拉萨大黄中曲札茋苷的大孔树脂纯化工艺研究

Study on Purification of Piceatannol-3'-O-β-D-glucopyranoside from Rheum lhasaense by Macroreticular Resin

目的:对大孔树脂富集纯化曲札茋苷的工艺条件进行优化。方法:采用静态及动态吸附-解吸试验方法,以曲札茋苷的含量为指标进行考察。结果:D101型大孔树脂对拉萨大黄中曲札茋苷的纯化效果较好,综合试验结果确定的工艺条件为:上样液体积与树脂体积比为1∶4,上样液p H值为3左右,吸附时间为2 h,吸附流速为1 BV/h,水洗脱4 BV后25%乙醇洗脱6 BV,洗脱流速为4 BV/h,树脂柱径高比为1∶12。结论:拉萨大黄提取液经D101大孔树脂纯化后,曲札茋苷纯度提高约2.5倍。本文首次提供了曲札茋苷的纯化工艺,经多次试验确定该工艺稳定可行且重复性好,可用于工业化放大生产。

Objective： To establish a optimum technological parameters for the purification of piceatannol-3＇-O- β-D-glucopyranoside with macroporous resin. Methods： Static adsorption, dynamic adsorption and separation methods were used, which made the piceatannol-3＇-O- β-D-glucopyranoside content as an indicator for study. Results： The purification of piceatannol-3＇-O- β-D-glucopyranoside with D101 macroporous resin was better than others. The optimum technological parameters were： The ratio of extracting solution and resin was 1：4. The pH was 3 approximate. Resin standing time was 2 h. The Best adsorption flow rate was 1 BV/h. The Optimum eluent was water for 4 BV and 25% ethanol for 6 BV. The Best elution flow rate was 4 BV/h. The ratio of resin column diameter was 1：12. Conclusion： The purity of piceatannol-3＇-O- β-D-glucopyranoside was higher about 2.5 times. After process validation, separation and purification of piceatannol-3＇-O- β-D-glucopyranoside has good reproducibility under these parameters. It can be used for amplification of industrialization production.