Abstract - The Evodiae Fructus is known for containing a number of indolquinazoline and quinoline type alkaloids. Evodiamine, evocarpine and rutaecarpine are the major constituents of alkaloids. These alkaloids were isolated and determined by forming complex compounds from Evodiae Fructus in O-Su-You-Tang. For the determination of these alkaloids, a new spectrophotometric method was developed with a simple and selective sample clean-up using thiocyanatocobaltate[II] compIεx compound ion. The absorbance of alkaloidal complex compounds in 1,2-dichloroethane solution was measured at 625 nm. The method proved to be rapid, simple and reliable for the isolation and the determination of the alkaloids in O-Su-You-Tang.