In this study, we report about the preparation of nickel cobalt telluride nanorods (NiCoTe NRs) by the hydrothermal method using ascorbic acid and cetyltrimethylammonium bromide as reducing agents. The NiCoTe NRs (NCT 1 NRs) were characterized through use of different methods. The nonlinear optical measurements were carried out using Z-scan techniques. The results give the nonlinear absorption that arises from the combined two photon absorption and free carrier absorption. NCT 1 has an excellent electrocatalytic activity toward hydrogen peroxide with a sensitivity of 3464 μA mM –1 cm –2 , a wide linear range of 0.002–1835 μM, and the lower detection limit of 0.02 μM, and the prepared electrode was strong in sensing in vivo H 2 O 2 free from raw 264.7 cells. Therefore, the binary transition metal chalcogenide based nanostructures have promising potential in live cell biosensing applications.