한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)

  • 제37권6호
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  • Pages.373-384
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  • 2022
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  • 1229-1153(pISSN)
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  • 2465-9223(eISSN)
한국식품위생안전성학회 (The Korean Society of Food Hygiene and Safety)
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농산물 중 살균제 Fluoxastrobin의 시험법 개발 및 유효성 검증

Development and Validation of an Analytical Method for Fungicide Fluoxastrobin Determination in Agricultural Products

  • 이소은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이수정 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 구선영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 박채영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 신혜선 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 강성은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이정미 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정윤미 (식품의약품안전처 광주지방식품의약품안전청 유해물질분석과) ;
  • 장귀현 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 문귀임 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • So Eun, 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) ;
  • Su Jung, 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) ;
  • Sun Young, Gu (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chae Young, 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) ;
  • 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) ;
  • Sung Eun, Kang (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Jung Mi, 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) ;
  • Yun Mi, Chung (Hazardous Substances Analysis Division, Gwangju Regional Food and Drug Administration) ;
  • Gui Hyun, 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) ;
  • Guiim, Moon (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 투고 : 2022.08.29
  • 심사 : 2022.10.28
  • 발행 : 2022.12.30
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초록

플루옥사스트로빈은 Strobilurus 속의 버섯에서 추출한 천연물을 기반으로 개발된 살균제로서 곰팡이성 질병 방제에 효과적이다. 잔류물의 정의는 유럽(EU), 미국(EPA), 일본(JFCRF)에서는 플루옥사스트로빈과 플루옥사스트로빈 Z 이성질체의 합으로 정의하고 있으며, 감자, 대두 등 90품목에 대하여 0.01-60 mg/kg으로 잔류허용기준이 설정되어 있다. 코덱스(CODEX)와 국내에는 잔류허용기준이 설정되어 있지 않음에 따라 본 연구에서는 추후 국내·외 수입 및 재배 농산물 중 플루옥사스트로빈에 대한 잔류허용기준 준수 여부 확인을 위한 시험법을 개발하고자 하였다. 전처리 과정은 플루옥사스트로빈의 물리·화학적 특성을 고려하여 QuEChERS법을 이용한 추출 및 정제방법으로 최적화하였으며, LC-MS/MS를 이용하여 시험법을 개발하였다. 추출 용매는 아세토니트릴로 하고, MgSO4 및 PSA를 이용하여 정제과정을 확립하였다. 대표 농산물 5종에 대해 0.01, 0.1 및 0.5 mg/kg의 처리농도로 실험을 진행한 결과, 플루옥사스트로빈 및 플루옥사스트로빈 Z 이성질체의 결정계수(R2)는 0.998 이상이고 플루옥사스트로빈의 평균 회수율(n=5)은 75.5-100.3%, 플루옥사스트로빈 Z 이성질체는 75.0-103.9%이었다. 상대표준편차는 플루옥사스트로빈이 5.5% 이하, 플루옥사스트로빈 Z 이성질체가 4.3% 이하로 확인되었다. 또한 시험법의 유효성을 확인하기 위해 외부 실험기관인 광주지방식품의약품안전청과의 실험실간 검증을 진행하였으며, 검증 결과 두 실험실간의 회수율은 플루옥사스트로빈의 경우 80.3-101.4%, 플루옥사스트로빈 Z 이성질체는 80.2-105.0%이었고, 상대표준편차는 모두 18.1% 이하로 정확성 및 재현성이 우수함을 확인할 수 있었다. 따라서 본 연구 결과는 CODEX 가이드라인(CAC/GL 40-1993, 2003) 및 식품의약품안전평가원의 가이드라인(MFDS, 2016)에 만족함에 따라 공정시험법으로 활용 가능할 것이다.

Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO4 and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R2) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

키워드

과제정보

본 연구는 2022년도 식품의약품안전평가원 "2022년 식품 중 잔류농약 안전관리를 위한 위해평가 및 신규 시험법 확립 연구(22191농축산316)"의 연구개발비 지원에 의해 수행되었으며, 이에 감사드립니다.

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