HPLC法测定黄连中主要生物碱的方法学研究

Study on methodology for determination of main alkaloids in Rhizoma Coptidis by HPLC

目的建立2010年版《中国药典》黄连项下主要生物碱的含量测定方法。方法以十八烷基硅烷键合硅胶为填充剂;流动相为乙腈-50mmol/L磷酸二氢钾溶液(50∶50)(混合液中加15mmol/L十二烷基硫酸钠,再以磷酸调节pH为4.0);流速0.6ml/min;检测波长345nm;柱温:30℃。结果盐酸表小檗碱、盐酸黄连碱、盐酸巴马汀、盐酸小檗碱的线性范围依次为0.0113-0.7240μg、0.0218-1.3920μg、0.0148-0.9440μg、0.0719-4.6020μg;加样回收率依次为98.61%、99.70%、98.26%、100.20%,RSD依次为1.4%、1.3%、1.3%、1.5%。结论该方法简便、准确、可靠,可作为2010年版《中国药典》黄连质量标准中的含量测定方法 。

Objective To establish an HPLC method to determine the main alkaloids of the Coptidis for Chinese Pharmacopoeia of 2010 edition.Methods The C18 column was used.The mobile phase was CH3CN-50 mmol/L KH2PO4（50∶50）（containing 15 mmol/L SDS and adjusting pH=4.0 with H3PO4） at the flow rate of 0.6 ml/min,the detective wavelength was 345 nm and the column temperature was 30℃.Results The linear ranges of epiberberine hydrochloride,coptisine hydrochloride,palmatine hydrochloride and berberine hydrochloride were at 0.0113-0.7240 μg,0.0218-1.3920 μg,0.0148-0.9440 μg and 0.0719-4.6020 μg respectively.The average recoveries were 98.61%,99.70%,98.26%and100.20%;and RSD were 1.4%,1.3%and1.3%,1.5% respectively.Conclusion The method is simple and accurate,and can be used to determine the contents of epiberberine,coptisine,palmatine,and berberine in the Coptidis.