Currently, electrospraying is a novel process for obtaining the nanoparticles from biopolymers. Zein nanoparticles have been obtained by this method and used to protect both hydrophilic and hydrophobic antioxidant molecules from environmental factors. The objective of this work was to prepare and characterize gallic acid-loaded zein nanoparticles obtained by the electrospraying process to provide protection to gallic acid from environmental factors. Thus, it was related to the concentration of gallic acid in physicochemical and rheological properties of the electrosprayed solution, and also to equipment parameters, such as voltage, flow rate, and distance of the collector in morphology, and particle size. The physicochemical properties showed a relationship in the formation of a Taylor cone, in which at a low concentration of gallic acid (1% w/v), low viscosity (0.00464 ± 0.00001 Pa·s), and density (0.886 ± 0.00002 g/cm3 ), as well as high electrical conductivity (369 ± 4.3 µs/cm), forms a stable cone-jet mode. The rheological properties and the Power Law model of the gallic acid-zein electrosprayed solution demonstrated Newtonian behavior (n = 1). The morphology and size of the particle were dependent on the concentration of gallic acid. Electrosprayed parameters with high voltage (15 kV), low flow rate (0.1 mL/hr), and short distance (10 cm) exhibited a smaller diameter and spherical morphology. FT-IR showed interaction in the gallic acid-loaded zein nanoparticle by hydrogen bonds. Therefore, the electrospraying process is a feasible technique for obtaining gallic acid-loaded zein nanoparticles and providing potential protection to gallic acid from environmental factors.