• Title/Summary/Keyword: Splitless method

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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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Volatile Free Acid Profiling of Body Fluids by Gas Chromatography (기체 Chromatograph를 이용한 체액내 Volatile Free Acid의 분석연구)

  • Kim, Kyoung-Rae;Hahn, Mi-Kyoung
    • YAKHAK HOEJI
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    • v.32 no.1
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    • pp.6-13
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    • 1988
  • A gas chromatographic method is described for the determination of volatile free acids(VFAs) in body fluids. VFAs were trace enriched from body fluids by liquid-solid extraction using Chromosorb P as the solid sorbent and ether as the eluant. The enriched VFAs were injected in splitless injection mode onto a HP-20M fused silica capillary column. The flame ionization detector was used as the detector. The present method was applied to the profiling of VFAs in body fluids from patients suffering from the infectious disease, hepatitis. The VFAs concentrations were high in saliva of hepatitis patients and isobutyric acid detected in sera of hepatitis patients compared to healthy subjects.

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Effect of Bile Salt on the Pharmacokinetics of Bretylium in the Rat (I) - Increased Lipophiiicity of Bretylium by Ion-Pair Complexation with Taurodeoxycholate -

  • Shim, Chang-Koo;Chung, Suk-Jae;Lee, Jeong-Uk;Lee, Min-Hwa;Kim, Shin-Keun
    • Archives of Pharmacal Research
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    • v.9 no.2
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    • pp.111-114
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    • 1986
  • Bretylium tosylate is a quaternary ammonium compound used for the treatment of ventricular fibrilation in humans. It is advantageous to other cationic compound in the study of biliary excretion in that negligible amount is bound to plasma protein and metabolite is not likely is to be formed. Some researchers reported that the formation of ion-pair complex caused to increase the lipothilicity of cationic compound. The partition of bretylium between water and organic phase was increased with the addition of sodium taurodeoxycholate. Also sensitive gas chromatographical assay procedure using flame ionization detector was studied. This procedure can detect as low as 0.1 mg/ml using 0.1 ml biological sample, but contamination by previous injection is the major problem of this method.

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Headspace gas chromatographic analysis as an objective method for measuring rancidity in soybean oil (Headspace 가스크로마토그라피를 이용한 대두유 산화진행도의 객관적 평가방법)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.154-161
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    • 1991
  • An objective method for measuring rancidity in soybean oil was developed based on the volatile contents obtained by headspace gas chromatographic analysis. Apparatus for headspace volatile cold trapping-thermal desorption was described, designed to collect and analyze volatiles of soybean oil. Samples of commercially processed soybean oil were stored under controlled condition and then evaluated for flavor by a eight member trained panel and for volatile contents by headspace gas chromatographic analysis. Twenty-three GC peaks were identified on the basis of relative retention time of reference compounds and gas chromatography-mass spectrometry. The volatile compounds identified were autoxidation products of principal unsaturated fatty acids of soybean oil. The simple linear regressions of flavor score with the pentanal or hexanal contents in aged soybean oil gave correlation coefficient of 0.990 and 0.994. respectively. Pentanal and hexanal contents could be used as a potentially useful index for predicting flavor scores of soybean oil.

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Evaluation of soybean oil rancidity by pentanal and hexanal determination (Pentanal과 hexanal 측정에 의한 대두유의 산패도 측정)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.149-153
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    • 1991
  • Several commercial soybean oils were stored at $20^{\circ}C,\;40^{\circ}C$ and $60^{\circ}C$ with daily exposure of fluorescent light for 12 hours and evaluated their rancidity by headspace gas chromatographic analysis of pentanal and hexanal. The data of gas chromatographic analysis was compared with organoleptic flavor evaluation. For headspace gas chromatographic analysis, the volatile compounds were recovered by porous polymer trap and flushed into a fused silica capillary column at $250^{\circ}C$, The pentanal and hexanal separated were identified by gas chromatography and gas chromatography-mass spectrometric method. The results showed that the contents of pentanal and hexanal were linearly increased during storage for 100 days. A very simple linear relationship was found between organoleptic flavor scores and amounts of two volatile compounds with very high correlation coefficient. A similar linear relationship was also obtained for acid and peroxide value with sensory data. This results suggested the possible implication of pentanal and hexanal as an quality index for rancidity evaluation of soybean oil.

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