Microencapsulation by atomization can be used to minimize the loss of bioactive compounds, improving the characteristics and applicability of the powdered product. This study evaluates the effect of different encapsulating agents (maltodextrin, gum arabic, and chitosan) and three spray nozzle diameters (1.0, 1.2, and 1.5 mm) on the atomization of guavira (Campomanesia adamantium) pulp with added 6% bocaiuva (Acrocomia aculeata) dehydrated pulp in the green maturation stage. The experiment followed a simplex-centroid mixed design, with carrier agent concentrations and spray nozzle diameters as independent variables and powder yield, solubility, hygroscopicity, and vitamin C content as dependent variables. The results show that gum arabica increased powder yield and vitamin C retention. The addition of maltodextrin resulted in powders with increased solubility and low hygroscopicity. Furthermore, the optimization tool indicated that the best process conditions were achieved with the addition of gum arabic (10.8%) and chitosan (7.2%), resulting in powders with 29.48% yield, 82.96% solubility, 15.90% hygroscopicity and 741.11 mg/100g vitamin C. Furthermore, the 1.0 mm diameter spray nozzle was considered the most suitable for obtaining guavira pulp microparticles with higher ascorbic acid content.