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LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발 KCI 등재

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS

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한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)
한국식품위생안전성학회 (Korean Society of Food Hygiene and Safety)
초록

본 연구는 농산물 중 2019년 기준신설 예정농약 Broflanilide에 대한 공정시험법을 개발하고자 수행하였다. Broflanilide는 meta-diamide계 살충제로 중추신경계 억제성 신경전달물질인 gamma-aminobutyric acid (GABA) 수용 가이드라인(2016)’에 적합한 수준임을 확인하였다. 개발된 시험법은 낮은 검출한계 및 정량한계, 우수한 직선성, 회수율 실험을 통한 정확성과 정밀성, 재현성 등이 입증되 어 농산물 중 broflanilide의 잔류검사를 위한 공정시험법 으로 활용되기에 적합한 것으로 판단된다.

An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl (C18). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

목차
ABSTRACT
 Materials and Methods
  시약 및 재료
  표준원액 및 표준용액의 조제
  추출 및 정제
  LC-MS/MS 분석조건
  시험법의 유효성 검증
 Results and Discussion
  최적기기분석조건 확립
  추출 및 정제 조건 확립
  시험법 유효성 검증
  실험실간 시험법 검증
 국문요약
 Reference
저자
  • 박지수(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Ji-Su Park (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 도정아(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Jung-Ah Do (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) Correspondence to
  • 이한솔(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Han Sol Lee (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 박신민(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Shin-min Park (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 조성민(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Sung Min Cho (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 김지영(식품의약품안전처 서울지방식품의약품안전청 수입식품분석과) | Ji-Young Kim (Division of Import Food Analysis, Ministry of Food and Drug Safety-Seoul Region, Ministry of Food and Drug Safety)
  • 신혜선(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Hye-Sun Shin (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 장동은(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Dong Eun Jang (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 정용현(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Yong-hyun Jung (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 이강봉(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Kangbong Lee (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)