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选取D-101型大孔树脂,以总黄酮、总萜和总生物碱的转移率评价上样质量浓度、上样量、吸附时间和洗脱液体积流量对纯化效果的影响,以落干酸、6’-O-β-D-葡萄糖基龙胆苦苷、獐牙菜苦苷、龙胆苦苷、獐牙菜苷、杠柳苷、延胡索乙素、四氢小檗碱和延胡索甲素的转移率评价洗脱液浓度对纯化效果的影响,以延胡索甲素的转移率确定洗脱终点,最终优化出最佳纯化工艺条件:上样质量浓度75mg/mL,样品:填料为1:70,吸附时间为2h,洗脱液体积流量为4.0mL/min,洗脱条件为先用3BV蒸馏水除杂,再依次用2BV 30%乙醇、2BV 60%乙醇和10BV95%乙醇洗脱。该纯化工艺稳定可行,可作为黑骨藤复方药物有效部位制备工艺。
D-101 macroporous resin was selected to evaluate the effect of loading mass concentration, loading volume, adsorption time and eluent volume flow on the purification efficiency by the transfer rate of total flavonoids, total terpene and total alkaloids, , 6’-O-β-D-glucosyl gentiopicroside, swertia glycoside, gentiopicroside, swertia glycoside, dipalphalide, tetrahydropalmatine, tetrahydroberberine, Of the transfer rate evaluation of the concentration of the eluate on the purification effect, the elution of faucetin A transfer rate was determined to determine the final purification process, the final optimization of the optimal purification conditions: loading mass concentration of 75mg / mL, sample: packing 1:70 , The adsorption time was 2h, the eluent volume flow rate was 4.0mL / min, the elution conditions were first with 3BV distilled water, and then with 2BV 30% ethanol, 2BV 60% ethanol and 10BV95% ethanol. The purification process is stable and feasible, and can be used as an effective preparation process of the black kudzu vine compound drug.