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Biocompatible materials that can control crystallization while carrying large amounts of active pharmaceutical ingredients (APIs) with diverse chemical properties are in demand in industrial practice. In this study, we investigate the utility of biocompatible alginate (ALG) hydrogels as a rational material for crystallizing and encapsulating model APIs that present drastically different solubilities in water. Acetaminophen (ACM) and fenofibrate (FEN) are utilized as the model hydrophilic and hydrophobic moieties, respectively. ALG hydrogels with different ALG concentrations (hence different mesh sizes) are utilized as heteronucleants to control the nucleation kinetics of ACM from solution. ALG hydrogels with smaller mesh sizes showed faster nucleation kinetics. We hypothesize that this behavior is due to the interplay between the polymer–solute interactions and the mesh-induced confinement effects. The loading of ACM …