韭莲总生物碱分离纯化工艺研究

Study on Separation and Purification Technology of Total Alkaloids from Zephyranthes Carinata

目的:研究利用大孔吸附树脂对韭莲总生物碱进行分离纯化的工艺,为韭莲总生物碱的开发利用奠定基础。方法:以石蒜碱含量为指标,采用紫外分光光度法测定总生物碱含量,考察D101、AB-8、HPD300、NKA-9、ADS-7和DM130大孔吸附树脂对韭莲生物碱的吸附与解吸附性能,并系统考察了分离纯化韭莲总生物碱的最佳工艺。结果:HPD300大孔吸附树脂具有最优的吸附和解吸附性能,最佳纯化工艺为:上样提取液浓度1.328~1.593 mg/mL,上样流速2 BV/h(BV:柱体积),上样后静态吸附4 h,先用6 BV水洗脱至无色,再用5 BV 70%乙醇洗脱,洗脱流速2 BV/h,收集洗脱液,减压浓缩后冻干,所得提取物中总生物碱含量为67.62%。结论:HPD300大孔吸附树脂对韭莲总生物碱的分离纯化效果良好,且纯化条件简单,重现性好。

Objective:To explore the purification method of total alkaloids from Zephyranthes carinata with macropopous adsorbing resin,and to lay a foundation for the development and utilization of the total alkaloids of Zephyranthes carinata.Methods:The content of lycorine was used as the index,and the content of total alkaloids were determined by ultraviolet spectrophotometry.The adsorption and desorption properties of D101,AB-8,HPD300,NKA-9,ADS-7 and DM130 macroporous adsorption resins for the alkaloids in Zephyranthes carinata were investigated,and the best process for the separation and purification of the total alkaloids in Zephyranthes carinata was systematically investigated.Results:HPD300 macroporous adsorption resin has the best adsorption and desorption performance.The best purification process is as follows:the concentration of the loading extract is 1.328-1.593 mg/mL,the flow rate is 2 BV/h(BV:Bed volume).HPD300 macroporous adsorption resin was statically adsorbed for 4 hours after loading the samples,then eluted with 6 BV water to colorless,and finally eluted with 5 BV 70%ethanol(flow rate was 2 BV/h).The elution solution was collected,concentrated and freeze-dried under reduced pressure.The total alkaloid content of the obtained extract was 67.62%.Conclusion:HPD300 macroporous adsorption resin has a good effect on the separation and purification of the total alkaloids from Zephyranthes carinata.The purification conditions are simple with good reproducibility.