• Title/Summary/Keyword: GC column

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Isolation of 3,4-Dihydroxybenzoic Acid with Antimicrobial Activity from Bark of Aralia elata (두릅수피에서 항미생물활성을 갖는 3,4- dihydroxybenzoic acid의 분리)

  • Ma, Seung-Jin;Ko, Byoung-Seub;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.27 no.5
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    • pp.807-812
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    • 1995
  • The methanol extracts of Aralia elata bark showed antimicrobial activities against bacteria, yeast, fungi. The solvent fractionated acidic fraction that showed the activity was then successively purified with silica gel adsorption column chromatography, Sephadex LH-20 column chromatography, silica gel partition column chromatography, HPLC and TLC. The isolated major active substance was identified as 3,4-dihydroxybenzoic acid by MS, GC-MS, IR, $^{1}H-NMR\;and\;^{13}C-NMR$. The content of 3,4-dihydroxybenzoic acid was 0.869㎎/g in dried bark of Aralia elata.

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Comparison of GC-Profile on Tobacco Smoke Components (담배 연기성분의 GC-Profile 특성비교)

  • 나효환;한상빈;복진영;이운철;백순옥;장기철;양광규
    • Journal of the Korean Society of Tobacco Science
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    • v.16 no.2
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    • pp.152-162
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    • 1994
  • This study was designed to establish an analytical method for the properties of leaf tobacco smoke. Lyophilized TPM from leaf tobacco smoke was extracted with MeOH, dried under reduced pressure, and trimethyl-silylated(TMS). Gas chromatography of the material using SPB-5 column showed 120 quantifiable peaks. Among those, 26 compounds including a hydrocarbons, Neophytadiene. and Levulinic acid could be identified through GC-MS. Smoke properties of 5 manufacturing grades and 2 oriental cultivars of domestic and imported leaf tobacco including AB3O-1 were analyzed. For flue-cured tobacco, content of the compounds in the smoke was generally higher in American leaf tobacco except for glycerol compounds. For burley tobacco, domestic leaves were found to have much higher amount of smoke compound than imported leaves. Among oriental tobacco, Izmir contained slightly higher amount of smoke compounds than Basma. Key words : GC - profile. TPM. TMS. Leaf tobacco.

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Analysis of Phenolic Acids in Tobacco Leaf by GC/MS (GC/MS에 의한 잎담배중 Phenolic Acid의 분석)

  • 박진우
    • YAKHAK HOEJI
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    • v.26 no.2
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    • pp.129-132
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    • 1982
  • A GC/MS method was developed to analyze phenolic acid extract from tobacco leaf. Extracted acids were converted to their methyl esters by refluxing with 3M hydrogen chloride in methanol, and the esters were reacted with his (trimethylsilyl) trifluoroacetamide plus 10% trimethylchlorosilane to silylate the phenolic groups. Derivatives of standard salicylic, p-hydroxybenzoic, vanillic, gentisic, p-coumaric, syringic, ferulic, and sinapic acids prepared by this procedure were analyzed by GC/MS on $20m{\times}0.2mm$ column of SE-54 glass capillary. GC/MS analysis of the extract from tobacco leaf revealed the presence of salicylic, p-hydtoxybenzoic, vanillic, gentisic, protocatechuic, p-coumaric, syringic, gallic, ferulic, caffeic, sinapic, and quinic acids, respectively. The quantitative analysis of these phenolic acids were achieved by using multiple ion selection technique.

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Determination of N. N-dimethylaniline in penicillins by GC-MS

  • Choi, Jung-Kap;Park, Man-Ki
    • Archives of Pharmacal Research
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    • v.4 no.2
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    • pp.85-90
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    • 1981
  • A quantitative GC-MS spectrometric assay was used for the determination of residual N, N-dimethylaniline as a contaminant in commercial penicillin derivatives from various sources. The assay utilizes selective ion focusing to monitor in a GC effluent the molecular ions of DMA generated by electron impact ionization. This method includes dissolution of the sample in alkaline solution, extraction of organic base with cyclohexane and injection into GC-MS with a 3% OV-17 column. Levels of 50 ppb of DMA were easily measured with a coeffecient of varation less than 5 % and recoveries from spiked samples exceeded 97 %. The results of the determinations of DMA in various commercial penicillins were relatively free of this contaminant.

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Effects of Phosphorus Starvation on Fatty Acid Production by Microalgae Cultivated from Wastewater Environment (인 결핍에 따른 하수배양 미세조류의 지방산 특성 분석 연구)

  • Woo, Sung-Geun;Park, Joon-Hong
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.32 no.4B
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    • pp.253-259
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    • 2012
  • Wastewater-adapted microalgae such as Chlorella vulgaris AG10032, Ankistrodesmus gracilis SAG278-2 and Scenedesmus quadricauda AG10308 are useful biological resources for recovering biofuel and other bio-based materials from wastewater because of their efficient removals of nitrogen and phosphorus from wastewater and their high fatty acid contents in biomass. Although the concentrations of phosphorus typically vary in wastewater environment, very little is known about the effect of phosphorus concentration, especially phosphorus starvation, on microalgal fatty acid synthesis. This is partially due to the lack of methodological establishment for algal fatty acid analysis. In this study, we compared the analysis performances of microalgal fatty acids by two different methods; one is a non-polar GC (gas chromatography) column based method, which is generally used for microbial fatty acids, and the other is a polar WAX-type GC column method, which is typically used for plant fatty acids. And then, we explored the effect of phosphorus concentration levels on fatty acid production in microalgae cultivated from wastewater. As results, the polar WAX-type column method has better ability to separate poly unsaturated fatty acids (PUFA) including $C_{18:3}$ (linolenic acid), and was found to be more applicable in analyzing fatty acids from wastewater-cultivated microalgae than the non-polar column method. The fatty acid characterization by the WAX-type column method revealed little effect of phosphorus starvation on the quantity and composition of fatty acids from wastewater-cultivated microalgae.

Pattern Analysis of Volatile Components for Domestic and Imported Cnidium officinale Using GC Based on SAW Sensor (SAW센서를 바탕으로한 GC를 이용한 국내산 및 수입산 천궁의 향기 패턴분석)

  • Oh, Se-Yeon;Noh, Bong-Soo
    • Korean Journal of Food Science and Technology
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    • v.35 no.5
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    • pp.994-997
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    • 2003
  • Domestic and imported Cnidium officinale were investigated using GC based on a SAW sensor. Volatile components from the herb were detected by GC with a Surface Acoustic Wave (SAW sensor without any pretreatment. This system produced a frequency proportional to the amount of column effluent deposited on the SAW sensor. It could discriminate between domestic and imported Cnidium officinales. This was achieved by using a pattern recognition and a visual pattern called a $VaporPrint^{TM}$, derived from the frequency and chromatogram of the GC-SAW sensor. The origins of Cnidium officinale was well discriminated with the direct use of $VaporPrint^{TM}$.

Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

Development of Analytical Method for Fipronil Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Fipronil의 잔류 분석법 개발)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.309-317
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    • 2015
  • BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

Simultaneous Determination of Biliary Free and Phospholipid Fatty Acids Using Gas Chromatography-Mass Spectrometry (GC-MS를 이용한 담즙내 유리 지방산 및 인지질 지방산들의 동시 분석)

  • Yang, Yoon Jung;Lee, Seon Hwa;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.592-600
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    • 2000
  • The concentration of free fatty acids and fatty acid composition as well as cholesterol supersaturation in bile may be an important factor in the gallstone formation. Therefore, we simultaneously determinded 23 fatty acids in bile by selected ion monitoring (SIM) method of gas chromatography-mass spectrometry (GC-MS). Biliary fatty acids were extracted by aminopropyl column and the extracts with (phospholipid fraction) or without (free fatty acid fraction) alkaline hydrolysis of phospholipid were derivatized with MSTFA/TMCS (N-methyl-N-trimethylsilyl-trifluoroacetamide/trimethylsilylchloride) mixture in order to be detected on the GC-MS. The recovery range of this method was 61.1-99.0% and the RSD value of within-a-day and day-to-day test were 3.1-25.6% and 3.8-27.0%, respectively. Using this method, biliary profile was investigated in the bile of normal controls and patients with gallstones. The amounts and their distribution of free and phospholipid fatty acids showed different pattern between normal subjects and patients.

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Volatile flavor components of Korean ginger(Zingiber officinale Roscoe)extracted with liquid carbon dioxide (액체 이산화탄소 추출법에 의한 생강 (Zingiber officinale Roscoe)의 향기성분)

  • Kim, Myung-Kon;Na, Mun-Su;Hong, Jai-Sik;Jung, Soon-Taek
    • Applied Biological Chemistry
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    • v.35 no.1
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    • pp.55-63
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    • 1992
  • The essential oil of Korean ginger(Zingiber officinale Roscoe) was isolated by liquid carbon dioxide extraction method and fractionated into one hydrocarbon fraction and two oxygenated hydrocarbon fractions by using silica gel column chromatography. The compositions of the resulting oils were investigated by GC and GC-MS spectrometry. Out of 102 identified compounds, 44 were identified by comparing GC retention time and mass spectral data with authentic samples and 58 were tentatively identified according to mass spectral data only. The major compounds of hydrocarhon fraction were $zingiberene,\;{\beta}-sesquiphellandrene,\;{\gamma}-bisabolene,\;{\gamma}-cardinene,\;ar-curcumene$, and those of oxygenated hydrocarbon fractions wee geranal, sesquisabinene hydrate, borneol and zingiberenol. The major compounds of ginger oil were zingiberene, $citronellol+{\beta}-sesquiphellandrene,\;geranial,\;{\gamma}-bisabolene\;and\;ar-curcumene+geranyl\;acetate$, and ginger oil contained higher amounts of sesquiterpene hydrocarbons. The yield of extract was 6.96%.

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