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<p>The extensive use of hydroxylamine hydrochloride (HH) in pharmaceutical, agricultural, and chemical industries has led to increasing environmental residues, posing a potential threat to public health and ecological safety. To address this issue, we developed a high-performance electrochemical sensor based on a willow-catkin-derived hierarchical hollow tubular NiCo₂S₄/NSC composite for highly sensitive detection of HH. Using willow catkins as a biomass template, the hierarchical hollow tubular NiCo₂S₄/NSC composite was synthesized through a hydrothermal-assisted bio-templated method. The material integrates the high electrical conductivity of the N, S co-doped carbon (NSC) framework, the large specific surface area offered by the biomass template, and the abundant active sites and excellent catalytic properties of the bimetallic spinel NiCo₂S₄. The electrochemical sensor constructed with this composite demonstrates outstanding performance toward HH detection, achieving a low detection limit of 2.24 nM, a wide linear range from 60 nM to 5 mM, and excellent selectivity, anti-interference capability, and stability. In real river water analysis, the sensor exhibits recoveries of 99.12%-100.4% with relative standard deviations (RSD) below 2%, indicating good practical applicability. The superior performance of the sensor is attributed to the synergistic effect between the abundant redox-active sites provided by NiCo₂S₄ and the enhanced electron-transfer capability of the NSC framework, which significantly improves interfacial reaction kinetics and reduces charge-transfer resistance. This study not only offers a highly sensitive approach for trace detection of HH, but also provides a feasible strategy for developing eco-friendly electrochemical sensors using low-cost biomass materials, showing promising potential in environmental monitoring.</p> Graphical Abstract <p></p>

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Synthesis of hierarchical structured NiCo₂S₄/NSC composites via willow-catkin biotemplate for trace and highly sensitive electrochemical detection of hydroxylamine hydrochloride

  • 期刊论文

  • 发表日期：

    2026年3月24日

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  • Xiaohan Sun,
  • Menghao Li,
  • XinYu Guo,
  • Xianfa Zhang,
  • Yingming Xu,
  • Xiaoli Cheng,
  • Shan Gao,
  • Lihua Huo

摘要

The extensive use of hydroxylamine hydrochloride (HH) in pharmaceutical, agricultural, and chemical industries has led to increasing environmental residues, posing a potential threat to public health and ecological safety. To address this issue, we developed a high-performance electrochemical sensor based on a willow-catkin-derived hierarchical hollow tubular NiCo₂S₄/NSC composite for highly sensitive detection of HH. Using willow catkins as a biomass template, the hierarchical hollow tubular NiCo₂S₄/NSC composite was synthesized through a hydrothermal-assisted bio-templated method. The material integrates the high electrical conductivity of the N, S co-doped carbon (NSC) framework, the large specific surface area offered by the biomass template, and the abundant active sites and excellent catalytic properties of the bimetallic spinel NiCo₂S₄. The electrochemical sensor constructed with this composite demonstrates outstanding performance toward HH detection, achieving a low detection limit of 2.24 nM, a wide linear range from 60 nM to 5 mM, and excellent selectivity, anti-interference capability, and stability. In real river water analysis, the sensor exhibits recoveries of 99.12%-100.4% with relative standard deviations (RSD) below 2%, indicating good practical applicability. The superior performance of the sensor is attributed to the synergistic effect between the abundant redox-active sites provided by NiCo₂S₄ and the enhanced electron-transfer capability of the NSC framework, which significantly improves interfacial reaction kinetics and reduces charge-transfer resistance. This study not only offers a highly sensitive approach for trace detection of HH, but also provides a feasible strategy for developing eco-friendly electrochemical sensors using low-cost biomass materials, showing promising potential in environmental monitoring.

Graphical Abstract