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

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-C₁₈（100 mm×2.1 mm，2.7 μm）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-C₁₈(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 r>0.995.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.