2026-04-18T07:38:21Zhttps://riubu.ubu.es/oai/request

oai:riubu.ubu.es:10259/93212025-06-09T11:30:45Zcom_10259_3844com_10259_5086com_10259_2604col_10259_3845

Perales Rondon, Juan Víctor 432 600 0000-0001-7182-6289 Hernández Muñoz, Sheila 275 600 0000-0002-0466-8759 González Baró, Ana C. 8193c5ec-ef8e-4c67-bbe5-31596f1fbeb2 600 Heras Vidaurre, Aránzazu 273 600 0000-0002-5068-2164 Colina Santamaría, Álvaro 122 600 0000-0003-0339-356X 2024-07-01T06:54:37Z 2024-07-01T06:54:37Z 2023-06-23 0003-2700 http://hdl.handle.net/10259/9321 10.1021/acs.analchem.2c05468 1520-6882 The combination of instrumental techniques allows obtaining precise and reliable information about the reactions taking place at the electrode/solution interface. Although UV–Vis absorption spectroelectrochemistry (UV–Vis SEC) provides a molecular insight about the species involved in the electrode process, obtaining information about the redox state of the products generated in this process is not always accessible by this technique. In this sense, scanning electrochemical microscopy (SECM) has a clear advantage, since it provides additional information on the oxidation state of the intermediates/products. Therefore, the combination of these two techniques facilitates obtaining a more complete picture of the electrochemical reaction studied from two different points of view, but under exactly the same experimental conditions. In this work, the combination of UV–Vis SEC in parallel configuration and SECM is carried out for the first time. This new technique allows distinguishing between those species that are electrochemically active and, at the same time, exhibit changes in the UV–Vis absorption spectra during the electrochemical reaction. The new experimental setup is first validated using ferrocenemethanol as a standard probe, concomitantly obtaining spectroscopic and electrochemical information that accurately describes the oxidation process. Finally, the strength of this combined technique is demonstrated by studying the antioxidant activity of o-vanillin (o-HVa) in the presence of electrogenerated superoxide. The information extracted from the new UV–Vis SEC/SECM technique makes it possible to identify, beyond any doubt, not only the origin of the electrochemical signals recorded in the SECM tip but also to evaluate the antioxidant effect of o-HVa at different concentrations. The authors acknowledge Ministerio de Ciencia e Innovación and Agencia Estatal de Investigación (MCIN/AEI/10.13039/501100011033 and PID2020-113154RB-C21) and Ministerio de Ciencia, Innovación y Universidades (RED2018-102412-T) for the support of this work. J.V.P.-R. acknowledges Ministerio de Universidades and European Union─NextGenerationEU for his Maria Zambrano fellowship. S.H. thanks JCyL and European Social Fund for her predoctoral fellowship. application/pdf eng ACS Publications Analytical Chemistry. 2023, V. 95, n. 28, p. 10532-10539 https://doi.org/10.1021/acs.analchem.2c05468 info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica, Técnica y de Innovación 2017-2020/PID2020-113154RB-C21/ES/APLICACION DE NUEVOS MATERIALES Y DISPOSITIVOS PARA EC-SERS Y EC-SOERS/ info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/RED2018-102412-T/ES/RED DE SENSORES Y BIOSENSORES ELECTROQUIMICOS/ Atribución 4.0 Internacional http://creativecommons.org/licenses/by/4.0/ info:eu-repo/semantics/openAccess Química analítica Electroquímica Chemistry, Analytic Electrochemistry Simultaneous Scanning Electrochemical Microscopy and UV–Vis Absorption Spectroelectrochemistry info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion Analytical Chemistry 95 28 10532 10539 THUMBNAIL Perales-ac_2023.pdf.jpg Perales-ac_2023.pdf.jpg IM Thumbnail image/jpeg 5274 https://riubu.ubu.es/bitstream/10259/9321/4/Perales-ac_2023.pdf.jpg fe4781ced69383ed133ad1053816f8e8 MD5 4 LICENSE license.txt license.txt text/plain; charset=utf-8 999 https://riubu.ubu.es/bitstream/10259/9321/3/license.txt b295bcbce42e2caabeb0c623d3860c06 MD5 3 CC-LICENSE license_rdf license_rdf application/rdf+xml; charset=utf-8 908 https://riubu.ubu.es/bitstream/10259/9321/2/license_rdf 0175ea4a2d4caec4bbcc37e300941108 MD5 2 ORIGINAL Perales-ac_2023.pdf Perales-ac_2023.pdf application/pdf 5412016 https://riubu.ubu.es/bitstream/10259/9321/1/Perales-ac_2023.pdf 16bfc45a7650e876a9fcc49192744d33 MD5 1 10259/9321 oai:riubu.ubu.es:10259/9321 2025-06-09 13:30:45.016 Repositorio Institucional de la Universidad de Burgos bubrep@ubu.es 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