Analysis of 236 Pesticides in Apple for Validation of Multiresidue Method using QuEChERS Sample Preparation and PTV-GC/TOFMS Analysis

QuEChERS법과 PTV-GC/TOFMS 이용 잔류농약 분석법 개발을 위한 사과시료 중 236종 농약의 동시분석

  • Ju, Ok-Jung (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kwon, Hye-Young (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Park, Byeong-Jun (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Kim, Chan-Seob (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Jin, Yong-Duk (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Lee, Je-Bong (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration) ;
  • Yun, Seo-Hee (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) ;
  • Hong, Su-Myeong (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)
  • 주옥정 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 박병준 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김찬섭 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 진용덕 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 이제봉 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 윤서희 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 손경애 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 임건재 (농촌진흥청 국립농업과학원 농산물안전성부)
  • Received : 2011.09.19
  • Accepted : 2011.10.30
  • Published : 2011.12.31

Abstract

The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GC/TOFMS (gas chromatography/ time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV-GC/TOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.

최근 농식품 중 잔류농약의 분석을 위해서 전처리를 빠르고 단순하게 하면서 고감도의 정밀기기를 이용하여 정성 및 정량을 동시에 행하는 분석방법의 개발이 확대되고 있다. 따라서 신속한 전처리법으로 빠르게 확산되고 있는 QuEChERS(quick, easy, cheap, effective, rugged and safe)법과 PTV(programmable temperature vaporizer)가 장착된 GC/TOFMS을 이용하여 분석법을 개발하였다. PTV조건을 확립했으며 사과 시료를 대상으로 3농도 수준에서(50, 100, 400 ng/g) QuEChERS법(acetate buffer법)으로 전처리 한 후 PTV-GC/TOFMS로 분석하여 회수율 및 RSD를 조사한 결과 400 ng/g 농도에서는 230성분(97%)이 80-120%의 회수율을 보였으며 5성분(2.1%)을 제외한 모든 성분에서 RSD값이 10%미만으로 양호한 재현성을 보였다. 가장 낮은 농도인 50 ng/g의 경우에서는 검출되지 않은 33성분을 제외한 203성분 중 197성분(97%)에서 70-120%의 회수율을 보였으며, 4성분(2.0%)을 제외한 모든 성분에서 RSD값이 20%미만으로 나타났다. 따라서 본 연구에서 확립된 QuEChERS 전처리법과 PTV-GC/TOFMS 분석조건을 이용하여 과일과 야채중의 잔류농약 분석이 가능할 것으로 보였다.

Keywords

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