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目的:建立抗癫痫中成药中非法添加苯巴比妥和卡马西平的UPLC-MS/MS检测方法。方法:采用Waters ACQUITY UPLC/Quattro Premier液质联用仪,以BEH-C18(100 mm×2.1 mm,1.7μm)色谱柱分离,0.02 mol·L-1醋酸铵水溶液-乙腈(1∶1)为流动相,质谱检测器采用多反应监测(MRM)模式进行定性定量检测;供试样品的处理,采用以甲醇为溶剂的超声提取方法。结果:苯巴比妥和卡马西平的保留时间分别为1.1 min和1.3 min,检测限分别为2.2μg·mL-1和0.10μg·mL-1,定量限分别为7.5μg·mL-1和0.35μg·mL-1,标准曲线范围分别为11.2~112μg·mL-1和1.04~52μg·mL-1,重复性的RSD(n=6)分别为3.7%和1.7%,3种浓度的平均回收率分别为101.3%~105.4%和98.8%~101.0%,日间精密度的RSD(n=9)分别为2.7%和1.7%。9批样品中3批检出苯巴比妥,1批检出苯巴比妥和卡马西平。结论:本方法专属性强,操作简单,快捷,可作为中成药中非法添加苯巴比妥和卡马西平的有效检测方法。
OBJECTIVE: To establish a UPLC-MS / MS method for the detection of phenobarbital and carbamazepine illegally added to Chinese epilepsy proprietary Chinese medicines. METHODS: The chromatographic separation was performed on a BEH-C18 (100 mm × 2.1 mm, 1.7 μm) column using a Waters ACQUITY UPLC / Quattro Premier mass spectrometer with 0.02 mol·L -1 ammonium acetate in water (1: 1) Mobile phase and mass spectrometry detector were used for qualitative and quantitative detection by multi-reaction monitoring (MRM) mode. The samples were processed by ultrasonic extraction using methanol as solvent. Results: The retention times of phenobarbital and carbamazepine were 1.1 min and 1.3 min, respectively. The detection limits were 2.2 μg · mL-1 and 0.10 μg · mL-1, respectively. The limits of quantification were 7.5 μg · mL-1 and The standard curves ranged from 11.2 to 112 μg · mL-1 and 1.04 to 52 μg · mL-1, respectively. The repeatability of RSD (n = 6) were 3.7% and 1.7% The recoveries ranged from 101.3% to 105.4% and from 98.8% to 101.0%, respectively. The intraday precision RSD (n = 9) was 2.7% and 1.7%, respectively. Phenobarbital was detected in 3 lots in 9 batches of samples and phenobarbital and carbamazepine in 1 batch. Conclusion: This method is specific, easy to operate and fast, and can be used as an effective detection method of phenobarbital and carbamazepine illegally added in Chinese patent medicines.