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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1.56~218.2 ng·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 establish a method for simultaneous determination of 24 prohibited psychotropic substances in health food by ultra performance liquid chromatography-mass spectrometry (UPLC-ESI-Q-TOF / MS). Methods: The samples were extracted by ultrasonic oscillation of methanol and filtered through a 0.22μm filter. The separation was performed on an Agilent Eclipse Plus C18 column using a mobile phase of 0.1% formic acid (A), 0.1% formic acid-methanol (B), gradient elution; electrospray ionization, positive and negative ion mode, Level precision qualitative qualitative qualitative ion qubit ion level quantitative detection. Results: The linear range of 24 psychotropic drugs was good, the correlation coefficient was greater than 0.990, the detection limit was between 1.56 ~ 218.2 ng · ml-1, the recovery rate was 64.60% -99.33%, and the relative standard deviations were less than 7 %. Conclusion: The method is selective, sensitive and simple in treatment. It can be used in the screening and determination of banned and sedative chemicals in health products.