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目的:建立东北铁线莲中抗肿瘤活性成分3-O-α-L-吡喃鼠李糖-(1→6)-β-D-吡喃葡萄糖-(1→4)-β-D-吡喃葡萄糖-(1→4)-β-D-吡喃核糖-(1→3)-α-L-吡喃鼠李糖-(1→2)-α-L-吡喃阿拉伯糖齐墩果酸苷(W2)的大孔树脂纯化工艺。方法:采用HPLC测定W2含量,通过对9种大孔树脂的吸附-洗脱能力进行考察,筛选最适宜的大孔树脂型号,对选定的大孔吸附树脂进行静态吸附动力学考察和动态梯度洗脱考察,通过单因素试验考察上样液浓度、吸附流速、除杂溶媒用量和流速等参数对大孔树脂纯化工艺的影响。结果:最佳纯化工艺为上样液质量浓度0.4 g·m L-1,以1.5 BV·h-1的流速过LX-17型大孔树脂柱,加水4 BV和40%乙醇5 BV除杂,除杂流速3 BV·h-1,加80%乙醇1 BV洗脱以替换柱内液体,加80%乙醇6 BV富集W2,洗脱流速1.5 BV·h-1。浸膏中W2质量分数43.14%。结论:LX-17型大孔树脂适用于W2的的分离纯化,优选的工艺稳定可行,可得到纯度相对较高的样品,为该成分的后续药理作用研究提供保障。
Objective: To establish an antitumor active ingredient 3-O-α-L-rhamnopyranosyl- (1 → 6) -β-D-glucopyranosyl- (1 → 4) -β-D- Glucopyranose- (1 → 4) -β-D-ribofuranose- (1 → 3) -α-L-rhamnopyranose- (1 → 2) -α- Macroporous resin purification of glycoside (W2). Methods: The content of W2 was determined by HPLC. The adsorption and elution capacity of nine kinds of macroporous resins were investigated. The optimum macroporous resin model was screened. The selected macroporous adsorption resins were investigated by static adsorption kinetics and dynamic gradient Elution study, through the single factor test to examine the sample concentration, adsorption flow rate, the amount of impurity removal and flow rate and other parameters of the macroporous resin purification process. Results: The optimum purification process was as follows: the mass concentration of the sample was 0.4 g · m L-1, the flow rate of 1.5 BV · h-1 was passed through the LX-17 macroporous resin column, the water was added 4 BV and 40% ethanol 5 BV , The removal rate was 3 BV · h-1, 80% ethanol was added to 1 BV to replace the column liquid, 80% ethanol 6 BV was enriched in W2, and the elution flow rate was 1.5 BV · h-1. Extract in the W2 mass fraction of 43.14%. CONCLUSION: The LX-17 macroporous resin is suitable for the separation and purification of W2. The optimal process is stable and feasible, and the sample with relatively high purity can be obtained, which can provide the guarantee for the follow-up pharmacological study of this component.