本文建立了液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)检测鱼肉中氯霉素残留的分析方法.试样经乙酸乙酯提取,氮吹浓缩后通过QuEChERS净化,C18 色谱柱分离,以水和甲醇为流动相进行洗脱,电喷雾负离子模式检测,溶剂内标法定量.结果表明,氯霉素在1～20 ng/mL线性范围内线性关系良好,检出限为0.2 μg/kg,定量限为0.5 μg/kg,3个水平浓度加标下的平均回收率在88.0%～91.0%之间,相对标准偏差为3.39%～5.28%(n = 6).该方法具有前处理简便、基质效应低、准确性高等优点,可用于批量水产品中氯霉素药物残留检测.
Detection of Chloramphenicol Residues in Fish by Liquid Chromatography-Tandem Mass Spectrometry
A method for the determination of chloramphenicol residues in fish by liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established.Samples were extracted with ethyl acetate,concentrated with nitrogen blowing,purified by QuEChERS,separated with C18 chromatographic column,eluted with water and methanol as mobile phases,detected by negative mode of electrospray,and quantified by solvent internal standard method.The results showed that chloramphenicol had a good linear relationship within the range of 1-20 ng/mL,and the detection limit was 0.2 μg/kg,with the quantification limit 0.5 μg/kg.The average recovery rates at three levels of concentration ranged from 88.0%-91.0%,and the relative standard deviations(RSDs)were 3.39%-5.28%(n = 6).This method has the advantages of simple pretreatment,low matrix effect and high accuracy,and can be used for the detection of chloramphenicol drug residues in batch aquatic products.
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