Abstract Volatile compounds from sour guava (Psidium guineense Swartz) fruit were isolated by headspace solid-phase microextraction (HS-SPME) and simultaneous distillation-solvent extraction (SDE), and identified by GC-FID and GC/MS. A total of 181 compounds were reported for the first time in this fruit, 119 and 163 compounds were identified as headspace volatiles and fruit volatiles, respectively. Ethyl butyrate, ethyl hexanoate, β-caryophyllene and selin-11 -en-4α-ol were the major compounds. Esters (69.5%) and terpenes (60.8%) were the major classes of compounds found in the headspace volatiles and fruit volatiles.