• Title/Summary/Keyword: capillary column GC/MS

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Simultaneous Determination of Cholesterol, Bile Acids and Sterols in Human Bile Juices and Gallstones Using GC/MS (GC/MS에 의한 담석과 담즙내의 Cholesterol, Bile Acids 및 Sterols의 동시 Profiling)

  • Yang, Yoon Jung;Lee, Seon Hwa;Kim, Hyun Joo;Chung, Bong Chul
    • Journal of the Korean Chemical Society
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    • v.42 no.3
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    • pp.266-276
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    • 1998
  • Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

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기체크로마토그래피-질량분석검출기와 고체상미량추출법을 이용한 물 중의 MTBE 미량분석

  • Jeon Chi-Wan;Lee Jeong-Hwa;Jeong Yeong-Uk
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.195-198
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    • 2005
  • A solid-phase microextraction and gas chromatography-mass spectrometry for the extraction and analysis of methyl-tert-butyl ether has been described. methyl-tert-butyl ether was extracted from aqueous solution using SPME fiber coated polydimethylsiloxane and analysed by GC-MS with capillary column. Extraction parameters and chromatographic separation conditions were optimized. The applied method represented good analytical performance in terms of precision (3-8%, RSD) and accuracy(93-102%, mean recovery) with a method detection limit of 0.03 ppb.

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Trans Fatty Acid Isomers of Processed Foods Commonly Consumed in Korea (한국인 상용 가공식품의 trans 지방산 이성체)

  • 노경희;원미숙;송영선
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.3
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    • pp.325-337
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    • 2003
  • This study was designed to determine the distribution of trans fatty acids (tFAs) isomers of Processed foods commonly consumed in Korea. The tFAs positional isomers were analyzed using GC/MS spectrometer with HP-23 cis/trans FAME, capillary column (50m $\times$ 0.20 mm, id., 0.2 ${\mu}{\textrm}{m}$ film thickness) for 41 food samples. TFAs isomers were identified by comparing retention time with standards and GC/MS spectrum. In margarines, the content of tFAs ranged from 4.0% to 25.16% and the most abundant positional isomer of tFAs was C18:1 $\Delta$9t. In oils and fats, lards contained higher levels of tFAs (5.70~16.54%) than shortenings (6.77~10.55%). Shortenings contained higher levels of C18:1 $\Delta$9t (3.1~5.1%) than lard (1.6~4.3%), but corn oils had no tFAs. In seasonings, mayonnaise had no C16:1 $\Delta$9t, whereas C18:3t was detected. The content of tFAs in confectioneries was wide (16.20~52.16%). Among them, instant popcorns contained the highest amount of tFAs. Milk and dairy products showed even distribution of tFAS such as C18:1t, C18:2t, and C18:3t. Predominant tFAS isomer of condensed milk and ice cream was C16:1 $\Delta$9t. Frozen french fries and fried chicken contained higher levels of C18:1$\Delta$9t (9.4%), whereas grilled pork (jowl) had no C18:1 $\Delta$9t. The amount of tFAs per serving size was the highest in popcorn, followed by frozen pizza, frozen french fries, fried chicken, and bakeries.

Studies on the Analysis of Tobacco Leaf Alkaloids (잎담배 Alkaloid분석에 관한 연구)

  • 장기철;한상빈;김용옥;이운철
    • Journal of the Korean Society of Tobacco Science
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    • v.13 no.2
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    • pp.20-26
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    • 1991
  • This study was carried out to develop the method of alkaloids analysis and investigate the kinds and contents of alkaloids in flue-cured, burley and oriental tobacco leaves using developed analytical method. The developed analytical method of alkaloids was as followed : Tobacco sample was treated with acid(pH 2∼3) and extracted with chloroform to remove chemical components except alkaloids. Sample solution was treated with alkali(pH 12∼ 13) and was extracted with chloroform to obtain alkaloids from sample solution. After extraction of alkaloids from tobacco leaves, alkaloids were separated and identified by GC, GC/MS using SE-54 fused silica capillary column. Nicotine, nornicotine, myosmine, 9-nicotyline, anabasine, anatabine, 2, 3-bipyridyl, cotinine, formyl nornicotine, acetyl nornicotine and formal anatabine were isolated and identified from the extracts of tobacco leaves. The contents of alkaloids were burley > flue-cured > oriental tobacco leaves, but oriental tobacco leaves were higher nornicotine, cotinine, formyl nornicotine and acetyl nornicotine contents than those of flue-cured tobacco leaves. The burley tobacco harvested in Korea was higher nornicotine contents by 2-6 times in the portions of cutter, leaf and tips position than that of burley tobacco(B3F) harvested in V. S. A.

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Studies on the Essential Oil of Korean Valerian Root (Valeriana fauriei var. dasycarpa Hara) (한국산 쥐오줌풀(Vaieriana fauriei var. dasycarpa Hara)의 정유성분에 관한 연구)

  • 김용태;박준영;김영회;김근수;장희진;권영주;이종철;최영현
    • Journal of the Korean Society of Tobacco Science
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    • v.14 no.1
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    • pp.66-78
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    • 1992
  • The essential oil of Korean valerian root ( Valeriana fauriei roar. dasycarpa Hara) was isolated by simultaneous distillation Sl extraction. The oil content of fresh root was 0.7% (wb) and that of dried root was 2.1 5 (db) and sensory analysis of the oil indicated sweet-balsamic, woody and floral characteristic aroma notes. The oil was fractionated into one hydrocarbon fraction and three oxygenated hydrocarbon fractions by using silica gel column chromatograpy. Each fraction was analyzed by capillary GC and GC-MS. Out of 81 characterized compounds, the major compounds were a-pinene, camphene, $\beta$-pinene, bornyl acetate, borneol , bornyl iso-valerate and sesquiphellandrene and the characteristic floral and woody aroma of neutral fraction of Korean valerian root could be due to be the presence of oxygenated compounds such as borneol, bornyl acetate, bornyl iso-valerate, p-ionone ana $\beta$-ionone epoxide. Comparing the yield of Korean valerian root with those from other origins reported, oil content of Korean valerian root was higher than those of European and Indian origins.

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Flavor Components in the Bellflower Roots (Platycodon glaucum Nakai) (도라지 뿌리의 향기성분에 관하여)

  • Chung, Tae-Yung;Kim, Jeong-Lim;Hayase, Fumitaka;Kato, Hiromichi
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.16 no.2
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    • pp.136-146
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    • 1987
  • Flavor components were trapped by stimultaneous steam distillation-extraction method for investigating it in the bellflower roots and fractionated into four groups such as a neutral, a basic, a phenolic and an acidic fraction. An acidic fraction methylated with diazomethane solution and three others were analysed by GC and GC-MS equipping a fused silica capillary column, and S-containing compounds in these were detected with a flame photometric detector (FPD). The total of one hundred and three compounds from the bellflower roots were identified: they were 6 aliphatic hydrocarbons, 10 aromatic hydrocarbons, 2 terpene hydrocarbons, 12 alcohols, 8 terpene alcohols, 17 aldehydes, 3 terpene aldehydes, 5 ketones, 5 esters, 3 furans, 2 thiazoles, 2 lactones, 2 sulfides, 9 phenols, l2 carboxylic acids and 5 others. The greater part of the others except carboxylic acids were identified from a neutral fraction of which was assumed to be indispensable for the reproduction of bellflower root odor in a sensory evaluation. As a result of a sensory evaluation, 1-hexanal, trans-2-hexenal, 1-hexanol, cis-3-hexenol, trans-2-hexenol, 1-octen-3-ol and so forth identified in a neutral fraction were considered to be the key compounds of grass-like odor in the bellflower roots.

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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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The Aroma Components of Duchung Tea and Persimmon Leaf Tea (두충차와 감잎차의 향기성분)

  • Choi, Sung-Hee
    • Korean Journal of Food Science and Technology
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    • v.22 no.4
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    • pp.405-410
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    • 1990
  • The aroma components of duchung tea and persimmon leaf tea were collected simultaneous distillation and extraction method. Those were analyzed and identified by GC-MS using a fused sillica capillary column. Seventy seven components, including 17 alcohols, 3 hydrocarbons, 15 ketones, 16 aldehydes, 8 esters,8 acids, 8 heterocyclic compounds and 2 phenols were confirmed in duchung tea. Seventy one components, including 17 alcohols, 10 hydrocabrons, 11 ketones, 13 aldehydes, 8 esters, 6 acids, 5 heterocyclic compounds and 1 phenol were confirmed in persimmon leaf tea. The most abundant components of duchung tea were aldehydes(23.31%) including 2-pentenal and heterocyclic compounds(16.71%) including $epoxy-{\beta}-ionone$. The most abundant components of persimmon leaf tea were alcohols(25.57%) including linalool and aldehydes(19.45%) including hexanal and hydrocarbons(10.40%) including ${\alpha}-copaene$.

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Establishment of an Analytical Method for Prometryn Residues in Clam Using GC-MS (GC-MS를 이용한 바지락 중 prometryn 잔류분석법 확립)

  • Chae, Young-Sik;Cho, Yoon-Jae;Jang, Kyung-Joo;Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.531-536
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    • 2013
  • We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

Enantiomeric Separation of Methamphetamine Abused in Korea (우리나라에서 남용되는 메스암페타민의 거울상 이성질체분리)

  • Yoo, Young-Chan;Chung, Hee-Sun;Choi, Hwa-Kyung;Kim, Eun-Mi;Kim, Mi-Kyung;Kim, Sun-Choon
    • YAKHAK HOEJI
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    • v.41 no.3
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    • pp.277-282
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    • 1997
  • Methamphetamine, which is the most commonly abused drug in Korea, exists in terms of d-, l- isomers and a racemate(dl). d-Methamphetamine is a potent central nervous system stimulant, whereas l-Methamphetamine is sold freely as a nasal decongestant. In addition, methamphetamine appears in different ratios of optical isomers by the clandestine synthesis applied. In this study, enetiomeric separation of methamphetamines was estabilished to distinguish the chirality of methamphetamines trafficked and abused in Korea. A gas chromatograph/mass spectrometer(GC/MS) system equipped with an achiral capillary column is used to isolate the isomers of methamphetamine after (S)-N-(trifluoroacetyl)-l-prolyl(TFP) deravatization.After analyzing 10 illicit methamphetamine powders and 10 positive urine samples, following findings were found: d-Methamphetamine was well resolved from l-Methamphetamine by chromatographic separation of TFP derivatibes on DB-5 with retention time of 11.80 and 11.35 min respectively. The detection of d-Methamphetamine in all 10 powders and 10 urine samples proves that all methamphetamines abused in Korea are illegally manyfactured and administred.

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