• 제목/요약/키워드: gas chromatography #1

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Capillary Column Gas Chromatography/Nitrogen Phosphorus Detector를 이용한 흥분제 및 마약성 진통제의 동시분석에 관한 연구 (Simultaneous Analysis of Stimulants and Narcotic Analgesics by Capillary Column Gas Chromatography with Nitrogen Phosphorus Detector)

  • 노동석;신호상;강보경;백형기;김승기;이정애;김영림;박종세
    • 대한화학회지
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    • 제35권6호
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    • pp.659-666
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    • 1991
  • 질소를 함유한 흥분제와 마약성 진통제 18종류의 약물들을 gas chromatography-nitrogen phosphorus detector(GC-NPD)를 사용하여 human urine으로부터 동시에 신속하게 분석할 수 있는 최적조건을 찾기 위하여 pH 변화와 추출용매 변화에 따른 회수율을 조사하였다. pH 8.5에서 에테르를 추출용매로 사용하였을 때 가장 적은 방해영향과 가장 좋은 회수율을 나타냈다. NPD에 대한 각 약물들의 상대 감응인자를 구하였고, 이 상대감응인자는 약물이 가지고 있는 질소원자의 갯수가 증가할수록 작은 값을 나타냈다. 생체시료 중의 약물들을 신속하게 검정하기 위하여 내부표준물질인 diphenylamine에 대한 relative retention time(RRT)을 작성하였다. 상대머무름 시간은 0.1% 이하의 정밀도를 나타냈다.

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GC/MS를 이용한 뇨 중 환경 에스트로겐들의 동시 프로필 (Profiling of Urinary Environmental Estrogens by Gas Chromatography/Mass Spectrometry)

  • 양윤정;이선화;정봉철
    • 분석과학
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    • 제12권4호
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    • pp.265-272
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    • 1999
  • 에스트로겐처럼 행동하여 호르몬 수용체와 결합하거나 세포의 신호전달 과정에 영향을 미침으로서 내분비계를 교란시킬 수 있는 환경 에스트로겐 19종 (phytoestrogen: 12종, mycoestrogen: 5종, synthetic estrogen: 2종)의 동시 프로필 분석을 시도하였다. Gas Chromatography/Mass Spectrometry (GC/MS)의 selected ion monitoring (SIM) 방법을 기본으로 하였으며, 액체-고체 추출, 효소 기수분해, 액체-액체 추출 그리고 trimethylsilyl (TMS)-ether 형태의 유도체화를 거치는 비교적 간편한 전처리 방법으로 47.6~99.5%의 회수율과 0.66~9.33%, 1.66~16.14%의 within-a-day 및 day-to-day 분석의 RSD 값을 얻었다. 이 방법을 적용하여 정상 성인 여성과 남성의 뇨 시료에 존재하는 대상 물질들의 농도범위를 결정함으로서 환경 에스트로겐의 영향을 평가하는데 기준이 될 수 있는 한국인 정상인 참고치를 설정하였다.

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Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS

  • Hem, Lina;Khay, Sathya;Choi, Jeong-Heui;Morgan, E.D.;El-Aty, A.M. Abd;Shim, Jae-Han
    • Toxicological Research
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    • 제26권2호
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    • pp.149-155
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    • 2010
  • The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

Gas Chromatography에 의한 잎담배와 담배연기응축물 중의 유기산 정량 (A Gas Chromatograpic Determination of Organic acids in Tobacco leaves and Cigarette Smoke Condensate)

  • 이문수;이운철;오세열;이규서
    • 한국연초학회지
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    • 제5권1호
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    • pp.67-72
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    • 1983
  • Gas Chromatography를 이용하여 잎담배와 연기응축물 중의 비휘발성유기산과 지방산을 정량 분석하였다. 특히 이들 유기산들은 단엽담배일 때 주류연으로 이행율을 조사하였는 바 linolenic acid, 31~62%, linoleic, 21~59% palmitic 29~38%, malic acid 4~6% 정도의 이행율을 보였다.

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Fast Determination of Multiple-Reaction Intermediates for Long-Chain Dicarboxylic Acid Biotransformation by Gas Chromatography-Flame Ionization Detector

  • Cho, Yong-Han;Lee, Hye-Jin;Lee, Jung-Eun;Kim, Soo-Jung;Park, Kyungmoon;Lee, Do Yup;Park, Yong-Cheol
    • Journal of Microbiology and Biotechnology
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    • 제25권5호
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    • pp.704-708
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    • 2015
  • For the analysis of multiple-reaction intermediates for long-chain dicarboxylic acid biotransformation, simple and reproducible methods of extraction and derivatization were developed on the basis of gas chromatography with flame ionization detector (GC-FID) instead of mass spectrometry. In the derivatization step, change of the ratio of pyridine to MSTFA from 1:3 to 9:1 resulted in higher peak intensity (p = 0.021) and reproducibility (0.6%CV) when analyzing 32 g/l ricinoleic acid (RA). Extraction of RA and ω-hydroxyundec-9-enoic acid with water containing 100 mM Tween 80 showed 90.4-99.9% relative extraction efficiency and 2-7%CV compared with those with hydrophobic ethyl acetate. In conclusion, reduction of the pyridine content and change of the extraction solvent to water with Tween 80 provided compatible derivatization and extraction methods to GC-FID-based analysis of longchain carboxylic acids.

Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

  • Lee, Soojin;Pyo, Heesoo;Chung, Bong Chul;Kim, Haidong;Lee, Jeongae
    • Bulletin of the Korean Chemical Society
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    • 제35권11호
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    • pp.3280-3288
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    • 2014
  • Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method ($r^2$ > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to $200ng\;mL^{-1}$. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

환경시료로부터 미량 페놀류의 분석을 위한 isoButoxycarbonyl 유도체화 분석방법 적용 및 최적화 (Application and Optimization of the IsoButoxycarbonyl Derivatization method to the Analysis of Trace Level Phenols in Environmental Samples)

  • 김협;홍종기;김용화;김경례
    • Environmental Analysis Health and Toxicology
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    • 제17권1호
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    • pp.37-51
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    • 2002
  • Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9% and 90.3∼126.6% for the US-EPA method and the isoBOC.

Determination of barbiturates in plasma by gas chromatography-fralme photometric detector after N, N'-flame photometric detector after N, N'-dimethylthiomethyl derivatization

  • Hyung, Yung;Park, Man-Ki
    • Archives of Pharmacal Research
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    • 제9권3호
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    • pp.131-138
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    • 1986
  • A specific and sensitive gas chromatographic (GC) procedure with the flame photometric detector (FPD) was developed for determination of barbiturates such as barbital, allobarbital, secobarbital, phenobarbital and thiopental in plasma. In order to evaluate the performance of the FPD, the results were campared with those of the flame ionization detector (FID). After extraction of barbiturates from plasma, the barbiturates were quantitatively N, N-dimethylthiometyl (MTM)-derivatized with methylthiomethyl chloride in 1, 8-diazabicyclo [5, 4, 0] undec-7-ene catalyst. The data indicate that the FPD is about 4 times more sensitive than the FID for barbiturates, although it is less reproducible. The FPD also produced chromatogram with less back ground for extracted plasma sample. The FPD also produced chromatogram with less background for extracted plasma sample. The minimum detectable amount of MTM-thiopental on 3% OV-225 column was 4, 4fmol and that of other MTM-barbiturate was about 10.0fmol.

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직접 분사식 디젤기관에서 바이오디젤유의 적용에 관한 실험적 연구 (An Experimental Study on Application of Biodiesel Fuel in Direct Injection Diesel Engine)

  • 오영택;최승훈
    • 대한기계학회:학술대회논문집
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    • 대한기계학회 2001년도 추계학술대회논문집B
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    • pp.818-823
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    • 2001
  • Because the exhaust emissions from automobiles are increased, our environment is faced with very serious problems related to the air pollution in these days. In particular, the exhaust emissions of diesel engine are recognized main cause which influenced environment strong. Lots of researcher have been attempted to develop various alternative fuel on purpose to reduce these harmful emissions. In this study, the potential possibility of esterfied rice bran oil which is a kind of biodiesel fuel was investigated as an alternative fuel for diesel engine. And, we tried to analysis not only total hydrocarbon but hydrocarbon components from $C_1$ to $C_6$ in exhaust gas using gas chromatography to seek the reason for remarkable reduction of exhaust emission. Individual hydrocarbon$(C_1\simC_6)$ as well as total hydrocarbon of biodiesel fuel is reduced remarkably than that of diesel fuel in this experiment.

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