The object of this study was tilapia fish that were fried in soybean oil. Volatile compounds were extracted from the fish by ASE-HVE and were studied by GC-O-MS and the AEDA analysis method. A total of 30 aroma compounds were initially determined, and these compounds contribute to the aroma of fried tilapias. The key volatile compounds in fried tilapia were quantitatively analyzed by GC-MS, and the volatile compounds in soybean-fried tilapia were studied by flavor recombination and deletion experiments. Trimethylamine, hexanal, 2,3-dimethylpyrazine, dimethyl trisulfide, trans-2-octenal, 2,3-dimethyl-5-ethylpyrazine, (E)-2-nonenal, 2-propyl-pyridine, and (E,E)-2,4-decadienal were finally determined to be the key volatile compounds in soybean-fried tilapia.