橘核中柠檬苦素类物质纯化工艺

Purification Technology of Limonoids in Citri Reticulatae Semen

目的：优选橘核中柠檬苦素类物质的大孔树脂纯化工艺.方法：通过静态吸附-洗脱试验综合考察16种不同厂家和极性大孔树脂对橘核中柠檬苦素类物质的纯化效果,筛选最佳树脂型号.通过单因素试验考察HPD-722型大孔树脂对柠檬苦素类物质的动态吸附-洗脱条件,包括清洗剂用量、上样液质量浓度、洗脱剂浓度及用量等.结果：HPD-722型大孔吸附树脂对柠檬苦素类物质的纯化效果最佳;最佳纯化工艺为上样液质量浓度在3.503 3～5.4034 g·L^-1,上样流速1～2 BV·h^-1,样品溶液pH 6,水洗用量1 BV,80％乙醇6 BV为洗脱剂,洗脱流速2 BV·h^-1,洗脱液pH 7;洗脱液中柠檬苦素类物质纯度82.82％,其中柠檬苦素22.53％,诺米林45.90％.结论：采用HPD-722型大孔吸附树脂纯化橘核中柠檬苦素类物质的工艺可行性较高,可有效提高柠檬苦素类物质纯度.

Objective：To optimize purification process of limonoids in Citri Reticulatae Semen by macroporous resin.Method：Static adsorption and desorption tests were adopted to select optimal type from 16 kinds of macroporous resin with different manufacturers and polarities.Purification process was optimized by single factor tests.Result：HPD-722 macroporous resin was selected,optimal purification process was as following：the concentration of sample solution between 3.503 3-5.403 4 g ·L^- 1,sampling speed of 1-2 BV ·h^-1,pH of sample solution 6,washed impurity by 1 BV of water and eluted by 6 BV of 80% ethanol with elution rate of 2 BV ·h^-1,eluent pH of 7 ; under these conditions,purity of limonoids was 82.82%,including limonin of 22.53% and nomilin of 45.90%.Conclusion：Limonoids can be purified by HPD-722 macroporous resin,this process can effectively improve the purity of limonoids.