LC-MS法检测消风止痒颗粒中马兜铃酸A

目的:建立检测消风止痒颗粒中马兜铃酸A的液相色谱-质谱分析方法。方法:采用Venusil mp C18(250 mm×4.6mm,5μm)色谱柱,流动相为乙腈-0.1%甲酸水溶液(40∶60),流速1.0 mL.min-1。采用电喷雾电离源正离子质谱检测。结果:马兜铃酸A在0.005086～0.4069μg范围内线性关系良好(r=1.000),平均回收率(n=7)为97.1%(RSD=2.1%)。87批制剂均未检出马兜铃酸A。结论:本法快速、灵敏、准确,可用于消风止痒颗粒中是否混入关木通的确证检查,以防马兜铃酸A造成的用药安全,为消风止痒颗粒的质量控制提供了科学依据。

LC-MS detection of aristolochic acid A in Xiaofeng Zhiyang granula

Objective: To establish an LC-MS method for detection of aristolochic acid A in Xiaofeng Zhiyang granula.Methods: The separation was performed on Venusil mp C18(250 mm×4.6 mm,5 μm)column with the mobile phase of acetonitrile-0.1% formic acid water-solution(40∶ 60)at a flow rate of 1.0 mL·min-1.The detection was done by positive-ion electrospray ionization mass spectrometry.Results: The linear range was 0.005086-0.4069 μg(r=1.000).The average recovery(n=7)was 97.1%(RSD=2.1%).In addition,aristolochic acid A was not detected in 87 preparations.Conclusion:The method is rapid,sensitive,and accurate for the detection of aristolochic acid A in Xiaofeng Zhiyang granula.Further more,the method can be used to corroborate the adulteration of Caulis Aristolochiae Manshuriensis in the preparations to avoid the misusage of aristolochic acid A,which can ensure medication safety.The study may provide a scientific basis for the quality control of Xiaofeng Zhiyang granula.