Electrochemical sensors are inherently dependent upon novel electrocatalyst materials with excellent properties. A rapid analytical technique was developed to determine 5-aminosalicylic acid (5-ASA) without the need for time-consuming separation steps. In this study, the perovskite-type barium molybdate (BaMoO3) nanocubes and phosphorous-doped graphitic carbon nitride (P-gC3N5) were prepared by coprecipitation followed the chemical vapour deposition method. Various spectroscopic techniques were performed to analyse the morphology and structure of the proposed electrocatalyst (BaMoO3/P-gC3N5). BaMoO3/P-gC3N5 modified glassy carbon electrodes (GCE) exhibit superior electrocatalytic activity towards 5-ASA detection over unmodified electrodes. Difference Pulse Voltammetry (DPV) was used under optimal experimental conditions for determining 5-ASA accurately. Combining BaMoO3 and P-gC3N5 forms an electrocatalytic hybrid composite with a large specific surface area, rapid electron transfer, and high electrical conductivity. BaMoO3/P-gC3N5 modified electrodes possess a broad detection range (0.01–723 µM), low limit of detection (4.0 nM), excellent selectivity, sensitivity (1.046 µAµM-1cm−2), and good reproducibility toward the detection of 5-ASA. Human serum, urine, and river water samples were successfully tested for 5-ASA content with the electrochemical sensor fabricated.
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