In this work, we developed cerium oxide/tin oxide (CeO2/SnO2) nanocatalyst with the assistance of urea by a simple sonochemical method and utilized as an efficient electrode material for electrochemical sensing of anti-inflammatory drug 5-aminosalicylic acid (Mesalamine, MES). The CeO2/SnO2 nanoparticles (NPs) were systematically characterized in terms of their crystal structure, morphologies, and physicochemical properties using XRD, Raman, FESEM, HR-TEM, EDX, mapping, and XPS analysis. The characterization results clearly confirmed that the prepared NPs was formed in the phase of CeO2/SnO2 without any other impurities. The electrochemical properties of CeO2/SnO2 NPs were investigated by EIS, CV, and DPV techniques. The CeO2/SnO2 NPs (9.6 μA) modified GCE demonstrated an excellent and improved electrocatalytic activity in terms of higher anodic peak current and lower peak potential when compared to bare GCE (6.7 μA) and CeO2 NPs/GCE (8.2 μA) for the sensing of MES. The CeO2/SnO2 NPs/GCE shows broader linear response range and lower detection limit of 0.02–1572 μM and 0.006 μM, respectively. Moreover, other potentially interfering compounds such as a similar functional group containing biological substances and inorganic species have no interference effect towards MES sensing. In addition, the practicability of the CeO2/SnO2 NPs/GCE was tested by real sample analysis in commercial MES tablet, human urine, and serum samples with the appreciable recovery results.
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