In this study, we developed a separation method to extract iron from steel solutions using a solid phase extraction resin to determine the composition of trace elements in high-purity steel, with the aid of inductively coupled plasma mass spectrometry (ICP-MS). The acidic solution of steel was passed through the resin and amounts of the trace elements were determined by analyzing the eluate. To obtain optimum analytical conditions, maximum amount of iron was extracted into the resin and the effects of the acid species used to decompose the steel, and their concentrations were examined. Methods to reuse the resin were also investigated. Under optimal conditions, the quantities of many elements such as Mn, Ni, Cr, Cu, Co, Al, As, Bi, Mg, Ce, La, Se, Pb, Sb, Te, Zn, and Cd were determined. However, some elements such as Mo, Sn, and W, which were dissolved as oxyacid anions, were extracted into the resin, in addition to iron. The estimated amounts of trace elements in reference materials of high-purity steel were found to be in good agreement (in the order of mu g/g) with the certified values.