Leonan dos Santos Rodrigues, Guilherme Sales da Rocha, Franccesca Fornasier, Raquel Ferreira Matos, João Victor Nicolini, Helen Conceição Ferraz
{"title":"3D-Printed Electrodes Based on Polylactic Acid and Carbonaceous Materials for Electrochemical Sensors and Biosensors: Fabrication and Surface Activation via Chemical, Electrochemical, and Laser/Plasma Methods","authors":"Leonan dos Santos Rodrigues, Guilherme Sales da Rocha, Franccesca Fornasier, Raquel Ferreira Matos, João Victor Nicolini, Helen Conceição Ferraz","doi":"10.1002/elan.70020","DOIUrl":"10.1002/elan.70020","url":null,"abstract":"<p>Surface preparation of 3D-printed electrodes fabricated from conductive filaments is essential for enhancing their electroanalytical performance, as the inherent presence of insulating polymer matrices limits electrical conductivity. To overcome this limitation, a variety of post-treatment strategies have been investigated, including chemical and electrochemical approaches, which have demonstrated promising results. In contrast, biological methods, such as enzymatic treatments, are often time-consuming, and reagent-free techniques may suffer from reproducibility issues, when not automated, due to operator-dependent variability. Among the reagentless methods, laser and plasma treatments have emerged as reliable strategies to expose the conductive material, offering an environmentally friendly route for surface activation. This review explores 3D printing technologies, commonly used filaments, and the diverse activation protocols reported for electrodes based on polylactic acid and carbon-based materials, including chemical, electrochemical, laser/plasma methods and their combinations. A critical analysis of these activation techniques and others found in the literature is also presented, highlighting their advantages, limitations, and applicability. Despite significant progress, no consensus has been reached regarding optimal treatment conditions, and the lack of standardized protocols remains a challenge. Furthermore, many studies select activation strategies based solely on electrochemical performance metrics, often without statistical validation, which may lead to the adoption of unnecessarily resource-intensive procedures. Surface treatment methods should be chosen carefully, considering reagent availability, health and environmental risks, and economic feasibility. Optimizing surface activation protocols is essential to ensure improved electrode performance and reliability. Continued research is needed to refine these methods and establish standardized methodologies, ultimately advancing the development and application of 3D-printed electrodes in electrochemical sensing and biosensing.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/elan.70020","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Leonan dos Santos Rodrigues, Guilherme Sales da Rocha, Franccesca Fornasier, Raquel Ferreira Matos, João Victor Nicolini, Helen Conceição Ferraz
{"title":"3D-Printed Electrodes Based on Polylactic Acid and Carbonaceous Materials for Electrochemical Sensors and Biosensors: Fabrication and Surface Activation via Chemical, Electrochemical, and Laser/Plasma Methods","authors":"Leonan dos Santos Rodrigues, Guilherme Sales da Rocha, Franccesca Fornasier, Raquel Ferreira Matos, João Victor Nicolini, Helen Conceição Ferraz","doi":"10.1002/elan.70020","DOIUrl":"https://doi.org/10.1002/elan.70020","url":null,"abstract":"<p>Surface preparation of 3D-printed electrodes fabricated from conductive filaments is essential for enhancing their electroanalytical performance, as the inherent presence of insulating polymer matrices limits electrical conductivity. To overcome this limitation, a variety of post-treatment strategies have been investigated, including chemical and electrochemical approaches, which have demonstrated promising results. In contrast, biological methods, such as enzymatic treatments, are often time-consuming, and reagent-free techniques may suffer from reproducibility issues, when not automated, due to operator-dependent variability. Among the reagentless methods, laser and plasma treatments have emerged as reliable strategies to expose the conductive material, offering an environmentally friendly route for surface activation. This review explores 3D printing technologies, commonly used filaments, and the diverse activation protocols reported for electrodes based on polylactic acid and carbon-based materials, including chemical, electrochemical, laser/plasma methods and their combinations. A critical analysis of these activation techniques and others found in the literature is also presented, highlighting their advantages, limitations, and applicability. Despite significant progress, no consensus has been reached regarding optimal treatment conditions, and the lack of standardized protocols remains a challenge. Furthermore, many studies select activation strategies based solely on electrochemical performance metrics, often without statistical validation, which may lead to the adoption of unnecessarily resource-intensive procedures. Surface treatment methods should be chosen carefully, considering reagent availability, health and environmental risks, and economic feasibility. Optimizing surface activation protocols is essential to ensure improved electrode performance and reliability. Continued research is needed to refine these methods and establish standardized methodologies, ultimately advancing the development and application of 3D-printed electrodes in electrochemical sensing and biosensing.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/elan.70020","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673068","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dongxue Sun, Shijie Chen, Jinlong Li, Guozhe Sui, Dongxuan Guo, Ning Liu, Renjiang Lv, Shuang Sui
{"title":"Synthesis of ZnO/ZnS/g-C3n4 Nanocomposite for the Sensitive and Selective Electrochemical Detection of Ascorbic Acid","authors":"Dongxue Sun, Shijie Chen, Jinlong Li, Guozhe Sui, Dongxuan Guo, Ning Liu, Renjiang Lv, Shuang Sui","doi":"10.1002/elan.70023","DOIUrl":"https://doi.org/10.1002/elan.70023","url":null,"abstract":"<p>In this study, ZnO/ZnS/g-C<sub>3</sub>N<sub>4</sub> composite materials were successfully synthesized via a combination of hydrothermal treatment and calcination for the electrochemical detection of ascorbic acid (AA). A systematic experimental design was implemented to evaluate the influence of key parameters, including the amount of ZnS added, the loading ratio of ZnO/ZnS onto g-C<sub>3</sub>N<sub>4</sub>, and the pH conditions during detection, on sensor performance. Comprehensive material characterization was conducted using scanning electron microscopy transmission electron microscopy X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier-transform infrared spectroscopy, providing detailed insights into the composites’ microstructure, crystallinity, elemental composition, and chemical bonding. The sensor exhibited excellent performance for AA detection, with a broad linear detection range of 20–5000 μM, a low detection limit of 1.2 μmol/L (S/N = 3), and high recovery rates between 98.23% and 105.02%, accompanied by low relative standard deviations (1.56–3.12%). Furthermore, application of the sensor in cyclic voltammetry analysis of commercial vitamin C tablets yielded accurate and reliable results, confirming its strong stability, anti-interference capacity, and reproducibility.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673096","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Novel Modified Invertase-Saccharomyces Cerevisiae Hybrid Biosensor for the Determination of Sucrose","authors":"Vural Efe, Erol Akyilmaz","doi":"10.1002/elan.70006","DOIUrl":"10.1002/elan.70006","url":null,"abstract":"<p>A biosensor system based on invertase-<i>Saccharomyces cerevisiae</i> hybrid system has been developed for the determination of sucrose molecule. For the determination of sucrose in the linear determination range of 0.1–5.0 µM, at 0.5 V potential, the limit of detection (LOD) was found to be 0.08 µM and the limit of quantification (LOQ) was 0.25 µM. With repeatability experiments, the mean value (<span></span><math></math>), standard deviation (±S.D.), and % coefficient of variation (% V.K.) were found to be 1.81 µM, ±0.09 µM, and 4.93%, respectively. Substrate specificity, interference effect, and storage stability were investigated. Sucrose was determined in fruit juice samples.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673070","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Novel Modified Invertase-Saccharomyces Cerevisiae Hybrid Biosensor for the Determination of Sucrose","authors":"Vural Efe, Erol Akyilmaz","doi":"10.1002/elan.70006","DOIUrl":"https://doi.org/10.1002/elan.70006","url":null,"abstract":"<p>A biosensor system based on invertase-<i>Saccharomyces cerevisiae</i> hybrid system has been developed for the determination of sucrose molecule. For the determination of sucrose in the linear determination range of 0.1–5.0 µM, at 0.5 V potential, the limit of detection (LOD) was found to be 0.08 µM and the limit of quantification (LOQ) was 0.25 µM. With repeatability experiments, the mean value (<span></span><math></math>), standard deviation (±S.D.), and % coefficient of variation (% V.K.) were found to be 1.81 µM, ±0.09 µM, and 4.93%, respectively. Substrate specificity, interference effect, and storage stability were investigated. Sucrose was determined in fruit juice samples.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673097","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dongxue Sun, Shijie Chen, Jinlong Li, Guozhe Sui, Dongxuan Guo, Ning Liu, Renjiang Lv, Shuang Sui
{"title":"Synthesis of ZnO/ZnS/g-C3n4 Nanocomposite for the Sensitive and Selective Electrochemical Detection of Ascorbic Acid","authors":"Dongxue Sun, Shijie Chen, Jinlong Li, Guozhe Sui, Dongxuan Guo, Ning Liu, Renjiang Lv, Shuang Sui","doi":"10.1002/elan.70023","DOIUrl":"10.1002/elan.70023","url":null,"abstract":"<p>In this study, ZnO/ZnS/g-C<sub>3</sub>N<sub>4</sub> composite materials were successfully synthesized via a combination of hydrothermal treatment and calcination for the electrochemical detection of ascorbic acid (AA). A systematic experimental design was implemented to evaluate the influence of key parameters, including the amount of ZnS added, the loading ratio of ZnO/ZnS onto g-C<sub>3</sub>N<sub>4</sub>, and the pH conditions during detection, on sensor performance. Comprehensive material characterization was conducted using scanning electron microscopy transmission electron microscopy X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier-transform infrared spectroscopy, providing detailed insights into the composites’ microstructure, crystallinity, elemental composition, and chemical bonding. The sensor exhibited excellent performance for AA detection, with a broad linear detection range of 20–5000 μM, a low detection limit of 1.2 μmol/L (S/N = 3), and high recovery rates between 98.23% and 105.02%, accompanied by low relative standard deviations (1.56–3.12%). Furthermore, application of the sensor in cyclic voltammetry analysis of commercial vitamin C tablets yielded accurate and reliable results, confirming its strong stability, anti-interference capacity, and reproducibility.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144673069","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yue Song, Meichen Pan, Pengkun Wei, Chuanlang Zhan, Yang Yang
{"title":"Strain-Engineered Self-Optimizing Heterointerface Catalysts for Enhanced Oxygen Evolution","authors":"Yue Song, Meichen Pan, Pengkun Wei, Chuanlang Zhan, Yang Yang","doi":"10.1002/elan.70014","DOIUrl":"https://doi.org/10.1002/elan.70014","url":null,"abstract":"<p>The development of cost-effective and durable oxygen evolution reaction catalysts remains crucial for sustainable hydrogen production. A Ni(OH)<sub>2</sub>@CoOOH electrocatalyst was engineered through heterogeneous interfacial design, synthesized on nickel foam via a one-step solvothermal method. Atomic-level lattice mismatches generate interfacial strain that optimizes electronic structures, while hierarchical nanosheet/nanoribbon architectures ensure structural stability. In situ surface remodeling during operation produces hydroxyl-rich Co<sup>3+<i>δ</i></sup><span></span>OOH species, enabling sustained performance enhancement. The catalyst achieves low overpotentials of 320 mV@50 mA cm<sup>−2</sup> and 337 mV@100 mA cm<sup>−2</sup>, outperforming commercial RuO<sub>2</sub>. Notably, it exhibits a 3.5% potential decrease during 152 h operation at 500 mA cm<sup>−2</sup>, where operando fragmentation generates fresh active interfaces. This work establishes a universal heterointerface design strategy that bridges scalable synthesis with atomic-level control for industrial water electrolysis.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666401","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Electrochemically Embedded Cerium Oxide Nanoparticles on Activated Carbon Electrode for Simultaneous Determination of Quercetin and Rutin","authors":"Lokesh Bettada, Hao-Chuan Chang, Shu-Hua Cheng","doi":"10.1002/elan.70017","DOIUrl":"10.1002/elan.70017","url":null,"abstract":"<p>Flavonoids (FLs) are bioactive compounds commonly found in medicinalplants, fruits, andvegetables. FLs have received considerable attention due to their medical applications as therapeutic agents. This study presents an electrochemical sensor for detecting two well-known FLs, quercetin (Qrt) and rutin (Ru). The sensor utilizes a preanodized screen-printed carbon electrode (SPCE*) modified with cerium oxide nanoparticles (CeO<sub>2</sub>). Preanodization activates the carbon surface of the electrode to enhance its electroactivity, while the immobilized CeO<sub>2</sub> acts as an electrocatalyst. The modified electrode SPCE*/CeO<sub>2</sub> was characterized using various techniques, including field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and energy-dispersive X-ray spectroscopy (EDS). Compared to the unmodified SPCE, SPCE*/CeO<sub>2</sub> exhibits superior conductivity, increased active surface area, and oxygen vacancies, all of which contribute to improved performance in electrochemical sensing for Qrt and Ru. Under optimized conditions, the constructed sensor, analyzed by differential pulse voltammetry (DPV), achieved low limits of detection (LOD), with linear ranges of 0.6–45 and 0.6–35 μM for Qrt and Ru, respectively. Furthermore, the developed assay exhibited low interference, good reproducibility, and moderate stability. The method successfully detected Qrt and Ru in fruit juice via the standard addition approach with satisfactory recoveries, demonstrating its potential application in the food industry.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yue Song, Meichen Pan, Pengkun Wei, Chuanlang Zhan, Yang Yang
{"title":"Strain-Engineered Self-Optimizing Heterointerface Catalysts for Enhanced Oxygen Evolution","authors":"Yue Song, Meichen Pan, Pengkun Wei, Chuanlang Zhan, Yang Yang","doi":"10.1002/elan.70014","DOIUrl":"10.1002/elan.70014","url":null,"abstract":"<p>The development of cost-effective and durable oxygen evolution reaction catalysts remains crucial for sustainable hydrogen production. A Ni(OH)<sub>2</sub>@CoOOH electrocatalyst was engineered through heterogeneous interfacial design, synthesized on nickel foam via a one-step solvothermal method. Atomic-level lattice mismatches generate interfacial strain that optimizes electronic structures, while hierarchical nanosheet/nanoribbon architectures ensure structural stability. In situ surface remodeling during operation produces hydroxyl-rich Co<sup>3+<i>δ</i></sup><span></span>OOH species, enabling sustained performance enhancement. The catalyst achieves low overpotentials of 320 mV@50 mA cm<sup>−2</sup> and 337 mV@100 mA cm<sup>−2</sup>, outperforming commercial RuO<sub>2</sub>. Notably, it exhibits a 3.5% potential decrease during 152 h operation at 500 mA cm<sup>−2</sup>, where operando fragmentation generates fresh active interfaces. This work establishes a universal heterointerface design strategy that bridges scalable synthesis with atomic-level control for industrial water electrolysis.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.3,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666397","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Electrochemically Embedded Cerium Oxide Nanoparticles on Activated Carbon Electrode for Simultaneous Determination of Quercetin and Rutin","authors":"Lokesh Bettada, Hao-Chuan Chang, Shu-Hua Cheng","doi":"10.1002/elan.70017","DOIUrl":"https://doi.org/10.1002/elan.70017","url":null,"abstract":"<p>Flavonoids (FLs) are bioactive compounds commonly found in medicinalplants, fruits, andvegetables. FLs have received considerable attention due to their medical applications as therapeutic agents. This study presents an electrochemical sensor for detecting two well-known FLs, quercetin (Qrt) and rutin (Ru). The sensor utilizes a preanodized screen-printed carbon electrode (SPCE*) modified with cerium oxide nanoparticles (CeO<sub>2</sub>). Preanodization activates the carbon surface of the electrode to enhance its electroactivity, while the immobilized CeO<sub>2</sub> acts as an electrocatalyst. The modified electrode SPCE*/CeO<sub>2</sub> was characterized using various techniques, including field emission scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and energy-dispersive X-ray spectroscopy (EDS). Compared to the unmodified SPCE, SPCE*/CeO<sub>2</sub> exhibits superior conductivity, increased active surface area, and oxygen vacancies, all of which contribute to improved performance in electrochemical sensing for Qrt and Ru. Under optimized conditions, the constructed sensor, analyzed by differential pulse voltammetry (DPV), achieved low limits of detection (LOD), with linear ranges of 0.6–45 and 0.6–35 μM for Qrt and Ru, respectively. Furthermore, the developed assay exhibited low interference, good reproducibility, and moderate stability. The method successfully detected Qrt and Ru in fruit juice via the standard addition approach with satisfactory recoveries, demonstrating its potential application in the food industry.</p>","PeriodicalId":162,"journal":{"name":"Electroanalysis","volume":"37 7","pages":""},"PeriodicalIF":2.7,"publicationDate":"2025-07-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144666402","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}