In this work, a gallium–nickel alloy target with a weight percentage ratio of 7:3 was successfully prepared on Cu substrate in a chloride system at room temperature. A novel organic-solvent-free separation procedure based on two columns for extracting 68Ge from irradiated Ga–Ni alloy target with high radionuclidic purity (99.99 %) was developed. By this separation procedure, the recovery of 68Ge is 95 ± 5 % and the yield of 68Ge via the nuclear reaction natGa(p,xn)68Ge was measured to be 0.27 ± 0.02 MBq/μA h.