Abstract <p>Antibiotic residues in food threaten public health by promoting antimicrobial resistance. Chloramphenicol (CAP), banned in food-producing animals, can be rapidly and sensitively detected using cost-effective electrochemical techniques. In this study, an iron-doped zeolite (Fe/ZSM-5) modified carbon paste electrode (CPE-30 wt%/Fe-ZSM-5) was fabricated and characterized electrochemically using cyclic voltammetry. The sensor exhibited the highest current response of 202.03 µA and the largest electroactive surface area of 0.162 cm² in the Fe(CN)₆³⁻/Fe(CN)₆⁴⁻ redox system, with a low charge transfer resistance (R_ct = 285 Ω), confirming superior conductivity. Linear sweep voltammetry (LSV) was employed for CAP detection using CPE-30 wt%/Fe-ZSM-5, which produced a maximum response of 73.65 µA, significantly higher than the unmodified CPE (6.51 µA), GPE (6.39 µA), and GCE (4.43 µA). Comparison of different electrochemical techniques using CPE-30 wt%/Fe-ZSM-5 revealed LSV as the most sensitive (71 µA), outperforming CV (38.91 µA), DPV (10.84 µA), NPV (23.46 µA), and SWV (13.64 µA). Optimization of scan rate and pH yielded maximum responses at 100 mV/s (5.32 µA) and pH 7.0, respectively. The sensor demonstrated high selectivity in the presence of potential interferents at twice the molar concentration of the CAP, with excellent repeatability (3.24% RSD), reproducibility (3.05% RSD), and stability (98.79%). Analytical performance showed a linear dynamic range of 1–1000 µM, a LOD = 1.4 µM, a LOQ = 4.3 µM, and a sensitivity of 1.833 µA/µM·cm². Recovery studies in spiked full-fat milk (88.37–107.71%) demonstrated accurate quantification of CAP, confirming the sensor’s practical applicability for food safety monitoring and antibiotic residue detection.</p> Graphical Abstract <p></p>