The determination of total aglycons released by enzymatic hydrolysis of cupuaçu, bacuri, and acerola glycosidic extracts indicates significant amounts of glycosidically bound volatile components in these fruits. Glucosides and rutinosides were the main glycoconjugates present as indicated by structural analysis of the saccharidic moieties. Moreover malonylated derivatives were detected in bacuri and cupuaçu; and "unusual" glycosides were possible constituents of the heterosidic fraction of amazonian fruits. In cupuaçu, aliphatic and terpenic alcohols were characteristic volatile compounds liberated by enzymatic hydrolysis of glycosides. Terpenic alcohols and diols, as well as 2-phenylethanol, were the most abundant aglycons in bacuri, whereas aliphatic alcohols and norisoprenoid compounds were detected as major components of acerola glycosidically bound volatiles. In agreement with the results obtained for aglycon determinations, several glucosides, rutinosides and one vicianoside were identified in these fruits by GC/EI-MS and/or GC/NCI-MS of their TFA derivatives.