• Title/Summary/Keyword: GC-MS (SIM)

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The analysis of ethylene glycol and metabolites in biological specimens (생체시료에서 에틸렌 글리콜과 그 대사체 분석에 관한 연구)

  • Park, Seh-Youn;Kim, Yu-Na;Kim, Nam-Yee
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.69-77
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    • 2011
  • Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

Quantitative Analysis of The Fruit Flesh of Prunus mume Siebold & Zuccarni. (매실 과육성분의 분석)

  • Lee, Oh-Kyu;Lee, Hak-Ju;Shin, Yu-Su;Ahn, Yun-Gyong;Jo, Hyun-Jin;Shin, Hyeon-Cheol;Kang, Ha-Young
    • Korean Journal of Medicinal Crop Science
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    • v.15 no.3
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    • pp.143-147
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    • 2007
  • The fruit flesh of four Prunus mume cultivated varieties, P. mume 'Nanko', P. mume 'Viridicalyx', P. mume 'Baigo', P. mume var, microcarpa 'Koshusaisho' Siebold & Zuccarni, were ground and extracted with ethyl acetate and their chemical components were analyzed by GC/MS-SIM. In the ten compounds which was used fer the calibration, maleic anhydride, citraconic anhydride, 5-hydroxymethylfurfural, vanillin, linoleic acid, ethyl linoleate, and squalene were determined in all the four cultivated varieties. However, palmitic acid was detected only in P. mume var. microcarpa 'Koshusaisho'. Isopropyl palmitate was found only in P. mume 'Baigo' and var, microcarpa 'Koshusaisho', while stearic acid was determined in P. mume 'Nanko', 'Viridicalyx', and var, microcarpa 'Koshusaisho'. In the variation of quantities, maleic anhydride was contained 245.4, 153.6, 20.1, and 2.7 ppm in P. mume 'Baigo', 'Nanko', var. microcarpa 'Koshusaisho', and 'Viridicalyx', respectively. Citraconic anhydride was also contained 637.4, 543.1, 150.7, and 38.7 ppm in P. mume 'Baigo', 'Nanko', var. microcarpa 'Koshusaisho', and 'Viridicalyx', respectively. The amounts of stearic acid were 105.5, 64.4, and 32.3 ppm in P. mume var. microcarpa 'Koshusaisho', 'Viridicalyx', and 'Nanko', respectively. Squalene was found in amounts of 7.6, 1.7, 1.0, and 0.5 ppm in P. mume var. microcarpa 'Koshusaisho', 'Baigo', 'Nanko', and 'Viridicalyx', respectively. The amounts of other minor compounds also were varied in the P. mume cultivated varieties.

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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A Study on the Pollution of Polycyclic Aromatic Hydrocarbons(PAHs) in the Surface Sediments Around Gwangyang Bay (광양만 주변해역 표층퇴적물에서의 다환방향족탄화수소류(PAHs)의 오염에 관한 연구)

  • You, Young-Seok;Choi, Young-Chan;Cho, Hyeon-Seo
    • Journal of the Korean Society of Marine Environment & Safety
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    • v.13 no.1 s.28
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    • pp.9-20
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    • 2007
  • PAHs(Polycyclic Aromatic Hydrocarbons) are widespread contaminants in the marine environment. They are of mainly anthropogenic origin from urban runoff, oil spill and combustion of fossil fuels. Some PAHs are potentially carcinogenic and mutagenic to aquatic organism The contamination of PAHs in the coastal environments has not been well known yet in Korea. This study was carried out to survey the contamination of PAHs in sediments around Gwangyang bay. The Yeosu petrochemical industrial complex, POSCO(Pohang steel company) and Gwangyang container harbor are located around the bay. PAHs in sediment samples were extracted in soxhlet extractor and were identified and quantified by GC-MS(Gas Chromatography-Mass Spectrometry) TOC(Total Organic carbon) and textural parameters in sediment samples were also analyzed 13 species of PAHs were detected at all of the surface sediments. Total PAHs concentrations in the surface sediments ranged from 171.40 to $1013.54{\mu}g/kg$ dry wt.. In most of the surface sediments, Naphthalene was the highest in the range of 14.08 to $691.39{\mu}g/kg$ dry wt. and Anthracene was the lowest in the range of 0.49 to $22.66{\mu}g/kg$ dry wt.. The correlation coefficients between individual PAHs and Total PAHs in the surface sediments were relatively higher in the low molecular compounds such as Naphthalene and Phenanthrene. In the relationship of the P/A(Phenanthrene/Anthracene) ratio and F/P(Fluoranthene/Pyrene) ratio, P/A ratio was generally above 10 and F/P ratio was shown to be above 1 in all sediment samples. These data indicate that PAHs in sediments around Gwangyang bay seem to be of both pyrolytic and petrogenic origin. Total PAHs in the surface sediments were correlated with TOC and textural parameters. The values of PAHs in the surface and core sediments were lower than the biological effect guidelines.

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Bioequivalence of Bucilin Tablet to Rimatil Tablet (Bucillamine 100 mg) (리마틸 정(부시라민 100 mg)에 대한 부시린 정의 생물학적 동등성)

  • Cho, Hea-Young;Lee, Moon-Seok;Oh, In-Joon;Kim, Dong-Hyun;Moon, Jai-Dong;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.31 no.2
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    • pp.125-130
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    • 2001
  • Bucillamine is a novel cysteine derivative with two free intramolecular sulfhydryl groups, and has a preventive and therapeutic effect on adjuvant arthritis, suggesting its antirheumatic action. With respect to the effect on the immune system, bucillamine-exerted such immunoregulating actions are to nomalize an excessive reduction or acceleration in immune reaction. It is useful not only in patients with early stage of rheumatoid arthritis (RA) but also in those with active RA retained for more than 10 years. The purpose of the present study was to evaluate the bioequivalence of two bucillamine tablets, $Rimatil^{TM}$ (Chong Kun Dang Pharmaceutical Co., Ltd.) and $Bucilin^{TM}$ (Kuhn Il Pharmaceutical Co., Ltd.), according to the guidelines of Korea Food and Drug Administration (KFDA). Eighteen normal male volunteers, $23.67{\pm}2.09$ years in age and $65.03{\pm}6.73\;kg$ in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After three tablets containing 100 mg of bucillamine per tablet were orally administered, blood was taken at predetermined time intervals and the concentrations of bucillamine in serum were determined using GC/MS with mass selective detector. Pharmacokinetic parameters such as $AUC_t$, $C_{max}\;and\;T_{max}$ were calculated and ANOVA test was utilized for the statistical analysis of the parameters. The results showed that the differences in $AUC_t$, $C_{max}\;and\;T_{max}$ between two tablets were -0.29%, -3.20% and 8.22%, respectively, when calculated against the $Rimatil^{TM}$ tablet. The powers $(1-{\beta})$ for $AUC_t\;and\;C_{max}$ were 84.31 % and 91.16%, respectively. Minimum detectable differences $({\Delta})$ at ${\alpha}=0.10$ and $1-{\beta}=0.8$ were less than 20% (e.g., 18.58% and 16.51% for $AUC_t\;and\;C_{max}$, respectively). The 90% confidence intervals were within ${\pm}20%$ (e.g.,$-12.77{\sim}12.20$ for $AUC_t$ and $-14.30{\sim}7.90$ for $C_{max}$). Two parameters met the criteria of KFDA for bioequivalence, indicating that $Bucilin^{TM}$ tablet is bioequivalent to $Rimatil^{TM}$ tablet.

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Plant Growth Promotion Activity of Endophytic Fungi Isolated from the Roots of Calystegia soldanella (갯메꽃 뿌리로부터 분리된 내생진균의 식물생장촉진활성)

  • You, Young-Hyun;Yoon, Hyeok-Jun;Woo, Ju-Ri;Seo, Yeong-Gyo;Shin, Jae-Ho;Choo, Yeon-Sik;Lee, In-Jung;Kim, Jong-Guk
    • Microbiology and Biotechnology Letters
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    • v.39 no.4
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    • pp.324-329
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    • 2011
  • Eight endophytic fungal strains were isolated from the roots of Calystegia soldanella from the western coast of South Korea. The culture filtrate of the eight endophytic fungi were applied to waito-c rice seedlings in order to verify potential plant growth promotion activities. The results of bioassay indicated that the Cs-9-7 fungal strain possessed the highest plant growth promotion activity. Fungal culture filtrates were analyzed to verify secondary metabolites using gas chromatography and mass spectroscopy with selected ion monitoring (GC/MS-SIM). The culture filtrate of the Cs-9-7 fungal strain was confirmed to contain gibberellins GA3 (1.229 ng/mL), GA4 (3.535 ng/mL), GA7 (1.408 ng/mL) and GA12 (0.378 ng/mL). Polymerase chain reactions (PCR) were performed so as to determine the internal transcribed spacer (ITS) regions for the identification of isolated strains with universal primers ITS-1 and ITS-4. The Cs-9-7 fungal strain, isolated from the root of C. soldanella, has been named Aspergillus tubingensis Cs-9-7.

Characteristics of Bacterial-Koji and Doenjang(soybean paste) Made by using Bacillus subtilis DJI (Bacillus subtilis DJI을 이용하여 제조된 세균형 코지와 속성된장의 특성)

  • Chang, Mi;Chang, Rae-Choon
    • Microbiology and Biotechnology Letters
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    • v.35 no.4
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    • pp.325-333
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    • 2007
  • One bacterium with high proteinase production and spore-forming ability was isolated from korean traditional soybean paste(doenjang). The isolated strain was identified as Bacillus subtilis, based on gram-staining, biochemical properties and l6S rRNA gene sequencing, and designated as B. subtilis DJI. Its growth rate was very fast, and it reached its stationary phase within 9 h, and then started to form spores. Bacterial-koji and doenjang were prepared using B. subtilis DJI. Chemical components of the doenjang were determined after 2 months of aging period: amino nitrogen 507 mg%, crude protein 14.3%, crude fat 4.8% and water 54.9%. The composition of total and free amino acids and their ratios of doenjang were changed during the aging period. Among total amino acids in DJI doenjang, glutamic acid, aspartic acid, leucine and arginine were the major amino acids. The fibrinolytic activities of DJI doenjang and traditional doenjangs were 909.7 units/ml and $363.3{\sim}618.6\;units/ml$, respectively. Flavor compounds of DJI doenjang and traditional doenjang were extracted by SDE(simultaneous steam distillation and extraction), and analyzed by GC/MS; DJI doenjang possessed the typically favorable flavor compounds in traditional korean doenjang, with reduced off-flavor compounds.

Plant growth-promoting activity and identification of endophytic fungi isolated from native plant in East coast (동해안 자생식물로부터 분리된 내생균류의 식물생장촉진활성 및 동정)

  • You, Young-Hyun;Jin, Yong Ju;Kang, Sang-Mo;Oh, Sejong;Lee, Myung-Chul;Kim, Jong-Guk
    • Korean Journal of Microbiology
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    • v.51 no.1
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    • pp.14-20
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    • 2015
  • Coastal plant species, Plantago camtschatica Cham. native to the coastal region of the East Sea were sampled and then morphologically different 20 endophytic fungal strains were purely isolated. Phylogenetic analysis of isolates was done by the Bayesian program based on sequenced internal transcribed spacer (ITS-rDNA) region. Culture filtrates of each of 20 isolates were treated to Waito-c rice (WR) seedlings for verifying plant growth-promoting activity, respectively. As the results, E/PC/10/1 strain showed the highest plant growth-promoting activity among them. The culture filtrate of the strain E/PC/10/1 was revealed as containing gibberellins ($GA_1$, $GA_3$, $GA_4$) by using HPLC, and gas GC/MS with selected ion monitoring (SIM). Finally, this strain was identified as novel Penicillium spinulosum species that producing new GAs with microscopic observation and further molecular analysis with beta-tubulin gene sequence.

Effect of Deodorizing Conditions on Formation of trans-Fatty Acids of Soybean Oil (대두유의 탈취과정에서 생성되는 trans 지방산의 정량)

  • Park, Choul-Soo;Yoon, Kwang-Ro
    • Korean Journal of Food Science and Technology
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    • v.30 no.1
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    • pp.6-12
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    • 1998
  • Degummed and bleached soybean oil was deodorized at a temperature range of $220{\sim}280^{\circ}C$ under the vacuum (4-5 torr) for 1 or 2 hrs. Gas chromatography with SP-2560 100 m capillary column was used to separate and quantitate fatty acid methyl esters and their isomers. Fatty acids were identified by comparing retention time with standards and GC-MS spectrum. The isomers of linoleic acid and linolenic acid in deodorized soybean oils were identified to be $C_{18:2}\;{\Delta}9-cis,\;{\Delta}12-trans,\;C_{18:2}\;{\Delta}9-trans,\;{\Delta}12-cis,\;C_{18:2}\;{\Delta}9-cis,\;{\Delta}12-cis,\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-cis,\;{\Delta}15-trans,\;C_{18:3}\;{\Delta}9-trans,\;{\Delta}12-cis,\;{\Delta}15-cis,\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-trans,\;{\Delta}15-cis,\;and\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-cis,\;{\Delta}15-cis$. The formation of trans-fatty acids by deodorization at $240{\sim}280^{\circ}C$ for 2 hrs was in the range of 1.78 to 5.74%. Conclusively, the deodorizing conditions of $240^{\circ}C$ for 2 hrs or $250^{\circ}C$ for 1 hr were suggested as the best conditions which could minimize the formation of trans isomers of fatty acids in soybean oils.

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Determination of ethyl carbamate in maesil wine by alcohol content and ratio of maesil (Prunus mume) during ripening period (알코올 농도 및 담금비에 따른 숙성 기간별 매실주의 에틸카바메이트 함량조사)

  • Kim, Nan-Young;Eom, Mi-Na;Do, Young-Sook;Kim, Jung-Beom;Kang, Suk-Ho;Yoon, Mi-Hye;Lee, Jong-Bok
    • Food Science and Preservation
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    • v.20 no.3
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    • pp.429-434
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    • 2013
  • This study was designed to investigate the formation of ethyl carbamate (EC) during the ripening of Maesil with sugar and Soju (19.5~35% alcohol contents) using a homemade method. Maesil, sugar and Soju were purchased at ordinary market in June of 2012. The preparation of sample for analysis was conducted by method of Henry et al. The analysis of GC/MS was used SIM mode (m/z 89, 74, 62). Quantification was performed in terms of the 62 ion and was based on an internal standard procedure. Good linearity was obtained with a regression coefficient ($r^2$ = 0.993). Low detection limits (LOD) was achieved 4.31 ug/kg and recovery for alcohol was 74.8%. During 90 days, fermentation with sugar was not detected EC (under LOQ). 15 days ripened Maesil wine contained EC between non detected~32.7 ug/kg and 90 days ripened Maesil wine was 19.7~87.4 ug/kg. Higher proportion of Maesil and Soju increased EC contents. EC levels were increased 32.7 ug/kg to 87.4 ug/kg in the ratio of Maesil to 35% alcohol-Soju (1:1). In the ratio of Maesil to 35% alcohol-Soju (1:3) was increased non detected to 69.7 ug/kg. After 90 days, Maesil wine was filtered Maesil through a seive and ripened by 180 days to investigate the formation of EC compared with non filtered. Treatment of filtered, EC contents was much higher level compared with non filtered. Therefore, this result showed that alcohol contents contribute to increase EC formation more than Maesil.