Objective To establish a headspace gas chromatography method for two residual solvents determination in sodium morrhuate injection. Methods The residual solvents in sodium morrhuate injection were separated on DB-624 column(30 m×0.32 mm,0.18 μm)with an FID detector. Nitrogen was used as the carrier gas. The flow rate was 2.0 mL·min-1. The injector temperature and the detector temperature was set at 200 ℃ and 250 ℃, respectively. The containers of headspace injector were in equilibrium for 20 min at 80 ℃. Results The peaks of ethanol and diethyl ether could be effectively separated. Good linear relationship of ethanol and ether was obtained within the range of 20.08-1004 and 0.999-999.2 μg·mL-1(r≥0.999 7), respectively; The average recoveries (n=9) were 100.0% and 100.0%, respectively, and RSDs were 0.7% and 0.8%, respectively. Conclusion The method is simple, sensitive, accurate and reliable, and has good repeatability, and is suitable for analysis and detection of residual solvents in sodium morrhuate injection.