QuEChERS-超高效液相色谱-质谱联用法测定熊胆粉中9种苯二氮䓬类药物残留量

Simultaneous Determination of Nine of Benzodiazepine Residues in Bear Bile Powder by QuEChERS-UPLC-MS/MS

关键词:  超高效液相色谱-质谱联用法  熊胆粉  苯二氮䓬类药物  残留量

Key words:  ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS)  bear bile powder  benzodiazepine drug  residues

摘要:

建立了超高效液相色谱-质谱联用法(UPLC-MS/MS)快速测定中药材熊胆粉中9种苯二氮?类药物残留的方法。样品以乙腈为提取溶剂，经萃取盐包除杂提取，采用分散式固相萃取管 (EMR-Lipid dSPE) 净化，ACQUITY BEH C18色谱柱(1.7 μm，2.1×100 mm)分离，多反应监测模式(MRM)采集数据，外标法定量。在优化的条件下，虽9种药物存在不同程度的基质效应，但不影响检测结果的准确性。方法学考察结果显示，9种苯二氮?类药物在对应的浓度范围内线性关系良好，决定系数(R²)≥0.9961，方法检出限(LOD，S/N =3)在0.06～0.71 μg/kg范围内，定量限(LOQ，S/N =10)在0.20～2.60 μg/kg范围内，3个加标水平的平均回收率在69.1%～108.0%范围内，日内RSD为1.8%～9.0%，日间RSD为2.6%～9.3%。该方法前处理操作简便、重现性好，准确度高，为熊胆粉中苯二氮?类药物残留的风险监控提供了一种有效的检测技术。

Abstract:

An method of ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS) was developed for the rapid determination of nine benzodiazepines in Chinese traditional medicine of bear bile powder. The samples were extracted by acetonitrile, impurities was removed under the role of salt package, cleaned up by enhanced matrix removal lipid-dispersed solid phase extraction (EMR-Lipid dSPE). The separation was performed on an ACQUITY BEH C18 column (1.7 μm, 2.1×100 mm)，the data were collected in multiple reaction monitoring mode (MRM), and quantified by external standard method. Under the optimized conditions, the accuracy of the detection results was not affected by the matrix effect of 9 drugs. Methodological investigation results show that there are good linear relationships for the 9 analytes in the corresponding concentration ranges with their coefficient of determination (R²) not less than 0.9961, the limits of detection (LOD, S/N=3) of the method were in the range of 0.06 ~ 0.71 μg/kg, the limits of quantification (LOQ, S/N=10) were in the range of 0.20 ~ 2.60 μg/kg,the average recoveries of the three spiked levels were in the range of 69.1% ~ 108.0%, the relative standard deviations (RSD) of intra-day and inter-day were in the range of 1.8%～9.0% and 2.6%～9.3%, respectively. The method was simple, reproducible and sensitive, and providing an effective detection technology for the monitoring and risk control of nine of benzodiazepine residues in bear bile powder.