This study presents the development of zirconium polycarboxylate gel systems as substrates for advanced fluorescence sensing devices. Zirconium-based metal–organic gels (MOGs) offer a promising alternative due to the robustness of the Zr–O bond, which provides enhanced chemical stability. In this work, zirconium polycarboxylate gels were synthesized using green solvents in a rapid room temperature method. Fluorescein, naphthalene-2,6-dicarboxylic acid, and 4,4′,4″,4‴-(porphine-5,10,15,20-tetrayl)tetrakisbenzoic acid were incorporated as fluorophores to give the gel luminescent properties, enabling it to be used as a sensor. These fluorophores produce specific changes in the perceived color and intensity of the fluorescence emission upon interaction with different analytes in a solution, allowing a qualitative identification of different solvents and compounds. However, the fragile structure of neat gels hinders reproducible quantitative analysis of fluorescence emission. Therefore, to increase their mechanical stability during manipulation, a composite material was developed by combining the MOGs with quartz microcrystals, which proved to be a more reliable fluorescent system. The results show that the material can identify univocally different solvents and analytes in aqueous solutions by the quantitative analysis of the emission intensities. This work presents an innovative approach to create advanced fluorescence sensors with improved mechanical properties and stability using zirconium polycarboxylate gels and multiple fluorophores.