The invention belongs to the technical field of dopamine and uric acid, and discloses a three-dimensional carbon fabric/nickel iron layered hydroxide coated cobaltosic oxide nano-wire composite material, as well as a preparation method and application thereof. The preparation method comprises the following steps: 1, reacting a carbon cloth in nitric acid having a concentration of 3mol/L for 2 hours to prepare a functional three-dimensional carbon cloth; 2, soaking the functional three-dimensional carbon cloth in mixture of cobalt nitrate, urea and ammonium fluoride, reacting for 6-8 hours, cooling, washing, drying, and calcining the dried product in a tube furnace in presence of nitrogen at 400 DEG C for 2 hours; and 3, reacting for 100 seconds at a working voltage of negative 1.0V by using the three-dimensional carbon cloth/cobaltosic oxide nano-wire array composite material as a work electrode, and washing with deionized water to prepare the composite material. The preparation methodis simple, can be used for quickly and efficiently detecting dopamine and uric acid, and has a wider linear detection range and lower detection limit.