超高压液相色谱质谱联用法同时测定牛肝中七种磺胺类药物

Simultaneous determination of seven sulfonamide residues in cow liver by ultra performance liquid chromatography and mass spectrometry

建立了牛肝中7种磺胺类药物残留量的超高压液相色谱质谱联用的测定方法。样品经乙腈提取后经过MCX阳离子交换小柱净化后,利用超高压液相色谱进行检测。方法检出限为0.02μg/g。7种磺胺类药物的加标回收率为70.6%～112.5%(添加水平为0.02,0.05,0.1,0.2μg/g),相对标准偏差为2.6%～14.3%。同时建立了阳性样品检测的质谱确证方法,能够满足国际上对药物残留的要求。

A ultra performance liquid chromatography and mass spectrometry （UPLC-MS/MS） for the simultaneous determination of seven commonly used sulfonamide （SA） residues in cow liver has been developed. Samples were prepared by homogenizing the liver, extracted with acetonitrile, and cleaned-up on a Waters Oasis MCX column. The detection limits of 0.02μg/g was proved to be much better than the previously reported ones. Average recoveries of seven SAs （spiked at the levels of 0.02, 0.05, 0.1, 0.2μg/g） ranged from 70.6% to 112.5%, with relative standard deviations between 2.6% and 14.3%. The results demonstrate that the method is simple, accurate and suitable for the identification and quantification of these sulfonamide residues in cow liver.