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Analysis of Systemic Pesticide Imidacloprid and Its Metabolites in Pepper using QuEChERS and LC-MS/MS

QuEChERS 전처리와 LC-MS/MS를 이용한 고추 중 침투성농약 Imidacloprid 및 대사물질 동시분석법

  • Seo, Eun-Kyung (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kim, Taek-Kyum (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Hong, Su-Myeong (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kwon, Hye-Yong (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kwon, Ji-Hyung (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Son, Kyung-Ae (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kim, Jang-Eok (School of Applied Biosciences, Kyungpook National University) ;
  • Kim, Doo-Ho (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
  • 서은경 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김택겸 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권지형 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 손경애 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김장억 (경북대학교 응용생명과학부) ;
  • 김두호 (농촌진흥청 국립농업과학원 농산물안전성부)
  • Received : 2013.10.24
  • Accepted : 2013.11.22
  • Published : 2013.12.31

Abstract

Imidacloprid is a systemic insecticide which act as an insect neurotoxin. It used for control of pest such as aphids and other sucking insects in fruits and vegetables. Systemic pesticides move inside a crop following absorption by the plant, and these were converted into a variety of metabolites. Sometimes these metabolites make a problem about safety of agricultural products. So a simultaneous determination method of pesticide and its metabolites is needed, to monitor their presence in agricultural product and study on the fate of pesticide in a plant. This study's aim is to investigate simultaneous analysis method of imidacloprid and its metabolites, imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, and 6-chloronicotinic acid in red pepper using QuEChERS method and LC-MS/MS systems. QuEChERS method was modifed beacuase $MgSO_4$ salts decreased the recoveries of 6-chloronicotinic acid in extraction procedure. Imidacloprid and its metabolites were extracted by acetonitrile with 1% glacial acetic acid and the extracts were purified through QuEChERS with primary secondary amine (PSA) and $C_{18}$ and analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.999. Recovery studies were carried out on spiked pepper blank sample at four concentration levels (0.01, 0.04 and 0.1, 0.4 mg/kg). The average recoveries of imidacloprid and its metabolites were in the range of 70~120% with < 20% RSD. This result indicated that the method using QuEChERS and LC-MS/MS was suitable for the simultaneous determination of imidacloprid and its metabolites in red pepper.

Acknowledgement

Supported by : 국립농업과학원

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