Diazepam (DZP), a long‐lasting benzodiazepine and controlled substance, is prevalent on the illegal market, notably as a date rape drug. This study presents a novel electrochemical sensor (CPE/GCPE/MWCNTs) for DZP determination in lab routines. Characterized through LSV, EIS, and SEM, the sensor revealed a pH‐dependent, irreversible reduction process at approximately −0.70 V (vs. Ag/AgCl(sat)). Optimization with SWV and 0.1 mol L−1 B–R solution (pH 1.0) produced a calibration curve spanning 1.49 to 21.5 μmol L−1. LOD and LOQ were 0.33 and 1.10 μmol L−1, respectively. Quantification in spiked samples exhibited no significant differences compared to HPLC‐DAD, endorsing the sensor for monitoring date rape drugs in forensic analysis.