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Beet is a nutritious and health-promoting food with important bioactive compounds in its industrial by-products. The encapsulation of antioxidants from beet by-products has been proposed for valorization. For this, an ethanol–water extract was mixed with polyvinylpyrrolidone (PVP) (used as a carrier agent) and then encapsulated. The encapsulation was performed by spray drying, where the effects of temperature (140–160 °C), extract input flow rate (10–30%), and extraction solvent (ethanol–water 50/50 v/v and ethanol) were evaluated for the total phenol content and the spray-drying yield. The yields obtained were between 60 and 89%, and total phenols were between 136 and 1026 mg gallic acid equivalents/g of encapsulated product. Both responses were affected (p < 0.05) by the extraction solvent. The optimal spray-drying conditions were determined by response surface methodology (RSM). The encapsulated product obtained at optimal conditions was characterized by infrared spectrometry, X-ray fluorescence, Ultra-High Performance Liquid Chromatography, and scanning electron microscopy analysis. The results show that the encapsulated product has a high content of total phenols and compounds such as betanin, isobetanin, and neobetanin. Considering the results of physicochemical properties and the bioactive compounds, the optimized encapsulated product could be applied in the food industry as a bioactive ingredient or natural colorant. However, the further investigation of alternative carrier agents needs to be performed to reduce caking. [ABSTRACT FROM AUTHOR]