High activity, excellent durability and low cost are three key issues in development of advanced fuel cell catalysts. In this context, alloy and intermetallic Pt-based nanoparticles are attractive candidates as their electronic structures and surface atom arrangements can be finely tuned. Herein, we present the synthesis and electrochemical property of alloyed PtAg and intermetallic PtPb nanostructures. PtAg alloyed nanoparticles with compositions in their miscibility gap were obtained through simultaneous reduction of Pt acetylacetonate (Pt(acac)2) and Ag stearate by 1,2-hexadecanediol (HDD) at elevated temperatures using long carbon chain amines and acids as capping reagents. PtPb nanorods were made from Pt(acac)2 and lead acetylacetonate (Pb(acac)2) using tert-butylaminborane (TBAB) complex as the reducants. The electrochemical properties of these nanoparticles were characterized. Both PtAg and PtPb systems showed enhanced electrocatalytic performance in fuel oxidation reaction of small molecules.