Phytochemical investigations of the aqueous extract of Planchonia careya leaves revealed two known flavonol glycosides, kaempferol 3-O-gentiobioside (1) and quercetin 3-O-glucoside (isoquercitrin) (2), and a novel acylated kaempferol tetraglycoside, kaempferol 3-O-[α-rhamnopyranosyl(1 ! 3)-(2-O-p-coumaroyl)]-β-glucopyranoside, 7-O-[α-rhamnopyranosyl-(1 ! 3)-(4-O-p-coumaroyl)]-α-rhamnopyranoside (3). Structural elucidation was achieved using UV, NMR, and mass spectrometry.