Faculty of Materials Science and Ceramics, AGH University of Science and Technology, 30-059 Kraków, Poland.
Sensors (Basel). 2021 Nov 27;21(23):7928. doi: 10.3390/s21237928.
The diversity of materials proposed for non-enzymatic glucose detection and the lack of standardized protocols for assessing sensor performance have caused considerable confusion in the field. Therefore, methods for pre-evaluation of working electrodes, which will enable their conscious design, are currently intensively sought. Our approach involved comprehensive morphologic and structural characterization of copper sulfides as well as drop-casted suspensions based on three different polymers-cationic chitosan, anionic Nafion, and nonionic polyvinylpyrrolidone (PVP). For this purpose, scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy were applied. Subsequently, comparative studies of electrochemical properties of bare glassy carbon electrode (GCE), polymer- and copper sulfides/polymer-modified GCEs were performed using electrochemical impedance spectroscopy (EIS) and voltammetry. The results from EIS provided an explanation for the enhanced analytical performance of Cu-PVP/GCE over chitosan- and Nafion-based electrodes. Moreover, it was found that the pH of the electrolyte significantly affects the electrocatalytic behavior of copper sulfides, indicating the importance of OH in the detection mechanism. Additionally, diffusion was denoted as a limiting step in the irreversible electrooxidation process that occurs in the proposed system.
用于非酶葡萄糖检测的材料多样性以及缺乏评估传感器性能的标准化协议,导致该领域出现了相当大的混乱。因此,目前正在积极寻找用于预评估工作电极的方法,这将使人们能够有意识地设计这些电极。我们的方法涉及对硫化铜以及基于三种不同聚合物(阳离子壳聚糖、阴离子 Nafion 和非离子聚乙烯吡咯烷酮(PVP)的滴铸悬浮液进行全面的形态和结构表征。为此,应用了扫描电子显微镜(SEM)、X 射线衍射(XRD)和拉曼光谱。随后,使用电化学阻抗谱(EIS)和伏安法对裸玻碳电极(GCE)、聚合物和铜硫化物/聚合物修饰的 GCE 的电化学性质进行了比较研究。EIS 的结果解释了 Cu-PVP/GCE 相对于壳聚糖和基于 Nafion 的电极增强的分析性能。此外,还发现电解质的 pH 值显著影响铜硫化物的电催化行为,表明 OH 在检测机制中的重要性。此外,扩散被标记为在所提出的系统中发生的不可逆电化学氧化过程中的限制步骤。