<p>Sterilization methods are widely used in food research to prevent and eradicate microbial contamination prior to inoculation with microorganisms of interest. Thermal treatments such as autoclaving may alter the physical, chemical, and sensory properties of agricultural products. This study evaluated the effect of autoclaving parchment coffee beans on chemical composition with focus on volatile organic compounds (VOC) and sensory attributes in comparison with conventional processing (non-autoclaved). VOC were tentatively identified by SPME/GC–MS in green coffee beans, roasted coffee beans, and the resulting coffee beverage. Sensory evaluation was performed using discrimination and acceptance tests with untrained panelists. Among the 83 VOC detected, 16, 5, and 10 compounds showed significant differences — between autoclaved and non-autoclaved — in green coffee beans, roasted coffee beans, and coffee beverage, respectively. Multivariate analysis indicated that most discriminant VOC were associated with autoclaved samples across all matrices. Autoclaving significantly altered the volatile profile and affected key sensory attributes of the beverage, contributing to a more intense aroma and flavor perception. The triangular test confirmed that panelists were able to discriminate between beverages prepared from autoclaved and non-autoclaved green coffee beans. These findings demonstrate that autoclaving parchment coffee beans induces persistent chemical changes that influence sensory perception and should be carefully considered in food research and coffee processing applications. To the best of our knowledge, this is the first study reporting the impact of autoclaving parchment coffee beans on both the volatile composition and sensory properties of the resulting coffee beverage.</p>