Abstract: A method for determination of oxygenates and benzene in gasoline was established using two-column switching-back flushing two-dimensional gas chromatography technique. By optimizing the hromatographic valve switching time and chromatographic conditions, the analyses were cut from precolumn to separation column. The results show that the detection range of oxide and benzene is 0.10%-20.00% and 0.05%-2.50% respectively, recovery rate is 96.4%-102.3%, and the relative standard deviation(RSD) of the method is less than 1.14%. The method has good reproducibility and the detection results are accurate and reliable.