超高效液相色谱-串联质谱法测定牛肉中非衍生化的脱呋喃甲酰基头孢噻呋残留量

建立了牛肉中脱呋喃甲酰基头孢噻呋(DFC)的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。牛肉样品经DTE-硼酸盐缓冲液提取,过HLB固相萃取小柱净化浓缩,甲醇洗脱,UPLC-MS/MS法测定,仪器检测程序总色谱时间仅为5 min。方法平均回收率为80.7%～89.6%;批内变异系数范围在5.2%～9.7%之间;批间变异系数范围在6.1%～11.4%之间;检测限为0.55μg/kg;定量限为1.82μg/kg。方法可用于牛肉样品中脱呋喃甲酰基头孢噻呋药物残留量的确证检测。

Determination of non-derivative desfuroylceftiofur in beef by UPLC-MS/MS

An UPLC-MS/MS method was established for the determination of non-derivative desfuroylceftiofur in beef.Beef samples were extracted with dithioerythritol-phosphate buffer,then concentrated and purified by HLB SPE cartridge,finally,eluted with methanol.It was determined by UPLC-MS/MS,and it took only 5 mins for the total chromatographic time of the instrument testing procedures.The average recoveries for desfuroylceftiofur ranged from 80.7% to 89.6%.The intra-assay coefficients of variation were in the range of 5.2%~9.7%,the inter-assay coefficients of variation were in the range of 6.1%~11.4%.The limit of detection was 0.55 μg/kg and the quantitation limit was 1.82 μg/kg for beef.The method adapts to confirming analysis of desfuroylceftiofur in beef.