目的 考察大孔吸附树脂分离纯化香青兰提取液的最佳工艺条件。方法 以总黄酮、田蓟苷、木犀草素-7-O-β-D-葡萄糖醛酸苷、迷迭香酸为检测指标,利用静态吸附实验对7种大孔吸附树脂进行筛选,并通过与动态吸附实验相结合的方法,优选大孔吸附树脂分离纯化香青兰提取液的最佳工艺条件。结果 HPD600型大孔树脂宜于香青兰提取液的纯化,最佳纯化工艺参数为香青兰提取液质量浓度为80 mg/mL,柱径高比为1:9,上样量为生药0.32 g/mL树脂,上样体积流量为1.5BV/h(BV为柱体积),吸附时间为12 h,水除杂用量4 BV,洗脱溶剂为70%乙醇,洗脱体积为6 BV,洗脱体积流量为1.5BV/h,纯化后总黄酮、田蓟苷、木犀草素-7-O-β-D-葡萄糖醛酸苷和迷迭香酸的质量分数分别达到53%、5.5%、4.7%和2.5%以上。结论 HPD600型大孔树脂分离纯化香青兰提取液的方法可行。

Objective To investigate the technology for the separation and purification of extract in Dracocephalum moldevica (EDM) by macroporous resin. Methods Static and dynamic adsorption-desorption were used to select the best one from seven different type macroporous resins; With the content of total flavonoids, tilianin, luteolin-7-O-β-D-glucuronide, and rosmarinic acid as indexes, the purification technology parameters of EDM were optimized. Results HPD600 resin showed the best purifying profile, its optimum technology conditions were as follows: The optimum concentration of the sample liquid was 0.08 g/mL equivalent to raw material, the resin column diameter-height ratio was 1:9, the amount of used adsorption was 0.32 g dried medicinal herb/mL resin, sample flow rate was 1.5 BV/h, and adsorption time was 12 h. In the course of elution, the resin column chromatography was eluted with 6 BV of 70% ethanol after removing impurities with 4 BV of water by flow rate of 1.5 BV/h. The contents of total flavonoids, tilianin, luteolin-7-O-β-D-glucuronide, and rosmarinic acid were more than 53%, 5.5%, 4.7%, and 2.5%. Conclusion Macroporous resin HPD600 is suitable to separate and purify EDM.

国家科技重大专项"重大新药创制"课题(2012ZX09102201-009)