Rapid analysis for 90Sr, 232Th, and 238U in human urine samples collected in a radiation emergency can be developed by co-precipitation with calcium phosphate and separation using a Sr-resin (Eichrom Technologies, Inc.) column. The nuclides were measured by inductively coupled plasma mass spectrometry (ICP-MS) or a low background β-counter. Spike tests yielded a good recovery of above 90%. Fractions of 90Sr and the other nuclides (232Th and 238U) were separated in about 2 hours. It was judged that the developed method would be an effective bioassay method in radiation emergency.