In this work, a nickel cobalt oxide (Ni/Co oxide) nanoflake based 21 electrochemical sensor for the fast determination of estriol in milk is presented for the 22 first time. Nanostructured Ni/Co oxide with controlled morphology was synthesized 23 by a facile hydrothermal method. The morphology and the electrochemical 24 performance of the Ni/Co oxide were characterized by scanning electron microscopy 25 transmission electron microscope, and energy dispersive X-ray spectroscopy, 26 respectively. Results indicated that the porous hexagonal sheet-like Ni/Co oxide 27 exhibited excellent electrocatalytic activity toward estriol, with a low detection limit 28 of 0.42 nM, and linear range from 1 nM to 14 nM. Good specificity, stability and 29 reproducibility were also demonstrated. Recovery was determined from 92.7% to 30 103.7% for spiked milk samples, providing a promising platform for fast screening of 31 estriol. 32 33 KEYWORDS: Nickel cobalt oxide; electrochemical sensor; estriol; milk 34 35 36 37 38 39 40 41