Carbon nanotubes/Au nanoparticles ( CNT/AuNP ) composite film was fabricated on glassy carbon electrode ( GCE) by first dropping CNTs on the electrode surface and then electrodeposition of AuNPs by multi-potential step. The antibody of microcystin-( leucine-arginine ) ( anti-MCLR ) was immobilized on the modified electrode surface through adsorption on AuNPs. Subsequently, bovine serum albumin ( BSA) was used to block the non-specific adsorption to obtain the immunosensor for MCLR assay. The immunosensor could effectively capture MCLR by the specific immunoreaction between the electrode surface-confined antibody and MCLR, followed by the attachment of the anti-MCLR HRP-labeled to form a sandwich-type system. The analysis of MCLR was performed based on the catalytic reaction of HRP toward the oxidation of hydroquinone ( QH2 ) by H2 O2 . Under the optimal experimental conditions, the peak current response increased linearly with the concentration of MCLR in the range of 0 . 50-12 μg/L with a detection limit of 0. 30 μg/L (S/N=3). The developed immunosensor was used to determine MCLR in real water samples, and the recoveries of standard addition experiments were in the range of 93 . 0%-108 . 5%, with the relative standard deviation of 3 . 8%-5 . 0%.