A graphitic mesoporous carbon (GMC) had been successfully synthesized using Ni-Fe layered double hydroxide (LDH) as both template and catalyst under a relatively low pyrolysis temperature. The techniques of X-ray diffraction, transmission electron microscopy, Raman spectrum and N-2 adsorption/desorption were used to characterize the physico-chemical properties of the as-prepared GMC. Meanwhile, the voltammetric behaviors of hydroquinone (HQ) and catechol (CC) were studied at the GMC modified glassy carbon electrode (GMC/GCE). The separation of the oxidation and reduction peak (Delta E-p) for HQ and CC were decreased from 369 to 42 mV and from 365 to 52 mV, respectively, and the anodic peak currents for the oxidation of both HQ and CC were also remarkably increased at the GMC/GCE. Furthermore, at the GMC/GCE, the two components could be entirely separated with a large oxidation peak potential separation between HQ and CC. Under the optimized condition, the peak currents of HQ and CC increased linearly with increasing HQ and CC contents. The detection limit for HQ and CC was 3.7 x 10(-7) and 3.1 x 10(-7) mol Li. respectively. (C) 2012 Elsevier B.V. All rights reserved.