were also measured using the Knudsen effusion method in the temperature range (319.1 to 341.2) K. From the dependence of the vapor pressures on the temperature, the standard molar enthalpies and entropies of sublimation and of vaporization were derived. Differential scanning calorimetry was used to measure the temperatures and molar enthalpies of fusion of the three isomers. The results enabled the estimation of the enthalpy of the intermolecular (N−H … O) hydrogen bond in the crystalline methyl p-aminobenzoate. A correlation relating the temperature of fusion and the enthalpy and Gibbs energy of sublimation of benzene, methyl benzoates and benzoic acids was derived.

  17. Phase distribution of ecologically controlled chemical elements in production of extraction phosphoric acid

    International Nuclear Information System (INIS)

    Kazak, V.G.; Agnelov, A.I.; Zajtsev, P.M.

    1995-01-01

    Content of 16 ecologically controlled chemical element (among them Cd, Sr, Th, U, V, Y) in solid and liquid phases of extraction phosphorus acid (EPA) production is determined. These elements are recommended to control by Scientific research institute of human ecology and environment to establish their extraction coefficients to phosphogypsum and EPA and optimal variant of production of ecologically sate phosphorus fertilizers. X-ray fluorescent, atomic-absorption and polarographic methods are used for analysis these elements

  18. Stationary measure in the multiverse

    International Nuclear Information System (INIS)

    Linde, Andrei; Vanchurin, Vitaly; Winitzki, Sergei

    2009-01-01

    We study the recently proposed ''stationary measure'' in the context of the string landscape scenario. We show that it suffers neither from the ''Boltzmann brain'' problem nor from the ''youngness'' paradox that makes some other measures predict a high CMB temperature at present. We also demonstrate a good performance of this measure in predicting the results of local experiments, such as proton decay

  19. Online analytical investigations on solvent-, temperature- and water vapour-induced phase transformations of citric acid

    Energy Technology Data Exchange (ETDEWEB)

    Helmdach, L.; Ulrich, J. [Martin-Luther-Universitaet Halle-Wittenberg, Zentrum fuer Ingenieurwissenschaft, Verfahrenstechnik/TVT, Halle (Saale) (Germany); Feth, M.P. [Sanofi-Aventis Deutschland GmbH, Chemical and Process Development Frankfurt Chemistry, Frankfurt (Germany)

    2012-09-15

    It was demonstrated exemplarily for the crystallization of citric acid that the usage of an ultrasound device as well as Raman spectroscopy enables the inline measurement and the control of phase transitions. The influence of different solvent compositions (water and ethanol-water) on the crystallization of citric acid was investigated. By increasing the ethanol content the transformation point was shifted towards higher temperatures. In addition, a strong impact on the nucleation point as well as on the crystal habit was detected in ethanol-water mixtures. The results lead to the assumption that a citric acid solvate exists, which is, however, highly unstable upon isolation from mother liquor and converts fast into the known anhydrate or monohydrate forms of citric acid. The presence of such a solvate, however, could not be proven during this study. Furthermore, factors such as temperature and humidity which might influence the phase transition of the solid product were analyzed by Hotstage-Raman Spectroscopy and Water Vapor Sorption Gravimetry-Dispersive Raman Spectroscopy. Both, temperature as well as humidity show a strong influence on the behaviour of CAM. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  20. Solid phase extraction of uranium from phosphoric acid. Kinetic and thermodynamic study

    Energy Technology Data Exchange (ETDEWEB)

    Abdel-Magied, Ahmed Fawzy [Nuclear Materials Authority, Cairo (Egypt); Stockholm Univ. (Sweden). Dept. of Organic Chemistry

    2017-07-01

    There is a high interest to develop suitable solid phase extractants for uranium separation from aqueous solutions in order to reduce cost and enhance the efficiency. This paper describes solid phase extraction of uranium(VI) from aqueous phosphoric acid solution using MCM-41 based D2HEPA-TOPO organophosphorous extractants. The mixture of D2HEPA (di-2-ethyl-hexylphosphoric acid) and TOPO (tri-n-octylphosphine oxide) was impregnated into the pores of MCM-41 and the synthesized sorbent was fully characterized. The influences of different factors such as synergistic mixture ratio, phosphoric acid concentration, mixing time and temperature were investigated. The results showed that 90% of uranium(VI) extraction can be achieved within 5 min, using D2HEPA-TOPO rate at MCM-41 (mass ratio 2:1 w/w) from 1 M phosphoric acid containing 64 ppm of uranium at room temperature. High adsorption capacity of uranium(VI) have been achieved at the mentioned conditions. The rate constant for the chemical adsorption of uranium(VI) was 0.988 g mg{sup -1} min{sup -1} calculated by the pseudo-second order rate equation. The obtained thermodynamics parameters showed that uranium(VI) adsorption from H{sub 3}PO{sub 4} is an exothermic and spontaneous process.

  1. Adhesion of glucosyltransferase phase variants to Streptococcus gordonii bacterium-glucan substrata may involve lipoteichoic acid.

    Science.gov (United States)

    Vickerman, M M; Jones, G W

    1992-10-01

    Growing Streptococcus gordonii Spp+ phase variants, which have normal levels of glucosyltransferase (GTF) activity, use sucrose to promote their accumulation on surfaces by forming a cohesive bacterium-insoluble glucan polymer mass (BPM). Spp- phase variants, which have lower levels of GTF activity, do not form BPMs and do not remain in BPMs formed by Spp+ cells when grown in mixed cultures. To test the hypothesis that segregation of attached Spp+ and unattached Spp- cells was due to differences in adhesiveness, adhesion between washed, [3H]thymidine-labeled cells and preformed BPM substrata was measured. Unexpectedly, the results showed that cells of both phenotypes, as well as GTF-negative cells, attached equally well to preformed BPMs, indicating that attachment to BPMs was independent of cell surface GTF activity. Initial characterization of this binding interaction suggested that a protease-sensitive component on the washed cells may be binding to lipoteichoic acids sequestered in the BPM, since exogenous lipoteichoic acid inhibited adhesion. Surprisingly, the adhesion of both Spp+ and Spp- cells was markedly inhibited in the presence of sucrose, which also released lipoteichoic acid from the BPM. These in vitro findings suggest that, in vivo, sucrose and lipoteichoic acid may modify dental plaque development by enhancing or inhibiting the attachment of additional bacteria.

  2. Retention prediction and hydrophobicity estimation of weak acidic compounds by reversed-phase liquid chromatography using acetic and perchloric acids as ion suppressors.

    Science.gov (United States)

    Han, Shu-ying; Ming, Xin; Qi, Zheng-chun; Sheng, Dong; Lian, Hong-zhen

    2010-11-01

    Simple acids are usually applied to suppress the ionization of weakly ionizable acidic analytes in reversed-phase liquid chromatography. The purpose of this study is to investigate the retention behavior of various weak acidic compounds (monoprotic, diprotic, triprotic, and tetraprotic acids) using acetic or perchloric acid as ion suppressor in a binary hydroorganic mobile phase. The apparent n-octanol-water partition coefficient (K(ow)") was proposed to calibrate the n-octanol-water partition coefficient (K(ow)) of weak acidic compound. LogK(ow)" was found to have a better linear correlation with logk(w), the logarithm of the retention factor obtained by extrapolating to neat aqueous fraction of the mobile phase, for all weakly ionizable acidic compounds. This straightforward relationship offers a potential medium for direct measurement of K(ow) data of weak acidic analytes and can be used to predict retention behavior of these compounds in the ion suppression reversed-phase liquid chromatographic mode.

  3. 新型靛红衍生化β-环糊精键合SBA-15液相色谱固定相的制备与表征%Preparation and Characterization of a Novel Isatin Derivative of β-Cyclodextrin-bonded SBA-15 Stationary Phase for HPLC

    Institute of Scientific and Technical Information of China (English)

    张杨; 李来生; 程彪平; 周仁丹; 聂桂珍

    2014-01-01

    for HPLC. Its chemical and physical parameters were characterized by infrared spectroscopy, mass spectroscopy, elemental analysis, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and BET specific surface area analysis. The basic chromatographic property of ISCDP was evaluated by using polar halogenated uracils and disubstituted benzene positional isomers as solute probes in reversed-phase chromatography. ISCDP was also used to enantioseparate twoβ-blocker drugs in polar organic mode and two dansyl amino acids in reversed-phase mode, respectively. The related chromatographic separation mechanism was also discussed. Above studies were expected to provide experimental basis for the practical application of ISCDP in the future. The results showed that the introduction of isatin indole ring could enhanced the reversed-phase chromatographic separation ability of ISCDP for halogenated uracils within 7 min. The new packing also exhibited high stereoselectivity for the position isomers of nitroaniline, aminophenol and benzenediol, in which the para isomers were finally eluted due to strong inclusion interaction between the isatin derivative of β-cyclodextrin ligand and the isomers. Meanwhile, the introduction of isatin indole ring could also improve the chiral separation ability of ISCDP. For example the fast enantioseparations of chiral β-adrenergic blockers and dansyl-amino acids on ISCDP were achieved within 20 min (Rs>1. 3). Obviously, besides hydrophobicity, various synergistic interactions could enhance the separation selectivities of the new stationary phase for chiral and achiral analytes, including dipole-dipole, hydrogen bonding,π-π and inclusion interactions. The ordered pore structure of SBA-15 facilitated to fast and efficient separation and analysis for drugs with good permeability and low mass transfer resistance.

  4. Construção de câmara de luz ultravioleta para fotopolimerização de fases estacionárias monolíticas Coinstruction of ultraviolet-light chamber for monolithic stationary phases photo-polymerization

    Directory of Open Access Journals (Sweden)

    Fernando Antonio Simas Vaz

    2008-01-01

    Full Text Available The assembly of a photochemical reactor with six fluorescent lamps, used for photopolymerizations is described. This chamber presents a mobile support, allowing the placement of samples at different heights and a safety lock that interrupts the radiation, if it is opened during operation. The mirrored internal walls avoid the dispersion and non-uniform distribution of light. There is no high heating because the own character of the used lamps. All parts could be purchased in commerce with less than U$ 150,00. This reactor was successfully used for monolithic stationary phase photopolymerization.

  5. Virtual Stationary Automata for Mobile Networks

    National Research Council Canada - National Science Library

    Dolev, Shlomi; Gilbert, Seth; Lahiani, Limor; Lynch, Nancy; Nolte, Tina

    2005-01-01

    We define a programming abstraction for mobile networks called the Virtual Stationary Automata programming layer, consisting of real mobile clients, virtual timed I/O automata called virtual stationary automata (VSAs...

  6. Enhanced detection of amino acids in hydrophilic interaction chromatography electrospray tandem mass spectrometry with carboxylic acids as mobile phase additives.

    Science.gov (United States)

    Yin, Dengyang; Hu, Xunxiu; Liu, Dantong; Du, Wencheng; Wang, Haibo; Guo, Mengzhe; Tang, Daoquan

    2017-06-01

    Liquid chromatography coupled with mass spectrometry technique has been widely used in the analysis of biological targets such as amino acids, peptides, and proteins. In this work, eight common single carboxylic acids or diacids, which contain different pKa have been investigated as the additives to the analysis of amino acids. As the results, carboxylic acid additive can improve the signal intensity of acidity amino acids such as Asp and Glu and the chromatographic separation of basic amino acids such as Arg, His, and Lys. In particular, the diacids have better performance than single acids. The proposed mechanism is that the diacid has hydrogen bond interaction with amino acids to reduce their polarity/amphiprotic characteristics. Besides, oxalic acid has been found having better enhancement than phthalic acid by overall consideration. Therefore, we successfully quantified the 15 amino acids in Sepia bulk pharmaceutical chemical by using oxalic acid as the additive.

  7. Syntrophic acetate oxidation in two-phase (acid-methane) anaerobic digesters.

    Science.gov (United States)

    Shimada, T; Morgenroth, E; Tandukar, M; Pavlostathis, S G; Smith, A; Raskin, L; Kilian, R E

    2011-01-01

    The microbial processes involved in two-phase anaerobic digestion were investigated by operating a laboratory-scale acid-phase (AP) reactor and analyzing two full-scale, two-phase anaerobic digesters operated under mesophilic (35 °C) conditions. The digesters received a blend of primary sludge and waste activated sludge (WAS). Methane levels of 20% in the laboratory-scale reactor indicated the presence of methanogenic activity in the AP. A phylogenetic analysis of an archaeal 16S rRNA gene clone library of one of the full-scale AP digesters showed that 82% and 5% of the clones were affiliated with the orders Methanobacteriales and Methanosarcinales, respectively. These results indicate that substantial levels of aceticlastic methanogens (order Methanosarcinales) were not maintained at the low solids retention times and acidic conditions (pH 5.2-5.5) of the AP, and that methanogenesis was carried out by hydrogen-utilizing methanogens of the order Methanobacteriales. Approximately 43, 31, and 9% of the archaeal clones from the methanogenic phase (MP) digester were affiliated with the orders Methanosarcinales, Methanomicrobiales, and Methanobacteriales, respectively. A phylogenetic analysis of a bacterial 16S rRNA gene clone library suggested the presence of acetate-oxidizing bacteria (close relatives of Thermacetogenium phaeum, 'Syntrophaceticus schinkii,' and Clostridium ultunense). The high abundance of hydrogen consuming methanogens and the presence of known acetate-oxidizing bacteria suggest that acetate utilization by acetate oxidizing bacteria in syntrophic interaction with hydrogen-utilizing methanogens was an important pathway in the second-stage of the two-phase digestion, which was operated at high ammonium-N concentrations (1.0 and 1.4 g/L). A modified version of the IWA Anaerobic Digestion Model No. 1 (ADM1) with extensions for syntrophic acetate oxidation and weak-acid inhibition adequately described the dynamic profiles of volatile acid production

  8. Thermal Characterization of Lauric-Stearic Acid/Expanded Graphite Eutectic Mixture as Phase Change Materials.

    Science.gov (United States)

    Zhu, Hua; Zhang, Peng; Meng, Zhaonan; Li, Ming

    2015-04-01

    The eutectic mixture of lauric acid (LA) and stearic acid (SA) is a desirable phase change material (PCM) due to the constant melting temperature and large latent heat. However, its poor thermal conductivity has hampered its broad utilization. In the present study, pure LA, SA and the mixtures with various mass fractions of LA-SA were used as the basic PCMs, and 10 wt% expanded graphite (EG) was added to enhance the thermal conductivities. The phase change behaviors, microstructural analysis, thermal conductivities and thermal stabilities of the mixtures of PCMs were investigated by differential scanning calorimetry (DSC), scanning electronic microscope (SEM), transient plane source (TPS) and thermogravimetric analysis (TGA), respectively. The results show that the LA-SA binary mixture of mixture ratio of 76.3 wt%: 23.7 wt% forms an eutectic mixture, which melts at 38.99 °C and has a latent heat of 159.94 J/g. The melted fatty acids are well absorbed by the porous network of EG and they have a good thermal stability. Furthermore, poor thermal conductivities can be well enhanced by the addition of EG.

  9. Stationary measure in the multiverse

    Energy Technology Data Exchange (ETDEWEB)

    Linde, Andrei [Department of Physics, Stanford University, Stanford, CA 94305 (United States); Vanchurin, Vitaly; Winitzki, Sergei, E-mail: alinde@stanford.edu, E-mail: vitaly@cosmos2.phy.tufts.edu, E-mail: winitzki@physik.uni-muenchen.de [Department of Physics, Ludwig-Maximilians University, Munich (Germany)

    2009-01-15

    We study the recently proposed ''stationary measure'' in the context of the string landscape scenario. We show that it suffers neither from the ''Boltzmann brain'' problem nor from the ''youngness'' paradox that makes some other measures predict a high CMB temperature at present. We also demonstrate a good performance of this measure in predicting the results of local experiments, such as proton decay.

  10. Non-stationary Markov chains

    OpenAIRE

    Mallak, Saed

    1996-01-01

    Ankara : Department of Mathematics and Institute of Engineering and Sciences of Bilkent University, 1996. Thesis (Master's) -- Bilkent University, 1996. Includes bibliographical references leaves leaf 29 In thi.s work, we studierl the Ergodicilv of Non-Stationary .Markov chains. We gave several e.xainples with different cases. We proved that given a sec[uence of Markov chains such that the limit of this sec|uence is an Ergodic Markov chain, then the limit of the combination ...

  11. Determination of trace elements in acid rain by reversed phase extraction chromatography and neutron activation

    International Nuclear Information System (INIS)

    Rao, R.R.; Goski, D.G.; Chatt, A.

    1991-01-01

    A preconcentration neutron activation analysis (PNAA) method has been developed for the simultaneous determination of selected trace elements in acid rain and other water samples. The method consists of preconcentration of the elements by reversed phase extraction chromatography using oxine-loaded Amberlite XAD-2 resin. Nearly 100% recoveries were obtained for Co, Cu, Hg, V and Zn at pH 6.0 and for Cd at pH 7.0. Manganese gave incomplete recoveries at the pH range of 4.0-8.0 studies. Various factors that can influence preconcentration of the elements have been investigated in detail. The precision and accuracy of measurements have been evaluated by analyzing certified reference materials. The detection limits have been found to be of the order of ppb. The PNAA method has been applied to a number of acid rain and other water samples

  12. Supported Ionic Liquid Phase (SILP) Catalysis for the Production of Acetic acid by Methanol Carbonylation

    DEFF Research Database (Denmark)

    Hanning, Christopher William

    at the beginning with the construction of a suitable test reactor, then followed by the synthesis and testing of all the catalysts reported. A variety of nitrogen based ionic liquids were initially tested, giving good results and stability in the system. Later a number of phosphonium based salts were tested (these......The work presented here is focused on the development of a new reaction process. It applies Supported Ionic Liquid Phase (SILP) catalysis to a specific reaction. By reacting methanol and carbon monoxide over a rhodium catalyst, acetic acid can be formed. This reaction is important on a large scale...... were no longer classified as ionic liquids due to melting points above 100◦C). The phosphonium salts showed even better activity in the system compared to the ionic liquids. Overall the work has shown that this process for the manufacture of acetic acid is viable industrially. This is backed up...

  13. Nickel-cadmium batteries: effect of electrode phase composition on acid leaching process.

    Science.gov (United States)

    Nogueira, C A; Margarido, F

    2012-01-01

    At the end of their life, Ni-Cd batteries cause a number of environmental problems because of the heavy metals they contain. Because of this, recycling of Ni-Cd batteries has been carried out by dedicated companies using, normally, pyrometallurgical technologies. As an alternative, hydrometallurgical processes have been developed based on leaching operations using several types of leachants. The effect of factors like temperature, acid concentration, reaction time, stirring speed and grinding of material on the leaching yields of metals contained in anodic and cathodic materials (nickel, cadmium and cobalt) using sulphuric acid, is herein explained based on the structural composition of the electrode materials. The nickel, cobalt and cadmium hydroxide phases, even with a small reaction time (less than 15 minutes) and low temperature (50 degrees C) and acid concentration (1.1 M H2SO4), were efficiently leached. However, leaching of the nickel metallic phase was more difficult, requiring higher values of temperature, acid concentration and reaction time (e.g. 85 degrees C, 1.1 M H2SO4 and 5 h, respectively) in order to obtain a good leaching efficiency for anodic and cathodic materials (70% and 93% respectively). The stirring speed was not significant, whereas the grinding of electrode materials seems to promote the compaction of particles, which appears to be critical in the leaching of Ni degrees. These results allowed the identification and understanding of the relationship between the structural composition of electrode materials and the most important factors that affect the H2SO4 leaching of spent Ni-Cd battery electrodes, in order to obtain better metal-recovery efficiency.

  14. Raman study of the molecular motions of pivalic acid: the liquid—plastic phase transition

    Science.gov (United States)

    Balevičius, V.; Orel, B.; Hadži, D.

    Raman spectra of pivalic acid in the plastic and liquid phase have been measured. The reorientational correlation times have been evaluated from the ν asCH, νCO and νCC bands as a function of temperature. The reorientational correlation time corresponding to ν as CH and νCC bands is τ 4ps ( T = 20°C). The calculated activation energy is 26 KJ mol -1. The reorientation of the carboxylic groups which may be assisted by the proton transfer along the hydrogen bonds in dimers is discussed.

  15. Thermotropic phase transition in an adsorbed melissic acid film at the n-hexane-water interface

    Science.gov (United States)

    Tikhonov, A. M.

    2017-06-01

    A reversible thermotropic phase transition in an adsorption melissic acid film at the interface between n-hexane and an aqueous solution of potassium hydroxide (pH ≈ 10) is investigated by X-ray reflectometry and diffuse scattering using synchrotron radiation. The experimental data indicate that the interface "freezing" transition is accompanied not only by the crystallization of the Gibbs monolayer but also by the formation of a planar smectic structure in the 300-Å-thick adsorption film; this structure is formed by 50-Å-thick layers.

  16. Preparation, characterization, and thermal properties of starch microencapsulated fatty acids as phase change materials thermal energy storage applications

    Science.gov (United States)

    Stable starch-oil composites can be prepared from renewable resources by excess steam jet-cooking aqueous slurries of starch and vegetable oils or other hydrophobic materials. Fatty acids such as stearic acid are promising phase change materials (PCMs) for latent heat thermal energy storage applica...

  17. The removal of fatty acids from edible oil : removal of the dispersed phase of a water-in-oil dispersion by a hydrophilic membrane

    NARCIS (Netherlands)

    Keurentjes, J.T.F.; Doornbusch, G.I.; Riet, van 't K.

    1991-01-01

    Fatty acids can be extracted from an oil phase by forming a dispersed phase of saponified fatty acids/water/isopropanol in oil. This dispersion can be separated in the two phases by two membranes of opposite polarity in series. In this study the separation of the water phase from the dispersion by a

  18. Thermal properties of lauric acid filled in carbon nanotubes as shape-stabilized phase change materials.

    Science.gov (United States)

    Feng, Yanhui; Wei, Runzhi; Huang, Zhi; Zhang, Xinxin; Wang, Ge

    2018-03-14

    Carbon nanotubes (CNTs) filled with lauric acid (LA) as a kind of shape-stabilized phase change material were prepared and their structures and phase change properties were characterized. The results showed that the melting point and latent heat of LA confined in carbon nanotubes were lower than those of the bulk material, and both decrease as the diameters of CNTs and the filling ratios of LA decrease. Molecular dynamics (MD) simulations indicated that LA molecules form a liquid layer near pore walls and crystallize at the pore center. When the LA filling ratio was reduced to a certain value, all LA molecules were attached to the inner walls of CNTs, hindering their crystallization. A linear relationship between the melting temperature shift and structural properties was obtained based on the modified Gibbs-Thomson equation, which gives a reliable interpretation of the size effect of nanochannels in phase change materials. We also found that the thermal conductivity of the composite CNTs/LA was four times larger than that of pure LA. This study will provide insights into the design of novel composite phase change materials with better thermal properties by the selection of suitable porous materials and tailoring their pore structures.

  19. Deep desulfurization of diesel via peroxide oxidation using phosphotungstic acid as phase transfer catalyst

    Energy Technology Data Exchange (ETDEWEB)

    Sachdeva, T.O.; Pant, K.K. [Department of Chemical Engineering, Indian Institute of Technology, Delhi, New Delhi, 110016 (India)

    2010-09-15

    High sulfur level in diesel fuel has been identified as a major contributor to air pollutant in term of sulfur dioxide (SO{sub x}) through diesel fueled vehicles. The main aim of the present work is to develop a promising methodology for ultra deep desulfurization of diesel fuel using oxidation followed by phase transfer of oxidized sulfur. Experiments were carried out in a batch reactor using n-decane as the model diesel compound and also using commercial diesel feedstock. To remove sulfur tetraoctylammonium bromide, phosphotungstic acid, and hydrogen peroxide were used as phase transfer agent, catalyst and oxidant respectively. The percent sulfur removal increases with increasing the initial concentration of sulfur in fuel and with increasing the reaction temperature. Similar trends were observed when commercial diesel was used to carry out desulfurization studies. The amphiphilic catalyst serves as a catalyst and also as an emulsifying agent to stabilize the emulsion droplets. The effects of temperature, agitation speed, quantity of catalyst and the phase transfer agent were studied to estimate the optimal conditions for the reactions. The sulfur removal from a commercial diesel by phase transfer catalysis has been found effective and removal efficiency was more than 98%. Kinetic experiments carried out for the desulfurization revealed that the sulfur removal results are best fitted to a pseudo first order kinetics and the apparent activation energy of desulfurization was 30.6 kJ/mol. (author)

  20. Deep desulfurization of diesel via peroxide oxidation using phosphotungstic acid as phase transfer catalyst

    International Nuclear Information System (INIS)

    Sachdeva, T.O.; Pant, K.K.

    2010-01-01

    High sulfur level in diesel fuel has been identified as a major contributor to air pollutant in term of sulfur dioxide (SO x ) through diesel fueled vehicles. The main aim of the present work is to develop a promising methodology for ultra deep desulfurization of diesel fuel using oxidation followed by phase transfer of oxidized sulfur. Experiments were carried out in a batch reactor using n-decane as the model diesel compound and also using commercial diesel feedstock. To remove sulfur tetraoctylammonium bromide, phosphotungstic acid, and hydrogen peroxide were used as phase transfer agent, catalyst and oxidant respectively. The percent sulfur removal increases with increasing the initial concentration of sulfur in fuel and with increasing the reaction temperature. Similar trends were observed when commercial diesel was used to carry out desulfurization studies. The amphiphilic catalyst serves as a catalyst and also as an emulsifying agent to stabilize the emulsion droplets. The effects of temperature, agitation speed, quantity of catalyst and the phase transfer agent were studied to estimate the optimal conditions for the reactions. The sulfur removal from a commercial diesel by phase transfer catalysis has been found effective and removal efficiency was more than 98%. Kinetic experiments carried out for the desulfurization revealed that the sulfur removal results are best fitted to a pseudo first order kinetics and the apparent activation energy of desulfurization was 30.6 kJ/mol. (author)

  1. Climatic feedbacks between stationary and transient eddies

    International Nuclear Information System (INIS)

    Branscome, L.E.

    1994-01-01

    Stationary eddies make a significant contribution to poleward heat transport during Northern Hemisphere winter, equaling the transport by transient eddies. On the other hand, stationary eddy transport during the summer is negligible. The effect of topography on time-mean stationary waves and low-frequency variability has been widely studied. In contrast, little attention has been given to the climatic feedbacks associated with stationary eddies. Furthermore, the relationship between stationary and transient eddies in the context of global and regional climate is not well understood. The response of the climate system to anthropogenic forcing is likely to have some dependence on stationary wave transport and its interaction with transient eddies. Some early GCM simulations and observational analyses indicate a strong feedback between the meridional heat fluxes of stationary and transient eddies

  2. The antidepressant role of dietary long-chain polyunsaturated n-3 fatty acids in two phases in the developing brain.

    Science.gov (United States)

    Ferraz, Anete Curte; Kiss, Agata; Araújo, Renata Lins Fuentes; Salles, Hélidy Maria Rossi; Naliwaiko, Katya; Pamplona, Juliana; Matheussi, Francesca

    2008-03-01

    In this work we investigated the effect from fish oil (FO) supplementation, rich in n-3 fatty acids, on an antidepressant effect on adult rats in Phase A (supplementation during pregnancy and lactation) and phase B (supplementation during post-weaning until adulthood). During Phase A, female rats, used as matrix to obtain male rats, were divided in three groups: FO (daily supplemented), CF (coconut fat daily supplemented) and control (not supplemented). Our results showed that adult rats whose mothers were supplemented with FO during Phase A and rats supplemented during phase B demonstrated a significantly decreased immobility time when compared to control and CF groups. There was no difference in neither motor activity nor anxiety behavior in the three groups excluding false positive results. Our results suggest that n-3 fatty acids supplementation during Phases A and B had a beneficial effect on preventing the development of depression-like behavior in adult rats.

  3. Contributions to reversed-phase column selectivity: III. Column hydrogen-bond basicity.

    Science.gov (United States)

    Carr, P W; Dolan, J W; Dorsey, J G; Snyder, L R; Kirkland, J J

    2015-05-22

    Column selectivity in reversed-phase chromatography (RPC) can be described in terms of the hydrophobic-subtraction model, which recognizes five solute-column interactions that together determine solute retention and column selectivity: hydrophobic, steric, hydrogen bonding of an acceptor solute (i.e., a hydrogen-bond base) by a stationary-phase donor group (i.e., a silanol), hydrogen bonding of a donor solute (e.g., a carboxylic acid) by a stationary-phase acceptor group, and ionic. Of these five interactions, hydrogen bonding between donor solutes (acids) and stationary-phase acceptor groups is the least well understood; the present study aims at resolving this uncertainty, so far as possible. Previous work suggests that there are three distinct stationary-phase sites for hydrogen-bond interaction with carboxylic acids, which we will refer to as column basicity I, II, and III. All RPC columns exhibit a selective retention of carboxylic acids (column basicity I) in varying degree. This now appears to involve an interaction of the solute with a pair of vicinal silanols in the stationary phase. For some type-A columns, an additional basic site (column basicity II) is similar to that for column basicity I in primarily affecting the retention of carboxylic acids. The latter site appears to be associated with metal contamination of the silica. Finally, for embedded-polar-group (EPG) columns, the polar group can serve as a proton acceptor (column basicity III) for acids, phenols, and other donor solutes. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Mapping the conformational free energy of aspartic acid in the gas phase and in aqueous solution.

    Science.gov (United States)

    Comitani, Federico; Rossi, Kevin; Ceriotti, Michele; Sanz, M Eugenia; Molteni, Carla

    2017-04-14

    The conformational free energy landscape of aspartic acid, a proteogenic amino acid involved in a wide variety of biological functions, was investigated as an example of the complexity that multiple rotatable bonds produce even in relatively simple molecules. To efficiently explore such a landscape, this molecule was studied in the neutral and zwitterionic forms, in the gas phase and in water solution, by means of molecular dynamics and the enhanced sampling method metadynamics with classical force-fields. Multi-dimensional free energy landscapes were reduced to bi-dimensional maps through the non-linear dimensionality reduction algorithm sketch-map to identify the energetically stable conformers and their interconnection paths. Quantum chemical calculations were then performed on the minimum free energy structures. Our procedure returned the low energy conformations observed experimentally in the gas phase with rotational spectroscopy [M. E. Sanz et al., Phys. Chem. Chem. Phys. 12, 3573 (2010)]. Moreover, it provided information on higher energy conformers not accessible to experiments and on the conformers in water. The comparison between different force-fields and quantum chemical data highlighted the importance of the underlying potential energy surface to accurately capture energy rankings. The combination of force-field based metadynamics, sketch-map analysis, and quantum chemical calculations was able to produce an exhaustive conformational exploration in a range of significant free energies that complements the experimental data. Similar protocols can be applied to larger peptides with complex conformational landscapes and would greatly benefit from the next generation of accurate force-fields.

  5. Formation of U(IV) Nanoparticles and Their Growth Mechanism in Mildly Acidic Aqueous Phases

    Energy Technology Data Exchange (ETDEWEB)

    Cha, Wan Sik; Kim, Sun Tae; Cho, Hye Ryun; Jung, Euo Chang [KAERI, Daejeon (Korea, Republic of)

    2016-05-15

    Previous studies suggest that U(IV) nanoparticle (NP) formation is one of key steps in mineralization or immobilization of uranium which can be mediated either by microbes or by abiotic geochemical reactions. Colloidal NPs in a groundwater system are potential carrier phases influencing RN migration in subsurface environment. However, the mechanism of U(IV) NP formation and the potential reaction intermediates during this solid phase formation process have not been elucidated in detail so far. In this study we attempted to examine the U(IV) nanoparticle formation reactions preceded by the hydrolysis of U{sup 4+} at different pHs, concentrations and temperatures. The kinetics of U(IV) NP formation from dissolved U(IV) species was monitored under mildly acidic conditions (pH 2 ∼ 3) mainly by using UV-Vis absorption spectrophotometry. Dynamic light scattering (DLS) analysis, nanoparticle tracking analysis (NTA) and transmission electron microscopy (TEM) were used to characterize the NPs produced during the reactions. The results demonstrate that the U(IV) NP formation process is very sensitive toward temperature variation. The main outcome of this study is the discovery of the autocatalytic nature of U(IV) NP formation from the supersaturated U(OH){sup 3+} solution in a mildly acidic aqueous solution. The structure of reaction intermediates is proposed to contain oxide linkage. In the presentation the proposed mechanism of the U(IV) NP formation reaction and the properties of primary NPs and their clusters will be discussed in detail.

  6. Mapping the conformational free energy of aspartic acid in the gas phase and in aqueous solution

    Science.gov (United States)

    Comitani, Federico; Rossi, Kevin; Ceriotti, Michele; Sanz, M. Eugenia; Molteni, Carla

    2017-04-01

    The conformational free energy landscape of aspartic acid, a proteogenic amino acid involved in a wide variety of biological functions, was investigated as an example of the complexity that multiple rotatable bonds produce even in relatively simple molecules. To efficiently explore such a landscape, this molecule was studied in the neutral and zwitterionic forms, in the gas phase and in water solution, by means of molecular dynamics and the enhanced sampling method metadynamics with classical force-fields. Multi-dimensional free energy landscapes were reduced to bi-dimensional maps through the non-linear dimensionality reduction algorithm sketch-map to identify the energetically stable conformers and their interconnection paths. Quantum chemical calculations were then performed on the minimum free energy structures. Our procedure returned the low energy conformations observed experimentally in the gas phase with rotational spectroscopy [M. E. Sanz et al., Phys. Chem. Chem. Phys. 12, 3573 (2010)]. Moreover, it provided information on higher energy conformers not accessible to experiments and on the conformers in water. The comparison between different force-fields and quantum chemical data highlighted the importance of the underlying potential energy surface to accurately capture energy rankings. The combination of force-field based metadynamics, sketch-map analysis, and quantum chemical calculations was able to produce an exhaustive conformational exploration in a range of significant free energies that complements the experimental data. Similar protocols can be applied to larger peptides with complex conformational landscapes and would greatly benefit from the next generation of accurate force-fields.

  7. Quantum cosmology and stationary states

    International Nuclear Information System (INIS)

    Padmanabhan, T.

    1983-01-01

    A model for quantum gravity, in which the conformal part of the metric is quantized using the path integral formalism, is presented. Einstein's equations can be suitably modified to take into account the effects of quantum conformal fluctuations. A closed Friedman model can be described in terms of well-defined stationary states. The ''ground state'' sets a lower bound (at Planck length) to the scale factor preventing the collapse. A possible explanation for matter creation and quantum nature of matter is suggested. (author)

  8. Phase equilibrium measurements of ternary systems formed by linoleic and linolenic acids in carbon dioxide/ethanol mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Rosso, Sibele R. [EQA/UFSC, Chemical and Food Engineering Department, Federal University of Santa Catarina, C.P. 476, CEP 88040-900, Florianopolis, SC (Brazil); Franceschi, Elton; Borges, Gustavo R.; Corazza, Marcos L.; Oliveira, J. Vladimir [Department of Food Engineering, URI - Campus de Erechim, Av. Sete de Setembro, 1621, Erechim, RS 99700-000 (Brazil); Ferreira, Sandra R.S. [EQA/UFSC, Chemical and Food Engineering Department, Federal University of Santa Catarina, C.P. 476, CEP 88040-900, Florianopolis, SC (Brazil)], E-mail: sandra@enq.ufsc.br

    2009-11-15

    This work reports phase equilibrium measurements for the ternary systems linoleic (acid + CO{sub 2} + ethanol) and (linolenic acid + CO{sub 2} + ethanol). The fatty acids present in the ternary systems were selected based on composition of banana peel oil extracted by supercritical CO{sub 2} at 20 MPa and 313 K. The motivation of this research relies on the fact that these unsaturated fatty acids are recognized to play an important role in lowering blood pressure and serum cholesterol and because they are present in high concentrations in banana peel extract. Besides that, equilibrium data of these compounds are scarce in literature. The phase equilibrium experiments were performed using a high-pressure variable-volume view cell over the temperature range of (303 to 343) K and pressures up to 19 MPa. For both systems, only vapour-liquid phase transitions were visually recorded for all data measured.

  9. Gas phase hydrolysis of formaldehyde to form methanediol: impact of formic acid catalysis.

    Science.gov (United States)

    Hazra, Montu K; Francisco, Joseph S; Sinha, Amitabha

    2013-11-21

    We find that formic acid (FA) is very effective at facilitating diol formation through its ability to reduce the barrier for the formaldehyde (HCHO) hydrolysis reaction. The rate limiting step in the mechanism involves the isomerization of a prereactive collision complex formed through either the HCHO···H2O + FA and/or HCHO + FA···H2O pathways. The present study finds that the effective barrier height, defined as the difference between the zero-point vibrational energy (ZPE) corrected energy of the transition state (TS) and the HCHO···H2O + FA and HCHO + FA···H2O starting reagents, are respectively only ∼1 and ∼4 kcal/mol. These barriers are substantially lower than the ∼17 kcal/mol barrier associated with the corresponding step in the hydrolysis of HCHO catalyzed by a single water molecule (HCHO + H2O + H2O). The significantly lower barrier heights for the formic acid catalyzed pathway reveal a new important role that organic acids play in the gas phase hydrolysis of atmospheric carbonyl compounds.

  10. Reduction of NOx emission from stationary combustion sources

    International Nuclear Information System (INIS)

    Nelson, P.F.

    1992-01-01

    The environmental impacts of NO x emission from stationary combustion sources are briefly described. These include the formation of both acid rain and photochemical smog, major environmental problems. The three mechanisms which have been identified for the formation of NO x in combustion (thermal, prompt and fuel) are also briefly outlined. Recently stringent standards have been introduced to control emissions of NO x and the review describes the major primary and secondary measures. 10 refs. 2 tabs., 5 figs

  11. Phase diagrams in blends of poly(3-hydroxybutyric acid with various aliphatic polyesters

    Directory of Open Access Journals (Sweden)

    2011-07-01

    Full Text Available Phase behavior with immiscibility, miscibility, crystalline morphology, and kinetic analysis in blends of poly(3-hydroxybutyric acid (PHB with aliphatic polyesters such as poly(butylene adipate (PBA, poly(ethylene adipate (PEA, poly(trimethylene adipate (PTA, or poly(ethylene succinate (PESu, respectively, were explored mainly using differential scanning calorimeter (DSC and polarized-light optical microscopy (POM. Immiscibility phase behavior with reversible upper-critical-solution-temperature (UCST is common in the PHB/polyester blends. The polyester/polyester blend of PHB/PTA is partially miscible with no UCST in melt and amorphous glassy states within a composition range of PTA less than 50 wt%. The miscible crystalline/crystalline blend exhibits ring-banded spherulites at Tc = 50~100°C, with inter-ring spacing dependent on Tc. All immiscible or partially miscible PHB/polyester blends, by contrast, exhibit disrupted ringbanded spherulites or discrete spherical phase domains upon cooling from UCST to crystallization. The blends of PHB with all other aliphatic polyesters, such as PESu, PEA, PBA, etc. are only partially miscible or immiscible with an upper critical solution temperature (UCST at 180~221°C depending on blend composition. UCST with reversibility was verified.

  12. Palmitic acid/polypyrrole composites as form-stable phase change materials for thermal energy storage

    International Nuclear Information System (INIS)

    Silakhori, Mahyar; Metselaar, Hendrik Simon Cornelis; Mahlia, Teuku Meurah Indra; Fauzi, Hadi; Baradaran, Saeid; Naghavi, Mohammad Sajad

    2014-01-01

    Highlights: • A novel phase change composite of palmitic acid–polypyrrole(PA–PPy) was fabricated. • Thermal properties of PA–PPy are characterized in different mass ratios of PA–PPy. • Thermal cycling test showed that form stable PCM had a favorable thermal reliability. - Abstract: In this study a novel palmitic acid (PA)/polypyrrole (PPy) form-stable PCMs were readily prepared by in situ polymerization method. PA was used as thermal energy storage material and PPy was operated as supporting material. Form-stable PCMs were investigated by SEM (scanning electron microscopy) and FTIR (Fourier transform infrared spectrometer) analysis that illustrated PA Particles were wrapped by PPy particles. XRD (X-ray diffractometer) was used for crystalline phase of PA/PPy composites. Thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC) were used for investigating Thermal stability and thermal energy storage properties of prepared form-stable PCMs. According to the obtained results the form stable PCMs exhibited favorable thermal stability in terms of their phase change temperature. The form-stable PCMs (79.9 wt% loading of PA) were considered as the highest loading PCM with desirable latent heat storage of 166.3 J/g and good thermal stability. Accelerated thermal cycling tests also showed that form stable PCM had an acceptable thermal reliability. As a consequence of acceptable thermal properties, thermal stability and chemical stability, we can consider the new kind of form stable PCMs for low temperature solar thermal energy storage applications

  13. [Determination of geniposidic acid and chlorogenic acid in male flowers and related products of Eucommia ulmoides by reversed-phase high performance liquid chromatography].

    Science.gov (United States)

    Dong, Juane; Ma, Xihan

    2007-03-01

    A simple and rapid high performance liquid chromatographic method has been developed for the determination of geniposidic acid and chlorogenic acid in the male flowers and related products of Eucommia ulmoides. Two components were separated by a Shim-pack VP-ODS column (150 mm x4.6 mm, 5 [microm) with a mobile phase of methanol-water-acetic acid (24 :75: 1, v/v) at a flow rate of 1 mL/min, column temperature of 30 93 and detection wavelength of 240 nm. Under the chromatographic conditions mentioned above, the method performance, such as the number of theoretical plate, resolution, trailing etc have all reached required level. The linear ranges were 0. 025 - 0. 400 g/L for geniposidic acid and 0. 075 - 1. 200 g/L for chlorogenic acid, with the correlation coefficients of 0. 999 7 and 0. 999 9, respectively. The average recoveries were 100. 2% and 100. 5%, and the relative standard deviations (RSDs) were 1. 47% and 1. 49% respectively. The minimum detection limits were 0. 02 microg/L for geniposidic acid, and 0. 06 microg/L for chlorogenic acid. The method developed has demonstrated the characteristics of simple mobile phase composition, short retention, good resolution, high repeatability and precision. It is suitable for the determination of the two compounds in the male flowers of E. ulmoides and related products.

  14. Strong Stationary Duality for Diffusion Processes

    OpenAIRE

    Fill, James Allen; Lyzinski, Vince

    2014-01-01

    We develop the theory of strong stationary duality for diffusion processes on compact intervals. We analytically derive the generator and boundary behavior of the dual process and recover a central tenet of the classical Markov chain theory in the diffusion setting by linking the separation distance in the primal diffusion to the absorption time in the dual diffusion. We also exhibit our strong stationary dual as the natural limiting process of the strong stationary dual sequence of a well ch...

  15. Stationary analysis of signals and ratio decay determination in BWR type reactors by neuronal network

    International Nuclear Information System (INIS)

    Sanchis, R.; Palomo, M. J.; Munoz-Cobo, J. L.

    1998-01-01

    The signals registered in the nuclear plants have non stationary characteristics, in numerous times. This made difficult the application of the methods of analysis. There are determinate temporal intervals in that the signal is stationary with determinate mean, value together of zones with corrupt registers, and other zones with mean value distinct, but stationary during a temporal interval. The methodology consist in a stationary analysis to the signal received of the nuclear plant. With the Gabor Transformation are determined the temporal intervals of the stationary signals, synthesised it, as previous phase to the application of the methods of the analysis of stability parameters with methods ARMA, SVD, Neural Net,... to the reconstructed signal. 4 refs. (Author)

  16. Phase Transition of Poly(acrylic acid-co-N-isopropylacrylamide) Core-shell Nanogels

    Science.gov (United States)

    Liu, Xiao-bing; Zhou, Jian-feng; Ye, Xiao-dong

    2012-08-01

    A series of poly(acrylic acid) macromolecular chain transfer agents with different molecular weights were synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization and characterized by 1H NMR and gel permeation chromatography. Multiresponsive core-shell nanogels were prepared by dispersion polymerization of N-isopropylacrylamide in water using these poly(potassium acrylate) macro-RAFT agents as the electrosteric stabilizer. The size of the nanogels decreases with the amount of the macro-RAFT agent, indicating that the surface area occupied by per polyelectrolyte group is a critical parameter for stabilizing the nanogels. The volume phase transition and the zeta potentials of the nanogels in aqueous solutions were studied by dynamic light scattering and zetasizer analyzer, respectively.

  17. Condensational theory of stationary tornadoes

    International Nuclear Information System (INIS)

    Makarieva, A.M.; Gorshkov, V.G.; Nefiodov, A.V.

    2011-01-01

    Using the Bernoulli integral for air streamline with condensing water vapor a stationary axisymmetric tornado circulation is described. The obtained profiles of vertical, radial and tangential velocities are in agreement with observations for the Mulhall tornado, world's largest on record and longest-lived among the three tornadoes for which 3D velocity data are available. Maximum possible vortex velocities are estimated. -- Highlights: → Water vapor condensation causes a logarithmic drop of air pressure towards tornado center. → The first ever theoretical description of tornado velocities is obtained. → The maximum vortex velocity grows logarithmically with decreasing tornado eye radius. → Air motion with high velocities can only develop in sufficiently large condensation areas.

  18. Fatty acids profile and nutritional composition of two tropical diatoms from the Costa Rican Pacific Coast

    Directory of Open Access Journals (Sweden)

    K. Rodríguez-Núñez

    2017-09-01

    Full Text Available Microalgae represent an important nutritional source for diverse organisms, therefore, their nutritional value, and more specifically, total lipid and fatty acid contents, must be considered. This study evaluated the nutritional contents and potential growth under controlled conditions of Nitzschia sp. and Chaetoceros sp. Tropical microalgae, isolated from the Gulf of Nicoya, Costa Rica. In both strains, the nutritional composition and the fatty acid profile were evaluated in exponential and stationary phases. With regards to fatty acids, v sp. had more Eicosapentaenoic Acid (EPA in both the exponential (32.80% and stationary (27.20% phases. The results in growth rate, production and biochemical composition indicated two tropical microalgae strains suitable for cultivation under controlled conditions. The studies of the phytoplankton in this geographical area is highly relevant because of its importance in the primary production of nutrients and the importance of finding sources of fatty acids such as the EPA.

  19. Fatty acids profile and nutritional composition of two tropical diatoms from the Costa Rican Pacific Coast

    International Nuclear Information System (INIS)

    Rodríguez-Núñez, K.; Toledo-Aguero, P.

    2017-01-01

    Microalgae represent an important nutritional source for diverse organisms, therefore, their nutritional value, and more specifically, total lipid and fatty acid contents, must be considered. This study evaluated the nutritional contents and potential growth under controlled conditions of Nitzschia sp. and Chaetoceros sp. Tropical microalgae, isolated from the Gulf of Nicoya, Costa Rica. In both strains, the nutritional composition and the fatty acid profile were evaluated in exponential and stationary phases. With regards to fatty acids, Nitzschia sp. had more Eicosapentaenoic Acid (EPA) in both the exponential (32.80%) and stationary (27.20%) phases. The results in growth rate, production and biochemical composition indicated two tropical microalgae strains suitable for cultivation under controlled conditions. The studies of the phytoplankton in this geographical area is highly relevant because of its importance in the primary production of nutrients and the importance of finding sources of fatty acids such as the EPA. [es

  20. Gas-Phase Thermal Tautomerization of Imidazole-Acetic Acid: Theoretical and Computational Investigations

    Directory of Open Access Journals (Sweden)

    Saadullah G. Aziz

    2015-11-01

    Full Text Available The gas-phase thermal tautomerization reaction between imidazole-4-acetic (I and imidazole-5-acetic (II acids was monitored using the traditional hybrid functional (B3LYP and the long-range corrected functionals (CAM-B3LYP and ωB97XD with 6-311++G** and aug-cc-pvdz basis sets. The roles of the long-range and dispersion corrections on their geometrical parameters, thermodynamic functions, kinetics, dipole moments, Highest Occupied Molecular Orbital–Lowest Unoccupied Molecular Orbital (HOMO–LUMO energy gaps and total hyperpolarizability were investigated. All tested levels of theory predicted the preference of I over II by 0.750–0.877 kcal/mol. The origin of predilection of I is assigned to the H-bonding interaction (nN8→σ*O14–H15. This interaction stabilized I by 15.07 kcal/mol. The gas-phase interconversion between the two tautomers assumed a 1,2-proton shift mechanism, with two transition states (TS, TS1 and TS2, having energy barriers of 47.67–49.92 and 49.55–52.69 kcal/mol, respectively, and an sp3-type intermediate. A water-assisted 1,3-proton shift route brought the barrier height down to less than 20 kcal/mol in gas-phase and less than 12 kcal/mol in solution. The relatively high values of total hyperpolarizability of I compared to II were interpreted and discussed.

  1. L-lysine-L-tartaric acid: New molecular complex with nonlinear optical properties. Structure, vibrational spectra and phase transitions

    International Nuclear Information System (INIS)

    Debrus, S.; Marchewka, M.K.; Baran, J.; Drozd, M.; Czopnik, R.; Pietraszko, A.; Ratajczak, H.

    2005-01-01

    The first X-ray diffraction and vibrational spectroscopic analysis of a novel complex between L-lysine and L-tartaric acid is reported. The structure was solved in two temperatures (320 and 260 K) showing incommensurate phase between them. Room-temperature powder infrared and Raman measurements for the L-lysine-L-tartaric acid molecular complex (1:1) were carried out. DSC measurements on powder samples indicate two phase transitions points at about 295, 300 and 293, 300 K, for heating and cooling, respectively, with noticeable temperature interval between them. Second harmonic generation efficiency d eff =0.35 d eff (KDP)

  2. Critical Test of Some Computational Chemistry Methods for Prediction of Gas-Phase Acidities and Basicities.

    Science.gov (United States)

    Toomsalu, Eve; Koppel, Ilmar A; Burk, Peeter

    2013-09-10

    Gas-phase acidities and basicities were calculated for 64 neutral bases (covering the scale from 139.9 kcal/mol to 251.9 kcal/mol) and 53 neutral acids (covering the scale from 299.5 kcal/mol to 411.7 kcal/mol). The following methods were used: AM1, PM3, PM6, PDDG, G2, G2MP2, G3, G3MP2, G4, G4MP2, CBS-QB3, B1B95, B2PLYP, B2PLYPD, B3LYP, B3PW91, B97D, B98, BLYP, BMK, BP86, CAM-B3LYP, HSEh1PBE, M06, M062X, M06HF, M06L, mPW2PLYP, mPW2PLYPD, O3LYP, OLYP, PBE1PBE, PBEPBE, tHCTHhyb, TPSSh, VSXC, X3LYP. The addition of the Grimmes empirical dispersion correction (D) to B2PLYP and mPW2PLYP was evaluated, and it was found that adding this correction gave more-accurate results when considering acidities. Calculations with B3LYP, B97D, BLYP, B2PLYPD, and PBE1PBE methods were carried out with five basis sets (6-311G**, 6-311+G**, TZVP, cc-pVTZ, and aug-cc-pVTZ) to evaluate the effect of basis sets on the accuracy of calculations. It was found that the best basis sets when considering accuracy of results and needed time were 6-311+G** and TZVP. Among semiempirical methods AM1 had the best ability to reproduce experimental acidities and basicities (the mean absolute error (mae) was 7.3 kcal/mol). Among DFT methods the best method considering accuracy, robustness, and computation time was PBE1PBE/6-311+G** (mae = 2.7 kcal/mol). Four Gaussian-type methods (G2, G2MP2, G4, and G4MP2) gave similar results to each other (mae = 2.3 kcal/mol). Gaussian-type methods are quite accurate, but their downside is the relatively long computational time.

  3. Kinetic study of solid phase demineralization by weak acids in one-step enzymatic bio-refinery of shrimp cuticles

    OpenAIRE

    Baron, Regis; Socol, Marius; Arhaliass, A.; Bruzac, Sandrine; Le Roux, Karine; Del Pino, J. Rodriguez; Berge, Jean-pascal; Kaas, Raymond

    2015-01-01

    We describe a one-step bio-refinery process for shrimp composites by-products. Its originality lies in a simple rapid (6 h) biotechnological cuticle fragmentation process that recovers all major compounds (chitins, peptides and minerals in particular calcium). The process consists of a controlled exogenous enzymatic proteolysis in a food-grade acidic medium allowing chitin purification (solid phase), and recovery of peptides and minerals (liquid phase). At a pH of between 3.5 and 4, protease ...

  4. A Linker for the Solid-Phase Synthesis of Hydroxamic Acids and Identification of HDAC6 Inhibitors

    DEFF Research Database (Denmark)

    Bang, Claus Gunnar; Jensen, Jakob Feldthusen; Cohrt, Anders Emil O'Hanlon

    2017-01-01

    We herein present broadly useful, readily available and nonintegral hydroxylamine linkers for the routine solid-phase synthesis of hydroxamic acids. The developed protocols enable the efficient synthesis and release of a wide range of hydroxamic acids from various resins, relying on high control...... and flexibility with respect to reagents and synthetic processes. A trityl-based hydroxylamine linker was used to synthesize a library of peptide hydroxamic acids. The inhibitory effects of the compounds were examined for seven HDAC enzyme subtypes using a chemiluminescence-based assay....

  5. Partition Coefficients of Amino Acids, Peptides, and Enzymes in Dextran + Poly(Ethylene Glycol) + Water Aqueous Two-Phase Systems

    Energy Technology Data Exchange (ETDEWEB)

    Kakisaka, Keijiro.; Shindo, Takashi.; Iwai, Yoshio.; Arai, Yasuhiko. [Kyushu University, Fukuoka (Japan). Department of Chemical Systems and Engineering

    1998-12-01

    Partition coefficients are measured for five amino acids(aspartic acid, asparagine, methionine, cysteine and histidine) and tow peptides(glycyl-glycine and hexa-glycine) in dextran + poly(ethylene glycol) + water aqueous two-phase system. The partition coefficients of the amino acids and peptides are aorrelated using the osmotic virial equation. The interaction coefficients contained in the equation can be calculated by hydrophilic group parameters. The partition coefficients of {alpha}-amylase calculated by the osmotic virial equation with the hydrophilic group parameters are in fairly good agreement with the experimental data, though a relatively large discrepancy is shown for {beta}-amylase. (author)

  6. Partition Coefficients of Amino Acids, Peptides, and Enzymes in Dextran + Poly(Ethylene Glycol) + Water Aqueous Two-Phase Systems

    Energy Technology Data Exchange (ETDEWEB)

    Kakisaka, Keijiro.; Shindo, Takashi.; Iwai, Yoshio.; Arai, Yasuhiko. (Kyushu University, Fukuoka (Japan). Department of Chemical Systems and Engineering)

    1998-12-01

    Partition coefficients are measured for five amino acids(aspartic acid, asparagine, methionine, cysteine and histidine) and tow peptides(glycyl-glycine and hexa-glycine) in dextran + poly(ethylene glycol) + water aqueous two-phase system. The partition coefficients of the amino acids and peptides are aorrelated using the osmotic virial equation. The interaction coefficients contained in the equation can be calculated by hydrophilic group parameters. The partition coefficients of [alpha]-amylase calculated by the osmotic virial equation with the hydrophilic group parameters are in fairly good agreement with the experimental data, though a relatively large discrepancy is shown for [beta]-amylase. (author)

  7. Groebner Basis Methods for Stationary Solutions of a Low-Dimensional Model for a Shear Flow

    Science.gov (United States)

    Pausch, Marina; Grossmann, Florian; Eckhardt, Bruno; Romanovski, Valery G.

    2014-10-01

    We use Groebner basis methods to extract all stationary solutions for the nine-mode shear flow model described in Moehlis et al. (New J Phys 6:56, 2004). Using rational approximations to irrational wave numbers and algebraic manipulation techniques we reduce the problem of determining all stationary states to finding roots of a polynomial of order 30. The coefficients differ by 30 powers of 10, so that algorithms for extended precision are needed to extract the roots reliably. We find that there are eight stationary solutions consisting of two distinct states, each of which appears in four symmetry-related phases. We discuss extensions of these results for other flows.

  8. Synthesis and characterization of microencapsulated myristic acid–palmitic acid eutectic mixture as phase change material for thermal energy storage

    International Nuclear Information System (INIS)

    Alva, Guruprasad; Huang, Xiang; Liu, Lingkun; Fang, Guiyin

    2017-01-01

    Highlights: •Myristic acid–palmitic acid eutectic was microencapsulated with silica shell. •Structure, morphology of microencapsulated phase change material were investigated. •Thermal capacity, stability of microencapsulated phase change material were analyzed. •Silica shell improved thermal stability of microencapsulated phase change material. -- Abstract: In this work microencapsulation of myristic acid–palmitic acid (MA–PA) eutectic mixture with silica shell using sol−gel method has been attempted. The core phase change material (PCM) for thermal energy storage was myristic acid−palmitic acid eutectic mixture and the shell material to prevent the PCM core from leakage was silica prepared from methyl triethoxysilane (MTES). Thermal properties of the microcapsules were measured by differential scanning calorimeter (DSC). The morphology and particle size of the microcapsules were examined by scanning electronic microscope (SEM). Fourier transformation infrared spectrophotometer (FT–IR) and X–ray diffractometer (XRD) were used to investigate the chemical structure and crystalloid phase of the microcapsules respectively. The DSC results indicated that microencapsulated phase change material (MPCM) melts at 46.08 °C with a latent heat of 169.69 kJ kg −1 and solidifies at 44.35 °C with a latent heat of 159.59 kJ kg −1 . The thermal stability of the microcapsules was analyzed by a thermogravimeter (TGA). The results indicated that the MPCM has good thermal stability and is suitable for thermal energy storage application.

  9. Stationary and non-stationary occurrences of miniature end plate potentials are well described as stationary and non-stationary Poisson processes in the mollusc Navanax inermis.

    Science.gov (United States)

    Cappell, M S; Spray, D C; Bennett, M V

    1988-06-28

    Protractor muscles in the gastropod mollusc Navanax inermis exhibit typical spontaneous miniature end plate potentials with mean amplitude 1.71 +/- 1.19 (standard deviation) mV. The evoked end plate potential is quantized, with a quantum equal to the miniature end plate potential amplitude. When their rate is stationary, occurrence of miniature end plate potentials is a random, Poisson process. When non-stationary, spontaneous miniature end plate potential occurrence is a non-stationary Poisson process, a Poisson process with the mean frequency changing with time. This extends the random Poisson model for miniature end plate potentials to the frequently observed non-stationary occurrence. Reported deviations from a Poisson process can sometimes be accounted for by the non-stationary Poisson process and more complex models, such as clustered release, are not always needed.

  10. Stationary power fuel cell commercialization status worldwide

    Energy Technology Data Exchange (ETDEWEB)

    Williams, M.C. [Dept. of Energy, Morgantown, WV (United States)

    1996-12-31

    Fuel cell technologies for stationary power are set to play a role in power generation applications worldwide. The worldwide fuel cell vision is to provide powerplants for the emerging distributed generation and on-site markets. Progress towards commercialization has occurred in all fuel cell development areas. Around 100 ONSI phosphoric acid fuel cell (PAFC) units have been sold, with significant foreign sales in Europe and Japan. Fuji has apparently overcome its PAFC decay problems. Industry-driven molten carbonate fuel cell (MCFC) programs in Japan and the U.S. are conducting megawatt (MW)-class demonstrations, which are bringing the MCFC to the verge of commercialization. Westinghouse Electric, the acknowledged world leader in tubular solid oxide fuel cell (SOFC) technology, continues to set performance records and has completed construction of a 4-MW/year manufacturing facility in the U.S. Fuel cells have also taken a major step forward with the conceptual development of ultra-high efficiency fuel cell/gas turbine plants. Many SOFC developers in Japan, Europe, and North America continue to make significant advances.

  11. Multi-phase partitioning, ecological risk and fate of acidic pharmaceuticals in a wastewater receiving river: The role of colloids

    International Nuclear Information System (INIS)

    Duan, Yan-Ping; Meng, Xiang-Zhou; Wen, Zhi-Hao; Ke, Run-Hui; Chen, Ling

    2013-01-01

    The occurrence and multi-phase distribution of five pharmaceutical compounds were investigated in an urban wastewater treatment plant (WWTP) receiving river by analysis of pharmaceuticals in sediment, particulate matter, conventional dissolved phase (> 0.7 μm), colloidal phase (5 kDa to 0.7 μm), and truly dissolved phase (< 5 kDa) water. Diclofenac was found in all samples, followed by clofibric acid, ibuprofen, ketoprofen, and naproxen with the decreasing detection frequency. All targets in WWTP outfall site were higher than those in the upstream and downstream, indicating that the WWTP is an important input source of pharmaceuticals in the river. The colloidal phase contributed 10–14% of ketoprofen, 8–26% of naproxen, 17–36% of clofibric acid, 22–33% of diclofenac, and 9–28% of ibuprofen in the aquatic system, suggesting the colloids will play an important role as carrier to contaminants in the aquatic environment. Based on truly dissolved concentrations of pharmaceuticals in water, only the risk quotient (RQ) value for diclofenac towards fish was higher than 1, indicating it poses a potential risk to aquatic organisms. Finally, a Level III fugacity model was used to further assess the environmental fate of the selected pharmaceuticals (exemplified for clofibric acid and diclofenac). Both clofibric acid and diclofenac tend to accumulate in water compartment with the percentage of 99.7% and 60.6%, respectively. Advection in river is a significant loss process for clofibric acid (56.4%) and diclofenac (54.4%). - Highlights: ► WWTP is the main source of pharmaceuticals to the receiving river in Shanghai. ► The colloids contribute 9–36% to the total pharmaceutical concentration in water. ► Truly dissolved diclofenac poses a potential risk to aquatic organisms. ► Clofibric acid and diclofenac tend to accumulate in water compartment

  12. Multi-phase partitioning, ecological risk and fate of acidic pharmaceuticals in a wastewater receiving river: The role of colloids

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Yan-Ping [State Key Laboratory of Pollution Control and Resources Reuse, College of Environmental Science and Engineering, Tongji University, Shanghai 200092 (China); Meng, Xiang-Zhou, E-mail: xzmeng@tongji.edu.cn [State Key Laboratory of Pollution Control and Resources Reuse, College of Environmental Science and Engineering, Tongji University, Shanghai 200092 (China); Wen, Zhi-Hao [State Key Laboratory of Pollution Control and Resources Reuse, College of Environmental Science and Engineering, Tongji University, Shanghai 200092 (China); Ke, Run-Hui [China National Research Institute of Food and Fermentation Industries, Beijing 100027 (China); Chen, Ling [State Key Laboratory of Pollution Control and Resources Reuse, College of Environmental Science and Engineering, Tongji University, Shanghai 200092 (China)

    2013-03-01

    The occurrence and multi-phase distribution of five pharmaceutical compounds were investigated in an urban wastewater treatment plant (WWTP) receiving river by analysis of pharmaceuticals in sediment, particulate matter, conventional dissolved phase (> 0.7 μm), colloidal phase (5 kDa to 0.7 μm), and truly dissolved phase (< 5 kDa) water. Diclofenac was found in all samples, followed by clofibric acid, ibuprofen, ketoprofen, and naproxen with the decreasing detection frequency. All targets in WWTP outfall site were higher than those in the upstream and downstream, indicating that the WWTP is an important input source of pharmaceuticals in the river. The colloidal phase contributed 10–14% of ketoprofen, 8–26% of naproxen, 17–36% of clofibric acid, 22–33% of diclofenac, and 9–28% of ibuprofen in the aquatic system, suggesting the colloids will play an important role as carrier to contaminants in the aquatic environment. Based on truly dissolved concentrations of pharmaceuticals in water, only the risk quotient (RQ) value for diclofenac towards fish was higher than 1, indicating it poses a potential risk to aquatic organisms. Finally, a Level III fugacity model was used to further assess the environmental fate of the selected pharmaceuticals (exemplified for clofibric acid and diclofenac). Both clofibric acid and diclofenac tend to accumulate in water compartment with the percentage of 99.7% and 60.6%, respectively. Advection in river is a significant loss process for clofibric acid (56.4%) and diclofenac (54.4%). - Highlights: ► WWTP is the main source of pharmaceuticals to the receiving river in Shanghai. ► The colloids contribute 9–36% to the total pharmaceutical concentration in water. ► Truly dissolved diclofenac poses a potential risk to aquatic organisms. ► Clofibric acid and diclofenac tend to accumulate in water compartment.

  13. Morphology and phase transformations of tin oxide nanostructures synthesized by the hydrothermal method in the presence of dicarboxylic acids

    International Nuclear Information System (INIS)

    Zima, Tatyana; Bataev, Ivan

    2016-01-01

    A new approach to the synthesis of non-stoichiometric tin oxide structures with different morphologies and the phase compositions has been evaluated. The nanostructures were synthesized by hydrothermal treatment of the mixtures of dicarboxylic acids ― aminoterephthalic or oxalic ― with nanocrystalline SnO 2 powder, which was obtained via the sol-gel technology. The products were characterized by Raman and IR spectroscopy, SEM, HRTEM, and XRD analysis. It was shown that the controlled addition of a dicarboxylic acid leads not only to a change in the morphology of the nanostructures, but also to SnO 2 –SnO 2 /Sn 3 O 4 –Sn 3 O 4 –SnO phase transformations. A single-phase Sn 3 O 4 in the form of the well-separated hexagonal nanoplates and mixed SnO 2 /Sn 3 O 4 phases in the form of hierarchical flower-like structures were obtained in the presence of organic additives. The effects of concentration, redox activity of the acids and heat treatment on the basic characteristics of the synthesized tin oxide nanostructures and phase transformations in the synthesized materials are discussed. - Graphical abstract: The controlled addition of aminoterephthalic or oxalic acid leads not only to a change in the morphology of the nanostructures, but also to SnO 2 –SnO 2 /Sn 3 O 4 –Sn 3 O 4 –SnO phase transformations. - Highlights: • A new approach to the synthesis of non-stoichiometric tin oxide structures is studied. • Tin oxide structures are synthesized via hydrothermal method with dicarboxylic acids. • Morphology and phase composition are changed with redox activity and dosage of acid. • The redox activity of acid has an effect on ratio of SnO and SnO 2 in crystal structure. • A pure phase Sn 3 O 4 nanoplates and SnO 2 /Sn 3 O 4 hierarchical structures are formed.

  14. Stationary black holes as holographs

    Energy Technology Data Exchange (ETDEWEB)

    Racz, Istvan [Yukawa Institute for Theoretical Physics, Kyoto University, Kyoto 606-01 (Japan); MTA KFKI, Reszecske- es Magfizikai Kutatointezet, H-1121 Budapest, Konkoly Thege Miklos ut 29-33 (Hungary)

    2007-11-21

    Smooth spacetimes possessing a (global) one-parameter group of isometries and an associated Killing horizon in Einstein's theory of gravity are investigated. No assumption concerning the asymptotic structure is made; thereby, the selected spacetimes may be considered as generic distorted stationary black holes. First, spacetimes of arbitrary dimension, n {>=} 3, with matter satisfying the dominant energy condition and allowing a non-zero cosmological constant are investigated. In this part, complete characterization of the topology of the event horizon of 'distorted' black holes is given. It is shown that the topology of the event horizon of 'distorted' black holes is allowed to possess a much larger variety than that of the isolated black hole configurations. In the second part, four-dimensional (non-degenerate) electrovac distorted black hole spacetimes are considered. It is shown that the spacetime geometry and the electromagnetic field are uniquely determined in the black hole region once the geometry of the bifurcation surface and one of the electromagnetic potentials are specified there. Conditions guaranteeing the same type of determinacy, in a neighbourhood of the event horizon, on the domain of outer communication side are also investigated. In particular, they are shown to be satisfied in the analytic case.

  15. Eddy covariance captures four-phase crassulacean acid metabolism (CAM) gas exchange signature in Agave.

    Science.gov (United States)

    Owen, Nick A; Choncubhair, Órlaith Ní; Males, Jamie; Del Real Laborde, José Ignacio; Rubio-Cortés, Ramón; Griffiths, Howard; Lanigan, Gary

    2016-02-01

    Mass and energy fluxes were measured over a field of Agave tequilana in Mexico using eddy covariance (EC) methodology. Data were gathered over 252 d, including the transition from wet to dry periods. Net ecosystem exchanges (FN,EC ) displayed a crassulacean acid metabolism (CAM) rhythm that alternated from CO2 sink at night to CO2 source during the day, and partitioned canopy fluxes (FA,EC ) showed a characteristic four-phase CO2 exchange pattern. Results were cross-validated against diel changes in titratable acidity, leaf-unfurling rates, energy exchange fluxes and reported biomass yields. Projected carbon balance (g C m(-2)  year(-1) , mean ± 95% confidence interval) indicated the site was a net sink of -333 ± 24, of which contributions from soil respiration were +692 ± 7, and FA,EC was -1025 ± 25. EC estimated biomass yield was 20.1 Mg (dry) ha(-1)  year(-1) . Average integrated daily FA,EC was -234 ± 5 mmol CO2  m(-2)  d(-1) and persisted almost unchanged after 70 d of drought conditions. Regression analyses were performed on the EC data to identify the best environmental predictors of FA . Results suggest that the carbon acquisition strategy of Agave offers productivity and drought resilience advantages over conventional semi-arid C3 and C4 bioenergy candidates. © 2015 John Wiley & Sons Ltd.

  16. Induced Smectic X Phase Through Intermolecular Hydrogen-Bonded Liquid Crystals Formed Between Citric Acid and p- n-(Octyloxy)Benzoic Acid

    Science.gov (United States)

    Sundaram, S.; Subhasri, P.; Rajasekaran, T. R.; Jayaprakasam, R.; Senthil, T. S.; Vijayakumar, V. N.

    2017-08-01

    Hydrogen-bonded liquid crystal (HBLC) is synthesized from citric acid (CA) and 4-(octyloxy)benzoic acid (8OBA) with different mole ratios. Fourier transform infrared spectroscopy (FT-IR) confirms the presence of hydrogen bond between CA and 8OBA. Nuclear magnetic resonance (NMR) spectroscopic studies validate the intermolecular complementary, cyclic type of hydrogen bond, and molecular environment in the designed HBLC complex. Powder X-ray diffraction analysis reveals the monoclinic nature of liquid crystal complex in solid phase. Liquid crystal parameters such as phase transition temperature and enthalpy values for the corresponding mesogenic phases are investigated using a polarizing optical microscope (POM) and differential scanning calorimetry (DSC). It is observed that the change in chain length and steric hindrance while increasing the mole ratio in HBLC complex induces a new smectic X (Sm X) along with higher-order smectic G (Sm G) phases by quenching of smectic C (Sm C). From the experimental observations, induced Sm X phase has been identified as a finger print texture. Also, Sm G is a multi-colored mosaic texture in 1:1, 1:2, and 1:3 mol ratios. The optical tilt angle, thermal stability factor, and enhanced thermal span width of CA + 8OBA complex are discussed.

  17. Fatty acid esters-based composite phase change materials for thermal energy storage in buildings

    International Nuclear Information System (INIS)

    Sarı, Ahmet; Karaipekli, Ali

    2012-01-01

    In this study, fatty acid esters-based composite phase change materials (PCMs) for thermal energy storage were prepared by blending erythritol tetrapalmitate (ETP) and erythritol tetrastearate (ETS) with diatomite and expanded perlite (EP). The maximum incorporation percentage for ETP and ETS into diatomite and EP was found to be 57 wt% and 62 wt%, respectively without melted PCM seepage from the composites. The morphologies and compatibilities of the composite PCMs were structurally characterized using scanning electron microscope (SEM) and Fourier transformation infrared (FT–IR) analysis techniques. Thermal energy storage properties of the composite PCMs were determined by differential scanning calorimetry (DSC) analysis. The DSC analyses results indicated that the composite PCMs were good candidates for building applications in terms of their large latent heat values and suitable phase change temperatures. The thermal cycling test including 1000 melting and freezing cycling showed that composite PCMs had good thermal reliability and chemical stability. TG analysis revealed that the composite PCMs had good thermal durability above their working temperature ranges. Moreover, in order to improve the thermal conductivity of the composite PCMs, the expanded graphite (EG) was added to them at different mass fractions (2%, 5%, and 10%). The best results were obtained for the composite PCMs including 5wt% EG content in terms of the increase in thermal conductivity values and the decrease amount in latent heat capacity. The improvement in thermal conductivity values of ETP/Diatomite, ETS/Diatomite, ETP/EP and ETS/EP were found to be about 68%, 57%, 73% and 75%, respectively. Highlights: ► Fatty acid esters-based composite PCMs were prepared by blending ETP and ETS with diatomite and expanded perlite. ► The composite PCMs were characterized by using SEM, FT–IR, DSC and TG analysis methods. ► The DSC results indicated that the composites PCMs had good thermal

  18. Ru decorated carbon nanotubes - a promising catalyst for reforming bio-based acetic acid in the aqueous phase

    NARCIS (Netherlands)

    de Vlieger, Dennis; Lefferts, Leonardus; Seshan, Kulathuiyer

    2014-01-01

    Catalytic reforming of biomass derived waste streams in the aqueous phase is a promising process for the production of sustainable hydrogen. Acetic acid will be a major component (up to 20 wt%) in many anticipated gasification feed streams (e.g. the aqueous fraction of pyrolysis oil). Conventional

  19. In situ observation of a deprotonation driven phase transformation-4,4'-Biphenyldicarboxylic acide on Au(111)

    NARCIS (Netherlands)

    Schwarz, Daniel; van Gastel, Raoul; Zandvliet, Henricus J.W.; Poelsema, Bene

    2013-01-01

    We have studied the growth of 4,4′-biphenyldicarboxylic acid (BDA) domains on Au(111) by means of low-energy electron microscopy (LEEM) and selective area low-energy electron diffraction (μLEED). Between 300 and 400 K, BDA forms three different 2-D crystalline phases, which are attributed to

  20. SOLVENT EFFECTS IN THE LIQUID-PHASE HYDRATION OF CYCLOHEXENE CATALYZED BY A MACROPOROUS STRONG ACID ION-EXCHANGE RESIN

    NARCIS (Netherlands)

    PANNEMAN, HJ; BEENACKERS, AACM

    1992-01-01

    The liquid-phase hydration of cyclohexene, a pseudo first order reversible reaction catalyzed by a strong acid ion exchange resin, macroporous Amberlite XE 307, was investigated in solvent mixtures of water and sulfolane. A decrease by a factor of 3 and 6 is observed in the experimentally measured

  1. Dosage simultané des acides sorbique et benzoïque dans les vins par chromatographie en phase gazeuse

    Directory of Open Access Journals (Sweden)

    F. Ureta

    1984-12-01

    Dans ce travail nous décrivons une méthode par chromatographie en phase gazeuse sur colonne capillaire qui permet en une seule opération de déterminer les acides benzoïque et sorbique dans les vins.

  2. Measuring Gas-Phase Basicities of Amino Acids Using an Ion Trap Mass Spectrometer: A Physical Chemistry Laboratory Experiment

    Science.gov (United States)

    Sunderlin, Lee S.; Ryzhov, Victor; Keller, Lanea M. M.; Gaillard, Elizabeth R.

    2005-01-01

    An experiment is performed to measure the relative gas-phase basicities of a series of five amino acids to compare the results to literature values. The experiments use the kinetic method for deriving ion thermochemistry and allow students to perform accurate measurements of thermodynamics in a relatively short time.

  3. Conformational preferences of γ-aminobutyric acid in the gas phase and in water

    Science.gov (United States)

    Song, Il Keun; Kang, Young Kee

    2012-09-01

    The conformational study of γ-aminobutyric acid (GABA) has been carried out at the M06-2X/cc-pVTZ level of theory in the gas phase and the SMD M06-2X/cc-pVTZ level of theory in water. In the gas phase, the folded conformation gG1 with gauche- and gauche+ conformations for the Cβsbnd Cα and Cγsbnd Cβ bonds, respectively, is found to be lowest in energy and enthalpy, which can be ascribed to the favored hyperconjugative n → π* interaction between the lone electron pair of the amine nitrogen atom and the Cdbnd O bond of the carboxylic group and the favored antiparallel dipole-dipole interaction between the Nsbnd H bond and the Cdbnd O bond. In addition, the intramolecular hydrogen bonds between the carboxylic group and the amine Nsbnd H group have contributed to stabilize some low-energy conformers. However, the most preferred conformation is found to be tG1 and more stable by 0.4 kcal/mol in ΔG than the conformer gG1, in which the favored entropic term due to the conformational flexibility and the other favored n → σ*, σ → σ*, and π → σ* interactions seem to play a role. The conformational preferences of the neutral GABA calculated by ΔG's are reasonably consistent with the populations deduced from FT microwave spectroscopy in supersonic jets combined with laser ablation. In water, the two folded conformers Gg and gG of the zwitterionic GABA are dominantly populated, each of which has the population of 47%, and the hydrogen bond between the ammonium Nsbnd H group and the lone electron pair of the Csbnd O- group seems to be crucial in stabilizing these conformers. Our calculated result that the folded conformers preferentially exist in water is consistent with the 1H NMR experiments in D2O.

  4. Interactions of hydrated divalent metal cations with nucleic acid bases. How to relate the gas phase data to solution situation and binding selectivity in nucleic acids

    Czech Academy of Sciences Publication Activity Database

    Šponer, Judit E.; Sychrovský, Vladimír; Hobza, Pavel; Šponer, Jiří

    2004-01-01

    Roč. 6, č. 10 (2004), s. 2772-2780 ISSN 1463-9076 R&D Projects: GA MŠk LN00A016; GA MŠk LN00A032 Grant - others:Wellcome Trust(GB) GR067507MF Institutional research plan: CEZ:AV0Z5004920 Keywords : nucleic acids * gas phase * guanine Subject RIV: BO - Biophysics Impact factor: 2.076, year: 2004

  5. Rapid Determination of Bile Acids in Bile from Various Mammals by Reversed-Phase Ultra-Fast Liquid Chromatography.

    Science.gov (United States)

    Si, Gu Leng Ri; Yao, Peng; Shi, Luwen

    2015-08-01

    A valid and efficient reversed-phase ultra-fast liquid chromatography method was developed for the simultaneous determination of 13 bile acids in the bile of three mammal species, including rat, pig and human gallstone patients. Chromatographic separation was performed with a Shim-pack XR-ODS column, and the mobile phase consisted of acetonitrile and potassium phosphate buffer (pH 2.6) at a flow rate of 0.5 mL min(-1). The linear detection range of most bile acids ranged from 2 to 600 ng µL(-1) with a good correlation coefficient (>0.9995). The precision of each bile acid was bile acids were separated in 15 min with satisfactory resolution, and the total analysis time was 18 min, including equilibration. The method was successfully applied in rapid screening of bile samples from the three mammals. Significant metabolic frameworks of bile acids among various species were observed, whereas considerable quantitative variations in both inter- and intraspecies were also observed, especially for gallstone patients. Our results suggest that detecting the change of bile acid profiles could be applied for the diagnosis of gallstone disease. © Crown copyright 2014.

  6. Nuclear dynamics in the metastable phase of the solid acid caesium hydrogen sulfate.

    Science.gov (United States)

    Krzystyniak, Maciej; Drużbicki, Kacper; Fernandez-Alonso, Felix

    2015-12-14

    High-resolution spectroscopic measurements using thermal and epithermal neutrons and first-principles calculations within the framework of density-functional theory are used to investigate the nuclear dynamics of light and heavy species in the metastable phase of caesium hydrogen sulfate. Within the generalised-gradient approximation, extensive calculations show that both 'standard' and 'hard' formulations of the Perdew-Burke-Ernzerhof functional supplemented by Tkatchenko-Scheffler dispersion corrections provide an excellent description of the known structure, underlying vibrational density of states, and nuclear momentum distributions measured at 10 and 300 K. Encouraged by the agreement between experiment and computational predictions, we provide a quantitative appraisal of the quantum contributions to nuclear motions in this solid acid. From this analysis, we find that only the heavier caesium atoms reach the classical limit at room temperature. Contrary to naïve expectation, sulfur exhibits a more pronounced quantum character relative to classical predictions than the lighter oxygen atom. We interpret this hitherto unexplored nuclear quantum effect as arising from the tighter binding environment of this species in this technologically relevant material.

  7. Gas-phase Dehydration of Glycerol over Supported Silicotungstic Acids Catalysts

    International Nuclear Information System (INIS)

    Kim, Yong Tae; Park, Eun Duck; Jung, Kwang Deog

    2010-01-01

    The gas-phase dehydration of glycerol to acrolein was carried out over 10 wt % HSiW catalysts supported on different supports, viz. γ-Al 2 O 3 , SiO 2 -Al 2 O 3 , TiO 2 , ZrO 2 , SiO 2 , AC, CeO 2 and MgO. The same reaction was also conducted over each support without HSiW for comparison. Several characterization techniques, N 2 -physisorption, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), the temperature-programmed desorption of ammonia (NH 3 - TPD), temperature-programmed oxidation (TPO) with mass spectroscopy and CHNS analysis were employed to characterize the catalysts. The glycerol conversion generally increased with increasing amount of acid sites. Ceria showed the highest 1-hydroxyacetone selectivity at 315 .deg. C among the various metal oxides. The supported HSiW catalyst showed superior catalytic activity to that of the corresponding support. Among the supported HSiW catalysts, HSiW/ZrO 2 and HSiW/SiO 2 -Al 2 O 3 showed the highest acrolein selectivity. In the case of HSiW/ZrO 2 , the initial catalytic activity was recovered after the removal of the accumulated carbon species at 550 .deg. C in the presence of oxygen

  8. Gas-phase hydrolysis of triplet SO2: A possible direct route to atmospheric acid formation

    Science.gov (United States)

    Donaldson, D. James; Kroll, Jay A.; Vaida, Veronica

    2016-07-01

    Sulfur chemistry is of great interest to the atmospheric chemistry of several planets. In the presence of water, oxidized sulfur can lead to new particle formation, influencing climate in significant ways. Observations of sulfur compounds in planetary atmospheres when compared with model results suggest that there are missing chemical mechanisms. Here we propose a novel mechanism for the formation of sulfurous acid, which may act as a seed for new particle formation. In this proposed mechanism, the lowest triplet state of SO2 (3B1), which may be accessed by near-UV solar excitation of SO2 to its excited 1B1 state followed by rapid intersystem crossing, reacts directly with water to form H2SO3 in the gas phase. For ground state SO2, this reaction is endothermic and has a very high activation barrier; our quantum chemical calculations point to a facile reaction being possible in the triplet state of SO2. This hygroscopic H2SO3 molecule may act as a condensation nucleus for water, giving rise to facile new particle formation (NPF).

  9. Monolithic columns based on a poly(styrene-divinylbenzene-methacrylic acid) copolymer for capillary liquid chromatography of small organic molecules

    Czech Academy of Sciences Publication Activity Database

    Svobodová, A.; Křížek, T.; Širc, Jakub; Šálek, Petr; Tesařová, E.; Coufal, P.; Štulík, K.

    2011-01-01

    Roč. 1218, č. 11 (2011), s. 1544-1547 ISSN 0021-9673 R&D Projects: GA AV ČR KAN200520804 Institutional research plan: CEZ:AV0Z40500505 Keywords : capillary liquid chromatography * methacrylic acid * polystyrene-based monolithic stationary phase Subject RIV: EI - Biotechnology ; Bionics Impact factor: 4.531, year: 2011

  10. Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

    Science.gov (United States)

    Martha J.M. Wells; Jerry L. Michael

    1987-01-01

    Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

  11. Acidic ionic liquids for n-alkane isomerization in a liquid-liquid or slurry-phase reaction mode

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, C.; Hager, V.; Geburtig, D.; Kohr, C.; Wasserscheid, P. [Erlangen-Nuernberg Univ. (Germany). Lehrstuhl fuer Chemische Reaktionstechnik; Haumann, M. [Chemical Reaction Engineering, FAU Busan Campus, Korea (Korea, Republic of)

    2011-07-01

    Highly acidic ionic liquid (IL) catalysts offer the opportunity to convert n-alkanes at very low reaction temperatures. The results of IL catalyzed isomerization and cracking reactions of pure n-octane are presented. Influence of IL composition, [C{sub 4}C{sub 1}Im]Cl / AlCl{sub 3} / H{sub 2}SO{sub 4} and [C{sub 4}C{sub 1}Im]Cl / AlCl{sub 3} / 1-chlorooctane, on catalyst activity and selectivities to branched alkanes was investigated. Acidic chloroaluminate IL catalysts form liquid-liquid biphasic systems with unpolar organic product mixtures. Thus, recycling of the acidic IL is enabled by simple phase separation in the liquid-liquid biphasic reaction mode or the IL can be immobilized on an inorganic support with a large specific surface area. These supported ionic liquid phase (SILP) catalysts offer the advantage to get a macroscopically heterogeneous system while still preserving all benefits of the homogeneous catalyst which can be used for the slurry-phase n-alkane isomerization. The interaction of the solid support and acidic IL influences strongly the catalytic activity. (orig.)

  12. Dampers for Stationary Labyrinth Seals

    Science.gov (United States)

    El-Aini, Yehia; Mitchell, William; Roberts, Lawrence; Montgomery, Stuart; Davis, Gary

    2011-01-01

    Vibration dampers have been invented that are incorporated as components within the stationary labyrinth seal assembly. These dampers are intended to supplement other vibration-suppressing features of labyrinth seals in order to reduce the incidence of high-cycle-fatigue failures, which have been known to occur in the severe vibratory environments of jet engines and turbopumps in which labyrinth seals are typically used. A vibration damper of this type includes several leaf springs and/or a number of metallic particles (shot) all held in an annular seal cavity by a retaining ring. The leaf springs are made of a spring steel alloy chosen, in conjunction with design parameters, to maintain sufficient preload to ensure effectiveness of damping at desired operating temperatures. The cavity is vented via a small radial gap between the retaining ring and seal housing. The damping mechanism is complex. In the case of leaf springs, the mechanism is mainly friction in the slippage between the seal housing and individual dampers. In the case of a damper that contains shot, the damping mechanism includes contributions from friction between individual particles, friction between particles and cavity walls, and dissipation of kinetic energy of impact. The basic concept of particle/shot vibration dampers has been published previously; what is new here is the use of such dampers to suppress traveling-wave vibrations in labyrinth seals. Damping effectiveness depends on many parameters, including, but not limited to, coefficient of friction, mode shape, and frequency and amplitude of vibrational modes. In tests, preloads of the order of 6 to 15 lb (2.72 to 6.8 kilograms) per spring damper were demonstrated to provide adequate damping levels. Effectiveness of shot damping of vibrations having amplitudes from 20 to 200 times normal terrestrial gravitational acceleration (196 to 1,960 meters per square second) and frequencies up to 12 kHz was demonstrated for shot sizes from 0.032 to

  13. Stationary axisymmetric Einstein--Maxwell field equations

    International Nuclear Information System (INIS)

    Catenacci, R.; Diaz Alonso, J.

    1976-01-01

    We show the existence of a formal identity between Einstein's and Ernst's stationary axisymmetric gravitational field equations and the Einstein--Maxwell and the Ernst equations for the electrostatic and magnetostatic axisymmetric cases. Our equations are invariant under very simple internal symmetry groups, and one of them appears to be new. We also obtain a method for associating two stationary axisymmetric vacuum solutions with every electrostatic known

  14. Stationary infinitely divisible processes

    DEFF Research Database (Denmark)

    Barndorff-Nielsen, Ole E.

    Several recent strands of work has led to the consideration of various types of continuous time stationary and infinitely divisible processes. A review of these types, with some new results, is presented.......Several recent strands of work has led to the consideration of various types of continuous time stationary and infinitely divisible processes. A review of these types, with some new results, is presented....

  15. Gas chromatography of alkylphosphonic and dialkylphosphinic acids

    International Nuclear Information System (INIS)

    Gasco, L.; Barrera, R.; Ramirez, A.; Martin Munoz, N.

    1978-01-01

    After carrying out an optimization study on the separation conditions for the TMS-derivatives, of the hexyl-, cyclohexyl-, heptyl-, and octyl-phosphonic acids; dihexyl-, dicyclohexyl-, heptyl-, and octyl-phosphinic acids, and dioctylphosphine oxide, their retention indices (I) at two temperatures and on the 0V-1 and 0V-17 stationary phase were determined. Correlations between I and molecular structure were established. Calibration factors of these compounds in the flame ionization detector were studied, and the results analized taking into account the variables afecting the quantitative results. These results were unbiased but they had a lower precission than usually achieveble in gas chromatography. (author)

  16. Preparation of Paraffin@Poly(styrene-co-acrylic acid) Phase Change Nanocapsules via Combined Miniemulsion/Emulsion Polymerization.

    Science.gov (United States)

    Zhang, Feng; Liu, Tian-Yu; Hou, Gui-Hua; Guan, Rong-Feng; Zhang, Jun-Hao

    2018-06-01

    The fast development of solid-liquid phase change materials calls for nanomaterials with large specific surface area for rapid heat transfer and encapsulation of phase change materials to prevent potential leakage. Here we report a combined miniemulsion/emulsion polymerization method to prepare poly(styrene-co-acrylic acid)-encapsulated paraffin (paraffin@P(St-co-AA)) nanocapsules. The method could suppress the shortcomings of common miniemulsion polymerization (such as evaporation of monomer and decomposition of initiator during ultrasonication). The paraffin@P(St-co-AA) nanocapsules are uniform in size and the polymer shell can be controlled by the weight ratio of St to paraffin. The phase change behavior of the nanocapsules is similar to that of pure paraffin. We believe our method can also be utilized to synthesize other core-shell phase change materials.

  17. Simultaneous measurements of formaldehyde and nitrous acid in dews and gas phase in the atmosphere of Santiago, Chile

    Science.gov (United States)

    Rubio, María A.; Lissi, Eduardo; Villena, Guillermo; Elshorbany, Y. F.; Kleffmann, Jörg; Kurtenbach, Ralf; Wiesen, Peter

    2009-12-01

    The amounts of formaldehyde and nitrous acid (HONO) in gas phase and dews of Santiago de Chile were simultaneously measured. Formaldehyde concentrations values in the liquid phase (dews) correlate fairly well with those in the gaseous phase and are even higher than those expected from gas-dew equilibrium. On the other hand, nitrite concentrations in dews were considerably smaller (ca. 15 times) than those expected from the gas-phase concentrations. This under-saturation is attributed to diffusion limitations due to the relatively large HONO solubility. In agreement with this, under-saturation increases with the rate of dew formation and the pH of the collected waters, factors that should increase the rate of gas to liquid HONO transfer required to reach equilibrium.

  18. Equilibrium aluminium hydroxo-oxalate phases during initial clay formation; H +-Al 3+-oxalic acid-Na + system

    Science.gov (United States)

    Bilinski, Halka; Horvath, Laszlo; Ingri, Nils; Sjöberg, Staffan

    1986-09-01

    The conditions necessary for initial clay formation have been studied in different model systems comprising different organic acids besides Si and Al. In the present paper the solid phases and the precipitation boundary characterizing the subsystem H +-Al 3+-oxalic acid (H 2L) are discussed. pH and tyndallometric measurements were performed in an ionic medium of 0.6 M Na(Cl) at 25 °C. The two phases Al 3(OH) 7(C 2O 4) · 3H 2O (phase I) and NaAl(OH) 2(C 2O 4) · 3H 2O (phase II) determine the precipitation boundary. The following formation constants for the two phases were deduced: lgβ1 = lg([ Al3+] -3[ H2C2O4] -1[ H+] 9 = -21.87 ± 0.08 and lgβ11 = lg([ Al3+] -1[ H2C2O4] -1[ H+] 4 = -5.61 ± 0.06. Phase I exists in the range [ Al] tot≥ 10 -4.4moldm-3,[ H2C2O4] tot ≥ 10 -4.9moldm-3 and at pH oxalic-rich natural waters. The more soluble sodium phase is unlikely to exist in natural waters. The two phases are metastable relative to crystalline gibbsite and may be considered as the first precipitation step in the transition from aqueous Al oxalates down to stable Al hydroxide. Model calculations illustrating these competing hydrolysis-complexation reactions are discussed in terms of predominance and speciation diagrams. The solid phases have been characterized by X-ray analysis of powders, TGA and IR spectra, and tentative structures are proposed. Phase I seems to be an octahedral layer structure, in which 3/5 of the octahedral sites between two close packed oxygen sheets are occupied by Al 3+ and the oxalate ion acts as a bridge ligand between two aluminium atoms. Phase II forms a more open sheet structure and has ion exchange properties. Powder data for a phase crystallized from the studied solution after a year are also presented. This phase, Na 4Al 2(OH) 2(C 2O 4) 4 · 10H 2O, supports the results from the equilibrium analysis of recent solution data by SJöBERG and ÖHMAN (1985), who have found the dinuclear complex Al 2(OH) 2(C 2O 4) 44- to exist in a

  19. Stationary Liquid Fuel Fast Reactor

    International Nuclear Information System (INIS)

    Yang, Won Sik; Grandy, Andrew; Boroski, Andrew; Krajtl, Lubomir; Johnson, Terry

    2015-01-01

    For effective burning of hazardous transuranic (TRU) elements of used nuclear fuel, a transformational advanced reactor concept named SLFFR (Stationary Liquid Fuel Fast Reactor) was proposed based on stationary molten metallic fuel. The fuel enters the reactor vessel in a solid form, and then it is heated to molten temperature in a small melting heater. The fuel is contained within a closed, thick container with penetrating coolant channels, and thus it is not mixed with coolant nor flow through the primary heat transfer circuit. The makeup fuel is semi- continuously added to the system, and thus a very small excess reactivity is required. Gaseous fission products are also removed continuously, and a fraction of the fuel is periodically drawn off from the fuel container to a processing facility where non-gaseous mixed fission products and other impurities are removed and then the cleaned fuel is recycled into the fuel container. A reference core design and a preliminary plant system design of a 1000 MWt TRU- burning SLFFR concept were developed using TRU-Ce-Co fuel, Ta-10W fuel container, and sodium coolant. Conservative design approaches were adopted to stay within the current material performance database. Detailed neutronics and thermal-fluidic analyses were performed to develop a reference core design. Region-dependent 33-group cross sections were generated based on the ENDF/B-VII.0 data using the MC2-3 code. Core and fuel cycle analyses were performed in theta-r-z geometries using the DIF3D and REBUS-3 codes. Reactivity coefficients and kinetics parameters were calculated using the VARI3D perturbation theory code. Thermo-fluidic analyses were performed using the ANSYS FLUENT computational fluid dynamics (CFD) code. Figure 0.1 shows a schematic radial layout of the reference 1000 MWt SLFFR core, and Table 0.1 summarizes the main design parameters of SLFFR-1000 loop plant. The fuel container is a 2.5 cm thick cylinder with an inner radius of 87.5 cm. The fuel

  20. Stationary Liquid Fuel Fast Reactor

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Won Sik [Purdue Univ., West Lafayette, IN (United States); Grandy, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States); Boroski, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States); Krajtl, Lubomir [Argonne National Lab. (ANL), Argonne, IL (United States); Johnson, Terry [Argonne National Lab. (ANL), Argonne, IL (United States)

    2015-09-30

    For effective burning of hazardous transuranic (TRU) elements of used nuclear fuel, a transformational advanced reactor concept named SLFFR (Stationary Liquid Fuel Fast Reactor) was proposed based on stationary molten metallic fuel. The fuel enters the reactor vessel in a solid form, and then it is heated to molten temperature in a small melting heater. The fuel is contained within a closed, thick container with penetrating coolant channels, and thus it is not mixed with coolant nor flow through the primary heat transfer circuit. The makeup fuel is semi- continuously added to the system, and thus a very small excess reactivity is required. Gaseous fission products are also removed continuously, and a fraction of the fuel is periodically drawn off from the fuel container to a processing facility where non-gaseous mixed fission products and other impurities are removed and then the cleaned fuel is recycled into the fuel container. A reference core design and a preliminary plant system design of a 1000 MWt TRU- burning SLFFR concept were developed using TRU-Ce-Co fuel, Ta-10W fuel container, and sodium coolant. Conservative design approaches were adopted to stay within the current material performance database. Detailed neutronics and thermal-fluidic analyses were performed to develop a reference core design. Region-dependent 33-group cross sections were generated based on the ENDF/B-VII.0 data using the MC2-3 code. Core and fuel cycle analyses were performed in theta-r-z geometries using the DIF3D and REBUS-3 codes. Reactivity coefficients and kinetics parameters were calculated using the VARI3D perturbation theory code. Thermo-fluidic analyses were performed using the ANSYS FLUENT computational fluid dynamics (CFD) code. Figure 0.1 shows a schematic radial layout of the reference 1000 MWt SLFFR core, and Table 0.1 summarizes the main design parameters of SLFFR-1000 loop plant. The fuel container is a 2.5 cm thick cylinder with an inner radius of 87.5 cm. The fuel

  1. Hydrocarbon fuels from gas phase decarboxylation of hydrolyzed free fatty acid

    KAUST Repository

    Wang, Weicheng

    2012-01-01

    Gas phase decarboxylation of hydrolyzed free fatty acid (FFA) from canola oil has beeninvestigated in two fix-bed reactors by changing reaction parameters such as temperatures,FFA feed rates, and H 2-to-FFA molar ratios. FFA, which contains mostly C 18 aswell as a few C 16, C 20, C 22, and C 24 FFA, was fed into the boiling zone, evaporated, carriedby hydrogen flow at the rate of 0.5-20 ml/min, and reacted with the 5% Pd/C catalystin the reactor. Reactions were conducted atmospherically at 380-450 °C and the products,qualified and quantified through gas chromatography-flame ionization detector(GC-FID), showed mostly n-heptadecane and a few portion of n-C 15, n-C 19, n-C 21, n-C 23 as well as some cracking species. Results showed that FFA conversion increased withincreasing reaction temperatures but decreased with increasing FFA feed rates and H 2-to-FFA molar ratios. The reaction rates were found to decrease with higher temperatureand increase with higher H 2 flow rates. Highly selective heptadecane was achieved byapplying higher temperatures and higher H 2-to-FFA molar ratios. From the results, ascatalyst loading and FFA feed rate were fixed, an optimal reaction temperature of 415 °C as well as H 2-to-FFA molar ratio of 4.16 were presented. These results provided goodbasis for studying the kinetics of decarboxylation process. © 2012 American Society of Mechanical Engineers.

  2. Prostate hypofractionated radiation therapy with injection of hyaluronic acid: acute toxicities in a phase 2 study.

    Science.gov (United States)

    Chapet, Olivier; Decullier, Evelyne; Bin, Sylvie; Faix, Antoine; Ruffion, Alain; Jalade, Patrice; Fenoglietto, Pascal; Udrescu, Corina; Enachescu, Ciprian; Azria, David

    2015-03-15

    Hypofractionated radiation therapy (RT) in prostate cancer can be developed only if the risk of rectal toxicity is controlled. In a multicenter phase 2 trial, hypofractionated irradiation was combined with an injection of hyaluronic acid (HA) to preserve the rectal wall. Tolerance of the injection and acute toxicity rates are reported. The study was designed to assess late grade 2 toxicity rates. The results described here correspond to the secondary objectives. Acute toxicity was defined as occurring during RT or within 3 months after RT and graded according to the Common Terminology Criteria for Adverse Events version 4.0. HA tolerance was evaluated with a visual analog scale during the injection and 30 minutes after injection and then by use of the Common Terminology Criteria at each visit. From 2010 to 2012, 36 patients with low-risk to intermediate-risk prostate cancer were included. The HA injection induced a mean pain score of 4.6/10 ± 2.3. Thirty minutes after the injection, 2 patients still reported pain (2/10 and 3/10), which persisted after the intervention. Thirty-three patients experienced at least 1 acute genitourinary toxicity and 20 patients at least 1 acute gastrointestinal toxicity. Grade 2 toxicities were reported for 19 patients with urinary obstruction, frequency, or both and for 1 patient with proctitis. No grade 3 or 4 toxicities were reported. At the 3-month visit, 4 patients described grade 2 obstruction or frequency, and no patients had any grade 2 gastrointestinal toxicities. The injection of HA makes it possible to deliver hypofractionated irradiation over 4 weeks with a dose per fraction of > 3 Gy, with limited acute rectal toxicity. Copyright © 2015 Elsevier Inc. All rights reserved.

  3. Prostate Hypofractionated Radiation Therapy With Injection of Hyaluronic Acid: Acute Toxicities in a Phase 2 Study

    International Nuclear Information System (INIS)

    Chapet, Olivier; Decullier, Evelyne; Bin, Sylvie; Faix, Antoine; Ruffion, Alain; Jalade, Patrice; Fenoglietto, Pascal; Udrescu, Corina; Enachescu, Ciprian; Azria, David

    2015-01-01

    Purpose: Hypofractionated radiation therapy (RT) in prostate cancer can be developed only if the risk of rectal toxicity is controlled. In a multicenter phase 2 trial, hypofractionated irradiation was combined with an injection of hyaluronic acid (HA) to preserve the rectal wall. Tolerance of the injection and acute toxicity rates are reported. Methods and Materials: The study was designed to assess late grade 2 toxicity rates. The results described here correspond to the secondary objectives. Acute toxicity was defined as occurring during RT or within 3 months after RT and graded according to the Common Terminology Criteria for Adverse Events version 4.0. HA tolerance was evaluated with a visual analog scale during the injection and 30 minutes after injection and then by use of the Common Terminology Criteria at each visit. Results: From 2010 to 2012, 36 patients with low-risk to intermediate-risk prostate cancer were included. The HA injection induced a mean pain score of 4.6/10 ± 2.3. Thirty minutes after the injection, 2 patients still reported pain (2/10 and 3/10), which persisted after the intervention. Thirty-three patients experienced at least 1 acute genitourinary toxicity and 20 patients at least 1 acute gastrointestinal toxicity. Grade 2 toxicities were reported for 19 patients with urinary obstruction, frequency, or both and for 1 patient with proctitis. No grade 3 or 4 toxicities were reported. At the 3-month visit, 4 patients described grade 2 obstruction or frequency, and no patients had any grade 2 gastrointestinal toxicities. Conclusions: The injection of HA makes it possible to deliver hypofractionated irradiation over 4 weeks with a dose per fraction of > 3 Gy, with limited acute rectal toxicity

  4. Prostate Hypofractionated Radiation Therapy With Injection of Hyaluronic Acid: Acute Toxicities in a Phase 2 Study

    Energy Technology Data Exchange (ETDEWEB)

    Chapet, Olivier, E-mail: olivier.chapet@chu-lyon.fr [Department of Radiation Oncology, Hospices Civils de Lyon, Centre Hospitalier Lyon Sud, Pierre Benite (France); EMR3738, Université Lyon 1, Lyon (France); Decullier, Evelyne; Bin, Sylvie [Pole Information Médicale Evaluation Recherche, Hospices Civils de Lyon, Lyon (France); Université Lyon 1, Lyon (France); EA SIS, Université de Lyon, Lyon (France); Faix, Antoine [Department of Urology, Clinique Beausoleil, Montpellier (France); Ruffion, Alain [Université Lyon 1, Lyon (France); Department of Urology, Hospices Civils de Lyon, Centre Hospitalier Lyon Sud, Pierre Benite (France); Jalade, Patrice [Department of Medical Physics, Hospices Civils de Lyon, Centre Hospitalier Lyon Sud, Pierre Benite (France); Fenoglietto, Pascal [Department of Radiation Oncology and Physics, Institut du Cancer de Montpellier, Montpellier (France); Udrescu, Corina; Enachescu, Ciprian [Department of Radiation Oncology, Hospices Civils de Lyon, Centre Hospitalier Lyon Sud, Pierre Benite (France); Azria, David [Department of Radiation Oncology and Physics, Institut du Cancer de Montpellier, Montpellier (France)

    2015-03-15

    Purpose: Hypofractionated radiation therapy (RT) in prostate cancer can be developed only if the risk of rectal toxicity is controlled. In a multicenter phase 2 trial, hypofractionated irradiation was combined with an injection of hyaluronic acid (HA) to preserve the rectal wall. Tolerance of the injection and acute toxicity rates are reported. Methods and Materials: The study was designed to assess late grade 2 toxicity rates. The results described here correspond to the secondary objectives. Acute toxicity was defined as occurring during RT or within 3 months after RT and graded according to the Common Terminology Criteria for Adverse Events version 4.0. HA tolerance was evaluated with a visual analog scale during the injection and 30 minutes after injection and then by use of the Common Terminology Criteria at each visit. Results: From 2010 to 2012, 36 patients with low-risk to intermediate-risk prostate cancer were included. The HA injection induced a mean pain score of 4.6/10 ± 2.3. Thirty minutes after the injection, 2 patients still reported pain (2/10 and 3/10), which persisted after the intervention. Thirty-three patients experienced at least 1 acute genitourinary toxicity and 20 patients at least 1 acute gastrointestinal toxicity. Grade 2 toxicities were reported for 19 patients with urinary obstruction, frequency, or both and for 1 patient with proctitis. No grade 3 or 4 toxicities were reported. At the 3-month visit, 4 patients described grade 2 obstruction or frequency, and no patients had any grade 2 gastrointestinal toxicities. Conclusions: The injection of HA makes it possible to deliver hypofractionated irradiation over 4 weeks with a dose per fraction of > 3 Gy, with limited acute rectal toxicity.

  5. Thermal phase diagram of acetamide-benzoic acid and benzoic acid-phthalimide binary systems for solar thermal applications

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Rohitash, E-mail: dootrohit1976@gmail.com [Defence Laboratory Jodhpur, Rajasthan, India 342011, +91-2912567520 (India); Department of Physics & Center for Solar Energy, Indian Institute of Technology Jodhpur, Rajasthan, India 342011, +91-291-2449045 (India); Kumar, Ravindra [Defence Laboratory Jodhpur, Rajasthan, India 342011, +91-2912567520 (India); Dixit, Ambesh, E-mail: ambesh@iitj.ac.in [Department of Physics & Center for Solar Energy, Indian Institute of Technology Jodhpur, Rajasthan, India 342011, +91-291-2449045 (India)

    2016-05-06

    Thermal properties of Acetamide (AM) – Benzoic acid (BA) and Benzoic acid (BA) – Phthalimide (PM) binary eutectic systems are theoretically calculated using thermodynamic principles. We found that the binary systems of AM-BA at 67.6 : 32.4 molar ratio, BA-PM at 89.7 : 10.3 molar ratio form eutectic mixtures with melting temperatures ~ 54.5 °C and 114.3 °C respectively. Calculated latent heat of fusion for these eutectic mixtures are 191 kJ/kg and 146.5 kJ/kg respectively. These melting temperatures and heat of fusions of these eutectic mixtures make them suitable for thermal energy storage applications in solar water heating and solar cooking systems.

  6. Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

    Science.gov (United States)

    Taherpour, Avat (Arman)

    2010-01-01

    Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

  7. Lipid membrane partitioning of lysolipids and fatty acids: Effects of membrane phase structure and detergent chain length

    DEFF Research Database (Denmark)

    Høyrup, Lise Pernille Kristine; Davidsen, Jesper; Jørgensen, Kent

    2001-01-01

    gel phase and at high temperatures in the disordered fluid phase of the phospholipid membrane vesicles. The long saturated acyl chains of the lysolipids and fatty acids varied from 10 to 16 carbon atoms and all titrations were performed below the critical micellar concentrations (cmc...... of magnitude higher when the saturated acyl chain of the detergents increases by two carbon atoms. The obtained partition coefficients are of importance in relation to a deeper understanding of the interplay between global aqueous and local membrane concentrations of the detergents and the functional influence...

  8. Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

    Science.gov (United States)

    Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

    2017-02-01

    Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Influence of stationary and non-stationary conditions on drying time and mechanical properties of a porcelain slab

    Science.gov (United States)

    Hammouda, Imen; Mihoubi, Daoued

    2017-12-01

    This work deals with a numerical study of the response of a porcelain slab when subjected to convective drying in stationary and non-stationary conditions. The used model describes heat, mass, and momentum transfers is applied to an unsaturated viscoelastic medium described by a Maxwell model. The numerical code allows us to determine the effect of the surrounding air temperature on drying kinetics and on mechanical stress intensities. Von Mises stresses are analysed in order to foresee an eventual damage that may occur during drying. Simulation results for several temperatures in the range of [30 °C, 90 °C] shows that for the temperature from 30 °C to 60 °C, Von Mises stresses are always lower than the yield strength. But above 70 °C, Von Mises stresses are higher than the ultimate strength, and consequently there is a risk of crack at the end of the constant drying rate period. The idea proposed in this work is to integrate a reducing temperature phase when the predicted Von Mises stress intensity exceeds the admissible stress. Simulation results shows that a non-stationary convective drying (90-60 °C) allows us to optimize costs and quality by reducing the drying time and maintaining Von Mises stress values under the admissible stress.

  10. Study of variation in thermal width of nematic and induced smectic ordering phase of citric acid (CA) and 4-heptyloxybenzoic acid (7OBA) hydrogen bonded liquid crystal complexes

    Science.gov (United States)

    Sundaram, S.; Jayaprakasam, R.; Praveena, R.; Rajasekaran, T. R.; Senthil, T. S.; Vijayakumar, V. N.

    2018-01-01

    Hydrogen-bonded liquid crystals (HBLCs) have been derived from nonmesogenic citric acid (CA) and mesogenic 4-heptyloxybenzoic acid (7OBA) yielding a highly ordered smectic C (Sm C) phase along with the new smectic X (Sm X) phase which has been identified as fingerprint-type texture. Optical (polarizing optical microscopy), thermal (differential scanning calorimetry) and structural (Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy) properties are studied. A noteworthy observation is that the intermolecular H-bond (between CA and 7OBA) influences on its melting point and clearing temperature of the HBLCs which exhibits lower value than those of the individual compounds. A typical extended mesophase region has been observed in the present complex while varying the mixture ratio (1:1 to 1:3) than those of individual compounds. The change in the ratio of the mesogenic compound in the mixture alters thermal properties such as enthalpy value and thermal span width in nematic (N) region of HBLC complex. Optical tilt angle measurement of CA+7OBA in Sm C phase has been discussed to identify the molecular position in the mesophase.

  11. Analyzing Non Stationary Processes in Radiometers

    Science.gov (United States)

    Racette, Paul

    2010-01-01

    The lack of well-developed techniques for modeling changing statistical moments in our observations has stymied the application of stochastic process theory for many scientific and engineering applications. Non linear effects of the observation methodology is one of the most perplexing aspects to modeling non stationary processes. This perplexing problem was encountered when modeling the effect of non stationary receiver fluctuations on the performance of radiometer calibration architectures. Existing modeling approaches were found not applicable; particularly problematic is modeling processes across scales over which they begin to exhibit non stationary behavior within the time interval of the calibration algorithm. Alternatively, the radiometer output is modeled as samples from a sequence random variables; the random variables are treated using a conditional probability distribution function conditioned on the use of the variable in the calibration algorithm. This approach of treating a process as a sequence of random variables with non stationary stochastic moments produce sensible predictions of temporal effects of calibration algorithms. To test these model predictions, an experiment using the Millimeter wave Imaging Radiometer (MIR) was conducted. The MIR with its two black body calibration references was configured in a laboratory setting to observe a third ultra-stable reference (CryoTarget). The MIR was programmed to sequentially sample each of the three references in approximately a 1 second cycle. Data were collected over a six-hour interval. The sequence of reference measurements form an ensemble sample set comprised of a series of three reference measurements. Two references are required to estimate the receiver response. A third reference is used to estimate the uncertainty in the estimate. Typically, calibration algorithms are designed to suppress the non stationary effects of receiver fluctuations. By treating the data sequence as an ensemble

  12. Stationary radiation of objects with scattering media

    International Nuclear Information System (INIS)

    Vasil'eva, Inna A

    2001-01-01

    The radiation observed inside or outside a stationary radiator with a scattering medium is a sum of components, each being determined by, first, the primary radiation from some part of the radiator and, second, the probability of this radiation reaching the region where it is observed. In this review, general and rather simple relations between these components are discussed. These relations, unlike the components themselves, are independent of the specific optical characteristics of the object as well as of its geometry, inhomogeneity, etc. In deriving the relations, the situations in which geometrical optics is either applicable or inapplicable to radiation in a scattering medium are considered. For the case where geometrical optics does apply, stationary relations are derived from the probabilistic stationarity condition for radiation passing through the medium, i.e., from the fact that all radiation emitted in a stationary regime disappears with probability unity. Equilibrium relations are derived from the stationary relations in the particular case of a thermal radiator in an isothermal cavity. To derive the stationary relations in the geometrical optics approximation, we obtain general solutions of the linear equation of transfer using the Green function approach. If geometrical optics cannot be applied to a scattering and radiating medium, only relations for the components of outgoing thermal radiation are obtained, and the generalized Kirchhoff law, obtained by Levin and Rytov using statistical radio-physics methods, is employed. In this case, stationary relations are also derived from a probabilistic stationarity condition; the equilibrium relations follow from the stationary ones as well as from the equilibrium condition for radiation in the isothermal cavity. The quantities involved in all the relations obtained are a subject of experimental and computational spectroscopic studies. Examples of current and potential applications are given. The relations

  13. Liquid-Phase Heat-Release Rates of the Systems Hydrazine-Nitric Acid and Unsymmetrical Dimethylhydrazine-Nitric Acid

    Science.gov (United States)

    Somogyi, Dezso; Feiler, Charles E.

    1960-01-01

    The initial rates of heat release produced by the reactions of hydrazine and unsymmetrical dimethylhydrazine with nitric acid were determined in a bomb calorimeter under conditions of forced mixing. Fuel-oxidant weight ratio and injection velocity were varied. The rate of heat release apparently depended on the interfacial area between the propellants. Above a narrow range of injection velocities representing a critical amount of interfacial area, the rates reached a maximum and were almost constant with injection velocity. The maximum rate for hydrazine was about 70 percent greater than that for unsymmetrical dimethylhydrazine. The total heat released did not vary with mixture ratio over the range studied.

  14. Assessment of Envi-Carb™ as a passive sampler binding phase for acid herbicides without pH adjustment.

    Science.gov (United States)

    Seen, Andrew; Bizeau, Oceane; Sadler, Lachlan; Jordan, Timothy; Nichols, David

    2014-05-01

    The graphitised carbon solid phase extraction (SPE) sorbent Envi-Carb has been used to fabricate glass fibre filter- Envi-Carb "sandwich" disks for use as a passive sampler for acid herbicides. Passive sampler uptake of a suite of herbicides, including the phenoxyacetic acid herbicides 4-chloro-o-tolyloxyacetic acid (MCPA), 2,4-dichlorophenoxyacetic acid (2,4-D) and 3,6-dichloro-2-methoxybenzoic acid (Dicamba), was achieved without pH adjustment, demonstrating for the first time a suitable binding phase for passive sampling of acid herbicides at neutral pH. Passive sampling experiments with Duck River (Tasmania, Australia) water spiked at 0.5 μg L(-1) herbicide concentration over a 7 d deployment period showed that sampling rates in Duck River water decreased for seven out of eight herbicides, and in the cases of 3,6-dichloro-2-pyridinecarboxylic acid (Clopyralid) and Dicamba no accumulation of the herbicides occurred in the Envi-Carb over the deployment period. Sampling rates for 4-amino-3,5,6-trichloro-2-pyridinecarboxylic acid (Picloram), 2,4-D and MCPA decreased to approximately 30% of the sampling rates in ultrapure water, whilst sampling rates for 2-(4,6-dimethylpyrimidin-2-ylcarbamoylsulfamoyl) benzoic acid, methyl ester (Sulfometuron-methyl) and 3,5,6-Trichloro-2-pyridinyloxyacetic acid (Triclopyr) were approximately 60% of the ultrapure water sampling rate. For methyl N-(2,6-dimethylphenyl)-N-(methoxyacetyl)-D-alaninate (Metalaxyl-M) there was little variation in sampling rate between passive sampling experiments in ultrapure water and Duck River water. SPE experiments undertaken with Envi-Carb disks using ultrapure water and filtered and unfiltered Duck River water showed that not only is adsorption onto particulate matter in Duck River water responsible for a reduction in herbicide sampling rate, but interactions of herbicides with dissolved or colloidal matter (matter able to pass through a 0.2 μm membrane filter) also reduces the herbicide sampling

  15. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases; Cromatografia en fase gaseosa sobre metilfenilpolisiloxanos. Estructura molecular y parametros de retencion para alcoholes y sus derivados benzoilados

    Energy Technology Data Exchange (ETDEWEB)

    Pias, J B; Gasco, L

    1976-07-01

    The retention indices of aliphatic alcohols of carbon number up to C{sub g}, and of their benzoyl derivatives up to C{sub 7}, were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH{sub 2}- group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices {delta}l , and positional and structural increments {delta}I, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs.

  16. Feasibility of semiautomated MR volumetry using gadoxetic acid-enhanced MRI at hepatobiliary phase for living liver donors.

    Science.gov (United States)

    Lee, Jeongjin; Kim, Kyoung Won; Kim, So Yeon; Kim, Bohyoung; Lee, So Jung; Kim, Hyoung Jung; Lee, Jong Seok; Lee, Moon Gyu; Song, Gi-Won; Hwang, Shin; Lee, Sung-Gyu

    2014-09-01

    To assess the feasibility of semiautomated MR volumetry using gadoxetic acid-enhanced MRI at the hepatobiliary phase compared with manual CT volumetry. Forty potential live liver donor candidates who underwent MR and CT on the same day, were included in our study. Semiautomated MR volumetry was performed using gadoxetic acid-enhanced MRI at the hepatobiliary phase. We performed the quadratic MR image division for correction of the bias field inhomogeneity. With manual CT volumetry as the reference standard, we calculated the average volume measurement error of the semiautomated MR volumetry. We also calculated the mean of the number and time of the manual editing, edited volume, and total processing time. The average volume measurement errors of the semiautomated MR volumetry were 2.35% ± 1.22%. The average values of the numbers of editing, operation times of manual editing, edited volumes, and total processing time for the semiautomated MR volumetry were 1.9 ± 0.6, 8.1 ± 2.7 s, 12.4 ± 8.8 mL, and 11.7 ± 2.9 s, respectively. Semiautomated liver MR volumetry using hepatobiliary phase gadoxetic acid-enhanced MRI with the quadratic MR image division is a reliable, easy, and fast tool to measure liver volume in potential living liver donors. Copyright © 2013 Wiley Periodicals, Inc.

  17. Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

    Science.gov (United States)

    Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

    2002-05-25

    A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

  18. Phase- and size-controllable synthesis of hexagonal upconversion rare-earth fluoride nanocrystals through an oleic acid/ionic liquid two-phase system.

    Science.gov (United States)

    He, Meng; Huang, Peng; Zhang, Chunlei; Ma, Jiebing; He, Rong; Cui, Daxiang

    2012-05-07

    Herein, we introduce a facile, user- and environmentally friendly (n-octanol-induced) oleic acid (OA)/ionic liquid (IL) two-phase system for the phase- and size-controllable synthesis of water-soluble hexagonal rare earth (RE = La, Gd, and Y) fluoride nanocrystals with uniform morphologies (mainly spheres and elongated particles) and small sizes (size are discussed in detail. More importantly, the mechanism of the (n-octanol-induced) OA/IL two-phase system, the formation of the RE fluoride nanocrystals, and the distinctive size- and morphology-controlling capacity of the system are presented. BmimPF(6) is versatile in term of crystal-phase manipulation, size and shape maintenance, and providing water solubility in a one-step reaction. The luminescent properties of Er(3+)-, Ho(3+)-, and Tm(3+)-doped LaF(3), NaGdF(4), and NaYF(4) nanocrystals were also studied. It is worth noting that the as-prepared products can be directly dispersed in water due to the hydrophilic property of Bmim(+) (cationic part of the IL) as a capping agent. This advantageous feature has made the IL-capped products favorable in facile surface modifications, such as the classic Stober method. Finally, the cytotoxicity evaluation of NaYF(4):Yb,Er nanocrystals before and after silica coating was conducted for further biological applications. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Characterization of Polyamide 66 membranes prepared by phase inversion using formic acid and hydrochloric acid such as solvents

    Directory of Open Access Journals (Sweden)

    Patrícia Poletto

    2011-12-01

    Full Text Available The membranes properties prepared from water/formic acid (FA/ polyamide 66 (PA66 and water/hydrochloric acid (HCl/polyamide 66 (PA 66 systems has been studied. The different solvents interact distinctly with the polymer, affecting the membrane morphology. The asymmetric structure of the membranes showed a dense top layer and a porous sublayer. The membranes M-HCl prepared from HCl/PA 66 system showed a larger dense layer (around 23 μm in compared to those prepared from FA/PA 66 system (M-FA (around 10 μm. The membrane morphology was a determinant factor in results of water absorption, porosity and pure water flux. The lower thickness of dense layer in M-FA membranes resulted in a higher water absorption and, consequently, porosity, approximately 50%, compared with M-HCl membranes, approximately 15%. The same trend was observed to permeate flux, the lower thickness of dense layer higher pure water flux.

  20. Compatibility of amino acids in ice Ih and high-pressure phases: implications for the origin of life

    Science.gov (United States)

    Hao, J.; Giovenco, E.; Pedreira-Segade, U.; Montagnac, G.; Daniel, I.

    2017-12-01

    Icy environments may have been common on the early Earth due to the faint young sun. Previous studies have proposed that the formation of large icy bodies in the early ocean could concentrate the building blocks of life in eutectic fluids and therefore facilitate the polymerization of monomers. This hypothesis is based on the untested assumption that organic molecules are virtually incompatible in ice Ih. In this study, we conducted freezing experiments to explore the partitioning behavior of selected amino acids (glycine, L-alanine, L-proline, and L-phenylalanine) between ice Ih and aqueous solutions analogous to seawater. We let ice crystals grow slowly from a few seeds in equilibrium with the solution and used Raman spectroscopy to analyze in situ the relative concentrations of amino acids in the ice and aqueous solution. During freezing, there was no precipitation of amino acid crystals, indicating that the concentrations in solution never reached their solubility limit, even when the droplet was mostly frozen. Analyses of the Raman spectra of ice and eutectic solution showed that considerable amounts of amino acids existed in the ice phase with partition coefficients ranging between 0.2 and 0.5. This study also explored the partitioning of amino acids between other phases of ice (ice VI and ice VII) and solutions at high pressures and observed similar results. These observations implied little incompatibility of amino acids in ice during the freezing of the solutions, rendering the hypothesis of a cold origin of life unwarranted. However, incorporation into ice could significantly improve the efficiency of extraterrestrial transport of small organics. Therefore, this study supports the hypothesis of extraterrestrial delivery of organic molecules in the icy comets and asteroids to the primitive Earth as suggested by an increasing number of independent observations.

  1. Determination of vitamin E acid succinate in biodegradable microspheres by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Martínez Sancho, C; Herrero Vanrell, R; Negro, S

    2004-01-01

    A simple, rapid, and reproducible reversed-phase high-performance liquid chromatographic (HPLC) method is applied to the routine assay of vitamin E acid succinate in biodegradable microspheres. Vitamin E acid-succinate-containing poly-(D,L-lactic-co-glycolic acid) microspheres are prepared by the solvent evaporation method. The starting drug-polymer ratio is 1:10 (w/w) and the total amount of drug and polymer processed is always 440 mg. The content of vitamin E acid succinate in the microspheres is evaluated by HPLC. Chromatography is carried out isocratically at 25 degrees C +/- 0.5 degrees C on an Extrasil ODS-2 column with a mobile phase composed of methanol-water (97:3, v/v) (pH 5.6) at a flow rate of 2 mL/min and UV detection at 284 nm. Parameters such as linearity, limits of quantitation (LOQ) and detection (LOD), precision, accuracy, recovery, specificity, and ruggedness are studied as reported in the International Conference on Harmonization guidelines. The stability of vitamin E acid succinate is also studied with satisfactory results after 48 h at 25 degrees C. The method is selective and linear for drug concentrations in the range 15-210 micro g/mL. The LOQ and LOD are 15 and 3 micro g/mL, respectively. The results for accuracy studies are good. Values for coefficient of variation for intra- and interassay are 2.08% and 2.32%, respectively. The mean percentage of vitamin E acid succinate in the recovery studies is 99.52% +/- 0.81%. The mean loading efficiency for microspheres is 96.53% +/- 1.31%.

  2. Method to separate lignin-rich solid phase from acidic biomass suspension at an acidic pH

    Science.gov (United States)

    Yasarla, Kumar Lakshmi Rakesh; Ramarao, Bandaru V; Amidon, Thomas

    2017-09-05

    A method of separating a lignin-rich solid phase from a solution suspension, by pretreating a lignocellulosic biomass with a pretreatment fluid having remove soluble components, colloidal material and primarily lignin containing particles; separating the pretreated lignocellulosic biomass from the pretreatment fluid with soluble components, colloidal material and primarily lignin containing particles; flocculating the separated pretreatment fluid with soluble components, colloidal material and primarily lignin containing particles using polyethylene oxide (i.e., PEO) or cationic Poly acrylamide (i.e., CPAM) as a flocculating agent; and filtering the flocculated separated pretreatment fluid with soluble components, colloidal material and primarily lignin containing particles to remove agglomerates.

  3. The fifth solvatomorph of gallic acid with a supramolecular channel structure: Structural complexity and phase transitions

    Science.gov (United States)

    Thomas, Sajesh P.; Kaur, Ramanpreet; Kaur, Jassjot; Sankolli, Ravish; Nayak, Susanta K.; Guru Row, Tayur N.

    2013-01-01

    A new solvatomorph of gallic acid was generated using chiral additive technique and characterized by single crystal and powder X-ray diffraction, C-13 NMR, IR spectroscopic techniques and thermal analysis. The supramolecular channels formed by hexameric motifs of gallic acid and solvent molecules contain highly disordered solvent molecules with fractional occupancies.

  4. Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using reversed-phase ultraperformance liquid chromatography.

    Science.gov (United States)

    Turak, Fatma; Güzel, Remziye; Dinç, Erdal

    2017-04-01

    A new reversed-phase ultraperformance liquid chromatography method with a photodiode array detector was developed for the quantification of ascorbic acid (AA) and caffeine (CAF) in 11 different commercial drinks consisting of one energy drink and 10 ice tea drinks. Separation of the analyzed AA and CAF with an internal standard, caffeic acid, was performed on a Waters BEH C 18 column (100 mm × 2.1 mm, 1.7 μm i.d.), using a mobile phase consisting of acetonitrile and 0.2M H 3 PO 4 (11:89, v/v) with a flow rate of 0.25 mL/min and an injection volume of 1.0 μL. Calibration graphs for AA and CAF were computed from the peak area ratio of AA/internal standard and CAF/internal standard detected at 244.0 nm and 273.6 nm, respectively. The developed reversed-phase ultraperformance liquid chromatography method was validated by analyzing standard addition samples. The proposed reversed-phase ultraperformance liquid chromatography method gave us successful results for the quantitative analysis of commercial drinks containing AA and CAF substances. Copyright © 2016. Published by Elsevier B.V.

  5. Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using reversed-phase ultraperformance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Fatma Turak

    2017-04-01

    Full Text Available A new reversed-phase ultraperformance liquid chromatography method with a photodiode array detector was developed for the quantification of ascorbic acid (AA and caffeine (CAF in 11 different commercial drinks consisting of one energy drink and 10 ice tea drinks. Separation of the analyzed AA and CAF with an internal standard, caffeic acid, was performed on a Waters BEH C18 column (100 mm × 2.1 mm, 1.7 μm i.d., using a mobile phase consisting of acetonitrile and 0.2M H3PO4 (11:89, v/v with a flow rate of 0.25 mL/min and an injection volume of 1.0 μL. Calibration graphs for AA and CAF were computed from the peak area ratio of AA/internal standard and CAF/internal standard detected at 244.0 nm and 273.6 nm, respectively. The developed reversed-phase ultraperformance liquid chromatography method was validated by analyzing standard addition samples. The proposed reversed-phase ultraperformance liquid chromatography method gave us successful results for the quantitative analysis of commercial drinks containing AA and CAF substances.

  6. Effect of Alcohols on the Phase Behavior and Emulsification of a Sucrose Fatty Acid Ester/Water/Edible Oil System.

    Science.gov (United States)

    Matsuura, Tsutashi; Ogawa, Akihiro; Ohara, Yukari; Nishina, Shogo; Nakanishi, Maho; Gohtani, Shoichi

    2018-02-01

    The effect of alcohols (ethanol, 1-propanol, propylene glycol, glycerin, sucrose) on the phase behavior and emulsification of sucrose stearic acid ester (SSE)/water/edible vegetable oil (EVO) systems was investigated. Adding sucrose, propylene glycol, and glycerin narrowed the oil-separated two-phase region in the phase diagram of the SSE/water/EVO systems, whereas adding ethanol and 1-propanol expanded the oil-separated two-phase region. Changing the course of emulsification in the phase diagram showed that the size of the oil-droplet particle typically decreased in a system with a narrowed oil-separated region. The emulsification properties of the systems varied with respect to changes in the phase diagram. The microstructure of the systems was examined using small-angle X-ray scattering, and the ability to retain the oil in the lamellar structure of the SSEs was suggested as an important role in emulsification, because the mechanism of the systems was the same as that for the liquid crystal emulsification method.

  7. Simultaneous determination of 18α-glycyrrhetinic acid and 18β-glycyrrhetinic acid in Glycyrrhiza glabra root by reversed phase high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Ambika Chamoli

    2016-01-01

    Full Text Available Background: The aim of the present research work is to develop a high-performance liquid chromatography (HPLC method for simultaneous analysis of 18α-glycyrrhetinic acid (18α-GA and 18β-GA (18β-GA of Glycyrrhiza glabra. Materials and Methods: About 20 μL aliquots of each 18α-GA and 18β-GA were analyzed using reversed-phase C-18 column. The mobile phase was acetonitrile:tetrahydrofuran:water (10:80:10, v/v/v. The run time was 10 min at flow rate of 1 ml/min. Ultraviolet detection was carried out at 254 nm. Results: 18α-GA and 18β-GA were well resolved in reversed phase C-18 column using mobile phase acetonitrile: tetrahydrofuran: water (10:80:10, v/v/v, pH 7.9. The Rtof 18α-GA and 18β-GA was detected at 2.091 and 2.377 min, respectively. Conclusion: The developed chromatography method could be extended for potential quantification or simultaneous determination of these markers in plant as well as in herbal formulation.

  8. Gas-phase ion/ion reactions of peptides and proteins: acid/base, redox, and covalent chemistries.

    Science.gov (United States)

    Prentice, Boone M; McLuckey, Scott A

    2013-02-01

    Gas-phase ion/ion reactions are emerging as useful and flexible means for the manipulation and characterization of peptide and protein biopolymers. Acid/base-like chemical reactions (i.e., proton transfer reactions) and reduction/oxidation (redox) reactions (i.e., electron transfer reactions) represent relatively mature classes of gas-phase chemical reactions. Even so, especially in regards to redox chemistry, the widespread utility of these two types of chemistries is undergoing rapid growth and development. Additionally, a relatively new class of gas-phase ion/ion transformations is emerging which involves the selective formation of functional-group-specific covalent bonds. This feature details our current work and perspective on the developments and current capabilities of these three areas of ion/ion chemistry with an eye towards possible future directions of the field.

  9. Development and Validation of a Reversed-Phase Liquid Chromatography Method for the Simultaneous Determination of Indole-3-Acetic Acid, Indole-3-Pyruvic Acid, and Abscisic Acid in Barley (Hordeum vulgare L.).

    Science.gov (United States)

    Nakurte, Ilva; Keisa, Anete; Rostoks, Nils

    2012-01-01

    A simple, sensitive, precise, and specific reverse HPLC method was developed and validated for the determination of plant hormones in barley (Hordeum vulgare L.). The method includes extraction in aqueous organic solvent followed by solid-phase extraction, sample evaporation, and reversed-phase HPLC analysis in a general purpose UV-visible (abscisic acid (ABA)) and fluorescence detection (indole-3-acetic acid (IAA) and indole-3-pyruvic acid (IPA)), high-performance liquid chromatography system. The separation was carried out on Zorbax Eclipse XDB C8 column (150  ×  4.6  mm I.D) with a mobile phase composed of methanol and 1% acetic acid (60 : 40 v/v) in isocratic mode at a flow rate of 1 ml min(-1). The detection was monitored at 270 nm (ABA) and at 282 nm (Ex) and 360 nm (Em) (IAA, IPA). The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification, and robustness. The determined validation parameters are in the commonly acceptable ranges for that kind of analysis.

  10. Visualization of Two Phase Natural Convection Flow in a Vertical Pipe using the Sulfuric Acid - Copper Sulfate Electroplating System

    Energy Technology Data Exchange (ETDEWEB)

    Ohk, Seung-Min; Chae, Myeong-Seon; Chung, Bum-Jin [Kyung Hee Univ., Yongin (Korea, Republic of)

    2014-10-15

    The passive containment cooling system (PCCS) driven by natural forces convection gain draws research interests after Fukushima NPP accident. The PCCS was classified into three categories: Containment pressure suppression, Containment passive heat removal/pressure suppression systems and Passive containment spray. Among the types of containment passive heat removal/pressure suppression systems, the system composed of an internal heat exchanger and an external coolant tank is considered. In a severe accident condition, the heat from the containment atmosphere is transferred to the outer surface of the heat exchanger by the convection and condensation of the mixture of steam and gases. On the other hand, the heat is transferred to external pool by single phase or two phase natural convection inside of heat exchanger pipes. The study aimed at investigating the influence of the diameter (D) and height (H) of the heat exchanger pipes on the single phase and two phase natural convection heat transfer. As the initial stage of the study, the two phase natural convection flow inside a vertical pipe is visualized. In order to achieve the aim with ample test rig, a sulfuric acid - cooper sulfate electroplating system was employed based on the analogy between heat and mass transfer. The reduction of hydrogen ion at the cathode surface at high potential was used to simulate the boiling phenomena. This study tried to visualize the boiling heat transfer inside a vertical pipe using a cupric acid-copper sulfate (H{sub 2}SO{sub 4}-CuSO{sub 4}) electroplating system. This seems to be successful so far. However further study has to be done to compare the result with real two phase flow situation. The surface tension and surface characteristics are to be tuned to simulate the real situation.

  11. Stability and instability of stationary solutions for sublinear parabolic equations

    Science.gov (United States)

    Kajikiya, Ryuji

    2018-01-01

    In the present paper, we study the initial boundary value problem of the sublinear parabolic equation. We prove the existence of solutions and investigate the stability and instability of stationary solutions. We show that a unique positive and a unique negative stationary solutions are exponentially stable and give the exact exponent. We prove that small stationary solutions are unstable. For one space dimensional autonomous equations, we elucidate the structure of stationary solutions and study the stability of all stationary solutions.

  12. Towards Gravitating Discs around Stationary Black Holes

    Science.gov (United States)

    Semerák, Oldřich

    This article outlines the search for an exact general relativistic description of the exterior(vacuum) gravitational field of a rotating spheroidal black hole surrounded by a realistic axially symmetric disc of matter. The problem of multi-body stationary spacetimes is first exposed from the perspective of the relativity theory (section 1) and astrophysics (section 2), listing the basic methods employed and results obtained. Then (in section 3) basic formulas for stationary axisymmetric solutions are summarized. Sections 4 and 5 review what we have learnt with Miroslav Žáček and Tomáš Zellerin about certain static and stationary situations recently. Concluding remarks are given in section 6. Although the survey part is quite general, the list of references cannot be complete.Our main desideratum was the informative value rather than originality — novelties have been preferred, mainly reviews and those with detailed introductions.

  13. Reversed-phase liquid chromatographic profile of free amino acids in strawberry-tree (Arbutus unedo L.) honey.

    Science.gov (United States)

    Spano, Nadia; Piras, Irene; Ciulu, Marco; Floris, Ignazio; Panzanelli, Angelo; Pilo, Maria I; Piu, Paola C; Sanna, Gavino

    2009-01-01

    The typical profile of the free amino acids contained in strawberry-tree (Arbutus unedo L.) honey is reported for the first time. An optimized reversed-phase liquid chromatographic (RP-LC) method with phenyl isothiocyanate precolumn derivatization was used. Fourteen free amino acids were identified and quantified in 16 analytical samples. Proline (65.63%) was found to be the most abundant free amino acid, followed by glutamic acid (6.49%), arginine (5.21%), alanine (5.17%), and phenylalanine (4.97%). The total free amino acid content of strawberry-tree honey (average value, 436 mg/kg) was found to be low in comparison to amounts cited in the literature concerning unifloral honeys. The analytical method was optimized and fully validated in terms of detection and quantitation limits, precision (by testing repeatability and reproducibility), linearity, and bias (by means of recovery tests). The acceptability of the validation protocol results was verified using Horwitz's mathematical model and AOAC guidelines.

  14. PEP3 overexpression shortens lag phase but does not alter growth rate in Saccharomyces cerevisiae exposed to acetic acid stress

    Science.gov (United States)

    Ding, Jun; Holzwarth, Garrett; Bradford, C. Samuel; Cooley, Ben; Yoshinaga, Allen S.; Patton-Vogt, Jana; Abeliovich, Hagai; Penner, Michael H.; Bakalinsky, Alan T.

    2017-01-01

    In fungi, two recognized mechanisms contribute to pH homeostasis: the plasma membrane proton-pumping ATPase that exports excess protons and the vacuolar proton-pumping ATPase (V-ATPase) that mediates vacuolar proton uptake. Here, we report that overexpression of PEP3 which encodes a component of the HOPS and CORVET complexes involved in vacuolar biogenesis, shortened lag phase in Saccharomyces cerevisiae exposed to acetic acid stress. By confocal microscopy, PEP3-overexpressing cells stained with the vacuolar membrane-specific dye, FM4-64 had more fragmented vacuoles than the wild-type control. The stained overexpression mutant was also found to exhibit about 3.6-fold more FM4-64 fluorescence than the wild-type control as determined by flow cytometry. While the vacuolar pH of the wild-type strain grown in the presence of 80 mM acetic acid was significantly higher than in the absence of added acid, no significant difference was observed in vacuolar pH of the overexpression strain grown either in the presence or absence of 80 mM acetic acid. Based on an indirect growth assay, the PEP3-overexpression strain exhibited higher V-ATPase activity. We hypothesize that PEP3 overexpression provides protection from acid stress by increasing vacuolar surface area and V-ATPase activity and, hence, proton-sequestering capacity. PMID:26051671

  15. Esterification of oleic acid in a three-phase, fixed-bed reactor packed with a cation exchange resin catalyst.

    Science.gov (United States)

    Son, Sung Mo; Kimura, Hiroko; Kusakabe, Katsuki

    2011-01-01

    Esterification of oleic acid was performed in a three-phase fixed-bed reactor with a cation exchange resin catalyst (Amberlyst-15) at high temperature, which was varied from 80 to 120 °C. The fatty acid methyl ester (FAME) yields in the fixed-bed reactor were increased with increases in the reaction temperature, methanol flow rate and bed height. Moreover, the FAME yields were higher than those obtained using a batch reactor due to an equilibrium shift toward the product that resulted from continuous evaporation of the produced water. In addition, there was no catalyst deactivation during the esterification of oleic acid. However, addition of sunflower oil to the oleic acid reduced the FAME yield obtained from simultaneous esterification and transesterification. The FAME yield was 97.5% at a reaction temperature of 100 °C in the fixed-bed with a height of 5 cm when the methanol and oleic acid feed rates were 8.6 and 9.0 mL/h, respectively. Copyright © 2010 Elsevier Ltd. All rights reserved.

  16. Modelling of the acid base properties of two thermophilic bacteria at different growth times

    Science.gov (United States)

    Heinrich, Hannah T. M.; Bremer, Phil J.; McQuillan, A. James; Daughney, Christopher J.

    2008-09-01

    Acid-base titrations and electrophoretic mobility measurements were conducted on the thermophilic bacteria Anoxybacillus flavithermus and Geobacillus stearothermophilus at two different growth times corresponding to exponential and stationary/death phase. The data showed significant differences between the two investigated growth times for both bacterial species. In stationary/death phase samples, cells were disrupted and their buffering capacity was lower than that of exponential phase cells. For G. stearothermophilus the electrophoretic mobility profiles changed dramatically. Chemical equilibrium models were developed to simultaneously describe the data from the titrations and the electrophoretic mobility measurements. A simple approach was developed to determine confidence intervals for the overall variance between the model and the experimental data, in order to identify statistically significant changes in model fit and thereby select the simplest model that was able to adequately describe each data set. Exponential phase cells of the investigated thermophiles had a higher total site concentration than the average found for mesophilic bacteria (based on a previously published generalised model for the acid-base behaviour of mesophiles), whereas the opposite was true for cells in stationary/death phase. The results of this study indicate that growth phase is an important parameter that can affect ion binding by bacteria, that growth phase should be considered when developing or employing chemical models for bacteria-bearing systems.

  17. Solubility and phase separation of 4-morpholinepropanesulfonic acid (MOPS), and 3-morpholino-2-hydroxypropanesulfonic acid (MOPSO) in aqueous 1,4-dioxane and ethanol solutions

    International Nuclear Information System (INIS)

    Taha, Mohamed; Lee, Ming-Jer

    2011-01-01

    Highlights: → Solubilities of MOPS and MOPSO buffers in aqueous 1,4-dioxane and ethanol solutions. → We found that MOPS-induced phase separation of aqueous solution of 1,4-dioxane. → The phase diagram of (MOPS + water + 1,4-dioxane) system at 298.15 K is documented. → The tie-lines within the two-liquid phase region were also determined at 298.15 K. → The effective excluded volume theory was applied to correlate the binodal LLE data. - Abstract: The buffers 4-morpholinepropanesulfonic acid (MOPS) and 3-morpholino-2-hydroxypropanesulfonic acid (MOPSO) are useful biological zwitterionic buffers within the pH range of 6.5 to 7.9 and 6.2 to 7.6, respectively. The solubilities of these buffers were determined in binary mixtures (1,4-dioxane + water) and (ethanol + water) at T = 298.15 K by using the results of density measurements. It has been observed that MOPS induced liquid-liquid phase splitting for the mixtures of 40% to 90% (w/w) 1,4-dioxane in water. The two-liquid phase formation was visualized with disperse orange 25. The phase equilibrium boundaries, including the regions of one liquid, two liquids, (one liquid + one solid) and (two liquids + one solid), for the (MOPS + water + 1,4-dioxane) system have been determined experimentally at T = 298.15 K. The tie lines of the (liquid + liquid) equilibrium were also measured. The Othmer-Tobias and Bancroft equation were used to evaluate the reliability of the tie-line data. The binodal curve was fitted to an empirical equation and the effective excluded volume (EEV) model. The apparent free energies of transfer (ΔG tr ' ) of MOPS and MOPSO from water to 1,4-dioxane and ethanol solutions have been calculated from the solubility data. These ΔG tr ' values were compared with those of some related biological buffers (TRIS, TAPS, TAPSO, and TABS). Furthermore, we also calculated the contribution of transfer free energies (Δg tr ' ) of -OH group from water to 1,4-dioxane and ethanol solutions.

  18. Effect of positively charged short peptides on stability of cubic phases of monoolein/dioleoylphosphatidic acid mixtures.

    Science.gov (United States)

    Masum, Shah Md; Li, Shu Jie; Awad, Tarek S; Yamazaki, Masahito

    2005-06-07

    To elucidate the stability and phase transition of cubic phases of biomembranes with infinite periodic minimal surface is indispensable from biological and physicochemical aspects. In this report, we investigated the effect of positively charged peptide-3K (LLKKK) and poly(L-lysine) on the phase stability of monoolein (MO) membranes containing negatively charged dioleoylphosphatidic acid (DOPA) (i.e., DOPA/MO membranes) using small-angle X-ray scattering. At first, the effect of peptide-3K on 10% DOPA/90% MO membrane in excess water, which is in the Q229 phase, was investigated. At 3.4 mM peptide-3K, a Q229 to Q230 phase transition occurred, and at >3.4 mM peptide-3K, the membrane was in the Q230 phase. Poly(L-lysine) (M(w) 1K-4K) also induced the Q230 phase, but peptide-2K (LLKK) could not induce it in the same membrane. We also investigated the effect of peptide-3K on the multilamellar vesicle (MLV) of 25% DOPA/75% MO membrane, which is in L(alpha) phase. In the absence of peptide, the spacing of MLV was very large (11.3 nm), but at > or = 8 mM peptide-3K, it greatly decreased to a constant value (5.2 nm), irrespective of the peptide concentration, indicating that peptide-3K and the membranes form an electrostatically stabilized aggregation with low water content. Poly(L-lysine) also decreased greatly the spacing of the 25% DOPA/75% MO MLV, indicating the formation of a similar aggregation. To compare the effects of peptide-3K and poly(L-lysine) with that of osmotic stress on stability of the cubic phase, we investigated the effect of poly(ethylene glycol) with molecular weight 7500 (PEG-6K) on the phase stability of 10% DOPA/90% MO membrane. With an increase in PEG-6K concentration, i.e., with an increase in osmotic stress, the most stable phase changed as follows; Q229 (Schwartz's P surface) --> Q224 (D) --> Q230 (G). On the basis of these results, we discuss the mechanism of the effects of the positively charged short peptides (peptide-3K) and poly

  19. Stationary Double Layers in a Collisionless Magnetoplasma

    DEFF Research Database (Denmark)

    Noriyoshi, Sato; Mieno, Tetsu; Hatakeyama, Rikizo

    1983-01-01

    of the plate on the low-potential side, being accompanied with current limitation. This localized potential drop moves along the plasma column, but finally stops and results in the formation of the stationary double layer in the presence of sufficient plasma supply from the plate on the high-potential side.......Stationary double layers are generated in a magnetoplasma by applying potential differences between two heated plates on which the plasma is produced by surface ionization. By measuring the double-layer formation process, a localized potential drop is found to be formed initially in front...

  20. A system dynamics model integrating physiology and biochemical regulation predicts extent of crassulacean acid metabolism (CAM) phases.

    Science.gov (United States)

    Owen, Nick A; Griffiths, Howard

    2013-12-01

    A system dynamics (SD) approach was taken to model crassulacean acid metabolism (CAM) expression from measured biochemical and physiological constants. SD emphasizes state-dependent feedback interaction to describe the emergent properties of a complex system. These mechanisms maintain biological systems with homeostatic limits on a temporal basis. Previous empirical studies on CAM have correlated biological constants (e.g. enzyme kinetic parameters) with expression over the CAM diel cycle. The SD model integrates these constants within the architecture of the CAM 'system'. This allowed quantitative causal connections to be established between biological inputs and the four distinct phases of CAM delineated by gas exchange and malic acid accumulation traits. Regulation at flow junctions (e.g. stomatal and mesophyll conductance, and malic acid transport across the tonoplast) that are subject to feedback control (e.g. stomatal aperture, malic acid inhibition of phosphoenolpyruvate carboxylase, and enzyme kinetics) was simulated. Simulated expression for the leaf-succulent Kalanchoë daigremontiana and more succulent tissues of Agave tequilana showed strong correlation with measured gas exchange and malic acid accumulation (R(2)  = 0.912 and 0.937, respectively, for K. daigremontiana and R(2)  = 0.928 and 0.942, respectively, for A. tequilana). Sensitivity analyses were conducted to quantitatively identify determinants of diel CO2 uptake. The transition in CAM expression from low to high volume/area tissues (elimination of phase II-IV carbon-uptake signatures) was achieved largely by the manipulation three input parameters. © 2013 The Authors. New Phytologist © 2013 New Phytologist Trust.

  1. Phase behavior and micellar properties of carboxylic acid end group modified pluronic surfactants

    NARCIS (Netherlands)

    Custers, J.P.A.; Broeke, van den L.J.P.; Keurentjes, J.T.F.

    2007-01-01

    The micellar behavior of three different carboxylic acid end standing (CAE) surfactants has been characterized using conductometry, differential scanning calorimetry, isothermal titration calorimetry, and dynamic light scattering. The CAE surfactants are modified high molecular weight Pluronic

  2. Liquid-Phase Catalytic Transfer Hydrogenation of Furfural over Homogeneous Lewis Acid-Ru/C Catalysts.

    Science.gov (United States)

    Panagiotopoulou, Paraskevi; Martin, Nickolas; Vlachos, Dionisios G

    2015-06-22

    The catalytic performance of homogeneous Lewis acid catalysts and their interaction with Ru/C catalyst are studied in the catalytic transfer hydrogenation of furfural by using 2-propanol as a solvent and hydrogen donor. We find that Lewis acid catalysts hydrogenate the furfural to furfuryl alcohol, which is then etherified with 2-propanol. The catalytic activity is correlated with an empirical scale of Lewis acid strength and exhibits a volcano behavior. Lanthanides are the most active, with DyCl3 giving complete furfural conversion and a 97 % yield of furfuryl alcohol at 180 °C after 3 h. The combination of Lewis acid and Ru/C catalysts results in synergy for the stronger Lewis acid catalysts, with a significant increase in the furfural conversion and methyl furan yield. Optimum results are obtained by using Ru/C combined with VCl3 , AlCl3 , SnCl4 , YbCl3 , and RuCl3 . Our results indicate that the combination of Lewis acid/metal catalysts is a general strategy for performing tandem reactions in the upgrade of furans. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Phase behaviour of the ternary mixture system of poly(L-lactic acid), dichloromethane and carbon dioxide

    International Nuclear Information System (INIS)

    Gwon, Jungmin; Cho, Dong Woo; Kim, Soo Hyeon; Shin, Hun Yong; Kim, Hwayong

    2012-01-01

    Highlights: ► The high pressure phase behaviour of poly(L-lactic acid), dichloromethane and carbon dioxide ternary mixtures was measured. ► The experimental data shows the characteristics of the LCST behaviour of polymer–solvent–gas systems. ► The experimental data correlation was performed using the hybrid EOS. - Abstract: In this study, the high pressure phase behaviour of poly(L-lactic acid) (M = 312,000), dichloromethane and carbon dioxide ternary mixtures was studied using a variable volume view cell at temperatures ranging from 313.15 K to 363.15 K and pressures of up to 30.0 MPa as functions of temperature and the CO 2 /dichloromethane mass ratio at poly(L-lactic acid) weight fractions of 1.0%, 2.5% and 3.0%. The experimental results were correlated with the hybrid equation of state for the CO 2 -polymer system using the van der Waals one-fluid mixing rule with three adjustable binary interaction parameters.

  4. 4. Workshop - Measurement techniques of stationary and transient multiphase flow

    Energy Technology Data Exchange (ETDEWEB)

    Prasser, H.M. (ed.)

    2001-05-01

    In November 2000, the 4th Workshop on Measurement Techniques for Stationary and Transient Multiphase Flows took place in Rossendorf. Three previous workshops of this series were national meetings; this time participants from different countries took part. The programme comprised 14 oral presentations, 9 of which are included in these proceedings in full length. A special highlight of the meeting was the main lecture ''Ultrasonic doppler method for bubbly flow measurement'' of Professor Masanori Aritomi, Dr. Hiroshige Kikura and Dr. Yumiko Suzuki. The workshop again dealt with high-resolution phase distribution and phase velocity measurement techniques based on electrical conductivity, ultrasound, laser light and high-speed cinematography. A number of presentations were dedicated to the application of wire-mesh sensors developed by FZR for different applications used by the Technical Universities of Delft and Munich and the Tokyo Institute of Technology. (orig.)

  5. 4. Workshop - Measurement techniques of stationary and transient multiphase flow

    International Nuclear Information System (INIS)

    Prasser, H.M.

    2001-05-01

    In November 2000, the 4th Workshop on Measurement Techniques for Stationary and Transient Multiphase Flows took place in Rossendorf. Three previous workshops of this series were national meetings; this time participants from different countries took part. The programme comprised 14 oral presentations, 9 of which are included in these proceedings in full length. A special highlight of the meeting was the main lecture ''Ultrasonic doppler method for bubbly flow measurement'' of Professor Masanori Aritomi, Dr. Hiroshige Kikura and Dr. Yumiko Suzuki. The workshop again dealt with high-resolution phase distribution and phase velocity measurement techniques based on electrical conductivity, ultrasound, laser light and high-speed cinematography. A number of presentations were dedicated to the application of wire-mesh sensors developed by FZR for different applications used by the Technical Universities of Delft and Munich and the Tokyo Institute of Technology. (orig.)

  6. Application of cyanuric chloride-based six new chiral derivatizing reagents having amino acids and amino acid amides as chiral auxiliaries for enantioresolution of proteinogenic amino acids by reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    Bhushan, Ravi; Dixit, Shuchi

    2012-04-01

    Six dichloro-s-triazine (DCT) reagents having L-Leu, D-Phg, L-Val, L-Met, L-Ala and L-Met-NH(2) as chiral auxiliaries in cyanuric chloride were introduced for enantioseparation of 13 proteinogenic amino acids. Four other DCTs and six monochloro-s-triazine (MCT) reagents having amino acid amides as chiral auxiliaries were also synthesized. These 16 chiral derivatizing reagents (CDRs) were used for synthesis of diastereomers of all the 13 analytes using microwave irradiation, which were resolved by reversed-phase high-performance liquid chromatography (RP-HPLC) using C18 column and gradient eluting mixture of aqueous TFA and acetonitrile with UV detection at 230 nm. It required only 60-90 s for derivatization using microwave irradiation. Better resolution and lower retention times were observed for the diastereomers prepared with CDRs having amino acids as chiral auxiliaries as compared to counterparts prepared with reagents having amino acid amides as chiral auxiliaries. As the best resolution of all the 13 analytes was observed for their diastereomers prepared using the DCT reagent having L-Leu as chiral auxiliary, this CDR was further employed for derivatization of Lys, Tyr, His and Arg followed by RP-HPLC analysis of resulting diastereomers. The results are discussed in light of acid and amide groups of chiral auxiliaries constituting CDRs, electronegativities of the atoms of achiral moieties constituting CDRs and hydrophobicities of side chains of amino acids constituting CDRs and analytes.

  7. Hepatocellular carcinoma: clinical significance of signal heterogeneity in the hepatobiliary phase of gadoxetic acid-enhanced MR imaging

    Energy Technology Data Exchange (ETDEWEB)

    Fujita, Nobuhiro; Nishie, Akihiro; Asayama, Yoshiki; Ushijima, Yasuhiro; Moirta, Koichiro; Honda, Hiroshi [Kyushu University, Department of Clinical Radiology, Graduate School of Medical Sciences, Fukuoka (Japan); Kubo, Yuichiro; Aishima, Shinichi [Kyushu University, Department of Anatomic Pathology, Graduate School of Medical Sciences, Fukuoka (Japan); Takayama, Yukihisa [Kyushu University, Department of Molecular Imaging and Diagnosis, Graduate School of Medical Sciences, Fukuoka (Japan); Shirabe, Ken [Kyushu University, Department of Surgery and Science, Graduate School of Medical Sciences, Fukuoka (Japan)

    2015-01-15

    To clarify the relationship between the biological behaviour of hepatocellular carcinomas (HCCs) and their signal intensity in the hepatobiliary phase of gadoxetic acid-enhanced MR imaging with a special focus on the signal heterogeneity. A total of 68 patients with 70 pathologically proven HCCs were enrolled. On the basis of the signal intensity in the hepatobiliary phase, the lesions were classified into three groups: group 1, homogeneous hypointensity (n = 44); group 2, heterogeneous hyperintensity (n = 20); and group 3, homogeneous hyperintensity (n = 6). The clinicopathological findings were compared among the three groups. The tumour size and the serum level of protein induced by vitamin K absence or antagonist-II (PIVKA-II) were significantly higher in group 2 compared to group 1 (p = 0.0155, p = 0.0215, respectively) and compared to group 3 (p = 0.0330, p = 0.0220, respectively). The organic anion transporting polypeptide 8 (OATP8) expression in group 2 and group 3 was significantly higher than in group 1 (p < 0.0001, p < 0.0001, respectively). Group 2 showed a significantly lower disease-free survival rate compared to group 1 (p = 0.0125), and group 2 was an independent prognostic factor for disease-free survival (p = 0.0308). HCCs in the hepatobiliary phase that are heterogeneously hyperintense on gadoxetic acid-enhanced MR imaging have more malignant potential than other types of HCCs. (orig.)

  8. Triple Arterial Phase MR Imaging with Gadoxetic Acid Using a Combination of Contrast Enhanced Time Robust Angiography, Keyhole, and Viewsharing Techniques and Two-Dimensional Parallel Imaging in Comparison with Conventional Single Arterial Phase

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Jeong Hee [Department of Radiology, Seoul National University Hospital, Seoul 03080 (Korea, Republic of); Department of Radiology, Seoul National University College of Medicine, Seoul 03087 (Korea, Republic of); Lee, Jeong Min [Department of Radiology, Seoul National University Hospital, Seoul 03080 (Korea, Republic of); Department of Radiology, Seoul National University College of Medicine, Seoul 03087 (Korea, Republic of); Institute of Radiation Medicine, Seoul National University Medical Research Center, Seoul 03087 (Korea, Republic of); Yu, Mi Hye [Department of Radiology, Konkuk University Medical Center, Seoul 05030 (Korea, Republic of); Kim, Eun Ju [Philips Healthcare Korea, Seoul 04342 (Korea, Republic of); Han, Joon Koo [Department of Radiology, Seoul National University Hospital, Seoul 03080 (Korea, Republic of); Department of Radiology, Seoul National University College of Medicine, Seoul 03087 (Korea, Republic of); Institute of Radiation Medicine, Seoul National University Medical Research Center, Seoul 03087 (Korea, Republic of)

    2016-11-01

    To determine whether triple arterial phase acquisition via a combination of Contrast Enhanced Time Robust Angiography, keyhole, temporal viewsharing and parallel imaging can improve arterial phase acquisition with higher spatial resolution than single arterial phase gadoxetic-acid enhanced magnetic resonance imaging (MRI). Informed consent was waived for this retrospective study by our Institutional Review Board. In 752 consecutive patients who underwent gadoxetic acid-enhanced liver MRI, either single (n = 587) or triple (n = 165) arterial phases was obtained in a single breath-hold under MR fluoroscopy guidance. Arterial phase timing was assessed, and the degree of motion was rated on a four-point scale. The percentage of patients achieving the late arterial phase without significant motion was compared between the two methods using the χ{sup 2} test. The late arterial phase was captured at least once in 96.4% (159/165) of the triple arterial phase group and in 84.2% (494/587) of the single arterial phase group (p < 0.001). Significant motion artifacts (score ≤ 2) were observed in 13.3% (22/165), 1.2% (2/165), 4.8% (8/165) on 1st, 2nd, and 3rd scans of triple arterial phase acquisitions and 6.0% (35/587) of single phase acquisitions. Thus, the late arterial phase without significant motion artifacts was captured in 96.4% (159/165) of the triple arterial phase group and in 79.9% (469/587) of the single arterial phase group (p < 0.001). Triple arterial phase imaging may reliably provide adequate arterial phase imaging for gadoxetic acid-enhanced liver MRI.

  9. Triple arterial phase MR imaging with gadoxetic acid using a combination of contrast enhanced time robust angiography, keyhole, and viewsharing techniques and two-dimensional parallel imaging in comparison with conventional single arterial phase

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Jeong Hee; Lee, Jeong Min; Han, Joon Koo [Dept. of Radiology, Seoul National University Hospital, Seoul (Korea, Republic of); Yu, Mi Hye [Dept. of Radiology, Konkuk University Medical Center, Seoul (Korea, Republic of); Kim, Eun Ju [Philips Healthcare Korea, Seoul (Korea, Republic of)

    2016-07-15

    To determine whether triple arterial phase acquisition via a combination of Contrast Enhanced Time Robust Angiography, keyhole, temporal viewsharing and parallel imaging can improve arterial phase acquisition with higher spatial resolution than single arterial phase gadoxetic-acid enhanced magnetic resonance imaging (MRI). Informed consent was waived for this retrospective study by our Institutional Review Board. In 752 consecutive patients who underwent gadoxetic acid-enhanced liver MRI, either single (n = 587) or triple (n = 165) arterial phases was obtained in a single breath-hold under MR fluoroscopy guidance. Arterial phase timing was assessed, and the degree of motion was rated on a four-point scale. The percentage of patients achieving the late arterial phase without significant motion was compared between the two methods using the χ2 test. The late arterial phase was captured at least once in 96.4% (159/165) of the triple arterial phase group and in 84.2% (494/587) of the single arterial phase group (p < 0.001). Significant motion artifacts (score ≤ 2) were observed in 13.3% (22/165), 1.2% (2/165), 4.8% (8/165) on 1st, 2nd, and 3rd scans of triple arterial phase acquisitions and 6.0% (35/587) of single phase acquisitions. Thus, the late arterial phase without significant motion artifacts was captured in 96.4% (159/165) of the triple arterial phase group and in 79.9% (469/587) of the single arterial phase group (p < 0.001). Triple arterial phase imaging may reliably provide adequate arterial phase imaging for gadoxetic acid-enhanced liver MRI.

  10. Main principles of development stationary training facilities

    International Nuclear Information System (INIS)

    Tsiptsyura, R.D.

    1986-01-01

    The designation of stationary training facilities is shown and the main requirements for them are formulated. When considering the above-mentioned requirements, special attention was paid to obligatory correspondence between training experience and practical skill of an operator. It is shown, that the switchboard block is the major unit of the training facility, which should develop skills and habits of an operator

  11. Stationary solutions and asymptotic flatness I

    International Nuclear Information System (INIS)

    Reiris, Martin

    2014-01-01

    In general relativity, a stationary isolated system is defined as an asymptotically flat (AF) stationary spacetime with compact material sources. Other definitions that are less restrictive on the type of asymptotic could in principle be possible. Between this article and its sequel, we show that under basic assumptions, asymptotic flatness indeed follows as a consequence of Einstein's theory. In particular, it is proved that any vacuum stationary spacetime-end whose (quotient) manifold is diffeomorphic to R 3 minus a ball and whose Killing field has its norm bounded away from zero, is necessarily AF with Schwarzschildian fall off. The ‘excised’ ball would contain (if any) the actual material body, but this information is unnecessary to reach the conclusion. In this first article, we work with weakly asymptotically flat (WAF) stationary ends, a notion that generalizes as much as possible that of the AF end, and prove that WAF ends are AF with Schwarzschildian fall off. Physical and mathematical implications are also discussed. (paper)

  12. Stone Stability under Stationary Nonuniform Flows

    NARCIS (Netherlands)

    Steenstra, Remco; Hofland, B.; Paarlberg, Andries; Smale, Alfons; Huthoff, Fredrik; Uijttewaal, W.S.J.

    2016-01-01

    A stability parameter for rock in bed protections under nonuniform stationary flow is derived. The influence of the mean flow velocity, turbulence, and mean acceleration of the flow are included explicitly in the parameter. The relatively new notion of explicitly incorporating the mean acceleration

  13. New interval forecast for stationary autoregressive models ...

    African Journals Online (AJOL)

    In this paper, we proposed a new forecasting interval for stationary Autoregressive, AR(p) models using the Akaike information criterion (AIC) function. Ordinarily, the AIC function is used to determine the order of an AR(p) process. In this study however, AIC forecast interval compared favorably with the theoretical forecast ...

  14. Relativistic elasticity of stationary fluid branes

    DEFF Research Database (Denmark)

    Armas, J.; Obers, N.A.

    2013-01-01

    under certain conditions that a given stationary fluid configuration living on a dynamical surface of vanishing thickness and satisfying locally the first law of thermodynamics will behave like an elastic brane when the surface is subject to small deformations. These results, which are independent...

  15. Characterization of Stationary Distributions of Reflected Diffusions

    Science.gov (United States)

    2014-01-01

    operations research to finance and mathemat- ical physics , and their stationary distributions often serve to characterize or approximate important...REFERENCES [1] Atar , R., Budhiraja, A. and Dupuis, P. (2001). On positive recurrence of constrained diffusion processes. Ann. Probab., 29 No. 2, 979-1000

  16. The stationary states of interacting fields

    NARCIS (Netherlands)

    Frazer, W.R.; Hove, Léon van

    1958-01-01

    As an application of a time-independent perturbation formalism developed earlier for systems with many degrees of freedom, we give in terms of diagrams the general perturbation expressions for the exact stationary states of interacting fields. The physical vacuum is obtained by applying to the bare

  17. Calendar Year 2016 Stationary Source Emissions Inventory

    Energy Technology Data Exchange (ETDEWEB)

    Evelo, Stacie [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-01-01

    The City of Albuquerque (COA) Environmental Health Department Air Quality Program has issued stationary source permits and registrations the Department of Energy/Sandia Field Office for operations at the Sandia National Laboratories/New Mexico. This emission inventory report meets the annual reporting compliance requirements for calendar year (CY) 2016 as required by the COA.

  18. Complexing blends of polyacrylic acid-polyethylene glycol and poly(ethylene-co-acrylic acid)-polyethylene glycol as shape stabilized phase change materials

    International Nuclear Information System (INIS)

    Alkan, Cemil; Günther, Eva; Hiebler, Stefan; Himpel, Michael

    2012-01-01

    Highlights: ► Complexing groups to PEGs in a polymer could stabilize PEG at different molecular weights. ► Shape stabilized PEGs for thermal energy storage are prepared using compounds with interacting groups. ► Phase change temperature of PEGs could be changed using a complexing copolymer with acid groups. - Abstract: Blends of poly(ethylene glycol) (PEG) at 1000, 6000, and 10,000 g/mole average molecular weights and poly(acrylic acid) (PAA) or poly(ethylene-co-acrylic acid) (EcoA) have been prepared by solution blending and accounted for thermal energy storage properties as shape stabilized polymer blends. The blends have been analyzed using Fourier transform infrared (FT-IR) spectroscopy and differential scanning calorimetry (DSC) techniques. Total thermal energy values of the complexes have been determined by the method of Mehling et al. As a result of the investigation it is found that polymers with acid groups form interpolymer complexes (IPCs) and miscible and immiscible IPC–PEG blends when blended with PEGs. PEGs formed IPCs with PAA and EcoA polymers in solutions and reach to saturation and turns to be blends of IPC and PEG polymer. PEGs in this work bleed out of the blends when its compositions reach to a degree of immiscibility. In the first range where blends are IPCs and in the third range where bleeding of PEG occurs, blends are not feasible for thermal energy storage applications. However, in the second range, the blends are potential materials for passive thermal energy storage applications.

  19. Dipolar phases in liquid crystals with the chiral part based on the lactic acid

    Czech Academy of Sciences Publication Activity Database

    Glogarová, Milada; Novotná, Vladimíra; Kašpar, Miroslav; Hamplová, Věra; Pociecha, D.

    2008-01-01

    Roč. 81, 11-12 (2008), 963-970 ISSN 0141-1594 R&D Projects: GA MŠk OC 175; GA AV ČR IAA100100710 Institutional research plan: CEZ:AV0Z10100520 Keywords : liquid crystals * paraelectric * ferroelectric and antiferroelectric phases * TGB phases * lactate unit Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.201, year: 2008

  20. Waste acid detoxification and reclamation: Phase 1, Project planning and concept development

    Energy Technology Data Exchange (ETDEWEB)

    Stewart, T.L.; Brouns, T.M.

    1988-02-01

    The objectives of this project are to develop processes for reducing the volume, quantity, and toxicity of metal-bearing waste acids. The primary incentives for implemeting these types of waste minimization processes are regulatory and economic in that they meet requirements in the Resource Conservation and Recovery Act and reduce the cost for treatment, storage, and disposal. Two precipitation processes and a distillation process are being developed to minimize waste from fuel fabrication operations, which comprise a series of metal-finishing operations. Waste process acids, such as HF/--/HNO/sub 3/ etch solutions contianing Zr as a major metal impurity and HNO/sub 3/ strip solutions containing Cu as a major metal impurity, are detoxified and reclaimed by concurrently precipitating heavy metals and regenerating acid for recycle. Acid from a third waste acid stream generated from chemical milling operations will be reclaimed using distillation. This stream comprises HNO/sub 3/ and H/sub 2/SO/sub 4/ which contains U as the major metal impurity. Distillation allows NO/sub 3//sup /minus// to be displaced by SO/sub 4//sup /minus/2/ in metal salts; free HNO/sub 3/ is then vaporized from the U-bearing sulfate stream. Uranium can be recovered from the sulfate stream in downstream precipitation step. These waste minimization processes were developed to meet Hanford's fuel fabrication process needs. 7 refs., 4 figs., 1 tab.

  1. Waste acid detoxification and reclamation: Phase 1, Project planning and concept development

    International Nuclear Information System (INIS)

    Stewart, T.L.; Brouns, T.M.

    1988-02-01

    The objectives of this project are to develop processes for reducing the volume, quantity, and toxicity of metal-bearing waste acids. The primary incentives for implemeting these types of waste minimization processes are regulatory and economic in that they meet requirements in the Resource Conservation and Recovery Act and reduce the cost for treatment, storage, and disposal. Two precipitation processes and a distillation process are being developed to minimize waste from fuel fabrication operations, which comprise a series of metal-finishing operations. Waste process acids, such as HF/--/HNO 3 etch solutions contianing Zr as a major metal impurity and HNO 3 strip solutions containing Cu as a major metal impurity, are detoxified and reclaimed by concurrently precipitating heavy metals and regenerating acid for recycle. Acid from a third waste acid stream generated from chemical milling operations will be reclaimed using distillation. This stream comprises HNO 3 and H 2 SO 4 which contains U as the major metal impurity. Distillation allows NO 3 /sup /minus// to be displaced by SO 4 /sup /minus/2/ in metal salts; free HNO 3 is then vaporized from the U-bearing sulfate stream. Uranium can be recovered from the sulfate stream in downstream precipitation step. These waste minimization processes were developed to meet Hanford's fuel fabrication process needs. 7 refs., 4 figs., 1 tab

  2. Phase I evaluation of intravenous ascorbic acid in combination with gemcitabine and erlotinib in patients with metastatic pancreatic cancer.

    Directory of Open Access Journals (Sweden)

    Daniel A Monti

    Full Text Available Preclinical data support further investigation of ascorbic acid in pancreatic cancer. There are currently insufficient safety data in human subjects, particularly when ascorbic acid is combined with chemotherapy.14 subjects with metastatic stage IV pancreatic cancer were recruited to receive an eight week cycle of intravenous ascorbic acid (three infusions per week, using a dose escalation design, along with standard treatment of gemcitabine and erlotinib. Of 14 recruited subjects enrolled, nine completed the study (three in each dosage tier. There were fifteen non-serious adverse events and eight serious adverse events, all likely related to progression of disease or treatment with gemcitabine or erlotinib. Applying RECIST 1.0 criteria, seven of the nine subjects had stable disease while the other two had progressive disease.These initial safety data do not reveal increased toxicity with the addition of ascorbic acid to gemcitabine and erlotinib in pancreatic cancer patients. This, combined with the observed response to treatment, suggests the need for a phase II study of longer duration.Clinicaltrials.gov NCT00954525.

  3. Adsorption mechanism of acids and bases in reversed-phase liquid chromatography in weak buffered mobile phases designed for liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2009-03-06

    The overloaded band profiles of five acido-basic compounds were measured, using weakly buffered mobile phases. Low buffer concentrations were selected to provide a better understanding of the band profiles recorded in LC/MS analyses, which are often carried out at low buffer concentrations. In this work, 10 microL samples of a 50 mM probe solution were injected into C(18)-bonded columns using a series of five buffered mobile phases at (SW)pH between 2 and 12. The retention times and the shapes of the bands were analyzed based on thermodynamic arguments. A new adsorption model that takes into account the simultaneous adsorption of the acidic and the basic species onto the endcapped adsorbent, predicts accurately the complex experimental profiles recorded. The adsorption mechanism of acido-basic compounds onto RPLC phases seems to be consistent with the following microscopic model. No matter whether the acid or the base is the neutral or the basic species, the neutral species adsorbs onto a large number of weak adsorption sites (their saturation capacity is several tens g/L and their equilibrium constant of the order of 0.1 L/g). In contrast, the ionic species adsorbs strongly onto fewer active sites (their saturation capacity is about 1g/L and their equilibrium constant of the order of a few L/g). From a microscopic point of view and in agreement with the adsorption isotherm of the compound measured by frontal analysis (FA) and with the results of Monte-Carlo calculations performed by Schure et al., the first type of adsorption sites are most likely located in between C(18)-bonded chains and the second type of adsorption sites are located deeper in contact with the silica surface. The injected concentration (50 mM) was too low to probe the weakest adsorption sites (saturation capacity of a few hundreds g/L with an equilibrium constant of one hundredth of L/g) that are located at the very interface between the C(18)-bonded layer and the bulk phase.

  4. [Determination of triterpenoic acids in fruits of Ziziphus jujuba using HPLC-MS with polymeric ODS column].

    Science.gov (United States)

    Zhang, Yong; Zhou, An; Xie, Xiao-Mei

    2013-03-01

    A simple and sensitive method has been developed to simultaneously determine betunilic acid, oleanolic acid and ursolic acid in the fruits of Ziziphus jujuba from different regions by HPLC-MS. This HPLC assay was performed on PAH polymeric C18 bonded stationary phase column with mobile phase contained acetonitrile-water (90: 10) and with negative ESI detection mode. The developed approach was characterized by short time consumption for chromatographic separation, high sensitivity and good reliability so as to meet the requirements for rapid analysis of large-batch fruits of Z. jujuba from different habitats.

  5. Hollow nanoporous covalent triazine frameworks via acid vapor-assisted solid phase synthesis for enhanced visible light photoactivity

    KAUST Repository

    Huang, Wei

    2016-04-11

    Herein, we report a novel trifluoromethanesulfonic acid vapor-assisted solid phase synthetic method to construct nanoporous covalent triazine frameworks with highly ordered hollow interconnected pores under mild reaction conditions. This unique solid state synthetic route allows not only the avoidance of undesired side reactions caused by traditional high temperature synthesis, but also the maintaining of defined and precise optical and electronic properties of the nonporous triazine frameworks. Promising photocatalytic activity of the polytriazine networks was demonstrated in the photoreduction reaction of 4-nitrophenol into 4-aminophenol under visible light irradiation.

  6. Hollow nanoporous covalent triazine frameworks via acid vapor-assisted solid phase synthesis for enhanced visible light photoactivity

    KAUST Repository

    Huang, Wei; Wang, Zi Jun; Ma, Beatriz Chiyin; Ghasimi, Saman; Gehrig, Dominik; Laquai, Fré dé ric; Landfester, Katharina; Zhang, Kai A. I.

    2016-01-01

    Herein, we report a novel trifluoromethanesulfonic acid vapor-assisted solid phase synthetic method to construct nanoporous covalent triazine frameworks with highly ordered hollow interconnected pores under mild reaction conditions. This unique solid state synthetic route allows not only the avoidance of undesired side reactions caused by traditional high temperature synthesis, but also the maintaining of defined and precise optical and electronic properties of the nonporous triazine frameworks. Promising photocatalytic activity of the polytriazine networks was demonstrated in the photoreduction reaction of 4-nitrophenol into 4-aminophenol under visible light irradiation.

  7. Characterization of polymer monolithic stationary phases for capillary HPLC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2003-01-01

    Roč. 26, č. 11 (2003), s. 1005-1016 ISSN 1615-9306 R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919; CEZ:MSM 253100002 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.108, year: 2003

  8. Different Stationary Phase Selectivities and Morphologies for Intact Protein Separati