The establishment of SPE-HPLC method for the determination of malachite green,crystal violet residues.By using potassium borohydride solution,malachite green and crystal violet was deoxidized to leucomalachite green and leuco crystal violet,and used acetonitrile/dichloromethane to extract the residues.The extracts were purified and washed down sequentially through the acidic alumina column/PRS column purification,elution.Experimental results showed that the method could well remove the disruptors in water,and the recovery rate was 84% ~93%,leueo-malachite green minimum detection limit was 0.96 μ g/L,leuco crystal violet minimum detection limit was 1.02 μ g/L,suit for the determination of malachite green and crystal violet assay in water,and had good laboratory application prospect.