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Development and validation of an analytical method for pyrimisulfan determination in agricultural commodities by LC-MS/MS

LC-MS/MS를 이용한 농산물 중 pyrimisulfan 잔류량 분석법 개발 및 확인

  • Do, Jung-Ah (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Lee, Mi-Young (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Cho, Yoon-Jae (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Kang, Iil-Hyun (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Kwon, Kisung (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation, KFDA)
  • 도정아 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 이미영 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 조윤제 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 강일현 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 권기성 (식품의약품안전청 식품의약품안전평가원 화학물질과) ;
  • 오재호 (식품의약품안전청 식품의약품안전평가원 화학물질과)
  • Received : 2012.12.24
  • Accepted : 2013.02.12
  • Published : 2013.04.25

Abstract

The maximum residue limits of pyrimisulfan is set as 0.05 mg/kg in rice in 2011, so very reliable and sensitive analytical method for pyrimisulfan residues is required for ensuring the food safety of pyrimisulfan residues in agricultural products. In this study, a rapid and sensitive analytical method was developed and validated using liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS) for the determination of herbicide pyrimisulfan residues in agricultural products. Average recoveries of pyrimisulfan ranged from 88.7 to 99.3% at the spiked level of 0.005 mg/kg and from 90.1 to 94.2% at the spiked level of 0.05 mg/kg, while the relative standard deviation was less than 10%. Linear range of pyrimisulfan was between 0.01~1.0 ${\mu}g/mL$ with the correlation coefficient ($r^2$) 0.999 and limit of quantification was 0.005 mg/kg. The results of method validation were satisfied Codex guideline. The results revealed that the developed and validated analytical method is possible for pyrimisulfan determination in agricultural product samples and will be used as an official analytical method.

Acknowledgement

Supported by : 식품의약품안전청

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