For characterization of corrosion resistance of metallic biomaterials, determination of trace amounts of metallic ions released from the materials in using static immersion into simulated body fluids (SBF) were investigated. In using a H₂SO₄-fume pre-treatment method, sensitive, precise and accurate determination of the trace metallic elements in SBFs could be performed by ICP-OES. For accurate analysis, it was necessary to employ a matrix-matched solution for the calibration. Moreover, usage of a PFA vessel in the static immersion test was recommended for the prevention of contamination. Thus, it was possible to determine μg dm⁻³ (ppb) order of elements in SBFs and evaluate nano-gram order of the released metallic ions.