顶空气相色谱法测定咪喹莫特中有机溶剂残留量  

Headspace GC determination of residual solvents in imiquimod

作　　者：许莉勇[1] 

机构地区：[1]浙江医药高等专科学校,宁波315100

出　　处：《药物分析杂志》2010年第6期1084-1086,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：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 determining the residues of seven kinds of solvents in imiquimod by headspace gas chromatography.Method：The determination was carried out on an HP-PLOT/Q capillary column（30 m×0.53 mm×40 μm）with sequential increasing of temperature programming.The injector temperature was 250 ℃,and the FID detector temperature was 270 ℃.Results：It appears a good linearity in the experimental concentration.The detector limit of methanol,dichloromethane,n-hexane,DMF,THF,trichloromethane and methylbenzene separately were 0.14,0.158,0.0088,0.452,0.0379,0.66,0.0518 μg·mL-1.The RSDs of precision were all less than 3.0%.The average recoveries were 90%-114%.Conclusion：The method is simple,sensitive and accurate.It can be used for detection of seven residual solvents in imiquimod.

关 键 词：咪喹莫特 有机溶剂残留量 顶空气相色谱法 

分 类 号：R917[医药卫生—药物分析学]