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The indiscriminate use of pesticides makes us susceptible to the toxicity of these chemical compounds, which may be present in high quantities in our food. It is crucial to develop inexpensive and rapid methods for determining these pesticides for government control or even for the general population. In this study, we investigated the fabrication of self-assembled LbL films using multi-walled carbon nanotubes (MWCNT) and nickel tetrasulphonated phthalocyanine (NiTsPc) as an electrochemical sensor for the herbicide Diquat (DQ). The Layer-by-Layer (LbL) assembly of the (MWCNT/NiTsPc) film was examined, along with its structural and morphological characteristics. The effect of the number of layers in DQ detection was evaluated by cyclic voltammetry, followed by the detection through differential pulse voltammetry. The achieved limit of detection was 9.62 × 10-7 mol L-1. A ~ 30% decrease in sensitivity was observed in the presence of Paraquat, a banned herbicide and electrochemical interferent due to the structural similarities, which is regularly neglected in the most published studies. The sensor was tested in real samples, demonstrating a recovery of 98.5% in organic apples.
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A wearable glove-based sensor is a portable and practical approach for onsite detection/monitoring of a variety of chemical threats. Herein, we report a flexible and sensitive wearable sensor fabricated on the nitrile glove fingertips by stencil-printing technique. The working electrodes were modified with multiwalled carbon nanotubes (MWCNTs)/poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) for sensitive and real-time analyses of hazardous or chemical treats, as picric acid (PA) explosive, diazepam (DZ) as drug-facilitated crimes and the emerging pollutant 4-nitrophenol (4-NP). The multi-sensing platform towards PA, 4-NP, and DZ offers the ability of in-situ qualitative and quantitative analyses of powder and liquid samples. A simple sampling by touching or swiping the fingertip sensor on the sample or surface under investigation using an ionic hydrogel combined with fast voltammetry measurement provides timely point-of-need analyses. The wearable glove-based sensor uses the square wave voltammetry (SWV) technique and exhibited excellent performance to detect PA, 4-NP, and DZ, resulting in limits of detection (LOD) of 0.24 µM, 0.35 µM, 0.06 µM, respectively, in a wide concentration range (from 0.5 µM to 100 µM). Also, we obtained excellent manufacturing reproducibility with relative standard deviations (RSD) in the range of 3.65%-4.61% using 7 different wearable devices (n = 7) and stability in the range of 4.86%-6.61% using different electrodes stored for 10 days at room temperature (n = 10), demonstrating the excellent sensor-to-sensor reproducibility and stability for reliable in-field measurements. The stretchable sensor presented great mechanical robustness, supporting up to 80 bending or stretching deformation cycles without significant voltammetric changes. Collectively, our wearable glove-based sensor may be employed for analyses of chemical contaminants of concern, such as explosives (PA), drugs (DZ), and emerging pollutants (4-NP), helping in environmental and public safety control.
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Diazepam , Técnicas Eletroquímicas , Nanotubos de Carbono , Nitrofenóis , Dispositivos Eletrônicos Vestíveis , Nanotubos de Carbono/química , Nitrofenóis/análise , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Diazepam/análise , Eletrodos , Humanos , Limite de Detecção , Substâncias Explosivas/análise , Polímeros/química , PicratosRESUMO
In this work, the electrochemical behavior of the glycosylated flavonoid kaempferitrin was studied, and an electroanalytical methodology was developed for its determination in infusions of Bauhinia forficata using a boron-doped diamond electrode (BDD). The electrochemical behavior of the flavonoid was studied by cyclic voltammetry, and two irreversible oxidation peaks at 0.80 and 1.0 V vs Ag/AgCl were observed. The influence of the pH on the voltammograms was examined, and higher sensitivity was found at pH 7.0. The electrochemical process corresponding to peak 1 at 0.80 V is predominantly diffusion-controlled, as the study shows at varying scan rates. An analytical plot was obtained by square wave voltammetry at optimized experimental conditions (frequency = 100 s-1, amplitude = 90 mV, and step potential = 8 mV) in the concentration range from 3.4 µmol L-1 to 58 µmol L-1, with a linearity of 0.99. The limit of detection and limit of quantification values were 1.0 µmol L-1 and 3.4 µmol L-1, respectively. Three samples of Bauhinia forficata infusions (2 g of sample in 100 mL of water) were analyzed, and the KF values found were 5.0 × 10-4 mol L-1, 3.0 × 10-4 mol L-1, and 7.0 × 10-4 mol L-1, with recovery percentages of 98 %, 106 % and 94 %, respectively. Finally, experiments were performed with two other flavonoids (chrysin and apeginin) to compare and propose an electrochemical oxidation mechanism for kaempferitrin, which was supported by quantum chemical calculations.
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Técnicas Eletroquímicas , Quempferóis , Oxirredução , Quempferóis/química , Quempferóis/análise , Técnicas Eletroquímicas/métodos , Glicosilação , Eletrodos , Bauhinia/química , Teoria Quântica , Flavonoides/química , Flavonoides/análise , Limite de Detecção , Diamante/químicaRESUMO
This paper reports a rapid and sensitive sensor for the detection and quantification of the COVID-19 N-protein (N-PROT) via an electrochemical mechanism. Single-frequency electrochemical impedance spectroscopy was used as a transduction method for real-time measurement of the N-PROT in an immunosensor system based on gold-conjugate-modified carbon screen-printed electrodes (Cov-Ag-SPE). The system presents high selectivity attained through an optimal stimulation signal composed of a 0.0 V DC potential and 10 mV RMS-1 AC signal at 100 Hz over 300 s. The Cov-Ag-SPE showed a log response toward N-PROT detection at concentrations from 1.0 ng mL-1 to 10.0 µg mL-1, with a 0.977 correlation coefficient for the phase (θ) variation. An ML-based approach could be created using some aspects observed from the positive and negative samples; hence, it was possible to classify 252 samples, reaching 83.0, 96.2 and 91.3% sensitivity, specificity, and accuracy, respectively, with confidence intervals (CI) ranging from 73.0 to 100.0%. Because impedance spectroscopy measurements can be performed with low-cost portable instruments, the immunosensor proposed here can be applied in point-of-care diagnostics for mass testing, even in places with limited resources, as an alternative to the common diagnostics methods.
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Técnicas Biossensoriais , COVID-19 , Espectroscopia Dielétrica , Ouro , SARS-CoV-2 , COVID-19/diagnóstico , COVID-19/virologia , Técnicas Biossensoriais/métodos , Técnicas Biossensoriais/instrumentação , Humanos , SARS-CoV-2/isolamento & purificação , SARS-CoV-2/imunologia , Espectroscopia Dielétrica/instrumentação , Espectroscopia Dielétrica/métodos , Ouro/química , Eletrodos , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Imunoensaio/métodos , Imunoensaio/instrumentação , Proteínas do Nucleocapsídeo de Coronavírus/imunologia , Proteínas do Nucleocapsídeo de Coronavírus/análise , Carbono/química , Fosfoproteínas/análiseRESUMO
The development of a portable analytical procedure is described for rapid sequential detection and quantification of the explosives 2,4,6-trinitrotoluene (TNT) and cyclotrimethylenetrinitramine (RDX) in forensic samples using a graphite sheet (GS). A single GS platform works as a collector of explosive residues and detector after its assembly into a 3D-printed cell. The detection strategy is based on cyclic square-wave stripping voltammetry. The cathodic scan from + 0.1 to -1.0 V with accumulation at 0.0 V enables the TNT detection (three reduction peaks), and the anodic scan from + 0.2 to + 1.55 V with accumulation at -0.9 V provides the RDX detection (two oxidation processes). Low detection limit values (0.1 µmol L-1 for TNT and 2.4 µmol L-1 for RDX) and wide linear ranges (from 1 to 150 µmol L-1 for TNT and from 20 to 300 µmol L-1 for RDX) were obtained. The sensor did not respond to pentaerythritol tetranitrate (PETN), which was evaluated as a potential interferent, because plastic explosives contain mixtures of TNT, RDX, and PETN. The GS electrode was also evaluated as a collector of TNT and RDX residues spread on different surfaces to simulate forensic scenarios. After swiping over different surfaces (metal, granite, wood, cloths, hands, money bills, and cellphone), the GS electrode was assembled in the 3D-printed cell ready to measure both explosives by the proposed method. In all cases, the presence of TNT and RDX was confirmed, attesting the reliability of the proposed device to act as collector and sensor.
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The study presents the successful development of a new electrochemical sensor with low cost and disposability for application in nitrofurazone detection in environmental and pharmaceutical samples. The sensors were fabricated using materials obtained from local storage and conductive carbon ink. The modification of the screen-printed electrodes with the hybrid nanomaterial based on silver nanoparticles, carbon quantum dots, and carbon nanotubes showed synergistic contributions in the nitrofurazone electrooxidation, as observed in the wide linear range (0.008 at 15.051 µM), with a sensitivity of 0.650 µA/µM. The limit of detection obtained was 4.6 nM. Differential pulse voltammetry, cyclic voltammetry, X-ray photoelectron spectroscopy, X-ray diffraction analysis, and high-resolution transmission electron microscopy were used to evaluate the electrochemical and structural characteristics. Studies of possible interferences were considered with nitrofurazone in the presence of the ions and organic molecules. The results were satisfactory, with a variation of 93.3% ± 4.39% at 100% ± 2.40%. The low volume used in the analyses (50 µL), disposability, high sensibility, selectivity, and low limit of detection are advantages that make the proposed sensor an electrochemical tool of high viability for the NFZ detection in environmental matrices and pharmaceutical formulations.
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Antibacterianos , Técnicas Eletroquímicas , Nanopartículas Metálicas , Nanotubos de Carbono , Nitrofurazona , Nitrofurazona/análise , Nitrofurazona/química , Técnicas Eletroquímicas/métodos , Nanotubos de Carbono/química , Nanopartículas Metálicas/química , Antibacterianos/análise , Limite de Detecção , Prata/química , Eletrodos , Pontos Quânticos/químicaRESUMO
The chemical stability of azithromycin (AZM) may be compromised depending on the imposed thermo-oxidative conditions. This report addresses evidence of this process under varying conditions of temperature (20-80 °C), exposure time to UV radiation (1-3 h irradiation at 257 nm), and air saturation (1-3 h saturation with atmospheric air at 1.2 L min-1 and 15 kPa) through electrochemical measurements performed with a thermoactivated cerium molybdate (Ce2(MoO4)3)/multi-walled carbon nanotubes (MWCNT)-based composite electrode. Thermal treatment at 120 °C led to coordinated water elimination in Ce2(MoO4)3, improving its electrocatalytic effect on antibiotic oxidation, while MWCNT were essential to reduce the charge-transfer resistance and promote signal amplification. Theoretical-experimental data revealed remarkable reactivity for the irreversible oxidation of AZM on the working sensor using phosphate buffer (pH = 8) prepared in CH3OH/H2O (10:90%, v/v). Highly sensitive (230 nM detection limit) and precise (RSD < 4.0%) measurements were recorded under these conditions. The results also showed that AZM reduces its half-life as the temperature, exposure time to UV radiation, and air saturation increase. This fact reinforces the need for continuous quality control of AZM-based pharmaceuticals, using conditions closer to those observed during their transport and storage, reducing impacts on consumers' health.
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The selective, rapid detection of low levels of hormones in drinking water and foodstuffs requires materials suitable for inexpensive sensing platforms. We report on core-shell Ag@C nanocables (NCs) decorated with carbon spherical shells (CSSs) and silver nanoparticles (AgNPs) by using a hydrothermal green approach. Sensors were fabricated with homogeneous, porous films on screen-printed electrodes, which comprised a 115 nm silver core covered by a 122 nm thick carbon layer and CSSs with 168 nm in diameter. NCs and CSSs were also decorated with 10-25 nm AgNPs. The NC/CSS/AgNP sensor was used to detect ethinylestradiol using square wave voltammetry in 0.1 M phosphate buffer (pH 7.0) over the 1.0-10.0 µM linear range with a detection limit of 0.76 µM. The sensor was then applied to detect ethinylestradiol in tap water samples and a contraceptive pill with recovery percentages between 93 and 101%. The high performance in terms of sensitivity and selectivity for hormones is attributed to the synergy between the carbon nanomaterials and AgNPs, which not only increased the sensor surface area and provided sites for electron exchange but also imparted an increased surface area.
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Carbono , Nanopartículas Metálicas , Prata , Etinilestradiol , Água , Hormônios , Eletrodos , Técnicas EletroquímicasRESUMO
Rhamnolipids (RHLs) are promising biosurfactants with important applications in several industrial segments. These compounds are produced through biotechnological processes using the bacteria Pseudomonas Aeruginosa. The main methods of analyzing this compound are based on chromatographic techniques. In this study, an electrochemical sensor based on a platform modified with reduced graphene oxide, manganese nanoparticles covered with a molecularly imprinted poly (L-Ser) film was used as an alternative method to quantify RHL through its hydrolysis product, acid 3-hydroxydecanoic acid (3-HDA). The proposed sensor was characterized microscopically, spectroscopically and electrochemically. Under optimized experimental conditions, an analytical curve was obtained in the linear concentration range from 2.0 × 10-12 mol L-1 to 1.0 × 10-10 mol L-1. The values estimated of LOD, LOQ and AS were 8.3 × 10-13 mol L-1, 2.7 × 10-12 mol L-1and 1.3 × 107 A L mol-1, respectively. GCE/rGO/MnNPs/L-Ser@MIP exhibits excellent selectivity, repeatability, and high stability for the detection of 3-HDA. Furthermore, the developed method was successfully applied to the recognition of the hydrolysis product (3-HDA) of RHLs obtained from guava agro-waste. Statistical comparison between GCE/rGO/MnNPs/L-Ser@MIP and HPLC method confirms the accuracy of the electrochemical sensor within a 95% confidence interval.
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Glicolipídeos , Grafite , Impressão Molecular , Nanopartículas , Manganês , Polímeros/química , Limite de Detecção , Grafite/química , Nanopartículas/química , Técnicas Eletroquímicas/métodos , Impressão Molecular/métodos , EletrodosRESUMO
Curcumin is a compound of great importance in the food industry due to its biological and pharmacological properties, which include being an antioxidant, anti-inflammatory, antibacterial, antiviral, and anticarcinogenic. This paper proposes the synthesis of an electrochemical sensor based on molecularly imprinted polymers (MIPs) and MWCNT by drop casting deposited on a glassy carbon electrode (GCE) for the selective quantification of curcumin in food samples. The synthesized compounds are characterized by Fourier transform infrared (IR), Brunauer-Emmett-Teller (BET), and electrochemical techniques such as cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The optimal conditions for further experiments were determined by selecting these parameters. We examined three food products, commercial capsules, turmeric rhizomes, and commercial turmeric powder, employing both electrochemical and HPLC methods for the analysis. The electrochemical method revealed a limit of detection (LOD) value of 0.1365 µmol L-1, compared with the HPLC analysis, which gave a value of 3.55 µmol L-1. Furthermore, the MIP material demonstrated superior selectivity for the analyte compared to potential interferents. The recovery percentage, determined using the HPLC method, fell within the range of 87.5% to 102.6.
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Butylated hydroxyanisole (BHA) is a synthetic phenolic antioxidant widely used in various food matrices to prevent oxidative rancidity. However, its presence has been associated with liver damage and carcinogenesis in animals. Thus, an electrochemical sensor was built using a composite of gold nanoparticles synthesized in peach extract (Prunus persica (L.) Batsch) and graphene. Peach extract served as a reducing and stabilizing agent for gold nanoparticles, as a dispersing agent for graphene, and as a film former to immobilize the composite on the surface of a glassy carbon electrode. The gold nanoparticles were characterized using spectroscopic and microscopic techniques, and the electrodes were electrochemically characterized using electrochemical impedance spectroscopy and cyclic voltammetry. The sensor provided higher current responses and lower charge transfer resistances compared to the unmodified glassy carbon electrode. Under the established optimized working conditions (0.1 mol L-1 Britton-Robinson buffer, pH 4.0, and differential pulse voltammetry), the calibration curve exhibited a linear range from 0.2 to 9.8 µmol L-1, with a detection limit of 70 nmol L-1. The proposed sensor represented a sensitive and practical analytical tool for the accurate determination of BHA in mayonnaise samples.
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Grafite , Nanopartículas Metálicas , Prunus persica , Grafite/química , Antioxidantes , Ouro/química , Hidroxianisol Butilado , Nanopartículas Metálicas/química , Carbono/química , Eletrodos , Técnicas Eletroquímicas/métodos , Limite de DetecçãoRESUMO
In this work we describe a straightforward approach for creating a nanocomposite comprising multiwalled carbon nanotubes (MWCNTs) and titanium dioxide (TiO2) using the hydrothermal technique, which is then characterized by scanning electron microscope (SEM), energy-dispersive X-ray spectrometer (EDS), X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FTIR), and thermal gravimetric analysis (TGA) to assess its properties. Nafion is employed as a reticular agent for the nanocomposite on the glassy carbon electrode (GCE), creating the MWCNT/TiO2/Nafion/GCE system. The electrochemical behavior of the system was evaluated using cyclic voltammetry, revealing its remarkable electrocatalytic activity for detecting hydrogen peroxide in water. The developed sensor showcased a broad linear response range of 14.00 to 120.00 µM, with a low detection limit of 4.00 µM. This electrochemical sensor provides a simple and highly sensitive method for detecting hydrogen peroxide in aqueous solutions and shows promising potential for various real-world applications, particularly in H2O2 monitoring.
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In this study, a selective and sensitive electrochemical approach for determining hydroxychloroquine (HCQ) was proposed. A novel nanocomposite based on gold nanoparticles synthesized by green synthesis in an extract of white pitaya (Hylocereus undatus) (AuNP-Ext) decorated with functionalized multi-walled carbon nanotubes (f-MWCNTs) was presented. AuNP-Ext was characterized by ultraviolet-visible spectroscopy and the f-MWCNTs/AuNP-Ext nanocomposite by transmission electron microscopy. The nanocomposite was used to modify a glassy carbon electrode (GCE). Using the f-MWCNT-AuNP-Ext/GCE sensor, an irreversible oxidation peak at +0.74 V vs. Ag/AgCl was verified by HCQ. The calibration plot was studied in two linear ranges, from 0.03 to 3.5 µmol/L and from 3.5 to 17.0 µmol/L, with a limit of detection of 0.0093 µmol/L and a limit of quantification of 0.031 µmol/L, regarding the first linear range. The proposed sensor was successfully applied to the determination of HCQ in pharmaceutical and clinical samples without any special purification, separation or pre-treatment steps. The accuracy was verified by UV-Vis spectrometry, and this revealed that the proposed method was accurate and precise, as evidenced by F- and t-tests.
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A rapid and simple method for the amperometric determination of glucose using a nanocomposite film of nickel oxyhydroxide and multi-walled carbon nanotube (MWCNTs) was evaluated. The NiHCF)/MWCNT electrode film was fabricated using the liquid-liquid interface method, and it was used as a precursor for the electrochemical synthesis of nickel oxy-hydroxy (Ni(OH)2/NiOOH/MWCNT). The interaction between nickel oxy-hydroxy and the MWCNTs provided a film that is stable over the electrode surface, with high surface area and excellent conductivity. The nanocomposite presented an excellent electrocatalytic activity for the oxidation of glucose in an alkaline medium. The sensitivity of the sensor was found to be 0.0561 µA µmol L-1, and a linear range from 0.1 to 150 µmol L-1 was obtained, with a good limit of detection (0.030 µmol L-1). The electrode exhibits a fast response (150 injections h-1) and a sensitive catalytic performance, which may be due to the high conductivity of MWCNT and the increased active surface area of the electrode. Additionally, a minimal difference in the slopes for ascending (0.0561 µA µmol L-1) and descending (0.0531 µA µmol L-1) was observed. Moreover, the sensor was applied to the detection of glucose in artificial plasma blood samples, achieving values of 89 to 98% of recovery.
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Nanotubos de Carbono , Níquel , Glucose , Oxirredução , Eletrodos , Impressão Tridimensional , Técnicas Eletroquímicas/métodosRESUMO
In this work, an electrochemical method was developed for rapid and sensitive detection of hydroxychloroquine (HCQ), an ineffective candidate drug for COVID-19 treatment however widely consumed during the pandemic, in aqueous samples using a multi-walled carbon nanotubes (MWCNT) film produced through the interfacial method on the indium tin oxide electrode (ITO). According to Raman spectroscopy, X-ray diffraction, UV-vis spectroscopy, Energy-dispersive X-ray spectroscopy, scanning electron microscopy, and atomic force microscopy, the interfacial method produces homogeneous thin films of carbon nanotubes on the substrate surface, which keep connected to the surface forming a three-dimensional microporous structure. The electrochemical behavior and oxidation kinetics of HCQ were also investigated in the MWCNT film. The sensor showed a 7 times higher oxidation current for (69.88 µA) for HCQ than the ITO electrode (9.33 µA) due to the electrocatalytic properties MWCNTs. The ITO-modified electrode was assembled on a portable 3D-printed batch-injection cell for the amperometric detection of HCQ. The oxidation peak current of HCQ is linearly proportional to the concentrations of HCQ ranging from 1.0 to 100.0 µmol L-1, with a limit of detection of 0.27 µmol L-1. Water samples (river and tap water) were spiked with HCQ, without the need for dispendious pretreatment (except filtration), and analyzed by the portable system, revealing the detection of HCQ with the recovery of 92.0%-99.8%, which suggested the great potential for real environmental monitoring application.
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In this work, an electrochemical sensor was developed for the determination of naphthalene (NaP) in well water samples, based on a glass carbon electrode (GCE) modified as a nanocomposite of manganese oxides (MnOx) and COOH-functionalized multi-walled carbon nanotubes (MWCNT). The synthesis of MnOx nanoparticles was performed by the sol-gel method. The nanocomposite was obtained by mixing MnOx and MWCNT with the aid of ultrasound, followed by stirring for 24 h. Surface modification facilitated the electron transfer process through the MnOx/MWCNT/GCE composite, which was used as an electrochemical sensor. The sensor and its material were characterized by cyclic voltammetry (CV), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). Important parameters influencing electrochemical sensor performance (pH, composite ratios) were investigated and optimized. The MnOx/MWCNT/GCE sensor showed a wide linear range of 2.0-16.0 µM, a detection limit of 0.5 µM and a quantification limit of 1.8 µM, in addition to satisfactory repeatability (RSD of 7.8%) and stability (900 s) in the determination of NaP. The determination of NaP in a sample of water from a gas station well using the proposed sensor showed results with recovery between 98.1 and 103.3%. The results obtained suggest that the MnOx/MWCNT/GCE electrode has great potential for application in the detection of NaP in well water.
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Alzheimer's disease (AD) is a neurodegenerative disease with only late-stage detection; thus, diagnosis is made when it is no longer possible to treat the disease, only its symptoms. Consequently, this often leads to caregivers who are the patient's relatives, which adversely impacts the workforce along with severely diminishing the quality of life for all involved. It is, therefore, highly desirable to develop a fast, effective and reliable sensor to enable early-stage detection in an attempt to reverse disease progression. This research validates the detection of amyloid-beta 42 (Aß42) using a Silicon Carbide (SiC) electrode, a fact that is unprecedented in the literature. Aß42 is considered a reliable biomarker for AD detection, as reported in previous studies. To validate the detection with a SiC-based electrochemical sensor, a gold (Au) electrode-based electrochemical sensor was used as a control. The same cleaning, functionalization and Aß1-28 antibody immobilization steps were used on both electrodes. Sensor validation was carried out by means of Cyclic Voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS) aiming to detect an 0.5 µg·mL-1 Aß42 concentration in 0.1 M buffer solution as a proof of concept. A repeatable peak directly related to the presence of Aß42 was observed, indicating that a fast SiC-based electrochemical sensor was constructed and may prove to be a useful approach for the early detection of AD.
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This study describes the use of copper nanoparticles (CuNPs) and reduced graphene oxide (rGO) as an electrode modifier for the determination of chloroquine phosphate (CQP). The synthetized rGO-CuNPs composite was morphologically characterized using scanning electron microscopy and electrochemically characterized using cyclic voltammetry. The parameters were optimized and the developed electrochemical sensor was applied in the determination of CQP using square-wave voltammetry (SWV). The analytical range for the determination of CQP was 0.5 to 110 µmol L-1 (one of the highest linear ranges for CQP considering electrochemical sensors), with limits of detection and quantification of 0.23 and 0.78 µmol L-1, respectively. Finally, the glassy carbon (GC) electrode modified with rGO-CuNPs was used for quantification of CQP in tap water; a study was carried out with interferents using SWV and obtained great results. The use of rGO-CuNP material as an electrode modifier was thus shown to be a good alternative for the development of low-cost devices for CQP analysis.
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The monitoring of endocrine disruptors in the environment is one of the main strategies in the investigation of potential risks associated with exposure to these chemicals. Bisphenol A is one of the most prevalent endocrine-disrupting compounds and is prone to leaching out from polycarbonate plastic in both freshwater and marine environments. Additionally, microplastics also can leach out bisphenol A during their fragmentation in the water environment. In the quest for a highly sensitive sensor to determine bisphenol A in different matrices, an innovative bionanocomposite material has been achieved. This material is composed of gold nanoparticles and graphene, and was synthesized using a green approach that utilized guava (Psidium guajava) extract for reduction, stabilization, and dispersion purposes. Transmission electron microscopy images revealed well-spread gold nanoparticles with an average diameter of 31 nm on laminated graphene sheets in the composite material. An electrochemical sensor was developed by depositing the bionanocomposite onto a glassy carbon surface, which displayed remarkable responsiveness towards bisphenol A. Experimental conditions such as the amount of graphene, extract: water ratio of bionanocomposite and pH of the supporting electrolyte were optimized to improve the electrochemical performance. The modified electrode displayed a marked improvement in current responses for the oxidation of bisphenol A as compared to the uncovered glassy carbon electrode. A calibration plot was established for bisphenol A in 0.1 mol L-1 Britton-Robinson buffer (pH 4.0), and the detection limit was determined to equal to 15.0 nmol L-1. Recovery data from 92 to 109% were obtained in (micro)plastics samples using the electrochemical sensor and were compared with UV-vis spectrometry, demonstrating its successful application with accurate responses.
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Grafite , Nanopartículas Metálicas , Grafite/química , Plásticos , Ouro/química , Nanopartículas Metálicas/química , Carbono , ÁguaRESUMO
Acute myocardial infarction (AMI) is the main cause of death worldwide, and the time of diagnosis is decisive for the effectiveness of the treatment of patients with AMI. Creatine kinase-myocardial band (CK-MB) has a predominance and high affinity with myocardial tissue, making it considered one of the main biomarkers for the diagnosis of AMI. In this work, we report a novel biodegradable composite material based on a polymer blend of Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) and Poly(butylene adipate-co-terephthalate) (PHBV:Ecoflex) and graphite microparticles for sensitive and selective electrochemical detection of CK-MB. The morphological and physicochemical characterizations of the thermoplastic composite material revealed a homogeneous and synergistic distribution of the graphite microparticles through the blend structure, providing low defects and high electrical conductivity with high electron transfer kinetics (k0 = 3.54 × 10-3 cm s-1) features with adequate flexibility for point-of-care applications. The portable and disposable devices were applied to detect CK-MB using the electrochemical impedance spectroscopy (EIS) technique in a relevant clinical concentration ranging from 5.0 ng mL-1 to 100.0 ng mL-1 and presented a limit of detection of 0.26 ng mL-1 CK-MB. The selectivity of the sensor was confirmed by testing the potential interference of major biomolecules found in biofluids and other relevant macromolecules. The accuracy and robustness were assessed by addition and recovery protocol in urine and saliva samples without sample pretreatment and demonstrated the potential of our method for rapid and decentralized tests of AMI. In addition, the study of the thermal, biological, and photodegradation of the devices after being used was also carried out, aiming at the disposal of the material more sustainably.