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Rapid and simple method for serum and urine iodine is necessary for iodine-related diseases. This study aimed to establish and validate a simple and rapid method for quantification of iodine in human urine and serum using inductively coupled plasma mass spectrometry (ICP-MS). Generally, samples were diluted using water with 1.5% isopropanol and 7 mmol hydrous ammonium before analysis by the ICP-MS. Performance of the method was validated, and the urine and serum iodine levels of 72 pregnant women were analyzed. Results showed that the lower limit of detection of the ICP-MS method was 0.87 µg/L. No significant memory effects were observed. Recovery in both serum and urine was approximately 100%. Compared with NIST SRM3668, bias was <1%, exhibiting good accuracy. The inter-run coefficients of variation (CVs) for serum and urine iodine were 2.8-3.5% and 3.5-6.7%, respectively, and total CVs for serum and urine iodine were 3.2-3.7% and 3.9-6.7%, respectively. Comparison of the iodine results obtained by the ICP-MS method and the conventional S-K method revealed excellent correlation (r = 0.984, mean bias = -1.7%). The median urine iodine of pregnant women (125.5 μg/L) was lower than that of WHO criteria for iodine deficiency (median urinary iodine <150 μg/L) while 55.6% of the individuals with urine iodine level less than 150 μg/L. The median serum iodine level of the pregnant women was 69.0 μg/L. In conclusion, a rapid and simple ICP-MS method for urine and serum iodine measurements has been established and validated, and the pregnant women in Beijing may still suffer from insufficient iodine intake. Abbreviations CV coefficients of variation HPLC high-performance liquid chromatography ICP-MS inductively coupled plasma mass spectrometry KED kinetic energy discrimination KI potassium iodide LOD limit of detection S-K Sandell-Kolthoff reaction PUMCH Peking Union Medical College Hospital.