LC-MS／MS法检查中药制剂及保健食品中非法添加的16种镇静催眠药物.pdfVIP

中圊善科夫挚学报 l42 Journal of China Pharmaceutical University 2008，39(2)：142—146 LC—MS／MS法检查中药制剂及保健食品中 非法添加的16种镇静催眠药物 高 青 ，车宝泉，张 嚣，戴 红，郭洪祝 (北京市药品检验所，北京 100035) 摘 要 目的：建立准确、灵敏的LC—MS／MS方法甄别中药制剂及保健食品中可能添加的l6种化学镇静催眠药物，以 打击中药制剂及保健食品中非法添加化学药物现象。方法和结果：采用Waters Sunfire C． 色谱柱，梯度洗脱：流动相A为20 mmol／L醋酸铵溶液，流动相B为甲醇，检测波长为230 IqlTI，流速为1 mL／min(分流比为4：1)。选择正负离子全扫描方式检 测临床常用的16种镇静催眠药物。利用质谱解析软件研究上述药物的质谱裂解规律，通过比较样品峰与对照品峰的一级 质谱、二级质谱质荷比，确定样品中是否掺杂了化学药物。LC—MS／MS方法测定上述化学物质的最小检出量为l～40 ng。 结论：该方法简便、快捷，灵敏度、准确性均可满足定性检查的要求。 关键词 镇静催眠药物；LC—MS／MS；中药制剂；保健食品 中图分类号 R917；R927．1 文献标识码 A 文章编号 1000—5048(2008)02—0142—05 Identification of 16 sedative-hypnotic drugs in traditional Chinese medicines and health foods by LC-MS／MS GAO Qing ，CHE Bao—quart，ZHANG Zhe，DAI Hong，GUO Hong—zhu 觇 ， Institute for Drug Control，Bering 100035，China Abstract Aim：To develop HPLC—electrospray ion trap mass spectrometry(Finnigan LCQ)for the analysis of 16 sedative．hypnotic drugs illegally adulterated into the traditional Chinese medicinesf TCM1 and health foods． Methods：The separation was conducted on a Sunfire C I R column using a mobile phase consisting of 20 nmoL／L ammonium acetate and methanol f 4：6 1 at a flow rat of 1 mL／min after the organic solvent．extraction of interests from TCM preparations．The mass spectrometer was operated in positive ion or negative mode and in three scan modes including fu】】scan MS．selected ion monitoring and fu】】scan MS ．The obtained pseudomolecular ions and product ions were used to identify whether these drugs were present in the mdeicines．Results：HPLC and MS resolution of the 16 sedative．hypnotic drugs were good．The limits of detection were 140 ng．Conclusion： The method proved specificity．rapidness and sensitivity in the quantitation． Key words sedative．hypnotic drugs；LC．Ms／MS：traditional Chinese medicines；health food