牛羊毛发中3种β-受体激动剂药物残留测定的EMR-Lipid方法研究

Method for determination of doping drug desidues with cattle and sheep hair as target tissues based on the EMR-Lipid technology

旨在建立一种以牛羊毛发为靶标结合强化基质去除技术(EMR-Lipid)对3种β-受体激动剂药物(克伦特罗、莱克多巴胺、沙丁胺醇)残留量进行测定的方法。毛发样品经选取、清洗、干燥、研磨后,经酸水解和氨化乙腈提取后加入到Captiva EMR-Lipid净化柱,加入石墨化炭黑(GCB)进行净化,过滤后用高效液相色谱-串联质谱仪进行测定,采用正离子(ESI^(+))扫描,多反应监测(MRM)模式进行分析,内标法定量。结果显示:待测药物在0.1~100 ng/mL的浓度范围内具有良好的线性相关性,相关系数R2≥0.995;方法检测限(LOD)为0.2μg/kg,定量限(LOQ)为0.5μg/kg;药物在1、20、100μg/kg添加浓度下,平均回收率为70%~120%,相对标准偏差≤20%。该方法取样方便,前处理步骤少,灵敏度和精密度高,符合残留检测要求,为动物性产品中β-受体激动剂类药物残留量测定提供了参考。

A UPLC-MS/MS method was developed using the enhanced matrix removal technology(EMR-Lipid)for rapid determination of residues ofβ-receptor agonist drugs(clenbuterol,ractopamine,salbutamol)in cattle and sheep hair.The samples to be tested were prepared by selecting,cleaning,drying and grinding.After acid hydrolysis and ammonified acetonitrile extraction,the hair samples were poured into the Captiva EMR-Lipid purification columns.The ultra-high performance liquid chromatography-tandem mass spectrometry instrument equipped with an ESI+electric spray ion source was used for determination under a multi-reaction monitoring mode(MRM),and the internal standard method was applied for quantitative analysis.The results showed that the linear range of the drug had a good linear correlation in the concentration range of 0.1-100 ng/mL,and the correlation coefficient was≥0.995.The limit of detection(LOD)of this method was 0.2μg/kg,and its limit of quantification(LOQ)was 0.5μg/kg.The average recovery rate of the drugs was 70%-120%,and its relative standard deviation was≥20%at concentrations of 1,20,100μg/kg of the drugs.To sum up,the present method was convenient for sampling,with less pre-treatment steps,high sensitivity and precision;which would meet the residue detection requirements and might serve as reference for determination of residues ofβ-receptor agonists in animal products.