土圞儿总生物碱的提取和纯化工艺研究

    Study on Extraction and Purification of the Total Alkaloids from Apios Fortunei Maxim.

    • 摘要: 目的 确定土圞儿中总生物碱最佳的提取、纯化条件,为其开发和利用提供科学的理论依据。方法 采用L9(34)正交试验,加酸水加热回流提取,考察溶剂用量、提取时间、提取次数3个因素对土圞儿中总生物碱得率的影响。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(D101,H-30,LSD-001,HPD450,DM130,AB-8)对土圞儿总生物碱的吸附和解吸性能,并以吸附量、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,采用紫外分光光度法测定土圞儿总生物碱的含量。结果 土圞儿中总生物碱的最佳提取工艺条件为15倍量酸水加热回流提取2次,每次1 h。HPD450型树脂具有最佳的吸附及洗脱参数,其最佳纯化条件:上样液总生物碱浓度为1.6 mg·mL-1,pH 8.0,先以5倍柱体积的水洗去杂质,再以4倍柱体积40%乙醇洗脱,最后用4倍柱体积90%乙醇洗脱,得总生物碱量是纯化前总生物碱量80%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 Apios fortunei Maxim. by optimizing the best extraction and purification process. METHODS The effects of the ratio of solid-to-liquid, extraction time and extraction times on total alkaloid yield of Apios fortunei Maxim. were investigated by L9 (34) orthogonal test. By the static and dynamic adsorption experiments, six types of macroporous adsorption resins(D101, H-30, LSD-001, HPD450, DM130, 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 to determine the content of the total alkaloids of Apios fortunei Maxim.. RESULTS Ratio of solid-to-liquid was 1:15, extracting twice and 1 h every time were optimal. The HPD450 macroporous adsorption resin provided the optimal adsorption and elution parameters through the comparison of 6 different types of macroporous resin. The best adsorption capacity was achieved with the following condition:the concentration of extract liquid was 1.6 mg·mL-1, pH 8.0,then the resin was washed by 5 BV water and 4 BV 40% ethanol to remove impurity and alkaloids were desorbed by 4 BV 90% ethanol. The total alkaloid was 80% of it before purifiction. CONCLUSION The process is simple, feasible and has a good prospect.

       

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