利湿通淋颗粒中小檗碱和益母草碱的质量控制

Quality control of berberine and leonurine in Lishitonglin Granules

建立了利湿通淋颗粒中小檗碱和益母草碱的质量控制方法。采用Diamonsil C18柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸溶液(体积比为50:50),且每100 mL加十二烷基硫酸钠0.1 g溶液为流动相,流速为1.0 mL/min,检测波长为265 nm测定小檗碱的含量;采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.4%辛烷磺酸钠的0.1%磷酸溶液(体积比为24:76)为流动相,流速为1.0 mL/min,检测波长为277 nm测定益母草碱的含量。结果显示,小檗碱在0.052~0.520μg质量范围内(r=0.9996),益母草碱在0.0396~0.3960μg质量范围内(r=0.9991),进样量与峰面积均呈良好的线性关系。小檗碱的加样回收率为98.51%~102.1%,相对标准偏差为2.08%(n=6);益母草碱的加样回收率为99.90%~102.6%,相对标准偏差为1.13%(n=6)。该含量测定方法专属性强、重现性好、操作简便,可用于利湿通淋颗粒的质量控制。

A quality control method to quantify berberine and leonurine in Lishitonglin Granules via HPLC was established.The content of berberine was determined using the Diamonsil-C18 chromatographic column(250 mm×4.6 mm,5μm)and acetonitrile-0.1%phosphoric acid(50:50,V/V)solution with 0.1 g sodium dodecyl sulfate per 100 mL of the solution as the mobile phase.The flow rate was 1.0 mL/min,and the detection wavelength was 265 nm.The content of leonurine was determined using the Diamonsil-C18 chromatographic column(250 mm×4.6 mm,5μm).The mobile phase was acetonitrile-0.1%phosphoric acid solution(24:76,V/V)containing 0.4%sodium octane sulfonate.The flow rate was 1.0 mL/min,and the detection wavelength was 277 nm.The results showed that berberine was linear in the range of 0.052~0.520μg(r=0.9996)and leonurine was linear in the range of 0.0396~0.3960μg(r=0.9991).Further,there was a good linear relationship between injection volume and peak area.The recovery rate of berberine was 98.51%~102.1%,with relative standard deviation(RSD)of 2.08%(n=6).The recovery rate of leonurine was 99.90%~102.6%,with RSD of 1.13%(n=6).The established method has high specificity,good reproducibility,and ease of operation and can be used for the quality control analysis of Lishitonglin Granules.