| Summary: | Design of a smart drug delivery system is a topic of current interest. Under this perspective, polymer nanocomposites (PNs) of butyl acrylate (BA), methacrylic acid (MAA), and functionalized carbon nanotubes (CNTs<sub>f</sub>) were synthesized by in situ emulsion polymerization (IEP). Carbon nanotubes were synthesized by chemical vapor deposition (CVD) and purified with steam. Purified CNTs were analyzed by FE-SEM and HR-TEM. CNTs<sub>f</sub> contain acyl chloride groups attached to their surface. Purified and functionalized CNTs were studied by FT-IR and Raman spectroscopies. The synthesized nanocomposites were studied by XPS, <sup>13</sup>C-NMR, and DSC. Anhydride groups link CNTs<sub>f</sub> to MAA–BA polymeric chains. The potentiality of the prepared nanocomposites, and of their pure polymer matrices to deliver hydrocortisone, was evaluated in vitro by UV–VIS spectroscopy. The relationship between the chemical structure of the synthesized nanocomposites, or their pure polymeric matrices, and their ability to release hydrocortisone was studied by FT-IR spectroscopy. The hydrocortisone release profile of some of the studied nanocomposites is driven by a change in the inter-associated to self-associated hydrogen bonds balance. The CNTs<sub>f</sub> used to prepare the studied nanocomposites act as hydrocortisone reservoirs.
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