HPLC法测定黄连中主要生物碱的方法学研究

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 。

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

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.