A series of multi-walled carbon nanotube (MWCNT)/nickel glycolate polymer core-shell nanostructures have been successfully synthesized in ethylene glycol medium using a solvothermal method, through which a conformal nickel glycolate polymer layer was deposited onto the MWCNTs. Furthermore, the thickness of the nickel glycolate polymer shell can be conveniently varied or controlled by the concentration of the metal salt (Ni(NO(3))(2)center dot 6H(2)O). Cyclic voltammetry study has revealed that these hybrid nanostructures possess significantly enhanced electrocatalytic activity toward the oxidation of glucose for the first time. There is an optimum Ni(NO(3))(2)center dot 6H(2)O concentration at which the nanostructure obtained possesses the maximum electrocatalytic activity. Most importantly, these new MWCNT/nickel glycolate polymer core-shell nanostructures have shown potential applications as nonenzymatic glucose sensors. (C) 2011 Elsevier B.V. All rights reserved.