Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector

HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립

  • Jang, Jin (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Heejung (Dental and Gastroenterology Devices Division, Department of Medical Device Evaluation, National Institute of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Do, Jung Ah (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Ko, Ah-Young (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Eun Hyang (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Ju, Yunji (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Eunju (Hazardous Substances Analysis Team, Center for Food and Drug Analysis, Gyeongin regional Korea Food and Drug Administration) ;
  • Chang, Moon-Ik (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Rhee, Gyu-Seek (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 장진 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김희정 (식품의약품안전처 식품의약품안전평가원 의료기기심사부 구강소화기기과) ;
  • 도정아 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 고아영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이은향 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 주윤지 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김은주 (경인지방식품의약품안전청 시험분석센터 유해물질분석과) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2016.03.08
  • Accepted : 2016.05.16
  • Published : 2016.06.30
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Abstract

An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

Oxathiapiprolin은 병원균의 포자형성과 효모성장을 저해하여 노균병을 방제하는 piperidinyl thiazole isoxazoline 계열 살균제로 2015년 국내 사용등록이 요청된 신규약제이다. 본 연구에서는 oxathiapiprolin의 신규등록과 관련해 안전관리를 위한 공정시험법 마련이 요구되어 농산물 중 잔류분석법을 개발하였다. 농산물 중 oxathiapiprolin은 acetonitrile로 추출한 뒤 분배효율 향상을 위해 1 N sodium hydroxide (NaOH)를 이용해 염기성으로 조절하여 비해리 상태로 만든 뒤 dichloromethane으로 액액분배하였으며 분배추출액은 silica SPE 카트리지로 정제한 뒤 HPLC-UVD로 분석하였다. 개발된 분석법의 검출한계(LOD) 및 정량한계(LOQ)는 각각 0.003, 0.01 mg/kg이었고, 대표농산물 5종(고추, 감귤, 감자, 대두, 현미) 중 oxathiapiprolin의 평균 회수율은 86.7-112.7%(상대표준편차, $RSD{\leq}10%$)으로 나타났다. 이는 잔류물 분석에 관한 CODEX 가이드라인(CAC/GL 40)을 만족하는 것으로 확인되었다. 따라서 개발된 분석법은 국내외 유통 농산물 중 oxathiapiprolin의 안전평가를 위한 잔류량 적부 판정에 있어 공정시험법으로 사용되기에 적합할 것으로 판단된다.

Keywords

References

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