This study presents the development and characterization of a Mg3Al-COX hybrid system, designed to enhance the bioavailability of celecoxib (COX), a BCS class II hydrophobic anti-inflammatory drug. Mg/Al layered double hydroxides (LDHs), with a 3 : 1 ratio, were synthesized via coprecipitation and calcination methods and then used to trap COX through a reconstitution process in a 60/40 v/v ethanol/water mixture. Comprehensive characterization using XRD, FTIR, TGA/DSC, BET, and SEM/EDS techniques confirmed the successful incorporation of COX within the LDHs matrix. Batch loading studies investigated the effects of contact time, initial pH, host material quantity, initial COX concentration, and temperature on the loading capacity Qe (mg/g). Kinetic analyses revealed that COX fixation follows a pseudo-second-order model, with intraparticle diffusion occurring in two distinct stages. Thermodynamic analysis detected a spontaneous and exothermic process. The Sips equation best represents the adsorption equilibrium by providing the highest correlation with a maximum loading capacity of 220.10 mg/g. Parameter calculations and error analyses validated the models used for the kinetic, thermodynamic, and equilibrium studies. These results demonstrate the feasibility of using LDHs as inclusion matrices to enhance the release properties of celecoxib, thereby paving the way for the development of controlled-release dosage forms.