大活络丸中贵细药的质量控制研究

目的：建立大活络丸中体外培育牛黄、人工麝香等贵细药的检测方法。方法：采用HPLC-MS/MS 法对大活络丸中的胆酸进行测定；使用Phenomenex Kinetex C18 色谱柱（2.10 mm×100 mm，2.6 μm），以乙腈-0.2% 醋酸（35:65）为流动相，流速0.2 mL·min^-1；电喷雾电离源（ESI），正离子扫描，扫描方式多反应监测（MRM）。采用气相色谱法对大活络丸中的麝香酮进行测定；使用Optima-17 MS 毛细管柱（30m×0.32 mm×0.25 μm）毛细管柱，柱温180 ℃，分流进样。结果：胆酸进样量在0.152~19.0 ng 范围内线性关系良好；平均回收率为95.94 %（RSD=4.03%，n=9）。麝香酮进样量在0.014 30~0.357 6 μg 范围内线性关系良好；平均回收率为95.36%（RSD=3.58%，n=6）。测定结果表明，有部分样品中胆酸和麝香酮含量均偏低。结论：所建立的方法经方法学验证，可作为大活络丸的质量控制方法。

Objective:To develop a method for the determination of valuable medicines such as Bovis Calculus Sativus and Moschus Artifactus in Dahuoluo pills.Methods:An HPLC-MS/MS method was employed for the determination of cholic acid in Dahuoluo pills.The column of Phenomenex Kinetex C18(2.10 mm×100 mm,2.6 μm)was adopted,and the mixture of acetonitrile and 0.2% acetic acid(35:65)was used as mobile phase with the flow rate of 0.2 mL·min^-1.The ion source was ESI+ and operated in multi-reaction monitoring(MRM)mode. Furthermore,GC method was useed for the determination of muscone.A column of Optima-17 MS(30 m×0.32 mm×0.25 μm)was used,the column temperature was controlled at 180 ℃,and the injector was operated in split mode.Results:Cholic acid has good linear relationship in the range of 0.152-19.0 ng,and the average recovery of cholic acid was 95.94%(RSD=4.03%,n=9).Muscone has good linear relationshipin the range of 0.014 30- 0.357 6 μg,and its average recovery was 95.36%(RSD=3.58%,n=6).The detection results demonstrated that the contents of cholic acid and muscone in some samples were lower than others.Conclusion:The developed method is proved by methodology validation that it can be used in the quality control of Dahuoluo pills.