精制益母草生物碱提取纯化工艺研究

Study on the Extraction and Purification of Alkaloid of Leonurus japonicus

目的:优选精制益母草生物碱的提取纯化工艺。方法:采用平行设计法,以总生物碱提取量为判断指标,分别观察超声、回流、浸渍法提取益母草中生物碱的提取率,确定最佳提取工艺;以生物碱含量为判断指标,采用4种不同化学特性的ADS树脂,分别观察其在提取液不同pH环境、不同洗脱条件下,回收生物碱的量和纯度,确定最佳纯化工艺。结果:超声结合不同溶剂提取对精制益母草生物碱提取率的影响不同,以0.05%盐酸乙醇的提取干膏生物碱含量和提取率最高,平均生物碱提取率为0.373%;在回流法中,以0.05%盐酸乙醇的提取干膏生物碱含量和提取率最高,平均生物碱提取率为0.317%;在浸渍法中,以1%盐酸的提取干膏生物碱含量和提取率最高,平均生物碱提取率为0.410%。在纯化工艺方面,在提取液pH为6～8之间时,4种ADS大孔树脂对生物碱均有吸附作用,其中pH为8时ADS-B的静态吸附最强。结论:本研究建立了高效、稳定的精制益母草生物碱的提取和纯化工艺,可为进一步开发新型具有抗心肌缺血或心血管保护作用的新药奠定基础。

OBJECTIVE：To optimize the extraction and purification technology of alkaloid of Leonurus japonicus. METHODS：Parallel designing methods was applied to observe the extraction rate of alkaloid of L. japonicus and fructus leonuri by ultrasonic wave,refluxing and impregnation with the extraction amount of alkaloid as evaluation index. The extraction amount and purity of alkaloid by 4 kinds of ADS resins with different chemical characteristics in different pH value and elution conditions were observed in order to optimize the extraction technology. RESULTS：Effects of ultrasonic wave combined with different solvents on the extraction ratio were different. Average extraction ratio of alkaloid with 0.05% hydrochloric acid ethanol was 0.373% and higher than those by other solvents. In the refluxing method,average alkaloid extraction ratio with 0.05% hydrochloric acid ethanol was 0.317%,which was higher than other solvents. In impregnation method,average extraction ratio of alkaloid with 1% hydrochloric acid was 0.410%,which was higher than other solvents. 4 kinds of ADS macroporous resins all showed adsorption to alkaloid when pH values of extraction solution were between 6 and 8. The static absorbability ADS-B was the highest among solvents when the pH value reached 8. CONCLUSION：This study establishes the effective and reliable extraction and purification method of alkaloid of L. japonicus. It provides basis for further development of tranquilization injection for myocardial ischemia or cardiovas-cular protection.