In this study, a method of determining zinc isotopes (64Zn, 66Zn, 67Zn, 68Zn, 70Zn) in biochemical samples by ICPMS inductive plasma mass spectrometry method is mentioned in this study. Analytical samples were treated with a microwave wet inorganic technique for serum samples, urine samples were centrifuged and then using ion-exchange chromatography were cleaned and removed influences. before analysis. Factors affecting zinc isotope analysis were investigated, Plasma high-frequency power 1400W, ion lens potential 9V for 5 individual isotopes, carrier gas flow for 2 isotopes 66Zn and 68Zn is 0, 0. 6L/min and 64Zn, 67Zn and 70Zn are 0.9L/min. Analytical procedures were applied to identify 5 zinc isotopes 64Zn, 66Zn, 67Zn, 68Zn, 70Zn in the serum and urine samples. The results showed that the 70Zn isotope has a low percentage in nature. Relative error meets the requirement of trace analysis.