• Title/Summary/Keyword: gas chromatography/mass spectrometry identification

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Determination of Trichlorfon Pesticide Residues in Milk via Gas Chromatography with μ-Electron Capture Detection and GC-MS

  • Hem, Lina;Khay, Sathya;Choi, Jeong-Heui;Morgan, E.D.;El-Aty, A.M. Abd;Shim, Jae-Han
    • Toxicological Research
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    • v.26 no.2
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    • pp.149-155
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    • 2010
  • The pesticide trichlorfon is readily degraded under experimental conditions to dichlorvos. A method has therefore been developed by which residues of trichlorfon in milk are determined as dichlorvos, using gas chromatography with ${\mu}$-electron capture detection. The identification of dichlorvos was confirmed by mass spectrometry. Milk was extracted with acetonitrile followed by centrifugation, freezing lipid filtration, and partitioning into dichloromethane. The residue after partitioning of dichloromethane was dissolved in ethyl acetate for gas chromatography. Recovery concentration was determined at 0.5, 1.0, and 2.0 of times the maximum permitted residue limits (MRLs) for trichlorfon in milk. The average recoveries (n = 6) ranged from 92.4 to 103.6%. The repeatability of the measurements was expressed as relative standard deviations (RSDs) ranging from 3.6%, to 6.7%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.7 and $11.1{\mu}g/l$, respectively. The accuracy and precision (expressed as RSD) were estimated at concentrations from 25 to $250{\mu}g/l$. The intra- and inter-day accuracy (n = 6) ranged from 89.2% to 91% and 91.3% to 96.3%, respectively. The intra- and inter-day precisions were lower than 8%. The developed method was applied to determine trichlorfon in real samples collected from the seven major cities in the Republic of Korea. No residual trichlorfon was detected in any samples.

Screening and identification of bioorganic light-emitting substances from marine macrophytes

  • Jung, Sang Mok;Lee, Han Seong;Lee, Han Joo;Kang, Seul Gi;Son, Ji Su;Jeon, Jae Hyuk;Chae, Hee Baik;Shin, Hyun Woung
    • ALGAE
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    • v.30 no.2
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    • pp.171-179
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    • 2015
  • Organic light-emitting materials in marine macrophytes from various coastal environments were identified. Twentyeight species from the solvent fractions were examined and identified as candidates for bioorganic light-emitting materials using photoluminescence (PL) spectra and gas chromatography-mass spectrometry. We selected 16 solvent fractions from a total of 1,221 prepared from Ishige okamurae, Sargassum confusum, Grateloupia elliptica, Chondracanthus intermedius, Porphyra yezoensis, Meristotheca papulosa, Gelidium amansii, and Scytosiphon lomentaria. The maximum light-emitting PL spectra appeared at various colors, mainly between blue and green, based on chromaticity coordinates, from solvent fractions of M. papulosa, G. amansii, G. elliptica, P. yezoensis, S. lomentaria, I. okamurae, and C. intermedius. These results will contribute to the development of novel organic light-emitting materials.

Flavor Components of Artemisia Lavandulaefolia DC (참쑥(Artemisia Lavandulaefolia DC)의 방향성분)

  • Choi, Kyoung-Sook;Choi, Bong-Young;Park, Hyoung-Kook;Kim, Jung-Han;Park, Jong-Sei;Yoon, Chang-No
    • Korean Journal of Food Science and Technology
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    • v.20 no.6
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    • pp.774-779
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    • 1988
  • The essential oil of Artemiisa lavandulaefolia DC was analyzed by gas chromatography/mass spectrometry (GC/MS). The oil was stored at different conditions for 6 weeks and the changes of color and chemical composition during storage were checked by GC/MS. The experimental results were as follows; (1) More than 186 chemicals were detected by GC. Major components were 1,8-cineol, thujone, camphor, borneol, coumarin, 2,3-dihydrobenzofuran and ${\beta}-biasbolene$. In this study, 3,3,6-trimethyl norpinanol, ${\beta}-farnesene,\;{\alpha}-curmene$ and 7-methoxy coumarin were detected as new compounds in Artemisia species. (2) It was proved that temperature and/ or light had and important effect on the changes of color and volatile components of the essential oil. The relative amounts of limonene and 1.8-cineol were decreasad, on the other hand, ${\beta}-phellandrene\;and\;{\alpha}-terpineol$ were increased during storage.

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Identification of New Urinary Metabolites of Byakangelicin, a Component of Angelicae dahuricae Radix, in Rats

  • Kwon, Oh-Seung;Song, Yun-Seon;Shin, Kuk-Hyun;Ryu, Jae-Chun
    • Archives of Pharmacal Research
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    • v.26 no.8
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    • pp.606-611
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    • 2003
  • Byakangelicin, 9-(2,3-dihydroxy-2-methylbutoxy)-4-methoxy-7H- furo[3,2-g][l]benzopyran-7-one (BKG), a component of Angelicae dahuricae Radix, is considered to be an inhibitor of aldose reductase for the treatment of diabetic cataract. An analytical method for the isolation of BKG developed by high-performance liquid chromatography has been reported. No literature on the metabolism of BKG, however, has been found. With the purpose of identifying new metabolites of BKG, BKG (100 mg/kg) was orally administered to Sprague-Dawley rats via a gavage. Using a metabolic cage, urine was collected for 24 h, and the urine samples were extracted by liquid-liquid extraction. For structural identification of new urinary metabolites of BKG, various instrumental analyses were conducted by gas-chromatography/mass spectrometry, high-performance liquid chromatography/diode array detector, liquid chromatography/mass spectroscopy with thermospray interface and $^1H$ nuclear magnetic resonance spectroscopy. Two metabolites produced from the Ο-demethylation or Ο-dealkylation of BKG were newly identified, and another new but unknown metabolite was assumed to be the hydroxylated form of BKG. These results indicate that the major metabolic products of BKG are formed by Ο-demethylation or Ο-dealkylation of BKG side chains.

A Study on the Identification of Phenol Production by GC/MS under Chemical Treatment of Industrial Wastewater (화학적 폐수처리 중 GC/MS에 의한 폐놀생성 규명에 관한 연구)

  • 박선구;고오석;신대윤
    • Journal of Environmental Science International
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    • v.9 no.1
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    • pp.89-93
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    • 2000
  • Twenty organic chemical substances(Table 2) were isolated from untreated wastewater, as well as treated wastewater, collected at 76 companys of 9 industry group located in the basin of Youngsan River. Those organic compounds were analyzed by Gas Chromatography/Mass Spectrometry(GC/MS) and confirmed through comparison with each standard reagents. Phenol, which was not detected in the raw wastewater, was identified in the effluent of treatment facility, indicating that phenol is generated from isopropylbenzene of plant wastewater.

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Formation of Polychlorinated Dibenzo-p-Dioxins and Their Thermal Decomposition Products from Pyrolysis Reactions of Chlorophenates

  • Hong, Jongki;Park, Jongsei;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.821-827
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    • 1995
  • Polychlorodibenzo-p-dioxins(PCDDs) have been prepared by microsacale pyrolysis of trichlorophenates. During the pyrolysis reaction, dechlorinated dibenzo-p-dioxins were also formed by the thermolysis of PCDDs. The dechlorination pathways of PCDDs were suggested in this reaction. The identification of these products was performed using capillary column gas chromatography-mass spectrometry.

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Formation of Tetra-Chlorinated Dibenzo-p-dioxins and Their Thermal Decomposition Products from Pyrolysis Reaction of Tri-Chlorophenates

  • 홍종기;박종세;김강진
    • Bulletin of the Korean Chemical Society
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    • v.17 no.4
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    • pp.334-338
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    • 1996
  • Tetra-chlorodibenzo-p-dioxins (tetra-CDDs) were prepared by microscale pyrolysis of trichlorophenates. During the pyrolysis reaction, tri-, di-, and mono-CDDs were also formed by the thermolysis of tetra-CDDs. The dechlorination pathways of tetra-CDDs were suggested for this reaction. The identification of these products was performed with capillary column gas chromatography-mass spectrometry.

Discovery of Urinary Biomarkers in Patients with Breast Cancer Based on Metabolomics

  • Lee, Jeongae;Woo, Han Min;Kong, Gu;Nam, Seok Jin;Chung, Bong Chul
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.59-66
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    • 2013
  • A metabolomics study was conducted to identify urinary biomarkers for breast cancer, using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS), analyzed by principal components analysis (PCA) as well as a partial least squares-discriminant analysis (PLS-DA) for a metabolic pattern analysis. To find potential biomarkers, urine samples were collected from before- and after-mastectomy of breast cancer patients and healthy controls. Androgens, corticoids, estrogens, nucleosides, and polyols were quantitatively measured and urinary metabolic profiles were constructed through PCA and PLS-DA. The possible biomarkers were discriminated from quantified targeted metabolites with a metabolic pattern analysis and subsequent screening. We identified two biomarkers for breast cancer in urine, ${\beta}$-cortol and 5-methyl-2-deoxycytidine, which were categorized at significant levels in a student t-test (p-value < 0.05). The concentrations of these metabolites in breast cancer patients significantly increased relative to those of controls and patients after mastectomy. Biomarkers identified in this study were highly related to metabolites causing oxidative DNA damage in the endogenous metabolism. These biomarkers are not only useful for diagnostics and patient stratification but can be mapped on a biochemical chart to identify the corresponding enzyme for target identification via metabolomics.

Identification of 4-Demethylsterols from Suspension Cultured Cells of Marchantia polymorpha L. (Marchantia polymopha(우산이끼) 현택배양 세포내으 4-methylster이들의 동정)

  • Seong-Ki Kim
    • Journal of Plant Biology
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    • v.38 no.3
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    • pp.219-225
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    • 1995
  • Five kinds of 4-demethylsterol were isolated from suspension cultured cells of a liverworth, Marchantia polymorpha. Four 4-demethylsterols among them were analyzed by a capillary gas chromatography-massspectrometry and 500 MHz 1H-NMR, and characterized to be avenasterol, 24-methylene-cholesterol, stigmasterol, and campesterol. And the fifth 4-demethylsterol was characterized to be sitosterol by a capillary gas chromatography-mass spectrometry. The concentration of the 4-demethylsterols in the cell decreased in order of avenasterol>stigmasterol>24-methylene-cholesterol>campesterol>sitosterol. When carbon skeleton and the oxidation state was compared with those of brassinosteroids, these 4-demethylsterols may be potent biosynthetic procusors of brassinosteroids in the cells.

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Analysis of Death Due to Poisoning in the National Capital Region (2014-2016) (수도권 부검시료에서 중독사 관련 사용물질 현황(2014-2016))

  • Park, Meejung;Park, Jongsin;Lee, Sangki;In, Sangwhan
    • Journal of The Korean Society of Clinical Toxicology
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    • v.15 no.2
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    • pp.101-106
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    • 2017
  • Purpose: This study examined the patterns of drugs, poisons, and chemicals detected in autopsy samples performed in the Seoul Institute and other regional forensic offices of the National Forensic Service (NFS) between 2014 and 2016. Methods: The investigation carried out using the laboratory information management system. Forensic toxicological identification and quantitation were performed in autopsy samples, including heart blood, peripheral blood, liver, kidney, vitreous humor and etc. Gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) were used to analyze the drugs and poisons. Results: Forensic autopsies were performed on 9,674 cases in this period. Based on the autopsy reports, 699 cases (7.2%) were considered as unnatural deaths caused by fatal intoxication. The number of male deaths was higher than that of female deaths, with the age of 50-59 being the most common age group. Conclusion: Drugs comprised the largest number of deaths due to poison, followed by alcohol, agrochemicals, drug with alcohol, carbon monoxide, and cyanide, in that order. Zolpidem was the most frequently used drug in all drug-related intoxication cases.