• Title/Summary/Keyword: Capillary Gas Chromatography

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Identification of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Gas Chromatography/Mass Spectrometry (GC/MS에 의한 오미자 Lignan성분의 동정)

  • Sohn, Hyun-Joo;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.344-349
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    • 1989
  • Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

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Factors Affecting HETP in Capillary Gas Chromatography (모세관 기체 크로마토그래미에서 HETP에 영향을 미치는 인자)

  • 노경호;나영진;정용안
    • KSBB Journal
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    • v.17 no.1
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    • pp.88-92
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    • 2002
  • The election profiles with different flow rates of motile phase were experimentally measured to investigate the effects on HETP in capillary gas chromatography. Based on the correlation coefficient ($r^2$), the first and second moments as well as HETP were determined from the elution cuties, and the parameters used in empirical equations were estimated. The empirical equations were expressed in terms of mobile phase velocity, and the theoretical Golay equation was considered. The samples were d-limonene and perillyl alcohol, potential anticancer agent mainly was contained in the peel of orange. From the experimental results, HETP of the samples were increased with mobile phase velocities. The correlation coefficient of d-limonene was in the range between 0.8265 and 0.8465, while that of perillyl alcohol was between 0.9353 and 0.9374. The total HETP was composed of $H_{g}$, $H_{l}$ and Hc, and Hg had the greatest effect on HETP, but HI showed a negligible effect. In terms of HETP, the optimum velocity of mobile phase was present.

The Determination of 5-Fluorourasil in Human Plasma by a Gas Chromatography-Mass Spectrometry (GC-MS에 의한 혈중 5-fluorouracil의 정량법)

  • Shin, Ho-Sang;Seo, Bae-Seck;Oh, Yun-Suk;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.11 no.1
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    • pp.36-41
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    • 1998
  • A gas chromatography-mass spectrometry method for the determination of 5-fluorourasil in human plasma is described. The method involves a single extraction procedure with 10 ml of isopropanol-ether(20:80) solution and pentafluoro-benzylation. Samples were injected using an automatic injector, followed by separation on a nonpolar capillary column and detection with a mass selective detector(MSD). No endogeneous compounds were found to interfere. The detection limit, based upon an assayed plasma volume of 0.5, was 3 ng/ml. The extraction yield was found to be above 80%. Plasma 5-FU concentrations were determined by this method in about 500 plasma samples from cancer patients undergoing treatment with 5-FU. This method is suitable for monitoring of 5-FU in plasma of cancer patients.

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Analysis of Automotive Paints using Pyrolysis-Gas Chromatography (열분해-가스크로마토그라피에 의한 자동차 페인트 분석)

  • Shon, Sung-Kun;Park, Ha-Sun;Lee, Jin-Sook;Hong, Sung-Wook;Park, Sung-Woo;Cho, Sung-Hye
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.101-107
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    • 2000
  • The automotive paints could be generally differentiated by color, layer sequence and chemistry of the paint layers comprising each of the topcoat and the primer system. The successful identification of hit-andrun a and traffic accidental vehicles from evidential paint fiagments is greatly facilitated with a comprehensive laboratory collection of reference paint samples and the technique for direct analysis without sample preparation. The Pyrolysis-Gas Chromatography(PGC) is a precise and reliable method for performing both quantitative and qualitative analysis of polymeric materials and forensic samples. Our Forensic Laboratory is conducting the examination and identification of 73 reference paint samples; 4 colors of each domestic automotive make that is popular in Korea, by Curie Point Pyrolyzer(JHP-3) and GC with capillary column(ultra alloy-5). This method can be used not only to compare paint traces with their suspected sources, but also to identify the type, make and model of the automotive car.

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A Study on Trans Fatty Acids Contents of Vegetable Oils Added to Can (통조림에 주입된 유지중 Trans 지방산 함량에 관한 연구)

  • 안미영;안명수
    • Korean journal of food and cookery science
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    • v.5 no.1
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    • pp.69-74
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    • 1989
  • Trans fatty acids are formed during refining process of vegetable oils (deodorization), hydrogenation, the high temperature treatment of oils and rancidity. Trans fatty acids contents were measured in vegetable oils added to tuna, oyster and mussel Can by Glass Capillary Gas Chromatography. Also Acid Values, Peroxide Values, iodine Values and Saponification Values of vegetable oils added to Can were determined. The results were as follows; 1. Among vegetable oils added to Can, trans fatty acids isomer of cotton seed oil were mostly t,c-18:2 and t,c,c-18:3. 2. Total average contents of trans fatty acids of soybean oil added to tuna Can (Ab) were shown the highest values among tuna (Aa, Ab), oyster, mussel (Cb) Cans. 3. All of oils added to Can had been keeping safe quality during 1 year or more with low Acid and Peroxide Values.

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Discrimination Analysis of the Geographical Origin of Foods (식품의 원산지 판별분석)

  • Choi, Jin-Young;Bang, Kyong-Hwan;Han, Kee-Young;Noh, Bong-Soo
    • Korean Journal of Food Science and Technology
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    • v.44 no.5
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    • pp.503-525
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    • 2012
  • Consumers are increasingly concerned about the origin of foods, so the geographical origin of foods has been a major topic of debate and extensive research. Various instrumental methods (e.g. high performance liquid chromatography (HPLC), gas chromatography (GC), capillary electrophoresis (CE), electronic nose, near-infrared spectroscopy (NIRS), nuclear magnetic resonance spectroscopy (NMR), DNA analysis, multi-isotope analysis) in conjunction with statistical analysis, were developed and applied in attempt to provide reliable answers to their geographical origin. This study reviews current developments in the application of various methods for a clear geographical origin of foods. The limitation of discrimination analysis for geographical origin was also discussed.

Separation and Identification of Polycyclic Aromatic Compounds in Pyrolysis Products of Cellulose and Lignin (셀룰로오스와 리그닌의 열분해 생성물중의 여러고리 방향족화합물의 분리와 동정)

  • Park, Nae-Joung;Lee, Milton L.
    • Journal of the Korean Chemical Society
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    • v.28 no.4
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    • pp.244-250
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    • 1984
  • Separation and identification of the polycyclic aromatic compounds (PAC) from pyrolysis products of cellulose and lignin were performed using a combination of acid-base solvent partitioning and silicic acid column chromatography with fused-silica capillary column gas chromatography/ mass spectrometry. Sixteen PAC were positively identifited by retention indices and mass spectra data. Both materials produced the same kinds of PAC. But lignin produced much more PAC than cellulose. Almost no highly carcinogenic heterocyclic PAC containing nitrogen and sulfur were produced.

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Volatile Flavor Components in Bogyojosaeng and Suhong Cultivars of Strawberry (Fragaria ananassa Duch.)

  • Park, Eun-Ryong;Lee, Hae-Jung;Kim, Kyong-Su
    • Preventive Nutrition and Food Science
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    • v.5 no.3
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    • pp.119-125
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    • 2000
  • Volatile flavor components of two strawberry (Fragaria ananassa Duch.) varieties, Bogyojosaeng and Suhong, ere extracted by SDE(Simultaneous steam distillation and extraction) using a mixture of n-pentane and diethylether (1:1, v/v) as an extract solvent. Analysis of the concentrate by capillary gas chromatography and gas chromatography-mass spectrometry led to the identification of 146 and 153 components in Bogyojosaengand Suhong respectively. There were 49 esters, 25 alcohols, 20 ketones, 24 aldehyds, 6 acids, 9 terpenes and terpene derivatives, 2ethers, 11 unknowns and miscelaneous in Bogyojosaeng and 67 ethers, 9 unknowns and miscellaneous in Suhong. Among these, (E)-2-hexenyl acetae (4.56%) in Bogyojosaeng and (E)-nerolidol (12.38%) in Suhong were major compounds and aceticacid, (E)-2-hexenal, hexyl acetate, ethyl acetate, ethyl butanoate, methyl butanoate, ethyl hexanoate and ${\gamma}$-dodecalactone were the main components in each sample, though there were several differences in composition and threshold of volatile compounds. Total contents of volatile components isolated and identified in Bogyojosaeng an Suhong were 9.010 and 12.527 mg/kg, respectively.

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Determination of Captan, Folpet, Captafol and Chlorothalonil Residues in Agricultural Commodities using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Captan, Folpet, Captafol 및 Chlorothalonil의 잔류분석법)

  • Lee, Su-Jin;Hwang, Young-Sun;Kim, Young-Hak;Kwon, Chan-Hyeok;Do, Jung-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.29 no.2
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    • pp.165-175
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    • 2010
  • A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

Chiral Separation of Lactic Acid in Culture Media and Cells of Lactobacillus delbrueckii subsp. lactis as O-Pentafluoropropionylated (S)-(+)-3-Methyl-2-Butyl Ester by Achiral Gas Chromatography-Mass Spectrometry

  • Paik, Man-Jeong;Nguyen, Duc-Toan;Yoon, Jae-Hwan;Chae, Han-Seung;Kim, Kyoung-Rae;Lee, Gwang;Lee, Pyung-Cheon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2418-2422
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    • 2011
  • The enantiomeric separation of lactic acid for its absolute configuration has become important task for understanding its biological origin and metabolic process involved in the formation of lactic acid. It involves the conversion of enantiomers as diastereomeric O-pentafluoropropionylated (S)-(+)-3-methyl-2-butyl ester and the direct separation by gas chromatography-mass spectrometry on a achiral capillary column. The (R)- and (S)-lactic acids were completely separated with a high resolution of 1.9. The newly developed method showed good linearity (r ${\geq}$ 0.999), precision (% relative standard deviation = 3.4-6.2), and accuracy (% relative error = -7.7-1.4) with the detection limit of 0.011 ${\mu}g/mL$. When the method was applied to determine the absolute configuration of lactic acid in Lactobacillus delbrueckii subsp. lactis 304 (LAB 304), the composition (%) of (R)-lactic acid in the cell pellet and in the culture medium were $89.0{\pm}0.1$ and $78.2{\pm}0.4$, respectively. Thus, it was verified that the present method is useful for the identification and composition test of lactic enantiomers in microorganisms.