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LC-MS/MS를 이용한 조피볼락 근육에서 구충제 febantel 및 그대사체들의 정량분석을 위한 시료 전처리 방법의 비교 분석

Comparison of sample preparation methods for quantification of febantel, an anthelmintic agent, and its metabolites in rockfish (Sebastes schlegeli) muscle using liquid chromatographytandem mass spectrometry

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초록

This study presents the evaluation of sample extraction and purification procedure for the determinationof residues of febantel and its metabolites, fenbendazole, oxfendazole and oxfendazole sulfonein rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry. Residues of febantel and its metabolites in rockfish muscle were analyzed using each different samplepreparation method from Korean Food Standards Codex (KFSC), Food Safety and Inspection Service(FSIS, USA), and the modified FSIS method using QuEChERS kit (FSIS-Q), respectively. Each methodwas compared for mean recoveries and repeatabilities. Since FSIS-Q showed higher repeatabilities(coefficient of variation, CV of 2.4%~10.9%) than those of FSIS method (CV of 4.6%~17.5%), recoveriesfrom FSIS-Q were compared with those from KFSC method. FSIS-Q showed significantly higherrecoveries of 83.1%~110.1% (P < 0.05) than those from KFSC method of 64.7%~107.4%. In addition,FSIS-Q showed a good linearity over the range of 2.5~200 μg/kg, and excellent sensitivities withlimit of detection of 0.46~0.71 μg/kg and limit of quantification of 1.08~2.15 μg/kg. Although allthe sample preparation methods turned out to be able to meet CODEX guideline for all the compounds,FSIS method and FSIS-Q validated in this study could be applied to screening and quantificationfor residues of febantel and its metabolites in rockfish muscle with efficient preparation procedures.

Abstract

This study presents the evaluation of sample extraction and purification procedure for the determinationof residues of febantel and its metabolites, fenbendazole, oxfendazole and oxfendazole sulfonein rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry. Residues of febantel and its metabolites in rockfish muscle were analyzed using each different samplepreparation method from Korean Food Standards Codex (KFSC), Food Safety and Inspection Service(FSIS, USA), and the modified FSIS method using QuEChERS kit (FSIS-Q), respectively. Each methodwas compared for mean recoveries and repeatabilities. Since FSIS-Q showed higher repeatabilities(coefficient of variation, CV of 2.4%~10.9%) than those of FSIS method (CV of 4.6%~17.5%), recoveriesfrom FSIS-Q were compared with those from KFSC method. FSIS-Q showed significantly higherrecoveries of 83.1%~110.1% (P < 0.05) than those from KFSC method of 64.7%~107.4%. In addition,FSIS-Q showed a good linearity over the range of 2.5~200 μg/kg, and excellent sensitivities withlimit of detection of 0.46~0.71 μg/kg and limit of quantification of 1.08~2.15 μg/kg. Although allthe sample preparation methods turned out to be able to meet CODEX guideline for all the compounds,FSIS method and FSIS-Q validated in this study could be applied to screening and quantificationfor residues of febantel and its metabolites in rockfish muscle with efficient preparation procedures.

참고문헌 (14)

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