• Title/Summary/Keyword: acid phase

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Rapid Gas Chromatographic Screening of Saliva Samples for Organic Acids (기체크로마토그래피법에 의한 타액내 유기산의 신속한 스크리닝)

  • 김경례;김정한;박영준;김정옥
    • YAKHAK HOEJI
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    • v.39 no.3
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    • pp.283-288
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    • 1995
  • Rapid gas chromatographic profiling method was applied to saliva from healthy subjects for the analysis of free organic acids. Saliva samples were first saturated with NaHCO$_{3}$ and extracted with diethyl ether. The aqueous phase was solid-phase extracted using Chromosorb P as the adsorbent and diethyl ether as the eluent after the acidification and NaCl saturation, followed by triethylamine treatment. The resulting tiiethylammonium salts of acids were directly converted into stable tert.-butyl-dimethylsflyl derivatives, with subsequent analysis by dual-capiuary column gas chromatography and gas chromatograpy -mass spectrometry. From the ten saliva samples studied, twenty eight free organic acids including various fatty acids, hydroxy acids, dicarboxylic acids, md aromatic acids were tentatively identified. Among the acids identified , the concentration of lactic acid was highest for five saliva samples while $\alpha$-hydroxyisocaproic acid was most abundant for me sample, and succinic acid and glycolic acid for two samples. respectively. When the GC profiles were simplified to the corresponding acid retention index spectra of bar graphical form, they presented characteristic patterns for each individual.

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반응추출을 이용한 당 지방산 에스테르의 분리정제

  • Seo, Deok-Gi;Kim, Gwang-Il;Kim, U-Gyeong;Yu, In-Sang;Yun, Hyeon-Hui
    • 한국생물공학회:학술대회논문집
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    • 2002.04a
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    • pp.504-507
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    • 2002
  • A separation/purification process for enzymatic sugar ester production was investigated The crude reaction mixture contained sugar ester and unreacted fatty acid in acetone. The reaction mixture was mixed with KOH/phosphate buffer. Hexane was then added to enhance phase separation. Three phases formed: a lower aqueous phase containing nothing of interest, a polar organic solvent middle phase that contained mostly fatty acid soaps, and a hexane-rich upper phase that contained mostly sugar ester. Distribution coefficient of each component was measured.

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Development of Chiral Stationary Phases for the Gas Chromatographic Separation of Amino Acid Enantiomers New diamide chiral stationary phase (아미노산 광학이성질체 분리를 위한 가스크로마토그라피용 키랄 고정상의 개발 -새로운 diamide계 키랄 고정상의 응용-)

  • Park, Man-Ki;Yang, Jeong-Sun;Lee, Mi-Yung
    • YAKHAK HOEJI
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    • v.33 no.2
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    • pp.129-139
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    • 1989
  • New diamide chiral stationary phases of four systematically substituted optically active N-(N-benzoyl-L-amino acid)-anilide synthesized from L-valine, L-leucine, L-isoleucine, and L-phenylalanine were described. The behaviors of these diamides as optically active stationary phases for the separation of N-trifluoroacetyl-D,L-amino acids were examined with respect to separation factors(${\alpha}$) and thermodynamic properties of interaction. The separation of twelve N-trifluoroacetyl-D,L-amino acid isopropyl esters were improved by the order of N-(N-benzoyl-L-leucyl)-anilide>N-(N-benzoyl-L-isoleucyl)-anilide>N-(N-benzoyl-L-valyl)-anilide>N-(N-benzoyl-L-phenylalanyl)-anilide. Eight amino acid derivatives with non-polar R-group and threonine, serine, aspartic acid, and glutamic acid enantiomers were separated on N-(N-benzoyl-L-leucyl)-anilide as chiral stationary phase with good separation factor between 1.07-1.25. The separation factors decreased with respect to increasing column temperature. Possible working temperature of diamide phase was between $130-190^{\circ}C$ for N-(N-benzoyl-L-phenylalanyl)-anilide and $130-180^{\circ}C$ for other three diamide phases. The differential Gibb's free energy (${\Delta}{\Delta}G$) of enantiomers was in the range of -100--180 cal/mol for ten amino acids and -40--60 cal/mol for alanine and aspartic acid.

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Resolution of Aryl α-Aminoalkyl Ketones on a Doubly Tethered Liquid Chromatographic Chiral Stationary Phase Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxylic Acid

  • Jin, Kab-Bong;Kim, Hee-Jin;Hyun, Myung-Ho
    • Journal of the Korean Chemical Society
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    • v.55 no.5
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    • pp.751-755
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    • 2011
  • A doubly tethered chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was applied to the resolution of various aryl ${\alpha}$-aminoalkyl ketones with the use of 80% ethanol in water containing 10 mM sulfuric acid as a mobile phase. The chiral resolution was quite successful, the separation factors (${\alpha}$) and the resolutions ($R_S$) being in the range of 1.39-2.05 and 3.18-5.22, respectively. The separation factors (${\alpha}$) on the doubly tethered CSP were slightly worse than those on the corresponding singly tethered CSP. However, the resolutions ($R_S$) on the doubly tethered CSP were generally greater than those on the corresponding singly tethered CSP. The chromatographic behaviors for the resolution of aryl ${\alpha}$-aminoalkyl ketones on the doubly tethered CSP were demonstrated to be dependent on the type and the content of the organic and acidic modifiers in aqueous mobile phase and the column temperature.

Formation Characteristics of Precipitated Calcium Carbonate by Carbonation Process

  • Kim, Chiho;Seok, Mingwang;Kim, Yangdo
    • Korean Journal of Materials Research
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    • v.31 no.1
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    • pp.1-7
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    • 2021
  • The characteristics and morphology of precipitated calcium carbonate (PCC) particles produced by carbonation process with various experimental conditions are investigated in this study. The crystal structures of PCC formed by carbonation process are calcite and aragonite. The crystal structure of PCC particles synthesized without adipic acid additive is calcite only, regardless of the reaction temperature. Needle-like shape aragonite phase started to form at reactor temperature of 80℃ with the adipic acid additive. Particle size of the single phase calcite PCC synthesized without adipic acid additive is about 1 ~ 3 ㎛, with homogenous distribution. The aragonite PCC also shows uniform size distribution. The reaction temperature and concentration of adipic acid additive do not show any significant effects on the particle size distribution. Aragonite phase grown to a large aspect ratio of needle-like shape showed relatively improved whiteness. The measured whiteness value of single calcite phase is about 95.95, while that of the mixture of calcite and aragonite is about 99.11.

Influence of Culture Comditions on Acid Tolerance of Lactobacillus casei YIT 9018 (배양조건에 따른 Lactobacillus casei YIT 9018의 니산성 변화)

  • Sim, Jae-Hun;Kim, Sang-Kyo;Baek, Young-Jin;Oh, Tae-Kwang;Yang, Han-Chul
    • Microbiology and Biotechnology Letters
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    • v.23 no.1
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    • pp.17-23
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    • 1995
  • We studied the influence of culture conditions on the acid tolerance of Lactobacillus casei YIT 9018 in artificial gastric juice with respect to relative amount of membrane bound ATPase and their biochemical characteristics. With raising incubation temperature from 30.5$\circ$C to 40.5$\circ$C and lengthening incubation time from exponential phase to late stationary phase, the acid tolerance of L. casei YIT 9018 was increased. As acid tolerance enhanced, C$_{18:1}$ content of membrane fatty acid was reduced and C$_{19:0 cyclo}$ was enriched but the others were not changed greatly. At high ATPase activity, proton permeability was relatively low but this phenomenon did not correspond to acid tolerance. In conclusion, it was considered that changes of C$_{18:1}$ and C$_{19:0 cyclo}$ were closely related to the acid tolerance of L. casei YIT 9018.

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Simultaneous HPLC Analysis of Arachidonic Acid Metabolites in Biological Samples with Simple Solid Phase Extraction

  • Kim, Hyung-Gun;Huh, Young-Na;Park, Kun-Suk
    • The Korean Journal of Physiology and Pharmacology
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    • v.2 no.6
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    • pp.779-786
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    • 1998
  • A reversed-phase high-performance liquid chromatogrphy (RP-HPLC) has been developed to analyze the metabolites of arachidonic acid based on the specificities of ultraviolet absorption of these various metabolites and is sensitive to the nanogram level. This procedure makes it possible to extract complex mixtures of eicosanoids efficiently with a single step and to analyze them simultaneously by RP-HPLC from biological samples using octadesylsilyl silica extraction column and $PGB_2$ as an internal standard. The cyclooxygenase products {prostaglandin $(PG)D_2,\;PGE_1,\;PGE_2,\;PGF_{1{\alpha}},\;PGF{2{\alpha}},\;6-keto-PGF_{1{\alpha}},$ and thromboxane $B_2(TXB_2)}$ and lipid peroxidation product, isoprostanes, of arachidonic acid were monitored by one isocratic HPLC system at 195 nm wavelength. The lipoxygenase products ${leukotriene(LT)B_4,\;LTC_4,\;LTD_4,$ and 5-hydroxyeicosatetraenoic acid (5-HETE), 12-HETE, 15-HETE} were measured by another isocratic HPLC system at 280 nm for LTs and 235 nm for HETEs. This method provides a simple and reliable way to extract and assess quantitatively the final arachidonic acid metabolites.

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Determination of ${\gamma}-Aminobutyric$ Acid and Glutamic Acid in Rat Brain by High Performance Liquid Chromatography with Electrochemical Detection (HPLC-ECD를 이용한 흰쥐의 뇌 중 감마 아미노부티르산 및 글루탐산의 정량)

  • 강종성;이순철
    • YAKHAK HOEJI
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    • v.43 no.3
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    • pp.300-305
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    • 1999
  • A sensitive and efficient assay method was applied to determine the level of glutamic acid (GA) and ${\gamma}-aminobutyric$ acid (GABA) in frontal cortex and hippocampus of rat administrated with ethanol and drugs. The compounds were derivatized with ο-phthalaldehyde (OPA) and 2-mercaptoethanof for precolunm analysis. The condition for the simultaneous determination of GA, GABA and $\beta-aminobutyric$ acid (BABA) by high performance liquid chromatography with electrochemical detection was reverse phase $C_{18}$ column as stationary phase, 0.1 M phosphate buffer containing 0.1 mM $Na_4EDTA$ : methanol = 55:45 (v+v) pH 3.8 as mobile phase and 0.7V electrode voltage. The stability of reaction product of GA, GABA and BABA with OPA could be increased by adding the same volume of polyethylene glycol 400 to reaction mixture. The GABA level in frotal cortex of rat was significantly decreased by the administration of picrotoxin and diazepam, but it was significantly increased by the administration of red ginseng total saponin, N-methyl-D-glucamine and (-)-deprenyl.

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Synthesis of Decapeptide of L-Aspartic Acid and Benzyl-L-Aspartic Acid by Solid Phase Peptide Synthesis

  • Yoo, Bong-K.;Jalil Miah, M.A.;Lee, Eung-Seok;Han, Kun
    • Archives of Pharmacal Research
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    • v.28 no.7
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    • pp.756-760
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    • 2005
  • Polyene macrolide amphotericin B (AmB) is the drug of choice for the treatment of disseminated fungal infections. However, because of its pronounced side effects, the drug has limited applicability. There are few interesting reports, which state that co-administration of the drug with homo-peptide of polyaspartic acid reduces the side effects of the drug. In our present study, an approach has been made to systematically synthesize low molecular weight heteropeptides consisting of L-aspartic acid and its derivative. It was hypothesized that such heteropeptides will reduce the toxic side effects of the drug by facile hydrophobic binding between the polymer and the drug. We have employed the strategy of solid phase peptide synthesis (SPPS) to synthesize low molecular weight hetero-peptides by using L-aspartic acid and benzyl-L-aspartic acid to induce the hydrophobic binding between the peptide and the drug. In future, the proposed methodology can be employed to tailor other polypeptides substituted with benzyl groups to reduce the nephrotoxicity of AmB.

Reactive Extraction of Succinic Acid by Amino Extractants and Comparison of Extraction Characteristics of Maleic Acid (아민계 추출제를 이용한 숙신산의 반응추출 및 말산과의 추출특성 비교)

  • 홍원희;홍연기
    • KSBB Journal
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    • v.19 no.1
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    • pp.33-37
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    • 2004
  • Succinic acid is of interested as the raw material of biodegradable polymer. In this study, succinic acid was separated by reactive extraction using amine extractants such as TOA (trioctylamine) and Aliquat 336. The extractability of TOA for succinic acid was higher than that of Aliquat 336. The distribution of succinic acid into organic phase was decreased with increasing pH in aqueous phase. However, the effect of pH on the extractability of Aliquat 336 was little. In the case of maleic acid which has similar structure to succinic acid, the extractability for maleic acid was higher than that for succinic acid. It was mainly due to the difficulty of deprotonation of second carboxylic group by intramolecular hydrogen bonding.