高效液相半制备色谱法制备决明酮-8-O-β-D-吡喃葡萄糖苷对照品

Preparation of Torachrysone-8-O-β-D-glucopyranoside Reference Substance from Polygoni Cuspidati Rhizoma et Radix by Semi-preparative HPLC

目的制备用于含量测定的决明酮-8-O-β-D-吡喃葡萄糖苷对照品。方法采用大孔吸附树脂柱和ODS柱色谱结合高效液相半制备色谱进行分离,质谱和核磁共振波谱数据鉴定结构,高效液相色谱不加校正因子的主成分自身对照法检测纯度。结果从虎杖中分离制备了符合含量测定用要求的决明酮-8-O-β-D-吡喃葡萄糖苷对照品,HPLC检测质量分数>98.0%。结论本研究制备的决明酮-8-O-β-D-吡喃葡萄糖苷可作为含有该成分的天然产物及其制剂质量评价和药效物质基础研究的对照品。

OBJECTIVE To prepare torachrysone-8-O-β-D-glucopyranoside reference substance for quantitative analysis. METHODS Torachrysone-8-O-β-D-glucopyranoside was isolated and purified by macroporous resin column chromatography, ODS chromatography, and semi-preparative HPLC. Its structue was identified by ESI-MS and NMR spectral techniques. The purity was determined by HPLC analysis using the main component self-compare with no corretion factor method. RESULTS The reference substance of torachrysone-8-O-β-D-glucopyranoside was prepared and its purity was 98.0% in line with the standard of quantitative analysis. CONCLUSION Torachrysone-8-O-β-D-glucopyranoside prepared by this method can be used as reference substance to the quality control for natural product and their preparations, as well as the research of pharmacodynamic material basis.