• Title/Summary/Keyword: gas chromatography column

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Separation of Tetrodotoxin, DHA and EPA from Pufferfish Liver Waste (복어간 폐기물로부터 Tetrodotoxin, DHA 및 EPA의 분리)

  • 차병윤;최진석;임정규;이동익;이원갑;이은열;김희숙;김동수
    • Journal of Life Science
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    • v.10 no.2
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    • pp.115-124
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    • 2000
  • The present study was undertaken to separate the available components effectively, such as tetrodotoxin(TTX), docosahexaenoic acid(DHA, C22:6,ω-3) and eicosapentaenoic acid (EPA, C20:5,ω -3) from pufferfish liver waste, which are known to have high values as bioactive materials. By using ultrafiltration, it was possible to separate high contents of 68mg TTX from pufferfish liver waste. In contrast, by activated charcoal column, it was to obtain about 54mg TTX. The recovering ratios were 65.3% and 45.0% in the two different methods of ultrafiltration and activated charcoal column, respectively. From the results of HPLC and gas chromatography-mass spectrometry(GC-MS), the obtained toxins were identified to be TTX and its derivatives. In addition, it was also possible to obtain 72.3g DHA and 11.4g EPA from 1kg of pufferfish liver by high performance liquid chromatography (HPLC). These amounts of DHA and EPA were also 17.70% and 1.04% in the total lipid of pufferfish liver oil from analysis of gas chromatography(GC), respectively.

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Determination of Dienestrol in Dienestrol Cream by Gas Liquid Chromatography (Gas Liquid Chromatography에 의한 Dienestrol Cream 중의 Dienestrol 정량)

  • 백남호;박만기;염정록
    • YAKHAK HOEJI
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    • v.23 no.1
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    • pp.7-10
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    • 1979
  • A gas chromatographic determination of dienestrol in dienestrol cream has been studied. Dienestrol cream was dissolved in pyridine and silylation was done by using N, O-bis (trimethylsilyl) trifluoroacetamide. The derivative was injected into 3% silicone OV-17 column for chromatographic estimation. The dienestrol peak was found to be well separated from the other components of the cream. The detection limit was obtained to be $5.6{\times}10^{11}$ mol of dienestrol for this method. As there is no need for prior separation procedure, this experiment is extremely simple and less time consuming as compared to the conventional methods for estimation of dienestrol in cream.

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Determination of Nitrogen Dioxide by Gas-Solid Chromatography (기.고 크로마토그래피법에 의한 이산화질소 측정)

  • Yim, Going;Serth Robert W.
    • The Journal of Engineering Research
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    • v.2 no.1
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    • pp.147-149
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    • 1997
  • Nirogen dioxide is rapidly converted to nitric oxide by the water absortbed on a Linde Molecular Sieve column. The resultant wave form is indistinguishable from that of pure nitric oxide introduced to the column. Thus, by conversion to the low boiling nitric oxide, the complication of oxidation of organic partitioning liquids is obviated.

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Analytical Methods for the Isolation of Dehydrotomatine and ${\alpha}$-Tomatine in Tomato Fruits by Use of Alumina Column Chromatography and High-Performance Liquid Chromatography (Alumina Column Chromatography와 HPLC에 의한 토마토의 Dehydrotomatine 및 ${\alpha}$-Tomatine 단리방법 연구)

  • Choi, Suk-Hyun;Kim, Hyen-Ryung;Lee, Jin-Shik
    • The Korean Journal of Food And Nutrition
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    • v.23 no.4
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    • pp.556-561
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    • 2010
  • Tomato fruits(Lycoperisicon esculentum) synthesize the glycoalkaloids dehydrotomatine and ${\alpha}$-tomatine, possibly as defense against bacteria, fungi and insects. We developed a new effective method to prepare and purify dehydrotomatine and ${\alpha}$-tomatine that exists in tomato fruits using alumina column chromatography and high performance liquid chromatography (HPLC). The tomato glycoalkaloids(TGA) in tomato was extracted with 2% acetic acid, and then precipitated with ammonium hydroxide(pH=10.5). The dry precipitate substance was applied on alumina column, and then fractionated with water saturated n-butylalcohol. The TGA(Fr. No. 26~36) were collected and dried under reduced pressure. The TGA was performed on a reverse phase HPLC(Inertsil ODS-2, $5\;{\mu}m$), eluted with acetonitrile/20mM $KH_2PO_4$(24:76, v/v) at 208 nm. Two peaks were detected on HPLC, and individual peak was collected by repeating HPLC. Furthermore, to confirm the identity dehydrotomatine and ${\alpha}$-tomatine, each peak isolated was hydrolyzed with 1N HCl into sugar and aglycone tomatidine. The sugars were converted to trimethylsilyl ester derivatives. The nature and molar ratios of sugars were identified by gas-liquid chromatography(GLC) and the aglycone by high-performance liquid chromatography(HPLC). The first peak (Rt=17.5 min) eluted from HPLC was identified as dehydrotomatine, and second peak(Rt=21.0 min) was as ${\alpha}$-tomatine. This technique has been used effectively to prepare and isolate dehydrotomatine and ${\alpha}$-tomatine from tomato fruits.

Simultaneous Determination of Haloperidol and Its Metabolite, Reduced Haloperidol, in Plasma by Gas Chromatography Using Nitrogen Phosphorous Selective Detection (Gas Chromatography-Nitrogen Phosphorous Selective Detection을 이용한 혈장중 Haloperidol 및 대사체인 Reduced Haloperidol의 동시정량)

  • Park, Kyoung-Ho;Lee, Min-Hwa;Shim, Chang-Koo;Lee, Myung-Gull;Park, Jong-Sei
    • Journal of Pharmaceutical Investigation
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    • v.22 no.3
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    • pp.197-204
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    • 1992
  • A gas chromatographic method using nitrogen phosphorous selective detection was developed for simultaneous determination of haloperidol and its metabolite, reduced haloperidol, in human plasma. Combelen was used as internal standard, The method involved extraction and trimethylsilylation followed by the injection of $2-4\;{\mu}l$ of benzene layer, which was used to dissolve the trimethylsilylated derivatives of haloperidol and reduced haloperidol, onto SE-54 column [5% phenyl methyl silica fused capillary column, $16m{\times}0.22\;mm$ $(I.D.){\times}0.33\;{\mu}m$ (coated thickness)]. The temperature of column oven was programmed from $200^{\circ}C\;to\;300^{\circ}C$ at the increase rate of $10^{\circ}C/min and also the temperatures of injector and detector were set at $300^{\circ}C$. Helium was used as carrier gas and its flow rate was maintained at 30 ml/min. The detection was conducted with nitrogen phosphorous selective detector. The retention times for combelen, reduced haloperidol and haloperidol were found to be 9.14, 9.75 and 9.99 min, respectively. The detection limits for haloperidol and reduced haloperidol in human plasma were both 0.2 ng/ml. The coefficients of variation of the intra-assay were generally low (below 9.8%). The mean absolute recoveries of added haloperidol and reduced haloperidol from plasma were 72% and 84%, respectively. No interferences from endogenous substances were found.

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폐기물 매립지 토양에서의 PCBs 분석법

  • Lee Jeong-Hwa;Jeon Chi-Wan;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.199-201
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    • 2005
  • This paper describes a simple procedure for the quantitative analysis of 7 PCBs (polychlorinated biphenyls) in soils on the waste reclaimed land, The procedure involved sample clean up using silicagel column, acetonitrile partition and sulfuric acid procedures. The instrumental technique is applied GC/PDD(gas chromatography/pulsed discharge detector) and GC/ECD(gas chromatography/electron capture detector). Concentration of $sub-{\mu}g/g$ level was attainable with 20g soils on the waste reclaimed land.

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The Screening and Pattern Comparison of Organic Acids in 3 Kinds of Medicinal Herbal Extracts (3가지 약용 허브 추출물에 함유된 유기산 검색 및 조성 비교)

  • Chung, Ha-Yull;Jung, Do-Hyun;Park, Young-Joon
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.997-1001
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    • 2000
  • The organic acids in 3 kinds of medicinal herbal extracts were screened and compared each other according to their organic acid contents by an efficient gas chromatographic method. It involves solid-phase extraction of organic acids using Chromosorb P with subsequent conversion to stable tert-butyldimethysilyl derivatives for the direct analysis by capillary column gas chromatography and gas chromatography-mass spectrometry. Total of 24 organic acids were reproducibly identified from 3 kinds of herbal extracts. When the GC profiles were simplified to their retention index spectra, characteristic patterns were obtained for each herb sample. As expected, three kinds of herbal extracts showed three distinct patterns.

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Extraction and Bioassay of Allelochemicals in Jerusalem Artichoke

  • Sungwook Chae;Lee, Ho-Jin
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.4
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    • pp.309-316
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    • 2001
  • Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

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Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.