半枝莲中总生物碱的提取和纯化条件研究

Study on Extraction and Purification of the Total Alkaloids from Scutellaria Barbata D.Don

关键词:  半枝莲  总生物碱  提取  纯化

Key words:  Scutellaria barbata D.Don  total alkaloids  extraction  purification

摘要:

目的 确定最佳的提取、纯化条件，为半枝莲中总生物碱的开发和利用提供科学的理论依据。方法 采用L₉(3⁴)正交试验，超声提取，考察酸浓度、料液比、温度、提取次数4个因素对半枝莲中总生物碱得率的影响。然后结合静态和动态吸附实验，分别比较了6种不同型号的大孔树脂对半枝莲总生物碱的吸附和解吸性能，并以比吸附量、比洗脱量为考察指标，对大孔树脂纯化总生物碱的条件进行了筛选。以盐酸小檗碱为对照品，甲醇-盐酸(100∶1)溶解，采用紫外分光光度法测定半枝莲总生物碱的含量。结果 半枝莲中总生物碱的最佳提取工艺条件为12倍量1%的硫酸水超声提取3次，每次1 h，温度为70 ℃。通过对6种不同型号的大孔树脂的比较，表明HPD100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1.015 7 mg·mL^-1，pH在3.0~4.0之间，先以3.7倍柱体积的水洗去杂质，再以3.5倍柱体积45%乙醇洗脱，得总生物碱量是纯化前总生物碱量60%左右。结论 该提取、纯化条件简单、可行，具有良好的应用前景。

Abstract:

OBJECTIVE To provide a theoretical basis for development and ulitization of the total alkaloids of Scutellaria barbata D.Don by optimizing the best extraction and purification process. METHODS The concentration of extracting solvent, ratio of solid-to-liquid, temperature, extraction times were investigated and the L₉(3⁴) orthogonal test was adopted to optimize the process. By the static and dynamic adsorption experiments, six types of macroporous adsorption resins(D101, HPD100, HPD400, HPD500, HPD600, AB-8) were evaluated to find the optimum one in purificating efficiency with measuring the adsorption and eluting ratio of the total alkaloids as indexes and used berberine hydrochloride as a comparison, methanol-hydrochloride(100∶1) for the reagent to determine the content of the total alkaloids of Scutellaria barbata D.Don. RESULTS The results showed that 1% sulfuric acid solution as extracting solvent, ratio of solid-to-liquid was 1∶12, temperature was 70 ℃ and extracting three times and 1 hour every time were optimal. The HPD100 macroporous adsorption resin provided the optimal adsorption and elution parameters. The best adsorption capacity was achieved with the following condition the concentration of extract liquid was 1.015 7 g·mL^-1, pH 3.0-4.0，then the resin was washed by 3.7 BV water to remove impurity and alkaloids were desorbed by 3.5 BV 45% ethanol. CONCLUSION The process is simple, feasible and has a good prospect.