HPLC-Q-TOF/MS测定保健食品中19种抗抑郁药物

Determination of 19 antidepressants in health food by high-performance liquid chromatography-Time-of-flight mass spectrometry

目的:建立保健食品中非法添加19种抗抑郁药物的高效液相色谱-四极杆-飞行时间质谱快速筛查定性与定量分析方法。方法:样品采用甲醇溶液进行超声提取,提取液经C_(18)色谱柱分离,以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,在电喷雾正离子模式下进行检测,检测结果以试验方法建立的19种抗抑郁药物一级精确质量数据库和二级碎片质谱库进行筛查匹配。结果:在5~100μg/L质量浓度范围内,19种目标化合物线性关系良好,相关系数为0.9887~0.9999,在2,5,10μg/kg 3个加标水平下样品的回收率为81.2%~98.6%,相对标准偏差为0.9%~6.7%。结论:所建立的方法适用于保健食品中非法添加抗抑郁药物的快速筛查定性与定量分析。

Objective:To establish a rapid qualitative and quantitative analysis method,HPLC-quadrupole-time-of-flight mass spectrometry was used to determine the illegal addition of 19 antidepressants in healthy food.Methods:The samples were extracted by methanol with ultrasonic extraction procedure and then separated on a reversed-phase C_(18) column,with acetonitrile and 0.1%formic acid aqueous as the mobile phases in gradient elution mode.The target compounds were detected in electrospray positive ion,and the data were matched with the established database of precursor ion and secondary fragment accurate mass.Results:The linear range of the 19 compounds was 5~100μg/L,and the correlation coefficient was 0.9887~0.9999,with the detection limit of 0.2~2.0μg/kg.The average recoveries of the 19 antidepressants ranged from 81.2%to 98.6%,and the relative standard deviation was less than 6.7%.Conclusion:The established method is suitable for rapid screening qualitative and quantitative analysis of illegally added antidepressant drugs in healthy food.