超高效液相色谱-串联质谱法测定牛奶中的赛拉嗪残留

Determination of Xylazine in Milk Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

采用乙腈提取,HLB固相萃取柱净化、超高效液相色谱-串联质谱测定,建立了一种简单、快速的牛奶中赛拉嗪残留的检测方法。对样品的提取、净化过程进行了优化改进,经ACQUITY UPLC^TM BEH C18色谱柱分离,正离子电喷雾电离串联质谱测定,牛奶中赛拉嗪的检测限为0.2μg/kg,定量限为0.5μg/kg。选取0.5、10、50μg/kg三个浓度进行空白添加回收率实验,批内变异系数5.8%~14.6%,批间变异系数小于5%。整个实验过程简单、快速,各项技术指标满足国内外法规的要求,非常适合大量牛奶样品中赛拉嗪药物残留的检测。

A method of the simultaneous analysis of xylazine in milk was developed with ultra performance liquid chromatography-tandem mass spectrometry.The residue from milk was extracted with acetonitrile,and the extracting solutions were purified using HLB solid phase extraction（SPE）cartridges.The xylazine residue was separated on a ACQUITY UPLCTM BEH C18 column,and detected by MS/MS with positive electrospray ionization mode.The limit of detect（LOD） was 0.2 μg/kg,and the limit of quantification（LOQ） was 0.5 μg/kg.At three spiking levels of 0.5、10、50 μg/kg,intra-assay coefficient of variation were between 5.8%~14.6% and inter-assay of variation were below 5.0%.The experiment results showed that the method was simple,rapid and was applicable to quantify and confirm the residue of xylazine in milk.