High speed centrifugal countercurrent chromatography (HSCCC) was successfully applied to preparative isolation of the main polar phenolics from the Peruvian Caricaceae Vasconcellea quercifolia A. St.-Hil. High-performance liquid chromatography with diode array (HPLC-DAD) and electrospray ionisation mass spectrometric detection (ESI-MS) was used to carry out a comprehensive characterisation of phenolic compounds from fruits and leaves of this plant. The main phenolics were the quercetin diglycoside rutin and the triglycoside manghaslin. Nine minor flavonoids were tentatively identified as kaempferol, quercetin, isorhamnetin and methoxymyricetin glycosides. HSCCC combined with other chromatographic methods allowed the isolation of the main phenolics from the plant. HPLC-DAD-MS analysis shows that the main phenolic compounds in V. quercifolia are similar to those described for V. pubescens but differs in the identity of the minor constituents.