The electrochemical oxidation reaction of glucose was extensively investigated for applications in glucose-oxygen fuel cells 1 and in glucose sensors. 2 The electrocatalytic oxidation of glucose in alkaline medium was studied using Cu, Ni, Fe, Pt, and Au electrodes.3 Among them, gold nanoparticles (Au NPs) have been intensively examined as the most attractive material for the electrocatalysis of glucose owing to their chemical stability, good biocompatibility, high catalytic activity, good antipoisoning property, and more negative oxidation potential compared to the other materials.2b-4 Although the high surface-to-volume ratio and high surface energy of Au NPs increase their catalytic performance, the fast aggregation of Au NPs during the catalytic process led the development of nanoscopic supporting materials to improve their practical applications. Recently, two-dimensional nanosheet of exfoliated layered double hydroxide (LDH) has emerged as a new type of solid support to immobilize the diverse metal NPs 5 because of the large metal hydroxide area, good biochemical stability, and highly charged positive potential of 1-to 2-nm thick LDH layers. LDHs consist of a continuous stack of positively charged metal hydroxide layers with counter anions and water molecules placed in interlayer spaces. The general formula of LDHs is expressed by2+ and M 3+ are divalent and trivalent metal ions, respectively, capable of occupying the octahedral holes of brucite-like layers. 6 The compositional flexibility and tunable layer charge have allowed LDHs to be useful in a wide variety of applications. Recently, sequentially assembled Au NPs/LDH nanosheet layers were used in glucose electrocatalysis, in which the catalyst was prepared by the layer-by-layer of Au NPs and LDH nanosheet.7 In this study, we synthesized a uniform nanocomposite of Au NPs and LDH nanosheet, denoted as Au/LDH nanosheet (inset photo in Figure 1(a)), by in situ chemical reduction with NaBH 4 , efficiently forming the spherical Au NPs in the diameter range of 2-10 nm on the entire surface of LDH nanosheet. The current method does not require additional organic stabilizers to prevent the aggregation of Au NPs and surface modifiers to immobilize the Au NPs on LDH surface. Importantly, the catalytic activity of Au/LDH nanosheet for the electrochemical oxidation reaction of glucose was also investigated. The Au/LDH nanosheet exhibited an excellent electrocatalytic activity, although very small amount of gold was used as an active material. Figure 1 shows the optical properties of the nanocomposite of Au NPs and LDH nanosheet. In general, the Au NPs exhibited a strong visible-light absorption ascribed to the surface plasmon resonance (SPR) effect, which directly corresponds to their size and shape, as well as the distribution on the supports. 8 For example, uniform and spherical Au NPs in aqueous solution exhibit a sharp and single extinction band at in the wavelength range of 520-530 nm, depending on the size. However, the large aggregates or nonspherical sha...