Abstract: OBJECTIVE To establish a headspace GC method for the determination of residual organic solvents-methanol, pentane, ethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate in rocuronium bromide. METHODS The residual organic solvents were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃. The inlet temperature was 150 ℃, and water as the solvent. RESULTS The linear ranges of methanol, pentane, ethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate were respectively 0.06-3.00 (r=0.999 9)，0.01-2.0(r=0.999 9)，0.01-2.0 (r=0.999 8)，0.01-2.0 (r=0.999 9 )，0.008 2-0.410 0 (r=0.999 8)，0.012-0.600(r=0.999 8)，0.01-2.0 (r=0.999 9)，0.01-2.0mg·mL-1 (r=0.999 9). The average recoveries were ranged from 97.1% to 99.6% with RSD ranged from 1.1% to 2.2%. The detection limits were 0.15-6.44 μg·mL-1. The residual levels for the eight organic solvents in 3 batches samples were all up to the standard stipulated in Ch.P(2005). CONCLUSION The method is simple, accurate, sensitive and reproducible. It can be used for the determination of the residual organic solvents in rocuronium bromide.