This work introduces a novel approach by synthesizing a pyrazole azo dye (PZ) and demonstrating its application in a highly effective electrochemical sensor. The structure of the newly synthesized dye was confirmed through 1H NMR, UV–visible, mass, and FT-IR. The PZ-modified carbon paste electrode (PZ/MCPE) was further employed for the simultaneous voltammetric detection of paracetamol (PA) and folic acid (FA) in phosphate buffer solution (PBS) at pH 7.0. Electrochemical studies were carried out using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The PZ/MCPE revealed well-defined and distinctly separated oxidation peaks for PA and FA. The fabricated sensor exhibited a linear detection range between 10 and 70 µM, along with low limits of detection and quantification for both PA and FA, respectively. Further, interference studies confirmed the sensor’s selectivity in the presence of potential coexisting species. The reproducibility and stability of the sensor were also evaluated, demonstrating consistent performance and reliable analytical performance.