In order to find a versatile high speed counter-current chromatography solvent system that can be used as a general prefractionation system for most alkaloids, the crude extracts of five Chinese traditional medicinal herbs, Cortex phellodendri, Semen strychni, green tea, Sophora flavescens ait, and Datura mete L. were resolved. All separations were performed only with a two-phase system composed of CHCl3-CH3OH-water (4:3:2). The water had different acidities controlled by adding NaH2PO4 or HCl to each sample. The fractionated components were identified by thin-layer chromatography, which confirmed this solvent system was versatile and very useful for the separation of alkaloids.