Nickel hexacyanoferrate (NiHCF) and Ni-Al layered double hydroxide (LDH) hybrid film was fabricated on the gold electrode by a two-step electrodeposition method. Varying the strategies of electrodeposition of NiHCF, the hybrid films showed different morphology, composition and electrochemical behavior. As a demonstration, the hybrid film fabricated by using the absorbed Ni2+ on Ni-Al LDH modified gold electrode for the next electrodeposition of NiHCF was used for the electroanalysis of ascorbic acid (AA). The analytical performance of the proposed electrode was investigated by cyclic voltammetry and chronamperometry. The linearity range of AA was from 0.1 to 3.5 mM with a detection limit (S/N =3) of 21 mu M. The developed method was found to be linear, sensitive, selective, precise and accurate. The applicability of the method was confirmed by the satisfactory results in real sample analysis. (C) 2013 Elsevier Ltd. All rights reserved.