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This paper focusses on the intercalation of clay mineral with gentamicin (an aminoglycoside antibiotic). The smectite clay-gentamicin hybrids were prepared by a solution intercalation at 60 • C and the process was carried out on unmodified smectite clay and on smectite after Na + ionic activation. The resulting structural/microstructural properties and the potential for introducing gentamicin between smectite clay layers were investigated by means of X-ray diffraction, Fourier transform infrared spectroscopic techniques and transmission electron microscopy and scanning electron microscopy with energy-dispersive spectroscopy X-ray analysis. The results confirm the successful intercalation of gentamicin into the interlayer space of smectite clay, demonstrating that the material thus obtained could potentially be used as a drug carrier.