Abstract: The powder sample of hemostatic microspheres (0.15 g) and 5.00 mL of water were taken into a 20 mL-headspace flask. The headspace flask was then sealed hermetically and the headspace-sampling was carried out at 80℃ for 30 min. DB-5 capillary column was used as the stationary phase, electron capture detector (ECD) was adopted for detection of response signals, and residue of epichlorohydrin was determined by headspace-gas chromatography. As shown by the results, linear relationship between values of peak area and mass concentration of epichlorohydrin was obtained in the range of 0.02-2.0 mg·L^-1, with lower limit of determination (10S/N) of 0.005 mg·L^-1. Test for recovery was made by standard addition method, giving results in the range of 95.3%-101%, with RSDs (n=6) of the determined values less than 7.0%.