Non-alcoholic (NA) wines and spirits are becoming increasingly popular, just like NA beers. Unlike beer, these beverages present greater challenges for alcohol removal due to their higher starting alcohol concentrations. As a result, preserving the volatile organic compounds (VOCs) is more difficult, which contributes to the desired flavors of these beverages. To characterize the VOCs and sensory profiles of alcoholic and NA wines and spirits, this study employs a simultaneous immersion technique with GERSTEL’s Twister and thin film-solid phase microextraction (TF-SPME) devices. The GERSTEL Olfactory Detection Port (ODP 4) facilitated sensory-active compound identification, providing a detailed comparison between alcoholic and NA beverages.