For the analysis of Coptidis Rhizoma, high-speed liquid chromatography was examined, not only for its major alkaloid, berberine, but also for its minor alkaloids. It was found that under an appropriate condition [on starch gel (LS-170), eluted with the solvent system of H_2O : MeCN : AcOH : Et_3N=80 : 20 : 0.3 : 0.745,pH 8.5], sufficient separation of berberine, magnoflorine, jatrorrhizine, palmatine, coptisine, and some other unidentified alkaloids was obtained. By means of the present procedure, content of berberine and relative content of palmatine and coptisine to berberine in some of wild and commercial coptis rhizomes were determined. Since the solvent system does not contain any nonvolatile salt, the present technique also offers the possibility of application to rapidpreparative separation of alkaloids of this type by liquid chromatography. The application to analysis of alkaloids of phellodendron-cortex is also described.