黄连4种饮片特征图谱研究及生物碱含量测定

目的: 建立黄连4种不同炮制品的特征图谱,探讨饮片炮制前后化学成分的变化规律,并采用HPLC法对其中木兰碱、药根碱、黄连碱、巴马汀、小檗碱5个生物碱类成分进行定量分析比较。 方法: 采用Kromasil-C₁₈色谱柱 (4.6 mm×250 mm,5 μm);流动相乙腈-50 mmol·L^-1磷酸二氢钾溶液(磷酸调pH 3.0)(45: 55),内含十二烷基硫酸钠12.5 mmol·L^-1;检测波长275 nm;流速1 mL·min^-1;柱温为30℃;进样量10 μL。 结果: 所建立的特征图谱信息丰富,5个生物碱成分在测定范围内线性关系较好(r>0.9994),平均回收率分别为102.8%,96.9%,98.4%,104.8%,103.7%。 结论: 初步实验表明,黄连不同炮制品的特征图谱有所差别,相关成分在炮制前后发生了量变和质变,并呈现一定的变化规律。

Objective: To develop the HPLC specific chromatograms of four kinds of processed Rhizoma Coptis, to explore the regularity of component changes in processing of Rhizoma Coptis, and use HPLC to quantitatively analyze and compare magnoflorine, jatrorrhizine, coptisine, palmatine, berberine proportions . Method: The separation was performed on an Kromasil -C₁₈ column(250 mm×4.6 mm, 5 μm)with the mobile phase consisting of acetonitrile-0.05 mol·L^-1 potassium phosphate(adjusting pH=3.0 with phosphoric acid)(45: 55), containing 12.5 mmol·L^-1 SDS; The column temperature was set at 30℃. The flow rate was 1.0 mL·min^-1 and the injection volume was 10 μL. Detection wavelength was set at 275 nm. Results: The information of HPLC specific chromatogram was abundant. Other components’ proportion was increasing in different level except coptisine and epiberberine in Rhizoma Coptis processed with wine; the majority of components’ proportion increased obviously in Rhizoma Coptis processed with ginger juice; other components’ proportion increased slightly except magnoflorine in Rhizoma Coptis processed with Fructus Evodiae; The linear correlation of five alkaloids are good(r>0.9994), The average recoveries of five components were 102.8%,96.9%,98.4%,104.8%,and 103.7%. Conclusion: The HPLC specific chromatograms were varied in different processed products, all the component changed in quantity and quality after processing,and some regularity of changing was observed.