The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
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Multiresidue Analysis of 124 Pesticides in Soils with QuEChERS extraction and LC-MS/MS

QuEChERS 및 LC-MS/MS를 이용한 토양 중 124종 잔류농약다성분 분석법

  • Gwon, Ji-Hyeong (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) ;
  • Seo, Eun-Kyung (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) ;
  • Kyung, Ki-Sung (Chungbuk National University) ;
  • Kim, Jang-Eok (Kyungpook National University) ;
  • Cho, Nam-Jun (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
  • 권지형 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김택겸 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 서은경 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 경기성 (충북대학교 응용생명과학부) ;
  • 김장억 (경북대학교 응용생명과학부) ;
  • 조남준 (농촌진흥청 국립농업과학원 농산물안전성부)
  • Received : 2014.11.26
  • Accepted : 2014.12.16
  • Published : 2014.12.31
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Abstract

A QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) multiresidue method was developed for the simultaneous analysis of 124 pesticides in soil by LC-MS. The procedure involved liquid extraction of soil immersed with 0.2N $NH_4Cl$ by acetonitrile with 1% acetic acid, followed by anhydrous $MgSO_4$ and sodium acetate, and dispersive SPE cleanup with $MgSO_4$, primary secondary amine (PSA) and $C_{18}$. The extracts were 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 0.99. Recovery studies for the validation were carried out using two type soils, loam and sandy loam, at four concentration levels (0.005, 0.01, 0.02, and 0.1 mg/kg). The recoveries of pesticides were in the range of 70-120% with < 20% RSD except 4 pesticides, Benfuracarb, Ethiofencarb, Pymetrozine, and Pyrethrin. This result indicated that the method using QuEChERS and LC-MS/MS could be applied for the simultaneous determination of pesticide residues in soils.

토양환경 중 잔류농약 동시분석을 위해 124종의 농약을 대상으로 QuEChERS 전처리와 LC-MS-MS를 이용한 분석법을 개발하고자 하였다. QuEChERS 전처리 과정은 토양시료에 0.2N $NH_4Cl$ 용액 침지하고 1% acetic acid 포함 acetonitrile 용매로 추출 후 $MgSO_4$ 및 NaOAc로 salting out하고 PSA 50 mg, $C_{18}$ 50 mg, $MgSO_4$ 150 mg를 이용해 정제하였다. 분석법의 검증을 위해 양토 및 사양토 두 토양에서 0.005, 0.01, 0.02, 0.1 mg/kg 4수준으로 처리 후 회수율 실험을 실시하였다. 회수율 실험결과 Benfuracarb, Ethiofencarb, Pymetrozine, Pyrethrin 성분을 제외하고 나머지 성분들은 사양토와 양토 모두 70~120%의 적정 회수율을 나타내었으며, 상대표준편차도 20% 이내를 양호한 결과를 나타내었다. 따라서 QuEChERS 전처리 및 LC-MS를 이용한 분석법은 토양 중 잔류농약 다성분동시분석에 적용이 가능할 것으로 판단되었다.

Keywords

References

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