UPLC-MS/MS定性定量检测清脑保心康胶囊中非法添加的利血平

摘要

Objective To establish an UPLC-MS/MS method for determination of reserpine in Health Food. Methods Ultra performance liquid chromatography tandem three quadrupole mass spectrometer was adopted, LC condition:A agela Venusil ASB-C18(2.1 mm×50 mm,3 μm) column was used with the isocrstic elution of acetonitrile and 0.2% Formic acid at a flow rate 0.2 mL•min-1.MS/MS condition: adopted electrospray ionization(ESI),and multiple reaction monitoring, The relative intensities of the detected qualitative ion pairs using for qualitative, integrating the signals of the detected quantitative ion pairs using for quantitative. Results The reserpine had good linearity with correlation coefficient>0.9998, ranging from 1.092~27.300 ng/mL.The average recovery was 98.24%.The limit of quantitation was 109.2pg. Conclusion This method is reliable qualitative and quantitative accuracy, simple and rapid, and can be used for Health Food illegally added reserpine detection.%　　目的建立 UPLC-MS/MS 方法,快速定性定量检测保健食品中非法添加的利血平.方法采用超高效液相色谱串联三重四极杆质谱仪,色谱条件：Agela Venusil ASB-C18(2.1 mm×50mm,3μm)色谱柱,柱温35℃,流动相为：乙腈-0.2%甲酸水溶液=65∶35,流速为0.2 mL/min.质谱条件：ESI 源,多反应检测(MRM).以保留时间及定性离子对之间的相对丰度定性,以定量离子对峰面积定量.结果利血平在1.092~54.600 ng/mL 范围内呈现良好的线性关系(r >0.9998)；平均加样回收率98.24%；定量限为109.2pg.结论本方法定性可靠、定量准确,且快速简便,可用于保健食品中非法添加利血平的检测.