大孔吸附树脂富集纯化三七花总皂苷工艺研究

摘要

目的:研究D101大孔吸附树脂富集纯化三七花总皂苷的工艺条件及参数.方法:采用单因素试验,优选大孔吸附树脂型号、上样浓度、吸附平衡时间和洗脱溶剂;采用正交试验优选上样量、流速和洗脱溶剂量.以三七花总皂苷的转移率和纯度的平均值为指标,优选树脂富集三七花总皂苷的最佳工艺.结果:优选的工艺为选择D101型大孔吸附树脂50 mL(相当于4.515 g干树脂),树脂径高比为1:20,上样浓度为总皂苷含量25.01 mg·mL-1(即0.6 g(生药)/mL),上样药液15mL,静置2h,用0.1 mol·L-1NaOH溶液200mL(4倍柱体积)淋洗后用水洗至中性(pH＝7),再用70%乙醇以每小时3倍柱体积的流速洗脱,收集洗脱液200mL(1.5倍柱体积).结论:所选方法可较好地富集三七花总皂苷.%OBJECTIVE: To study the technique condition and parameter of the enrichment and purification of total saponins from flower buds of Panax notogimeng with D101 macroporous adsorptive resin. METHODS: Type of macroporous adsorptive resin, the concentration of sample, the time of the adsorption equilibrium and elution solvent were optimized by single factor test. The sample amount, flow rate and amount of elution solvent were optimized by orthogonal test. The optimal condition for the enrichment and purification of total saponins from flower buds of P. Notoginseng was optimized using the mean value of transfer rate and purity of total saponins from flower buds of P. Notoginseng as index.RESULTS: The optimal condition was as follows: D101 macroporous adsorptive resin was 50 mL (equal to 4.515 g dry resin), ratio of diameter to length was 1:20, the concentration of sample solution was 25.01 mg·mL-1(0.6 g crude drug per mL), the sample volume was 15 mL, washed with 0.1 mol·L-1 NaOH solution 200 mL (4 BV) after standing 2 h, and washed with water to neutral (pH value changed into 7), then 70% ethanol, 3 BV·h-1 flow rate, collecting eluant 200 mL (1.5-folds column volume). CONCLUSION: The method is good for the enrichment of total saponins from flower buds of P. Notoginseng.