Lyaloside, a monoterpenoid glucoindole alkaloid, was isolated from the leaves of Palicourea adusta together with a mixture of its hydroxycinnamic acid derivatives, (E)-O-(6')-cinnamoyl-4 -hydroxy-3 -methoxy-lyaloside and (E)-O-(6')-cinnamoyl-4 -hydroxy-3 ,5 -dimethoxy-lyaloside, which have been separated for the first time by high pressure liquid chromatography (HPLC). Their molecular weights were determined by HPLC electrospray ionization mass spectrometry (ESI-MS) and further identification of the structures was carried out by spectroscopic methods. (C) 1999 Elsevier Science Ltd. All rights reserved.