For encapsulating bioactive substances, electrospraying is a flexible and effective method that is especially useful in the nutraceutical industry. Using this technique, solutions, emulsions, or suspensions are turned into small droplets while being exposed to an electric field. Material encapsulation is achieved through the solidification of such tiny droplets into components that are either nano- or micro-sized. In this chapter, a methodology for encapsulation of bioactive compounds, especially epigallocatechin gallate (EGCG) within a low-cost commercially available natural biopolymer, i.e., gelatin through the electrospraying method, is described in detail. The chapter also elucidates the encapsulation efficiency of EGCG using the same method.