The drying process of microcrystalline cellulose and adipic acid particles in a cylindrical fluidized bed was investigated using the Gaussian spectral technique to monitor fluid–dynamic regime transitions associated with surface moisture loss. Pressure fluctuation signals were recorded and analyzed to assess hydrodynamic behavior. Excess moisture significantly alters the bubbling characteristics of the bed, leading to instability in the fluidization regime. The results demonstrated that the Gaussian spectral technique effectively captured these hydrodynamic changes, particularly at the critical moisture content threshold, when compared with the drying rate curves of the materials. For microcrystalline cellulose and adipic acid particles, it is reasonable to conclude that a mean central frequency above 5.75–6.0 Hz and a standard deviation exceeding 3.7–3.8 Hz correspond to a bubbling regime, indicating that the critical drying point has been reached. This approach provides a non-intrusive and sensitive method for identifying transitions in the drying process, offering a valuable tool for real-time monitoring and control. The ability to track fluidization regime changes with high precision reinforces the potential of this technique for optimizing drying operations in the pharmaceutical, food, and chemical industries.