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Development and validation of an analytical method for nematicide imicyafos determination in agricultural products by HPLC-UVD

HPLC-UVD를 이용한 살선충제 imicyafos의 시험법 개발 및 검증

  • Do, Jung-Ah (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Park, Hyejin (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kwon, Ji-Eun (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Choi, Won-Jo (Hazardous Substances Analysis Team, Center for Food and Drug Analysis, Busan Regional Korea Food and Drug Administration) ;
  • Lee, Hyun-Sook (Hazardous Substances Analysis Team, Center for Food and Drug Analysis, Gyeongin regional Korea Food and Drug Administration) ;
  • Chang, Moon-Ik (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Hong, Jin-Hwan (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Oh, Jae-Ho (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 도정아 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 박혜진 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 권지은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 최원조 (부산지방식품의약품안전청 유해물질분석팀) ;
  • 이현숙 (경인지방식품의약품안전청 유해물질분석팀) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 홍진환 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 오재호 (식품의약품안전처 식품의약품안전평가원 식품위해평가부)
  • Received : 2014.09.22
  • Accepted : 2014.10.11
  • Published : 2014.10.25

Abstract

Imicyafos which is a nematicide for controlling root-knot nematodes has been registered in the Republic of Korea in 2012, and the maximum residue limits of imicyafos are set to watermelon and korean melon as each 0.05 mg/kg. Extremely reliable and sensitive analytical method is required for ensuring food safety on imicyafos residues in agricultural commodities. Imicyafos residues in samples were extracted with acetone, partitioned with hexane and dichloromethane, and then purified with florisil. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. Linear range was between 0.1~5 mg/kg with the correlation coefficient ($r^2$) 0.99997. Average recoveries of imicyafos ranged from 77.0 to 115.4% at the spiked levels of 0.02 and 0.05 mg/kg with the relative standard deviations of 2.2~9.6%. Limit of detection and quantification were 0.005 and 0.02 mg/kg, respectively. An inter-laboratory study was conducted to validate the determination method in depth, and the results were satisfactory. All of the validation results revealed that the developed analytical method in this study is relevant for imicyafos determination in agricultural commodities and will be used as an official analytical method.

Keywords

imicyafos;nematicide;HPLC-UVD;LC-MS;official analytical method

Acknowledgement

Supported by : 식품의약품안전처

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