The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
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Gas Chromatographic Method for Multiresidue Analysis of Unregistered Pesticides in Imported Agricultural Commodities

가스 크로마토그래피를 이용한 수입농산물 중 국내 미등록 농약의 다성분 동시분석법 적용

  • Lee, Ji-Won (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kang, Jeong-Kyun (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kwon, Hyeyoung (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Ro, Jin-Ho (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Jin, Yong-Duk (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Lee, Je Bong (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Hong, Su-Myeoung (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Kim, Teak-Kyum (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration) ;
  • Cho, Nam-Jun (Agro-Food Safety & Crop Protection Department, National Academy of Agricultural Science, Rural Development Administration)
  • 이지원 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 강정균 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 권혜영 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 노진호 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 진용덕 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 이제봉 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 홍수명 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 김택겸 (농촌진흥청 국립농업과학원 농산물안전성부) ;
  • 조남준 (농촌진흥청 국립농업과학원 농산물안전성부)
  • Received : 2015.03.06
  • Accepted : 2015.08.31
  • Published : 2015.09.30
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Abstract

The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.

본 연구는 한국의 주요 농식품 수입대상국인 중국과 동남아국가에서 사용하고 있는 국내 미등록 농약 중 GC/ECD 및 GC/NPD로 분석 가능한 농약 24종에 대하여 농산물안전성 분석을 위한 다성분 잔류분석법을 확립하고자 오렌지, 현미, 바나나를 대표 농산물로 선정하여 식품공전상의 다종농약 다성분 동시분석법 적용 시험을 실시하였다. 시료의 추출은 acetonitrile을 사용하였고, 추출 후 잔류물은 Florisil SPE cartridge를 이용해 정제한 다음, GC/ECD 및 GC/NPD로 기기분석 하였다. 분석법의 유효성 확인을 위해 농산물 시료에 첨가농도 0.02~0.05, 0.2 mg/kg 수준에서 위의 분석법을 적용하여 회수율 실험을 진행하였으며 분석법의 정량한계는 0.02~0.05 mg/kg, 직선성은 0.05~5 mg/kg 범위에서 $R^2$ > 0.99 이상으로 나타났다. GC/ECD로 분석한 평균 회수율은 공통적으로 분석되지 않은 3성분(ethiprole, picloram, sulcotrione) 및 회수율 초과한 성분을 제외한 농약에 대해 0.02(0.05) mg/kg 수준에서 70.3%~114.1%로 나타났고, 0.2 mg/kg 수준에서 71.9%~117.6%로 나타났다. GC/NPD로 분석한 평균 회수율은 0.02 mg/kg 수준에서 71.2%~119.9%, 0.2 mg/kg 수준에서 82.7%~115.0%로 나타났으며 20% 이내의 변이계수 조건을 충족시켰다. 잔류분석의 확인분석을 위해 GC/MS를 이용하여 GC/ECD 및 GC/NPD로 분석된 성분에 대한 total-ion chromatogram (TIC)을 획득하고 각 성분의 mass spectrum을 해석하여 각 성분의 재확인을 위한 이온을 선정하였다. 본 연구에서 검토된 농약 24종 중 19종은 식품공전상의 잔류농약분석법의 적용이 가능하여 수입농산물의 분석에 사용될 수 있을것으로 판단된다.

Keywords

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