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

关键词:  超高效液相色谱-串联质谱  赛拉嗪  残留  牛奶

Key words:  Ultra Performance Liquid Chromatography - Tandem Mass Spectrometry  xylazine  residue  milk

摘要:

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Waters ACQUITY UPLCTM 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0.5μg/kg、10μg/kg、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

Abstract:

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 Waters ACQUITY UPLCTM BEH C18 column, and detected by MS/MS with positive Electrospray Ionization mode. The limit of detect (LOD) was 0.2μg/kg, and the limit of quantification (LOQ) was 0.5μg/kg. At three spiking levels of 0.5μg/kg、10μg/kg、50μg/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.