The volatiles of longon (Lansium domesticum Corr. var Dongon), mangosteen (Garcinia mangostana L. var Native), durian (Durio zibethinus L. var Monthong), rambutan (Nephelium lappaceum L. var Rong-rien), and sapodilla (Manilkara zapota van Royer var Kai) were identified by headspace-solid phase microextraction with the gas chromatography-mass spectrometry technique. The headspace volatiles of fresh, unheated, salted out with NaCl, and NaCl + heated samples were determined. Salting out gave the highest number of volatile components with the longon headspace. High temperature did not have much affect on the amount of volatiles in the headspace. Major volatiles of the total 43 volatiles in longon were 1,3,5 trioxane, (E)-2-hexenal, 3-carene, α-cubebene, isoledene, δ-selinene, and α-calacorene. Major volatiles of mangosteen were 2, 2-dimethyl-4-octanal, E-2-hexenal, benzaldehyde, (Z)-3-hexen-1-ol, hexyl–n-valerate, 1,4-pentadiene, and 2-methyl-1, 3-buten-2-ol. Volatile compounds in durian consisted of a large number of sulfur-containing compounds, which included diethyltrisulfide, diethyldisulfide, dithiolane, dimetyl sulfide, and 3-methyl-thiozolidine. Nonsulfur compounds 2-methyl butanoate, butanedioic acid, and propyl-2-ethylbutanoate were also abundant. Isocitonellol, 3-hydroxy-2-butanone, pentanal, and 4-tridecyl valerate were most abundant in ‘Rong-rien’ rambutan. A total of 23 components were characterized in sapodilla with ethyl acetate, acetaldehyde, benzyl alcohol, and 2-butenyl benzene being the major volatiles.