超高效液相色谱-四极杆串联飞行时间质谱定性定量检测保健食品及中成药中非法添加的25种降压类化合物

Qualitative and quantitative analysis of 25 hypotensive compounds in health care foods and traditional Chinese medicines using ultra performance liquid chromatography/quadrupoletime-of-flight mass spectrometry

目的:建立超高效液相色谱-四极杆串联飞行时间质谱(UPLC/Q-TOF-MS)快速定性定量检测保健食品及中成药中的25种降压类化合物。方法:采用Agilent ZORBAX SB-C(18)色谱柱(2.1 mm××50 mm,1.8μm)进行分离,流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,流速0.5 mL·min^-1;质谱采用电喷雾离子源,正离子模式,通过与对照品峰的保留时间、一级质谱精确相对分子质量、二级质谱碎片离子来定性,通过提取离子流色谱图峰面积与浓度的线性关系定量。结果:25种降压类化合物在相应浓度范围内线性良好(r≥0.996 5),精密度均小于3.5%,回收率处于83.4%~111.6%之间。采用已建立的方法,对15批市售辅助降血压类保健食品和中成药进行检测,结果1批软胶囊中检出厄贝沙坦,含量为10.8 mg·粒^-1。结论:实验所建立方法准确,灵敏度高,适用于常见降压类化合物的快速检测。

Objective:To establish a method for qualitative and quantitative analysis of hypotensive compounds in health care foods and traditional Chinese medicines using ultra performance liquid chromatography/quadrupole-time-offlight mass spectrometry(UPLC/Q-TOF-MS).Methods:The samples were separated b y Agilent ZORBAX SB-C18 column(2.1 mm × 50 mm,1.8μm)with 0.1%formic acid-water solution and acetonitrile as the mobile phase at a flow rate of 0.5 mL·min^-1 with gradient elution.Electronic spray ion(ESI)in positive ionization mode was performed in mass.Qualitative analysis was based on comparison of the retention time,accurate relative molecular mass and product ions with those of reference substances.Quantitative analysis was performed by using the linear relationship between the peak area and concentration of each hypotensive compound.Results:Good linearity was obtained in corresponding concentration of the 25 hypotensive compounds(r ≥ 0.996 5).The precisions were satisfactory with RSDs below 3.5%,and the recoveries were between 83.4% and 111.6%.The established method was used to test 15 batches of marketable health care foods and traditional Chinese medicines.Irbesartan was detected in one batch of soft capsule and the content of irbesartan was 10.8 mg per capsule.Conclusion:The established method is accurate with high sensitivity,and suitable for determination of common hypotensive compounds in health care foods and traditional Chinese medicines.