高效液相色谱-蒸发光散射检测器法测定肾宝片及其中间体中黄芪甲苷的含量

HPLC-ELSD Determination of Astragaloside Ⅳ in Shenbao Tablets and In-process Materials

目的:建立肾宝片及其中间体中黄芪甲苷 HPLC-ELSD 的分析方法。方法:采用 Alltech C_(18)色谱柱(250mm×4.6mm,5μm),以乙腈-水(35:65)为流动相,流速0.9 mL·min^(-1),ELSD 参数:漂移管温度100℃,氮气流速2.80 L·miN^(-1)。结果:黄芪甲苷在3.50～70.0μg·mL^(-1)范围内线性关系良好(r=0.9998),平均回收率为98.9%,RSD 为2.7%,经2次醇沉后黄芪甲苷的含量变化小于5%。结论:该方法准确,重现性好,为肾宝片及其中间体的质量控制提供了一种检测方法,以利于验证该制剂工艺的可行性。

Objective：To establish an HPLC - EKSD method for the determination of astragaloside Ⅳ in Shenbao tablets and in - process materials. Method ： HPLC system consisting of an Alhech C18 column （250 mm × 4.6 mm, 5μm）and a mixture of acetonitrile -water（ 35：65 ）as the mobile phase was adopted with flow rate of 0.9 mL·min^-1. The detector temperature was 100℃ and the flow rate of N2 was 2.80 L·min^-1. Results：Astragaloside Ⅳ showed good linearity （r = 0.9998 ）in the range of 3.50 -70.0μg·mL^-1. The average recovery was 98.9% , the RSD was 2.7%. The content difference of astragaloside Ⅳ in in - process materials was less than 5% even after twice alcohol precipitation. Conclusion：This method possesses merits of good accuracy and reproducibility. The method can be used for the quality control of Shenbao tablets and in - process materials and validate the manufacture technology of Shenbao tablets.