• Korean Journal of Food Science and Technology
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• v.29 no.3
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• pp.427-431
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• 1997

A simultaneous and rapid gas chromatographic determination of organophosphorus, organo-chlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The pesticides were extracted from samples with acetone by automated soxhlet apparatus and this extract was evaporated to dryness. The residue was dissolved in hexane, the solvent was applied to a Sep-Pak florisil catridge, was eluted with 50% ethyl acetate in n-hexane, and was injected to dual GC-ECD/NPD system. This simple method affords a high recovery of hydrophilic pesticides, allows rapid analysis, and is cheap to perform. Except for dichlorvos and captan, recoveries of 46 pesticides were over 60%.

• Analytical Science and Technology
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• v.7 no.3
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• pp.339-347
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• 1994

A multicolumn system consisted of two valve(10-port and 6-port valve)-three column (28% DC 200, SP 1700 and Chromosorb 102 column) was developed. Nine natural gas components composed of $N_2$, $CH_4$, $CO_2$, $C_2H_6$, $C_3H_8$, $i-C_4H_{10}$, $n-C_4H_{10}$, $i-C_5H_{12}$ 및 $n-C_5H_{12}$ completed all the baseline separation within 18 minutes. The accuracy and the precision of this system was tested. The retention times and the peak areas were determined with a repeatability between 0.02 and 0.16%, and less than 1%, respectively. Calibration curves for natural-gas components were plotted by the partial pressure injection method of pure gases, and good linear relationships for each component were presented. By using these calibration curves the accuracy of the multicolumn system compaired with that of the single column system for a certified standard gas of natural gas. As a result, relative error in the single and the multicolumn system was less than 0.5% and 0.04%, respectively. The result of application of this system in the analysis of importing LNG composition showed that the heating values calculated by the multicolum system were estimated lower compared with those calculated by the single column system and consequently, the importing price of LNG was able to be cut down.

• Journal of the Korean Chemical Society
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• v.30 no.4
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• pp.369-376
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• 1986

Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

• Korean Journal of Environmental Agriculture
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• v.16 no.4
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• pp.333-340
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• 1997

An analytical method was developed to determine residues of haloxyfop-R and its methyl ester in soils and soybeans using gas-liquid chromatography (GLC) with electron capture detector (ECD). Soil or soybean sample was acidified and extracted with acetone. The extract was then subjected to ion-associated partition to individually separate haloxyfop-R and the neutral methyl ester. One phase containing haloxyfop-R was methylated with $BF_3$/methanol, partitioned to n-hexane and analyzed by GLC/ECD. The other phase containing the methyl ester was further purified by Florisil column chromatography prior to GLC determination. No cross contamination was found between two phases containing each of the acid and methyl ester, thus two compounds can be separately determined as the identical haloxyfop-R-methyl. Overall recoveries of haloxyfop-R from fortified samples averaged 88.2${\pm}$3.9% (n=12) and 88.3${\pm}$4.0% (n=6) for soils and soybeans respectively, and those of haloxyfop-R-methyl showed mean values of 89.2${\pm}$4.0% (n=12) and 85.6${\pm}$5.6% (n=6). Detection limits of both haloxyfop-R and its methyl esterwere 0.005㎎/㎏ and 0.01㎎/㎏ for soil and soybean samples respectively.

• Applied Biological Chemistry
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• v.26 no.2
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• pp.104-109
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• 1983

Gas chromatographic method for the analysis of phorate(0,0-diethyl S-ethyl-thiomethyl phosphorithioate) and its metabolites in soil and vegetables was studied by using a mixed phase column(10% DC-200+8% Reoplex-400+2% QF-1 on Gas Chrom Q, $1.8{\times}2mm$ i.d, borosilicate glass column). This column can separate completely phorate and its four metabolites except phoratoxon sulfoxide. Retention time of standard mixture ranged 1.8 to 16.1 minutes at column temperature programming from 130 to $200^{\circ}C$ at $5^{\circ}C/min$ and detector sensitivity was also very high(0.05 to 1.05ng). Recoveries from soil and vegetables untreated but fortified with phorate and its three major metabolites at 0.05 and 0.5ppm levels were above 90% for phorate, phorate sulfoxide and phorate sulfone while recovery of phoratoxon metabolite was about 84%.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.389-400
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• 2011

A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

• Applied Biological Chemistry
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• v.27 no.3
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• pp.139-145
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• 1984

For the ultimate manufacture of vinegar with watermelon juice, we examined the preliminarily alcoholic fermentation of watermelon juice using Saccharomyces cerevisiae, Saccharomyces cerevisiae var. ellipsoideus and Kluyveromyces fragilis. The juice contained 3.2% total reducing sugar by the Somogyi-Nelson method. Strains of yeast culture, pH, temperature and concentration of sugar in the juice were important factors affecting alcoholic fermentation. Saccharomyces cerevisiae var. ellipsoideus produced 5.3% alcohol from the juice fortified with 12% glucose under the conditions of pH 5.73 and $27^{\circ}C$ for 8 days. Generally, small quantities of various salts and N-sources affected little the alcoholic fermentation of the juice. The sterilization of the juice by autoclaving improved efficiency of fermentation than that by $SO_2$ sterilization. Determination of alcohol was carried out by the gas chromatographic method using Chromosorb W: Carbowax as packing material.

• Korean Journal of Food Science and Technology
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• v.24 no.1
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• pp.82-85
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• 1992

Sterols in mayonnaise were determined by the gas liquid chromatographic(GLC) analysis using two different columns, packed column(silicone SE30) and fused silica capillary column(CBPl). Four kinds of sterol(cholesterol, campesterol, stigmasterol and ${\beta}-sitosterol$) were detected in mayonnaise. The method using capillary column proved to be superior in rapidity, reproducerbility and separability for the determination of sterols. The ranges of concentration of egg york in mayonnaise predicted from cholesterol content using packed and capillary columns were $2.69{\sim}7.11%\;and\;2.42{\sim}6.08%$, respectively. Analyzing the composition of campesterol, stigmasterol and (${\beta}-sitosterol$ in mayonnaise, it could be known that soybean oil and cottonseed oil are commonly used for the manufacture of mayonnaise.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 2003.11a
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• pp.85-88
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• 2003

Polycyclic aromatic hydrocarbons (PARs) are an important group of organic contaminants present in sewage sludge, due to their persistence, toxic, bioaccumulative and long range transfer. These characters make themselves as Persistent Organic Pollutants(POPs) in Long Range Transboundary Air Pollutions convention(LRT AP) of Europe. A method of the gas chromatographic-mass spectrometric (GC-MS) determination of PARs present in sewage sludge was developed and applied to analyzed samples from five sewerage treatment plants (SWTPs), having different treatment types. PARs were extracted from freeze-dried samples by toluene 16 hours in a soxhlet extraction system. The sludge extracts were cleaned-up by an activated silica gel column chromatography. The sum of the 16 US Environmental Protection Agency PARs sewage sludge samples varied from 2.44 to 4.82 ${\mu}g$/g. Concentration of emission carcinogen PARs(PARcarc), such as Benzo(a)anthracene, Benzo(b)fluoranthene, Benzo(k)fluoranthene, Benzo(a)pyrene, Dibenzo(a, h)anthracene and Indeno(1, 2, 3-cd)pyrene ranged from 0.62 to 1.03 ${\mu}g$/g. The total amount of PAHs emission from sewage sludge in Korea was calculated as a top-down approach. PARs and $\sum$PAHcarc from sewage treatment plants had several pathway each by-products. In the ocean dumping, PAHs and $\sum$PAHcarc emissions were 1155.95 kg/year and 5040.32 kg/year. In recycle, PAHs and $\sum$PAHcarc emissions were 98.36 kg/year and 428.87 kg/year. In the landfill, PAHs and $\sum$PAHcarc emissions were 190.40 kg/year and 830.21 kg/year. In the incineration, PAHs and $\sum$PAHcarc emission were 33.10 kg/year and 830.21 kg/year. (In case of incineration, the whole provisions of PARs and $\sum$PAHcarc contained to flowed in sludge was supposed to be exhausted to environment through exhaust after incineration.)

• Journal of Environmental Science International
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• v.15 no.1
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• pp.85-94
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• 2006

The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.