The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
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Determination of Pyribencarb and Its Metabolite KIE-9749 in Agricultural Commodities by High-Performance Liquid Chromatography

액체크로마토그래피를 이용한 농산물중 pyribencarb와 대사물 KIE-9749의 잔류 분석법

  • Kwon, Hyeyoung (Chemical Safety Division, National Institute of Agricultural Sciences, Rural Development Administration) ;
  • Hong, Su-Myeong (Chemical Safety Division, National Institute of Agricultural Sciences, Rural Development Administration) ;
  • Kim, Taek-Kyum (Chemical Safety Division, National Institute of Agricultural Sciences, Rural Development Administration) ;
  • Kim, Hyung-Jin (Chemical Safety Division, National Institute of Agricultural Sciences, Rural Development Administration) ;
  • Moon, Byeong-Chul (Chemical Safety Division, National Institute of Agricultural Sciences, Rural Development Administration) ;
  • Kyung, Kee-Sung (Department of Environmental and Biological Chemistry, College of Agricultural Life and Environmental Sciences, Chungbuk National University)
  • 권혜영 (농촌진흥청 국립농업과학원 화학물질안전과) ;
  • 홍수명 (농촌진흥청 국립농업과학원 화학물질안전과) ;
  • 김택겸 (농촌진흥청 국립농업과학원 화학물질안전과) ;
  • 김형진 (농촌진흥청 국립농업과학원 화학물질안전과) ;
  • 문병철 (농촌진흥청 국립농업과학원 화학물질안전과) ;
  • 경기성 (충북대학교 환경생명화학과)
  • Received : 2016.04.18
  • Accepted : 2016.09.28
  • Published : 2016.09.30
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Abstract

The aim of this study was to develop an analytical method for the determination of pyribencarb and its metabolite KIE-9749 in agricultural commodities. The experiment was performed with a range of concentrations $0.05{\sim}2.5{\mu}g/g$ in apple, green pepper, potato, hulled rice, soybean, pear, peach, grape and cucumber. Each samples were extracted with acetone and cleaned by dichloromethane/saline water partition and purified with Florisil solid phase extraction (SPE) cartridge and aminopropyl SPE cartridge. Pyribencarb and KIE-9749 were separated and quantified by HPLC/UVD at 265nm using acetonitrile and water as mobile phase. The recoveries of pyribencarb and KIE-9749 were within 78.3~108.4% and 73.9~113.7% with RSD below 12.2% and 15.0%, respectively. The limits of quantification (LOQ) were both $0.05{\mu}g/g$. LC/ESI-MS/MS was optimized for confirmation of residue identity.

농산물중 pyribencarb와 그 대사물 KIE-9749의 잔류분석법을 개발하였다. 분석법 개발에 사용된 농산물은 5대 작물군의 대표작물인 사과, 고추, 감자, 현미, 대두와 잔류허용기준이 설정된 배, 복숭아, 오이, 포도였다. 각 농산물은 아세톤으로 추출하였으며 액-액분배를 이용하여 1차 정제하고 Florisil solid phase extraction (SPE) cartridge와 aminopropyl SPE cartridge를 이용하여 2차 정제를 실시하는 조건을 확립하였다. 기기분석 조건은 HPLC/UVD 265 nm 파장에서 acetonitrile과 물을 이동상으로 사용하여 확립하였다. 확립된 분석법을 분석자를 달리하여 검증한 결과 pyribencarb의 회수율과 RSD값은 78~108%, 2.7~12.2%였으며, KIE-9749의 회수율과 RSD값은 74~114%와 1.7~15.0%를 보였다. 분석법의 정량한계(LOQ)는 두 성분 모두 $0.05{\mu}g/g$이었으며 LC/ESI-MS/MS를 사용하여 확립된 정성조건에서 방해 피크는 발견되지 않았다. 확립된 분석법은 pyribencarb와 그 대사물 KIE-9749에 대한 농산물의 안전성 검사를 위해 사용될 수 있을 것이다.

Keywords

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