Abstract: OBJECTIVE To establish a method for the determination of residual organic solvents in nelarabine by gas chromatography. METHODS Chromatographic column was capillary column SE-54(30 m×0.53 mm, 1.0 μm), with FID detector and nitrogen as carrier gas, the flow rate was 40 mL·min^-1. Injector temperature was 200 ℃ and the detector temperature was 250℃, the split ratio was 50∶1, column temperature was programmed and initial temperature was 40 ℃, maintained for 5 min, raised to 200 ℃ with a rate of 50 ℃·min^-1, maintained for 5 min. The external standard method was used for quantitative analysis. Analytical conditions were studied. RESULTS The standard curves were linear in the range of 14.93-746.4 ng(r=0.999 4) for methanol, 1.950-97.45 ng(r=0.999 8) for acetonitrile, 2.980-149.0 ng(r=0.999 6) for methylene chloride and 25.12-1 256 ng(r=0.999 8) for ethyl acetate. The average recoveries (n=9) were 100.6%(RSD=1.87%), 101.0%(RSD=2.27%), 99.7%(RSD=3.41%), 100.4%(RSD=1.52%). CONCLUSION The method is rapid, accurate, sensitive, reproducible and can be used for detecting residual organic solvents in nelarabine.