Abstract: A detection method to determine residual solvents in aceclofenac by the headspace-gas chromatography (HS-GC) has been set up. DB-624 (30 m×0.32 mm, 1.8 μm) was used as the chromatographic column, and a hydrogen flame ionization detector (FID) was used in the experiment. The column temperature was programmed, equilibrium temperature and time of headspace were 80 ℃ and 30 min. The results showed that isobutylene, methanol, methyl acetate and tert-butanol can be efficiently separated, and the detection limits were 0.013, 0.722, 0.300, 0.550 μg/mL respectively. For all solvents, the linear relationship was good (r>0.999), the recoveries (n=9) were in the range of 95%~105% and the RSD was less than 10%. The method is of simple operation, strong specificity and high accuracy, and can be used to detect the residual solvents in aceclofenac.