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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.

Acknowledgement

Supported by : 식품의약품안전청

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