An analytical method was developed to extract and determine 2methyl4chlorophenoxyacetic acid(MCPA) residue in sugarcane and soil using solid-phase extraction and high-performance liquid chromatography (SPEHPLC). The MCPA residue in sugarcane and soil was dissolved in 0.04 mol/L sodium hydroxide aqueous solution，and purified through basic aluminaSPE column. Then the sample was detected by HPLCUV. The method could be used to determine the MCPA residue in sugarcane and soil with fine linear relationship (R2=0.999 3) when the concentration range of MCPA was 0.0510 mg/L and the limit of detection was 0.01 mg/kg. The recovery rates of MCPA from sugarcane and soil fortified with MCPA at 0.05,0.1,1.0 mg/kg were 82.2%89.1% and 84.0%85.7% respectively, with relative standard deviation＜10%. The results showed that the half-life of degradation for MCPA was 1.782.69 d in sugarcane, 2.403.64 d in soil.