The invention relates to a preparation method of a Sb2O5 adsorbent containing doped metal ions. The method comprises the steps of combining H2O2 oxidation and ultraviolet irradiation in a non-aqueous system which takes alcohol as a solvent to promote Sb (III) to be oxidized into Sb (V); further utilizing a small amount of water introduced by an H2O2 solution as a reactant to realize hydrolysis for the Sb (V) and metal ion Mn<+> (Si<4+> or Ti<4+>) and form metal ion partial substitution type Sb2O5; preparing a metal ion Si-doped Si/ Sb2O5 adsorbent with a cubic pyrochlore structure and forming metal ion Ti-doped Ti/ Sb2O5 adsorbent with a continuous solid solution structure within different Ti/ Sb proportional ranges. The prepared adsorbent material can be used for effectively removing radioactive isotope Sr ions and complexes of the radioactive isotope Sr ions as well as stable isotope Sr ions and complexes of the stable isotope Sr ions.