The research presents an electrochemical approach for the highly sensitive determination of 2-amino-5-nitrophenol (ANP) based on the use of a modified electrode comprising a composite of boron carbon nitride (BCN), poly β-cyclodextrin (pβCD), and sulfur-doped graphene quantum dots (SGQDs). Each layer of the developed BCN/pβCD/SGQD-modified electrode was characterized using spectroscopic and microscopic techniques, and the composite electrode demonstrated remarkable sensitivity for the voltammetric detection of the analyte under optimized conditions. Chronoamperometric analysis under dynamic conditions showcased the electrode's capability for precise ANP sensing in a flow system. The optimized conditions viz. pH of the electrolyte solution and scan rate were employed for both cyclic voltammetry and square wave voltammetry analysis and revealed a linear correlation between anodic current and ANP concentration. Interference studies confirmed the selectivity of the modified electrode toward ANP, in the presence of structurally similar compounds. In addition, the fabricated electrode was tested for detecting ANP levels in real-world matrices like hair dye and tap water. The excellent performance of the developed electrode, with a detection limit of 6.63 × 10 −8 M, positions it as a promising tool for the electrochemical determination of ANP, offering potential applications in environmental monitoring analysis.