Improved determination of quinolones in milk at their MRL levels using LC–UV, LC–FD, LC–MS and LC–MS/MS and validation in line with regulation 2002/657/EC

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• 作者：M.P. Hermo ; E. Nemutlu ; S. Kı ; r ; D. Barró ; n ; J. Barbosa
• 关键词：Milk ; Quinolones ; EU criteria ; Liquid chromatography– ; ultraviolet detection ; Liquid chromatography– ; fluorescence detection ; Liquid chromatography– ; mass spectrometry ; Liquid chromatography– ; tandem mass spectrometry
• 刊名：Analytica Chimica Acta
• 出版年：2008
• 期刊代码：2_00032670
• 类别：ch
• 出版时间：14 April 2008
• 卷：613
• 期：1
• 页码：98-107
• 文件大小：599 K

摘要

This paper reports the multi-residue determination of quinolones included in the European Union regulations (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin and flumequine) in bovine milk, using liquid chromatography with ultraviolet (LC–UV), fluorescence (LC–FD), mass spectrometry (LC–MS) and tandem mass spectrometry detection (LC–MS/MS). The methods were validated, in line with EU requirements (Commission Decision 2002/657/EC). Linearity, decision limit (CCect.com/scidirimg/entities/204e.gif" alt="greek small letter alpha" title="greek small letter alpha" border="0">), detection capability (CCβ), detection limit (LOD), quantification limits (LOQ), recoveries, precision, selectivity and stability were determined and adequate results were obtained. Recoveries higher than 80%were obtained for all quinolones. The methods developed were used to quantify enrofloxacin and its main metabolite, ciprofloxacin, in milk from animals treated with enrofloxacin.