顶空毛细管气相色谱法测定普卢利沙星中有机残留溶剂

目的:建立合成普卢利沙星工艺中乙腈、正己烷、1,2-二氯乙烷、氯仿、甲苯、1,4-二氧六环、N,N-二甲基甲酰胺(DMF)7种有机残留溶剂的测定方法。方法:采用顶空毛细管气相色谱法,程序升温,HP-5(30m×0.53mm×0.88μm)毛细管柱,氢火焰离子化检测器(FID),以二甲亚砜为溶剂进行测定。进样口温度250℃,检测器温度250℃。结果:乙腈、正己烷、1,2-二氯乙烷、氯仿、甲苯、1,4-二氧六环、DMF 7种有机残留溶剂均达到完全分离。在所考察的浓度范围内呈良好线性,各成分线性回归方程相关系数均在0.999以上。结论:经方法学验证,该方法准确可靠和灵敏,适用于普卢利沙星中有机残留溶剂测定。

Determination of residual organic solvents in prulixacin by headspace capillary gas chromatography

Objective :To establish a method for the determination of acetonitrile,n-hexane,1,2-dichlorom ethane,chloroform,toluene,1,4-dioxane,and N,Ndimethylformamide(DMF) in synthetic prulixacin.Methods: Using headspace capillary gas chromatography with HP-5(30m×0.53mm×0.88μm),FID detector and programablly increased temperature to determine the samples dissolved in dimethyl sulfoxide.The injection port and detector temperature were 250℃.Results: Seven residual organic solvents consisting of acetonitrile,n-hexane,1,2-dichlorom ethane,chloroform,toluene,1,4-dioxane,and N,N-dimethylformamide(DMF) in prulixacin were completely separated.There was a good linearity and the correlation coefficient was higher than 0.999.Conclusion : The method was proved to be accurate,reliable and sensitive,and can be used as a method of the determination of residual organic solvents in prulixacin.