L/CM/SMS法测定水产品中(氟)喹诺酮类药物残留

Determination of(Fluoro)quinolones residues in aquatic products by high performance liquid chromatography/tandem mass spectrometry

目的：建立高效液相色谱-串联质谱法检测水产品中（氟）喹诺酮类药物残留分析方法。方法：样品经乙酸铵缓冲液-乙腈提取,正已烷脱脂净化后,用Atlantis C18柱分离,以乙腈水（含0.4%甲酸）作为流动相,采用电喷雾离子源（ESI）,阳离子模式,多反应监测（MRM）方式检测,外标法定量。结果：在本实验条件下,（氟）喹诺酮药物在0.020～5.0 mg/L范围内线性良好,最低检出浓度0.50～31.4μg/kg,相对标准偏差值（RSD）在0.99%～5.94%之间,样品平均加标回收率在62.2%～99.2%之间。结论：该方法能同时对水产品中多种（氟）喹诺酮类药物残留进行定性及定量分析,方法精密度较好、准确度较高,结果较满意。

Objective：To establish a method for determination of（Fluoro）quinolones residues in aquatic products by high performance liquid chromatography/tandem mass spectrometry.Methods：Homogenized samples were extracted with ammonium acetate buffer-acetonitrile,defatted by hexane,then separated by Atlantis C18 column with mobile phase consisting of water and acetonitrile（contains 0.4% formic acid）.Analyte identification and quantification were performed by electrospray ionization（ESI） in positive mode using multiple reaction monitoring.External standard method was also used.Results：The correlation coefficients were good in the concentration range of 0.020～5.0 mg/L.The limits of detection were 0.50～31.4 μg/kg.The relative standard deviation（RSD） was 0.99%～5.94% and the recoveries 62.2%～99.2%.Conclusion：The method can be applied to identification and quantification of（Fluoro）quinolones residues in aquatic products.It is simple,effective,and accurate.