芪龙活络颗粒质量标准研究

Quality Standard of Qilong Huoluo Granules

目的建立芪龙活络颗粒的质量标准。方法采用薄层色谱法对制剂中黄芪、川牛膝、鸡血藤药材进行定性鉴别;采用高效液相色谱法测定丹酚酸B的含量,色谱柱为Eclipse XDB-C_(18)柱(150 mm×4.6 mm,5µm),流动相为乙腈-0.1%磷酸溶液(23∶77,V/V),流速为1.0 mL/min,检测波长为286 nm,柱温为30℃,进样量为10µL。结果薄层色谱斑点清晰,且阴性对照无干扰。丹酚酸B的进样量在0.0624~1.248µg范围内与峰面积线性关系良好(r=1.000,n=5);精密度、稳定性、重复性试验结果的RSD均小于2.00%(n=6);平均回收率为107.61%,RSD为4.28%(n=6)。5批样品中丹酚酸B的含量为1.09~1.32 mg/g。结论该方法专属性好、结果准确,可用于芪龙活络颗粒的质量控制。暂订芪龙活络颗粒中丹酚酸B的含量应不低于1.0 mg/g。

Objective To establish the quality standard of Qilong Huoluo Granules.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify Cyathulae Radix,Astragali Radix,and Spatholobi Caulis in the preparation.High-performance liquid chromatography(HPLC)method was used to determine the content of salvianolic acid B in the preparation,the chromatographic column was Eclipse XDB-C_(18)column(150 mm×4.6 mm,5µm),the mobile phase was acetonitrile-0.1%phosphoric acid solution(23∶77,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 286 nm,the column temperature was 30℃,and the injection volume was 10µL.Results The TLC spots were clear,and the negative control had no interference.The linear range of salvianolic acid B was 0.0624-1.248µg(r=1.000,n=6).The RSDs of precision,stability,and repeatability test results were all lower than 2.00%(n=6).The average recovery of salvianolic acid B was 107.61%with an RSD of 4.28%(n=6).The content of salvianolic acid B in five batches of samples was in the range of 1.09-1.32 mg/g.Conclusion This method is specific and accurate,which can be used for the quality control of Qilong Huoluo Granules.The content of salvianolic acid B in Qilong Huoluo Granules is temporarily set at no lower than 1.0 mg/g.