The present work introduces new biohybrid materials involving layered double hydroxides (LDH) and biopolymers to
produce bionanocomposites, able to act as effective drug delivery systems (DDS). Ibuprofen (IBU) and 5-aminosalicylic
acid (5-ASA) have been chosen as model drugs, being intercalated in a Mg–Al LDH matrix. On the one side, the LDHIBU
intercalation compound prepared by ion-exchange reaction was blended with the biopolymers zein, a highly
hydrophobic protein, and alginate, a polysaccharide widely applied for encapsulating drugs. On the other side, the LDH-
5-ASA intercalation compound prepared by co-precipitation was assembled to the polysaccharides chitosan and pectin,
which show mucoadhesive properties and resistance to acid pH values, respectively. Characterization of the intercalation
compounds and the resulting bionanocomposites was carried out by means of different experimental techniques: X-ray
diffraction, infrared spectroscopy, chemical and thermal analysis, as well as optical and scanning electron microscopies.
Data on the swelling behavior and drug release under different pH conditions are also reported.