Studies have shown that herbal extractions may be effective against various diseases like cancer and cardiovascular disease. In this study, we intended to evaluate the cytotoxicity and antioxidation activity of phytochemical constituents from the leaves of Aquilaria agallocha and the stems of Aquilaria sinensis. The chemical structures were identified by UV, IR, ESI-MS, 1H NMR and 13C NMR analyses. 5- hydroxy-7, 4'-dimethoxyflavone (1), 5, 3'-dihydroxy-7, 4'-dimethoxyflavone (2), 5-hydroxy-7, 3', 4'- trimethoxyflavone (3), 5, 7, 4′-trihydroxyflavone (4), and 3', 4', 5, 7-tetrahydroxyflavone (5) were isolated and further examined antioxidation and antiproliferation activity by 2, 2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging and MTT assay. According these results, 5-hydroxy-7, 3', 4'- trimethoxyflavone (3) had DPPH radical scavenging activity. Further, 5-hydroxy-7, 3', 4'- trimethoxyflavone (3) also showed significant positive anticancer activities (10-100 μM) against human skin cancer cell line A375 cells.