Determination of the residual orgamic solvents in Nalmefene Hydrochloride by headspace GC / 中国生化药物杂志

ABSTRACT

Objective To develop a headspace GC method for simultaneously determining the residual organic solvents Ethanol, Diethyl ether, Acetone, Dichloromethane, Ethyl acetate, and Tetrahydrofuran in Nalmefene Hydrochloride. Methods Samples dissolved in DMF and six organic residual organic solvents were separated on a DB 624 capillary column (30.0 m×0.32 mm,1.8μm) with a FID detector. The inlet temperature was 220℃and the FID detector temperature was 250℃. The column temperature rose by programthe initial temperature was 35℃, maintained for 8 min, raise to 180cwith a rate of 30℃/min, maintained for 5 min. The heated temperature of the headspace oven was 80℃, the heated time lasted 30 min, and the injection volume was 1.0 mL. Results Six residual orgamic solvents, including Ethanol, Diethyl ether, Acetone, Dichloromethane, Ethyl acetate, and Tetrahydrofuran in Nalmefene Hydrochloride were completely separated. It was appeared to present a good linearity within the experimental concentration. The limit of detection for Ethanol, Diethyl ether, Acetone, ichloromethane, Ethyl acetate, and Tetrahydrofuran were 0.25,0.076,0.15,0.55,0.26 and 0.30μg?mL-1.The method has a good average recovery. Conclusion The method is proved to be accurate and sensitive after validation. It is suitable to determine the residual orgamic solvents in Nalmefene Hydrochloride .