超高效液相色谱-串联三重四极杆线性离子阱质谱法同时检测猪肉中33种兽药残留

Simultaneous Determination of 33 Veterinary Drugs in Pork by Ultra Performance Liquid Chromatography-Tandem Tripe-Quadrupole Linear Ion Trap Mass Spectrometry

建立了利用QuEChERS方法与中空纤维素膜净化相结合的样品前处理技术,以及超高效液相色谱-串联三重四极杆线性离子阱质谱(UPLC-QTrap MS/MS)检测技术,同时分析猪肉中33种兽药残留的新方法。样品用乙腈溶液提取,提取液经PSA与C18混合填料及聚丙烯中空纤维超滤膜净化。采用C18色谱柱分离,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相,进行梯度洗脱。使用电喷雾正离子源(ESI+),在多反应监测(MRM)模式下检测。结果表明,33种兽药标准曲线的线性关系良好,相关系数r大于0.9901。猪肉样品中,3种兽药的定量限为2.0μg·kg^(-1),其余30种为0.5μg·kg^(-1),回收率为57.1%~102.3%,相对标准偏差(RSD,n=3)为1.7%~22.8%。

A method has been developed for the simultaneous determination of 33 veterinary drugs in pork using ultra performance liquid chromatography-tandem tripe-quadrupole linear ion trap mass spectrometry（UPLC-Qtrap MS/MS）and QuEChERS combined with hollow fiber membrane.The sample was extracted with acetonitrile,and then cleaned up by PSA and C18 mixed packing and polypropylene hollow fiber ultrafiltration membrane.With the mobile phases of 0.1%formic acid water solution and 0.1%formic acid acetonitrile solution,agradient elution was implemented.The separation was performed by a C18 column.The ESI-MS/MS detection was achieved in positive mode under multiple reactions monitoring（MRM）mode.The linear relationships of the standard curves of the drugs are good with the correlation coefficients greater than 0.9901.The limits of quantitative of 3 veterinary drugs are 0.5μg·kg^-1 and others are 2.0μg·kg^-1 in pork.The recoveries of the 33 veterinary drugs are 57.1%-102.3%.