In this work, we synthesized NiCo 2 O 4 , Fe-MOF nanostructures, and their composite using eco-friendly hydrothermal, simple solvothermal, and ultrasound-assisted co-precipitation methods, respectively. In particular, the metal-organic framework (MOF) employed provided a suitable specific surface area, which served as an appropriate substrate for the transport of ions and electrons. To facilitate this transport, NiCo 2 O 4 nanoparticles were incorporated into the MOF, enhancing not only the substrate efficacy but also the capability for rapid charge transfer, thus improving the electrochemical properties. To validate these attributes, structural, morphological, and surface analyses were conducted, including SEM, XRD, FTIR, BET, and EDXS. Electrochemical evaluation of the prepared electrode, performed using conventional electrochemical techniques (CV, CA, SWV, GCD, and EIS) confirmed its effectiveness as a supercapacitor electrode and a modified electrode for sensing naproxen concentrations. The accomplishment of a specific capacitance (Cs) of 261.4 F g − 1 at 1.0 A g − 1 , coupled with a retention of 95.4% of the initial capacity following 5*10 3 cycles, underscores the impressive performance of the electroactive material. In electrochemical detection of naproxen, under optimized experimental conditions, square wave voltammetry (SWV) revealed a linear response within the 0.05-80 µmol L − 1 range, with LOD of 3.20 × 10 − 3 µmol L − 1 . These findings confirm the reliability of the modified electrode for naproxen quantification in pharmaceutical formulations. Overall, the results show that the used technique has high selectivity and sensitivity, enabling accurate determination of naproxen even in the presence of tablet excipients.
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Mahdi et al. (2026) studied this question.
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