Development of Analytical Method and Monitoring for Bifenazate in Commercial Agricultural Products

농산물 중 Bifenazate의 분석법 개선 및 모니터링

  • Park, Eun-Heui (Gwangju Regional Korea Food and Drug Administration) ;
  • Go, Myoung-Jin (Gwangju Regional Korea Food and Drug Administration) ;
  • Cho, Myong-Shik (Gwangju Regional Korea Food and Drug Administration) ;
  • Kim, Young-Sun (Seoul Regional Korea Food and Drug Administration) ;
  • Lee, Jin-Ha (Gwangju Regional Korea Food and Drug Administration) ;
  • Choi, Dong-Mi (Gwangju Regional Korea Food and Drug Administration)
  • 박은희 (광주지방식품의약품안전청) ;
  • 고명진 (광주지방식품의약품안전청) ;
  • 조명식 (광주지방식품의약품안전청) ;
  • 김영선 (서울지방식품의약품안전청) ;
  • 이진하 (광주지방식품의약품안전청) ;
  • 최동미 (광주지방식품의약품안전청)
  • Received : 2010.01.28
  • Accepted : 2010.02.12
  • Published : 2010.03.31

Abstract

The analytical method for bifenazate was developed using a HPLC (UVD). Also, analytical condition of LC/MS was set up for bifenazate. We validated the method for the precision and the reproducibility. The correlation coefficient of bifenazate ranged from 0.05 to 2.5 mg/kg was 1.0. Limit of quantitation (LOQ) was 0.01 mg/kg. To measure recoveries from agricultural products such as foxtail millet (cereal grains), kidney bean (beans), orange (fruits), perilla leaves (vegetables) and oak mushroom (mushrooms), bifenazate was spiked. Mean recoveries of bifenazate for each sample were 82.7~104.1% at the level of 0.1 mg/kg and 73.1~104.3% at the level of 0.5 mg/kg. The relative standard deviations (n=3) were 0.2~9.7%. Pesticide residues for bifenazate were investigated in 16 commodities (rice, foxtail millet, buckwheat, kidney bean, peanut, sesame, orange, grapefruit, kiwifruit, spinach, perilla leaves, leek, garlic stem, garlic, ginger and oak mushroom) collected from 22 provinces in 2009. Bifenazate was analyzed using analytical method by HPLC from 304 samples, and residue was not detected.

농산물 중 bifenazate의 잔류 실태를 조사하기 위하여 HPLC를 사용한 분석법을 개선하였고, LC/MS 분석법을 확립하였다. 개선된 분석법에 대한 직선성과 재현성에 대한 검증을 수행한 결과 bifenazate 0.05~2.5 mg/kg 범위에서 상관계수는 1.0이었고, 정량한계(LOQ)는 0.01 mg/kg이었다. 회수율은 현미(곡류), 강낭콩(콩류), 오렌지(과실류), 들깻잎(채소류), 표고버섯(버섯류)에 대해 0.1 mg/kg 수준에서 82.7~104.1%였고, 0.5 mg/kg에서는 73.1~104.3%였다. 또한 회수율에 대한 상대표준편차(n=3)는 0.2~9.7%였다. 전국 22개 지역에서 수거한 농산물 16품목(쌀, 조, 메밀, 강낭콩, 땅콩, 참깨, 오렌지, 자몽, 키위, 시금치, 들깻잎, 부추, 마늘쫑, 마늘, 생강, 표고버섯) 304건을 대상으로 bifenazate의 잔류량을 조사한 결과 모든 농산물에서 검출되지 않았다.

Keywords

References

  1. Alder L, Greulich K, Kempe G, Vieth B. Residue analysis of 500 High Priority Pesticides: Better by GC-MS or LC-MS/ MS. Mass Spectrometry Reviews., 25, 838-865 (2006). https://doi.org/10.1002/mas.20091
  2. Codex Alimentarius Commission. Pesticide Residues in Food.Available from: http:www.codex alimentarius.net/mrls/pesticides. Accessed Oct. 15, 2009.
  3. European Commission, Monitoring of Pesticide Residues in Products of Plant Origin in the European Union, Norway and Iceland and Liechtenstein 2001 Report, SANCO/20/03 final (2003).
  4. European Commission, Monitoring of Pesticide Residues in Products of Plant Origin in the European Union, Norway and Iceland and Liechtenstein 2002 Report, SANCO/17/04 final (2004).
  5. European Commission, Monitoring of Pesticide Residues in Products of Plant Origin in the European Union, Norway and Iceland and Liechtenstein 2003 Report (2005).
  6. European Commission, Monitoring of Pesticide Residues in Products of Plant Origin in the European Union, Norway and Iceland and Liechtenstein 2004 Report (2006).
  7. European Commission, Monitoring of Pesticide Residues in Products of Plant Origin in the European Union, Norway and Iceland and Liechtenstein 2005 Report (2007).
  8. European Commission, Monitoring of Pesticide Residues in Products of Plant Origin in the European Union, Norway and Iceland and Liechtenstein 2006 Report (2008).
  9. EFSA Scientific Report, 2007 Annual Report on Pesticide Residues according to Article 32 of Regulation (EC) No 396/ 20051 Prepared by Pesticides Unit (PRAPeR) of EFSA, (Question No EFSA-Q-2008-714), Issued on 10 June 2009.
  10. Hengel, M. J., Miller, M. : Analysis of Flonicamid and Its Metabolites in Dried Hops by Liquid Chromatography-Tandem Mass Spectrometry, J. Agric. Food Chem., 55, 8033-8039 (2007). https://doi.org/10.1021/jf0719297
  11. Korea Food and Drug Administration, MRLs fo Pesticides in Foods. 11-1470000-001707-14: 110. KFDA, Seoul, Korea (2008).
  12. Li Bo, Deng Xiaojun, Guo Dehua, Jin Shuping: Determination of glyphosate and aminomethylphosphonic acid residues in foods using high performance liquid chromatography-mass spectromethy/mass spectrometry, Chinese J.Chromatography, 15, 486-490, (2007).
  13. Matt J. Hengel, Marion Miller : Analysis Pesticides in Dried Hops by Liquid Chromatography-Tandem Mass Spectrometry, J. Agric. Food Chem., 56, 6851-6856 (2008). https://doi.org/10.1021/jf8009624
  14. The Japan Food Chemical Research Foundation. MRLs for Pesticides in Food Available from: http://www.ffcr.or.jp. Accessed Aug. 20, 2009.
  15. U.S. Food and Drug Administration, Food and Drug Administration Pesticide Program Residue Monitoring 2002 (2004).
  16. U.S. Food and Drug Administration, Food and Drug Administration Pesticide Program Residue Monitoring 2003 (2005).
  17. U.S. Food and Drug Administration, Food and Drug Administration Pesticide Program, Residue Monitoring 2004-2006 (2008).
  18. U.S. Food and Drug Administration, Food and Drug Administration Pesticide Program, Residue Monitoring 2007 (2009).
  19. 박주황, 김택겸, 오창환, 김정한, 이영득, 김장억 : Gas-Liquid Chromatography를 이용한 사과 및 배 중의 농약 다성분 잔류분석법, 한국환경농학회지, 23, 148-157 (2004).
  20. 식품의약품안전청, 식품의약품안전청연구보고서, (2005).
  21. 식품의약품안전청, 식품의약품안전청연구보고서, (2006).
  22. 식품의약품안전청, 식품의약품안전청연구보고서, (2007).
  23. 식품의약품안전청, 식품의약품안전청연구보고서, (2008).
  24. 일본식품위생협회, 후생노동성 생활위생국 식품화학관련, 식품 중 잔류농약 (1999).
  25. 최재원, 문부식 : 고분해능 질량분석장치를 이용한 동시분석법 1. 수계의 유기인계 농약-II, 한국환경분석학회지, 11, 55-65 (2008).