• Bulletin of the Korean Chemical Society
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• v.29 no.5
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• pp.985-987
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• 2008

Parathion is an organophosphate pesticide being legally applied for the purpose of agriculture and is being manufactured in Korea. A gas chromatography/mass spectrometric method was developed for the determination of parathion urinary metabolite, p-nitrophenol. p-Nitrophenol was extracted from weak acidic urine, and then measured by gas chromatography-mass spectrometry (selected ion monitoring). The recovery of pnitrophenol in the overall procedure was 88.2%. The detection limit of the assay was 1.0 $\mu$ g/L based upon assayed urine of 2.0 mL. The method was applied to the determination of p-nitrophenol in urine of workers of a parathion industry. Spot urines of workers of a parathion industry were sampled at the end of shift and pnitrophenol was analyzed using above developed method. p-Nitrophenol could be detected in all of the urine samples at concentrations varying from 3.0 to 681 $\mu$ g/L.

• Korean Journal of Food Science and Technology
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• v.44 no.3
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• pp.378-381
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• 2012

The monitoring of the uniconazole residual pesticide for agricultural products was conducted by multiclass pesticide multiresidue methods. Samples were collected from June to November, 2011. Uniconazole pesticide was detected in 49 samples from a total of 3,939 samples. The amount of uniconazole pesticide ranged from 0.09 to 17.89 mg/kg in 49 samples. This method was described for the simultaneous determination of uniconazole by gas chromatography with a nitrogen phosphorus detector (GC-NPD) and mass spectrometry (MS). The limit of detection and quantification were 0.006 and 0.018 mg/kg GC-NPD, respectively. For an evaluation of the GC-NPD method, uniconazole spiked into gyeojachae at a level of 0.5, 5 mg/kg was determined. The recoveries of uniconazole by the GC-NPD method ranged from 83.4 to 101.4%. The results indicate that the method of simultaneous analysis is applicable to uniconazole analysis.

• Applied Biological Chemistry
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• v.32 no.4
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• pp.350-356
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• 1989

The determinabilities of several lignan compounds by capillary-GC (F1D) were studied. The lignan compounds used were deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H and tigloylgomisin H which were isolated from fruits of Schisandra chinensis BAILLON and identified with GC/MS(EI, 70eV), 1H-NMR(300MHz) and IR. The GC column used was SPB-1 fused silica capillary$(0.25mm\;ID{\times}30m,\;Supelco)$, and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The linearities between concentration and FID response were maintained in $2{\sim}500ppm$ of deoxyschizandrin and wuweizisu C and in $5{\sim}500ppm$ of gomisin N, schizandrin, gomisin A, angeloylgomisin H and tigloylgomisin H. The contents of lignan compounds in fruits of S. chinensis BAILLON produced at Moo-ju area were analyzed by the GC method: the values obtained of schizandrin and gomisin N were 6.5 and 5.9mg/g respectively, and those of gomisin A, wuweizisu C, angeloylgomisin H, deoxyschizandrin and tigloylgomisin H were $0.5{\sim}1.6mg/g$.

• Korean journal of food and cookery science
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• v.7 no.1
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• pp.45-51
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• 1991

In this study, several standard fatty acids were analyzed by three analysis instruments. And also, for the two kinds of soybean oils, fatty acids compositions were determined by three instruments. The results were obtained as follows: 1. In the case of Gas Chromatography (GC), standard fatty acids (Myristic, Stearic, Linoleic, Linolenic, Arachidonic acid) were determined with high reproducibility, but oleic acid/elaidic acid were not seperated. By Capillary Gas Chromatography (CGC), most of standard fatty acids were determined with very high reproducibility than saturated fatty acids, and palmitic acid/oleic acid were not seperated. 2. In the analytical ability of cis-trans fatty acids isomer (oleic acid/elaidic acid), CGC was shown better analytical ability of geometrical isomer than HPLC. Oleic acid/elaidic acid were not seperated by packed column (15% DEGS). The rquire time for standard fatty acids analysis was as follows; GC, 7.21 min., CGC, 9.84 min., HPLC, 24.48 min. 3. The major compositions of fatty acids of each soybean oil (CSOY; refined, DSOY; unrefined) by GC and CGC were linoleic acid, oleic acid, palmitic acid, linolenic acid and stearic acid. But in the case of HPLC, palmitic acid/oleic acid were not seperated. Analytical ability of three instruments on fatty acids composition in each soybean oil was same trend as in the standard fatty acids mixture.

• Journal of the Korean Chemical Society
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• v.42 no.3
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• pp.266-276
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• 1998

Cholesterol supersaturation in bile, which causes gallstone formation, is the result of low bile acid secretion or high cholesterol secretion. The quantitative analysis of cholesterol, bile acids and sterols which are precursors of cholesterol have been used to examine the changes in bile component. We described a simple, sensitive and reproducible method for simultaneous determination of cholesterol, five bile acids and seven sterols in human bile juices and gallstones by capillary column gas chromatography-mass spectrometry (GC/MS). Clinical samples were hydrolyzed by alcoholic KOH, extracted twice (pH 14 and 1) and derivatized to trimethylsilyl (TMS) ether with $MSTFA/NH_4I$ (N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide) mixture in order to be detected on the GC/MS. The good quality control data were obtained through within-a-day and day-to-day test (RSD values were 1.72-13.79, 0.68-14.10, respectively) and the recovery range of them was 73.56-96. 95 Using this method, biliary and gallstone compositions in the patients with intrahepatic stones were analyzed. The amounts and its relative distribution of cholesterol, bile acids and sterols showed different pattern in bile juices and gallstones.

• Analytical Science and Technology
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• v.33 no.3
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• pp.134-142
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• 2020

Twenty-one allergy-induced aromatic material in children's products were analyzed using gas chromatography mass spectrometer(GC-MSD). The analytes were extracted using an automatic Soxhlet extractor, centrifuged for 10 minutes in a fast freezing centrifuge, and the supernatant was filtered with a syringe filter and then transferred into a 2 mL vial and injected in a split mode. In the established condition, the calibration curve showed linearity with a determination coefficient of 0.9981 or more. Sensitivity was 0.3145 ~ 1.6757, which showed a fairly wide range of sensitivity for each substance. The detection limit of the device was 0.0016 ~ 0.0423 ㎍/mL and the maximum detection limit was less than 0.05 ㎍/mL. The method detection limit ranged from 0.0030 ~ 0.0589 ㎍/mL. In addition, the limit of quantification ranged from 0.0096 to 0.1876 ㎍/mL, with precision ranging from 0.41 to 10.49 % and accuracy ranging from 83 to 116 %. The analytical method developed in this study was applied to commercial products.

• Analytical Science and Technology
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• v.25 no.6
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• pp.382-387
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• 2012

Ethylene oxide ($C_2H_4O$, EtO) is used as a raw material for the production of ethylene glycol and other industrially important material such as ethanolamines and also used as a disinfecting agent. It is applied for gas-phase sterilization of thermally sensitive medical equipment, and for processing of storage facilities as a mixture with fluorinated hydrocarbon. In this perspective, accurate determination of the mole fractions of components in the liquefied gas mixture is required for the quality control and safety of production and use. Each component of the liquefied gas mixture has different chemical and physical properties such as vapor pressure and boiling point. Therefore, we can suppose that analytical results can be different according to the introduction method for the gas phase of upper layer, or for the liquid phase of lower layer in gas cylinder. In this study, we designed a new on-line sample injection device for the liquefied gas mixture in liquid or gas state, and applied to the analysis of liquefied gas mixture of ethylene oxide and fluorinated hydrocarbons by GC/AED (gas chromatograph-atomic emission detector). We studied performance of AED, and effect of sample introduction and selected wavelength to the accuracy and repeatability of analytical results.

• Journal of Applied Biological Chemistry
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• v.63 no.2
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• pp.153-159
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• 2020

The analytical method was established for simultaneous determination of fungicide prochloraz and its metabolites in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). Samples including beef meat, pork meat, chicken meat, milk, and egg were hydrolyzed with pyridine hydrochloride which converts prochloraz and its metabolites to 2,4,6-trichlorophenol (2,4,6-TCP) because residue definition for prochloraz was 'sum of prochloraz and its metabolites containing the 2,4,6-trichlorophenol moiety, expressed as prochloraz', for compliance with MRLs from animal commodities. Therefore, residual prochloraz was extracted with acetone, decomposed to 2,4,6-TCP, partitioned with dichloromethane, purified with aminopropyl SPE and quantified as 2,4,6-TCP with GC-ECD. The instrumental limit of quantitation and method LOQ (MLOQ) was 0.01 ㎍/mL and 0.02 mg/kg for prochloraz and 0.005 ㎍/mL and 0.01 mg/kg for 2,4,6-TCP, respectively. The linearity of the calibration curve was good with R² >0.995 in the range of 0.005-0.2 ㎍/mL. Fortification levels of prochloraz were 0.02 mg/kg (MLOQ) and 0.2 mg/kg (10MLOQ) for recovery tests. Overall recoveries of prochloraz were >90% with <10% of coefficient variation (C.V.). This established analytical method was fully validated and could be useful for quantification of prochloraz and its metabolites in animal commodities as official analytical method.

• Korean Journal of Environmental Agriculture
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• v.36 no.1
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• pp.63-66
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• 2017

BACKGROUND: The phenol concentrations in water samples were determined using gas chromatography after derivatization of the analyte to phenyl acetate followed by extraction using a large volume of solvent. However, this procedure requires an additional purification step and is not analytically efficient. METHODS AND RESULTS: In this study, phenol was first extracted from an acidified water sample using ethyl acetate and then acetylated using acetic anhydride in the presence of a small amount of water and $K_2CO_3$. The derivative was extracted using 1mL of n-butyl acetate. One microliter of the extract was analyzed by GC-MS without further purification. The calibration curve showed good linearity with the $r^2$ value of 0.9968. The method detection limit and the limit of quantitation were estimated to be $0.18{\mu}g/L$ and $0.56{\mu}g/L$, respectively. Repeatability (RSD, n=3) and recovery (n=3) were 9.1%-4.3% and 90.6%-110.5%, respectively. The concentrations of phenol in a few samples of stream water were distributed in the range of $2.51-7.51{\mu}g/L$. CONCLUSION: This method is simpler and faster to implement than those currently utilized and shows high analytical reliability. It can be applied to the quantitative determination of phenol concentrations in surface water and groundwater samples.

• Analytical Science and Technology
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• v.26 no.5
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• pp.326-332
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• 2013

Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.