This study aims to improve knowledge on donkey meat and the vacuum aging effect on the Volatile Organic Compounds (VOCs), oxidative profile and status and the sensory characteristics. Ten 18-month old Martina Franca donkeys’ male foals were involved in the trial. Longissimus thoracis (LT) muscle was extracted from each left half carcass, between the fourth and the ninth rib. Each muscle was divided into five sections, vacuum packaged, stored at 2 °C, and randomly assigned to one of the different aging time (1, 3, 6, 9, and 14 days of aging). Volatile compounds, oxidation parameters, and antioxidant enzymes were analysed, and a sensory test was performed. A nested one-way analysis of variance (ANOVA) was performed for aging time as an independent variable. Significance was set at p < 0.05. Aldehydes are the most produced VOCs, but no changes were observed during vacuum aging (p > 0.05). Nitrogen compounds increased during aging (p < 0.01). TBARs and hydroperoxides did not change during the storage, whereas the protein carbonyls increased (p < 0.05). Vacuum aging slowed down lipid oxidation and put in evidence the presence of protein oxidation and degradation, influencing the VOCs productions and sensory evaluation.