• 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.

• 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%.

• Archives of Pharmacal Research
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• v.9 no.3
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• pp.131-138
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• 1986

A specific and sensitive gas chromatographic (GC) procedure with the flame photometric detector (FPD) was developed for determination of barbiturates such as barbital, allobarbital, secobarbital, phenobarbital and thiopental in plasma. In order to evaluate the performance of the FPD, the results were campared with those of the flame ionization detector (FID). After extraction of barbiturates from plasma, the barbiturates were quantitatively N, N-dimethylthiometyl (MTM)-derivatized with methylthiomethyl chloride in 1, 8-diazabicyclo [5, 4, 0] undec-7-ene catalyst. The data indicate that the FPD is about 4 times more sensitive than the FID for barbiturates, although it is less reproducible. The FPD also produced chromatogram with less back ground for extracted plasma sample. The FPD also produced chromatogram with less background for extracted plasma sample. The minimum detectable amount of MTM-thiopental on 3% OV-225 column was 4, 4fmol and that of other MTM-barbiturate was about 10.0fmol.

• Environmental Analysis Health and Toxicology
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• v.17 no.2
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• pp.117-123
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• 2002

A gas chromatographic method for the determination of airborne formaldehyde was established. In order to be highly detectable with the electron capture detector, formaldehyde was derivatized to its pentafluorobenzyl oxime form by reacting with O- (2,3,4,5,6- pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) at pH of 4.6 and temperature of 50$^{\circ}C$ for 1 hour. Air samples were collected into a Tedlar$\^$(R)/ bag followed by transferring into water contained in two impingers in series. Collection efficiency in the front trap was higher than 90％. Measurement of selected indoor and outdoor air samples showed higher formaldehyde concentrations in indoor air environments and the importance of ventilation for reducing indoor pollution.

• Archives of Pharmacal Research
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• v.27 no.8
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• pp.820-824
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• 2004

An optical purity test was indirectly performed on (S)-ibuprofen as its diastereomeric (R)-(+)-1-phenylethylamide derivative using achiral gas chromatography (GC). The method for the determination of trace (R)-ibuprofen (optical impurity), within the range 1.0 to 50 ng, from a racemic ibuprofen standard was linear (r＝0.9997) with acceptable precision (％ $RSD{\leq}5.3$) and accuracy (％ RE＝0.7~-3.9). Similar results were obtained with the method validation for the quantification of (S)-ibuprofen within the range 0.1 to 2.0 $\mu\textrm{g}$ using a (S)-ibuprofen stan-dard. When applied to seven different commercial (S)-ibuprofen products, their optical purities (98.7~99.1％) were determined with good precision (％ $RSD{\leq}4.0$).

• YAKHAK HOEJI
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• v.28 no.4
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• pp.243-248
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• 1984

For gas chromatographic determination with the sulfur-specific flame photometric detector, nine ${\beta}$-lactam antibiotics without ${\alpha}$-amino group were esterified with borontrifluoride-methanol complex and then N-benzoylated with benzoyl chloride. The gas chromatographic separation of these products was successfully carried out on various silicon polymers (OV-1, OV-101, OV-17, OV-225, and QF-1) coated on the acid washed, silanized diatomite. The structure of the esterified and N-benzoylated product was confirmed by mass spectromer.

• Archives of Pharmacal Research
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• v.19 no.6
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• pp.566-569
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• 1996

A sensitivity method has been developed for the detection and determination of niflmic acid(NA) in human urine. Samples were extracted with diethylether. Flunixin (FN) was added to the sample prior to extraction as an internal standard. Niflumic acid was converted to its methyl derivative and analyzed by capillary gas chromatography/negative chemical isonization mass spectrometry. Using selected ion monitoring (SIM), the levels of NA down to 5 pg/ml could be detected in 5 ml spiked urine sample. Calibration curve was linear over the range of 0.5 ppm-50 ppm. The recovery of niflumic acid from urine at 40 pg/ml was to be $91.7{\pm}3.8(n=3)$ and the coefficient of variation was 4.1%.

• Korean Journal of Food Science and Technology
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• v.26 no.6
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• pp.750-758
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• 1994

Flavour components of seven Korean folk sojues, five Chinese kaoliangchiews and Japanese shochu were determined by GC and GC-MS after solid phase extraction with polydivinyl benzene. Less volatile ethyl succinate and ethyl pelargonate were present in Korean folk sojues while volatile ethyl acetate and ethyl butyrate in Chinese kaoliangchiews. In the case of alcohols, the amount of isopentyl alcohol was relatively higher than that of isobutyl alcohol or n-propyl alcohol in Korean folk sojues. On the contrary, less volatile n-propyl alcohol was present more than isopentyl alcohol in Chinese kaoliangchiews. Multivariate statistical analyses involving principal components analysis (PCA) and discriminant analysis (DA) were applied to the GC data. The results of PCA clearly demonstrate that the first principal scores of Korean folk sojues were similar but the second principal scores were different from each other. Classification of Korean sojues and Chinese kaoliangchiews into two groups could be conducted by DA. These results suggested that the common charateristics and identities as a distilled liquors was found in Korean folk sojues.

• Journal of the Korean GEO-environmental Society
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• v.10 no.2
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• pp.37-43
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• 2009

With the economic development of Korea, sewage treatment facilities and waste food treatment facilities have been steadily increased. These facilities have positive effects such as the conservation of the water resources quality and waste food recycling while they also affect the neighborhood life with severe odor problems. Therefore, it was first collected sludge samples from 5 sewage treatment facilities and 5 waste food treatment facilities where the amounts of waste produced from above sites are relatively immense in Busan and estimate the $H_2S$ emission rates. Then it was selected 1 sample which has the highest emission rate of $H_2S$. Using flux chamber and GC/FPD analyses, it was tried to quantify the emitted amount of sulfonic gas concentration under anoxic condition. The sludge sample obtained from Noksan sewage treatment facility has the highest emission rate of $H_2S$. This sample contained 156.18 mg/kg $H_2S$. The odor compounds were analyzed using GC/FPD and the concentrations were converted to odor quotient. Among odor compounds the ratio of $CH_3SH$ (methylmercaptan) for the total odor quotient was 47.3% and considered to be the main odor compound in the sample.

• Analytical Science and Technology
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• v.18 no.4
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• pp.320-328
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• 2005

The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).