• Title/Summary/Keyword: Capillary column

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Determination of the Concentration of Panaxynol, Panaxydol and Panaxytrio1 by Capillary-GC(FID) (Capillary-GC(FID)에 의한 panaxynol, panaxydol 및 panaxytriol의 정량)

  • 노길봉;손현주
    • Journal of Ginseng Research
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    • v.13 no.2
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    • pp.183-188
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    • 1989
  • A gas chromatographic method was developed for determination of the concentration of three major polyacetylene compounds in ginseng roots---panaxynol, panaxydol and panaxytriol. The column and the detector used were an SPB-1 fused silica capillary (0.2mm i.d.$\times$30m, Supelco) and a flame ionization detector (FID). The column oven temperature was kept at $250^{\circ}C$ isothermally The retention times of panaxynol, panaxydol and panaxytriol peaks were 4.2,5.1 and 6.9 min before TMS-derivatitration and 4.5,5.4 and 7.4 min after TMS-derivatization, respectively. The minimum determinable concentrations of panaxynol, panaxydol and panaxytriol before TMS-derivatiEation were at the 20, 50 and 100 ppm levels, while the concentrations of panaxydol and panaxytriol as well as panaxynol after TMS- derivatisation could be towered to the 5 ppm level. The panaxynol, panaxydol and panaxytriol contents in red ginseng were determined by use of this method after TMS-derivatization : the amounts obtained were 724, 721 and 71$\mu\textrm{g}$/g, respectively.

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Enhanced UV-Visible Absorbance Detection in Capillary Electrophoresis Using Modified T-Shaped Post-Column Flow Cell

  • Lim, Kwan-Seop;Kim, Su-Hyeon;Hahn, Jong-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.23 no.2
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    • pp.295-300
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    • 2002
  • The construction of the T-shaped post-column flow cell has been changed to enhance the practicability as a UV-visible absorbance detector for capillary electrophoresis. In this new design, a rectangular cube-shaped inner structure is employed, which completely fits the outer rectangular tubing. This arrangement has greatly facilitated the fabrication of the T-cells. In addition, the volume for the auxiliary flow has been dramatically reduced down to 300 ${\mu}L$, and its volume flow rate is optimized at 4.2 ${\mu}L$/min. The short optical path length in the sheath flows (500 ${\mu}m$ on each side) minimizes background absorption, and thus enhances its performance in low-UV wavelengths. We have optimized the auxiliary flow rate at 50 ${\mu}m$/s, so that migration times are insensitive to the flow rate. This optimization has improved repeatabilities in migration times and peak heights. A double-beam detection scheme using a pair of photodiodes is employed to increase the signal-to-noise ratio.

A Study on the Separation and Determination of Organochlorine Pesticides by Capillary Column Gas-liquid Chromatography (모세관 컬럼 기체크로마토그래피에 의한 유기염소제 농약의 분리 정량에 관한 연구)

  • Taek-Jae Kim;Yun-Woo Eo;Young-Sang Kim
    • Journal of the Korean Chemical Society
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    • v.31 no.5
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    • pp.425-433
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    • 1987
  • The separation of 19 organochlorine pesticides was studied by capillary column gas chromatography. The applicability of this method to the fresh rice was investigated. Comparison of the resolution of pesticides by OV-17 and SE-30 capillary columns revealed that OV-17 column (25m ${\times}$ 0.20mm, 0.27${\mu}$m thickness) showed better resolution. The relative standard deviations (RSD) for their retention times and peak areas obtained by splitless injection mode were within 0.16% and 8.2%, respectively. The recoveries of pesticides spiked in fresh rice were mostly over 85% and their RSDS did not exceed 11.4%.

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Analysis of lipopolysaccharides of Pasteurella multocida and several Gram-negative bacteria by gas chromatography on a capillary column (Gas chromatography의 capillary column을 이용한 Pasteurella multocida 및 기타 그람음성 세균의 lipopolysaccharide 분석)

  • Ryu, Hyo-ik;Kim, Chul-joong
    • Korean Journal of Veterinary Research
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    • v.40 no.1
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    • pp.72-80
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    • 2000
  • Lipopolysaccharides (LPS) of Pasteurella multocida (P multocida) and several Gram-negative bacterial pathogens were analyzed by methanolysis, trifluoroacetylation and gas chromatography (GC) on a fused-silica capillary column. The GC analysis indicated that LPS prepared from a strain of P multocida by phenol-water (PW) or trichloroacetic acid (TCA) extraction were quite different in chemical composition. However, LPS prepared from Salmonella enteritidis by the two extraction methods were very similar. PW-LPS extracts from different Pasteurella strains of a serotype had essentially identical GC patterns. Endotoxic LPS extracted from 16 different serotypes of P multocida by PW or by phenol-chloroform-petroleum ether procedures yielded chromatograms indicating similar composition of the fatty acid moieties but minor differences in carbohydrate content. When the chemical composition of endotoxic LPS extracted from several Gram-negative bacteria (P multocida, Pasteurella hacmolytica, Haemophilus somnus, Actinobacillus ligniersii, Brucella abortus, Treponema hyodysenteriae, Escherichia coli, Bacteriodes fragilis, Salmonella abortus equi and Salmonella enteritidis) were examined, each bacteria showed a unique GC pattern. The carbohydrate constituents in LPS of various Gram-negative bacteria were quite variable not only in the O-specific polysaccharides but also in the core polysaccharides. The LPS of closely related bacteria shared more fatty acid constituents with each other than with unrelated bacteria.

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A Study on Capillary Column Ion Chromatography

  • 김호현;표동진
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2001.05a
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    • pp.115-116
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    • 2001
  • 본 연구에서는 이온 크로마토그래피로 환경오염물질들을 분석하고자 할때의 단전들을 해소하기 위하여 모세관 컬럼 이온 크로마토그래피를 개발하였다. 모세관 컬럼은 두가지 형태로 개발하였는데 하나는 packed capillary 컬럼이며 다른하나는 open tubular capillary 컬럼이다. 또한 위와 같이 모세관 컬럼을 개발하여 사용하게됨을써, 부수적으로 펌프, 시료주입기, 억압장치 그리고 전도도 셀 등을 모두 적은 부피를 다룰 수 있는 구조로 바꾸어 주었다. 따라서 본 연구의 결과로 미량환경오염 물질의 분석에 모세관 컬럼 이온크로마토그래피를 이용할 수 있는 가능성을 확인할 수 있었고, 나아가 이온 크로마토그래피의 소형화로 현장에서 직접 분리, 분석을 할 수 있으리라 기대된다.

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Determination of Co(II) Ion as a 4-(2-Thiazolylazo)resorcinol or 5-Methyl-4-(2-thiazolylazo)resorcinol Chelate by Reversed-Phase Capillary High-Performance Liquid Chromatography

  • Chung, Yong-Soon;Chung, Won-Seog
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1781-1784
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    • 2003
  • Determination of Co(II) ion as a 4-(2-thiazolylazo)resorcinol(TAR) or 5-methyl-4-(2-thiazolylazo)resorcinol(5MTAR) chelate was accomplished by reversed-phase capillary high-performance liquid chromatography (RP-Capillary-HPLC) using a Vydac $C_4$ column and MeCN-water mixture as mobile phase. The effect of change in pH and MeCN percentage of the mobile phase on the retention factor, k and peak intensity were evaluated. It was found that 30% MeCN (v/v) of pH 5.60 or 7.20 was adequate as mobile phase when TAR or 5MTAR is used. Detection limit (D.L., S/N=3) in each case was $2.0\;{\times}\;10^{-7}$M (11.8 ppb) and $3.0\;{\times}\;10^{-7}$ M (17.7 ppb). The Co(II) ion in mineral and waste water was determined with the optimum column and mobile phase.

Determination of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Capillary-GC(FID) (Capillary-GC(FID)에 의한 오미자 Lignan 성분의 정량)

  • Sohn, Hyun-Joo;Bock, Jin-Young;Baik, Soon-Ok;Kim, Yong-Ha
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.350-356
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    • 1989
  • The determinabilities of several lignan compounds by capillary-GC (F1D) were studied. The lignan compounds used were deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H and tigloylgomisin H which were isolated from fruits of Schisandra chinensis BAILLON and identified with GC/MS(EI, 70eV), 1H-NMR(300MHz) and IR. The GC column used was SPB-1 fused silica capillary$(0.25mm\;ID{\times}30m,\;Supelco)$, and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The linearities between concentration and FID response were maintained in $2{\sim}500ppm$ of deoxyschizandrin and wuweizisu C and in $5{\sim}500ppm$ of gomisin N, schizandrin, gomisin A, angeloylgomisin H and tigloylgomisin H. The contents of lignan compounds in fruits of S. chinensis BAILLON produced at Moo-ju area were analyzed by the GC method: the values obtained of schizandrin and gomisin N were 6.5 and 5.9mg/g respectively, and those of gomisin A, wuweizisu C, angeloylgomisin H, deoxyschizandrin and tigloylgomisin H were $0.5{\sim}1.6mg/g$.

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Studies on Simultaneous Analysis of Organophosphorus Pesticide Residues in Crops by Gas-Liquid Chromatography (II). Separation of Pesticides by Capillary Column (기체-액체 크로마토그래피에 의한 농작물 중 유기인제 잔류농약의 동시 분석에 관한 연구 (제 2 보). 모세관 컬럼에 의한 분리)

  • Kim, Taek-Jae;Eo, Yun-Woo;Kim, Young-Sang
    • Journal of the Korean Chemical Society
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    • v.31 no.3
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    • pp.236-243
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    • 1987
  • The optimum resolution condition of 11 organophosphorus pesticides by gas-liquid chromatography was studied using a capillary column. The injection modes and types of vaporization tubes were evaluated in relation to pesticide analysis. The best reproducibility of peak heights of pesticides was obtained by the split mode with the vaporization tube packed with quartz wool. A 25m SE-30 capillary column provided better resolution than SE-54 column for their optimum resolution. The column at $200^{\circ}C$ initially was heated by $5^{\circ}C/min\;to\;230^{\circ}C$ followed by $10^{\circ}C/min\;to\;270^{\circ}C$ and the temperatures were held constant for 5 minutes at $230^{\circ}C\;and\;270^{\circ}C$, respectively. The relative standard deviations of their retention times were less than 0.19%.

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Effect of Extraction Solvent on Volatile Compounds of Garlic Oleoresin (마늘 Oleoresin 제조시 휘발성성분에 관한 추출용매효과)

  • 정은주;김종필;조지은;이재우;이양봉;김우정
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.30 no.6
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    • pp.1033-1037
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    • 2001
  • Garlic oleoresins were made by extracting with four solvents of methanol, methyl acetate hexane and acetone from chopped garlic, respectively, and the volatile compounds of each extract were separated by gas chromatography installed with polar (supelcowax-10$^{TM}$) and nonpolar (HP-5) capillary columns, respectively, and identified by matching mass data of mass selective detector and Kovat\`s retention index with references. The numbers of the volatile compounds identified the garlic oleoresin by polar and nonpolar columns from in garlic oleoresins were 41 and 32, respectively. In polar column, 13 pyrans, 11 sulfur-containing compounds 6 furans 2 alcohols and 2 heterocyclic compounds were identified. In nonpolar column, 11 sulfur-containing compounds 5 acids 3 furans and eugenol were identified. The major sulfur-containing compounds identified from the oleoresins were 3, 3'-thiobis-1-propene, methyl 2-propenyl disulfide, dimethyl trisulfide, di-2-prnpenyl-trisulfide, 2-thiophenecarboxylic acid. The amount of these sulfur-containing compounds isolated from the oleresins were more abundant in polar column than in nonpolar column. The most efficient solvent for extracting volatile compounds of garlic was methanol but the most useful solvent for extracting sulfur-containing compounds was methyl acetate of less polarity.y.

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