A two-step pretreatment method for the analysis of Fischer-Tropsch cold trap oils by column liquid chromatography was developed. First step was the separation of Fischer-Tropsch cold trap oils into paraffin-olefin fraction and oxygenates fraction by means of column liquid chromatography with silica gel of pore size of 0.15 similar to 0.18 mm as stationary phase and (dimethylsulfoxide ( DMSO) as eluent. Second step was similar to the first one except that the pore diameter of silica gel was smaller pore size of 0.064 - 0.154 mm, and the paraffin-olefin fraction was further separated into paraffins and olefins. Through this pretreatment, the cold trap oils were separated into three different groups, namely, paraffins, olefins and oxygenates. All preparation fractions were resolved in the high resolution capillary column gas chromatography, respectively. Using pure reagents as standards, components of three separated groups were identified by comparing gas chromatography retention time and carbon number rule of samples with corresponding pure reagents. Then components were quantified by correction factor normalization metho(l. On the basis of the above research, the results of 63 components were given, which were above 80% of total. The results will benefit to Fischer-Tropsch synthesis process development.