UHPLC-MS/MS法测定鸡蛋中11种头孢菌素的残留量

Determination of Eleven Cephalosporin Residues in Egg by UHPLC-MS/MS

采用UHPLC-MS/MS技术建立了鸡蛋中11种头孢菌素含量的同步测定方法。鸡蛋样品采用60%乙腈溶液进行超声波提取,离心后以阴离子小柱(PAX)净化除杂后,再以UHPLC-MS/MS进行分析测定。在最优条件下进行方法验证,在0.5~50 ng/mL质量浓度范围具有较好的线性关系,11种头孢菌素的相关系数(R^(2))均高于0.99;鸡蛋中头孢菌素的检出限(LOD)均为0.2μg/kg,定量限(LOQ)均为0.5μg/kg;以阴性鸡蛋样品为基质分别添加1,2,10μg/kg的加标回收试验(n=6),11种头孢菌素的平均回收率在81.7%~97.1%,平行实验的RSD在2.8%~6.8%。建立的方法具有高灵敏度、高准确度和高精密度的特点,可用于鸡蛋中11种头孢菌素含量的测定。

A method was established for the simultaneous determination of 11 kinds of cephalosporin residues in egg by UHPLCMS/MS.The samples were extracted by 60%acetonitrile solution,purified by mixed anion solid phase extraction column(PAX),and finally analyzed using UHPLC-MS/MS.The results showed good linearity in the range of 0.5-50 ng/mL,and the correlation coefficients(R^(2))were more than 0.99.The limit of detection(LOD)and the limit of quantification(LOQ)were 0.2 and 0.5μg/kg.The average recoveries and relative standard deviation were 81.7%~97.1%and 2.8%~6.8%,respectively in the spiked of 1,2 and 10μg/kg.The method has high sensitivity,accuracy and reproducibility,and is suitable for the determination of 11 cephalosporin residues in egg.