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

HPLC-UVD를 이용한 살균제 fenpyrazamine의 시험법 개발 및 검증

  • Park, Hyejin (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Do, Jung-Ah (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kwon, Ji-Eun (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Ji-Young (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Cho, Yoon-Jae (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Heejung (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Oh, Jae-Ho (Food Safety Risk Assessment Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Rhee, Kyu-Sik (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Sang-Jae (Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Chang, Moon-Ik (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 박혜진 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 도정아 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 권지은 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 이지영 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 김희정 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 오재호 (식품의약품안전처 식품의약품안전평가원 식품위해평가과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 이상재 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 잔류물질과)
  • Received : 2013.09.30
  • Accepted : 2014.05.29
  • Published : 2014.06.25

Abstract

Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, and Monilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 and the maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues is required for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted with hexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LC-MS and quantified using external standard method. Linear range of fenpyrazamine was between $0.1{\sim}5.0{\mu}g/mL$ with the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked level of 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limit of detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that the developed and validated analytical method is possible for fenpyrazamine determination in agricultural product samples and will be used as an official analytical method.

Keywords

fenpyrazamine;pyrazole fungicide;HPLC-UVD;LC-MS

Acknowledgement

Supported by : 식품의약품안전처

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