Antibiotics are essential for treating illnesses, but abuse has resulted in serious consequences. Rapid and precise detection of antibiotic residues, such as sulfamethazine (SFZ), in water and biological samples is critical for public health and environmental safety. To address this challenge, we have introduced a pioneering electrochemical sensor incorporating a nanocomposite of perovskite-structured praseodymium cobaltite (PrCoO 3 ) integrated with carbon nanofibers (CNFs) on a glassy carbon electrode (GCE|CNF/PrCoO 3 ). We synthesized the CNF/ PrCoO 3 nanocomposite using ultrasonic fabrication and confirmed its formation with advanced techniques. GCE|CNF/PrCoO 3 offer superior SFZ detection with a 2.889 nM/L limit and high selectivity, due to PrCoO 3 's electrocatalytic properties and CNF's enhanced conductivity. We validated the sensor's effectiveness in detecting SFZ in various real-water samples, demonstrating its repeatability, reproducibility, and stability. This confirms its reliability for environmental monitoring. The study highlights the potential of perovskite−carbon composites and paves the way for developing cost-effective sensors for pharmaceutical contaminants.