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当前位置: 首页 > 文章 > 超高效液相色谱-串联质谱法测定牛奶中的赛拉嗪残留 中国兽药杂志 2011,45 (1) 10-13
Position: Home > Articles > Determination of Xylazine in Milk Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry Chinese Journal of Veterinary Drug 2011,45 (1) 10-13

超高效液相色谱-串联质谱法测定牛奶中的赛拉嗪残留

作  者：
毕言锋;仲锋;孙雷;汪霞;王树槐;徐士新
单  位：
中国兽医药品监察所
关键词：
超高效液相色谱-串联质谱;赛拉嗪;残留;牛奶
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ACQUITY UPLCTMBEH 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。
译  名：
Determination of Xylazine in Milk Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry
作  者：
BI Yan-feng,ZHONG Feng,SUN Lei,WANG Xia,WANG Shu-huai,XU Shi-xin(China Institute of Veterinary Drug Control,Beijing 100081;China)
关键词：
ultra performance liquid chromatography-tandem mass spectrometry;xylazine;residue;milk
摘  要：
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.

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