We studied electrochemical responses and morphologies of metal nanoparticles (MNPs) which were prepared by using pulsed laser deposition (PLD) method. Pt and NiO were deposited on a silicon (Si) and a grassy carbon (GC) substrate. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) images did not determine their nanoparticles. Auger Electron Spectroscopy (AES) and X ray Photoelectron Spectroscopy (XPS) for Pt and NiO coated Si substrates showed that MNPs were certainly formed. Pt with the deposition time of 60 sec had highest activity to detect hydrogen peroxide in phosphate buffer solution. NiO with the deposition time of 90 sec showed highest activity to detect glucose in sodium hydroxide solution. These characteristics might be caused by catalytic activity of MNPs.