Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Development and Interlaboratory Validation of an Analytical Method for the Determination of Saflufenacil in Agricultural Products by HPLC-UVD and LC-MS

  • Do, Jung-Ah (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Park, Hyejin (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Kwon, Ji-Eun (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Cho, Yoon-Jae (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Chang, Moon-Ik (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Choi, Won-Jo (Hazardous Substances Analysis Division, Center for Food and Drug Analysis, Busan regional Korea Food and Drug Administration) ;
  • Lee, Hyun-Sook (Hazardous Substances Analysis Division, Center for Food and Drug Analysis, Gyeongin regional Korea Food and Drug Administration) ;
  • Hong, Jin-Hwan (Food Chemical Residues Division, National Institute of Food and Drug Safety Evaluation)
  • Received : 2014.05.04
  • Accepted : 2014.11.07
  • Published : 2014.12.31
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Abstract

Saflufenacil is a low-volatile and uracil-based herbicide. This herbicide is used for pre-and post-emergence control of major broadleaf weeds. The objective of present study was to develop and validate an analytical method for saflufenacil determination in agricultural products for ensuring the food safety. The saflufenacil residues in samples were extracted with acetone, dichloromethane, and then purified with silica and graphitized carbon cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of saflufenacil was $0.1{\sim}5.0{\mu}gmL^{-1}$ with the correlation coefficient (r) = 0.999. Average recoveries of saflufenacil ranged from 80.5% to 110.2% at the spiked level of $0.02{\sim}0.5mgkg^{-1}$, while the relative standard deviation was 0.3~7.3%. In addition, the limit of detection and limit of quantification were 0.005 and $0.02mgL^{-1}$, respectively. Furthermore, an interlaboratory study among three labs was conducted to validate the method, and the results were satisfactory.

농산물 중에 있는 제초제 saflufenacil의 잔류량을 검사하기 위해 HPLC-UVD와 LC-MS를 이용한 정확하고 감도가 좋은 분석방법을 개발하였다. Saflufenacil 잔류물은 acetone 추출, dichloromethane을 이용한 액-액 분배, silica와 carbon 카트리지 정제를 거쳐 기기분석을 수행하였다. 검량선 작성을 위해 $0.1{\sim}5.0{\mu}gmL^{-1}$ 범위로 표준품을 만들어 실험한 결과 상관계수($r^2$)는 0.999로 높은 직선성을 보였다. $0.02{\sim}0.5mgkg^{-1}$ 처리수준으로 회수율을 실험한 결과는 80.5~110.2% 이었으며, 상대표준편차는 10% 미만이었다. 분석방법의 검출한계와 정량한계는 각각 0.005와 $0.02mgL^{-1}$ 이었다. 확립된 시험법으로 본청, 부산지방식품의 약품안전청과 경인지방식품의약품안전청에서 실험실간 검증을 실시한 결과 만족스런 결과를 얻었다. 이러한 결과들을 통해 확립된 시험법은 농산물 중 saflufenacil의 잔류량 분석에 적합함을 확인할 수 있었다.

Keywords

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