8-Hydroxypyrene-1,3,6-trisulfonic acid (HPTS) dye, a fluorescent dye often used as a pH indicator, is embedded within the bioactive glass matrix and undergoes changes in its fluorescent properties when exposed to carbon dioxide (CO2). The aim of the current study is to investigate the use of bioactive glass (BG) particles containing gamma-Fe2O3@ZnO to enhance the CO2 sensitivity of HPTS. X-ray diffraction, Fourier transform infrared, scanning electron microscopy, and photoluminescence spectroscopies were used to characterize the sol-gel synthesized powders. The sensing slides were prepared in the form of a thin film by immobilizing the fluorescent dye and gamma-Fe2O3@ZnO-based additives into the poly(methyl methacrylate) matrix. The addition of gamma-Fe2O3@ZnO nanoparticles with bioactive glass additives to the HPTS improves the performance characteristics of the sensor, including the linear response range, relative signal variation, and sensitivity. Meanwhile, the CO2 sensitivities were measured as 10.22, 7.73, 16.56, 17.82, 19.58, and 42.40 for the undoped form and M, M@ZnO, 5M@ZnO-BG, 10M@ZnO-BG, and 20M@ZnO-BG NP-doped forms of the HPTS-based thin films, respectively. The response and recovery times of the HPTS-based sensing slide along with 20M@ZnO-BG NPs have been measured as 44 and 276 s, respectively. The gamma-Fe2O3/ZnO-containing BG particle-doped HPTS composites can be used as a promising sensor agent in the detection of CO2 gas in various fields such as environmental monitoring, medical diagnostics, and industrial processes.