Herein, we designed a new electrochemical sensor based on a carbon paste electrode modified with poly oxometalates@carbon spheres-multiwalled carbon nanotubes and β-cyclodextrin composite (H3PW12O40@CSMWCNTs-βCD/CPE) for the simultaneous determination of phenolic compounds. The CSs were synthesized from glucose using a hydrothermal carbonization (HTC) process. The prepared CS were then modified with H3PW12O40. Following characterization studies of the synthesized compounds using various electron microscopy and spectroscopic methods, an electrochemical sensor was developed based on a CPE modified with the H3PW12O40@CS-MWCNTs-βCD composite. This electrochemical sensor was employed for the detection and determination of phenolic compounds, such as 2-aminophenol (2-AP) and 4-chlorophenol (4-CP), in aqueous media. The obtained results demonstrated the facilitated electron and mass transfer of 2-AP and 4-CP, attributed to the high conductivity and porous structure of the H3PW12O40@CS-MWCNTs-βCD modifier. Consequently, the differential pulse voltammetry displayed a wide two-step linear dynamic range (LDR), (0.005–0.100 µM and 5–100 µM), with limits of detection (LODs) ranging from 0.0014 to 0.0015 µM under optimal condition. The prepared electrochemical sensor boasts numerous advantages, including excellent electrocatalytic performance, low LOD, wide LDR, and high reproducibility for the simultaneous detection of 2-AP and 4-CP in aqueous media. Furthermore, the constructed electrochemical sensor exhibited good recovery results (97 %–112 %, RSD ≤ 6 %) for 2-AP and 4-CP in real samples.
