Volatile organic compounds (VOCs) are key aroma determinants in pork, and gas chromatography-ion mobility spectrometry (GC-IMS) is an effective technique for their detection. However, the detection conditions for pork using GC-IMS have yet to be standardized. This study employed GC-IMS to investigate the effects of incubation (temperature/duration) and medium (water and different concentrations of NaCl) environments on VOCs in pork. Statistical analyses including t-tests, PLS-DA, and OPLS-DA were employed to assess VOC differences. The results showed that: (1) VOC diversity and intensity increased with incubation temperature and time, with optimal signals obtained at 100 °C for 20 min. (2) The sample medium significantly influenced aroma release. When the medium contained 10% NaCl, the relative content of aldehydes increased, showing that these compounds were optimally released. (3) Under the optimized conditions, 15 key differential VOCs were identified from different muscle tissues, including 10 aldehydes, 2 esters, 1 ketone, 1 alcohol and 1 ether. This work establishes practical GC-IMS parameters for pork VOC analysis and provides a reliable reference for flavor-related studies.