For the first time the composition of the bufadienolide complex in URGINEA HESPERIA Webb & Berth. has been investigated. From an extract of lyophilized plants, thirteen bufadienolides were isolated. By means of FAB-MS, (1)H-NMR, and (13)C-NMR studies the compounds were structurally elucidated as scillarenin, scilliphaeosidin, scillarenin-3- O-alpha- L-rhamnoside, scilliphaeosidin-3- O-alpha- L-rhamnoside, gamabufotalin-3- O-alpha- L-rhamnoside, 11alpha-hydroxyscilliglaucosidin-3- O-alpha- L-rhamnoside, scillarenin-3- O-alpha- L-2',3'-diacetylrhamnosido-4'-beta- D-glucoside, scillarenin-3- O-alpha- L-rhamnosido-4'-beta- D-glucosido-3''-beta- D-glucoside, scillarenin-3- O-alpha- L-rhamnosido-4'-beta- D-glucosido-4''-beta- D-glucoside, scillarenin-3- O-alpha- L-2',3'-diacetylrhamnosido-4'-beta- D-glucosido-3''-beta- D-glucoside, scillarenin-3- O-alpha- L-2',3'-diacetylrhamnosido-4'-beta- D-glucosido-4''-beta- D-glucoside, scilliphaeosidin-3- O-alpha- L-rhamnosido-4'-beta- D-glucosido-3''-beta- D-glucoside, and scilliphaeosidin-3- O-alpha- L-rhamnosido-4'-beta- D-glucosido-4''-beta- D-glucoside.