OBJECTIVE： To establish a method for the determination of 4 kinds of residual solvents in racemic ketoisoleucine calcium. METHODS： Headspace gas chromatography was performed on the column of DB-624 capillary column by temperature programmed， detector was FID， inlet temperature was 200 ℃， detector temperature was 250 ℃， carrier gas was nitrogen， flow rate was 1.0 ml/min， injection volume was 1 ml by headspace sampling， equilibrium temperature was 70 ℃ and equilibrium time was 30 min. RESULTS： The linear range was 120.04-480.16 μg/ml for methanol （r＝0.997 8）， 200.21-800.83 μg/ml for ethanol （r＝0.998 5）， 204.05-816.19 μg/ml for ethyl acetate （r＝0.999 2）， 28.35-113.39 μg/ml for tetrahydrofuran（r＝0.998 9）； detection limits were 6.002 μg/ml， 50.05 μg/ml， 51.01 μg/ml and 7.087 μg/ml； RSD of precision was lower than 3％； recoveries were 95.0％-105.6％（RSD＝3.95％，n＝9），97.5％-106.4％（RSD＝3.67％，n＝9），98.1％-105.9％（RSD＝3.16％，n＝9） and 88.8％-99.2％ （RSD＝3.79％，n＝9）， respectively； 4 kinds of residual solvents were not detected. CONCLUSIONS： The method is simple， accurate and reliable， and can be used for the determination of residual solvents in racemic ketoisoleucine calcium.