• Title/Summary/Keyword: Gas chromatography-mass spectrometry (GC/MS)

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Study of Pyrolysis Pattern and Transfer Rate of Organochlorine Pesticide in Tobacco

  • Min, Hye-Jeong;Jang, Seok-Su;Kim, Ick-Joong;Kim, Yong-Ha;Min, Young-Keun
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.118-124
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    • 2007
  • GRLs(Guidance Residue Levels) of agricultural chemicals for tobacco are recommended by the CORESTA Agro-Chemical Advisory Committee guide. In the GRLs list, organochlorine group is one of pesticides commonly used on tobacco cultivation. In this model study, the quantitative correlation in the transfer rate of pesticide residue into tobacco smoke by spiking of organochlorine pesticides to cigarette and pyrolysates were investigated. The spiking concentration referred to the range of GRLs list and the organochlorine pesticides in mainstream smoke were analyzed by GC-MS. For the understanding of the composition variation versus temperature, the behavior of pesticides was investigated by pyrolysis-gas chromatography-mass spectrometry(Py-GC-MS). In this study, the transfer rate of pesticide residue into tobacco smoke at four different spiking concentration and the composition of pyrolysates were analyzed differently. At $10\;{\mu}g/cig$ spiking concentrations, the organochlorine pesticides were transferred into tobacco smoke in $0.02\;{\sim}\;10.19\;%$ each of component and the most of pesticides were pyrolyzed during smoking. It was found that the decomposition compounds from organochlorine pesticides were mainly composed of oxygenated and nitrogenous compounds. This study could estimate that the transfer rate of pesticides into tobacco smoke is very small amount.

A Study on 10 Metabolites Separated from DNA Adduce of Blood Lymphocytes in Rats Exposed Orally with 3,3-dichlorobenzidine(DCB) by GC/MS-SIM

  • Shin, Ueon-Sang;Lee, Jin-Heon
    • Journal of Environmental Health Sciences
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    • v.28 no.4
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    • pp.6-11
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    • 2002
  • 3.3'-Dichlorobenzidine(DCB) has be shown carcinogenic in several animals, and the development of non-invasive biomonitoring method in workers exposed with it is a very important subject. DNA adduct is a good biomarker for biomonitoring about carcinogens exposure, and lymphocytes is a good non-invasive samples. So we studied to analyze metabolites in blood lymphocytes of female Sprague-Dawley rats exposed orally with DCB(20, 30, and 40 mg/kg wt.) for 3 weeks. For analysis of them, we isolated DNA adducts from blood lymphocytes by using the enzymes method in /sup 32/P-postlabeling, and measured them by using gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM). 4-aminobiphenyl and phenanthrene-d/sub 10/ were added as internal standard for blank sample. Standard metabolites of DCB were synthesized with using pyridine and acetic acid which were promoter and controller in acetylation of DCB. And they were used for calibration curve. Our results showed two kinds of metabolites in DNA adducts of blood lymphocytes. They were N-acetyl 3,3'-dichlorobenzidine(acDCB) and N,N'-diacetyl 3,3'-dichiorobenzidine(di-acDCB ). They were combined with DNA at the same time as an acetyl of it was removed. So we measured DCB and acDCB for two kinds of metabolites in DNA adducts of blood lymphocytes. Our results showed the levels of DCB were 1.46∼2.26 times more than that of acDCB. And also the levels of metabolites in 20, 30 and 40 mg/kg wt. were gradually increased with going days from 1st to 3rd week. They are 1.66, 1.38 and 0.90 times in total metabolites, 1.76, 1.49 and 1.02 times in DCB, and 1.51, 1.22 and 1.28 times in acDCB. In conclusion, the results of this study showed DCB exposed to rats formed DNA adduct in blood lymphocytes after acetylated to N-acetyl 3.3'-dichloro benzidine(acDCB) and N,N'-diacetyl 3,3'-dichlorobenzidine(di-acDCB), and they could be analyzed by us ing gas chromatography/mass spectrometry-selected ion monitoring(GC/MS-SIM).

Chemical Composition and Antifungal Activity of Plant Essential Oils against Malassezia furfur (비듬균(Malassezia furfur)에 대한 식물 오일들의 항균활성 및 활성오일의 성분 분석)

  • Lee, Jeong-Hyun;Lee, Jae-Sug
    • Microbiology and Biotechnology Letters
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    • v.38 no.3
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    • pp.315-321
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    • 2010
  • Malassezia furfur is an important causal factor for seborrheic dermatitis. Nowadays, the drugs available to treat this fungal infection are few. Several studies have documented the biological activity of essential oils. However, its antifungal properties are not completely understood, especially its anti-Malassezia activity. The aim of this study were to evaluate the effect of the plant essential oils on the growth of M. furfur using disk diffusion method and analyze by Gas chromatography-mass spectrometry (GC-MS) most active essential oils. In first screening, the 17 plant essential oils have possesses inhibitory activity against M. furfur at 2 mg/mL. Among the plant essential oils, oil of Citrus auranifoli was most active against M. furfur and its activity showed dose dependency. This anti-malassezial activity was high than that of itraconazole at 2 mg/mL. Oil of Citrus auranifolia also was phytochemically examined by GC-MS analysis, its main constituents were identified as limonene, ${\gamma}$-terpinene and terpinolene. It can be concluded that essential oils of Citrus auranifolia may have interesting applications to control fungal-derived diseases.

Volatile Flavor Components in Green Tea Blended with Parched Naked Barley (볶은 쌀보리를 혼합한 녹차의 휘발성 향기성분)

  • Choi, Sung-Hee
    • Journal of Life Science
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    • v.22 no.7
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    • pp.981-986
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    • 2012
  • To produce a new tea with a good flavor and functional properties using green tea of low quality, naked barley and barley were selected to blend with the green tea. The simultaneous distillation extraction method (SDE) using Likens and Nickerson's extraction apparatus was used to extract the volatile flavor compounds from the samples. The concentrated flavor extracts were analyzed and identified by GC and GC-MS. The GC patterns of the flavor components in two parched barleys were very different. The main volatile flavor components in two of the samples were alkyl pyrazines. Compounds including 3-methylbutanal, 2-methylbutanal, dihydro-2-methyl-3(2H)-furanone, 2,5-dimethyl pyrazine, and 3-ethyl-2.5-dimethyl pyrazine were isolated from the naked barley. Compounds including thiophenes, thiazoles, sulfides, and pyrroles with burnt odor were isolated from the barley. The parched naked barley was better than barley for adding to green tea. The main aroma components of the green tea blended with the naked barley were hexanol, hexanal, trans-2-hexenal, ${\beta}$-ionone, ${\alpha}$-ionone, alkyl pyrazines, 3-methylbutanal, 2-methylbutanal, and furfural.

Analysis of Volatile Components of a Chicken Model Food System in Retortable Pouches (레토르트 파우치 계육 모형식품의 휘발성분 분석)

  • Choi, Jun-Bong;Chung, Ha-Yull;Kong, Un-Young;Moon, Tae-Wha
    • Korean Journal of Food Science and Technology
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    • v.28 no.4
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    • pp.772-778
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    • 1996
  • In order to investigate changes of flavor during food sterilization in retortable pluches, a model food system consisting of 50% chicken breast meat, 1% salt and 49% chicken stock was analyzed before and after retorting using GC and GC-MS. In the analysis of the volatile components collected by the nitrogen purge and trap technique before and after retorting, a total of 53 peaks were observed on chromatograms and 42 peaks were identified. Among the 42 peaks identified were 17 caused by aldehydes, 9 by hydrocarbons, 8 by alcohols, 6 by ketones, 1 by furan and 1 by terpene. Analysis of the data obtained from our model food system strongly suggested that the compounds responsible for retort flavor are 2-heptanone, 2-pentyl furan and various ketones.

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Gas Chromatographic/Mass Spectrometric Characterization of Dromostanolone Metabolites in Human Urine

  • 김태욱;최만호;정병화;정봉철
    • Bulletin of the Korean Chemical Society
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    • v.19 no.2
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    • pp.194-196
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    • 1998
  • The metabolism of dromostanolone (2α-methyl-5α- androstan-17β-ol-3-one) was studied in three adult volunteers after oral dose of 20 mg. Solvent extracts of urine obtained after enzyme hydrolysis were derivatized with MSTFA/TMCS and MSTFA/TMIS. The structures of intact drug and its metabolites were determined by gas chromatography/mass spectrometry (GC/MS) in electron impact (EI) mode. The major metabolite (2α-methyl-5α- androstan-3α-ol-17-one), its 3β-epimer, parent compound, and several hydroxylated metabolites including intact drug were detected by comparing total ion chromatograms of control urine with that of the administered sample. Two epimers of 2α-methyl-5α- androstan-3,17β-diol were detected using selected ion monitoring. The maximum excretion of dromostanolone and 2α-methyl-5α- androstan-3α-ol-17-one was reached in 6.2-15 hr. The half-life of intact dromostanolone was 5.3 hr. About 3.0% of the administered amount was found to be excreted within 95 hr as unchanged form.

Development and validation of a qualitative GC-MS method for THCCOOH in urine using injection-port derivatization

  • Sim, Yeong Eun;Kim, Ji Woo;Kim, Jin Young
    • Analytical Science and Technology
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    • v.34 no.2
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    • pp.68-77
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    • 2021
  • Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

Quantitative Analysis of Marker Compounds and Matabolic Profiling of Zanthoxylum piperitum (Chopi) according to Different Parts and Harvest T imes

  • Hyejin Hyeon;Eunbi Jang;Yoonji Lee;Sung Hye Han;Baek Kwang Yeol;Su Young Jung;Ki Sung Shin;Weon-Jong Yoon
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2023.04a
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    • pp.62-62
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    • 2023
  • Zanthoxylum piperitum ("chopi" in Korean) has been used as traditional medicinal plants with high anti-inflammatory, antioxidant, and antifungal activities. The aims of the study were to identify marker compounds and to investigate metabolites variation of chopi according to different parts and harvest times. Every month from June to September, chopi were harvested with three different parts: leaves, leaf-twig mixtures, twigs. Using liquid chromatography-tandem mass spectrometry (LC-MS/MS), two main marker compounds (quercitrin and quercetin-3-O-glucoside) were characterized in 70% ethanol extracts of chopi. Quantification of the two marker compounds were subsequently conducted by high performance liquid chromatography (HPLC), representing that contents of these compounds were higher in leaves and leaf-twig mixtures rather than twigs. For the comprehensive analysis of metabolites associated with production of marker compounds, 35 primary metabolites were identified using gas chromatography-mass spectrometry (GC-MS). Multivariate analysis results represented that plant parts were main contributors to the separation of chopi. However, significant differences were not observed between leaves and leaf-twig mixtures samples. The partial least square (PLS) predictive model revealed that monosaccharides (fructose, galactose, glucose, mannose, xylose) and branched-chain amino acids (isoleucine, valine, leucine) were important determinants for the production of marker compounds together with alanine, inositol, GABA, and theronic acid. This study could be extended to stabilize and utilize chopi as an industrial material, as well as to find good candidates with various nutritional traits.

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Volatile Component of Pine Needles from Pinus densiflora S. using Solid Phase Microextraction-Ges Chromatography-Mass Spectrometry

  • Lee Jae-Gon;Lee Chang-Gook;Back Shin;Jang Hee-Jin;Kwag Jae-Jin;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.18 no.4
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    • pp.373-379
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    • 2005
  • The volatile components of Pinus densiflora needles were studied by gas chromatography-mass spectrometry(GC-MS), using seven kinds of solid phase microextraction (SPME) fibers, seven in SPME fibers: 100 ${\mu}m$ PDMS, 65 ${\mu}m$ PDMS/DVB, 65 ${\mu}m$ SF-PDMS/DVB, 85 ${\mu}m$ PA, 75 ${\mu}m$ CAR/PDMS, 65 ${\mu}m$ CW/DVB and 50/30 ${\mu}m$ DVB/CAR/PDMS fibers. A total of 40 components were identified by using the seven different SPME fibers. The identified components were classified, according to their functionalities, as follows: 26 hydro-carbons, 7 alcohols, 4 carbonyl compounds, and 3 esters. The major volatile components of Pinus densiflora needles identified by these SPME fibers were $\alpha$-pinene ($1.7\~21.7\;{\mu}g/g$), $\beta$-myrcene ($2.0\~20.1\;{\mu}g/g$), $\beta$-phel-landrene ($4.6\~22.8\;{\mu}g/g$), $\beta$-caryophyllene ($6.7\~26.0\;{\mu}g/g$) germacrene D ($1.1\~11.9\;{\mu}g/g$). In the comparison of the seven SPME fibers, PDMS appeared to be the most suitable fiber for the analysis of hydrocarbon compounds and CAR/DPMS, PDMS/DVB, CW/VB and DVB/CAR/PDMS are shown to be optimal for analysis of the alcohols and carbonyl compounds.

Proteome Analysis of Waito-c Rice Seedlings Treated with Culture Fluid of Gibberellin-producing Fungus, Fusarium proliferatum KGL0401

  • Rim, Soon-Ok;Lee, Jin-Hyung;Hwang, Seon-Kap;Suh, Seok-Jong;Lee, Jin-Man;Rhee, In-Koo;Kim, Jong-Guk
    • Journal of Microbiology and Biotechnology
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    • v.16 no.12
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    • pp.1990-1994
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    • 2006
  • Fusarium proliferatum KGL0401 was previously isolated from Physalis alkekengi var. francheti plant roots and exhibited a high GA productivity. A gas chromatography-mass spectrometry (GC-MS) analysis of extracts of the culture fluid of F proliferatum KGL0401 also revealed the presence of $GA_1$, $GA_3$, $GA_4$, $GA_7$, $GA_{20}$, and $GA_{24}$. Therefore, the present study conducted a proteome analysis of waito-c rice treated with the culture fluid of the isolated F proliferatum KGL0401 to identify the protein expression triggered by the GA-containing culture fluid. The results revealed the overexpression of 180 protein spots in the sample treated with the culture fluid. Among them, 75 induced proteins were selected and analyzed by MALDI-TOF (matrix-assisted laser desorption-iorrization time-of-flight) mass spectrometry, followed by database searching, and 51 proteins were identified.