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16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 C18色谱柱,梯度洗脱:流动相A为20mmol/L醋酸铵溶液,流动相B为甲醇,检测波长为230 nm,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1~40 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。
Aim： To develop HPLC-electrospray ion trap 16 sedative-hypnotic drugs illegally adulterated into the mass spectrometry （Finnigan LCQ） for the analysis of traditional Chinese medicines（TCM） and health foods. Methods： The separation was conducted on a Sunfire C^8 column using a mobile phase consisting of 20 nmol/L ammonium acetate and methanol （4： 6） 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 full scan MS, selected ion monitoring and full scan MS2. 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 1-40 ng. Conclusion： The method proved specificity, rapidness and sensitivity in the quantitation.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2008年第2期142-146,共5页
Journal of China Pharmaceutical University
基金
北京市"2006药品安全及服务平台"资助项目(No.D02060260000703)~~
作者简介
通讯作者 Tel：010-66124424 E-mail：gaoqingq@sohu．com
