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目的建立从虎杖药材中高效制备分离大黄素-8-O-β-D-吡喃葡萄糖苷(EG)的方法。方法采用大孔吸刚树脂柱色谱和ODS柱色谱分离目标组分,高速逆流色谱(HSCCC)纯化目标化合物,质谱和核磁共振波谱数据鉴定结构,HPLC不加校正因子的主成分自身对照法检测纯度。结果优化确定以二氯甲烷-醋酸乙酯-甲醇-水(8:1:6:5)为HSCCC溶剂系统,上相为固定相,下相为流动相,纯化制备了符合定量测定用要求的EG对照品,HPLC法检测质量分数大于98%。结论方法适于从虎杖药材中大量制备高纯度EG,为含有该成分的天然产物及其制剂质量评价提供对照物质。
OBJECTIVE To establish a method for the efficient preparation of emodin-8-O-β-D-glucopyranoside (EG) from Polygonum Cuspidatum. Methods The target compounds were isolated by macroporous resin as adsorbent and ODS column chromatography. The target compounds were purified by high-speed countercurrent chromatography (HSCCC). The structures were identified by mass spectrometry and nuclear magnetic resonance spectroscopy. . The results were optimized by using dichloromethane-ethyl acetate-methanol-water (8: 1: 6: 5) as HSCCC solvent system. The upper phase was stationary phase and the lower phase was mobile phase. EG reference substance, HPLC method for the detection of mass fraction greater than 98%. Conclusion The method is suitable for the preparation of high purity EG from Polygonum Cuspidatum and provides a control substance for the evaluation of the natural products containing this component and the quality evaluation of the preparation.