摘要
目的:建立山黄胶囊中盐酸小檗碱、黄芩苷含量测定的方法。方法:采用HPLC法,测定盐酸小檗碱含量的色谱柱为Phenomenex Gemini C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸(50:50),每100 m L加0.1 g十二烷基磺酸钠,流速为1.0 m L/min,检测波长为265 nm;测定黄芩苷含量的色谱柱为Phenomenex Luna C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水-磷酸(70:30:0.2),检测波长280 nm,流速0.6 m L/min。结果:盐酸小檗碱在5.08~50.80 g/m L范围内线性关系良好,R2=0.999 8,平均回收率为98.08%,RSD为1.09%。黄芩苷在15.03~150.30 g/m L范围内线性关系良好,R2=0.999 9,平均回收率为98.13%,RSD为1.28%。结论:该方法专属性强、准确性高、重复性好,可应用于山黄胶囊的质量控制。
Objective To develop a method for the determination of berberine hydrochloride and baicalin in Shanhuang capsule. Methods The assay of berberine hydrochloride was performed on Phenomenex Gemini C18column(250 mm× 4.6 mm,5 μm)with a DAD 265 nm.The mobile phase was acetonitrile-0.01% phosphate(50:50),join 0.1 g sodium dodecyl sulfate per 100 m L solution with a flow rate of 1.0 m L/min. The determination of baicalin was on a Phenomenex Luna C18column(250 mm ×4.6 mm,5 μm)with a DAD 280 nm.The mobile phase was methanol-water – phosphate(70:30:0.2) with a flow rate of 0.6 m L/min. Results The linear range of berberine hydrochloride was 5.08 ~50.80 g/m L,R2=0.999 8,and the average recovery ratio was 98.08%,RSD=1.09%; The linear range of baicalin was 15.03~150.30 g/m L,R2=0.999 9,and the average recovery ratio was 98.13%,RSD=1.28%.Conclusion The method is exclusive,accurate and reproducible,which may be applied in the quality control of Shanhuang capsule.