超高效液相串联质谱法分析猪肉中残留的15种β-受体激动剂

摘要

Objective]To develop a method for determination of 15β-agonists residues in pork by ultra-performance liquid chromatography-mass spectrometry.[Method]The samples were enzyme hydrolyzed byβ-Glucuronidase/aryl sulfatase,etracted with 0.2 mol/L Acetic acid-ammonium acetate buffering solution(pH=5.0),and cleaned up on a SPE cartridge,separated on a C18 column using 0.01mol/L ammonium acetate(contain 0.1%Formic Acid)-Methanol as mobile phase,and detected under multiple reaction monitoring(MRM)mode.[Results]The resultes displayed a good linearity for 15β-agonists over the range of 5~100 ng/mL.The mean recoveries were from 74.2%to 115.6%at three different concentrations.[Conclusion]The method was precise,sensitive,and highly efficient in extraction and purification,and it is suitable for fast analysis ofβ-agonists residues in a large number of pork samples.%[目的]应用超高效液相色谱串联质谱技术建立同时测定猪肉中15种β-受体激动剂的检测方法。[方法]样品经β-盐酸葡萄糖醛苷酶/芳基硫酸酯酶酶解、0.2mol/L乙酸铵溶液(乙酸调pH至5.0)提取，阳离子固相萃取柱净化，以0.01mol/L乙酸铵(含0.1%甲酸)-甲醇为流动相梯度洗脱，C18柱为色谱柱进行分离，串联质谱多反应检测(MRM)模式测定。[结果]15种β-受体激动剂在5~100 ng/mL浓度范围内线性关系良好，3种添加水平下样品平均回收率在74.2%~115.6%之间。[结论]该方法提取效率高，净化效果好，具有良好的灵敏度和准确性，适合大批量猪肉样品中15种β-受体激动剂的快速测定。