We have successfully prepared a series of magnetically separable "quasi-homogeneous" Pd-Ni nanoalloy catalysts with tunable composition in a one-pot wet chemical route. We have evaluated the catalytic activity of these Pd-Ni alloy catalysts with different compositions through the Miyaura-Suzuki coupling reaction. These palladium/non-noble metal alloy catalysts show better catalytic activity than an equal amount of palladium nanoparticles. Furthermore, these catalysts exhibited excellent I performance in superparamagnetism owing to its great advantage for reducing the usage of noble metal.