固相萃取-超高效液相色谱-串联质谱法同时测定猪肉中20种精神药物残留

建立了固相萃取和超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)同时测定猪肉中20种精神药物残留的方法。样品采用碱性乙腈作为提取试剂,提取液经Oasis MCX固相萃取柱净化后,以含0.1%(v/v)甲酸的水溶液和乙腈作为流动相梯度洗脱,用C18色谱柱分离,正离子模式扫描,多反应监测模式检测。20种化合物在5~100μg/L质量浓度范围内均呈良好的线性关系,线性相关系数均大于0.99,以S/N≥10计算方法的定量限为5μg/kg。在空白猪肉中添加5、10和50μg/kg水平的20种药物,其平均回收率为66.8%~97.2%,相对标准偏差(RSD)为4.2%~12.4%。本方法快速、准确、可靠,适用于猪肉中精神药物多残留的同时测定。

Simultaneous determination of twenty psychoactive drugs in pork by solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

A method for the simultaneous determination of 20 psychoactive drugs in pork by solid phase extraction coupled with ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was established. The samples were extracted with alkalified acetonitrile, and then cleaned up using solid phase extraction with an Oasis MCX column. The UPLC separation was performed on a C18 column (50 mm×2.1 mm, 1.7 μm) using a gradient elution with the mobile phases of 0.1% (v/v) formic acid in water and acetonitrile. The ESI-MS/MS detection was achieved in positive mode under multiple reaction monitoring (MRM) mode. The calibration curves showed good linearity in the range of 5-100 μg/L with the correlation coefficients more than 0.99 for the 20 psychoactive drugs. The limits of quantification (LOQ, S/N≥10) for the 20 psychoactive drugs were 5 μg/kg. The average recoveries of the 20 psychoactive drugs spiked in blank pork at three levels of 5, 10 and 50 μg/kg were 66.8%-97.2% with the relative standard deviations from 4.2% to 12.4%. The method is suitable for the simultaneous determination of the 20 psychoactive drugs in pork with the characteristics of easy operation, high accuracy and precision.