高效液相色谱-串联质谱法测定莱芜香肠中3种β-受体激动剂残留

Determination of Residues ofβ-agonists in Laiwu Sausages by HPLC-MS/MS

为建立一种快速测定莱芜香肠中盐酸克伦特罗、莱克多巴胺和沙丁胺醇等3种β-受体激动剂残留量的液质联用检测方法,将样品加入乙酸铵溶液,经β-葡糖醛酸苷肽酶/芳基磺酸酯酶水解以及固相萃取柱净化后,以甲醇-0.1%甲酸水溶液作为流动相进行梯度洗脱,采用电喷雾离子源,以多反应监测方式进行采集,外标法定量。结果显示,3种β-受体激动剂在0.5~50.0 ng/mL范围内线性关系良好(R2≥0.9996);该方法检出限均为0.25μg/kg,平均回收率为90%~110%,相对标准偏差为0.1%~2.0%。该方法优化了盐酸克伦特罗、莱克多巴胺和沙丁胺醇的仪器分析条件,操作方便、结果准确、重现性好、回收率高,能满足莱芜香肠中食品安全控制检测的需要。

In order to establish a rapid liquid-mass spectrometry method for determining three kinds ofβ-agonists including clenbuterol hydrochloride,ractopamine and salbutamol in Laiwu sausages,after adding the samples to ammonium acetate solution,the samples were hydrolyzed byβ-glucuronidopeptidase/arylsulfonesterase and purified by solid phase extraction(SPE),methanol-0.1%formic acid aqueous solution was used as a flowing phase for gradient elution and collected by means of multi-response monitoring by electrospray ion(ESI)source,then quantified by external standard method.The results showed that the threeβ-agonists were with good correlation coefficien(t R2≥0.9996)within the range of 0.5 to 50.0 ng/mL;the detection limit of the established method was 0.25μg/kg,and the average recovery rate was 90%to 110%with relative standard deviation of 0.1%to 2.0%.The analysis conditions of instruments for clenbuterol hydrochloride,ractopamine and salbutamol were optimized with the advantages of easy operation,accuracy,good reproducible and high recovery,which could satisfy the need for food safety control and detection of Laiwu sausages.