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。
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 reac-tion 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 aver-age recoveries of the 20 psychoactive drugs spiked in blank pork at three levels of 5,10 and 50μg/kg were 66. 8%-97. 2% with the relative standard deviations from 4. 2% to 12. 4%. The meth-od is suitable for the simultaneous determination of the 20 psychoactive drugs in pork with the characteristics of easy operation,high accuracy and precision.
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