HPLC测定胃康宁颗粒中5种指标成分含量

Content Determination of Five Marker Components in Weikangning Granules by HPLC

目的建立胃康宁颗粒中指标成分表小檗碱、黄连碱、盐酸巴马汀、盐酸小檗碱和黄芩苷的含量测定方法,为胃康宁颗粒的质量控制提供依据。方法采用HPLC,色谱柱Agilent Eclipse Plus C18为(4.6 mm×250 mm,5μm)。黄连生物碱流动相为乙腈-0.05 mol/L磷酸二氢钾溶液(50∶50,每100 mL中加十二烷基硫酸钠0.4g,再以磷酸调节pH值为4.0),检测波长为345nm;黄芩苷流动相为乙腈-0.2%磷酸(21∶79),检测波长为280nm。结果黄连生物碱及黄芩苷测定均无阴性干扰,表小檗碱、黄连碱、盐酸巴马汀、盐酸小檗碱及黄芩苷的进样量分别在0.005 26～0.211μg(r=0.999 6)、0.005 37～0.215μg(r=1)、0.005 55～0.222μg(r=1)、0.028 06～1.123μg(r=1)、0.096 5～1.930μg(r=0.999 8)范围内线性关系良好,精密度、稳定性均良好,平均回收率分别为97.63%(RSD=2.32%)、99.05%(RSD=2.21%)、97.66%(RSD=1.94%)、101.50%(RSD=1.92%)、100.31%(RSD=1.12%)。结论本方法准确、稳定、重复性好,可用于胃康宁颗粒中表小檗碱、黄连碱、盐酸巴马汀、盐酸小檗碱和黄芩苷的含量测定。

Objective To establish an HPLC method for content determination of epiberberine, coptisine, palmatine, berberine and baicalin; To provide the basis for the quality control standard of Weikangning Granules. Methods Agilent Eclipse Plus C18 column （4.6 mm × 250 mm, 5 μm） was used. For rhizoma coptidis alkaloids, mobile phase was acetonitrile - 0.05 mol/L potassium dihydrogen phosphate solution （50：50, 0.4 g sodium dodecyl sulfate was added in each 100 mL, to adjust the pH 4.0 with phosphoric acid）, and detection wavelength was 345 nm; For baicalin, mobile phase was acetonitrile - 0.2% phosphoric acid solution （21：79）, and detection wavelength was 280 nm. Results No negative interference was found in determination of rhizoma coptidis alkaloids and baicalin. Epiberberine, coptisine, palmatine, berberine and baicalin showed good liner relationship in the range of 0.005 26– 0.211 μg （r=0.999 6）, 0.005 37–0.215 μg （r=1）, 0.005 55–0.222 μg （r=1）, 0.028 06–1.123 μg （r=1）, 0.096 5–1.930 μg （r=0.999 8）; degree of precision of instrument and the stability of samples were good. The average recovery rates were 97.63% （RSD=2.32%）, 99.05% （RSD=2.21%）, 97.66% （RSD=1.94%）, 101.50% （RSD=1.92%） and 100.31% （RSD=1.12%）, respectively. Conclusion The method is accurate, stable and reproducible. It can be used for the content determination of epiberberine, coptisine, palmatine, berberine and baicalin of Weikangning Granules.