Mesoporous nickel cobalt oxide hierarchical structures are successfully synthesized by a controlled calcination of nickel cobalt oxalate hydrate hierarchical structures. More importantly, a mesoporous nickel cobalt oxide hierarchical structures modified electrode shows remarkable electrochemical performance for non-enzymatic glucose detection. The electrode modified with mesoporous Ni_0.3Co_2.7O₄ hierarchical structures shows a low detection limit of 1.0 μM glucose, good sensitivity of 206.5 mA mM⁻¹ cm⁻², and good selectivity.