Globalization and industrialization have significantly exacerbated air pollution, particularly through the increase of volatile organic compounds (VOCs), posing severe health risks and environmental challenges. The need for effective VOC detection at room temperature has become critical. In this study, a novel β-Cyclodextrin coated MoO3-ZrO2 nanocomposite was synthesized via a cost-effective simple sol-gel method, aiming to enhance gas sensing properties. Comprehensive characterization techniques confirmed the formation of a mesoporous Zr(MoO4)2 structure with smooth surface morphology in the β-CD coated nanocomposites. The gas sensing performance of the synthesized nanocomposites was rigorously evaluated, with results indicating significantly improved activity towards VOCs at room temperature (30 °C). Among the various compositions, the 10 % β-CD coated MoO3-ZrO2 nanocomposite exhibited the highest response to acetone vapors, with a remarkable sensing response of 1.97, a fast response time of 30 s, and a recovery time of 39 s at a concentration of 100 ppm. This enhanced performance is attributed to the increased specific surface area, the porous structure of the composite, and the unique interaction between acetone and the active sites on the nanocomposite. Comparative analysis with literature-reported materials highlights the superior room-temperature performance of the 10βMZ nanocomposite, positioning it as a promising material for VOC detection in environmental monitoring and industrial safety. This study not only advances the understanding of composite gas sensors but also introduces a novel catalytic system with enhanced gas sensing activity, selectivity, and reusability.