Spray-drying is one of the oldest and most widely used dehydration techniques. It involves converting liquid feeds, such as solutions, dispersions, or emulsions, into powders. Additionally, spray-drying is a popular method for encapsulating or immobilizing compounds into polymeric matrices when a carrier is used. Among the carriers, maltodextrins, modified starches, and Arabic gum are the most commonly used materials. The particles produced by spray-drying are matrix-type, shrunken hollow spheres that vary in size from submicron to micron scale, depending on the atomizer employed. Using spray-dried particles as carriers for food compounds has several advantages, including protection against degradation, improved dispersibility or solubility, easier handling of labile liquids, reduced volatilization, and masking unpleasant tastes or odors. This protocol aims to guide the reader through the key steps of spray-drying encapsulation, including selecting carriers and operational conditions, providing an overview of the most critical influencing factors, and offering tips on how to overcome some of the process challenges.