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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 3~5.403 4 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 the macroporous resin purification process of limonoids in orange kernels. Methods: Through the static adsorption - elution test, 16 different manufacturers and polar macroporous resins were used to purify the limonoids from the orange nucleus, and the best resin type was screened. The dynamic adsorption-eluting conditions of limonoids by HPD-722 macroporous resin were investigated by single factor test, including the amount of cleaning agent, the concentration of the sample solution, the concentration and the amount of eluent. Results: HPD-722 macroporous resin had the best purification effect on limonin. The optimal purification process was as follows: the mass concentration of sample was 3.503 3 ~ 5.403 4 g · L-1, the flow rate of sample was 1 ~ 2 BV · h-1, the pH of the sample solution was 6, the volume of water was 1 BV, the volume of water was 2 BV · h-1 with 80% ethanol 6 BV, the eluent was pH 7; Material purity 82.82%, of which limonin 22.53%, nimindulin 45.90%. Conclusion: HPD-722 macroporous resin purification orange citrus limonoids in the process of high feasibility, which can effectively improve the limonoids purity.