顶空毛细管气相色谱法测定普卢利沙星中有机残留溶剂

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

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。

Objective ：To establish a method for the determination of acetonitrile, n-hexane, 1, 2-dichlorom ethane, chloroform, toluene, 1, 4-dioxane, and N, N-dimethylformamide （DMF） in synthetic prulixacino 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 sulfoxideo The injection pert and detector temperature were 250℃. Results： Seven residual organic solvents eonsisting of aeetonitrile, n-hexane, 1,2-diehlorom ethane, ehloroform, toluene, 1,4-dioxane, and N,N-dimethylformamide（DMF） in pmlixacin were eompletely separated. There was a good linearity and the eorrelation eoeffieient 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 detemaination of residual orgamoic solvents in pmlixacin.