A method was established for determination of 5 solvents residues in ibutilide fumarate active pharmaceutical ingredient (API) by headspace-gas chromatog.The sample was dissolved in N,N-dimethylformamide (DMF) and separated on DB-624 capillary column, with initial column temperature of 40°C.The flame ionization detector was used for detection.The results showed that 5 solvents including dichloromethane, THF, Et acetate, ethanol and acetone, could be completely separated, and linear relationships of 5 solvents were found in definite ranges.The detection limits (3S/N) were 0.74, 0.042, 0.056, 0.17, 0.050 mg·L-1 resp.Tests for recovery were made by standard addition method, giving results in the range of 102%-105%, and RSDs (n=5) of the determined values all less than 2.0%.