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Development of Multi-residue Analysis of 320 Pesticides in Apple and Rice Using LC-MS/MS and GC-MS/MS

LC-MS/MS와 GC-MS/MS를 이용한 사과와 쌀 시료에서 320종 농약의 다성분 분석

  • Kim, Jong-Hwan (Environmental Toxicology Research Center, Korea Institute of Toxicology) ;
  • Kim, Yeong-Jin (Environmental Toxicology Research Center, Korea Institute of Toxicology) ;
  • Kwon, Young-Sang (Environmental Toxicology Research Center, Korea Institute of Toxicology) ;
  • Seo, Jong-Su (Environmental Toxicology Research Center, Korea Institute of Toxicology)
  • 김종환 (안전성평가연구소 환경독성연구센터) ;
  • 김영진 (안전성평가연구소 환경독성연구센터) ;
  • 권영상 (안전성평가연구소 환경독성연구센터) ;
  • 서종수 (안전성평가연구소 환경독성연구센터)
  • Received : 2016.03.25
  • Accepted : 2016.06.17
  • Published : 2016.06.30

Abstract

A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

본 연구는 사과와 쌀에서 320성분 농약에 대한 다성분 동시분석법을 확립하고자 수행되었다. 시료의 추출은 QuEChERS법을 사용하였고, 추출 후 잔류물은 LC-MS/MS와 GC-MS/MS로 기기분석 하였다. 시험 농약은 LC-MS/MS 251성분, GC-MS/MS 110성분을 선발하였으며, 41성분은 공통적으로 적용되었다. 분석법의 정량한계는 LC-MS/MS에서 $0.01{\sim}20{\mu}g/kg$, GC-MS/MS에서 $0.1{\sim}100{\mu}g/kg$으로 산출되었다. 사과와 쌀에서 회수율 70~120%, 상대표준편차 20% 이내의 조건을 충족한 성분은 LC-MS/MS로 분석한 농약 중 각각 242성분(96%)과 237성분(94%)로 나타났으며, GC-MS/MS로 분석한 농약 중에는 각각 103성분(94%)과 83성분(76%)로 나타났다. 본 연구를 통해 QuEChERS 전처리와 LC-MS/MS 및 GC-MS/MS를 이용한 분석법은 농산물(사과 및 쌀) 중 잔류농약 다성분 동시 분석에 효과적으로 적용될 것으로 기대된다.

Keywords

Acknowledgement

Supported by : 안전성평가연구소

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