高效液相色谱-串联质谱法同时测定动物源性食品中15种禁限兽药残留

Simultaneous determination of 15 prohibited and restricted veterinary drug residues in animal derived food by high performance liquid chromatographytandem mass spectrometry

建立高效液相色谱-串联质谱法,对猪肉、鸡肉、牛肉、羊肉中15种禁限兽药进行快速筛查测定。样品经1%(v/v)乙酸-乙腈提取,涡旋混匀后超声波助提,重复提取一次后经萃取盐包除水、SCRS净化柱净化除脂,Kinetex F5五氟苯基色谱柱分离,电喷雾离子源(ESI)正离子模式下,采用多反应监测模式(MRM)进行检测,外标法定量。15种禁限兽药在0.5~50μg/L浓度范围内线性关系良好(R2>0.997),检出限(LODs)和定量限(LOQs)均低于1μg/kg,加标回收率为78%~98%,相对标准偏差(RSDs)为2.6%~8.3%(n=6)。该方法前处理过程操作简单,具有回收率稳定、成本低等优点,可适用于大批量样本分析,为风险监测提供有效的数据支撑。

A high performance liquid chromatography tandem mass spectrometry(HPLC-MS)method was established for rapid screening and determination of 15 prohibited veterinary drugs in pork,chicken,beef and mutton.The sample was extracted by 1%(v/v)acetic acid acetonitrile,vortex mixing and ultrasonic assisted extraction.After repeated extraction,it was purified and degreased by extraction salt package,SCR purification column,Kinetex F5 pentafluorophenyl chromatographic column separation,electrospray ion source(ESI+)mode,multiple reaction monitoring mode(MRM)was used for detection,and external standard method was used for quantification.15 prohibited and restricted veterinary drugs have good linear relationship within the concentration range for 0.5~50μg/L(R2>0.997),and the limits of detection(LODs)and limits of quantification(LOQs)are lower than 1μg/kg,the recovery range of spiking is 78%~98%,and the relative standard deviation(RSDs)is 2.6%~8.3%(n=6).This method has the advantages of simple operation,stable recovery rate,low cost,etc.,and can be applied to the analysis of large quantities of samples,providing effective data support for risk monitoring.