The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
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The analysis of pesticide residue in leafy vegetables using the modified QuEChERS pre-treatment methods

QuEChERS 시료 처리법을 활용한 엽채류 중 잔류농약분석

  • Kim, Yang-Hyeon (Croen Research Inc.) ;
  • Hong, Su-Myeong (Agro-Food Safety Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Son, Kyung-Ae (Agro-Food Safety Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Lee, Ju-Young (Agro-Food Safety Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Min, Zaw Win (Agro-Food Safety Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kwon, Hye-Young (Agro-Food Safety Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kim, Taek-Kyum (Agro-Food Safety Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kyung, Kee-Sung (Department of Environmental and Biological Chemistry, College of Agriculture, Life and Environmental Sciences, Chungbuk National University)
  • 김양현 ((주)크로엔리서치) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 손경애 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 이주영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김택겸 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 경기성 (충북대학교 농업생명환경대학 환경생명화학과)
  • Received : 2012.04.30
  • Accepted : 2012.05.30
  • Published : 2012.06.30
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Abstract

In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient ($R^2$ > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.

농약의 잔류분석은 일반적으로 기존의 액액분배 추출법(liquid liquid extraction, LLE)이 적용되어 왔으나, 시료 전처리에 많은 유기용매와 분석기구가 사용되고, 분석시간이 길며, 복잡한 분석단계로 인하여 보다 신속하고 효율적인 방법의 개발이 요구되고 있다. 이에 따라 경제적이고 간편한 농약 잔류 분석법을 확립하고자, 기존 분석법과 고체상 분말을 시료에 직접 주입하여 농약성분을 추출, 정제하는 QuEChERS (quick, easy, cheap, effective, rugged and safe)시료 전처리법을 비교 실험하였다. 엽채소류 중 상추, 참나물 및 취나물을 대상으로 농가에서 많이 사용하고, LC로 분석 가능한 대표적인 농약 6종(boscalid, cyazofamid, dimethomorph, fludioxonil, imidacloprid, pyraclostrobin)을 선정하였다. 두 분석법 모두 검량선의 상관계수($R_2$)는 0.99 이상으로 양호하였고, 검출한계는 imidacloprid는 0.02 mg/kg, 나머지 농약성분들은 0.05 mg/kg 수준이었다. 실험 결과, 액액분배법의 회수율은 92.8-100.9%, RSD는 2.5%이하였고, QuEChERS법의 회수율은 92.2-101.6%, RSD는 1.9%이하였다. Paired t-test를 이용하여 두 분석법 간의 시간에 따른 농약 잔류량을 비교한 결과, p-value는 0.3148-0.9890으로 두 분석법 간의 유의한 차이가 발견되지 않았다. 이 결과들을 볼 때 QuEChERS법은 기존의 액액분배법를 이용한 분석과 비교하여 동등한 회수율 결과를 보였으며, 분석 시간은 기존보다 약 1/4 정도 단축되었다. 또한 추출 과정 중 dichloromethane 등의 유해 유기용매 사용을 배제하여 실험자의 건강보호 및 폐용매의 양을 현저하게 줄일수 있어 친환경적이면서 경제적인 분석법으로 판단되었다.

Keywords

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