Cerium oxide nanoparticles ͑NanoCeO 2 ͒ and chitosan ͑CH͒ based nanobiocomposite film deposited onto indium-tin-oxide coated glass substrate has been used to coimmobilize rabbit immunoglobin ͑r-IgGs͒ and bovine serum albumin ͑BSA͒ for food borne mycotoxin ͓ochratoxin-A ͑OTA͔͒ detection. Electrochemical studies reveal that presence of NanoCeO 2 increases effective electro-active surface area of CH-NanoCeO 2 /indium tin oxide ͑ITO͒ nanobiocomposite resulting in high loading of r-IgGs. BSA/ r-IgGs/ CH-NanoCeO 2 / ITO immunoelectrode exhibits improved linearity ͑0.25-6.0 ng/dl͒, detection limit ͑0.25 ng/dl͒, response time ͑25 s͒, sensitivity ͑18 A / ng dl −1 cm −2 ͒, and regression coefficient ͑r 2 ϳ 0.997͒. © 2009 American Institute of Physics. ͓doi:10.1063/1.3249586͔Electrochemical immunosensors due to accuracy, sensitivity, selectivity and cost-effectiveness have been extensively used to detect proteins, biomarkers, biological toxins, and biological-warfare agents in critical situations, food, environment, pharmaceutical chemistry, and clinical diagnostics. [1][2][3] The choices of nanomaterials as appropriate matrices due to unique optical, electrical, and molecular properties and in particular high reactivity and beneficial chemically tailored physicochemical properties have been utilized for antibodies immobilization with proper orientation that help to obtain sensitive, compact, and stable immunosensor. 2,3 Among nanomaterials, metal oxides have been found to exhibit high surface-to-volume ratio, high surface reaction activity, high catalytic efficiency, and strong adsorption ability that make them potential candidate materials for the fabrication of biosensor. 2-5 Among these, nanostructured CeO 2 due to high mechanical strength, oxygen ion conductivity, biocompatibility, oxygen storage capacity, nontoxicity, high chemical stability and high electron transfer have aroused much interest for development of implantable biosensors. Moreover, high isoelectric point ͑IEP͒ of CeO 2 ͑ϳ9.2͒ can be helpful to immobilize desired biomolecules of low IEP via electrostatic interactions. 2,[5][6][7][8][9][10][11][12][13] Nanostructured CeO 2 has been used for various biosensor applications such as immunosensor for mycotoxin, 2 to immobilize cholesterol oxidase/glucose oxidase to detect cholesterol/glucose, 5-7 as an insoluble oxidant to minimize interferents, 8 for hydrogen peroxide detection via immobilizing horseradish peroxidase, 9,10 and DNA hybridization detection. 11 However, there is a considerable scope to improve the biosensing characteristics of NanoCeO 2 by dispersing these in electroactive biopolymer e.g., chitosan ͑CH͒ to fabricate nanobiocomposite. CH due to its excellent filmforming ability, mechanical strength, biocompatibility, nontoxicity, susceptibility to chemical modification, costeffectiveness, etc., has been explored for biosensor development. 3 Moreover, amino groups of CH provide a hydrophilic environment compatible with the biomolecules. 3,14 In this context, nanoporous CH-NanoCeO 2 composite has ...