论文部分内容阅读
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,2.6μm),以乙腈-0.2%醋酸(35∶65)为流动相,流速0.2 m L·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~(-1)7 MS毛细管柱(30 m×0.32 mm×0.25μm)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 6μg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 establish a method for the determination of Guihuang, artificial musk and other precious and drug substances in Oxytropis pills in vitro. Methods: Cholic acid was determined by HPLC-MS / MS in a large active pill. Phenomenex Kinetex C18 column (2.10 mm × 100 mm, 2.6 μm) and acetonitrile-0.2% acetic acid Phase, flow rate 0.2 m L · min ~ (-1), electrospray ionization source (ESI), positive ion scan, scanning multi-reaction monitoring (MRM) Determination of musk ketone in Zhuluo pills by gas chromatography was performed on a capillary column with Optima ~ (-1) 7 MS capillary column (30 m × 0.32 mm × 0.25 μm). The column temperature was 180 ℃. Results: The linearity of bile acid injection in the range of 0.152-19.0 ng was good. The average recovery was 95.94% (RSD = 4.03%, n = 9). Musk ketone injection volume in the range of 0.014 30 ~ 0.357 6μg good linear relationship; the average recovery was 95.36% (RSD = 3.58%, n = 6). Determination results show that some samples of bile acids and musk ketone levels are low. Conclusion: The established method is validated by methodology and can be used as a quality control method for Omeprazole.