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A new chemically modified electrode(CME) immobilized on the surface of multi-wall carbon nanotubes functionalized with carboxylic groups was fabricated. The results indicate that the CME exhibits efficiently electrocatalytic oxidation of 6-mercaptopurine(6-MP). The CME can be used as the working electrode in the liquid chromatography for the determination of 6-MP. The peak current of 6-MP is linearly changed with its concentration ranging from 4.0×10-7 to 1.0×10-4 mol/L with the calculated detection limit (S/N= 3) of 2.0×10-7 mol/L. Coupled with microdialysis sampling, the method has been successfully applied to assessing the content of 6-MP in rat blood.