A simple and sensitive method has been developed for the determination of azide ion (N 3 -) in biological fluids and beverages. The procedure was based on the formation of a ternary complex Cu(N 3 ) 2 (4-methylpyridine) x in benzene, followed by its detection by electron paramagnetic resonance. The complex in benzene showed a characteristic four-peak hyperfine structure with a g-value of 2.115 at room temperature.Cu 2+ reacted with N 3 most strongly among common metals found in biological fluids.Several anions and metal ions in biological fluids did not interfere with the determination of N 3 in the presence of large amounts of Cu 2+ and oxidants. In the present method, N 3 at the concentration from 5 μM to 2 mM in 100 μl solution could be determined with the detection limit of 20 ng. The recoveries were more than 95 % for N 3 added to 100 μl of blood, urine, milk and beverages at 200 μM. Our method is recommendable because it takes less than 10 min to determine N 3 and the produced complex is quite stable.*Corresponding author. Tel/