Four alkaloids of the phenethylamine derivatives have been isolated from the n -butanol fraction of the aerial parts of Stapelia hirsuta L. The structures of the isolated alkaloids were determined as N -acetyl hordenine (a new natural compound), hordenine, candicine and hordenine-1- O -β-D-glucoside, in addition to luteolin-7- O -β-D-glucopyranoside.