顶空气相色谱法测定替加氟中残留的有机溶剂

Determination of Residual Organic Solvents in Tegafur by Headspace Gas Chromatography

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 headspace gas chromatography method for determining the residual organic volatile solvents in Tegafur. Method： The samples were injected by a headspace sampler under temperature programmed heating. The determination was performed on an HP-INNOWAX capillary column （30. 0mm×0.32mm×0.50μm） while DMSO was used as solvent media, FID as detector and nitrogen as carrier gas. Result： The four residual organic solvents consisting of methanol, ethanol, chloroform and DMF were completely separated, and the linear relationships were promising. Their minimal detective levels was 0. 299,0. 100,3.060 and 1. 850μg·ml^-1, respectively. Conclusion： The method is simple, sensitive, accurate, and can be used for detection of four residual solvents in Tegafur.