OBJECTIVE: To establish a method for the residual determination of ethanol and acetone in Nimodipine sustained-release tablet. METHODS: Headspace GC was on the column of capillary column with fixative solution of 6% cyanopropyl phenyl-94% dimethyl polysiloxane (DB-624) by temperature programming, injector temperature was 230 ℃, detector was a flame ionization detector, detector temperature was 250 ℃, carrier gas was nitrogen gas, flow rate was 2.0 ml/min, split ratio was 5 ∶ 1, equilibrium temperature was 90 ℃, equilibrium time was 20 min, and volume of sample was 1.0 ml. RESULTS: The linear range was 1.25-500.0 μg/ml for ethanol (r=0.999 9) and 0.50-202.0 μg/ml for acetone (r=0.999 2); limits of quantitative were 5.01, 2.02 μg/ml, limits of detection were 1.67, 0.67 μg/ml, respectively; RSDs of precision, stability and reproducibility tests were lower than 3.0%; recoveries were 96.81%-102.00%(RSD=1.89%,n=9),96.64%-102.31%(RSD=1.82%,n=9), respectively. CONCLUSIONS: The method is simple, rapid, accurate, and can be used for simultaneous residual determination of ethanol and acetone in Nimodipine sustained-release tablet.