建立了固相萃取-高效液相色谱-串联质谱(UPLC-MS/MS)测定肉类中沃尼妙林和泰妙菌素残留量的分析方法。样品用乙腈提取,OasisMCX SPE小柱净化,经C18色谱柱分离,以电喷雾离子源(ESI)在正离子多反应监测(MRM)模式下进行测定,外标法定量。沃尼妙林和泰妙菌素的检出限均为0.04μg/kg,定量下限均为0.1μg/kg,在0.1～50.0μg/L内线性关系良好,相关系数r均大于0.99。在0.1～10.0μg/kg的加标水平内的回收率为80%～94%,RSD为4.5%～8.2%。该方法实用、准确、灵敏,适用于肉类中沃尼妙林和泰妙菌素残留量的测定。

A method was developed for the determination of valnemulin and tiamulin residues in meat by solid-phase extraction clean up-liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted by acetonitrile,purified by solid phase extraction(SPE) with oasis MCX extraction catridge.C18 column was the separation column,positive electrospray ionization was performed under multiple reaction monitoring(MRM) mode.The limit of detection for valnemulin and tiamulin was 0.04μg/kg,and the limit of quantization was 0.1μg/kg.The calibration curve showed a good linear from 0.1μg/kg to 50.0μg/kg with a correlation coefficient of 0.99.The recoveries of valnemulin and tiamulin at spiked levels in the range of 0.1~10.0μg/kg were 80%~94% with relative standard deviations of 4.5%~8.2%.The method was practical,accurate and sensitive,and was suitable for the determination of valnemulin and tiamulin residues in meat.