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The present work introduces new hybrid materials based on the combination of layered double hydroxides (LDH) and two biopolymers (a protein and a polysaccharide) to produce LDH–biopolymer nanocomposites, able to act as effective drug delivery systems (DDS) in comparison to the LDH or the biopolymers alone. Ibuprofen (IBU) has been chosen as a model drug, being intercalated in a Mg–Al LDH matrix. The resulting hybrid is used to prepare bionanocomposite materials by association with two biopolymers: (i) zein, a highly hydrophobic protein, and (ii) alginate, a polysaccharide widely applied for encapsulating drugs. Characterization of the IBU/Mg–Al LDH intercalation compound and the bionanocomposites resulting from its incorporation into alginate–zein matrices of different composition was carried out by means of different experimental techniques: X-ray diffraction, infrared spectroscopy, chemical and …