QuEChERS-同位素质谱内标法检测动物源性食品中20种头孢菌素的残留量

Determination of 20 Kinds of Cephalosporins Residues in Animal Derived Food by QuEChERS-LC-MS/MS with Isotope Internal Standards Method

采用液相色谱-串联质谱同位素内标法检测动物源性食品中20种头孢菌素。以甲醇作为提取溶剂提取样品中的头孢菌素,十八烷基硅烷吸附剂净化处理提取液。采用Ascentis C_(8)色谱柱,以0.1%甲酸水溶液与乙腈作流动相,在多反应监测模式下分别以正、负扫描模式进行分析。结果表明,17种头孢菌素的线性范围为5~100μg/L,3种头孢菌素的线性范围为25~500μg/L。线性方程的决定系数范围为0.9913~0.9998。20种头孢菌素在动物源性样品中的检出限为1.0~20.0μg/kg,定量限为3.0~60.0μg/kg。20种头孢菌素的平均回收率为78.08%~115.47%,相对标准偏差为3.07%~12.44%。该方法操作便捷,结果准确,适用于检测动物源性食品中20种头孢菌素。

A detection method for the determination of 20 kinds of cephalosporins in animal derived food was established with multiple stable isotope internal standards by liquid chromatography-tandem mass spectrometry.Cephalosporins were extracted from samples with methanol,and purified with octadecylsilane sorbent.An Ascentis C_(8) column was used for analyzing with 0.1%formic acid aqueous solution and acetonitrile as mobile phases.Analysis of cephalosporins were respectively performed on the positive and negative scan mode by multiple reactions monitoring.Results showed that the linear range of the methods was 5~100μg/L for 17 kinds of cephalosporins with highly responsive,and 25~500μg/L for 3 kinds of cephalosporins with lowly responsive.The determination coefficients of the linear equations ranged from 0.9913 to 0.9998.The limit of detection for 20 kinds of cephalosporins ranged from 1.0 to 20.0μg/kg,and the limit of quantification ranged from 3.0 to 60.0μg/kg in animal derived sample.The average recovery rate of 20 cephalosporins ranged from 78.08%to 115.47%,and the relative standard deviation ranged from 3.07%to 12.44%.The validated method was simple and accurate.It was suitable for the determination of 20 cephalosporins in animal food.