In this study, we collected and prepared ethanol extracts from 30 vegetable and fruit by-products and screened for antioxidant activities using three methods, including determination of total phenolic content (TPC), 2,2-diphenyl-1-picrylhydrazyl free radical scavenging assay (DPPH assay), and ferric reducing/antioxidant power assay (FRAP assay). The coffee sediment (TN-16) and ginger peel extract (TN-17) showed vigorous activities and higher than those of other samples (p < 0.05). The TPC in TN-16 and TN-17 were 66.14 mgGAE/g and 146.52 mgGAE/g, respectively. For the DPPH assay, the IC 50 inhibited the values of 16.73 µg/mL with TN-17 and 33.57 µg/mL with TN-16. For the FRAP, a significant difference in absorbance was observed between all samples (p < 0.05), and TN-16 and TN-17 have strong activities with higher absorbances. Besides, fifteen compounds may present in TN-16 namely, metiamide, manitol, 3-amino phenol, malicyamide, phenyl ethanolamine, 3-methoxyamphetamine, caffeine, nisoldipine, doxenitoin, dicyclohexyl phthalate, febuprol, 2.4 xylidine, glycerol 2-palmitate, 4-(benzylamino) phenol, o-toluidine were identified by HPLC-EIS-MS. In addition, the coffee sediment extract was investigated the ability to preserve fish meal in 30 days at the room temperature. The result showed that the coffee sediment was the potent extract for the protection of fish meal against lipid peroxidation as compared to synthetic antioxidants.