A gas chromatographic micro-packed column prepared with titanium dioxide (TiO2) particles was developed. This study reports the fundamental retention behavior of the column for several organic and inorganic gaseous compounds, and quantitatively analyzes the high-temperature degradation behavior of the injected organic compounds. The anatase TiO2 particles were prepared by hydrolysis of titanium (IV) isopropoxide. The particle size was classified as 150 – 180 μm. The micro-packed column was prepared by packing the classified TiO2 particles into a stainless steel capillary of inner diameter of 1.0 mm and length of 1.0 m. The TiO2 micro-packed column was connected to a conventional gas chromatograph equipped with a flame ionization detector or a thermal conductivity detector. The column showed high retentivity for carbon dioxide and also for organic compounds, achieving a baseline separation of methane and ethane. The TiO2 packed column was highly thermally stable, with a temperature limit above 400°C. Above 300°C, the analytes injected into the column were thermally degraded by catalytic combustion of TiO2 under N2 carrier gas. On the other hand, the degradation was obtained above 200°C using air as the carrier gas.