顶空毛细管气相色谱法测定醋酸可的松中6种有机溶剂残留量

Determination of Six Residual Organic Solvents in Cortisone Acetate by Headspace Capillary GC

目的:建立顶空毛细管气相色谱法测定醋酸可的松中甲醇、乙醇、乙酸乙酯、三氯甲烷、吡啶和N,N-二甲基甲酰胺的残留量的方法。方法:采用外标法,DB-624毛细管色谱柱(30 m×0.53 mm,3μm),FID检测器,进样口温度为200℃,检测器温度为250℃。柱程序升温:起始温度50℃,保持6 min,再以15℃·min-1的速率升温至200℃,保持6 min。载气为氮气;流速为3.0 ml·min-1。顶空条件:平衡温度105℃,平衡时间为45 min。结果:各组分完全分离,线性关系良好,6种溶剂的平均回收率分别为107.87%(RSD=0.61%)、108.19%(RSD=0.93%)、102.78%(RSD=1.28%)、109.65%(RSD=3.81%)、109.35%(RSD=2.18%)和106.93%(RSD=3.01%)(n=9)。结论:本法简便、准确,可用于醋酸可的松中6种有机溶剂残留量的检测。

Objective：To establish a headspace capillary GC method for the determination of residual organic solvents （methanol,ethanol,ethyl acetate,chloroform,pyridine and N,N-dimethylformamide） in cortisone acetate.Methods：An external standard method was used.The analytical column was a DB-624 capillary column（30 m × 0.53 mm,3 μm） with an FID detector.The injector temperature was 200℃ and the detector temperature was 250℃.The initial temperature was 50℃,kept for 6 min,then raised to 200℃ at a rate of 15℃ · min-1,and kept for another 6 min.Nitrogen was used as the carrier gas.The flow rate was 3.0 ml · min-1.The headspace vials equilibrium temperature was 105℃ and the balance time was 45 min.Results：All the solvents could be completely separated with good linear relationship.The average recovery of the six solvents was 107.87% （RSD =0.61%）,108.19% （RSD =0.93%）,102.78% （RSD =1.28%）,109.65% （RSD =3.81%）,109.35% （RSD =2.18%） and 106.93% （RSD =3.01%） （n =9）,respectively.Conclusion：The method is simple and accurate,and can be used in the determination of residual solvents in cortisone acetate.