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Microdialysis sampling coupled with liquid chromatography and electrochemical detection (LC-ECD) was developed and applied to study the interaction of 6-Mercaptopurine (6-MP) with bovine serum albumin (BSA). In the LC-ECD, the multi-wall carbon nanotubes fuctionalized with carboxylic groups modified electrode (MWNT-COOH CME) was used as the working electrode for the determination of 6-MP. The results indicated that this chemically modified electrode (CME) exhibited efficiently electrocatalytic oxidation for 6-MP with relatively high sensitivity, stability and long-life. The peak currents of 6-MP were linear to its concentrations ranging from 4.0 x 10(-7) to 1.0 x 10(-4) mol l(-1) with the calculated detection limit (S/N = 3) of 2.0 x 10(-7) mol l(-1). The method had been successfully applied to assess the association constant (K) and the number of the binding sites (n) on a BSA molecular, which calculated by Scatchard equation, were 3.97 x 10(3) mol(-1) l and 1.51, respectively. This method provided a fast, sensible and simple technique for the study of drug-protein interactions.