https://hdl.handle.net/10259/7686 2026-04-20T21:38:01Z https://hdl.handle.net/10259/10768 Dataset of the work “Determination of nicotine in e-liquids by electrochemical generation of surface-enhanced Raman scattering substrates” Romay García, Luis; Pérez Estébanez, Martín; Heras Vidaurre, Aránzazu; Colina Santamaría, Álvaro Quantitative methods using surface-enhanced Raman scattering (SERS) for analysis in complex matrices are very attractive due to the high sensitivity and selectivity of this technique. In this work, a novel time-resolved electrochemical surface-enhanced Raman scattering (TR-EC-SERS) analytical method has been developed for the determination of nicotine in e-liquids of electronic cigarettes. One of the main challenges of SERS is its inherent lack of reproducibility. Here, this limitation was mitigated by employing an electrochemical pre-treatment step to generate a homogeneous distribution of silver nanoparticles (Ag-NPs) on a silver screen-printed electrode. The enhanced Raman scattering induced by the Ag-NPs enabled the detection of nicotine at nanomolar levels. The high sensitivity of the method allowed the quantitative analysis of diluted e-liquid samples, mitigating potential interferences from other components present in these complex matrices. Moreover, TR-EC-SERS, coupled with parallel factor analysis (PARAFAC), demonstrated the capability of trilinear spectroelectrochemistry data not only to detect nicotine but also to identify potential interfering compounds without prior knowledge of their spectral signatures. This multivariate approach offers significant potential for the detection of outliers in complex samples. 2025-05-20T00:00:00Z https://hdl.handle.net/10259/10766 Dataset of the work “Simultaneous UV/vis Absorption in Parallel Configuration, Photoluminescence and Raman Spectroelectrochemistry” Olmo Alonso, Fabiola; Pérez Estébanez, Martín; Heras Vidaurre, Aránzazu; Campo García, Francisco Javier del; Colina Santamaría, Álvaro Analytical Chemistry is the science of chemical measurements that seeks to acquire the most comprehensive information about a chemical system. Recent advances in technology have facilitated the development of new combined analytical techniques capable of supplying analytical signals of different natures. These signals subsequently provide diverse information related to specific chemical reactions. This technical note proposes a new combination of three different spectroscopic techniques (UV/vis absorption spectroscopy in a parallel configuration, photoluminescence and Raman spectroscopy) with electrochemistry. To illustrate the capabilities of this new technique, two chemical systems (tris(2,2' bipyridine)ruthenium(II) and ofloxacin) were selected. A comparison of the behavior of the two molecules during the electrode process demonstrates the advantages of obtaining several signals simultaneously in a single experiment. 2025-05-20T00:00:00Z https://hdl.handle.net/10259/10759 Dataset of the work “New screen-printed electrodes for Raman spectroelectrochemistry. Determination of p-aminosalicylic acid” Romay García, Luis; Núñez Marinero, Pello; Perales Rondon, Juan Víctor; Heras Vidaurre, Aránzazu; Campo García, Francisco Javier del; Colina Santamaría, Álvaro Background: The availability of new surface enhanced Raman scattering (SERS) substrates is essential to develop quantitative analytical methods. Electrochemistry is an easy, fast and reproducible methodology to prepare SERS substrates on screen-printed electrodes (SPEs). Results: This work proposes new SPEs based on a three-electrode system all made of silver. Using the same ink for the whole electrode system facilitates the fabrication process, reduces production costs, and leads to excellent analytical performance. The results showed that Raman enhancement depends strongly on the type of silver ink. To demonstrate the capabilities of the new electrodes developed, 4-aminosalicylic acid was determined in complex matrices and in the presence of strong interfering compounds such as salicylic acid and acetylsalicylic acid. The proposed analytical method is based on the electrochemical surface oxidation enhanced Raman scattering (EC-SOERS) strategy. AgCl nanocrystals are generated on the working electrode surface, which amplify the Raman signal of 4-aminosalicylic acid. Good figures of merit were obtained both in the absence and in the presence of the interfering compounds, achieving a correct estimation of a 4-aminosalicylic test sample in complex matrices. Significance: The new SPEs have been demonstrated to be very sensitive and reproducible which, together to the high specificity of the Raman signal, makes this methodology very attractive for chemical analysis. 2025-05-20T00:00:00Z https://hdl.handle.net/10259/10752 Dataset of the work “Activating the SERS features of screen-printed electrodes with thiocyanate for sensitive and robust EC-SERS analysis” Moldovan, Rebeca; Pérez Estébanez, Martín; Heras Vidaurre, Aránzazu; Bodoki, Ede; Colina Santamaría, Álvaro This study presents a novel electrochemical (EC) methodology for activating the SERS features of disposable silver screen-printed electrodes (AgSPEs) using a pseudohalide as a precipitating agent to guide the assembly of a nano-filamentous silver network responsible for a strong SERS enhancement. To the best of our knowledge, the use of thiocyanate for SPEs activation for quantitative purposes has not been reported before. In order to better study this complex system, time-resolved (TR) operando spectroelectrochemistry (SEC) measurements were performed by SERS and UV-Vis and correlated with SEM imaging of the electrode surface at different steps. Moreover, to significantly increase the reproducibility of the assays, a rapid EC protocol was proposed for the first time to obtain a reliable Ag/AgSCN reference electrode (RE) and a comprehensive optimization process was conducted to determine the critical parameters. Additionally, propranolol, as an emerging pharmaceutical pollutant has been selected as a model molecule to demonstrate the applicability of the method for rapid (3 min) quantitative analysis in the nM range from real river and tap water samples. 2025-05-20T00:00:00Z