Abstract: Head space-GC was applied to the determination of 7 organic solvents, including methanol, ethanol, acetone, isopropanol, diethyl ether, pyridine and methylbenzene, in esmolol hydrochloride. The balanced temperature and time of head space were set out at 70 ℃ and 30 min. The analyte were separated on DB-1 125-1032 capillary column and detected by FID. Linear relationships between values of peak area and mass concentration of 7 organic solvents were kept in definite ranges. Detection limits (3S/N) found were ranged from 0.5 to 3.8 mg·L-1. Tests for recovery were performed by addition of mixed standard of 7 organic solvents at 2 concentration levels for 9 parallel determinations, results of recovery found were in the range of 96.2%-102.7% with RSD′s in the range of 0.69%-3.0%.