顶空毛细管气相色谱法测定头孢克肟颗粒中乙醇残留量

Determination of Ethanol Residue in Cefixime Granules by Head-space Capillary GC

目的:建立顶空毛细管气相色谱法测定头孢克肟颗粒剂中的乙醇残留量分析方法。方法:采用顶空进样气相色谱法,以丙酮为内标,键合聚乙二醇(HP-INNOWAX)石英毛细管色谱柱;柱升温程序:50℃(保持6 min),以40℃·min^(-1)的速率升至150℃(保持5 min);进样口温度200℃;检测口(FID)温度250℃;氮气为载气,流速:1.0 ml·min^(-1);分流进样,分流比1.0:1;顶空温度85℃,平衡时间30 min,进样时间1 min。结果:乙醇在0.02～1.00 mg·nl^(-1)浓度范围内线性关系良好,r=0.999 7,最低检测限为0.1μg·ml^(-1)。加样回收率为86.8%,RSD=1.96%。结论:本法简便、快速、结果准确,适用于头孢克肟颗粒剂中乙醇残留量检测。

Objective：To establish a head-space capillary GC method for the determination of ethanol residue in cefixime granules. Method：A GC instrument coupled with head-space sampler was used.The separation was carried on an HP-INNOWAX capillary column with the oven temperature raised from 50℃（6 min） to 150℃（5 min） at the rate of 40℃· min^-1.The temperature of the injection inlet was 200℃and that of FID was 250T.The carried gas was nitrogen at a flow rate of 1.0 ml · min ^-1.The split ratio was 1.0：1.The headspace vials were balanced at 85℃for 30 min,and the injection time was 1 min.Result：The linear range of ethanol was 0.02-1.00 mg· ml^-1（r = 0.999 7）.The average recovery was 86.8%with RSD of 1.96%.The minimum detection concentration was 0.1μg· ml^-1.Conclusion：The developed method is convenient,reproducible and accurate in the residual solvent analysis of cefixime granules.