【摘要】 目的:建立鱼肉中氯霉素残留的HPLC/MS/MS检测方法。方法:采用负离子MRM监测模式,以氘代氯霉素为内标,样品用乙腈、乙酸乙酯、正己烷萃取后再用C18小柱净化。以保留时间和离子对(母离子和两个子离子)进行定性,以母离子和响应值高的子离子进行定量。结果:工作曲线在0.1μg/kg～10μg/kg范围内线性良好(r=0.9990),方法的检出限可达到0.03μg/kg,平均回收率为99%～105%,日内和日间RSD均小于8%。结论:该方法具有分析速度快、灵敏度高和特异性强等特点,可用于鱼肉中氯霉素残留的定量和定性检测。更多还原

【Abstract】 Objective:A liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the determination of chloramphenicol residues in fish.Methods: D5-chloramphenicol was used as internal standard.The sample was extracted with acetonitrile and ethyl acetate,then defatted with n-hexane.Sample concentration and purification were performed on C18.The qualification analysis was done by using retention time and distribution of diagnostic ion pairs,and the quantification analysis was based on the peak intensity of parent ion and a fragment ion with higher signal.A mass spectrometer was operated in the positive ion mode.Results: The standard curve was linear over the concentration range of 0.1 μg/kg～10 μg/kg.The detection limit of the method was 0.03 μg/kg and the limit of quantification was 0.1 μg/kg,average recoveries of chloramphenicol ranged from 99% to 105%,both the intra-day and inter-day RSD were less than 8%.Conclusion: This method is simple,rapid,sensitive and accurate.It was suitable for the detection of chloramphenicol residues in fish.更多还原