| Summary: | This study used substituted barium hexaferrites, which were previously prepared and reported by the authors, to detect acetaminophen by the modification of a conventional glassy carbon electrode (GCE), which led to promising results. The synthesis of this electrode-modifying material was conducted using a citrate sol gel process. A test synthesis using glycerin and propylene glycol revealed that glycerin produced a better result, while less positive anodic potential values were associated with the electrooxidation of N-acetyl-p-aminophenol (NAP). Excellent electroactivity was exhibited by the cobalt-substituted barium-hexaferrite-nanomaterial-modified electrode. A good linear relationship between the concentration and the current response of acetaminophen (paracetamol) was obtained with a detection limit of (0.255 ± 0.005) µM for the Ba<sub>1.0</sub>Co<sub>1.22</sub>Fe<sub>11.41</sub>O<sub>18.11</sub> GCE, (0.577 ± 0.007) µM for the Ba<sub>1.14</sub>Cu<sub>0.82</sub>Fe<sub>11.65</sub>O<sub>18.02</sub> GCE, and (0.595 ± 0.008) µM for the bare GCE. The levels of NAP in a real sample of urine were quantitatively analyzed using the proposed method, with recovery ranges from 96.6% to 101.0% and 93.9% to 98.4% for the modified electrode with Cobalt-substituted barium hexaferrites (CoF<sub>M</sub>) and Copper-substituted barium hexaferrites (CuF<sub>M</sub>), respectively. These results confirm the high electrochemical activity of Ba<sub>1.0</sub>Co<sub>1.22</sub>Fe<sub>11.41</sub>O<sub>18.11</sub> nanoparticles and thus their potential for use in the development of sensing devices for substances of pharmaceutical interest, such as acetaminophen (NAP).
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