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Nanorods assembled 3D microspheres of TiO2/MnO2 were prepared via a simple one-pot hydrothermal approach. The resultant composite material exhibited remarkable electrocatalytic activity for hydrogen peroxide (H2O2) in comparison to each single component. The electrochemical sensor constructed with TiO2/MnO2 exhibited a linear relationship within the range 0.0001–5.6 mmol·L−1 for H2O2. The limit of detection (LOD) and sensitivity for H2O2 were 0.03 µmol·L−1 (S/N = 3) and 316.6 µA (mmol·L−1)−1 cm−2. Moreover, this sensor can be employed to detect trace amount of H2O2 in serum and urine samples successfully, supporting an insight and strategy for a more sensitive electrochemical sensor. [ABSTRACT FROM AUTHOR]

[Display omitted] • Near-spherical ZnO/N-rGO nanocomposite was prepared by a facile hydrothermal method. • Systematic study of electrochemical sensing property of ns-ZnO/N-rGO for nitrite. • Sensor was used for detection of nitrite in ham sausage, pickle and tap water. • The electrochemical sensing mechanism of ns-ZnO/N-rGO for nitrite was explored. A hierarchical near-spherical ZnO (ns-ZnO)/Nitrogen-doped reduced graphene oxide (N-rGO) nanocomposite was synthesized via a facile hydro/solvo-thermal route. Then, a non-enzymatic nitrite electrochemical sensor (ns-ZnO/N-rGO/GCE) was obtained by modifying glassy carbon electrode (GCE) with the prepared nanocomposite. More adsorption sites and electro-catalytic active sites were provided at the electrode interface thanks to the formation of hierarchical structure, making the fabricated GCE possess a remarkable amperometric sensing property for nitrite. The limit of detection (LOD) was as low as 0.08 μM, and the detection range was as broad as 0.037 μM–5.9 mM. Furthermore, this sensor showed satisfactory recovery for nitrite in genuine samples including ham sausage, pickle and tap water, suggesting the potential practical application performance of ns-ZnO/N-rGO/GCE in the fields of food analysis and environmental monitoring. [ABSTRACT FROM AUTHOR]