Ana Teresa da Silva Cardoso Brandão

Abstract Carbon nanotubes (CNTs) are receiving special attention due to their remarkable thermal, electrical, and mechanical properties. The present work reports an innovative synthesis procedure to decorate MWCNTs with silver nanoparticles (Ag-NPs) via pulsed reverse deposition technique using a deep eutectic solvent (DES) based on choline chloride and glycerol as an electrolyte at room temperature, not requiring any previous surface modification of MWCNTs. MWCNTs decorated with Ag-NPs disclose a significant enhancement of their electrochemical performance as demonstrated by the increase of electrode stability and specific capacitance. Electrochemical characterization of the composite material was performed using cyclic voltammetry and charge/discharge curves, achieving a specific capacitance up to 28.50 F. g-1, against 4.70 F. g-1 for the commercial MWCNTs in a three-electrode system. Retention of the specific capacitance up to 99% for the Ag-MWCNTs composites compared with a value of 78% for electrodes modified with commercial MWCNTs. The Ag-MWCNTs composites were characterized through SEM/EDX analysis, ultrahighresolution STEM, in which the Z - Contrast image was collected, and Raman analysis to prove the successful attachment of the Ag-NPs to the MWCNTs surface. AFM was performed to evaluate the conductivity of the composites. (c) 2021 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Abstract Here we report the rational development of a carbon dot (CDs)-based fluorescent pH nanosensor by employing an active surface preservation strategy. More specifically, citric acid, urea and fluorescein were subjected to a one-pot hydrothermal treatment, which preserved fluorescein-like structures on the surface of the CDs. The obtained CDs showed pH-sensitive green emission, which can be used to determine pH variations from 3.7 to 12.1 by fluorescence enhancement. Moreover, the obtained nanoparticles showed excellent selectivity toward pH, fluorescence reversibility in different pH values, photostability, while being compatible with human cell lines (even at high concentrations). Furthermore, their performance as pH sensors was comparable with reference pH determination procedures. Thus, an active surface preservation strategy was successfully employed to develop fluorescence pH nanosensors in a rational manner and without post-synthesis functionalization strategies, which show potential for future use in pH determination.

Abstract <jats:p>The design and synthesis of artificial receptors based on molecular imprinting (MI) technology for the development of a new MIP-based biosensor for detection of the stress biomarker α-amylase in human saliva in point-of-care (PoC) applications is described in this work. The portable electrochemical devices for monitoring α-amylase consists of cost-effective and disposable gold screen-printed electrodes (AuSPEs). To build the electrochemical device, the template biomolecule was firstly immobilized directly over the working area of the gold chip previously activated with a self-assembled monolayer (SAM) of cysteamine (CA). Then, pyrrole (Py) monomer was selected as building block of a polymeric network prepared by CV electropolymerization. After the electropolymerization process, the enzyme was removed from the polymer film in order to build the specific recognition sites for the target enzyme. The MIP biosensor showed a very wide linear concentration range (between 3.0 × 10−4 to 0.60 mg mL−1 in buffer solution and between 3.0 × 10−4 to 3.0 × 10−2 mg mL−1 in human saliva) and low detection levels were achieved (LOD &lt; 3.0 × 10−4 mg mL−1) using square wave voltammetry (SWV) as the electroanalytical technique.</jats:p>

Abstract Considering the high incidence level and mortality rate of ovarian cancer, particularly among the European female population, the carbohydrate antigen 125 (CA-125) was selected as the protein target for this study for the development of a MIP-based biosensor. This work presents the development of molecular imprinting polymers (MIPs) on gold electrode surface for CA-125 biomarker recognition. The preparation of the CA-125 imprinting was obtained by electropolymerization of pyrrole (Py) monomer in a gold electrode using cyclic voltammetry (CV) in order to obtain highly selective materials with great molecular recognition capability. The quantification of CA-125 biomarker was made through the comparison of two methods: electrochemical (square wave voltammetry -SWV) and optical transduction (surface plasmon resonance -SPR). SWV has been widely used in biological molecules analysis since it is a fast and sensitive technique. In turn, SPR is a non-destructive optical technique that provides high-quality analytical data of CA-125 biomarker interactions with MIP. Several analytical parameters, such as sensitivity, linear response interval, and detection limit were determined to proceed to the performance evaluation of the electrochemical and optical transduction used in the development of the CA-125 biosensor. The biosensor based in the electrochemical transduction was the one that presented the best analytical parameters, yielding a good selectivity and a detection limit (LOD) of 0.01 U/mL, providing a linear concentration range between 0.01 and 500 U/mL. This electrochemical biosensor was selected for the study and it was successfully applied in the CA-125 analysis in artificial serum samples with recovery rates ranging from 91 to 105% with an average relative error of 5.8%.

Abstract Nano carbons, such as graphene and carbon nanotubes, show very interesting electrochemical properties and are becoming a focus of interest in many areas, including electrodeposition of carbon-metal composites for battery application. The aim of this study was to incorporate carbon materials (namely oxidized multi-walled carbon nanotubes (ox-MWCNT), pristine multi-walled carbon nanotubes (P-MWCNT), and reduced graphene oxide (rGO)) into a metallic tin matrix. Formation of the carbon-tin composite materials was achieved by electrodeposition from a choline chloride-based ionic solvent. The different structures and treatments of the carbon materials will create metallic composites with different characteristics. The electrochemical characterization of Sn and Sn composites was performed using chronoamperometry, potentiometry, electrochemical impedance, and cyclic voltammetry. The initial growth stages of Sn and Sn composites were characterized by a glassy-carbon (GC) electrode surface. Nucleation studies were carried out, and the effect of the carbon materials was characterized using the Scharifker and Hills (SH) and Scharifker and Mostany (SM) models. Through a non-linear fitting method, it was shown that the nucleation of Sn and Sn composites on a GC surface occurred through a 3D instantaneous process with growth controlled by diffusion. According to Raman and XRD analysis, carbon materials were successfully incorporated at the Sn matrix. AFM and SEM images showed that the carbon incorporation influences the coverage of the surface as well as the size and shape of the agglomerate. From the analysis of the corrosion tests, it is possible to say that Sn-composite films exhibit a comparable or slightly better corrosion performance as compared to pure Sn films.