Establishment of Analytical Method for Fenhexamid Residue in Korean Cabbage, Apple, Mandarin and Green Pepper

HPLC를 이용한 배추, 사과, 감귤, 고추 중 살균제 Fenhexamid의 정밀 분석법 확립

  • Lee, Hye-Ri (Department of Agricultural Biotechnology, Seoul National University) ;
  • Riu, Myoung-Joo (Department of Agricultural Biotechnology, Seoul National University) ;
  • Park, Hee-Won (Department of Agricultural Biotechnology, Seoul National University) ;
  • Na, Ye-Rim (Department of Agricultural Biotechnology, Seoul National University) ;
  • Song, Hyuk-Hwan (Department of Agricultural Biotechnology, Seoul National University) ;
  • Keum, Young-Soo (Department of Agricultural Biotechnology, Seoul National University) ;
  • Zhu, Yongzhe (Qingdao Agricultural University) ;
  • Kim, Jeong-Han (Department of Agricultural Biotechnology, Seoul National University)
  • 이혜리 (서울대학교 농생명공학부) ;
  • 류명주 (서울대학교 농생명공학부) ;
  • 박희원 (서울대학교 농생명공학부) ;
  • 나예림 (서울대학교 농생명공학부) ;
  • 송혁환 (서울대학교 농생명공학부) ;
  • 금영수 (서울대학교 농생명공학부) ;
  • ;
  • 김정한 (서울대학교 농생명공학부)
  • Published : 2009.12.31

Abstract

This study was performed to develop a precise single residue analytical method of fungicide fenhexamid in representative crops for general residue analytical method which could be applied to most of crops. Korean cabbage, mandarin, apple and green pepper were selected, macerated, extracted with acetone, concentrated and partitioned with dichloromethane. Then the extracts were concentrated and cleaned-up through Florisil column with ethyl acetate/0.1% acetic acid in hexane [15:85, (v/v)] before concentration and analysis with HPLC. LOQ (Limit of Quantitation) of fenhexamid was 1 ng (S/N>10) and MQL (Method Quantitative Limit) was 0.01 mg/kg. Recoveries were measured at two fortification levels (10 MQL and 50 MQL) on crop samples and ranged from 85.2% to 94.8% (mean recoveries) and coefficients of variation were <10% regardless of sample type.

본 연구는 살균제 fenhexamid의 잔류분석을 대부분의 농작물에 적용할 수 있도록 대표 작물을 이용한 fenhexamid의 단성분 정밀 분석법을 개발하고자 하였다. 대표 작물로는 배추, 감귤, 사과, 고추로 선정하였고, 마쇄한 농작물 시료에 acetone을 가한 후 진탕하여 잔류물을 추출하였다. 추출액을 감압농축 한 뒤, 농축물을 포화식염수와 증류수로 희석하고 dichloromethane으로 분배하였다. 분배액을 농축하고 ethyl acetate/0.1 % acetic acid 함유 hexane 혼합액[15:85, (v/v)]으로 용리하는 Florisil 크로마토그래피법으로 정제한 후 농축한 다음 HPLC로 분석하는 방법을 확립하였다. Fenhexamid의 정량한계(LOQ ; Limit of Quantitation)는 1 ng(S/N>10)이었고, 분석정량한계(MQL ; Method Quantitative Limit)는 0.01 mg/kg이었다. 무처리 시료에 fenhexamid 표준용액을 2수준(10MQL과 50MQL) 3반복으로 처리하여, 확립된 전체 분석과정을 거친 후, 회수율을 산출한 결과는 85.2~94.8%이었으며, 농산물 시료에 관계없이 반복 간 분석오차는 10% 미만이었다.

Keywords

References

  1. Bachmann, J and F. Nublein (1995) Method for the determination of KBR 2738 residues in plant material by HPLC, MR-144/94, Bayer AG, Germany
  2. Cabras, P., A. Angioni, V. L. Garau, F. M. Pirisi, F. Cabitza, M. Pala and G. A. Farris (2001) Fenhexamid residues in grapes and wine. Food Additives and Contaminants 18(7):625-629 https://doi.org/10.1080/02652030110038054
  3. Fong, W. G, H. A. Moye, J. N. Seiber and J. P. Toth (1999) Pesticide Residues in food: Methods, Technologies, and Regulations. Wiley Interscience. pp.3-4, 40-44, Canada
  4. Hengel, M., B. Hung, J. Engerbretson and T. Shibamoto (2003) Analysis of fenhexamid in caneberry, blueberry, and pomegranate by liquid chromatography-tandem mass spectrometry. J. Agric. Food Chem. 51:6635-6639 https://doi.org/10.1021/jf0301403
  5. McNair, H. M. and J. M. Miller (1997) Basic Gas Chromatography. pp.7, 51, Wiley Interscience, U.S.A.
  6. Mercader, J. V. and A. Abad-Fuentes (2009) Monoclonal antibody generation and direct competitive enzyme-linked immunosorbent assay evaluation for the analysis of the fungicide fenhexamid in must and wine. J. Agric. Food Chem. 57:5129-5135 https://doi.org/10.1021/jf900867u
  7. Miller, J. M. (2005) Chromatography : conseps and contrasts (2nd), Wiley Intersciense, pp.286-287, U.S.A.
  8. Rood, Dean (2007) The Troubleshooting and Maintenance Guide for Gas Chromatographyers pp.16-17, p.22, Wiley-VCH, U.S.A.
  9. Rosslenbroich, H. J. and D. Stuebler (2000) Botrytis cinerea -history of chemical control and novel fungicides for its management. Crop Protection 19:557-561 https://doi.org/10.1016/S0261-2194(00)00072-7
  10. Tomlin, C. D. S (2006) The Pesticide Manual (14th), pp.436-437, British Crop Production Council, UK
  11. 김강진, 김하석, 이대운, 이원 (1997) 분석화학 (제4판), pp.698, 자유아카데미
  12. 식품의약품안전청 (2009) 식품의 농약 잔류허용기준
  13. 식품의약품안전청 (2009) 식품공전
  14. 이영득 (2009) 식품공전 잔류농약분석법 실무 해설서 pp.3, 식품의약품안전청
  15. 이종화, 박희원, 금영수, 권찬혁, 이영득, 김정한 (2008) 시설 내 오이 재배 중 살균제 Boscalid의 잔류특성. 농약과학회지 12(1):67-73
  16. (주)랩프런티어 (2004) 식품 중 동시다성분 분석법 개선 연구 pp.89, 114, 187 식품의약품안전청
  17. 한국작물보호협회 (2009) 농약사용지침서, 삼정인쇄공사 pp.310-313
  18. 한성수, 노석초, 김원주, 박필재, 김일광 (2003) 작물(오이, 딸기, 포도) 중 살균제 Fenhexamid의 잔류성에 대한 기체 크로마토그래피 분석. Analytical science & technology 16(1):70-77