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Method Development and Validation for Analysis of Isopyrazam Residues in Agricultural Products

농산물 중 살균제 Isopyrazam의 개별 잔류분석법 확립

  • Kim, Ji-Yoon (Department of Biological Environment, College of Agriculture and Life Sciences, Kangwon National University) ;
  • Kim, Ja-Young (Department of Biological Environment, College of Agriculture and Life Sciences, Kangwon National University) ;
  • Ham, Hun-Ju (Environment Friendly Agricultural Products Safety Center) ;
  • Do, Jung-Ah (Food Standards Division, Korea Food and Drug Administration) ;
  • Oh, Jae-Ho (Food Standards Division, Korea Food and Drug Administration) ;
  • Lee, Young-Deuk (Division of Life and Environmental Science, Daegu University) ;
  • Hur, Jang-Hyun (Department of Biological Environment, College of Agriculture and Life Sciences, Kangwon National University)
  • 김지윤 (강원대학교 농업생명과학대학 바이오자원환경학과) ;
  • 김자영 (강원대학교 농업생명과학대학 바이오자원환경학과) ;
  • 함헌주 (친환경농산물안전성센터) ;
  • 도정아 (식품의약품안전청) ;
  • 오재호 (식품의약품안전청) ;
  • 이영득 (대구대학교 생명환경학부) ;
  • 허장현 (강원대학교 농업생명과학대학 바이오자원환경학과)
  • Received : 2013.04.08
  • Accepted : 2013.05.30
  • Published : 2013.08.30

Abstract

Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

Isopyrazam은 신규 농약으로 현재 국내에는 공정분석법이 확립되어 있지 않아 농산물 중 잔류농약 분석을 위한 개별 분석법 개발이 필요하다. 본 연구는 현미, 대두, 고추, 감귤, 참외, 오이를 대표 농산물로 선정하여 isopyrazam에 대한 공정 개별 분석법을 확립하고자 수행되었다. Isopyrazam의 syn과 anti 이성질체를 분석하기 위해 여러 가지 추출, 분배 및 정제방법을 비교하면서 최적의 조건을 충족해 가며 분석법을 확립하였다. 대표 농산물 시료 중 함유된 isopyrazam은 acetonitrile로 추출한 후 n-hexane으로 액-액 분배하였으며, florisil을 이용하여 정제한 후 HPLC/UVD로 최종 분석하였다. 시료 중 현미와 대두는 n-hexane/acetonitrile을 이용한 유지제거 과정을 추가하였다. 본 분석법의 isopyrazam에 대한 정량한계는 1.0 ng (S/N > 10)이었고, 분석정량한계는 0.04 mg $kg^{-1}$이었다. 회수율은 isopyrazam syn과 anti-isomer에서 각각 81.0~105.4%, 80.8~105.6%이었으며, 반복 간 분석오차는 10% 미만이었다. 분석성분에 대한 확인을 위하여 LC/MS SIM을 이용하였다. 본 연구에서 확립된 isopyrazam의 분석법은 우수한 정량성 및 재현성, 분석과정의 편의성을 고려할 때 농산물 중 잔류농약에 대한 검사 및 안전성 평가를 위한 공정 분석법으로 활용될 수 있을 것으로 사료된다.

Keywords

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