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수출입 원예작물의 검역을 위한 살균제 Fluazinam의 공정 잔류분석법 개발

Development of an Official Method for Measurement of Fluazinam Residues for Quarantine of Imported and Exported Horticultural Products

  • 김경하 (강원대학교 생약자원개발학과) ;
  • 안경근 (강원대학교 생약자원개발학과) ;
  • 김기쁨 (강원대학교 생약자원개발학과) ;
  • 황영선 (강원대학교 생약자원개발학과) ;
  • 장문익 (식품의약품안전평가원 잔류물질과) ;
  • 강인규 (경북대학교 원예과학과) ;
  • 이영득 (대구대학교 생명환경학부) ;
  • 정명근 (강원대학교 생약자원개발학과)
  • Kim, Gyeong-Ha (Department of Herbal Medicine Resource, Kangwon National University) ;
  • Ahn, Kyung-Geun (Department of Herbal Medicine Resource, Kangwon National University) ;
  • Kim, Gi-Ppeum (Department of Herbal Medicine Resource, Kangwon National University) ;
  • Hwang, Young-Sun (Department of Herbal Medicine Resource, Kangwon National University) ;
  • Chang, Moon-Ik (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kang, In-Kyu (Department of Horticultural Science, Kyungpook National University) ;
  • Lee, Young Deuk (Division of Life and Environmental Science, Daegu University) ;
  • Choung, Myoung-Gun (Department of Herbal Medicine Resource, Kangwon National University)
  • 투고 : 2015.08.25
  • 심사 : 2016.01.25
  • 발행 : 2016.02.29

초록

본 연구는 국내 및 수출입 원예작물의 일상적 잔류농약 검사에 활용 가능한 dinitroaniline계 광범위 살균제 fluazinam의 GC-ECD/MS 잔류 분석법을 확립하고자 하였다. 원예작물 중 채소류에서는 청양고추와 결구배추를, 과일류에서는 감귤과 사과를 대표 시료로 선정하였고, 아세톤으로 추출된 fluazinam은 식염수로 희석하고, 수용액층을 n-hexane 액-액 분배법으로 회수하였으며, 회수된 추출액으로부터 fluazinam의 최종적 정제를 위하여 florisil 칼럼 크로마토그래피법으로 추가 정제하여 GC-ECD/MS 분석용 시료로 사용하였다. Fluazinam의 정량적 분석을 위하여 DB-17 capillary column을 적용한 GC-ECD 분석 조건을 확립하였으며, 각 작물별 4수준의 농도로 fluazinam을 인위 첨가하여 회수율을 분석하였다. 각 대표 원예작물에 대해 정량한계, 정량한계의 10, 50, 및 100배 수준에서 회수율을 검토한 결과 모든 처리농도에서 82.5-99.9% 수준을 나타내었으며, 정량한계(LOQ)는 $0.004mg{\cdot}kg^{-1}$이었다. 반복 간 변이계수(CV)는 최대 6.6%를 나타내어 국제적 잔류분석 기준인 회수율 70-120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였다. 또한 GC/MS SIM을 이용하여 실제 각 작물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 fluazinam의 GC-ECD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로서 국내 및 수출입 검역을 위한 원예작물의 공정 잔류분석법으로 사용 가능할 것이다.

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

키워드

참고문헌

  1. Ahn, K.G., G.H. Kim, G.P. Kim, Y.S. Hwang, S.B. Hong, Y.D. Lee, and M.G. Choung. 2015. Determination of quintozene residues in agricultural commodities using GC-ECD/MS. Korean J. Pestic. Sci. 19:195-203. https://doi.org/10.7585/kjps.2015.19.3.195
  2. AOAC. 2000. Pesticide and industrial chemical residues, In official method of analysis. 17th ed. Arlington, VA, USA. p. 88.
  3. Codex Alimentarius Commission. 2003. Guidelines on good laboratory practice in residue analysis. CAC/GL 40-1993. Rev.1-2003. Rome. Italy.
  4. Fong, W.G., H.A. Moye, J.N. Seiber, and J.P. Toth. 1999. Pesticide residues in food: methods, techniques, and regulations. John Wiley and Sons, NY, USA.
  5. Guo, Z., H. Miyoshi, T. Komyoji, T. Haga, and T. Fujita. 1991. Uncoupling activity of a newly developed fungicide, fluazinam[3-chloroN-(3-chloro-2,6-dinitro-4-trifluoromethylphenyl)-5-trifluoromethyl-2-pyridinamine]. Biochim. Biophys. Acta, Bioenerg. 1056:89-92. https://doi.org/10.1016/S0005-2728(05)80077-5
  6. Hu, W, S.J. Lee, and J.E. Kim. 1997. Adsorption-desorption, leaching, and degradation pattern of fungicide fluazinam in the soil environment. J. Korean Soc. Agric. Chem. Biotechnol. 40:128-133.
  7. Jang, M.R., H.K. Moon, T.R. Kim, D.H. Yuk, J.H. Kim, and S.G. Park. 2010. Dietary risk assessment for pesticide residues of vegetable Seoul Korea. Korean J. Nutr. 43:404-412. https://doi.org/10.4163/kjn.2010.43.4.404
  8. Kim, M.O., H.S. Hwang, M.S. Lim, J.E. Hong, S.S. Kim, J.A. Do, D.M. Choi, and D.H. Cho. 2010. Monitoring of residual pesticides in agricultural products by LC/MS/MS. Korean J. Food Sci. Technol. 42:664-675.
  9. Kim, H.Y., S.H. Yoon, H.J. Park, H.J. Lee, I.S. Gwak, H.S. Moon, M.H Song, Y.M. Jang, M.S. Lee, J.S. Park, and K.H. Lee. 2007. Monitoring of residual pesticides in commercial agricultural products in Korea. Korean J. Food Sci. Technol. 39:237-245.
  10. Korea Crop Protection Association. 2015. Using guideline of crop protection agents. Korea. p. 378.
  11. Lee, J.H., H.W. Park, Y.S. Keum, C.H. Kwon, Y.D. Lee, and J.H. Kim. 2008. Dissipation pattern of boscalid in cucumber under greenhouse condition. Korean J. Pestic. Sci. 12:67-73.
  12. Lee, S.J., Y.H. Kim, L.S. Song, and M.G. Choung. 2011. Determination of ametryn residue in agricultural commodities using HPLC-UVD/MS. Korean J. Pestic. Sci. 15:125-133.
  13. Lee, S.J., Y.S. Hwang, Y.H. Kim, M.Y. Nam, S.B. Hong, W.K. Yun, C.H. Kwon, J.A. Do, M.H. Im, Y.D. Lee, and M.G. Choung. 2010. Determination of fomesafen residue in agricultural commodities using HPLC-UVD/MS. Korean J. Pestic. Sci. 14:95-103.
  14. Lee, Y.D. 2012. Pesticide Analytical Residues Manual in Food Code. MFDS.
  15. Miller, J.M. 2005. Chromatography : Concepts and Contrasts. 2nd ed. Wiley Interscience, USA. p. 286.
  16. Ministry of Food and Drug Safety 2012. Korea Food Code. Korea. p. 10-4-340.
  17. Ministry of Food and Drug Safety 2012. Korea Food Code. Korea. p. 10-4-9.
  18. Ministry of Food and Drug Safety 2014. MRLs for Pesticides in Foods. Korea. p. 100.
  19. Krieger, R. 2001. Handbook of pesticide toxicology, Vol.2 Set: principles and agents. Academic press, USA. p. 1243.
  20. Ulrich, S., J. Peter, and W. Matthias. 2012. Modern crop protection compounds: herbicides. John Wiley & Sons, Germany. p. 662.
  21. United States Environmental Protection Agency. 2001. Pesticide fact sheet for fluazinam. Washington D.C., USA.