Kowalski Grzegorz, Kwaczyński Karolina, Poltorak Lukasz
Electrochemistry@Soft Interfaces Team, Department of Inorganic and Analytical Chemistry, Faculty of Chemistry, University of Lodz, Tamka 12, 91-403, Lodz, Poland; BioMedChem Doctoral School of the University of Lodz and Institutes of Polish Academy of Sciences, University of Lodz, Matejki 21/23, 90-237, Lodz, Poland.
Electrochemistry@Soft Interfaces Team, Department of Inorganic and Analytical Chemistry, Faculty of Chemistry, University of Lodz, Tamka 12, 91-403, Lodz, Poland.
Talanta. 2025 Jun 17;296:128467. doi: 10.1016/j.talanta.2025.128467.
In this work, we manufactured the entire electrochemical configuration (all electrodes along with the ergonomic cell), which was 3D-printed using fused deposition modelling (FDM) technology. All electrodes were printed from carbon black/poly(lactic acid) (CB/PLA) filament, while the cell body was produced with neutral PLA. An activation process was conducted to enhance the electrochemical properties of all electrodes (working electrode (WE), counter electrode (CE), and reference electrode (RE)), which included immersion in dichloromethane followed by anodic, and cathodic treatment. The WE was only subjected to the activation process, providing the best output when the synergistic action of organic solvent and electrochemical electrode surface treatment were used. The novel aspects of this work originate from the applied electrode surface treatment, adjustment of all three electrodes' placement in an ergonomic and fully 3D printed cell, and finally, RE and CE properties adjustment. For the latter, the REs properties were defined by electrodeposition of silver particles further covered with AgCl, providing a stable and constant reference potential. The CE was made out of 3D-printed CB/PLA modified with platinum particles, which enhanced its electric conductivity. Even though, in both cases, the surface coverage was found to be nonhomogeneous the electrodes displayed desired properties, creating cheap substitutions to commercially available components. All electrodes were comprehensively inspected with a range of characterization techniques, including voltammetry, chronoamperometry, electrochemical impedance spectroscopy, scanning electron microscopy, optical profilometry, attenuated total reflectance Fourier-transform infrared spectroscopy, laser-induced breakdown spectroscopy along with surface wettability studies. The electrochemical behavior of the system, in the presence of a model redox probe, ferrocenemethanol, was analyzed using cyclic voltammetry. Finally, our fully 3D-printed sensing platform was assessed for paracetamol determination giving the limit of detection and limit of quantification to be 0.38 μM and 1.26 μM, respectively. The system was successfully applied to the determination of paracetamol in a pharmaceutical tablet using the standard addition method, confirming its suitability for quantitative analysis in complex sample matrices.
在这项工作中,我们制造了整个电化学配置(所有电极以及符合人体工程学的电池),该配置使用熔融沉积建模(FDM)技术进行3D打印。所有电极均由炭黑/聚乳酸(CB/PLA)细丝打印而成,而电池主体则由中性PLA制成。进行了激活过程以增强所有电极(工作电极(WE)、对电极(CE)和参比电极(RE))的电化学性能,该过程包括浸入二氯甲烷,然后进行阳极和阴极处理。仅对工作电极进行激活过程,当使用有机溶剂和电化学电极表面处理的协同作用时可提供最佳输出。这项工作的新颖之处源于所应用的电极表面处理、在符合人体工程学且完全3D打印的电池中调整所有三个电极的位置,以及最后对参比电极和对电极性能的调整。对于后者,参比电极的性能通过电沉积银颗粒并进一步覆盖AgCl来定义,从而提供稳定且恒定的参比电位。对电极由用铂颗粒改性的3D打印CB/PLA制成,这增强了其电导率。尽管在这两种情况下都发现表面覆盖率不均匀,但电极显示出所需的性能,成为市售组件的廉价替代品。使用一系列表征技术对所有电极进行了全面检查,包括伏安法、计时电流法、电化学阻抗谱、扫描电子显微镜、光学轮廓仪、衰减全反射傅里叶变换红外光谱、激光诱导击穿光谱以及表面润湿性研究。使用循环伏安法分析了在存在模型氧化还原探针二茂铁甲醇的情况下系统的电化学行为。最后,对我们的全3D打印传感平台进行了扑热息痛测定评估,检测限和定量限分别为0.38 μM和1.26 μM。该系统使用标准加入法成功应用于药物片剂中扑热息痛的测定,证实了其在复杂样品基质中进行定量分析的适用性。