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 Benzovindiflupyr in Agricultural Commodities Using LC-MS/MS

LC-MS/MS를 이용한 농산물 중 살균제 벤조빈디플루피르의 잔류시험법 개발 및 검증

  • Lim, Seung-Hee (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Do, Jung-Ah (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Park, Shin-Min (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Pak, Won-Min (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Yoon, Ji Hye (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Ji Young (Import Food Analysis Division, Seoul Regional Food and Drug Administration) ;
  • Chang, Moon-Ik (Audit and Inspection Office, Ministry of Food and Drug Safety)
  • 임승희 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 도정아 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 박신민 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 박원민 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 윤지혜 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김지영 (서울지방식품의약품안전청 수입식품분석과) ;
  • 장문익 (식품의약품안전처 감사담당관실)
  • Received : 2017.04.25
  • Accepted : 2017.07.04
  • Published : 2017.08.30
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Abstract

Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.

벤조빈디플루피르는 곡류, 두류 등 작물의 녹병(rust) 방제에 사용되는 pyrazole carboxamide계 신규 살균제로 국내에서는 2016년 대두와 밀에 대하여 잔류허용기준(Maximum Residue Limit, MRL)이 최초 신설되었다. 따라서 본 연구에서는 기준신설에 따른 농산물 중 이를 분석하기 위한 공정시험법을 개발하였다. 벤조빈디플루피르의 잔류물의 정의는 모화합물로, 벤조빈디플루피르의 물리화학적 특성을 고려하여 이를 검체에서 효율적으로 추출하기 위한 추출조건, 불순물을 효과적으로 정제하기 위한 액-액 분배조건과 정제조건을 확립하였다. 개발된 시험법의 검출한계, 정량한계, 선택성, 직선성, 및 회수율에 대한 검증을 통해 공정시험법으로 유효성을 입증하기 위해 실험실내 및 실험실간 검증을 수행 한 결과 회수율은 79.3~110.0%였고, 분석오차는 9.1% 이하이며, 실험실간 검증 결과는 83.4~117.3%, 변이계수(CV)는 9.0%로 나타났다. 본 연구결과는 CODEX 가이드라인(CAC/GL 40)과 식품의약품안전평가원의 가이드라인(2016)에 만족하는 것으로 확인되었으므로 농산물 중 벤조빈디플루피르의 잔류검사를 위한 공정시험법으로 사용되기에 적합할 것으로 판단된다.

Keywords

References

  1. Walter, H., Gribkov, D., Tobler, H.: Abstracts of Papers, 248th. ACS National Meeting & Exposition, San Francisco, CA, United States, 10-14 AGRO-621 (2014).
  2. Walter, H., Guicherit, E., Rambach-Jankowski, O., Dale, S.: Abstracts of Papers, 248th. ACS National Meeting % Exposition, San Francisco, CA, United States, 10-14 AGRO-730 (2014).
  3. CODEX, Pesticide Residue in Food and Feed. Available from http://www.fao.org/fao-sho-codexalimentarius/standards/pestres/pesticide/en Assessed (2015).
  4. EPA, United states Environmental Protection Agency. Benzovindiflupyr; Pesticide Tolerances. Federal Register, 80, 59627-59634 (2015).
  5. EU, European Commission. Amending Annexes II and III to Regulation (EC) No 396/2005 of the European Parliament and of the Council as regards maximum residue levels for abamectin, acequinocyl, acetamiprid, benzovindiflupyr, bromoxynil fludioxonil, fluopicolide, fosetyl, mepiquat, proquinazid, propamocarb, prohexadione and tebuconazole in or on certain products. Official Journal of the European Union, 24, 46-103 (2016).
  6. Health Canada: Benzovindiflupyr. PMRL (Proposed Maximum Residue Limit), 1-3 (2015).
  7. MFDS.: Ministry of Food an Drug Safety, Cheongju, Korea (2016).
  8. CAC (Codex Alimentarius Commission). Guidelines on good laboratory practice in residue analysis, CAC/GL 40-1993, Rome, Italy (2003).
  9. National Institute of Food and Drug Safety Evaluation: Guidelines on standard procedures for preparing analysis methods. Cheongju, Korea (2016).
  10. Pizzutti I.R., Kok A.D., Hiemstra M., Wickert C., and Prestes O.D.: Method validation and comparison of acetonitrile and acetone extraction for the analysis of 169 pesticides in soya grain by liquid chromatography-teandem mass spectrometry. J. Chromatogr. A., 1216, 4539-4552 (2009). https://doi.org/10.1016/j.chroma.2009.03.064
  11. Kown C.H., Chang M.I., Im M.H., Choi H., Jung D.I., Lee S.C., Yu J.Y., Lee Y.D., Lee J.O., and Hong M.K.: Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry. J. Anal. Sci. Technol., 21, 518-525 (2008).
  12. Lee YD.: Practical book of Korea Food Code pesticide residue analysis method, 4th ed. MFDS, Cheongju, Korea, 78-79 (2013).
  13. US FDA: Pesticide Analytical Manual, Multiresidue Methods, 3rd ed. US Food and Drug Administration, U.S.A. (1999).
  14. AOAC: Pesticide and industrial chemical residues, In Official method of analysis, 17th ed. AOAC International, Arlington, VA, USA. (2000).