Epidemiological evidence indicates that plant antioxidants activity can treat or help to prevent the development of various diseases. One species with great potential as an antioxidant is Curcuma longa. However, different extraction techniques can influence isolated chemical compounds. This study investigated chemical composition and antioxidant activity of two rhizome extracts of C. longa: hydroethanolic, obtained by exhaustion (HECLex); and dried by a spray dryer (HECLsd). The phytochemical composition was evaluated by GC/MS. Antioxidant activity was evaluated using DPPH and FRAP assays. Total phenolic compounds and soil analyses were performed. The main components of HECLex were ar-turmerone, γ-curcumene, α-turmerone, and β-sesquiphellandrene. The main components of HECLsd were 9,12,15-octadecatrienoic acid, 2,3-bis([trimethylsilyl]oxy)propyl ester, verrucarol, and 1-monolinoleoylglycerol trimethylsilyl ether. HECLsd had significantly higher levels of phenolic compounds and higher antioxidant capacity compared with HECLex. In conclusion, processes of the preparation of C. longa rhizomes alter the chemical components and consequently their biological activity.