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Determination of Oxycarboxin Residues in Agricultural Commodities Using HPLC-UVD/MS

HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 분석

  • Choung, Myoung-Gun (Department of Herbal Medicine Resource, College of Health Science, Kangwon National University)
  • 정명근 (강원대학교 생약자원개발학과)
  • Received : 2018.04.18
  • Accepted : 2018.06.23
  • Published : 2018.06.30

Abstract

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.

본 연구에서는 HPLC-UVD/MS를 이용하여 농산물 중 oxanthiin 살균제인 oxycarboxin의 잔류 분석법을 확립하였다. 대표 농산물은 현미, 콩, 배추, 고추 및 사과를 선정하였고 acetone을 가하여 추출된 oxycarboxin 성분을 dichloromethane 액-액 분배법과 Florisil 흡착크로마토그래피법으로 정제하여 HPLC-UVD/MS 분석대상 시료로 사용하였다. Oxycarboxin의 정량적 분석을 위한 최적 분석 조건을 확립하였으며, 정량한계(LOQ)는 0.04 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과 모든 처리농도에서 78.3~96.1% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 4.7%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였으며, LC/MS SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 oxycarboxin의 HPLC-UVD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

Keywords

Acknowledgement

Supported by : Ministry of Food and Drug Safety

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