吴茱萸碱的大孔树脂分离纯化工艺优选

Optimization of Purification Technology for Evodiamine from Euodiae Fructus by Macroporous Resin

目的:优选大孔树脂分离纯化吴茱萸醇提液中吴茱萸碱的工艺条件。方法:以吴茱萸碱的吸附量和洗脱率为考察指标,通过静态吸附-洗脱试验考察5种不同类型大孔吸附树脂(AB-8,S-8,NKA-9,HPD-100,D-101)对吴茱萸碱纯化效果的影响,通过单因素试验优选上样液质量浓度、上样量、上样流速、洗脱剂种类及用量等工艺参数。结果:D-101型大孔树脂对吴茱萸碱具有良好的吸附分离性能,最佳富集工艺条件为上样液质量浓度3 g·L-1,上样量4 BV,上样流速1 BV·h-1,加水5 BV去除水溶性杂质,加80%乙醇5 BV以2 BV·h-1洗脱。吴茱萸碱洗脱率达92.81%,吴茱萸碱的纯度由提取物的1.29%提高至26.77%。结论:D-101型大孔树脂适用于吴茱萸碱的纯化,优选的纯化工艺稳定可行,为该成分的开发利用提供参考。

Objective： To optimize separation and purification technology conditions of evodiamine from ethanol extract of Euodiae Fructus by macroporous resin. Method： With adsorption volume and elution rate of evodiamine as indexes, five kinds （AB-8, S-8, NKA-9, HPD-100, D-101） of macroporous resins were selected by static adsorption and desorption test. Sample solution concentration, sample volume, sample flow rate, eluent type, eluent amount and other parameters were investigated by single factor tests. Result： D-101 macroporous resin had the best separation and purification capacity for evodiamine in following technology conditions： sample concentration of 3 g·L^-1, sample volume of 4 BV, sample flow rate of 1 BV·h^-1, removed water-soluble impurities with 5 BV of water, eluted with 5 BV of 80% ethanol, eluting velocity of 2 BV·h^-1. Elution rate of evodiamine was 92.81% , its purity increased from 1.29% to 26.77%. Conclusion： D-101 macroporous resin is suitable for purifying evodiamine from Euodiae Fructus. This optimized method is stable and feasible, it can provide a reference for development and utilization of evodiamine.