Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS

LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증

  • Pak, Won-Min (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug 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) ;
  • Lim, Seung-Hee (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Park, Shin-Min (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Yoon, Ji-Hye (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, Dong-seouk (Korea Advanced Food Research Institute) ;
  • Chang, Moon-Ik (Audit and Inspection Office, Ministry of Food and Drug Safety)
  • 박원민 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 도정아 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 임승희 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 박신민 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 윤지혜 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이동석 (한국식품과학연구원) ;
  • 장문익 (식품의약품안전처 감사담당관)
  • Received : 2017.04.19
  • Accepted : 2017.06.13
  • Published : 2017.08.30
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Abstract

The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

본 연구는 2017년 수입식품 중 신규 기준설정 예정 농약인 tridemorph의 안전성 관리를 위한 공정시험법을 확립하기 위하여 수행하였다. Tridemorph의 잔류물의 정의는 모화합물로 규정하며, 확립된 시험법은 실험실내 및 실험실간 검증을 통해 공정시험법으로의 유효성을 확인하였다. 대표 농산물 5종(감귤, 감자, 고추, 대두, 현미)에 대하여 잔류분석이 가능하도록 선택성과 감도가 우수한 LC-MS/MS를 사용하여 수용성 유기용매인 ACN로 추출 후 $NH_2$ 카트리지에 가장 회수율이 우수한 용매인 MeOH/DCM (1/99, v/v)를 정제조건으로 확립하여 시험법을 개발하였다. 개발된 tridemorph의 직선성은 결정계수($r^2$)가 0.99 이상으로 우수하였으며, 검출한계 및 정량한계는 각각 0.001 및 0.005 mg/kg으로 높은 감도를 나타내었다. 개발된 시험법의 평균 회수율은 75.9~103.7%였으며, 분석오차는 8.5%이하로 정확성 및 재현성이 우수함을 확인할 수 있었다. 또한, 외부기관 검증 결과 평균 회수율은 87.0~109.2%이었으며, 상대표준편차는 모두 7.8% 이하로 조사되어 국제적 잔류농약 분석 가이드라인 및 식품의약품안전평가원 가이드라인에 적합한 수준임을 확인하였다. 따라서 본 시험법은 농산물 중 tridemorph의 잔류검사를 위한 공정시험법으로 활용할 수 있을 것으로 판단된다.

Keywords

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