Abstract: OBJECTIVE To establish a method for determination of residual solvents in azlocillin sodium. METHODS The residual solvents in this substance were determined by GC equipped with FID detector and linked with Agilent HP-1 capillary column (30.0 m×0.25 mm×1.00 mm). The inlet temperature was 200 ℃ and the FID detector temperature was 250 ℃. The column temperature rose by program: the initial temperature was 30 ℃, maintained for 7 min, raise to 180 ℃ with a rate of 50 ℃·min^-1, maintained for 5 min. The carries gas was nitrogen and the flow rate of carries gas was 2.0 mL·min^-1. The heated temperature of the headspace oven was 85 ℃, the heated time lasted 30 min, and the injection volume was 1.0 mL. The dissolved medium used was water and the internal standard was butanone. RESULTS Each solvent could be completely separated in chromatogram obtained from systemic suitability test, and the calibration curves of each solvent had good linear relationship within a certain range. CONCLUSION The method is accurate and reliable. It can be applied in determination of residual solvents in azlocillin sodium.