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HPLC-UVD를 이용한 농산물 중 스피노사드 분석법 개선 및 잔류실태 조사

Development of Analytical Methods of Spinosad in Agricultural Commodities by HPLC with UV Detector and Monitoring

  • 김희연 (서울지방식품의약품안전청 유해물질분석과) ;
  • 최선희 (서울지방식품의약품안전청 유해물질분석과) ;
  • 정소영 (서울지방식품의약품안전청 유해물질분석과) ;
  • 최희주 (서울지방식품의약품안전청 유해물질분석과) ;
  • 김용훈 (서울지방식품의약품안전청 유해물질분석과) ;
  • 조민자 (서울지방식품의약품안전청 유해물질분석과) ;
  • 서은채 (서울지방식품의약품안전청 유해물질분석과) ;
  • 한경진 (서울지방식품의약품안전청 유해물질분석과) ;
  • 최재천 (경인지방식품의약품안전청 수입식품분석과) ;
  • 박희옥 (서울지방식품의약품안전청 식품안전관리과) ;
  • 하상철 (대구미래대학 제과데코레이션과) ;
  • 신일식 (강릉원주대학 해양식품공학과 식품위생학연구실) ;
  • 엄지윤 (서울지방식품의약품안전청 유해물질분석과)
  • Kim, Hee-Yun (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Choi, Sun-Hee (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Chung, So-Young (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Choi, Hee-Ju (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Kim, Yong-Hoon (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Cho, Min-Ja (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Seo, Eun-Chae (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Han, Kyoung-Jin (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration) ;
  • Choi, Jae-Chun (Imported Food Analysis Division, Gyeongin Regional Korea Food and Drug Administration) ;
  • Park, Hee-Ok (Food Safety Management Division, Seoul Regional Korea Food and Drug Administration) ;
  • Ha, Sang-Chul (Department of Confectionery Decoration, Daegu Mirae College) ;
  • Shin, Il-Shik (Lab. of Food Safety Facul. Marine Bioscience and Tech. Kangnung National University) ;
  • Eom, Ji-Yoon (Hazard Substances Analysis Division, Seoul Regional Korea Food and Drug Administration)
  • 투고 : 2010.09.01
  • 심사 : 2010.11.25
  • 발행 : 2011.04.30

초록

본 연구는 단성분 농약 중 스피노사드의 잔류실태를 조사하기 위하여 식품공전의 스피노사드 분석법을 농산물에 적용되도록 개선하고 개선 된 시험법으로 잔류실태조사가 부족한 스피노사드에 대한 잔류실태를 조사하였다. 국내 유통 중인 16종의 농산물 304건에 대한 스피노사드 잔류량을 조사한 결과 모든 검체에서 검량한계 이상 검출 되지 않았다. 스피노사드 시험법의 회수율은 현미, 강낭콩, 오렌지, 들깻잎, 표고버섯에서 스피노사드 A의 경우 0.05 mg/kg 수준에 각각 76.2, 95.3, 83.5, 79.9, 98.6%이고, 0.25 mg/kg 수준에 각각 97.3, 86.6, 84.4, 94.0, 88.1%이고, 스피노사드 D 의 경우 0.05 mg/kg 수준에 각각 76.6, 104.0, 88.9, 74.9, 81.1%이고, 0.25 mg/kg 수준에 각각 92.7, 97.7, 86.9, 90.4, 85.4%였으며 검출한계 0.001 mg/kg, 검량한계 0.005 mg/kg이다. 회수율에 대한 모든 표준편차는 10% 미만이다. 스피노사드 A와 D는 0.1-5.0 mg/kg 범위에서 상관계수($r^2$) 0.9999 이상의 높은 직선성을 보이고, 검출한계는 0.001 mg/kg, 검량한계는 0.005 mg/kg이었다.

The purpose of this study was to develop a methodology to detect spinosad which are difficult to analyze by multi-component simultaneous analysis of pesticide residues. We monitored spinosad due to the paucity of related information. The spinosad was determined using HPLC with UV detector at 250 nm. Correlation coefficient ($r^2$) for standard curve of spinosad A and D at standard concentration of 0.1-5.0 mg/kg were 0.999, respectively. Limit of quantitation (LOQ) of HPLC analysis was 0.005 mg/kg while limit of detection (LOD) was 0.001 mg/kg. Recovery experiments were conducted on five representative agricultural products to validate the analytical method. The recovery of proposed methods ranged from 74.9% to 104.0% and relative standard deviations were less than 10%. Spinosad residues were investigated in 16 commodities collected from 22 provinces. In this study, residues on all samples were not detected.

키워드

참고문헌

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