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Analysis of Diflubenzuron in Agricultural Commodities by Multiresidue Method

동시 다성분 분석법에 의한 농산물 중 Diflubenzuron 분석

  • Park, Sun-Hee (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Han, Chang-Ho (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Ae-Kyung (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Shin, Jae-Min (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Lee, Jae-Kyoo (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Park, Young-Hae (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Ji-Min (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Hwang, Lae-Hong (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Chang, Min-Su (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Song, Mi-Ok (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Park, Ju-Sung (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Yun, Eun-Sun (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Mu-Sang (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Jung, Kweon (Gangnam Agro-Fishery Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment)
  • 박선희 (서울시보건환경연구원 강남농수산물검사소) ;
  • 한창호 (서울시보건환경연구원 강남농수산물검사소) ;
  • 김애경 (서울시보건환경연구원 강남농수산물검사소) ;
  • 신재민 (서울시보건환경연구원 강남농수산물검사소) ;
  • 이재규 (서울시보건환경연구원 강남농수산물검사소) ;
  • 박영혜 (서울시보건환경연구원 강남농수산물검사소) ;
  • 김지민 (서울시보건환경연구원 강남농수산물검사소) ;
  • 황래홍 (서울시보건환경연구원 강남농수산물검사소) ;
  • 장민수 (서울시보건환경연구원 강남농수산물검사소) ;
  • 송미옥 (서울시보건환경연구원 강남농수산물검사소) ;
  • 박주성 (서울시보건환경연구원 강남농수산물검사소) ;
  • 윤은선 (서울시보건환경연구원 강남농수산물검사소) ;
  • 김무상 (서울시보건환경연구원 강남농수산물검사소) ;
  • 정권 (서울시보건환경연구원 강남농수산물검사소)
  • Received : 2014.08.21
  • Accepted : 2014.10.08
  • Published : 2014.12.31

Abstract

The multiclass pesticide multiresidue method for the simultaneous determination of diflubenzuron in agricultural products was conducted by using HPLC-UVD. The method was validated through the guidelines of linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision with pesticide-free spinach, Korean cabbage, eggplant, squash, sweet pepper, cucumber, Korean melon. The calibration curve of diflubenzuron was linear over the concentration range of 0.05-5 mg/kg with correlation coefficient of above 0.99999. The limit of detection and quantification was 0.008 and 0.02 mg/kg. Mean recoveries of diflubenzuron for each sample were 77.5-105.6%. Relative standard deviation (RSD) in recoveries were all less than 20%. The intra-day and inter-day precision (RSD) were 0.4-1.9% and 0.7-1.9%, respectively. The result of validation indicated that this method was accurate and rapid assay.

HPLC-UVD를 이용하여 diflubenzuron이 다종농약다성분 분석법 제2법에 적합한지를 검증하고자 본 연구를 수행하였다. 유효성을 검증하기 위하여 농약이 검출되지 않은 시금치, 엇갈이배추, 가지, 애호박, 청피망, 오이, 참외 등 7종 농산물을 대상으로 직선성, 특이성, 검출한계, 정량한계, 정확성, 정밀성을 확인하였다. Diflubenzuron 표준용액을 0.05-5 mg/kg 농도로 희석하여 분석한 표준검량선의 직선성은($R^2=0.99999$)은 매우 만족할 만한 수준이었다. 검출한계는 0.008 mg/kg, 정량한계는 0.02 mg/kg 이며 회수율은 77.5-105.6%, 상대표준편차는 최대 20% 미만, 정밀도는 intra-day test에서 0.4-1.9%, inter-day test에서 0.7-1.9%를 나타내어 잔류농약분석법에서 허용하는 회수율 기준 70-120% 범위와 상대표준편차 20% 이하의 기준에 적합하였다. LC-MSD를 이용한 재확인 과정을 통해 잔류결과의 신뢰성을 확보하였다. 따라서 유통농산물 중 diflubenzuron의 일상적 검사법으로 빠르고 간편한 다종농약다성분 제2법을 적용할 수 있을 것으로 판단된다.

Keywords

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