The objective of this paper is to develop a gas chromatog. method and determine the contents of residual organic solvents-methanol, ethanol and toluene in aniracetam. Using a HP-INNOWAX capillary column and FID detector, N, N-dimethylformamide was used as the solvent. The oven temperature was set at 75° and maintained for 3 min, and the temperature was programmatically increased to 150° at the rate of 15° per min and maintained for 5 min. The temperature of injection port and the detector was set at 200°. The linear range of methanol, ethanol and toluene were 6.02-240.8 mg/L, 12.07-251.5 mg/L and 3.56-89.0 mg/L, resp., and the recovery rates were 95.1% (RSD = 2.9%), 100.6% (RSD = 2.2%), and 99.6% (RSD = 1.1%), resp. The detection limits of methanol, ethanol and toluene were 1.97, 1.63, and 0.59 mg/L, resp. This method can be used to determine the residue level of methanol, ethanol, and toluene in aniracetam.