超高效液相色谱-串联质谱法测定肌肉组织中6种β-受体激动剂残留

HPLC-TMS determination of 6 kinds of β-agonist residues in muscle tissue

目的:建立检测肌肉组织中6种β-受体激动剂残留的LC-MS/MS方法。方法:样品酶解后,经乙酸乙酯和叔丁基甲醚提取,固相萃取法净化,以BEH C18(50 mm×2.1 mm,1.7μm)为分离柱,0.1%甲酸乙腈溶液-0.1%甲酸水溶液为流动相进行梯度洗脱,超高效液相色谱-串联质谱配有电喷雾离子源进行检测。结果:此方法的线性范围为0.25～5 ng.mL-1,线性相关系数R2≥0.9858,检出限为0.25μg.kg-1。平均回收率为80.58%～91.87%,RSD小于5%(n=5)。结论:该方法样品前处理简便,灵敏度高,可用于肌肉组织中β-受体激动剂残留的监测。

Objective：To establish a method for the determination of 6 kinds of β-agonist residues in muscle tissue by liquid chromatography-tandem mass spectrometry（LC-MS/MS）.Methods：The resulting enzymolysis was extracted with ethyl acetate and tert-butyl ether,and solid phase extraction（SPE） was used to purify the sample after their disposal.BEH C18 column（50 mm×2.1 nm,1.7 μm）was used as separation column.And the mobile phase was 0.1% formic acid in acetonitrile-0.1% formic acid in water for gradient elution.The determination to the sample was taken by ultra performance liquid chromatography-tandem mass spectrometry with electrospray ionization source detection.Results：Under these conditions,the linear range was 0.25-5 ng·mL-1,the linear correlation coefficient was above 0.9858,the detection limit was 0.25 μg·kg-1,the average recovery was between 80.58% and 91.87%,and the relative standard deviation（RSD） was smaller than 5.0%（n=5）.Conclusion：The method is easy,sensitive,it can be used to analyze β-agonists residues in muscle tissue.