The present research was conducted to develop a potent electrochemical sensor based on multi-walled carbon nanotubes and TiO 2 nanoparticles in chitosan matrix (CS-MWCNTs+TiO 2 NPs). In the CS-MWCNTs+TiO 2 NPs nanocomposite film with excellent catalytic activities, good electrical conductivities and high surface areas of MWCNTs and TiO 2 NPs, the simultaneous determination of hydroquinone (HQ), catechol (CC) and resorcinol (RS) with proper analytical performance was realized in the individual or triple-components solution in comparison with the bare glassy carbon electrode (GCE) and the single component modified GCE. The linear response of HQ, CC and RS were obtained in the ranges of 0.4-276.0 μmol dm −3 , 0.4-159.0 μmol dm −3 and 3.0-657 μmol dm −3 and the detection limits (S/N = 3) were 0.06 μmol dm −3 , 0.07 μmol dm −3 , and 0.52 μmol dm −3 , respectively. In the real water sample analysis by the developed sensor, satisfactory results were obtained.