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目的:建立顶空气相色谱法测定咪喹莫特中7种有机溶剂残留量。方法:采用顶空气相色谱法,FID检测器,在毛细管色谱柱HP-PLOT/Q(30m×0.53mm×40μm)上程序升温,载气为氮气,进样口温度250℃,检测器温度270℃。结果:7种有机溶剂完全分离,在所考察的浓度范围内具有良好线性,甲醇、二氯甲烷、正己烷、DMF、THF、三氯甲烷、甲苯的最低检出浓度分别为0.14,0.158,0.0088,0.452,0.0379,0.66,0.0518μg.mL-1。精密度RSD均小于3.0%,平均回收率为90%～114%。结论:经方法学验证,本试验建立的方法简便灵敏,结果准确可靠,适用于咪喹莫特原料药中有机溶剂残留量的检测。
Objective: To establish a method for the determination of seven organic solvents in imiquimod by headspace gas chromatography. Methods: The temperature was programmed on a capillary column HP-PLOT / Q (30m × 0.53mm × 40μm) using headspace gas chromatography and FID detector. The carrier gas was nitrogen and the inlet temperature was 250 ℃. The detector temperature was 270 ℃. Results: Seven kinds of organic solvents were completely separated and had good linearities in the investigated concentration range. The minimum detectable concentrations of methanol, dichloromethane, n-hexane, DMF, THF, chloroform and toluene were 0.14,0.158 and 0.0088 , 0.452, 0.0379, 0.66, 0.0518 μg.mL-1. RSD precision less than 3.0%, the average recovery rate of 90% to 114%. Conclusion: The method established by this method is simple and sensitive, and the results are accurate and reliable. It is suitable for the determination of residual organic solvents in imiquimod raw materials.