• Analytical Science and Technology
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• v.25 no.5
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• pp.292-299
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• 2012

GC/MS has been utilized for many applications due to great resolution and reproducibility, which made it possible to build up the database of mass spectrum, while HS-SPME has the advantage of solventfree extraction of volatile compounds. The combination of these two methods, HS-SPME GC/MS, enabled many scientific applications with various possibilities. In this study, the analysis of trail pheromone excreted from live Camponotus japonicus with the feature of solvent-free extraction was carried out and the optimization for this analysis was performed. The major compounds detected were n-decane, n-undecane, and n-tridecane. Optimization for the best detection of these hydrocarbons was processed in the point of SPME parameter (selection of fiber, extraction temperature, extraction time, etc.). The advantage of the analysis of live sample is to analyze phenomenon right after it is excreted by ants. But the experimental process has restriction of extraction temperature and time because of the analysis of live ants. Establishing the process of HS-SPME GC/MS applied to live samples shown in this study can be a breakthrough for the ecofriendly and ethical research of live things.

• 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.

• Analytical Science and Technology
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• v.22 no.5
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• pp.407-414
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• 2009

A simultaneous determination method for cholesterol, lanosterol and desmosterol was developed using gas chromatography/mass spectrometry. Urine was enzymatically hydrolyzed with ${\beta}$-glucuronidase/arylsulfatase. Samples were prepared using extractions with a mixture of ethyl acetate-hexane (2:3, v/v), followed by derivatization with a mixture of MSTFA/TMSI/TMCS (100:2:5 v/v/v). All analyses were performed using GC/MS in selective ion monitoring mode. Good linearities ($r^2=0.998{\sim}0.999$) in calibration curve and a satisfactory recovery (80.0%~113%) were achieved. Accuracy and precision values within ${\pm}15%$ in the concentration range of 5 to 200 ng/mL were also observed for all compounds. The developed method was applied to pravastatin-treated (70 and 250 mg/kg/day for 7 days, oral) hyperlipidemia rats. Those sterols were significantly lower in drug-treated rats compared to the controls, which justifies the drug efficacy. Therefore, these results indicate that the developed method was successfully applied to examine statin drug efficacy with urine sample.

• Journal of the Korean Chemical Society
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• v.39 no.8
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• pp.635-642
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• 1995

Improved sample introduction system has been investigated for the determination of volatile organic compounds in water using a purge & trap preconcentration apparatus and a capillary gas chromatography/mass spectrometry. The present limitations associated with the moisture control module and cryorefocusing system suggested by EPA were discussed. To solve the problems such as improper separation of peaks due to the adsorption of water and contamination of purge & trap system, a more efficient connection system between the purge & trap apparatus and the gas chromatograph was introduced and the optimum operational conditions were suggested. A carbopack B/carboxen 1000 and 1001 trap was used for the purge & trap procedure and a custom made crosslinked dimethyldiphenylpolysiloxane capillary column was used for the separation of compounds. Accuracy and precision of the method suggested in this report were examined and the method detection limit of each compound was proposed for the simultaneous determination of 54 volatile organic compounds in water.

• Journal of the Korean Society of Marine Environment & Safety
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• v.27 no.6
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• pp.890-897
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• 2021

Since the enforcement of strict regulations on marine fuel oil sulfur content, demand for Low Sulfur Fuel Oil (LSFO) has been increasing. However, as LSFO properties vary greatly depending on the supply timing, region, and supplier, LSFOs can experience problems with sludge formation, blending compatibility, and stability once mixed into storage tanks. This study investigates using ultrasound cavitation effects to improve the quality of LSFOs in storage tanks. For marine gas oil (MGO), the results showed that the relative ratio of high molecular weight compounds to those of low molecular weight decreased after ultrasonic irradiation, due to cavitation-induced cracking of chemical bonds. For marine diesel oil (MDO) and blended oil, a small increase in the relative abundance of low weight molecular compounds was observed after treatment. However, no correlation between time and relative abundance was observed.

• Journal of Food Hygiene and Safety
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• v.9 no.1
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• pp.1-13
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• 1994

A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

• Analytical Science and Technology
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• v.11 no.1
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• pp.36-41
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• 1998

A gas chromatography-mass spectrometry method for the determination of 5-fluorourasil in human plasma is described. The method involves a single extraction procedure with 10 ml of isopropanol-ether(20:80) solution and pentafluoro-benzylation. Samples were injected using an automatic injector, followed by separation on a nonpolar capillary column and detection with a mass selective detector(MSD). No endogeneous compounds were found to interfere. The detection limit, based upon an assayed plasma volume of 0.5, was 3 ng/ml. The extraction yield was found to be above 80%. Plasma 5-FU concentrations were determined by this method in about 500 plasma samples from cancer patients undergoing treatment with 5-FU. This method is suitable for monitoring of 5-FU in plasma of cancer patients.

• Proceedings of the PSK Conference
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• 2003.04a
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• pp.314.2-315
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• 2003

Sophoricoside was isolated as the inhibitor of IL-5 bioactivity from Sophora japonica (Leguminosae). To develope as novel anti-allergic drug. kinetic study was performed in rats. Serum concentration of sophoricoside was measured by gas chromatography-mass spectrometry (GC/MS) in male Sprague-Dawley rat (250${\pm}$10g, n=5) after oral administration of sophoricoside (100mg/kg). (omitted)

• Journal of Applied Biological Chemistry
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• v.50 no.3
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• pp.120-126
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• 2007

Volatile components in red bean (Vigna angularis) were investigated. Extracts prepared by simultaneous steam distillation and solvent extraction were analyzed by gas chromatography/mass spectrometry. One hundred and forty-two components including alkanes/alkenes (17), aromatics (5), furans (15), miscellaneous compounds (2), other nitrogen-containing compounds (11), aldehydes (11), naphthalenes (11), alcohols (34), ketones (23), sulfur-containing compounds (5) and esters (8) were identified. Some of these components, e.g. hexanal, were known to contribute to the "beany" odor in other beans. Due to the presence of such odor, red beans may not be acceptable to some consumers.

• Food Science and Biotechnology
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• v.18 no.5
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• pp.1288-1292
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• 2009

Volatile flavor compounds were isolated from the flowers of Chrysanthemum indicum L. (gamguk) produced in Korea and China by the hydro distillation, and were analyzed by gas chromatography-mass spectrometry (GC/MS). The yield of oils from Korean and Chinese gamguk were 2.0 and 0.5%(v/w), respectively. Sixty-three volatile compounds of Korean gamguk representing 89.28% of the total peak area were tentatively identified, including 35 hydrocarbons, 12 alcohols, 6 ketones, 3 esters, 5 aldehydes, 1 oxide, and 1 miscellaneous component. Thirty-six volatile components of Chinese gamguk constituted 58.15% of the total volatile composition were tentatively characterized, consisting of 19 hydrocarbons, 7 alcohols, 2 ketones, 2 esters, 4 aldehydes, 1 oxide, and 1 miscellaneous component. The predominant components of Korean oil were ${\alpha}$-pinene, 1,8-cineol, and chrysanthenone. Whereas, camphor, ${\alpha}$-curcumene, and ${\beta}$-sesquiphellandrene were the main aroma compounds of Chinese gamguk.