顶空气相色谱法测定盐酸纳美芬的残留溶剂

Determination of the residual orgamic solvents in Nalmefene Hydrochloride by headspace GC

目的测定盐酸纳美芬原料药中的乙醇、乙醚、丙酮、二氯甲烷、乙酸乙酯和四氢呋喃的残留量。方法采用顶空气相色谱程序升温法,以DMF为溶剂,用DB 624毛细管柱(30.0m×0.32mm,1.8μm)和FID检测器;进样口温度220℃;检测器温度250℃;柱温:采用程序升温,35℃保持8min,再以30℃的速率升温至180℃保持5min;顶空进样,顶空平衡温度为80℃,平衡30min,进样体积1mL。结果原料药中6种溶剂均达到了完全分离,在考察的浓度范围内线性关系良好,最低检测浓度分别为0.25、0.076、0.15、0.55、0.26、0.30μg/mL,平均回收率良好。结论所用方法灵敏度、准确度均达到有机残留溶剂的检测要求,可用于盐酸纳美芬原料药中6种残留溶剂的同时检测与分析。

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 program:the 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 .