A new method coupling matrix solid phase dispersion（MSPD） with capillary electrophoresis was developed for the determination of acrylamide in rice product.The optimized conditions obtained in experiments were as follows：Florisil and C18 were used as a mixed dispersant with a mass ratio of 1∶4.The mass ratio of sample to dispersant was 5∶9.The mixture of 10 mL acetone-dichloromethane（6∶4） was used as elution solvent.Under the optimized experimental conditions，20 mmol/L borate solution（pH 8.4） was used as buffer.The sample was separated at a constant voltage of 15 kV.The linear range of acrylamide was in the range of 10-200 μg/mL，with a correlation coefficient（r） of 0.999 8.The limit of detection（LOD，S/N=3） was 0.62 μg/mL for acrylamide and the recoveries were in the range of 85.7%-96.4%.