The present paper demonstrated the impedance analysis of Au/TiO2 nanoparticles/Si-Al capacitive sensor for selective detection of VOCs at different frequency regimes. TiO2 nanoparticles (NP) were synthesized through solution process and characterized by Field-emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) analysis, Photoluminescence spectroscopy, and Atomic force microscopy (AFM). The gas sensitivity of Au/TiO2-NP/Si-Al was investigated, with the effect of temperature modulation (25-250°C) and dielectric variation at the vicinity of nanoparticles. Impedance spectroscopy of TiO2-NP was carried-out to obtain resonant peaks over the frequency ranging from 0.05-225 kHz and fitted with a complex nonlinear least-squares method. The optimum sensor response of 136%, 63%, 152%, and 174% was found at resonant frequencies of 0.38 kHz, 0.22 kHz, 0.15 kHz, and 0.1 kHz for the exposure of 2-propanol, acetone, ethanol, and methanol, respectively. The fastest response time and recovery time were found to be 32/21s, 31.2/8s, 32.5/9s, and 40/26s for acetone, 2-propanol, ethanol, methanol, respectively. Selective detection of different VOCs at various resonant frequencies has correlated with the dielectric variation of the NPs and its associated void region under gas exposure.