GC法测定匹多莫德片中有机溶剂的残留量

目的:建立匹多莫德片中乙醇、二氯甲烷、N,N-二甲基甲酰胺3种有机溶剂残留量的分离测定方法。方法:采用气相色谱法,检测器为FID,色谱柱为DB-624毛细管柱,载气为氮气,程序升温为在40℃下保持5min,然后以50℃.min-1的速率升至200℃,至少保持10min,进样口温度为160℃,检测器温度为280℃,分流比为5:1。结果:3种有机溶剂完全分离,样品中潜在杂质不干扰其测定;三者检测浓度的线性范围分别为10.036～802.88(r=0.9999)、26.44～105.76(r=0.9996)、1.76～140.8(r=0.9995)μg.mL-1;平均回收率分别为102.4%、99.0%、99.2%,RSD分别为1.99%、3.34%、0.55%。结论:本方法灵敏、准确、快捷,可用于该制剂中有机溶剂残留量的检测。

Determination of Residual Organic Solvents in Pidotimod Tablets by GC

OBJECTIVE： To establish a method for separation and determination of ethanol, dichloromethane and N, N- dimethylformamide in pidotimod tablets. METHODS： The residual organic solvents were quantitatively determined by GC on DB- 624 capillary column with FID detector, using nitrogen as the carries gas. Temperature programming was carried out in which the column temperature was initially maintained at 40 ℃ for 5 minutes, then increased at a rate of 50 ℃ per minute to 200 ℃, and maintained at 200 ℃ for at least 10 minutes. The temperature at injection mouth was maintained at 160 ℃ ; the detector temperature was maintained at 280 ℃. The split ratio was 5 ： 1. RESULTS： 3 residual organic solvents were completely separated and their determination was free of inference from hidden foreign substances. The linear ranges of the ethanol, dichloromethane and N, N - dimethylformamide were 10. 036- 802.88 （ r = 0. 999 9）, 26.44-105.76 （ r = 0. 999 6）, and 1.76- 140.8 （ r = 0. 999 5） μg ·mL^- 1, respectively, and their average recovery rates were 102.4%, 99.0%, and 99.2%, respectively, with RSD at 1.99%, 3.34%, and 0.55%, respectively. CONCLUSION： The method is sensitive, accurate and rapid, and it is suitable for determination of residual organic solvents in pidotimod tablets.