超高效液相色谱串联质谱法同时测定牛奶中三种头孢菌素类抗生素的研究  

Simultaneous Determination of Cefadroxil,Cephalexin and Cefradine in Milk by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：王建凤[1,2] 石佳丽[2,3] 刘艳[2] 杜振霞[1] 贾丽[2] 冯月超[2] 范筱京[2] 张经华[2] 

机构地区：[1]北京化工大学,北京100029 [2]北京市理化分析测试中心北京市食品安全分析测试工程技术研究中心,北京100089 [3]北京联合大学旅游学院,北京100101

出　　处：《中国奶牛》2017年第5期40-44,共5页China Dairy Cattle

基　　金：北京市科技计划项目(Z141100002614020)

摘　　要：本试验建立了固相萃取-超高效液相色谱串联质谱(SPE-UPLC-MS/MS)同时检测牛奶中3种头孢菌素类抗生素含量的方法,同时对三种物质断裂机理进行考察。样品用0.5mol/L的磷酸二氢钾缓冲溶液提取,MCX固相萃取柱进行净化,液相色谱串联质谱法进行测定,采用多反应监测(MRM)模式进行定性和定量分析。3种头孢菌素类抗生素的检出限(S/N=3)范围为0.1~0.5μg/kg,定量限(S/N=10)范围为0.25~1μg/kg,样品加标回收率范围为90%~117%。To developed a method for the detection of 3 kinds of cephalosporins in milk by solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry （SPE-UPLC-MS/MS）. The same fracture mechanism of the three cephalosporins was investgated. The samples were extracted with 0.05 mol/L phosphate buffer solution, cleaned up by MCX solid phase extraction column, and then analyzed by UPLC-MS/MS with multiple reaction monitoring （MRM） mode. The LODs and LOQs of 3 kinds of cephalosporins were in the range of 0.1-0.5 μg/kg and 0.25-1 μg/kg, respectively, with the mean recoveries varied from 90% to 117%.

关 键 词：MCX固相萃取 超高效液相色谱串联质谱 头孢菌素类抗生素 牛奶 

分 类 号：TS251.1[轻工技术与工程—农产品加工及贮藏工程]