New cardenolide glycoside 1 and steroid glycoside 2, named respectively corotoxigenin-3-O-β- digitalopyranosyl-(1–4)-O-β-digitoxopyanoside and 5∆-pregnene-3β,16α,20(S)-diol 20-O-[β-Ddigitalopyranosyl (1→2)-β-D-glucopyranoside], have been isolated from the leaves of Alafia sp. (Apocynaceae). Compound 2 was isolated for the first time in its natural state, together with the known compounds digitoxin, corotoxigenin, and β-sitosteryl-3-O-β-D-glycopyranoside. The structures of compounds 1 and 2 were elucidated through spectroscopic techniques and chemical methods.