• Title/Summary/Keyword: GC column

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Screening procedure for organochlorinated pesticide residues in meat fat using a matrix solid phase dispersion(MSPD) extraction and GC/ECD (MSPD법과 GC/ECD를 이용한 식육중의 잔류농약 분석)

  • 백미순;이영철;박병옥;김창수;박유순
    • Korean Journal of Veterinary Service
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    • v.22 no.1
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    • pp.15-23
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    • 1999
  • A multiresidue, simple and rapid isolation technique known as matrix-solid phase dispersoin (MSPD) for the extraction and quantitative gas chromatographic/electron capture detection (GC/ECD) determination of 14 organochlorinated pesticides($\alpha$-BHC, ($\beta$-BHC, ($\gamma$-BHC, aldrin, dieldrin, endrin, heptachlor, ($\alpha$-endosulfan, ($\beta$-endosulfan, endosulfan sulfate, p,p'-DDE, o,p'-DDD, p,p'-DDD, p,p'-DDT) from meat fats. The 14 pesticide were fortified into meat fat(0.5g) and blend with 2g $C_{18}$, $C_{18}$meat fat matrix blend and 2g activated florisil comprise an extraction column from which the pesticides are eluted by adding 8ml acetonitrile. Then 2${\mu}\ell$ of the eluate is analyzed by GC/ECD. Unfortified blank controls are tested similarly. The eluate contained all the pesticide analytes and was free of interfering coextractants. Recovery rate(31.3-500ng/g) were ranged from 80$\pm$4% to 97$\pm$4%. Any organochlorinated pesticides were not detected in 120 samples of beef and pork collected from slaughter houses in Kyeonggi province.

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Gas Chromatographic Determination of Benfuresate through On-column Injection (On-column Injector를 이용한 benfuresate의 분석)

  • Kwon, Jin-Wook;Kim, Kyun;Kim, Yong-Hwa
    • Environmental Analysis Health and Toxicology
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    • v.17 no.2
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    • pp.141-145
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    • 2002
  • Benfuresate의 잔류분석을 위해 GC-FPD(S-mode)를 이용하여 분석조건을 설정 중 열적 불안정으로 인해 열분해 산물과 모 화합물이 혼재됨이 확인되었다. 가스크로마토그라프를 이용한 열분해의 주된 요인은 주입구의 온도와 주입구내의 기화 정도인 것으로 판단되었으며, 주입구를 Chauhan과 Debre 가 고안한 on-column으로 교체 후 분석한 결과 분해산물이 없는 단일 봉우리의 크로마토그램을 얻을 수 있었고, 절대량으로 0.6-4ng의 정량 범위 내에서 유의성 높은 검량선을 얻을 수 있는 주입구 온도는 20$0^{\circ}C$였다.

Rapid Gas Chromatographic Screening of Dairy Products for Volatile and Nonvolatile Organic Acids (기체크로마토그래피법에 의한 유제품내 휘발성 및 비휘발성 유기산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook;Choi, Kyoung-Sook
    • Korean Journal of Food Science and Technology
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    • v.26 no.6
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    • pp.665-669
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    • 1994
  • A rapid gas chromatographic (GC) profiling method was applied to dairy products (milk and cheeses) for the simultaneous analysis of volatile and nonvolatile organic acids. Cheese samples were first made into aqueous samples by dissolving in water. The aqueous samples were then extracted with organic solvents after the acidification and NaCI saturation. The organic layers (diethyl ether : hexane= 1 : 1) were extracted with $NaHCO_3$ saturated solution with subsequent solid-phase extraction of the aqueous phases using Chromosorb P column/diethyl ether followed by triethylamine treatment. The resulting triethylammonium salts of acids were directly converted into volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC, and GC-mass spectrometry. From milk and four cheese samples studied, 31 organic acids including 21 fatty acids and other hydroxy and dioic acids were tentatively identified. The amounts of the fatty acids were different among the kinds of cheese and thus the simplified retention index (RI) spectra of organic acids were useful for the visual pattern recognition of each sample, when the Direct Comparision method between cheese and a blind sample were attempted, it was quickly recognized to be a gouda cheese with the 999 ppt match quality value.

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Identification of Antioxidative Substances in Allium fistulosum L. by GC-MS (GC-MS에 의한 대파의 항산화 물질 동정)

  • Seo, Gee-Woo;Cho, Jeong-Yong;Kuk, Ju-Hee;Wee, Ji-Hyang;Moon, Jae-Hak;Kim, Sung-Ho;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.35 no.5
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    • pp.988-993
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    • 2003
  • The ethyl acetate-soluble acidic fraction of juice, hot water, and MeOH extract of Allium fistulosum L. showed DPPH radical-scavenging activity. Each fraction was purified through silica gel adsorption column chromatography, and the active substances in the juice and hot water extract were identified as succinic acid, fumaric acid, 4-hydroxybenzoic acid, 4-hydroxy-3-methoxybenzoic acid, 4-hydroxycinnamic acid, and 4-hydroxy-3-methoxycinnamic acid. For the MeOH extract, 4-hydroxybenzoic acid, 4-hydroxy-3-methoxybenzoic acid, 4-hydroxycinnamic acid, and 4-hydroxy-3-methoxycinnmic acid were identified as the active substances by GC-MS. The contents of these compounds were determined by GC analysis, and their anti-oxidative activities were measured using the DPPH radical-scavenging assay. The results obtained showed that 4-hydroxy-3-methoxycinnamic acid was the dominant antioxidant in Allium fistulosum L.

Isolation and Identification of an Antibacterial Substance from Sea Mustard, Undaria pinnatifida, for Streptococcus mutans (미역 추출물로부터 충치 원인균, Streptococcus mutans에 대한 항균물질의 분리 및 동정)

  • Yun, So-Mi;Jang, Jun-Ho;Lee, Jong-Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.2
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    • pp.149-154
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    • 2007
  • An antibacterial substance to the Streptococcus mutans, a causative bacterium for decayed teeth, was isolated from the dried sea mustard, Undaria pinnatifida, and identified by GC and GC/MS. Acetone extract from the sea mustard (10.4 kg), was evaporated and partitioned to 4 fractions such as hexane, chloroform, butanol and water. The most active chloroform fraction were further purified through basic alumina, silicic acid and ODS column, successively, and finally, 3 antibacterial substances were isolated on the HPLC attached ODS column by using 95% MeOH and guided with UV detector (254 nm). Antibacterial substances (total 160mg, yield $1.5\times10^{-3}$%) had the same Rf value (0.42) on the TLC developed hexane diethyl ether acetic acid (80:30:1) and those methyl esters moved to 0.95. They were identified as the same unsaturated fatty acid, $C_{18:4,\;n-3}$ (3,6,9,12-octadecatetraenoic acid, stearidonic acid) compared relative retention times (15.5 min) with authentic fatty acid on the GC chromatogram. It was further confirmed unambiguously on the GC/MS giving molecular ion peak at m/z 290 which coincided with its methyl ester.

Primary study of sterols composition of Rhodiola sachalinensis by using GC/MS (GC/MS를 이용한 고산 홍경천의 스테롤 구성에 대한 초기연구)

  • Jin, Yinzhe;Li, Xifeng;Li, Donghao;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.219-227
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    • 2009
  • The steroid compounds in Rhodiola sachalinensis were determined with adsorption column chromatographic purification and GC/MS. Sterols were extracted by sonication and Soxhlet with ethanol and dichloromethane, respectively. The extract was partitioned with chloroform and water using liquid-liquid extraction, and purified with a silica column after the sterols had been converted to the corresponding silyl derivatives with BSTFA. Eighteen free sterols, including $\beta$-sitosterol, stigmasterol and cycloartenol, and nine sterol conjugates were found from Rhodiola sachalinensis by GC/MS. Among them, cholest-5-ene-3-ol, cholesterol, stigmasterol, $\beta$-sitosterol were confirmed and quantified with sterol standards. Most sterols were presented in the chloroform part, with $C_{29}$ being the most abundant group in this sterol group. $\beta$-sitosterol was the most abundant compound with a relative content of 45.94% followed by ergost-7-ene-3-ol (11.33%), 4,14-dimethyl-ergosta-8,24(28)-diene-3-ol (7.07%), stigmasterol (6.09%), cycloartenol (5.43%) and 4-methyl-cholest-5-ene-3-ol (5.39%).

Development of Portable Preconcentration-Gas Chromatography System for Fast Analysis of Trace Benzene, Toluene and Xylene in Air (대기 중 극미량의 벤젠, 톨루엔 및 자일렌의 신속한 분석을 위한 휴대용 농축-기체 크로마토크래피 시스템 개발)

  • Jung, Young-Rim;Kim, Man-Goo
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.432-441
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    • 2001
  • An automated on-line portable preconcentration-short column gas chromatograph was developed, which used preconcentrator using adsorption tube with Tenax-GR and Curie-point heating. The developed system operated with 3 steps of processing, preconcentration, thermal desorption, and analysis and cleaning, and could continued operating within 1~2 min cycle. The recoveries of preconcentrator for toluene was ranged between $94.7{\pm}6.6%$ and $103.8{\pm}3.1%$ with less than 7% of RSD. For benzene, toluene and xylene(BTX) standard gas test, IDL was 41, 49, $472ng/m^3$ benzene, toluene and o-xylene, respectively. The BTX mixture was analyzed within 30 sec with baseline separation by the system equipped with 4 m long capillary column. The deficiency of separation power caused by short column was solved by the control of sample injection volume and inlet/outlet pressure ratio. The automated portable preconcentration-short column gas chromatograph system was found to be useful for the continuous air monitoring of BTX at ppb levels in ambient air.

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Isolation and Identification of Antimicrobial Compound from Amarantus lividus (참비름 추출물에서 항균성 물질의 분리 및 동정)

  • Oh, Young-Sook;Lee, Shin-Ho
    • Microbiology and Biotechnology Letters
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    • v.33 no.2
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    • pp.123-129
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    • 2005
  • Isolation and identification of pathogens from slaughter and meat processing plant were investigated. Antimicrobial activity of Amaranthus lividus against isolated pathogens such as Aeromonas sobria, Escherichia coli, Escherichia coli O157, Listeria monocytogenes, Salmonella spp., and Staphylococcus aureus was investigated. Among the chloroform, ethyl acetate and buthanol fraction of amaranthus lividus showed inhibitory effect against Aeromonas sobria CLFM1 and Escherichia coli CLFM2. Antimicrobial substance in chloroform fraction was isolated by silica gel adsorption column chromatography, sephadex LH-20 column chromatography and silica gel partition column chromatography. The antimicrobial compound of amaranthus lividus was identified as diethyl phtalate by HPLC, GC-MS, H-NMR and C-NMR.

Headspace Hanging Drop Liquid Phase Microextraction and GC-MS for the Determination of Linalool from Evening Primrose Flowers

  • Kim, Nam-Sun;Jung, Mi-Jin;Yoo, Zoo-Won;Lee, Sun-Neo;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1996-2000
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    • 2005
  • Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

Studies on the Analytical Methods and Quantity of Residual Chlorfluazuron in Meat (식육중 Chlorfluazuron의 잔류분석법 및 잔류량에 관한 연구)

  • 박건상;홍무기;백선영;정병곤;박종세
    • Journal of Food Hygiene and Safety
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    • v.12 no.4
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    • pp.288-293
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    • 1997
  • Analytical method using capillary GC/ECD was developed to determine trace residues of chlofluazuron, 1-[3, 5-dichloro-5-trifluoromethyl-2-pyridyloxy)phenyl]-3-(2, 6-difiuorobenzoyl), in meat, and applied to analyze the residues in domestic and imported meats. The analytical scheme developed does not require column chromatographic cleanup; chlorfiuazuron was extracted with diethyl ether and petroleum ether (50: 50), partitioned against acetonitrile, cleaned up with silica Sep-Pak cartridge, identified GC/ECD, and comfirmed by GC/MS. The mean recoveries of the pesticide in meat fortified with standard solution 0.1, 0.5, 0.1 mg/kg were ranged from 82 to 95%. The limit of detection and limit of quantitation were 0.001 and 0.005 mg/kg, respectively. Chlorfluazuron residues were not found in domestic samples, but found in imported Australian beef ranging from 0.02 to 0.17 mg/kg, detected by 18% among the samples.

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