OBJECTIVE: To establish a method for simultaneous residual determination of dichloromethane and ethyl acetate in bisacodyl raw material. METHODS: Head-space GC was performed on the capillary column of 6% cyanopropyl phenyl-94% dimethyl polysiloxane (DB-624) by temperature programming, the temperature of injector was 220 ℃, detector was flame ionization detector with temperature of 250 ℃, carrier gas was high purity nitrogen with the flow rate of 3.0 ml/min, split ration was 1 ∶ 10, headspace heating temperature was 70 ℃, equilibration time was 30 min, volume of headspace vial was 5 ml, and the injection volume was 1 ml. RESULTS: The linear range was 6-120 μg/ml for dichloromethane (r=0.999 9) and 50-1 000 μg/ml for ethyl acetate (r=0.999 9); the limit of quantitation was 0.2, 1.7 μg, limit of detection was 0.06, 0.5 μg; RSDs of precision, stability and reproducibility tests were no higher than 3%; recoveries were 100.30%-102.00% (RSD=0.63%,n=9) and 100.10 %-101.30% (RSD=0.44%,n=9). CONCLUSIONS: The method is simple and accurate, and can be used for the simultaneous residual determination of dichloromethane and ethyl acetate in bisacodyl raw material.