顶空气相色谱法测定咪喹莫特中残留溶剂二甲基甲酰胺

Determination of Residual Solvent DMF in Imiquimod by HS-GC

目的:建立咪喹莫特中残留溶剂二甲基甲酰胺(DMF)检测的新方法。方法:采用顶空气相色谱法,Agilent HPPLOT/Q毛细管柱(30 m×0.530 mm,40.0μm),氢火焰离子化检测器(FID),载气为氮气,进样口温度为250℃,检测器温度为270℃,程序升温进行测定。结果:残留溶剂二甲基甲酰胺与其它残留溶剂的分离度符合要求,在所考察的浓度范围内线性关系良好,平均回收率分别为94.6%,RSD为4.0%(n=9)。定量限和检测限分别为4.809,0.963μg·ml-1。结论:该顶空气相色谱法简便﹑准确﹑灵敏度高﹑可以用于咪喹莫特中二甲基甲酰胺残留量的测定。

Objective： To establish a new method for determining residual organic solvent DMF in imiquimod. Methods： The samples were injected into an Agilent HP-PLOT /Q capillary column（ 30 m × 0. 530 mm,40. 0 μm） by a headspace sampler and analyzed with an FID detector,the carrier gas was nitrogen,the inlet temperature was 250℃,and the detector temperature was 270℃.The column temperature was programmed raised. Results： The resolution among the peaks of DMF and the other residual solvents could meet the requirements. There was a good linearity within the experimental concentration range. The average recovery was 94. 6%（ RSD =4.0%,n =9）. The limit of quantification and the limit of detection was 4.809μg·ml- 1and 0. 963 μg·ml- 1,respectively.Conclusion： The method is convenient,accurate and sensitive,which can be used in the determination of residual solvent DMF in imiquimod.