液质联用法筛查降压类中成药和保健食品中添加的54种化学药物

Screening of 54 illegally added chemical drugs in anti-hypertensive Chinese traditional patent medicine and health foods by liquid chromatography tandem mass spectrometry

目的:建立液相色谱-串联质谱法测定降压类中成药和保健食品中54种非法添加的化学药物。方法:样品以甲醇为溶剂超声提取后,采用Agilent Poroshell EC-C_(18)(100 mm×2.1 mm,2.7μm)色谱柱分离,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相梯度洗脱,采用电喷雾离子源正、负离子模式,多重反应监测(MRM)检测。结果:所有化合物在定量范围内相关系数均大于0.995,检测下限均在0.1～16 ng·mL^(-1)范围内,3个浓度平均加标回收率均高于50%。用本法筛查12批降压类市售样品,检出4批含有非法添加物。结论:该方法专属、灵敏、快捷,可用于筛查降压类中成药和保健食品中非法添加的化学药物。

Objective：To establish a high performance liquid chromatography tandem mass spectrometric（LC-MS/MS）method for the determination of 54 illegally added chemical drugs in anti-hypertensive Chinese traditional patent medicine and health foods.Methods：The analytes were extracted from samples with methanol,separated on a Poroshell EC-C_（18）（100 mm×2.1 mm,2.7 μm）column by a gradient elution with the mobile phase of 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile solution at a flow rate of 0.3 mL·min^（-1）.The compounds were detected by electrospray ion source in both positive and negative modes with multiple reaction monitoring（MRM）modes.Results：The detection limit of each component was 0.1-16 ng·mL^（-1）,and calibration curves showed good linearity with r0.995.The method was validated by evaluating the recovery after addition of the standard mixture into real samples（50%）.This method proposed is used to screen 12 batches of practical samples and 4 batches of samples containing illegal added chemical drugs.Conclusion：The method is specific,sensitive,simple,and rapid,which can be used for the screening of illegally added chemical drugs in anti-hypertensive Chinesetraditional patent medicine and health foods of pressure-relief samples.