• Title/Summary/Keyword: GC column

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Tissue Distribution of Tropane Alkaloids in Rats and its Determination by GC/MS After the Oral Administration of Scopolia Rhizome (GC/MS에 의한 tropane alkaloids의 분석 및 흰쥐의 생체내 분포)

  • 임미애;백승경;이주선;박세연
    • YAKHAK HOEJI
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    • v.43 no.6
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    • pp.729-735
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    • 1999
  • Scopolia rhizome is mistaken as an atractylodes rhizome because of their similarities in shape. That is why atractylodes rhizome imported from China sometimes contain scopolia rhizome, which is very toxic. 8 persons were intoxicated atractylodes after taking imported atractylodes rhizome which is tainted. In kampo medicine prepared with such imported atractylodes rhizome, the level of tropane alkaloids ranged from 1.12∼4.34 mg/dose. In this study, we tried to investigate the tissue distribution of scopolia rhizome in rats. The extracts of scopolia was administered orally to rats (a single dose of 10mg/kg, 20mg/kg and 7 days repeated dose of 10mg/kg). Their blood was collected at 0.5, 1, 2, 4, 6 hrs, and liver, kidney, lung and spleen were collected after 6 hrs. The tissue homogenate was applied to solid phase extraction column for the determination of tropane alkaloids. After the oral administration of 20mg/kg scopolia extracts, l-hyoscyamine was detected in rat blood to 2 hrs after dosing. The concentration of tropane alkaloids was the highest in liver followed by lung, kidney and spleen. However, lung, kidney and spleen were similar in amount.

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Analysis of the Organic Acid Contaminants on the surface of TEN-STORIED STONE PAGODA ON THE SITE OF WON-GAKSA (원각사지 십층석탑 오염물의 유기산 분석)

  • Lee, Kyu-Shik;Han, Sung-Hee
    • 보존과학연구
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    • s.16
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    • pp.112-122
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    • 1995
  • TEN-STORIED STONE PAGODA ON THE SITE OFWON-GAKSA(Temple) which is one of three marble pagodas in South Korea, were dated from the thirteenth year of the reign of King Sejo(1467). On the roof and surface of each the stories, there were large amount of the contaminants such as pigeon′s excretions, dust and environmental elements for a long time. The pH of contaminants is not acid, but is 7.2, neutral. To find the species of organic acidscontained in the contaminants and the degree of damaging for a marble pagoda, we analyzed the contaminants using GC-MSD method by the following procedures. Organic acids were extracted by saponifying whole contaminants. After Saponification, the organic acids were mathylated to increase their volatility upon subsequent GC-MSD analysis. The mathyl esters of the organic acids are extracted from the acidified aqueous solution. And the organic extracts were washed with adilute base solution. The washed extract were analyzed by GC(Hewlett Packard 5890)with a nonpolar capillary column(Crosslinked 5% Ph Me Silicone, $50×0.2㎜×0.33\mum$film thickness, USA) and Mass Spectrometric Detector(Hewlett Packard 5970B).As the result, it was found that 12 organic acids were the main compound in pagoda′contaminants, and the amount of organic acid were negligible.

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Characterization of Low Molecular Weight Polyphenols from Pine (Pinus radiata) Bark

  • Mun, Sung-Phil;Ku, Chang-Sub
    • Food Science and Biotechnology
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    • v.15 no.3
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    • pp.424-430
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    • 2006
  • Low molecular weight polyphenols were isolated from hot water extracts of radiata pine (Pinus radiata) bark using a Sephadex LH-20 column and characterized by $^1H$ and $^{13}C$ NMR, UV, FT-IR, and GC-MS analyses. Major compounds isolated and identified were protocatechuic acid, trans-taxifolin, and quercetin. Trans-taxifolin, an important intermediate in biosynthetic route of proanthocyanidin (PA), was isolated in large quantities and indicates that PA is a major component of radiata pine bark. Small amounts of polyphenols were identified by GC-MS analysis. The presence of p-hydroxybenzoic acid, vanillic acid, protocatechuic acid, cis- and trans-feruic acid, p-coumaric acid, trans-caffeic acid, (-)-epicatechin, (+)-catechin, trans- and cis-taxifolin, (+)-gallocatechin, and quercetin was confirmed by comparison of mass fragmentation patterns and retention times (RT) with authentic samples. In addition, the presence of astringenin, astringenin glycoside, trans- and cis-leucodelphinidin was strongly assumed from characteristic mass fragment ions due to their conjugated structure and retro Diels-Alder reaction, and also from biosynthetic route of PA. GC-MS analysis allowed us to detect small amounts of phenolic acids and flavonoids and eventually discriminate trans- and cis-configuration in the identified polyphenols.

Identification of Benzidine Metabolites in Rats by Gas Chromatography/Mass Selective Detector and its Toxicity in vitro (Gas-Chromatography/Mass Selective Detector를 사용하여 쥐의 뇨시료 중 benzidine 대사체의 확인 및 in vitro 독성)

  • 류재천;권오승
    • YAKHAK HOEJI
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    • v.44 no.5
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    • pp.384-390
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    • 2000
  • Metabolism study of the dye, benzidine, was performed by gas chromatography-mass selective detector (GC/MSD) in the urine of rats orally administered 100 mg/kg benzidine. Urine samples were collected in metabolic cages for 0-24, 24-48, and 48-72 hrs. Ten ml of the urine was extracted with XAD-2 resin and the XAD-2 column was eluted with methanol. After evaporation, benzidine and its metabolites were extracted with diethyl ether (for non-conjugated fraction). For conjugated metabolites, $\beta$-glucu-ronidase was added to the aqueous layer that was incubated for 1 hr at 5$0^{\circ}C$ and the aqueous layer was extracted as in non-conjugated fraction. Aliquot of trimethylsilylated derivatives was applied to the GC/MSD. The mutagenicity of benzidine and its acetylated metabolites was tested by histidine/reversion assay. Five metabolites observed and confirmed either by electron impact and chemical ionization modes of the GC/MSD, or authentic compounds were monoacetyl-, diacetyl-, hydroxyacetyl-, hydroxydiacetyl-, and hydroxy-benzidine. Monoacetyl-benzidine was more potent than benzidine in histidine/reversion assay. This data indicates that monoacetylation of benzidine may be one of the metabolites produced in metabolic activation process.

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A Study on the Pollution of Polycyclic Aromatic Hydrocarbons (PAHs) In the Column Sediments around Gwangyang Bay (광양만 주변해역 주상퇴적물에서의 다환방향족탄화수소류(PAHs)의 오염에 관한 연구)

  • You, Young-Seck;Cho, Chon-Rae;Cho, Hyeon-Seo
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.14 no.4
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    • pp.257-266
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    • 2008
  • PAHs are of mainly anthropogenic origin from urban runoff, oil spill and combustion of fossil fuels. Some PAHs are potentially carcinogenic and mutagenic to aquatic organisms. This study was carried out to survey the contamination of PAHs in the column sediments around Gwangyang bay. Yeosu petrochemical industrial complex, POSCO(Pohang steel compony) and Gwangyang container harbor are located near the bay. The column sediments were collected at 4 stations(A, B, C and D) and fractionated at intervals of two-centimeter depth on July 29, 1999. PAHs in colmn sediment samples were extracted in soxhlet extractor and were identified and quantified by GC-MS. PAHs compounds were analyzed and found to be 13 species. Total PAHs concentrations in the column sediments ranged from 275.04 to 2,838.64${\mu}g/kg$ dry wt. Naphthalene had the highest concentration in the range of 40.60 to 2,294.06${\mu}g/kg$ dry wt. and Anthracene had the lowest concentration in the range of 2.63 to 11.30${\mu}g/kg$ dry wt. The correlation coefficients between individual PAHs and total PAHs in the column sediments were relatively higher in the low molecular compounds such as Naphthalene, Acenaphthylene and Phenanthrene. The relationship between the P/A(Phenanthrene/Anthracene)ratio and F/P(Fluoranthene/Pyrene)ratio showed that P/A ratio was generally above 10 and F/P ratio was above 1 in all sediment samples. These data indicate that PAHs in the column sediments around Gwangyang bay seem to be of both pyrolytic and petrogenic origin The values of PAHs in the column sediments were lower than the biological effect guidelines.

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Studies on Essential Oils of Plants of Angelica Genus in Korea (IV) -Essential Oils of Angelicae koreanae Radix- (Angelica속 생약의 정유성분에 관한 연구(IV) -강활의 정유성분-)

  • Chi, Hyung-Joon;Kim, Hyun-Soo
    • Korean Journal of Pharmacognosy
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    • v.24 no.2
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    • pp.111-115
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    • 1993
  • Essential oil of the root of Angelica koreana Max. (Umbelliferae) was investigated. Essential oil was obtained from the dried roots by steam distillation and fractionated by column chromatography. Each isolate or fraction was identified by GC, GC-MS and spectral analysis. It was found to contain nine monoterpenes such as ${\alpha}-pinene$(7.0%), camphene, ${\beta}-pinene$, myrcene, ${\alpha}-phellandrene$, ${\Delta}-3-carene$, p-cymene, limonene(2.8%), terpinolene and also found to contain m-cresol(11.6%), citronellol, citral b, methylcinnamate, eudesmol and osthol. 2-Hydroxy-5-methylacetophenone and twelve compounds were tentatively identified.

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Studies on Essential Oil of Plants of Angelica Genus in Korea(III) -Essential Oils of Angelicae dahuricae Radix- (Angelica속 생약의 정유성분에 관한 연구(III) -백지의 정유성분-)

  • Kim, Hyun-Soo;Chi, Hyung-Joon
    • Korean Journal of Pharmacognosy
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    • v.21 no.2
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    • pp.121-125
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    • 1990
  • Essential oil of the root of Angelica dahurica Benth et Hook(Umbelliferae) was investigated. Essential oil was obtained from the dried roots by steam distillation and fractionated by column chromatography. Each isolate or fraction was identified by GC, GC-MS and spectral analysis. It was found to contain eleven monoterpenes such as ${\alpha}-pinene(4.74%),\;campben, {\beta}-pinene,\;myrcene,\;{\alpha}-phellandrene,\;{\delta}-3-carene(39.4%),\;{\alpha}-terpinene,\;{\rho}-cymene,\;{\beta}-phellandrene,\;{\alpha}-terpinene,\;terpinolene\;and\;also\;found\;to\;contain\;4-vinylguaiacol,\;iso-elemicin,\;{\beta}-elemene$, caryophyllene, ligustilide, osthol and seven tentatively identified sesquiterpenes.

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Studies on Essential Oils of Plants of Angelica Genus in Korea (I). -Essential Oils of Angelicae gigantis Radix- (Angelica속 생약의 정유성분에 관한 연구 (I). -참당귀의 정유성분-)

  • Chi, Hyung-Joon;Kim, Hyun-Soo
    • Korean Journal of Pharmacognosy
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    • v.19 no.4
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    • pp.239-247
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    • 1988
  • Essential oil of the root of Angelica gigas Nakai (Umbelliferae) was investigated. Essential oil was obtained from the dried roots by steam distillation and fractionated by column chromatography. Each isolate or fraction was identified by GC, GC-MS and spectral analysis. It was found to contain eleven monoterpenes such as ${\alpha}-pinene,\;camphene,\;{\beta}-pinene,\;myrcene,\;{\alpha}-phellandrene,\;{\Delta}-3-carene,\;{\alpha}-terpinene,\;p-symene,\;limonene,\;{\gamma}-terpinene$ and terpinolene and also found to contain 4-vinylguauacol, myristicin, elemol, ${\beta}-eudesmol,\;{\alpha}-eudesmol,\;four\;sesquiterpenes\;involving\;{\Delta}-elemene$. Four sesquiterpenes and five sesquiterpene alcohols were tentatively identified by comparison of their mass spectra.

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Analysis of Radiolytically Proudced Hydrocarbons and 2-Alkylcyclobutanones from Irradiated Pinenut (방사선 조사된 잣으로부터 조사 여부를 확인하기 위한 Hydrocarbon류와 2-Alkylcyclobutanone류의 분석)

  • 이해정;김경수
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.30 no.1
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    • pp.37-42
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    • 2001
  • Pinenut was irradiated with the dose of 0.5∼10 kGy. Radiation-induced hydrocarbons and 2-alkylcyclobutanones were extracted from pinenut, separated by florisil column chromatography and identified with GC/MS method. Concentrations of hydrocarbons and 2-alkylcyclobutanones were increased with the increase of irradiation dose and the composition of patty acids in pinenut affected on products detects. The major hydrocarbons in irradiated pinenut were 8-heptadecene and 1,7-hexadecadiene originated ferom oleic acid and 6,9-heptadecadiene and 1, 7, 10-hexadecatriene originated from linoleic acid. 2-(5'-Tetradecenyl) cyclobutanone originated from oleic acid was highest in the irradiated pinenut. Radiation-induced hydrocarbons hydrocarbons and 2-alkylcyclobutanones in pinenut were detected at 0.5 kGy and over, but not detected in the unirradiated samples.

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Sorbent Thermal Desorption/Gas Chromatography/Mass Selective Detection Method for Determination of Gaseous Polycyclic Aromatic Hydrocarbons in Indoor Air

  • Dai, Shugui;Zhang, Lin;Zhu, Tan
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.753-758
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    • 1995
  • Thermal desorption/gas chromatography/mass selective detection method using Tenax cartridges for the determination of gaseous polycyclic aromatic hydrocarbons(PAH) is described. Glass fiber filter can collect only PAH in particulate. Gaseous PAH may penetrate the filter. Glass cartridge packed Tenax-GC was uses fur adsorption of gaseous PAH. The air of inhalation zone was collected fur 2-10 hours. Cartridges were thermally desorbed in the reverse direction to sample flow. The desorption conditions were as follows; desorption temperature; $300^{\circ}C$; desorption time; 20min; column head pressure; 30psi; inlet split vent; closed during desorption.

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