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A method for in situ silylation was developed using supercritical carbon dioxide as a reaction medium and was applied to an endcapping of ODS-silica gels as well as a trimethylsilylation of silica gels. The results of the pyridine/phenol test and surface coverage of silica-based packings were improved by the proposed method. It was indicated that supercritical fluid is more effective than organic solvent as the silylation medium.