Abstract: OBJECTIVE To establish a method of GC for the determination of residual solvents in anastrozole, a method of GC/MS for the verification of residual solvents in anastrozole. METHODS DB-624 capillary column through head-space sampling mode was used. The column temperature was maintained at 40 ℃ for 7 min, then was raised to 180 ℃ at the rate of 10 ℃·min^-1 and maintained at 180 ℃ for 4 min. The sample was dissolved in dimethylformamide. RESULTS The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. The residual solvents in anastrozole were confirmed by GC-MS. CONCLUSION The established method is simple and reliable, which can be used for determination of residual solvents in anastrozole.