Abstract: 2,6-Di-butyl-β-cyclodextrin was synthesized,and a capillary column for use in gas chromatography was prepared by the sol-gel method with this β-cyclodextrin derivative as the stationary phase.This capillary column was proved to be vary efficient in the separation of isomers of xylene,the polar amines and alcohols,as well as the non-polar alkanes.The chromatographic parameters of this capillary column were measured and the following results were obtained: ① non-symmetric factor: 1;② column efficiency: 2876 plates per meter;③ polarity of stationary phase: 1215 (sum of McReynold′s constants);and ④ repeatability of retention time: RSD (n=10) less than 0.3%.All these data were favourable for this capillary column to be used in chromatographic separations.