超高效液相色谱-串联质谱法同时测定饮用水中林可霉素、替米考星和泰乐菌素残留

Simultaneous determination of lincomycin,tilmicosin and tylosin residues in drinking water by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定饮用水中林可霉素、替米考星和泰乐菌素残留的分析方法。方法样品经0.45μm水系滤膜过滤后用高氯酸溶液调节pH至2.5,加入螯合剂乙二胺四乙酸二钠,采用HLB固相萃取柱净化后,用超高效液相色谱-串联质谱仪测定,外标法定量。结果该方法在0.5~20.0ng/mL范围内线性关系良好,相关系数均大于0.999;方法的检出限为0.3~2.0ng/L,定量限为0.6~6.0ng/L;平均回收率范围为75.5%~107.9%,相对标准偏差(relative standard deviations,RSDs)为2.4%~5.8%。结论本方法操作简单、分离效果良好、灵敏度高,适用于饮用水中林可霉素、替米考星、泰乐菌素残留量的同时测定。

Objective To establish a method for the simultaneous determination of lincomycin,tilmicosin and tylosin residues in drinking water by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were filtered by 0.45μm water system filter membrane,adjusted the pH to 2.5 with perchloric acid solution,added ethylenediamine tetraacetic acid disodium,purified by HLB solid phase extraction,determined by UPLC-MS/MS and quantified by external standard method.Results This method had good linearity in the range of 0.5-20.0 ng/mL,all correlation coefficients were greater than 0.999;the limits of detection were in the range of 0.3-2.0 ng/L,and the limits of quantification were in the range of 0.6-6.0 ng/L;the average recoveries were ranged from 75.5%to 107.9%with the relative standard deviations(RSDs)of 2.4%-5.8%.Conclusion This method is simple to operate and has good separation and high sensitivity,and it is suitable for the simultaneous determination of lincomycin,tilmicosin and tylosin residues in drinking water.