Hybrid polysaccharide-based aerogels offer significant potential as advanced drug delivery platforms due to their tunable structure, high porosity, and biocompatibility. In this study, aerogel microparticles were synthesized using alginate, pectin, carrageenan, and their hybrid formulations via an emulsion–gelation technique followed by supercritical fluid CO2 extraction. The resulting aerogels exhibit mesoporous structures with specific surface areas ranging from 324 to 521 m2/g and pore volumes between 1.99 and 3.75 cm3/g. Comprehensive characterization (SEM, gas sorption, XRD, TGA, DSC, and FTIR) confirmed that hybridization improved morphological uniformity and thermal stability compared to single polymer aerogels. Ibuprofen was used as a model drug to evaluate loading efficiency and release kinetics. Among all formulations, the alginate/carrageenan (2:1) hybrid showed the highest drug loading efficiency (93.5%) and a rapid release profile (>90% within 15 min), closely matching the performance of commercial ibuprofen tablets. Drug release followed Fickian diffusion, as confirmed by the Korsmeyer–Peppas model (R2 > 0.99). These results highlight the potential of hybrid polysaccharide aerogels as vehicles for drug delivery and other fast-acting therapeutic applications.
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