The main compounds of off-odor volatiles from irradiated refrigerated vacuum-packaged pork were analyzed by gas chromatograph/mass spectrometer (GC-MS). The analytical results showed that the main compounds of off-odor volatiles were dimethyl disulfide, dimethyl sulfide, dimethyl trisulfide, S-methyl thioacetate, and methanethiol. It was proved that the off-odor volatile came from irradiated S-containing amino acid and thiamin.