• Title/Summary/Keyword: gas-liquid chromatography

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Isotope-Dilution Mass Spectrometry for Quantification of Urinary Active Androgens Separated by Gas Chromatography

  • Lee, Su-Hyeon;Choi, Man-Ho;Lee, Won-Yong;Chung, Bong-Chul
    • Mass Spectrometry Letters
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    • v.1 no.1
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    • pp.29-32
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    • 2010
  • Cross reacting antibodies can cause an overestimation of the results of immunoassays. Therefore, alternative methods are needed for the accurate quantification of steroids. Gas chromatography combined with isotope-dilution mass spectrometry (GC-IDMS) is developed to quantify urinary active androgens, testosterone, epitestosterone and dihydrotestosterone, which are clinically relevant androgens to both hair-loss and prostate diseases. The method devised involves enzymatic hydrolysis with $\beta$-glucuronidase, solid-phase extraction, liquid-liquid extraction using methyl tert-butyl ether and subsequent conversion to pentafluorophenyldimethylsilyl-trimethylsilyl (flophemesyl-TMS) derivatives for sensitive and selective analysis in selected-ion monitoring mode. Flophemesyl-TMS derivatization not only eliminates matrix interference but also has a good peak resolution within a 6 min-run. A selective and sensitive GC technique with flophemesyl-TMS derivatives also allows accurate quantitative analysis of three active androgens when combined with IDMS. The limit of quantification of the three analytes was <50 pg/mL, and extraction recoveries ranged from 91.9 to 102.1%. The precision and accuracy were 1.2~6.5% and 89.0~106.7%, respectively. This GC-IDMS method can be useful for evaluating the drug efficacy and monitoring the biological processes responsible for male-pattern baldness and prostate diseases.

Cellular Lipid Formation by Petroleum Hydrocarbon Fermentation (石油炭化水素 醱酵에 의한 脂質의 生成)

  • Park Tai Won;Suh Hyung Joon
    • Journal of the Korean Chemical Society
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    • v.21 no.6
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    • pp.449-452
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    • 1977
  • The effect of carbon number of hydrocarbon used as a carbon source in the production of cellular lipid of Rhodotorula sp. and its fatty acid composition were investigated. Using Rhodotorula sp. on n-tetradecane and n-hexadecane whose carbon numbers are even, fermentation was carried out in a jar fermentor of 2 liter-capacity at $28^{\circ}C$, with pH range of 4.0∼4.6 and at oxygen flowing rate of 0. 4 vvm and agitation velocity of 1000 rpm. Drying the produced cell after completion of fermentation, cellular lipid was extracted from the cell using soxhlet extractor and examined its fatty acid composition by gas-liquid chromatography. Cellular lipid content in the cell produced on n-tetradecane and n-hexadecane were 12.0 % and 25,8 % on the basis of dry cell weight, respectively and their fatty acids were mostly even numbered in carbon number.

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Analysis of the chemical burn-inducing components from the extraction of herb drug-mixed-medicine

  • Lee, Ju-Seon;Lim, Mie-Ae;Park, Hye-Young;Eo, Sang-Heui;Lee, Han-Sun;Park, Yoo-Sin
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.281.1-281.1
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    • 2002
  • Psoralen(7H-Furo[3.2-g] [1]benzopyran-7-one) and angelicin(2-Oxo-[2H]- furo[2.3-h]-1-benzopyran) are angular furocoumarin with diverse photobiological effects. They are major components of Psoralea corylifolia L.(破古紙). Psoralea corylifolia L. is used for a tonic and nursing one's energy. It can be also used for loss of virility. vitiligo. a skin disease, etc.. But a well known and often appreciated side effects f psoralens is the hyperpigmentation caused by this treatment. A women who used the herbal drug-mixed-medicine named'sobaeksu' to treat her vitiligo made a complaint against the orinetal medical doctor. She complained that her skin got burned to 2nd degree by the liquid. 'sobaeksu' through a medical celtficate. So we analyzed the components of that liquid with gas chromatography and gas chromatography/mass spectometry. It has 57.3% ethyl alcohol and two kinds of psoralens. Psoralens were psoralen and angelicin and each one of their contained quantity was 0.128mg/ml and 0.123mg/ml.

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Optimization of Gas-Liquid Chromatographic Parameters for the Multiresidue Analysis of 24 Pesticides (잔류농약 24성분의 다성분 동시분석을 위한 기체크로마토그래피 조건의 최적화)

  • Lee, Eun-Ju;Kim, Woo-Seong;Park, Kun-Sang;Oh, Jae-Ho;Kim, Dai-Byung
    • The Korean Journal of Pesticide Science
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    • v.4 no.2
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    • pp.11-17
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    • 2000
  • Optimum parameters were investigated for the simultanious analysis of 24 pesticide residuces using gas-liquid chromatography with electron capture detection. Electronic pressure control(EPC) on column enhanced resolution of 24 analyzes. Using DB-17, SPB-608, and Ultra-2 capillary column without EPC incomplete separation was observed in some pairs of pesticides. When EPC function was adopted, no severe overlapping was observed on SPB-608 column in every pesticides except vinclozolin/acetochlor pair. Total running time was 45 min, much shorter than $69{\sim}81$ min when used without EPC. Limit of determination of each analyze ranged $0.1{\sim}12.9$ ng/mL.

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Gas Liquid Chromatographic Studies on Sugars and Organic Acids in Different Portions of Hot Pepper Fruit (Capsicum annuum L.) (Gas Liquid Chromatography에 의한 고추 부위별(部位別) 당(糖) 및 유기산(有機酸) 조성(組成)에 관한 연구(硏究))

  • Lee, Sung-Woo
    • Korean Journal of Food Science and Technology
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    • v.11 no.4
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    • pp.278-282
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    • 1979
  • Sugars and organic acids in Korean hot pepper fruit (C, annuum L.) according to its portions, pericarp, seeds and placenta, were determined by gas liquid chromatography (GLC). ${\alpha}-\;and\;{\beta}-fructoses,\;{\alpha}-\;and\;{\beta}-glucoses$, galactose, sucrose and maltose were identified. Major sugar in pericarp was fructose, while those in seeds and placenta were surose and fructose. Amount of free sugars in seeds was higher than that in pericarp or placenta. Succinic, fumaric, malic, tartaric, citric and quinic acids were found. Citric acid was a major organic acid found in pericarp and placenta. The amount of each identified organic acid, however, was similar in seeds. Quantity of total organic acids identified in pericarp or placenta was higher than that in seeds.

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Determination of Monocrotophos Residues by HPLC

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.245-250
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    • 2004
  • An analytical method was developed to determine monocrotophos residues in apple, citrus, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Monocrotophos was extracted with acetone from apple, citrus and moist soil samples. The extract was concentrated, added with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives. Dichloromethane partition was then followed to recover monocrotophos from the aqueous phase. Silica gel column chromatography was employed to further purify the extract prior to HPLC determination. Reverse-phase HPLC using an oct-adecylsilyl column was successfully applied to separate and quantitate the monocrotophos residue in sample extracts at the wavelength of 230 nm. Overall recoveries of monocrotophos from fortified samples averaged $95.3{\pm}2.1%$ (n=6), $970{\pm}0.7%$ (n=6), and $92.8{\pm}4.3%$ (n=12) for apple, citrus, and soil, respectively. The proposed method was quite reproducible and sensitive enough to replace the troublesome gas-liquid chromatographic analysis for monocrotophos residues.

Analysis of 3-MCPD and 1,3-DCP in Various Foodstuffs Using GC-MS

  • Kim, Wooseok;Jeong, Yun A;On, Jiwon;Choi, Ari;Lee, Jee-yeon;Lee, Joon Goo;Lee, Kwang-Geun;Pyo, Heesoo
    • Toxicological Research
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    • v.31 no.3
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    • pp.313-319
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    • 2015
  • 3-Monochloro-1,2-propanediol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) are not only produced in the manufacturing process of foodstuffs such as hydrolyzed vegetable proteins and soy sauce but are also formed by heat processing in the presence of fat and low water activity. 3-MCPD exists both in free and ester forms, and the ester form has been also detected in various foods. Free 3-MCPD and 1,3-DCP are classified as Group 2B by the International Agency for Research on Cancer. Although there is no data confirming the toxicity of either compound in humans, their toxicity was evidenced in animal experimentation or in vitro. Although few studies have been conducted, free 3-MCPD has been shown to have neurotoxicity, reproductive toxicity, and carcinogenicity. In contrast, 1,3-DCP only has mutagenic activity. The purpose of this study was to analyze 3-MCPD and 1,3-DCP in various foods using gas chromatography-mass spectrometry. 3-MCPD and 1,3-DCP were analyzed using phenyl boronic acid derivatization and the liquid-liquid extraction method, respectively. The analytical method for 3-MCPD and 1,3-DCP was validated in terms of linearity, limit of detection (LOD), limit of quantitation, accuracy and precision. Consequently, the LODs of 3-MCPD and 1,3-DCP in various matrices were identified to be in the ranges of 4.18~10.56 ng/g and 1.06~3.15 ng/g, respectively.

A Study of Odorants and Volatiles Released from Pork Belly Meat When Treated by Different Cooking Methods (삼겹살 구이로부터 발생하는 유해물질의 특성 연구)

  • Kim, Bo-Won;Kim, Ki-Hyun;Kim, Yong-Hyun;Ahn, Jeong-Hyeon
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.3
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    • pp.211-222
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    • 2014
  • Pork belly meat is one of the most preferred food items for many Korean people. The odorants released from cooking of pork belly meat were measured by three kinds of cooking methods (Charcoal-grill (C), Electric Pan (E), and Gas burner-pan (G)). A total of 16 target compounds including carbonyl compounds, volatile organic compounds, and poly aromatic hydrocarbon were selected and analyzed for comparative purposes. Their emission concentrations were quantified using HPLC-UV, GC-MS, GC-TOF-MS, etc. The gas samples collected by Charcoal-grill cooking showed generally enhanced concentrations of most target compounds among all three kinds of cooking methods. In Charcoal-grill, concentration of benzene, formaldehyde and pyrene went up to 543, 516, and 402 ppb, respectively. It the results are compared in terms of the sum of odor intensity, the highest value (4.25) was also seen from Charcoal-grill. The results of this study confirm that the significantly reduced emission of harmful pollutants can be attained, it pork belly meat is cooked by the Gas or electric pan instead of Charcoal-grill.

Isolation of 3,4-Dihydroxybenzoic Acid, Which Exhibits Antimicrobial Activity, from Fruits of Gardenia jasminoides Ellis (치자 열매에서 항미생물 활성을 갖는 3,4-Dihydroxybenzoic Acid의 분리)

  • Yim, Cheol-Keun;Moon, Jae-Hak;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1386-1391
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    • 1999
  • The methanol extract of Gardenia jasminoides Ellis showed antimicrobial activity against bacteria and yeasts. The extract was successively purified with solvent fractionation, silica gel adsorption column chromatography, Sephadex LH-20 column chromatography, octadecylsilane column chromatography. The purified active substance was isolated by high performance liquid chromatography. The isolated compound was 3,4-dihydroxybenzoic acid which was determined by mass spectrometer, gas chromatograph-mass spectrometer, $^{1}H-nuclear$ magnetic resonance, $^{13}C-nuclear$ magnetic resonance and two-dimensional nuclear magnetic resonance. The content of 3,4-dihydroxybenzoic acid was $32.7\;{\mu}g/g$ in dried fruits of Gardenia jasminoides Ellis.

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Comparison of Triglyceride Composition between Red Pepper Seed Oils Harvested from the Chungsong and Youngyang Areas (청송.영양산 고추씨 기름의 Triglyceride 조성의 비교)

  • 김동수;전선미;정동윤;김현대;박영호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.20 no.3
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    • pp.225-232
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    • 1991
  • A Study was carried out to elucidate the triglyceride compositions of the red pepper seed oils harvested from two different areas. The oil was extracted from the red pepper seed with nhexane. Each triglyceride of the oil was separated by thin layer chromatography (TLC) and fractonated by reverse phase high performance liquid chromatography (HPLC) on the basis of acyl carbon numbers, and partition number group(PN) and fatty acid composition of triglyceride were analyzed by gas liquid chromatography (GLC). From the results, it was found that the red pepper seed oils of the Chungsong and Youngyang areas consisted of 14 and 18 kinds of triglycerides, respectively. The red pepper seed oil of the Chungsong area consisted of (C18:2, C18:2, C18:2=41.0%), (C16:0, C18:2, C18:2=37.1%), and that of the Youngyang area consisted of (C18:2, C18:2, C18:2=41.0%), (C16:0, C18:2, C18:2=36.3%) and (C16:0, C16:2, C18:2=8.4%), as the major triglycerides.

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