Resumen: A model (sucrose and gallic acid) solution was concentrated by block freeze concentration (BFC) at three centrifugation cycles, and the solutions were encapsulated in calcium alginate and corn starch calcium alginate hydrogel beads. Static and dynamic tests determined the rheological behavior, differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR) established thermal and structural properties, and the release kinetics was evaluated under in vitro simulated digestion experiment. The highest efficiency encapsulation value was close to 96%. As the concentrated solution increased in terms of solutes and gallic acid, the solutions were fitted to the Herschel–Bulkley model. Moreover, from the second cycle, the solutions exhibited the highest values of storage modulus (G′) and loss modulus (G″), contributing to form a more stable encapsulation. The FTIR and DSC results demonstrated strong interactions between corn starch and alginate, establishing a good compatibility and stability in the bead formation. The kinetic release model under in vitro conditions was fitted to the Korsmeyer–Peppas model, demonstrating the significant stability of the model solutions inside the beads. Therefore, the present study proposes a clear and precise definition for the elaboration of liquid foods obtained by BFC and its incorporation inside an edible material that facilitates the controlled release in specific sites.