Abstract: An acylated and silylated derivative of β-cyclodextrin,namely heptakis (2,3-di-O-acetyl-6-O-tert-butyl-dimethysilyl-β-cyclodextrin was synthesized and used as the stationary phase by applying it to the surface of the elastic fused silica capillary column statically.It was shown by the result of testing for its chromatographic characteristics,that the β-cyclodextrin derivative behaved with good film-forming property,relatively high column efficiency,good thermal stability and efficient separation ability toward halogen substituted benzene isomers and some disubstituted benzene isomers.