Araçá fruit extracts were dried at different air conditions, and an investigation of the impact of drying on the volatile composition and antioxidant activity of araçá extracts was conducted. The effective moisture diffusivity varied between 8.542 × 10−8 and 13.34 × 10−8 m2/min. Fruit extracts dried at 50°C and 2.0 m/s had the highest total antioxidant activity (1916.10 mgascorbic acid/100 garaçá). The highest phenolic content (556.28 mgGAE/100 garaçá) was obtained when fruits were dried at 40°C and 1.5 m/s, but the resulting extract contained high amounts of 5-hydroxymethylfurfural (HMF), a contaminant formed in sugar-rich foods as a result of heating. Araçá extracts had similar qualitative profiles of volatile compounds by GC-MS, with caryophyllene being the most abundant terpene, followed by 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, selina-3,7(11)-diene, γ-terpinene, γ-cadinene, and α-salinene. HMF corresponded to the major peak in all chromatograms, proving that thermal drying affected the quality of the extracts.