南天竹总生物碱提取纯化工艺研究

目的:确定最佳的提取、纯化条件,为南天竹中总生物碱的开发和利用提供科学的理论依据。方法:在单因素基础上,利用L9(34)正交试验,以南天竹总生物碱得率为指标,优选回流提取工艺;通过静态和动态吸附实验,以吸附量和洗脱量为考察指标,分别比较7种不同型号的树脂对南天竹总生物碱的吸附和解吸性能;并以盐酸小檗碱为对照品,应用酸性染料比色法,通过测定南天竹总生物碱的含量,筛选纯化最佳工艺。结果:南天竹中总生物碱的最佳提取工艺条件为8倍量75%的乙醇回流提取3次,每次1h。HPD-722型树脂具有最佳的吸附及洗脱参数,其最佳纯化条件为:上样液总生物碱质量浓度为4mg·m L^-1,上样量35m L,上样流速2m L·min^-1,先以6倍体积的水洗去杂质,再以10倍体积的80%乙醇以1m L·min^-1的流速洗脱,得总生物碱含量达到70%以上。结论:该提取、纯化条件简单、可行,具有良好的应用前景。

Study on Extraction and Purication of the Total Alkaloids from Nandina Domestica

Objective:To provide the best extraction and purification process of the total alkaloids of Nandina domestica and a theoretical basis for development and utilization of it.Methods:On the basis of single factor,the reflux extraction process was selected using L9(34)orthogonal test,and the total alkaloid yield of Nandina domestica as index.The optimization of the process purification as following:the berberine hydrochloride was chosen as the reference substance;the acidic dye colorimetry was used as the determination method;the static and dynamic adsorption experiments were used;the adsorption and elution capacity of seven different types of resins on total alkaloids of Nandina domestica were investigated.Results:The optimum extraction conditions of total alkaloids from Nandina domestica were 8 times75%ethanol and reflux extraction for 3 times,each for 1 h.The HPD722 macroporous adsorption resin provided the optimal adsorption and elution parameters through the comparison of 7 different types of macroporous resin.The best adsorption capacity was achieved with the following condition:the concentration of extract liquid was 4mg·m L^-1,sample volume 35 m L,sample flow rate 2m L·min^-1,then the resin was washed by 6 BV water and elute with 10 volumes of 80%ethanol at a flow rate of 1m L·min^-1 to obtain a total alkaloid content of more than 70%.Conclusion:The process is simple,feasible and has a good prospect.