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目的优选大孔吸附树脂分离纯化伊贝母中总生物碱的工艺条件。方法以伊贝母总生物碱的比吸附量、比解吸量、总生物碱含量为考察指标,通过静态、动态试验考察12种不同类型大孔吸附树脂对伊贝母总生物碱纯化效果的影响,通过单因素试验优选上样液质量浓度、上样量、洗脱剂种类及用量等工艺参数。结果 HPD-100型大孔树脂对伊贝母总生物碱有较好的富集纯化性能,最佳工艺条件:径高比为1∶9的树脂柱,上样药液质量浓度为0.25 g·m L?1,pH值为11,最大上样量为15 m L,8倍柱体积水洗除杂,9倍柱体积的70%乙醇洗脱总生物碱,洗脱流速1 m L·min?1。按照此工艺条件纯化的伊贝母总生物碱含量达到70.50%,收率达到4.30%。结论纯化工艺简便、稳定,适合伊贝母总生物碱的纯化。
Objective To optimize the conditions for the separation and purification of total alkaloids from Fritillaria macroporus macroporous resin. Methods The specific absorption, specific desorption and total alkaloid content of the total alkaloids of Fritillaria ussuriensis were taken as the indexes to investigate the effects of 12 different types of macroporous adsorption resins on the purification of total alkaloids from Fritillaria pallidiflora by static and dynamic tests Through the single factor test, the optimum conditions of sample concentration, sample loading, type and amount of eluent were optimized. Results HPD-100 macroporous resin had good enrichment and purification properties for the total alkaloids of Fritillaria cirrhosa. The optimum conditions were as follows: the resin column with the aspect ratio of 1: 9 and the mass concentration of the sample liquid was 0.25 g · m L · 1, pH 11, the maximum sample volume was 15 mL, eluted with 8 column volumes and eluted with 9 column volumes of 70% ethanol. The elution flow rate was 1 mL · min -1. 1. According to this process conditions, the total alkaloid content of E. fritillaryis reached 70.50% and the yield reached 4.30%. Conclusion The purification process is simple and stable, suitable for the purification of total alkaloids from Fritillaria.