摘要
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.
作者
洪丽
Hong Li(Fujian Inspection and Research Institute for Product Quality,National Quality Supervision and Testing Center for Processed Food,Fuzhou 350002,China)
出处
《山东化工》
CAS
2023年第17期162-165,共4页
Shandong Chemical Industry
基金
国家市场监督管理总局科技计划项目(2021MK054)。
