大孔吸附树脂纯化富集伊贝母总生物碱的工艺研究

Enrichment and Purification of Total Alkaloids in Fritillariae Pallidiflorae Bulbus with Macroporous Adsorption Resins

关键词:  伊贝母  总生物碱  大孔吸附树脂  纯化  富集

Key words:  Fritillariae Pallidiflorae Bulbus  total alkaloids  macroporous adsorption resins  purification  enrichment

摘要:

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·mL^-1，pH 值为11，最大上样量为15 mL，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 mL·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。

Abstract:

OBJECTIVE To optimize separating and purifying total alkaloids from Fritillariae pallidiflorae bulbus by macroporous resin. METHODS With adsorption capacity, specific solution desorption and total alkaloids as indexes, 12 different types of macroporous adsorption resin were selected by static and dynamic test. Sample solution concentration, the maximum loading amount, eluent type, eluent amount and other parameters were investigated by single factor tests. RESULTS HPD-100(diameter/high=1∶9) macroporous resin was selected as the best material in enrichment and purification of total alkaloids from Fritillariae pallidiflorae bulbus, the content of coumarin was 0.25 g·mL^-1, pH value was 11, and with 70% ethanol, the volume was 9 BV, the flow rate was 1 mL·min^-1. According to the optimal purification process, the content of total alkaloids was 70.50%, the yield was 4.30%. CONCLUSION The optimized technology is simple, stable, fit for separating and purifying total alkaloids from Fritillariae pallidiflorae bulbus.