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ABSTRACT This study was conducted to identify the key volatile compounds that characterize whether silage has deteriorated and to investigate the intrinsic link between the key compounds and silage odor. First, silages with different aerobic exposure durations were sampled, and sensory evaluation integrating aerobic stability monitoring was used to distinguish whether the silage had deteriorated. Subsequently, headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) was utilized to determine the relative content of the compounds. Using the relative content of the compounds in each silage as input, relative odor activity value (ROAV) calculations and orthogonal partial least squares discriminant analysis (OPLS-DA) were performed to determine the odor contribution of the compounds and the compounds with significant differences in relative content (based on variable importance for the projection, VIP) between the deteriorated and non-deteriorated silages. Next, the key compounds were identified by combining the conditions of average ROAV (aROAV) ≥ 1 and VIP > 1. Finally, the OPLS algorithm was used to analyze the intrinsic link of key compounds with the silage odor. The results showed that three out of 63 compounds—4-ethyl phenol, eugenol, and ethyl linoleate—were key compounds to characterize whether the silages deteriorated or not. In addition, ortho-guaiacol, 4-ethyl guaiacol, and 2-methoxy-4-vinyl phenol were the specific key compounds for deteriorated silage. Eugenol and ethyl linoleate were correlated with fruity, sour, and spicy odors. In addition, guaiacol, 4-ethylphenol, 4-ethyl guaiacol and 2-methoxy-4-vinyl phenol contributed to roasted, musty, and putrid odors.