• Title/Summary/Keyword: GC method

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New Methods for Isolation of Sesquiterpene from Panax ginseng (인삼 Sesquiterpene의 새로운 분리방법)

  • 위재준;신지영
    • Journal of Ginseng Research
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    • v.21 no.3
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    • pp.214-218
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    • 1997
  • New simple methods for the Isolation of sesquiterpenes from Panax ginseng were developed. First, volatile compounds were isolated by simultaneous distillation and extraction (SDE) with 30% methanol and $\alpha$-hexane instead of water and ethyl ether/pentane (1:1). Secondly, head space volatiles in U-shaped tube at 7$0^{\circ}C$ were passed through C18 Sep-Pak by nitrogen gas streaming and the adsorbed volatiles were fluted by $\alpha$-hexane. TLC analysis showed that the volatile concentrates consisted mainly of terpenes when colored by vanillin-sulfuric and. GC/MS data revealed that approximately 30 sesquiterpenes of molecular weight 204 occupied 81.1% or more of the volatile concentrates isolated by those two newly developed methods. Among these, alloaromadendrene, germacrene B, isocaryophyllene, $\alpha$-neoclovene, ${\gamma}$-muurolene, $\beta$-panaslnsene, and $\alpha$-humulene were identified as being major sesqulterpenes by authentic samples or literatme search Key words : Panax ginseng, volatile compound, sesquiterpene, isolation, new method, GC/MS.

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Comparison of Sampling and Analysis Methods for Volatile Organic Compounds in Ambient Air (대기중 휘발성 유기화합물의 채취 및 분석 방법 비교)

  • 나광삼;김용표
    • Journal of Korean Society for Atmospheric Environment
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    • v.14 no.5
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    • pp.507-518
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    • 1998
  • A field comparison study was carried out to quantify differences among various sampling and analytical methods for volatile organic compounds (VOCs) at a site in Vlsan in June 1997. Air sampling containers (SUMMA canisters) were used by the Korea Institute of Science and Technology (KIST) and adsorption tubes (carbotrap) were used by Yeungnam University (YN Univ.) for sampling ambient air. Duplicate samples obtained by KIST were analyzed by KIST with a GC-MS system for aromatics and halogenated hydrocarbons and by Atm AA with a GC -FID system for C2∼C9 hydrocarbons, respectively. The adsorption tube samples were analyzed by YN Univ. with a GC-FID system for aromatics. VOC levels for the duplicate canister sampls analyzed by KIST and Atm AA were in good agreement. Concentrations of aromatics by the adsroption tube method were generally higher than those by the canister sampling method by factor of 1.5 to 2.0. Differences between the two sampling methods were discussed.

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Development of an Analytical Approach to Measure Volatile Sulfur Compounds Using a Non-Cryogenic Preconcentration Method (비냉각형 선농축 방식에 의한 대기 중 휘발성 황화합물의 분석방법 개발)

  • 김기현;이강웅
    • Journal of Korean Society for Atmospheric Environment
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    • v.13 no.5
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    • pp.355-360
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    • 1997
  • The atmospheric concentration of dimethylsulfide (DMS), known as the predominant volatile organic. sulfur compound, is determined at subnanogram level by a combined application of non-cryogenic preconcentration method and gas chromatography with flame photometric detection (GC/FPD). The volatile DMS in air is preconcentrated using a trapping tube containing adsorbent like Molecular Sieve 5A (or gold-coated sands). The tube is then connected to the GC/FPD system via a six-way rotary valve, thermally desorbed at 40$0^{\circ}C$, separated on OV101 column, and detected by a flame photometric detector. The DMS peak elutes at about 2.5 mins and is integrated electronically. The analytical precision, if expressed in terms of relative standard error, is around 5%. The detection limit of our GC/FPD system is ca 1 ng of DMS. Details of our analytical system are presented.

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Comparative Identification of Oil Spills by Gas Chromatography Fingerprinting (海上 流出油 識別法에 關한 硏究)

  • 김영희
    • 한국해양학회지
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    • v.21 no.2
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    • pp.118-123
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    • 1986
  • A gas chromatographic oil fingerprinting method is a technique used for comparative source identification of spilled oil. The hydrocarbon and sulfur compound analysis by gas chromatography are generally used for analyzing oils. However, due to the complexity of oils, another technique is also needed for comparative identification. In this study, polycyclic aromatic hydrocarbons contained in crude oil and heavy fuel oil are analyzed by gas chromatography. They are relatively unaffected by weathering condition because they are stable. The oil fingerprinting of polycyclic aromatic hydrocarbons by GC seems to be a reliable technique for analyzing oils in identification of sources and kinds of oils.

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Determination of panthenol, cholecalciferol and tocopherol in cosmetic products by gas chromatography-mass spectrometry in SIM mode

  • Hye-Jin Jeong;Myo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.22 no.2
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    • pp.153-160
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    • 1996
  • A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

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Analysis of 3,4-Methylendedioxymethamphetamine (MDMA) in Human Hair by Gas Chromatography/Mass Spectrometry (GC/MS를 이용한 모발 중 MDMA(Methylendedioxymethamphetamine)의 분석)

  • 박미정;김은미;임미애;정희선
    • YAKHAK HOEJI
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    • v.47 no.4
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    • pp.195-199
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    • 2003
  • An analysis method for the determination of methylendedioxymethamphetamine (MDMA) and its metabolite methylendedioxymethamphetamine (MDA) in hair by gas chromatography/mass spectrometry was proposed. For MDMA and MDA analysis, hair samples were incubated in MeOH (1% HCl), derivatized with trifluoroacetic anhydride and assayed by GC/MS. Hair of 18 subjects for drug abuse was analyzed for MDMA and MDA. Calibration curves for the determination of MDMA and MDA in hair showed a good linearity at a concentration range from 0.5 ng to 250 ng ($r^2$=0.999) The extraction recovery was determined from hair blanks at 50, 100 ng. The percentage of recovery were found to be 96.08∼103.48 with CV value of 1.62∼3.89. The concentrations of MDMA and MDA ranged 1.14∼38.06 ng/mg and 0.07∼3.91 ng/mg, respectively in 18 hair samples from MDMA abusers. The ratio of MDMA to MDA ranged from 9.65∼28.46 in all specimen. Hair analysis for MDMA is a useful method for identification of long-term drug abuser.

Determination of methamphetamine in the hair of Korean abuser by CG/MS (GC/MS에 의한 한국인의 모발중 Methamphetamine검출)

  • 유영찬;정희선;최화경
    • YAKHAK HOEJI
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    • v.37 no.4
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    • pp.356-361
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    • 1993
  • A sensitive method for the determination of methamphetamine(MA) and amphetamine(AM) in hair was developed by gas chromatography/mass spectrometry using stable isotope-labeled internal standards, amphetamine-d$_{5}$ and methamphetamine-d$_{5}$. Hair sample was washed with MeOH, incubated with MeOH(I% HCI) overnight at $37^{\circ}C$ while stirring and extracted using solid phase extraction column on a vacuum manifold. The extract obtained was pentafluoropropionated, and applied to GC/MS. The calibration curves of MA and AM were linear from 2.5 to 250 ng (r>0.99 for both). The limit of detection was 0.1 ng/mg in hair and cut-off level was set at 0.25 ng/mg for both. Hair samples of 27 MA abusers showed positive results in the range 0.7 to 106.8 ng/mg. AM, its metabolite, was detected in 20 out of 27 samples. The ratio of MA versus AM was 4.6~38.3 in specimens. Hair analysis for methamphetamine by GC/MS is an effective method for identifying long-term drug abusers.

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Detection of Radiation-induced Hydrocarbons and 2-Alkylcyclobutanones from Peanuts

  • Lee, Hae-Jung;Lee, Myung-Yul;Kim, Kyung-Su
    • Preventive Nutrition and Food Science
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    • v.4 no.4
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    • pp.270-275
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    • 1999
  • Radiation-induced hydrocarbons and 2-alkylcyclobutanones are formed from the fatty acids of irradiated fats. Peanuts were irradiated with a dose of 0.1∼10 kGy. The method consists of the extraction of fat from peanuts, separation of hydrocarbons and 2-alkylcyclobutanones with florisil column chromatography and identification of hydrocarbons by the GC/MS method and 2-alkylcyclobutanones by GC/MS/selected ion monitoring (SIM). Concentrations of hydrocarbons and 2-alkylcyclobutanones were linearly increased with the dose levels of radiation. The major hydrocarbons in the irradiated peanut samples were 8-heptadecene and 1,7-hexadecadiene from oleic acid and 6,9-heptadecadiene and 1,7,10-hexadecatriene from linoleic acid. 2-(5'-Tetradecenyl)cyclobutanone, one of 2-alkylcyclobutanones, was the highest amount in the irradiated peanuts. Radiation-induced hydrocarbons in the peanuts were detected at doses of 0.5 kGy and over, and radation-induced 2-alkylcyclobutanones were detected at doses of 1 kGy and over. These compounds were not confirmed in unirradiate peanuts.

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Determination of ethylene glycol in alkali wastewater by gas chromatography/mass spectrometry (GC/MS를 이용한 알칼리 폐수 중 ethylene glycol 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.527-531
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    • 2004
  • Treatment with aqueous sodium hydroxide solution plays an important role to impart certain desirable properties - feel and luster on the surface of polyester fiber. In this process alkali wastewater contains disodium terephthalate, ethylene glycol (EG) and residual sodium hydroxide. In this paper we report a new method containing the pretreatments of derivatization with benzoyl chloride and solvent extraction using pentane. The calibration curve of EG determined by GC/MS-SIM shows a good linearity in the range of 0.1 to $25{\mu}g/mL$ having the standard deviation of ${\leq}8.7%$. The recovery and the detection limit of this method are 91.9-93.7% and $0.05{\mu}g/mL$ respectively.

Quantitative Analysis of amphetamines in hair by EI-GC-MS using SIM mode with uncertainty estimation

  • Yang, Won-Kyung;Han, Eun-Young;Lee, Jae-Sin;Park, Yong-Hoon;Kim, Eun-Mi;Lim, Mi-Ae;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.169.2-169.2
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    • 2003
  • A method using EI-GC-MS is described for the determination of amphetamines in hair. The method is applied to simultaneous quantify amphetamines (methamphetamine, amphetamine, MDMA and MDA). Drugs were extracted in 1 % HCl in methanol from hair. After derivertization with TFAA, the resulting drugs were separated on HP-5MS column during a 16 min program and identified by mass spectrometry with the SIM mode(EI-GC-MS). (omitted)

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