• Korean Journal of Environmental Agriculture
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• v.26 no.3
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• pp.246-253
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• 2007

This study was performed to enhance the cleanup efficiency of methoxyfenozide and bentazone by pH adjustment in the course of liquid-liquid partition and to develop an optimum analytical conditions using HPLC coupled with DAD for two matrices, brown rice and rice straw. Preparation procedure of brown rice sample was "extraction${\rightarrow}$coagulation${\rightarrow}$liquid-liquid partition$\rightarrow$-florisil C.C", and this procedure was samely applied to two compounds. In rice straw, preparation procedure of methoxyfenozide sample was "extraction$\rightarrow$-alkalization$\rightarrow$liquid-liquid extraction$\rightarrow$coagulation$\rightarrow$florisil C.C", and in the case of bentazone, "extraction$\rightarrow$alkalization$\rightarrow$liquid-liquid partition$\rightarrow$acidification$\rightarrow$liquid-liquid extraction$\rightarrow$florisil C.C". All these purified samples were redissolved in the mobile phases, acetonitile : 20 mM sodium acetate (75:25, v/v) for methoxyfenozide and acetonitrile : 75 mM sodium acetate, pH 6.0 (40:60, v/v) for bentazone. Recoveries of methoxyfenozide analysis in brown rice and rice straw were 83.5-97.4 and 86.4-97.3%, and detection limits were 0.02 and 0.04 mg/kg, respectively. Recoveries of bentazone in brown rice and rice straw were 86.8-101.9 and 88.3-94.5% and detection limits were 0.005 and 0.01 mg/kg, respectively. This methods seem to be usefully applied to the residue analysis of two compounds in the view of producing stable analytical condition and fair reproducibility.

• Korean Journal of Food Science and Technology
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• v.28 no.3
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• pp.421-427
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• 1996

Ethyl carbamate is an animal carcinogen and a suspected human carcinogen found in fermented foods and beverages. For the determination of ethyl carbamate in typical Korean diet, an analytical method was established for the food as complex as Kimchi. Kimchi samples collected from various locations in the country were homogenized and extracted four times with ethyl acelate. Following concentration and reconstitution with water, the extract was loaded onto $C_{18}$ column. Fraction containing ethyl carbamate was eluted with methanol, while most of the red pigment of the sample was retained on the column. The eluent was further purified with alumina, followed by Florisil column. The final eluent was analyzed by gas chromatography mass spectrometry in the selected ion monitoring mode. None of the twenty Kimchi samples showed ethyl carbamate level higher than 4.6 ppb without correction for the recovery. The concentration of ethyl carbamate in Kimchi increased as pH decreased, suggesting fermentation dependent formation of ethyl carbamate.

• Korean Journal of Food Science and Technology
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• v.31 no.2
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• pp.301-307
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• 1999

When fats are irradiated, hydrocarbons contained one or two fewer carbon atoms are formed from the parent fatty acids. A method to detect radiation-induced hydrocarbons consists of the extraction of fat from beef, pork and chicken, separation of hydrocarbons with a florisil column and identification of GC/MS methods. When beef, pork and chicken were irradiated, pentadecane, 1-tetradecene, heptadecane, 1-hexadecene, 8-heptadecene, 1,7-hexadecadiene, 6,9-heptadecadiene and 1,7,10-hexadecatriene were formed from palmitic, stearic, oleic and linoleic acids. Concentrations of the produced hydrocarbons tended to increase linearly with the dose levels of irradiation. Concentrations of hydrocarbons produced by ${\gamma}-irradiation$ depended upon the composition of fatty acids in beef, pork and chicken. The major hydrocarbons in irradiated beef, pork and chicken were 1,7-hexadecadiene and 8-heptadecene originating from oleic acid. 1,7-Hexadecadiene was the highest amount in irradiated beef, pork and chicken.

• Horticultural Science & Technology
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• v.34 no.1
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• pp.183-194
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• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 1997.10a
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• pp.37-39
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• 1997

Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

• Korean Journal of Pharmacognosy
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• v.12 no.4
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• pp.211-214
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• 1981

Solanesol has been isolated from aged Korean native tobacco leaf(Hyangcho and Sohyang) by water pretreatment, hexane extraction and column chromatography on Florisil in yields of 0.41% and 0.31% dry wt., respectively. Thin-layer densitometric analysis of the hexane extracts of samples(Hyangcho Sohyang) has shown that the amounts of solanesol present are 0.74% and 0.52% dry wt., respectively.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.185-194
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• 2015

This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

• Journal of the Korean Chemical Society
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• v.29 no.5
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• pp.496-502
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• 1985

The solvent extraction and cleanup processes for the simultaneous gas-liquid cliromatographic determination of 16 kinds of organochlorine pesticide residues were investigated. The pesticides were extracted out from-various crops with the aqueous acetone solution acidified (pH < 1.5) by adding conc. $H_3PO_4$. Most of the pesticides were partitioned from the solution with petroleum ether. Evaporated the extracting solvent, the residues were dissolved in ethylether-petroleum ether (6 : 94) eluent and eluted through the Florisil column activated at 650$^{\circ}$C for 2.5hrs. The extraction efficiency was over 94% and impurities were effectively removed by the column chromatography.

• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.117-124
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• 2018

BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

• Journal of the Korean Society of Food Science and Nutrition
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• v.33 no.1
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• pp.158-163
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• 2004

We investigated the usefulness of 2-alkylcyclobutanones as markers for irradiated eggs and egg products by comparing 2-alkylcyclobutanone concentrations in irradiated raw egg yolk, boiled egg yolk, and egg yolk powder. One method of detection radiation-induced 2-alkylcyclobutanones involves extraction fat from irradiated egg samples separating 2-alkylcyclobutanones by florisil column chromatography, and identifying GC/MS. 2-(5'-Tetradecenyl)cyclobutanone of 2-alkylcyclobutanones was high relatively in boiled egg yolk, but 2-dodecylcyclobutanone was high in raw egg yolk and egg yolk Powder. Concentrations of the radiation-induced 2-alkylcyclobutanones increased linearly with the irradiation dose. The radiation-induced 2-alkylcyclobutanones from egg samples at 0.5 kGy over and not detected at the non-irradiated samples. Therefore, these compounds could be used as marker of Post-irradiation for egg Products.