The combination of electrospinning and electrospraying techniques for the deposition of inorganic nanoparticles over polymeric nanofibers to create novel multifunctional nanomaterials has been carried out. The combination of these two techniques is essential because by conventional mixing of nanoparticles with polymers and then electrospinning resulted in nanoparticles covered by the polymer and thereby nanoparticles are unavailable for the catalysis applications. This technique is also useful to exploit the application of nanofibers for various applications. Based on the materials chosen, this technology can be applied to various applications such as protective suits, biological applications, catalysis, etc. Here the challenging task is to avoid the aggregation of nanoparticles and improve the distribution of nanoparticles over nanofibers. This was achieved by optimizing various electrospraying parameters (such as feed rate, voltage) and the dispersion properties. The dispersion in solution has been achieved by using a surfactant and optimization of silane modifier concentration and sonication time. Hydrolysis of paraoxon, a nerve agent stimulant was tested for these nanocomposite membranes by UV analysis. Decrease in absorbance was observed for these membranes with time suggesting the detoxification of nerve agent. Hence these membranes can be used as filter media in protective clothing (to detoxify chemical warfare agents to replace the existing charcoal based protection suits wherein the warfare agents are not detoxified rather adsorbed) and air filter applications.