超高效液相色谱-串联质谱法测定鸡蛋中多种药物残留

Determination of Multiple Drug Residues in Egg by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

建立鸡蛋中氯霉素类药物与氟虫腈及其代谢物的多残留同时检测的超高效液相色谱-串联质谱方法。以酸化乙腈为提取液,采用PRIME HLB净化的方式,超高效液相色谱-串联质谱法(HPLC-MS/MS)进行分析,多反应监测运行模式(MRM),电喷雾负离子模式,以甲醇水为流动相。该方法在0.005~10μg/L线性关系良好,决定系数在0.99907~0.99995,定量限范围为0.01~0.08μg/kg,平均回收率为93.5%~116.0%,相对标准偏差RSD值1.6%~8.8%。该方法过程简单,适用于鸡蛋中氯霉素类与氟虫腈及其代谢物的同时检测。

To develop a method for determination of chloramphenicol drugs and fipronil and its metabolite in egg by ultra performance liquid chromatography tandem mass spectrometry,extracted by acidic acetonitrile,and cleaned up by PRIME HLB,then determined by HPLC-MS/MS,Multi-response monitoring operation mode(MRM),electrospray ionization in negative ion mode,the mobile phase was methanol water.This method showed a good linearities between 0.005 and 10μg/L,the coefficient of determination was between 0.99907 and 0.99995,the limit of detection(LOD)was between 0.01~0.08μg/kg,the average recovery was in the range 93.6%~116.0%,the relative standard deviation(RSD)was 1.6%~8.8%.The method is simple and suitable for simultaneous detection of CAPS and fipronil and its metabolitein in eggs.