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Development and validation of an analytical method for the determination of lepimectin residues by HPLC-PDA

HPLC-PDA를 이용한 lepimectin 잔류량 분석법 개발 및 확인

  • Do, Jung-Ah (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Kwon, Ji-Eun (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Kim, Mi-Ra (Daejeon Regional KFDA) ;
  • Lee, Eun-Mi (Daejeon Regional KFDA) ;
  • Kuk, Ju-Hee (Gwangju Regional KFDA) ;
  • Kwon, Kisung (Busan Regional KFDA) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA)
  • 도정아 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 권지은 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 이은미 (대전지방식품의약품안전청 유해물질분석과) ;
  • 김미라 (대전지방식품의약품안전청 유해물질분석과) ;
  • 국주희 (광주지방식품의약품안전청 유해물질분석과) ;
  • 권기성 (부산지방식품의약품안전청 시험분석센터) ;
  • 오재호 (식품의약품안전청 식품의약품안전평가원 화학물질과)
  • Received : 2012.11.21
  • Accepted : 2013.03.05
  • Published : 2013.04.25

Abstract

A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl ($NH_2$) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient ($R^2$) of both lepimectin $A_3$ and $A_4$ solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate, rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

Acknowledgement

Supported by : 식품의약품안전청

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