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Rapid bioassay method for plutonium in urine samples are employed to assess the possible internal dose resulting from exposure to plutonium in the event of a radiological and nuclear emergency. In this work, a rapid method for the determination of plutonium isotopes (239Pu and 240Pu) in large volume of urine samples was developed using tandem quadrupole ICP-MS combined with a high-efficiency sample introduction system (APEX-Ω). The mixture gases of NH 3 and He was employed to effectively eliminate the tailing of 238U and the uranium hydride ions (238U1H+and 238U1H 2 +) and significantly improve the measurement sensitivity of plutonium. The method was validated by analyzing urine samples spiked with known amounts of 239Pu and 240Pu ranging from 1 to 60 fg. The detection limits for the method were estimated to be 0.83 fg for 239Pu, 0.14 fg for 240Pu in 1 L of urine. [Display omitted] • Tandem quadrupole ICP-MS was utilized to measure Pu isotopes in large volume of urine samples. • The interference of 238U (0.23 cps) would be much less a concern at 4.0 mL min−1 NH 3 and 3.0 mL min−1 He. • The detection limits of 239Pu (0.83 fg/L) and 240Pu (0.14 fg/L) are suitable for Pu routine analysis of urine. [ABSTRACT FROM AUTHOR]