Sun Ting, Wang Luxiao, Zeng Sanmei, Wu Min, Yan Lijuan, Zhang Feng, Huang Zhiqiang
Se Pu. 2014 Jul;32(7):702-6. doi: 10.3724/sp.j.1123.2014.03002.
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 x 2.1 mm, 1.7 microm) 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 microg/L with the correlation coefficients more than 0.99 for the 20 psychoactive drugs. The limits of quantification (LOQ, S/N > or = 10) for the 20 psychoactive drugs were 5 microg/kg. The average recoveries of the 20 psychoactive drugs spiked in blank pork at three levels of 5, 10 and 50 microg/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.
建立了一种固相萃取结合超高效液相色谱-电喷雾电离串联质谱法（UPLC-ESI-MS/MS）同时测定猪肉中20种精神活性药物的方法。样品用碱化乙腈提取，然后用Oasis MCX柱进行固相萃取净化。UPLC分离在C18柱（50 mm×2.1 mm，1.7μm）上进行，流动相为0.1%（v/v）甲酸水溶液和乙腈，采用梯度洗脱。ESI-MS/MS检测在正离子模式下的多反应监测（MRM）模式下进行。校准曲线在5-100μg/L范围内呈良好线性，20种精神活性药物的相关系数均大于0.99。20种精神活性药物的定量限（LOQ，S/N≥10）为5μg/kg。在空白猪肉中添加5、10和50μg/kg三个水平的20种精神活性药物，平均回收率为66.8%-97.2%，相对标准偏差为4.2%-12.4%。该方法操作简便、准确度和精密度高，适用于同时测定猪肉中的20种精神活性药物。
