HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 분석
Determination of Oxycarboxin Residues in Agricultural Commodities Using HPLC-UVD/MS
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BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-Nphenyl- 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 C18 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.
Abstract
BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-Nphenyl- 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 C18 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.
참고문헌 (10)
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