The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
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Development of Analytical Method for Fenoxycarb, Pyriproxyfen and Methoprene Residues in Agricultural Commodities Using HPLC-UVD/MS

HPLC-UVD/MS를 이용한 농산물 중 fenoxycarb, pyriproxyfen 및 methoprene의 분석법 확립

  • Lee, Su-Jin (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Kim, Young-Hak (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Song, Lee-Seul (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Hwang, Yong-Sun (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Lim, Jung-Dae (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Sohn, Eun-Hwa (Dept. of Herbal Medicine Resource, Kangwon National University) ;
  • Im, Moo-Hyeog (Food Standard Division, Korea Food and Drug Administration) ;
  • Do, Jung-Ah (Food Chemical Residues Division, National Institution of Food and Drug Safety Evaluation) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, National Institution of Food and Drug Safety Evaluation) ;
  • Kwon, Ki-Sung (Food Chemical Residues Division, National Institution of Food and Drug Safety Evaluation) ;
  • Lee, Joong-Keun (Korea Health Industry Development Institute) ;
  • Lee, Young-Deuk (Division of Life and Environmental Science, Daegu University) ;
  • Choung, Myoung-Gun (Dept. of Herbal Medicine Resource, Kangwon National University)
  • 이수진 (강원대학교 생약자원개발학과) ;
  • 김영학 (강원대학교 생약자원개발학과) ;
  • 송이슬 (강원대학교 생약자원개발학과) ;
  • 황영선 (강원대학교 생약자원개발학과) ;
  • 임정대 (강원대학교 생약자원개발학과) ;
  • 손은화 (강원대학교 생약자원개발학과) ;
  • 임무혁 (식품의약품안전청 식품기준과) ;
  • 도정아 (식품의약품안전평가원 화학물질과) ;
  • 오재호 (식품의약품안전평가원 화학물질과) ;
  • 권기성 (식품의약품안전평가원 화학물질과) ;
  • 이중근 (한국보건산업진흥원) ;
  • 이영득 (대구대학교 생명환경학부) ;
  • 정명근 (강원대학교 생약자원개발학과)
  • Received : 2011.09.14
  • Accepted : 2011.09.23
  • Published : 2011.09.30
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Abstract

Fenoxycarb, pyriproxyfen and methoprene are juvenile hormone mimic insecticide. These insecticides have been widely used for mosquito, fly, scale insects, and Lepidoptera. The purpose of this study was to develop a simultaneous determination procedure of fenoxycarb, pyriproxyfen and methoprene residues in crops using HPLC-UVD/MS. These insecticide residues were extracted with acetone from representative samples of four raw products which comprised brown rice, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and then n-hexane/dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The analytes were quantitated by HPLC-UVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at 3 levels per crop. Mean recovery ratios were ranged from 80.0 to 104.3% in four representative agricultural commodities. The coefficients of variation were less than 4.8%. Quantitative limit of fenoxycarb, pyriproxyfen, and methoprene was 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of fenoxycarb, pyriproxyfen and methoprene in the agricultural commodities.

HPLC-UVD/MS를 이용하여 농산물 시료에서 JH mimic 살충제인 fenoxycarb, pyriproxyfen 및 methoprene의 잔류 분석법을 확립하였다. 농산물 시료에 acetone을 가하여 추출된 fenoxycarb, pyriproxyfen 및 methoprene의 잔류분은 n-hexane/dichloromethane 분배법과 florisil 흡착 크로마토그래피법으로 정제하여 분석대상 시료로 하였다. $C_{18}$ 칼럼을 이용한 HPLC 분석 시 불순물의 간섭은 없었으며, 대표 농산물 중 fenoxycarb, pyriproxyfen 및 methoprene의 정량한계(LOQ)는 0.04 mg/kg이었다. 전체 농산물에 대한 회수율은 80.0~104.3%였으며, 농산물 시료 및 처리수준에 관계없이 10%미만의 분석오차를 나타내어 잔류분석 기준이내를 만족하였다. 본 연구에서 확립한 fenoxycarb, pyriproxyfen 및 methoprlene의 잔류분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족할 뿐만 아니라, LC/MS SIM을 이용한 잔류분의 재확인과정 및 회수율 검증의 결과를 총괄해 볼 때 분석과정의 편이성 및 신뢰성이 확보된 공정분석으로 사용이 가능 할 것으로 판단된다.

Keywords

Acknowledgement

Supported by : 식품의약품안전청

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