OBJECTIVE: To establish a method for the determination of ethanol, acetonitrile, dichloromethane, ethyl acetate, pyridine in vidarabine monophosphate. METHODS: Headspace GC was performed on the column of Agilent DB-624, programmed temperature, inlet temperature was 200 ℃, the detector was flame ionization detector, detecting temperature was 250 ℃, nitrogen was carrier gas, flow rate was 3 ml/min, split ratio was 1 ∶ 1, the top bottles equilibrium temperature was 100 ℃, and equilibrium time was 45 min, injection volume was 1 ml. external standard was used for quantitative analysis. RESULTS: The peaks of five residual solvents could be completely separated from the other peaks respectively,The linear rang was 24.7-296.3 μg/ml for ethanol(r=0.999 6)、1.9-23.2 μg/ml for acetonitrile(r=0.999 0), 2.8-33.6 μg/ml for dichloromethane(r=0.998 0), 24.7-295.9 μg/ml for ethyl acetate(r=0.999 5), 1.0-11.9 μg/ml for pyridine(r=0.998 6); RSDs of precision and reproducibility tests were lower than 4.35%;recoveries were 102.4%(RSD=2.0%,n=9)、102.1%(RSD=3.4%,n=9)、105.5%(RSD=4.8%,n=9)、100.3%(RSD=4.8%,n=9)、98.3%(RSD=4.0%,n=9). The minimum quantifation limit was 0.304 4-0.988 0 μg/ml and the minimum detection limit was 0.101 5-0.329 3 μg/ml. CONCLUSIONS: The method is simple, accurate and reproducible, and can be used for the determination of residual solvents in vidarabine monophosphate.