Isobyakangelicin angelate, a new furanocoumarin and the five known coumarins, columbianadin, (+)-oxypeucedanin, (±)-oxypeucedanin hydrate, ostruthol, and isoimperatorin, were isolated from roots of Peucedanum palustre (L.) Moench using medium-pressure liquid chromatography [MPLC] with normal phase and subsequently with reversed phase as stationary phases. The mobile phases were optimized in TLC and HPLC preassays according to the "PRISMA" system and then transferred without modification to preparative MPLC separations. The structures of the compounds were elucidated by a combination of spectroscopic methods, among others the rotating frame Overhauser enhancement spectroscopy [ROESY] experiment.