Abstract: Objective:To establish a gas chromatography(GC)method for determination of methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid in pomalidomide. Methods:A capillary column with 6% cyanpropyl phenyl-94% dimethyl siloxane(or similar polarity)as stationary phase was adopted. The test was performed with FID detector,DMSO solvent,and nitrogen as the carrier gas and direct injection. Results:Each component could be separated well under the chromatographic condition. There were good linear relationship with r=0.9950~0.9999 in the range of 76.28~610.20,126.38~1011.00,127.53~1020.20,10.30~82.40 and 126.5~1012.40 μg·mL^-1 for methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid respectively. The RSDs of the precision and repeatability were not more than 10.0%. The recoveries were 100.9%,97.95%,100.0%,98.79% and 98.90% for methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid respectively(n=9,RSD<10%). The limits of quantitation of methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid were 0.60,0.80,0.80,1.55,2.02 μg.mL^-1 respectively. The limits of detection of methanol,ethanol,ethyl acetate,1,4-Dioxane and acetic acid were 1.51,2.00,2.01,3.87,5.04 μg·mL^-1 respectively. Three batches of samples were tested,the detectable amount of methanol was 0.015%,0.014% and 0.013%,ethanol was 0.145%,0.212% and 0.124%,ethyl acetate,1,4-dioxane and acetic acid were not detected. Conclusion:The method is simple and accurate with high sensitivity and good specificity. It can be applicable to the determination of 6 residual solvents in pomalidomide.