顶空气相色谱法测定咪喹莫特中有机溶剂残留量

Determination of Residual Solvents in Imiquimod by Headspace Gas Chromatography

目的建立顶空气相色谱法测定咪喹莫特中9种有机溶剂残留量的方法。方法采用顶空气相色谱法,FID检测器,在毛细管色谱柱HP-INNOWAX（30 m×0.32 mm,0.25μm）上程序升温,载气为氮气,进样口温度250℃,检测器温度270℃。结果9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,正己烷、丙酮、四氢叶酸（THF）、醋酸乙酯、甲醇、二氯甲烷、乙醇、甲苯、二氢叶酸（DMF）的最低检出浓度分别为0.0077,0.0510,0.0373,0.263 3,0.1465,0.3145,0.2591,0.0463,0.4521μg·mL^-1。精密度RSD均〈3.0%,平均回收率90%-115%。结论经方法学验证,该方法简便灵敏,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 nine kinds of organic solvents in imiquimod by headspace gas chromatography. Methods Chromatography analysis was carried out in a HP-INNOWAX capillary column （30 m×0.32 mm,0.25μm） with sequential increase of temperature programming. The injector temperature was 250℃, and the FID detector temperature was 270℃. Results Nine kinds of solvents were separated completely. It appears a good linearity in the experimental concentration. The minimal detective levels of n-hexane, acetone, THF, ethyl acetate, methanol, dichloromethane,ethanol, methylbenzene and DMF separately were 0.007 7, 0. 051 0, 0. 037 3, 0. 263 3, 0. 146 5, 0. 314 5, 0. 259 1, 0. 046 3 and 0. 4521μg·mL^-1. The RSD of precision were all less than 3.0%. The average recovery rates were 90%-115%. Conclusion The method is simple with high sensitivity and accurateness. Gas chromatography could be an appropriate technique to detect residual solvents in imiquimod.