顶空毛细管气相色谱法测定醋酸氯地孕酮中有机溶剂残留量

Determination of Residual Organic Solvents in Chlormadinone Acetate by Headspace Capillary Gas Chromatography

目的同时测定醋酸氯地孕酮中3种有机溶剂残留量。方法顶空进样程序升湿法,采用氢离子火焰检测器,色谱柱为HP-5毛细管柱(30m×0.32mm,0.25μm)。结果乙醇、氯仿和N,N-二甲基甲酰胺的线性相关系数分别为0.9999,0.9991,0.9997,平均加样回收率分别为101.7%,92.8%,104.6%,RSD分别为2.3%,2.9%,1.8%(n=5)。结论顶空毛细管气相色谱法简便、准确、灵敏、重现性好,适用于醋酸氯地孕酮的有机溶剂残留量测定。

Objective To develop a headspace capillary gas chromatography method for the determination of residual organic solvents in chlormadinone acetate.Methods The samples were injected by headspace sampler while program heating and FID detector were used.The determination was performed on the HP-5 GC column（30 m × 0.32 mm,0.25 μm）.Results The regression coefficients of ethanol,chloroform and DMF were 0.999 9,0.999 1 and 0.999 7,respectively.The recovery rates were 101.7%,92.8% and 104.6% respectively with RSD 2.3%,2.9% and 1.8% accordingly.Conclusion The method is simple,accurate and sensitive with good reproducibility,which can be used for the determination of the residual organic solvents in chlormadinone acetate.