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目的:建立顶空气相色谱法测定替加氟中4种有机溶剂残留量的方法。方法:顶空进样程序升温,色谱柱为HP-IN-NOWAX(30.0 mm×0.32 mm×0.50μm),溶剂为二甲亚砜(DMSO),检测器为FID,载气为氮气。结果:4种有机溶剂完全分离,在所考察的浓度范围内线性关系良好,甲醇、乙醇、三氯甲烷、N,N-二甲基甲酰胺(DMF)的最低检出浓度分别为0.299,0.100,3.060,1.850μg·ml~(-1)。结论:该方法简便灵敏,结果准确可靠,适用于替加氟原料中有机溶剂残留量的检测。
Objective: To establish a method for the determination of four organic solvents residues in tegafur by headspace gas chromatography. Methods: Headspace sample preparation was heated with HP-IN-NOWAX column (30.0 mm × 0.32 mm × 0.50 μm), DMSO as solvent, FID as detector and nitrogen as carrier gas. Results: The four organic solvents were completely separated and the linearity was good within the investigated concentration range. The minimum detectable concentrations of methanol, ethanol, chloroform and N, N-dimethylformamide (DMF) were 0.299 and 0.100, respectively , 3.060,1.850μg · ml ~ (-1). Conclusion: The method is simple and sensitive, accurate and reliable. It is suitable for the determination of residual organic solvents in Tegafur raw materials.