Abstract: A headspace gas chromatography-mass spectrometric(HS/GC-MS) method was developed for the determination of organic solvent residues in acetate fiber filter rod. The target compounds were separated using the headspace gas chromatography and detected by the mass spectrometry in the selected ion monitoring mode. The results showed that the calibration curves were linear and correlation coefficients were higher than 0.998 0, the limits of detection ranged from 0.010 4 to 0.157 8 mg/kg, the average recoveries ranged from 90.3% to 102.2% of 9 organic solvent residues with relative deviations lower than 10%. The method is efficient, rapid, simple and is suitable for the determination of organic solvent residues in acetate fiber filter rod.