摘要
目的：建立超高效液相色谱-质谱法（UPLC—ESI-Q-TOF／MS）同时测定保健食品中24种违禁精神药品的检测方法。方法：样品经甲醇超声振荡提取，0．22μm滤膜过滤后进样，分析。采用Agilent Eclipse Plus C18柱分离，流动相：0．1％甲酸（A），0．1％甲酸-甲醇（B），梯度洗脱；采用电喷雾离子源、正、负离子模式、利用Q-TOF的一、二级精密质量数进行定性，一级准分子离子峰定量检测。结果：24种精神药品在线性范围内线性关系良好，相关系数均大于0．990；检出限在1．56～218．2ng·ml^-1之间；回收率为64．60％～99．33％；相对标准偏差均小于7％。结论：该方法选择性强、灵敏度高、处理方法简单，可用于保健品中违禁镇静安神类化学药品的筛查与测定。
Objective： To develop an UPLC- ESI-Q-TOF/MS method for the analysis of 24 sedative-hypnotic drugs illegally added into health foods. Methods： The separation was conducted on an Agilent Eclipse Plus C18 column with the mobile phase consisting of 0.1% formic acid （A） and 0.1% formic acid-methanol （B）. The mass spectrometer was operated in a positive or negative ion mode, the identification was performed by MS2 scan and the determination was conducted in an MS scan mode. Results： The UPLC and MS resolution of the 24 sedative-hypnotic drugs were good. The limits of detection were 1.56-218.20ng·ml^-1, and the recoveries were 64.60%-99.33%. Conclusion： The method is specific, rapid and sensitive in the identification and quantitative determination of sedative-hypnotic drugs illegally added into health foods.
出处
《中国药师》
CAS
2015年第7期1129-1132,1135,共5页
China Pharmacist
基金
苏州市科学技术局科学计划项目(编号:SS201220)
