高效液相色谱-串联质谱法测定羊肉中的4种β-受体激动剂

The Quantitative Determination of Four β-agonists in Mutton by Liquid Chromatography Coupled with Mass Spectrometry Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法测定羊肉中的4种β-受体激动剂(克伦特罗、莱克多巴胺、沙丁胺醇、特布他林)含量。样品经酶解、提取后,经MCX小柱净化,以乙腈和体积分数为0. 001的甲酸溶液为流动相,选择多反应监测(MRM)模式,并且用内标法定量,用高效液相色谱-串联质谱分析测定。β受体激动剂在0. 5～10μg/kg范围均有良好线性关系,相关系数均大于0. 99,定量限为0. 05～0. 50μg/kg,加标回收率为79. 29%～102. 63%,相对标准偏差(RSD)为2. 5%～5. 6%。该方法灵敏度高、结果准确,可作为检测羊肉中的4种β-受体激动剂的方法。

Objective:To establish the determination of the residues of β-agonists(salbutamol,ractopamine,clenbuterol,tbutalin) in sampled mutton by LC-MS/MS.Method:A mixture of deutered salbutamol and clenbuterol internal standard was added to the enzymatic hydrolyzed samples,purified by MCX cartridges and then analyzed by LC-MS/MS with multiple reactionmonitoring(MRM) using internal standard method,eluted with the gradient of mobile phase composed by 0.1% of acetonitrile format solution and 0.1% of formic acid solution.Result:β-agonists in mutton samples were in good linear(r^2>0.99) at the concentrations of 0.5~10 μg/kg.The LOQs of antibiotics and pesticides were in the range of 0.05~0.50 μg/kg.At the three spiking levels,the recoveries ranged in 79.29%~102.63% with relative standard deviations of 2.5%~5.6%.Conclusion:the method is proved to be sensitive and accurate,and it could fit for the requirements of four kinds of β-agonists in mutton.