Polyelectrolyte microcapsules represent a promising strategy for the controlled delivery of therapeutic enzymes, yet optimizing their properties remains challenging. This thesis investigates how the chemical composition of natural polymers, capsule shell thickness, and external protein concentration affect the enzyme loading efficiency, and release kinetics of polyelectrolyte microcapsules. β-galactosidase was encapsulated as a representative therapeutic enzyme. Capsules were fabricated by layer-by-layer (LbL) assembly on CaCO₃ microparticle templates, alternating gelatin or chitosan (polycations) with alginate or dextran sulfate (polyanions), and finally capping the shell with an outer hyaluronic-acid (HA) layer that can bind the CD44 receptor over-expressed on many cancer cells, enabling targeted delivery. Results indicated that gelatin-based capsules demonstrated significantly faster enzyme release than chitosan-based capsules, primarily due to differences in charge density, and electrostatic interactions. Increasing the number of polymer layer pairs effectively reduced capsule permeability, resulting in slower and sustained enzyme release. Additionally, the release of the enzyme was enhanced in the presence of bovine serum albumin (BSA), with higher BSA concentrations causing greater disruption of polymer interactions, thus facilitating increased enzyme release. This study contributes to the theoretical understanding of polymer-protein interactions and offers practical insights into designing biocompatible capsules for drug delivery applications, notably in targeted cancer immunotherapy. However, the research was limited by its approach and the use of a non-therapeutic model enzyme. Future work should examine in vitro capsule performance and using clinically relevant enzymes.