[关键词]
[摘要]
目的优化大孔吸附树脂分离纯化荷叶中阿朴啡类生物碱的洗脱条件。方法采用大孔吸附树脂柱色谱法, 以不同体积分数甲醇水溶液进行洗脱, 分离富集阿朴啡类生物碱, 并配以HPLC进行同步监控。结果基于不同体积分数甲醇水洗脱液对各种阿朴啡类生物碱洗脱能力不同, 采用70%、80%、95%甲醇水溶液进行梯度洗脱, 荷叶中3种主要的阿朴啡类生物碱得到了分离富集。70%甲醇水溶液洗去目标物以外的杂质后, 75.58%的N-降荷叶碱和65.03%的O-降荷叶碱富集于80%甲醇水洗脱液中, 69.46%荷叶碱富集于95%甲醇水洗脱液中。各洗脱液分别蒸干后得固体, N-降荷叶碱和O-降荷叶碱在相应的固体中质量分数分别为44.01%、7.61%。荷叶碱在相应的固体中质量分数为68.52%。结论此方法操作简单、重复性好, 能有效分离富集荷叶中阿朴啡类各种生物碱。
[Key word]
[Abstract]
Objective To study the optimal elution conditions of maeroporous adsorption resin for different aporphine-alkaloids in the leaves of Nelumbo nucifera.Methods Macroporous adsorption resin was used for adsorption,separation, and elution of aporphine concentration alkaloids.The process was monitored by HPLC.Results According to different abilities of methanol aqueous elutions in different concentration(70%,80%,and 95%)to elute different aporphine alkaloids,that were used for gradient elution in turn, and the three kinds of aporphine alkaloids were enriched and one of them was separated.After the impurities were abandoned in 70%methanol aqueous solution, 75.58%N-nornuciferine and 65.03%0 nornueiferine were mainly collected in 80%methanol aqueous solution,and 69.46%nuciferine was enriched in 95%methanol aqueous solution.With these elution solutions dried, their contents of N-nor-nuciferine,O-norciferine,and nuciferine were 44.01%,7.61%,and 68.52%in the relative solid,respectively.Conclusion The developed method is simple with good reproducibility.It is effective to enrich different aporphine alkaloids in the leaves of N.nuciferlne surely.
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[基金项目]
国家“十五”重大专项“创新药物及中药现代化”;国家“十五”重大专项“食品安全关键技术”;湖南省杰出青年基金资助(03JJY1002, 2001BA746C, 2001BA804A21, 2003AA2Z3515)。