pH区带逆流色谱法分离三尖杉生物碱

Separation of alkaloids from Cephalotaxus fortunine by pH-zone-refining countercurrent chromatography

目的:利用pH区带逆流色谱法(pH-zone-refining countercurrent chromatography)对三尖杉生物碱进行分离。方法:将三氟乙酸加入乙酸乙酯-石油醚-水(3∶1∶4)溶剂系统的上相(固定相)作为保留剂,用含10%氨水、中性和含三氟乙酸的下相(流动相)依次进行梯度洗脱,取得了较好的分离效果。结果:1次分离可进样500 mg,分离得到4组三尖杉生物碱,其中2组经核磁共振(NMR)分析为三尖杉碱和乙酰三尖杉碱。经HPLC分析,2种生物碱的纯度分别为95.4%和98.9%。结论:pH区带逆流色谱法是一种较好的三尖杉生物碱分离方法。

Objective ： Separation of cephalotaxine - type alkaloids in Cephalotaxus fortunine by pH - zone - refining countercurrent chromatography was studied in this paper. Method：Trifuoroacetic acid was added to the station- ary phase of a solvent system composed of acetate -light petroleum- water（3： 1：4）as a retainer, cephalotaxine - type alkaloids were eluted by step -gradient acetoelution with 10% ammonia water, water and trifuoroacetic acid, orderly. Result：In each separation,500 mg crude sample can be successfully separated into 4 sections of cephalo- taxine -type alkaloids in which two were acetylcephalotaxine and cephalotaxine identified by ^1H and ^13C NMR. The purity of the two alkaloids was 95.4% and 98.9%. Conclusion： It is a good way to separate the alkaloids from Cephalotaxus fortunine by pH- zone- refining countercurrent chromatography.