目的 优化大孔树脂对秦皮总香豆素的纯化工艺。方法 以秦皮总香豆素及秦皮甲素、秦皮乙素、秦皮苷、秦皮素4种香豆素的吸附率、解析率、转移率为考察指标,采用单因素方法,考察纯化秦皮总香豆素的树脂类型,树脂吸附、解吸附性能及纯化效果。结果 所选择的7种大孔树脂中ADS-5最适合秦皮总香豆素的纯化。吸附参数:吸附容量为生药量-树脂0.8 g/g,上样药液质量浓度为生药0.75 g/mL,上样药液pH值为4.0～4.3(原药液),上样体积流量为2～4 BV/h;洗脱参数:水清洗杂质1 BV,洗脱溶剂25%乙醇,洗脱体积流量2 BV/h,洗脱体积3 BV。经纯化,秦皮总香豆素转移率达74.27%,4种香豆素成分转移率达83.06%,秦皮总香豆素提取物出膏率为7.35%,除杂率达14.00%,其中总香豆素的量为54.72%,4种香豆素成分的量之和为36.01%,总香豆素提取率为4.02%。结论 ADS-5对秦皮总香豆素纯化效果较好,该纯化工艺稳定,提取物量符合中药5类新药的要求。

Objective To optimize the purification process of total coumarin from Fraxini Cortex using macroporous resin. Methods The single factor methods have been used to investigate the choice of type, adsorption performance, and desorption performance and the purification of the total coumarin from Fraxini Cortex by macroporous resin. The adsorption rate, resolution, resolution rate, and transfer rate of the total coumarin from Fraxini Cortex, four kinds of coumarin constituents, such as aesculin, aesculetin, fraxin, and fraxetin were used as examining indexes. Results The ADS-5 was the most suitable type for the purification of total coumarin from Fraxini Cortex among the seven kinds of macroporous resin. Adsorption parameters: Crude drug-the resin was 0.8 g/g which was the sample amount;The concentration of sample solution was 0.75 g crude drug/mL;The pH value of sample liquid was 4.0—4.3 (liquid sample);The speed of the sample through the resin column was 2—4 BV/h. Elution parameters: The volume of the water cleaning fluid impurities was 1 BV;The elution solvent was 25% ethanol;The elution speed was 2 BV/h;The elution volume was 3 BV. After the purification, the transfer rate of total coumarin from Fraxini Cortex was 74.27%, the transfer rate of four kinds of coumarin was 83.06%, the extract rate of total coumarin was 7.35%, the removal of impurities was 14.00%, among which the content of total coumarin was 54.72%, the contents of the four kinds of components were 36.01%, the total coumarin extraction yield was 4.02%. Conclusion This method to purify the total coumarin from Fraxini Cortex using ADS-5 can get better purification effect, the purification process is also stable.

中国中医科学院自主选题课题(YZ-1411)