Abstract Volatile compounds were isolated from camu-camu (Myrciaria dubia (HBK) McVaugh) fruit by liquid-liquid extraction (LLE), simultaneous distillation-solvent extraction (SDE) and headspace solid-phase microextraction (HS-SPME). The volatile concentrates were examined by GC and GC/MS. A total of 111, 114 and 138 compounds were identified in the LLE, SDE and HS-SPME of the fruit, respectively. Limonene was the major component of these concentrates, followed by Î±-pinene. The relative proportions of the major compounds are shown to be dependent upon the isolation methods.