Separation of alkaloids by pH-zone-refining counter-current chromatography

pH-Zone-refining counter-current chromatography was applied to the separation of alkaloids from a crude extract of Crinum moorei using a multilayer coil planet centrifuge. After methyl tert.-butyl ether and water were equilibrated, triethylamine (5-10 mM) was added to the organic phase and hydrochloric acid (5-10 mM) to the aqueous phase. The separation was performed by eluting the column with either the organic phase (displacement mode) or the aqueous phase (reverse-displacement mode) while the other phase was used as the stationary phase. From 3 g of the extract, crinine, powelline and crinamidine were separated in 2.5-7 h with minimum overlapping.