QuEChERS-高效液相色谱-串联质谱法测定 动物源性产品中9种β-受体激动剂残留

Determination of 9β-agonist Residues in Animal Products by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了一种测定牛肉中9种β-受体激动剂残留的HPLC-MS/MS方法。样品中加乙酸铵缓冲溶液,经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,2%甲酸-乙腈溶液提取,硫酸镁和乙酸钠盐析,采用N-丙基乙二胺(primary secondary amine,PSA)和十八烷基硅烷C18净化,正离子多反应监测模式测定,基质匹配标准溶液内标法定量。在优化条件下,9种β-受体激动剂在0.25~4.00μg/kg浓度范围内线性良好,定量限均为0.25μg/kg;0.25、0.50、2.50μg/kg共3个浓度添加水平平均回收率在67.73%~114.13%之间,变异系数在1.45%~9.14%之间。该方法灵敏度高、重现性好、操作简单、效率高,可用于畜产品中常见β-受体激动剂残留的检测确证。

The HPLC-MS/MS method for the determination of 9β-agonist residues in beef was established.Ammonium ac⁃etate buffer solution was added to the sample,which was hydrolyzed byβ-glucuronidase/arylsulfatase.After enzymolysis,it was extracted by 2%formic acid in acetonitrile,salted out with anhydrous magnesium sulfate and sodium acetate.Then,the extract was purified by the primary ethylene amine(PSA)and octadecyl silane C18.The target compounds were determined by positive ion multi-reaction monitoring mode,and the matrix matching standard solution was quantified by internal standard method.Under optimized conditions,9 kinds ofβ-agonists had a good linearity in the concentration range of 0.25~4.00μg/kg,and the limit of quantification was 0.25μg/kg.The average recovery rate of the three concentrations of 0.25,0.50,2.50μg/kg added levels was 67.73%~114.13%,and the coefficient of variation was 1.45%~9.14%.The method had high sensitivity,good reproducibility,simple operation and high efficiency,and could be used for the detection and confirmation of commonβ-receptor agonist residues in livestock products.