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Modified QuEChERS Multi-Residue Analysis Method for 61 pesticides in Fruits using with HPLC and GC-ECD/NPD

HPLC 및 GC-ECD/NPD를 이용한 과일 중 61종 농약의 QuEChERS 전처리 다성분 분석법 개발

  • Lee, Ju-Young (National Instrumentation Center for Environmental Management, Seoul National University) ;
  • Hong, Su-Myeong (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) ;
  • Min, Zaw Win (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kim, Yang-Hyeon (Croen research inc.) ;
  • Song, Kyung-Ae (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) ;
  • Lee, Hee-Dong (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Im, Geon-Jae (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kim, Doo-Ho (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kim, Jang-Eok (School of Applied Biosciences, Kyungpook National University)
  • 이주영 (서울대학교 농생명과학공동기기원) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김택겸 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • ;
  • 김양현 ((주)크로엔리서치) ;
  • 손경애 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 이희동 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 임건재 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김두호 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김장억 (경북대학교 응용생명과학부)
  • Received : 2012.08.06
  • Accepted : 2012.09.15
  • Published : 2012.09.30

Abstract

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe)분석법은 고체상의 분말을 시료에 직접 주입하여 농약성분을 추출하는 방법으로 분석법이 간단하고 빠르기 때문에 많이 연구되고 있다. 이 방법은 기존 분석법에 비하여 적은 시료량과 상대적으로 많은 불순물을 포함하고 있기 때문에 LC-MS/MS 등의 감도가 높은 분석기기를 필요로 하며, HPLC나 GC 분석을 위해서는 개선이 필요하다. 본 연구에서는 QuEChERS AOAC Official 2007.01 법을 개선하여 사과, 포도, 배, 단감 4가지 과일을 대상으로 UPLC-PDA, GC-${\mu}ECD$ 및 GC-NPD 을 이용하기 위한 QuEChERS 분석법을 개발하고자 하였으며 그 결과를 QuEChERS AOAC Official 2007. 01법을 적용한 LC-MS/MS 분석결과와 비교하였다. QuEChERS AOAC Official 2007. 01법을 이용한 네가지 과일별 회수율은 각각 사과 71.1~104%, 포도 75.7~132.2%, 배 84.8~108.7%, 감 78.3~127.4%이었으며, 개선된 QuEChERS법을 이용한 네가지 작물별 회수율은 각각 사과 70.9~112.9%, 포도 71.3~101, 배 71.3~126%, 감 76.4~122.5% 이었으며, 두 방법 모두 다성분 분석법의 회수율 기준인 70~130%이내 조건을 만족하였다. 대부분의 농약이 변형한 방법으로 실험을 수행하였을 때 좋은 회수율이 보이므로 ECD, NPD 및 UVD와 같이 현재 분석기관에서 많이 보급된 분석 장비로 사용하여 다성분 동시분석이 가능할 것으로 판단되었다.

Keywords

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