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We demonstrate for the first time an interfacial polymerization method for the synthesis of high-quality polyaniline-modified graphene nanosheets (PANI/GNs), which represents a novel type of graphene/polymer heterostructure. The interfacial polymerization at a liquid-liquid interface allows PANI to grow uniformly on the surface of the GNs. An ultra-high loading of Pt nanoparticles was then controllably deposited on the surface of the PANI/GNs to form a Pt/PANI/GNs hybrid. The obtained composites were characterized by scanning electron microscopy, transmission electron microscopy, energy-dispersive spectrometry, X-ray diffraction, X-ray photoelectron spectroscopy, and thermogravimetric analysis. The Pt/PANI/GNs hybrid shows excellent electrocatalytic activity toward methanol oxidation and oxygen reduction. H(2)O(2) and glucose were used as two representative analytes to demonstrate the sensing performance of a Pt/PANI/GNs-modified electrode. It is found that this sensing element shows high sensitivity and a low detection limit for H(2)O(2) and glucose. The results demonstrate that the Pt/PANI/GNs hybrid may be an attractive and advanced electrode material with potential applications in the construction of electrochemical sensors and biosensors., (Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)