A combined approach for the extraction of antioxidants fromHibiscus sabdariffaand entrapment of the extract in zein nanoparticles is proposed. Different green extraction techniques were adopted: high-pressure and -temperature extraction, ultrasound-assisted extraction, and microwave-assisted extraction, using an ethanol/water mixture as extracting solvent. The extracts were used for the preparation of zein nanoparticles by liquid antisolvent precipitation. The impacts of process variables were investigated using response surface modeling, demonstrating that the proposed strategy allows high extract encapsulation efficiency, good particle size control, and high particle stability.