The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
권호 표지

Determination of Fomesafen Residue in Agricultural Commodities Using HPLC-UVD/MS

HPLC-UVD/MS를 이용한 농산물 중 fomesafen의 분석

  • Lee, Su-Jin (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Hwang, Young-Sun (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Kim, Young-Hak (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Nam, Mi-Young (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Hong, Seung-Beom (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Yun, Won-Kap (Gyeongbuk Institute for Marine Bioindustry) ;
  • Kwon, Chan-Hyeok (National Institute of Food and Drug Evaluation) ;
  • Do, Jung-A (National Institute of Food and Drug Evaluation) ;
  • Im, Moo-Hyeog (Korea Food and Drug Administration) ;
  • Lee, Young-Deuk (Division of Life and Evnironmental Science, Daegu University) ;
  • Choung, Myoung-Gun (Dept. of Herbal Medicine Resource, Kangwon National University)
  • 이수진 (강원대학교 생약자원개발학과) ;
  • 황영선 (강원대학교 생약자원개발학과) ;
  • 김영학 (강원대학교 생약자원개발학과) ;
  • 남미영 (강원대학교 생약자원개발학과) ;
  • 홍승범 (강원대학교 생약자원개발학과) ;
  • 윤원갑 (경북해양바이오산업연구원) ;
  • 권찬혁 (식품의약품안전평가원 화학물질과) ;
  • 도정아 (식품의약품안전평가원 화학물질과) ;
  • 임무혁 (식품의약품안전청 식품기준과) ;
  • 이영득 (대구대학교 생명환경학부) ;
  • 정명근 (강원대학교 생약자원개발학과)
  • Received : 2010.05.03
  • Accepted : 2010.05.17
  • Published : 2010.06.30
Download PDF
⟨ Previous Next ⟩

Abstract

Fomesafen is a selective herbicide, and used to control annual and perennial broad-leaf grass on soybean and fruit fields in USA and China, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of fomesafen were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for fomesafen residue in crops using HPLC-UVD/MS. Fomesafen residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover fomesafen from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The fomesafen was quantitated by HPLC with UVD, using a Shiseido CAPCELL-PAK UG C18 column. The crops were fortified with fomesafen at 3 levels per crop. Mean recovery ratio were ranged from 87.5% for a 0.4 ppm in hulled rice to 102.5% for a 0.4 ppm in apple. The coefficients of variation were ranged from 0.6% for a 2.0 ppm in hulled rice to 7.7% for a 0.04 ppm in green pepper. Quantitative limit of fomesafen was 0.04 mg/kg in representative 5 crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fomesafen in agricultural commodities.

광엽 제초제로 사용되는 fomesafen은 미국 및 중국 등에서 두류 및 과수의 광엽 제초제로 사용되고 있으나, 국내에서는 미사용 농약이며, 잔류허용기준 및 분석법이 확립되어 있지 않다. 최근 FTA 등으로 외국에서 수입되는 농산물 중 fomesafen에 대한 안전성 검토가 필요하나, 국내 식품공전 상에는 fomesafen의 분석법이 확립되어 있지 않다. 본 연구는 HPLC-UVD/MS를 이용하여 농산물 중 fomesafen의 잔류 분석법을 확립하고자 하였으며, 대상 농산물은 현미, 콩, 사과, 배추 및 고추를 선정하였다. 농산물 시료에 acetone을 가하여 추출된 fomesafen 성분을 dichloromethane 액-액 분배법과 Florisil 흡착크로마토그래피법으로 정제하여 HPLC-UVD/MS 분석대상 시료로 하였다. Fomesafen의 정량적 분석을 위한 최적 HPLC 분석 조건을 확립하였으며, 정량한계(LOQ)는 0.04 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10 및 50배 수준에서 회수율을 검토한 결과 모든 처리농도에서 87.5~102.5% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 7.7%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였으며, LC/MS SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 fomesafen의 HPLC-UVD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용가능할 것이다.

Keywords

References

  1. AOAC (2000) 'Pesticide and industrial chemical residues, In Official method of analysis', 17th ed., pp. 1-88, AOAC International, Arlington, VA, USA.
  2. Bolygo, E., and N. C. Atreya (1991) Solid-phase extraction for multi-residue analysis of some trizole pyrimidine pesticides in water. Freseniu's Journal of Analytical Chemistry 339(6): 423-430. https://doi.org/10.1007/BF00322364
  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. Harris, J. R., B. J. Gossett, T R. Murphy, and J. E. Toler (1991) Response of broad leaf weeds and soybeans to the diphenyl ether herbicides. J. Prod. Agric. 4:407-411. https://doi.org/10.2134/jpa1991.0407
  5. Hazardous Substances Data Bank (1998) TOXNET profile from Hazardous Substances Database, No. 6660, Fomesafen.
  6. Kwon, C. H., M. I. Chang, M. H. Im, H. Choi, D. I. Jung, S. C. Lee, J. Y. Yu, Y. D. Lee, J. O. Lee, and M. K. Hong (2008) Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry. Analytical Sci. & Technoligy 21(6):518-525.
  7. Lagana, A., G. Fago, A. Marino, V. M. Penazzi (2000) Liquid chromatography mass spectrometry tandem for multiresidue determination of selected post-emergence herbicides after soil column extraction. Analytica Chimica Acta 415:41-56. https://doi.org/10.1016/S0003-2670(00)00857-6
  8. Lee, J., H. Park, Y. Keum, C. Kwon, Y. Lee, and J. Kim (2008) Dissipation pattern of Boscalid in cucumber under green house condition. Korean Journal of Pesticide Science 12: 67-73.
  9. Miller, J. M. (2005) Chromatography : concepts and contrasts (2nd), Wiley Intersciense, p. 286-287, USA.
  10. Standardization administration of the people's republic of China (2003) GB/T 5009. 130.
  11. Trezzi, M. M., R. A. Vidal, N. D. Kruse, R. P. Silva, M. S. Gustmann, and E. Franchin (2009) Fomesafen absorption site as a mechanism of resistance in an Euphorbia heterophylla biotype resistant to PROTOX inhibitors. Planta Daninha 27(1):139-148. https://doi.org/10.1590/S0100-83582009000100018
  12. United States Environmental Protection Agency (2007) Registration review ecological risk assessment problem formulation for fomesafen. Washington D.C., 20460.
  13. US FDA (1999) 'Pesticide Analytical Manual, Vol 1: Multi residue Methods (3rd ed.)', US Food and Drug Administration, USA.
  14. 박청진, 이영득 (2003) 살균제 boscalod의 포도와 딸기 중 잔류특성. 생명과학연구 2(2):9-16.
  15. 식품의약품안전청 (2009) 식품공전.
  16. 이영득 (2009) 식품공전 잔류농약분석법 실무 해설서, 식품의약품안전청.