Microchimica Acta ( IF 5.3 ) Pub Date : 2022-07-29 , DOI: 10.1007/s00604-022-05336-z Yan Huang 1 , Ziteng Han 1 , Xia Zhou 1 , Jiaxin Li 1 , Xiangling Gu 2 , Zhongfang Li 1 , Wei Sun 3 , Xueliang Niu 1
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A facile and novel electrochemical sensing platform is reported for quercetin determination with MoS2 nanoflowers-3D graphene aerogel (3D MoS2-GA) nanocomposite as signal amplified material. The 3D MoS2-GA nanocomposite was synthesized through a two-step hydrothermal method, in which MoS2 nanoflowers were prepared in advance. Characterizations of 3D MoS2-GA were performed by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The 3D MoS2-GA-modified glassy carbon electrode (3D MoS2-GA/GCE) was used to investigate the electrochemical behaviors of quercetin with electrochemical parameters calculated, reaction mechanism discussed, and experimental conditions optimized. Notably, the redox peak current densities of quercetin on 3D MoS2-GA/GCE raised 5.14 and 6.40 times compared with those on a bare GCE. Furthermore, a novel electroanalytical approach was proposed for the sensitive determination of quercetin within the concentration range 0.01 ~ 5.0 μmol/L, accompanied by a low detection limit of 0.0026 μmol/L (at a working potential of 0.38 V vs. Ag/AgCl). The recovery for practical sample analysis ranges from 97.0 to 105%, and the relative standard deviation is less than 4.2%. This established method shows reliable performance in determination of quercetin in tablets and urine samples.
Graphical abstract
中文翻译：
用于槲皮素电化学传感的三维 MoS2-石墨烯气凝胶纳米复合材料
报道了一种使用 MoS 2 nanoflowers-3D 石墨烯气凝胶 (3D MoS 2 -GA) 纳米复合材料作为信号放大材料来测定槲皮素的简便新型电化学传感平台。通过两步水热法合成3D MoS 2 -GA纳米复合材料，其中预先制备了MoS 2纳米花。3D MoS 2 -GA 的表征通过扫描电子显微镜、透射电子显微镜、拉曼光谱、X 射线衍射和 X 射线光电子能谱进行。3D MoS 2 -GA 改性玻碳电极（3D MoS 2-GA/GCE) 用于研究槲皮素的电化学行为，计算了电化学参数，讨论了反应机理，优化了实验条件。值得注意的是，槲皮素在 3D MoS 2 -GA/GCE 上的氧化还原峰值电流密度比裸 GCE 上提高了 5.14 倍和 6.40 倍。此外，提出了一种新的电分析方法，用于在 0.01 ~ 5.0 μmol/L 浓度范围内灵敏测定槲皮素，同时检测限低至 0.0026 μmol/L（工作电位为 0.38 V vs. Ag/AgCl） . 实际样品分析的回收率为97.0～105%，相对标准偏差小于4.2%。这种建立的方法在测定片剂和尿液样品中的槲皮素方面表现出可靠的性能。
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