A hexagonal boron carbon nitride hybrid (h-BCN) is developed by in situ high-temperature solid-state reaction and subsequent chemical reduction with hydrazine. The XRD and TEM results show that the h-BCN features interlayered structures with two characteristic d-spacing of 0.33 and 0.21 nm. The obtained h-BCN exhibits significant electrochemical sensor for dopamine and uric acid. The cyclic voltammetric and amperometric experiments revealed a good linear relationship between current densities and concentrations of dopamine (DA) of 10-300 μM and uric acid (UA) of 10-500 μM, with high sensitivities of 0.14 μA/μM and 0.32 μA/μM and detection limits of 5 μM and 2 μM, respectively.