OBJECTIVE： To establish a method for the residual simultaneous determination of methanol， alcohol， dichloromethane， n-hexane， tetrahydrofuran and benzene in tosufloxacin tosylat. METHODS： Headspace GC was performed on the capillary column with 6％ cyanopropylphenyl-94％ dimethylpolysiloxane （DB-624） as fixative lipid， temperature programmed， the inlet temperature was 180 ℃， detector was flame ionization detector with temperature of 300 ℃， carrier gas was high purity N2 at a flow rate of 1.5 mL/min， split ratio was 10 ∶ 1， headspace equilibrium temperature was 100 ℃， equilibrium time was 40 min， headspace sample volume was 10 mL， and the headspace sample volume was 1 mL. RESULTS： The linear range was 178.3-1 782.7 μg/mL for methanol （r＝0.999 1），301.2-3 012.1 μg/mL for alcohol（r＝0.999 7），33.81-338.10 μg/mL for dichloromethane（r＝0.999 3），18.02-180.22 μg/mL for n-hexane （r＝0.999 1）， 43.26-432.58 μg/mL for tetrahydrofuran （r＝0.999 1） and 0.126 8-1.268 1 μg/mL for benzene （r＝0.999 1）； limits of quantification were 0.31， 3.00， 0.67， 0.02， 0.005， 0.10 μg/mL， limits of detection were 0.15， 1.51， 0.22， 0.01， 0.001， 0.05 μg/mL； RSD of precision test was no higher than 3.1％； RSDs of methanol and n-hexane in stability and reproducibility tests were no higher than 5％； recoveries were 93.72％-102.20％（RSD＝3.1％，n＝9）， 90.10％-101.79％ （RSD＝4.0％，n＝9），97.07％-103.11％（RSD＝2.0％，n＝9），92.38％-103.83％（RSD＝3.9％，n＝9），95.44％-103.62％（RSD＝2.8％，n＝9），and 94.00％-104.73％（RSD＝4.1％，n＝9）. CONCLUSIONS： The method is rapid，sensitive，accurate，and suitable for the residual determination of methanol， alcohol， dichloromethane， n-hexane， tetrahydrofuran and benzene in tosufloxacin tosylat.