[关键词]
[摘要]
目的 探究一种有效分离纯化菊米黄酮的大孔树脂并对纯化工艺条件进行优化。方法 以树脂的饱和吸附容量、吸附速率和解吸附率为参考指标,从10种不同的大孔吸附树脂中筛选出综合性能较佳的树脂,并进一步考察此树脂纯化菊米总黄酮的影响因素和分离纯化效果。结果 HPD-100树脂的综合性能较好,饱和吸附容量达到60.2 mg/g(以湿重计),且吸附迅速,解吸附完全。较理想的吸附工艺:在树脂径高比为1∶10的条件下,质量浓度为4.3 mg/mL供试液以15 mL/min上柱时,最佳上样量为5倍柱床体积(BV),静态吸附时间为2 h;较理想的洗脱工艺:先用6 BV的纯水洗杂质,再以60%的乙醇为洗脱剂,洗脱体积流量为8 mL/min时,用量为3 BV,所得菊米总黄酮质量分数为(81.6±0.9)%。结论 HPD-100是一种分离纯化菊米黄酮较佳的树脂,其工艺简单,具有较好的工业化生产前景。
[Key word]
[Abstract]
Objective To screen a macroporous resin for effective separating and purifying the total flavonoids from the buds of Chrysanthemum indicum (TFBCI) and to further optimize the process conditions. Methods Through critical evaluating the absorption and desorption properties of macroporous resins including the absorption capacity, absorption velocity, and desorption rate, a preferable resin was selected from 10 kinds of macroporous resins, and the influence factors and purification effect on TFBCI were investigated further. Results HPD-100 resin had outstanding comprehensive performance, maximum static adsorption capacity was 60.2 mg/g (wet resin), and the adsorption was rapid and desorption complete. The optimum adsorption process was: under the condition of the resin’s diameter height ratio of 1:10, the sample solution concentration 4.3 mg/mL and flow rate 7 mL/min, the best processing volume was 5 BV, and static adsorption time was 2 h; The optimum elution process was: wash the impurities with 6 BV of pure water, elute product with 60% ethanol at the speed of 8 mL/min. The purity of the final product reached to (81.6 ± 0.9)%. Conclusion HPD-100 is an ideal resin for separating and purifying the TFBCI, and its process is simple and has preferable industrialization prospect.
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[基金项目]
国家自然科学基金资助项目(21076191,21006097,21276237)