Abstract: A conventional gas chromatography method has been developed for the measurement of the residual acetonitrile, ethanol and acetone in 2-Deoxy-2-18F fluoro -D- glucose 18F-FDG, the most popular positron emitting radiopharmaceutical. The three solvents were separated on Dex-CB column with FID detetor, and the temperature of column, detector and oven was 60℃,150℃ and 150℃, respectively. Under the condition, the residual solvents of acetonitrile,ethanol and acetone could be separated effectively, excellent linearity was obtained over the range of 0.10 mg/mL to 4.00 mg/m L, the R2 of standard curve was 0.997, 0.9949, 0.9909 respectively. The amounts of the three solvents in our 18F-FDG products have been found well below the maximum permissible levels. The method is very amenable to quality control testing for the radiopharmaceutical.