The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
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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
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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.

Imidacloprid는 곤충의 신경 독으로 작용하는 침투성 살충제이며, 과일과 채소에 진딧물 등의 해충 방제에 이용되고 있다. 침투성 농약은 작물체 내부로 흡수 이동되어 다양한 대사산물들이 생성되며 이중 일부 대사산물들은 농산물의 안전성에 문제가 되기도 한다. 따라서 농약과 대사산물의 동시분석법은 작물체 내에서 농약의 동태연구 및 농산물의 안전성을 확인하기 위해 필요하다. 본 연구의 목적은 고추 식물체 내에서 imidacloprid와 그 대사산물 4종, imidacloprid urea, imidacloprid olefin, idmidalcoprid guanidine, 그리고 6-chloronicotininic acid의 QuEChERS 법과 LC-MS/MS 시스템을 사용한 동시 분석법을 개발하고자 하였다. 실험방법은 고추 식물체 시료에 1% glacial acetic acid와 아세토니트릴 첨가한 후 추출하였고 그 추출물을 일정량 분취한 후 PSA와 $C_{18}$을 이용하여 정제하였다. 정제된 추출물은 LC-MS/MS로 분석하였으며, 표준정량곡선은 혼합표준용액(Matrix matched standard)를 제조하여 작성하였다. 표준정량곡선의 상관계수는 0.998 이상이었으며, LOQ도 0.05 mg/kg 이하였다. 0.01, 0.04, 0.1, 0.4 mg/kg 4개 수준으로 회수율시험을 수행하였으며, 그 결과 imidacloprid와 그 대사산물의 회수율은 70~120%이었고, RSD는 20%이하였다. 이러한 결과는 본 시험방법이 고추 식물체에서 imidacloprid 및 그 대사산물을 분석하는데 적합하다는 것을 보여준다.

Keywords

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