Composite nanostructures based on few-layers graphene with encased gold or silver nanoparticles (denoted as Gr-Au and Gr-Ag, respectively) were separately prepared in a single-step synthesis by radio frequency catalytic chemical vapor deposition (RF-cCVD) over Au-x/MgO and Ag-x/MgO catalytic system (where x = 3 wt.%), respectively. Their morphological properties were investigated by electron microscopy techniques (TEM/HRTEM), which demonstrated that the number of graphitic layers within the sheet varied between 2 and 7. Thorough TEM analysis also indicated that gold nanoparticles had a mean size of 22 nm, while silver nanoparticles were found to be larger with a mean size of 35 nm. X-ray powder diffraction proved that the crystallinity of the Gr-Au or Gr-Ag samples is less influenced by the type of metallic nanoparticles (silver or gold) encased between the graphitic layers. The mean value of the crystalline domain perpendicular to graphene (0 0 2) crystallographic plane was determined to be approximately 2.25 nm (for Gr-Au sample) and 2.14 nm (for Gr-Ag sample), both corresponding to 6 graphitic layers. Gr-Ag and Gr-Au nanostructures were used to modify platinum substrates and subsequently employed for the electrochemical analysis of carbamazepine. A significant decrease in the electrochemical oxidation potential of carbamazepine (150 mV) was obtained with both modified electrodes. The detection limit (DL) was found to be 2.75 x 10(-5) M and 2.92 x 10(-5) M for the Pt/Gr-Ag and Pt/Gr-Au electrode, respectively. (C) 2012 Elsevier Ltd. All rights reserved.