An ultrasensitive electrochemical immunosensor has been prepared using an immunofunctionalized zirconium (Zr)-based metalorganic framework (MOF) with gold (Au) decoration Au@UiO-66(NH 2 ) composite-coated glassy carbon electrode (GCE) for the determination of infectious hepatitis B surface antigen (HBsAg). We fabricated GCE with specific composite via immunefunctionalization using anti-HBsAg with Au nanoparticles embedded in UiO-66(NH 2 ). The electrochemical sensing performance of the immunofunctionalized Au@UiO-66(NH 2 )/GCE with HBsAg was characterized by cyclic voltammetry and differential pulse voltammetry. Under optimized conditions, there was a linear dynamic relationship in the buffer system between the electrical signal and HBsAg levels over the range 1.13 fg mL −1 -100 ng mL −1 (R 2 = 0.999) with a detection limit of 1.13 fg mL −1 . The total analysis time was 15 min per sample. Further validations were performed with HBsAg-spiked human serum samples, and similar detection limits as in the buffer system were observed with reduced signal intensities at lower concentrations of HBsAg (1, 10, and 100 fg mL −1 ) and minimal interference. The HBsAg electrochemical immunosensing assay had good selectivity and excellent reproducibility, thereby indicating its significant potential in the super-fast diagnosis of hepatitis B.
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