• Bulletin of the Korean Chemical Society
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• v.28 no.3
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• pp.432-438
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• 2007

Environmentally important phthalic esters have been analyzed by GC-MS in terms of individual phthalic esters or total phthalic esters directly or after derivatization. Derivatization improves the chromatographic characteristics of the highly polar phthalic esters. This study focused on the GC-MS determination of the total phthalic esters and the individual phthalic esters simultaneously. The phthalic esters were hydrolyzed to phthalate and corresponding alcohols in 1 M NaOH solution at 90 oC for 30 min followed by extraction with ethyl acetate after acidifcation. The phthalic acid and alcohols were simultaneously silyl derivatized using bis(trimethylsilyl)trifluoroacetamide (BSTFA) to their corresponding silyl ester and ethers in the mixture of 60% acetone and 40% ethyl acetate at room temperature within 30 min. Because of the high reactivity of BSTFA with the phthalic acid and alcohols effective silyl derivatization was possible simultaneously. GC-MS analysis of the silyl derivatives of phthalic acid and alcohols was performed. The total phthalic ester content was estimated from the analytical result of phthalic silyl ester, while the individual phthalic ester was quantified from the analytical results of alcoholic silyl ethers. This technique was applied to spiked tab water and real seawater samples from the Lake Shihwa in Korea. The results were checked against the results from the direct GC-MS analysis of the phthalic esters and reasonable recoveries with high sensitivity were achieved. The recoveries were higher than 75% with low relative standard deviation (below 10%).

• Tribology and Lubricants
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• v.28 no.6
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• pp.315-320
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• 2012

For proper functioning, general machines usually need lubricant oil as a cooling, cleaning, and sealing agent at points of mechanical contact. The quality of lubricant oil can deteriorate during operation owing to various causes such as high temperature, combustion products and extraneous impurities. In this study, a heavy load stopped during operation, and the oil was analyzed to check whether any impurities were added. Extraction using acetonitrile followed by reaction with BSTFA(bistrimethylsilyl trifluoroacetamide) showed that, trimethylsilylated ethylene glycol was present in the lubricant oil. To quantify the ethylene glycol in the oil, deuterium-substituted ethylene glycol, which acted as an internal standard, was added to the sample and then extracted with the solvent. Next, the extract was reacted with the derivatizing agent(BSTFA) and then analyzed with GC/MS. The detection limit of this method was found to be $0.5{\mu}g/g$ and the recovery of oil containing $20,000{\mu}g/g$ of ethylene glycol was measured to be 94.8%. A damaged O-ring and eroded cylinder liner were found during the overhaul, which implied the leakage of coolant containing ethylene glycol into the lubricating system. The erosion of the cylinder liner was assumed to be due to cavitation of the coolant in the cooling system.

• Journal of The Korean Society of Inherited Metabolic disease
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• v.15 no.3
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• pp.138-146
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• 2015

Purpose: If early diagnosis is not made, patients with metabolic disorders as homocystinemia rapidly progress to physical defect or mental retardation resulted in storage of the toxic material into the brain. Therefore, it is necessary to develop an analytical method for a rapid screening and/or correct confirmation diagnosis. Methods: The standard solution of sulfur amino acids spiked plasma was subjected to protein precipitation with methanol, and then consecutively derivatized with trimethylsilyl (TMS) and trifluoroacyl (TFA) and determined by GC-MS. The formation of TMS derivative of the hydroxyl and TFA derivative of amino functional group was performed by BSTFA and MBTFA, respectively. Selective ion monitoring (SIM) mode was used for quantification with selected specific ions. Results: A calibration curve on standard spiked pooled plasma showed a linear relationship with correlation coefficient of 0.9936-0.9992 for all compounds over the range of 0.1-300 ng. The precision and accuracy were within S.D. of 1-15% and RSD of 1-15% for intra-day assay at 2 ng/mL, 15 ng/mL and 30 ng/mL. LOD and LOQ was 0.4 ng/mL and 4 ng/mL respectively. Conclusion: A rapid analytical method was developed to quantify sulfur amino acids and methyl malonic acid, after two-step derivatization procedure with good sensitivity and specificity on human plasma. Advantages of a new method are simplicity and rapidity. The method could be useful for routine analysis, diagnosis of homocysteinemia.

• Korean Journal of Microbiology
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• v.37 no.1
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• pp.66-71
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• 2001

An aerobic microbiological process was tested in 1.5 L stirred tank reactors for the treatment of dinitrotoluenes (DNTs)[e.g., 2.4-dinitrotoluene (2,4-DNT), 2,6-dinitrotoluene (2,6-DNT)] in the test culture of Stenotrophomonas maltophilia, which had previously characterized. Both 2,4-DNT and 2,6-DNT were completely degraded within 10 days and 14 days of incubation, respectively. Addition of the secondary carbon was essential to degrade DNTs, and little degradation was achieved in the absence of the secondary carbons. The effect of additional nitrogens on the degradation of DNTs was evaluated. Complete degradation of DNTs was observed in the absence of any additional nitrogens, whereas DNTs were partially degraded in the growth media with additional nitrogens. Both HPLC and GC-MS were used to detect and verify the residual DNTs and their intermediates. As the results, the HPLC and GC-MS chromatograms demonstrated that the both parent compounds, 2, 4-DNT and 2,6-DNT, and respective intermediates, 2-amino-4-nitrotoluene and 2-amino-6-nitrotoluene, could be successfully identified under the analytical conditions.

• Analytical Science and Technology
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• v.12 no.3
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• pp.248-255
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• 1999

Sewage sludge samples were extracted with dichlomethane by Soxhlet extraction. The extracts were analysed for the endocrine disrupting compounds (EDC), octylphenol(OP), nonylphenol (NP) and bis (2-ethylhexyl)phthalate (DOP) using GC/MS-SIM. In industrial sewage sludge (sample Z-1) the concentration of NP and DOP were respectively $1168{\mu}g/g$ and $1172{\mu}g/g$ whereas in domestic sludge (sample Z-2) the concentration were respectively $10.8{\mu}g/g$ and $80{\mu}g/g$. OP was not detected in Z-2, but detected a small amount in Z-2 of the samples. Environmental EDC have been shown to affect the fertility of range of living organisms, including humans, and the high levels of NP and DOP in industrial sewage sludge could have serious implications for the reproductive health of humans particularly if the compounds entered the human food chain through water or the ingestion of vegetables or animal products.

• Analytical Science and Technology
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• v.13 no.5
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• pp.666-674
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• 2000

The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

• Horticultural Science & Technology
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• v.32 no.3
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• pp.359-365
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• 2014

Oriental pear (Pyrus communis L. cv 'Niitaka') was stored at $0^{\circ}C$ for 5 months and major metabolites involved in blackening of the peel were analyzed by untargeted GC-MS and targeted HPLC methods. In this study, peels of sound and skin-blackened pears were analyzed and compared. Skin-blackened fruit was clearly characterized by a distinctive pattern in changes which included a decrease of malic acid, succinic acid, and ascorbic acid, while an increase of fumaric acid, threonine, and gluconic acid, which indicated both reduced metabolic activity and anti-oxidative capacity of the cells. Chlorogenic acid was a major phenolic compound and the peel of sound fruit showed high levels of free phenolic compounds compared than the peel of skin-blackened fruit which are believed to be related to oxidation of phenolics in skin-blackened tissue. The changes or profiling of major metabolites by targeted or untargeted analysis method could become a useful tool for understanding physiology, disorder mechanism, and identifying metabolic networks connecting primary and secondary metabolism in postharvest research.

• 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.

• Journal of the Korean Chemical Society
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• v.47 no.6
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• pp.559-568
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• 2003

A procedure based on liquid liquid extraction(LLE)-GC/MS has been developed for the simultaneous analysis of antioxidants and insecticides known as endocrine disrupters. The endocrine disrupters investigated in this study are butylated hydroxy anisole(BHA) and butylated hydroxy toluene(BHT), and the insecticides are allethrin and fenvalerate. The limit of detection(LOD) was 0.071~0.159 ng/ml with RSD of 1.41~5.34% for the standard sample. From water reservior of Han river, Geum river, Nakdong river and Sumjin river, these compounds were not detected. For the synthesized sample, the LOD is 0.051~0.132 ng/ml with RSD of 6.39~13.4%.

• Journal of the Korean Wood Science and Technology
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• v.37 no.3
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• pp.265-273
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• 2009

The aim of this study was to investigate the antifungal activitiy of extracts from different parts of Cryptomeria japonica against Trichophyton mentagrophytes, Trichophyton rubrum and Microsporum gypseum. Disc diffusion and agar dilution methods were used for determining the antifungal activity of extracts, and their major constituents were analyzed by GC/MS. Black heartwood extract among the extracts showed the highest antifungal activity against dermatophytes. TLC was used for fractionating the effective fraction from the black heartwood extract with n-hexane and chloroform as developing solvents, and then antifungal activity of each fraction was examined against dermatophytes. As a result, seventh fraction showed the highest antifungal activity among nine fractions. The major constituent of the seventh fraction determined by GC/MS was expected to be sesquiterpene, damascone with 2 more carbon atoms. The other constituents were also identified as elemol, eudesmol and hinokione.