Abstract: An analytical method was developed to determine 2-methyl-4-chlorophenoxyacetic acid sodium (MCPANa) residue in sugarcane stem and soil by using HPLC. The MCPA-Na residue in sugarcane stem and soil was dissolved in acidic methanol and extracted by dichloromethane, the soil sample was purified through activated carbon-silica gel, while the sugarcane stem sample was purified through C18 column, then the samples were detected by HPLC-UV. This method could be used to determine the MCPA-Na residue in sugarcane and soil with good linear relationship 0.9998 when the concentration range of MCPA was 0.05~2.00 mg/L and both the limits of detection were 0.02 mg/kg. The recovery rates of MCPA-Na from sugarcane stem and soil fortified with MCPA at 0.05, 0.10, 1.00 mg/kg were 90.86%~93.25% and 84.99% ~89.77% respectively, with relative standard deviation in the range of 3.31%~8.98豫. The developed method, which had good separating effect, high recovery rate, accurancy and sensitivity, could be used to detect the MCPA-Na residue in sugarcane and soi1.