Hydroquinone (HQ), catechol (CC) and nitrite (NT) are considered aquatic environmental pollutants. They are highly toxic, harm humans’ health, and damage the environment. Thus, in the present work we introduce a simple and efficient electrochemical sensor for determination of HQ, CC, and NT simultaneously in wastewater sample. The sensor is fabricated by modifying the surface of a glassy carbon electrode (GCE) by two successive thin films from poly(3,4-ethylenedioxythiophene) (PEDOT) and a mixture of carbon nanotubes-graphene oxide (CNT-GRO). Under optimized conditions the HQ, CC, and NT are successfully detected simultaneously in wastewater sample with changing their concentrations in the ranges (0.04 → 100 µM), (0.01 → 100 µM) and (0.05 → 120 µM), the detection limits are 8.5 nM, 3.8 nM and 6.1 nM, respectively. Good potential peak separations: 117 mV and 585 mV are obtained between the HQ-CC, and CC-NT. The sensor has an excellent catalytic capability toward the oxidation of HQ, CC, and NT due to good synergism between its composite components: PEDOT, GRO and CNTs. The features of the sensor are large active surface area, good electrical conductivity, perfect storage stability, good reproducibility, anti-interference capability and accepted recovery rate for HQ, CC, and NT determination in wastewater sample.