• Title/Summary/Keyword: GC/MS spectrometry

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디클로벤지딘에 폭로된 흰쥐의 간장세포와 방광 상피세포에 형성된 DNA adducts의 $^{32}P-postlabeling$과 GC/MS-SIM에 의한 분석

  • 이진헌;신호상;장미선
    • Proceedings of the Korean Environmental Health Society Conference
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    • 2002.04a
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    • pp.49-51
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    • 2002
  • To identify and evaluate the dichlorobenzidine(DCB)-DNA adducts in liver cell and bladder epithelial cells by $^{32}$ P-postlabeling and GC/MS-SIM, we orally exposed the dichlorobenzidine (20mg/kh body wt.,/day)to male sprague-dawley rats for 14 days. Two kinds of DCB-DNA adduct were found at the same site of thin layer chromatogram of $^{32}$ P-postlabeling method in liver cells and bladder epithelial cells. In liver cells, relative adduct labeling(RAL) $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 34.1$\pm$3.71 and 69.9$\pm$5.02, that of adduct A2 were 74.1$\pm$10.1 and 105.1$\pm$10.1 on 10 and 14 days after treatment, respectively. And in bladder epithelia cells, RAL $\times$ 10$^{12}$ of DCB-DNA adduct A1 were 5.92$\pm$1.60 and 15.9$\pm$1.31, that of adduct A2 were 9,81$\pm$2.81 and 22.8$\pm$1.79 on 10 and 14 days after treatment, respectively. DCB metabolites formed DNA adducts were monoacetyl-dichlorobenzidine(acDCB) and diacety1-dichlorobenzidine(di-acDCB), which was identify by gas chromatography/mass spectrometry-scan ionization mode(GC/MS-SIM), along with hydrolysis, extraction and TFA(trifluoroacetyl anhyride) derivatization with DCB-DNA adducts isolated from live cells and bladder epithelial cells. The base peak of acDCB were 252 and 294 m/z, and that of di-acDCB were 252, 294 and 336 m/z. In conclusion, the exposed DCB formed two kinds of DCB-DNA adduct, the proximate materials of that were acDCB and di-acDCB in liver and bladder epithlial cells. And the above GC/MS-SIM method was found the DCB-DNA adducts could be monitoring by gas chromatography.

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Thermal Degradation of High Molecular Components Obtained from Pyrolysis of Mixed Waste Plastics (혼합폐플라스틱의 열분해로부터 생성된 고분자성분의 열적분해)

  • Oh, Sea Cheon;Ryu, Jae Hun;Kwak, Hyun;Bae, Seong-Youl;Lee, Kyong-Hwan
    • Applied Chemistry for Engineering
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    • v.19 no.2
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    • pp.191-198
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    • 2008
  • The thermal degradation characteristics of high molecular components obtained from pyrolysis of mixed waste plastics have been studied by thermogravimetric analysis (TGA) and gas chromatography spectrometry (GC-MS). The kinetics of thermal degradation has been studied by a conventional nonisothermal thermogravimetric technique at several heating rates between 10 and $50^{\circ}C/min$. The dynamic thermogravimetric analysis curve and its derivative have been analyzed using a variety of analytical methods reported in the literature to obtain information on the kinetic parameters such as activation energies and reaction orders. The yields of liquid products have been monitored by batch pyrolysis reactor under various reaction temperatures and reaction times. And the characteristic of liquid products with the increase in reaction temperature has been performed by GC-MS.

Identification of Volatile Compounds of 4 Grape Species by Storage Conditions (전자코와 GC/MS를 이용한 포도 품종별 저장 조건에 따른 휘발성 향기 성분 연구)

  • Lee, Yun-Jeung;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.7
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    • pp.874-880
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    • 2007
  • Volatile flavor compounds of 4 grape species (Campbell, Sheridan, Red globe, and Meoru) were identified during 3-day storage at either $4^{\circ}C$ or room temperature. Each sample was analyzed by solid-phase micro-extraction (SPME) method combined with gas chromatography-mass spectrometry. Also electronic nose composed of 12 different metal oxide sensors was used to differentiate flavors of grapes. Sensitivities (delta $R_{gas}/R_{air}$) of sensors from electronic nose were obtained by principal component analysis (PCA). Proportion of the first principal component was 99.30% at $4^{\circ}C$ and 99.36% at room temperature, respectively. In our result, flavor patterns of grape can be differentiated according to the storage period. The major volatile flavor compounds were 1-hexanol, hexanoic acid and its ethyl ester, and phenylethyl alcohol with the presence of butanoic acid and its ethyl ester, acetic acid, benzeneacetic acid and its ethyl ester.

Application of a Gas Chromatography/Mass Spectrometric Method for the Determination of Butyltin Compounds in Sediment

  • Won, Yong-Il;Jung, Pyong-Gil;Chung, Min-Young;Kim, Byung-Joo;Yim, Yong-Heon;So, Hun-Young;Kim, Yong-Seong
    • Bulletin of the Korean Chemical Society
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    • v.25 no.10
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    • pp.1508-1512
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    • 2004
  • A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry.

Soil properties and molecular compositions of soil organic matter in four different Arctic regions

  • Sujeong, Jeong;Sungjin, Nam;Ji Young, Jung
    • Journal of Ecology and Environment
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    • v.46 no.4
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    • pp.282-291
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    • 2022
  • Background: The Arctic permafrost stores enormous amount of carbon (C), about one third of global C stocks. However, drastically increasing temperature in the Arctic makes the stable frozen C stock vulnerable to microbial decomposition. The released carbon dioxide from permafrost can cause accelerating C feedback to the atmosphere. Soil organic matter (SOM) composition would be the basic information to project the trajectory of C under rapidly changing climate. However, not many studies on SOM characterization have been done compared to quantification of SOM stocks. Thus, the purpose of our study is to determine soil properties and molecular compositions of SOM in four different Arctic regions. We collected soils in different soil layers from 1) Cambridge Bay, Canada, 2) Council, Alaska, USA, 3) Svalbard, Norway, and 4) Zackenberg, Greenland. The basic soil properties were measured, and the molecular composition of SOM was analyzed through pyrolysis-gas chromatography/mass spectrometry (py-GC/MS). Results: The Oi layer of soil in Council, Alaska showed the lowest soil pH and the highest electrical conductivity (EC) and SOM content. All soils in each site showed increasing pH and decreasing SOC and EC values with soil depth. Since the Council site was moist acidic tundra compared to other three dry tundra sites, soil properties were distinct from the others: high SOM and EC, and low pH. Through the py-GC/MS analysis, a total of 117 pyrolysis products were detected from 32 soil samples of four different Arctic soils. The first two-axis of the PCA explained 38% of sample variation. While short- and mid-hydrocarbons were associated with mineral layers, lignins and polysaccharides were linked to organic layers of Alaska and Cambridge Bay soil. Conclusions: We conclude that the py-GC/MS results separated soil samples mainly based on the origin of SOM (plants- or microbially-derived). This molecular characteristics of SOM can play a role of controlling SOM degradation to warming. Thus, it should be further investigated how the SOM molecular characteristics have impacts on SOM dynamics through additional laboratory incubation studies and microbial decomposition measurements in the field.

Determination of 11 Phenolic Endocrine Disruptors using Gas Chromatography/Mass Spectrometry-Selected Ion Monitoring in Five Selected Wastewater Influents

  • Kim, Hyub
    • Environmental Engineering Research
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    • v.13 no.4
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    • pp.216-223
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    • 2008
  • An efficient method for the simultaneous determination of eleven phenolic endocrine-disrupting chemicals (EDCs) present in wastewater influent samples was described. The 11 phenolic EDCs including alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) following two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. The wastewater influent samples containing the 11 EDCs were adjusted to pH 2 with $H_2SO_4$ and then cleaned up with n-hexane. Next, they were subjected to solid-phase extraction (SPE) with XAD-4 resin and subsequently converted to isoBOC or TBDMS derivatives for sensitivity analysis with gas chromatography/mass spectrometry-selected ion monitoring (GC/MSSIM). Following isoBOC derivatization and TBDMS derivatization, the recoveries were 86.6-105.2% and 97.6-142.7%, the limits of quantitation (LOQ) for the 11 phenolic EDCs for SIM was 0.001-0.050 ng/mL and 0.003-0.050 ng/mL, and the SIM responses were linear with the correlation coefficient varying by 0.9717-0.9995 and 0.9842-0.9980, respectively. When these methods were applied to five selected wastewater influent samples, for isoBOC derivatization and TBDMS derivatization the ranges of concentration detected were 0.2-99.6 ng/mL and 0.4-147.4 ng/mL, respectively.

Identification and Quantification of Tar Compounds in Plant Cell Cultures of Taxus chinensis (주목 식물세포(Taxus chinensis) 배양 유래 타르 성분 동정 및 정량)

  • Kim, Gun-Joong;Park, Gyu-Yeon;Kim, Jin-Hyun
    • Microbiology and Biotechnology Letters
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    • v.41 no.3
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    • pp.272-277
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    • 2013
  • In this study, the tar compounds derived from the plant cell cultures of Taxus chinensis were first identified and then quantified via gas chromatography/mass spectrometry (GC/MS) and gas chromatography (GC). 2-Picoline, 2,5-xylenol, acenaphthene, 1-methylnaphthalene and o-xylene were found to be the major tar compounds by biomass. These compounds were identified and confirmed by comparing their retention times with those of authentic compounds. Each compound also spiked with the pure standard. The contents of 2-picoline, 2,5-xylenol, acenaphthene, 1-methylnaphthalene, and o-xylene in biomass were 0.2512, 0.1586, 0.1240, 0.0942 and 0.0525 wt%, respectively. Liquid-liquid extraction and adsorbent treatment were able to remove 42% and 94% of the tars from biomass, respectivly. After hexane precipitation, all of the tars were perfectly removed.

The Quantitative Analysis of Polycyclic Aromatic Hydrocarbons(PAHs) in Sewage Sludge by Gas Chromatography-Ion Trap Mass Spectrometry (가스크로마토그래피-이온트랩질량분석법을 이용한 하수슬러지 중 다핵방향족탄화수소(PAHs) 함량 분석)

  • 남재작;소규호;박우균;조남준;이상학
    • Journal of Environmental Science International
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    • v.11 no.4
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    • pp.367-373
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    • 2002
  • The polycyclic aromatic hydrocarbons(PAHs) content in sewage sludge was determined by gas chromatography linked to ion trap mass spectrometry(GC/ITMS) with five deuterated PAHs as internal standards. The minimum detection limit was from 1.66 to 7.14 pg for individual PAH by GC/ITMS. For determining total PAHs(∑PAH) in sewage sludge 84 samples from 74 waste water treatment plants in whole country were analyzed. The average content of ∑PAH far whole samples was 3,289$\pm$3,098 $\mu\textrm{g}$/kg, and ranged from 142 to maximum 20,102 $\mu\textrm{g}$/kg. According to the number of population of the city, the areas were classified as five regions, ie. big, large, middle, small, and rural area in which the waste water treated plants were grown. The contents of PAHs were 4,689$\pm$5,503, 5,839$\pm$6,401, 3,725$\pm$2,053, 2,237$\pm$2,069, and 2,475$\pm$1,489 $\mu\textrm{g}$/kg, in big, large, middle, small, and rural area, respectively.

The Changes of Aroma in Wine Treated with Reverse Osmosis System (역삼투압 시스템으로 처리한 포도주의 향기성분 변화)

  • Lee, Seung-Ryong;Lee, Kyu-Hee;Chang, Kyu-Seob;Lee, Suk-Kun
    • Korean Journal of Food Science and Technology
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    • v.32 no.1
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    • pp.17-24
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    • 2000
  • Reverse osmosis (RO) system was applied to improve wine quality. General wine (GEN) and wines containing different sugar levels $24^{\circ}Brix$ (RO-24) and $24^{\circ}Brix$ (RO-28) by removing pure water using RO system without sugar addition on brewing method. And they were compared by wine aroma analysis. The preparing method of analysis was LLCE (liquid-liquid continuous extraction). And volatile aroma compounds of different wines were prepared for raw, and diluted materials in same proportion. The wine aromas were described by trained twelve panelists for QDA (quantitative descriptive analysis) and showed for FD (flavor dilution)-chromatogram. Consequently, overall acceptability of RO-28 showed better than that of other treatments. Aromas of RO-28 also were represented the high contents of positive aroma compounds such as ethanol and ethyl acetate, which were identified by GC-O and GC-MS.

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Derivatization and Residual Determination of MCPP in Soil Leachate (토양 침투수중 MCPP의 유도체화 및 잔류분석)

  • Hong, Moo-Ki;Smith, Albert E.
    • Korean Journal of Environmental Agriculture
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    • v.13 no.2
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    • pp.199-208
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    • 1994
  • Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

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