Ternary PtRuFe and PtRuMo alloy systems were investigated for methanol electro-oxidation reaction (MOR). Rapid optimization of the ternary alloy compositions was achieved via combinatorial synthesis and high-throughput screening method. A combinatorial library was composed of 121 different compositions of the ternary PtRuFe and PtRuMo alloys. High MOR activities were observed in Pt5Ru3Fe2, Pt4Ru3Fe3, Pt5Ru4Mo1 and Pt4Ru4Mo2 Compositions (mass ratio) via quantitative analysis of each catalyst spots. Performances of these compositions were verified in their powder version catalysts: (1) on-set potential for CO electro-oxidation decreased by 0.05 V in the PtRuFe alloys and 0.15 V in the PtRuMo and (2) high MOR activities were observed in the Pt5Ru4Fe1/C (98% higher mass activity than that of commercial PtRu/C) and the Pt4Ru3Mo3/C (260% higher specific activity than that of commercial PtRu/C). Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.