骆驼蓬种子中骆驼蓬碱和去氢骆驼蓬碱的制备与鉴定

目的从骆驼蓬种子中大量制备骆驼蓬碱和去氢骆驼蓬碱单体。方法取骆驼蓬种子压榨后的油饼,用体积分数为95%的乙醇提取获得含生物碱的浸膏,该浸膏先后用体积分数为10%的硫酸和25%的氨水处理得到骆驼蓬种子总生物碱,再用氧化铝柱层析和溶剂重结晶等方法进一步纯化,得到骆驼蓬碱和去氢骆驼蓬碱单体。结果目标产物经过1 H-NMR、13 C-NMR、IR和ESI-MS等定性分析,再采用HPLC/DAD定量分析,骆驼蓬碱和去氢骆驼蓬碱的产物色谱图中以面积归一化法计质量分数达到98.7%和99.8%。结论该方法简便、有效,可用于骆驼蓬碱和去氢骆驼蓬碱对照品的制备。

Preparation and characterization of harmaline and harmine from the seeds of Peganum harmala L.

Objective To establish a method to isolate and prepare harmaline and harmine from the seeds of Peganum harmala L..Methods Oil dregs of the seeds of Peganum harmala L.was extracted with 95% ethanol.The concentrated crude extract was treated with 10% sulfuric acid and 25% ammonia solution to obtain total alkaloids from the seeds of Peganum harmala L..Harmine and harmaline were isolated and purified by Al2O3 column chromatography and recrystalization.The HPLC/DAD method was applied for the sample purity analysis.Results The prepared products were identified by 1H-NMR,13C-NMR,IR and ESI-MS.The purity of harmaline and harmine were 98.7% and 99.8% respectively, calculated with area normalization method by HPLC/DAD.Conclusion The preparation method was efficient and simple for the large-scale preparation of harmaline and harmine.