Abstract: Simultaneous separation and determination of plutonium and neptunium from the simulated uranium product specimen were developed for the requirement of uranium product quality control in nuclear fuel reprocessing. An argon pressurized anion-exchange evacuated column system was established for separation of plutonium and neptunium from the simulated uranium product specimen. After separation, neptunium and plutonium were measured with a large area grid ionization chamber-alpha spectrometry. The results show that determination of Np, Pu in uranium product with above-mentioned separation and measurement method meet the requirement of uranium product quality control in nuclear fuel reprocessing. The average decontamination factors are 8.6×10⁴， 9.6×10⁴ respectively for the uranium with respect to neptunium and plutonium. The average recoveries of neptunium and plutonium are 78% (n=6) and 86% (n=6) respectively. 