采用超高效液相色谱-串联质谱建立动物组织中丙哌维林、贝那替嗪、哌仑西平、美卡拉明等10种抗胆碱类药物残留检测方法。样品经过1%甲酸乙腈提取、Oasis PRiME HLB柱净化后,经Acquity UPLC BEH C18(50 mm×2.1 mm,1.7 μm)分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,正离子MRM信号采集数据,10种抗胆碱类药物能在10.5 min内完好分离,在1.0~50.0 μg/L浓度范围内,10种抗胆碱类药物线性良好,相关系数均在0.9951以上;最低定量限均低于1.0 μg/kg,通过1.0、2.0、10 μg/kg三个水平的添加回收实验表明,猪肉中平均回收率在64.7%~108.2%,批内变异系数为1.09%~10.5%,批间变异系数为2.31%~11.4%,猪肝中平均回收率在62.6%~108.0%,批内变异系数为0.38%~10.7%,批间变异系数为2.24%~11.2%。该方法较好的满足了动物组织中该药物多残留检测要求,对有效防范药物滥用和非法添加行为和打击注水肉起到了一定的技术支撑作用。
A multi-residue method based on ultra performance liquid chromatography tandem mass spectrometry was developed for the determination of ten anticholinergic drugs residues in animal tissues. In this method,analytes were extracted by acidified acetonitrile,and purified by Oasis PRiME HLB SPE column. Ten anticholinergic drugs were analyzed by Acquity UPLC BEH C18 column(50 mm×2.1 mm,1.7 μm)using methanol and 0.1% formic acid as the mobile phases. The signals were acquired through ESI+and MRM mode. All analytes could be well-separated by a gradient program during 10.5 minutes. The calibration curves of ten anticholinergic drugs were linear in a concentration range of 1.0~50.0 μg/L(r>0.9951),and the limits of quantitation were all less than 1.0μg/kg in animal tissues. The recoveries of 1.0,2.0,10 μg/kg fortified pork samples ranged from 64.7%~108.2% with the intra-assay coefficient of variation was 1.09%~10.5%,and the inter-assay coefficient of variation was 2.31%~11.4%. The recoveries fortified liversamples ranged from 62.6%~108.0% with the intra-assay coefficient of variation was 0.38%~10.7%,and the inter-assay coefficient of variation was 2.24%~11.2%.The method could meet the requirements of the drug residue detection in animal tissues,which played a certain technical support role in effectively preventing drug abuse,illegally adding behavior and combating water injection.