RESUMO
Coronavirus disease (COVID-19) is caused by infection with the SARS-CoV-2 virus, having already caused more than seven million deaths worldwide. Conventional techniques for SARS-CoV-2 detection have limitations, as high cost, low specificity, and longer analysis time, among others. Biosensors emerge as a necessary alternative to overcome the difficulties of current diagnostics. This paper reports a sensor platform where silver-doped zinc oxide nanomaterial (Ag:ZnONp) was used onto carbon screen-printed electrode and ethidium bromide as indicator for development of a specific electrochemical genosensor for COVID-19. This genosensor demonstrated good linearity between the concentrations of 5.62â¯×â¯104-5.62 copies/mL and a detection limit of 5 copies/mL with gRNA in patient's samples, with a response time within 30â¯min. Molecular modeling and morphological analysis are in agreement with obtained electrochemical results. Additional techniques such as AFM, SEM, and EIS were conducted to characterize the morphological and electrochemical properties of the biosensor's surface. The biosensor was also capable of detecting the target presence in spiked samples and demonstrated a stability of 60â¯days, higher than other similar biosensors for SARS-CoV-2.
Assuntos
Técnicas Biossensoriais , COVID-19 , Técnicas Eletroquímicas , RNA Viral , SARS-CoV-2 , Técnicas Biossensoriais/métodos , SARS-CoV-2/genética , SARS-CoV-2/isolamento & purificação , Humanos , COVID-19/diagnóstico , COVID-19/virologia , Técnicas Eletroquímicas/métodos , RNA Viral/análise , RNA Viral/genética , Prata/química , Limite de Detecção , Óxido de Zinco/química , Nanopartículas Metálicas/química , Eletrodos , Teste de Ácido Nucleico para COVID-19/métodos , Teste de Ácido Nucleico para COVID-19/instrumentaçãoRESUMO
This contribution describes the development of a simple, fast, cost-effective, and sensitive impedimetric immunosensor for quantifying bovine tuberculosis (TB) in bovine serum samples. The construction of the immunosensor involved immobilizing the purified protein derivative (PPD) of M. bovis onto a screen-printed electrode that was modified with gold nanoparticles (AuNPs) and a polypyrrole (pPy) film synthesized electrochemically. The immunosensor exhibited a linear range from 0.5 µg mL-1 to 100 µg mL-1 and achieved a limit of detection (LD) of 100 ng mL-1 for the detection of anti-M. bovis antibody. The recovery percentages obtained in bovine serum samples were excellent, ranging between 98 % and 103 %. This device presents several advantages over alternative methods for determining TB in bovine serum samples. These include direct, in situ measurement without the need for pre-treatment, utilization of small volumes, thus avoiding harmful solvents and expensive reagents, and portability. In addition, the immunosensor exhibits both physical and chemical stability, retaining effectiveness even after 30 days of modification. This allows simultaneous incubations and facilitates large-scale detection. Hence, this immunosensor presents itself as a promising diagnostic tool for detecting anti-M. bovis antibodies in bovine serum. It serves as a viable alternative to tuberculin and ELISA tests.
Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Ouro , Nanopartículas Metálicas , Tuberculose Bovina , Animais , Bovinos , Tuberculose Bovina/diagnóstico , Tuberculose Bovina/sangue , Tuberculose Bovina/imunologia , Ouro/química , Técnicas Eletroquímicas/métodos , Imunoensaio/métodos , Técnicas Biossensoriais/métodos , Nanopartículas Metálicas/química , Mycobacterium bovis/imunologia , Polímeros/química , Pirróis/química , Eletrodos , Limite de Detecção , Anticorpos Antibacterianos/sangue , Anticorpos Antibacterianos/imunologiaRESUMO
In response to the growing need for sustainable analytical methods, this study explores the repurposing of screen-printed electrodes (SPEs) that would otherwise be discarded. This involves recoating the working electrode surface with a graphite (Gr) and chitosan (CTS) dispersion, creating a reusable SPE (SPE-Gr/CTS). Demonstrating its utility, SPE-Gr/CTS was employed for the detection of 4-bromo-2,5-dimethoxyphenethylamine (2C-B), a phenylethylamine commonly used for recreational proposes. Identifying 2C-B in fluid oral and seized samples is of great interest for forensic and toxicological applications. The 2C-B detection using SPE-Gr/CTS was optimized in Britton-Robinson buffer solution (0.1 mol L-1) at pH 2.0, employing square-wave adsorptive stripping voltammetry. The electrochemical behavior of 2C-B on SPE-Gr/CTS exhibited one irreversible oxidation and a reversible redox process. The proposed method presented a dynamic linear range for 2C-B determination (0.05 to 7.5 µmol L-1) with a low LOD (0.015 µmol L-1). Moreover, the stability of 2C-B electrochemical responses on SPE-Gr/CTS was confirmed using the same or different electrodes (N = 3), with a relative standard deviation of less than 5.0%. Interference studies with seventeen other illicit drugs and adulterants demonstrated that the proposed method is selective for 2C-B detection even in the presence of these substances. Real seized and oral fluid samples containing 2C-B were analyzed using this method, and the results were confirmed by LC-MS. The proposed device demonstrates to be an environmentally friendly and selective sensor for 2C-B detection in forensic analysis, offering a rapid and straightforward screening method for seized and biological samples. In addition, a portable and sensitive determination of 2C-B in forensic samples is presented with minimal sample consumption (50 µL).
Assuntos
Dimetoxifeniletilamina , Técnicas Eletroquímicas , Eletrodos , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Humanos , Dimetoxifeniletilamina/análogos & derivados , Dimetoxifeniletilamina/análise , Dimetoxifeniletilamina/química , Grafite/química , Limite de Detecção , Quitosana/química , Detecção do Abuso de Substâncias/métodos , Detecção do Abuso de Substâncias/instrumentaçãoRESUMO
Glyphosate (GLY), a globally-used organophosphate herbicide, is frequently detected in various environmental matrices, including water, prompting significant attention due to its persistence and potential ecological impacts. In light of this environmental concern, innovative remediation strategies are warranted. This study utilized Serratia sp. AC-11 isolated from a tropical peatland as a biocatalyst in a microbial fuel cell (MFC) coupled with a homogeneous electron-Fenton (EF) process to degrade glyphosate in aqueous medium. After coupling the processes with a resistance of 100 Ω, an output voltage value of 0.64 V was obtained and maintained stable throughout the experiment. A bacterial biofilm of Serratia sp. AC-11 was formed on the carbon felt electrode, confirmed by attenuated total reflectance-Fourier transformed infrared (ATR-FTIR) and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). In the anodic chamber, the GLY biodegradation rate was 100% after 48 h of experimentation, with aminomethylphosphonic acid (AMPA) remaining in the solution. In the cathodic chamber, the GLY degradation rate for the EF process was 69.5% after 48 h experimentation, with almost all of the AMPA degraded by the in situ generated hydroxyl radicals. In conclusion, the results demonstrated that Serratia sp. AC-11 not only catalyzed the biodegradation of glyphosate but also facilitated the generation of electrons for subsequent transfer to initiate the EF reaction to degrade glyphosate. This dual functionality emphasizes the unique capabilities of Serratia sp. AC-11, it as an electrogenic microorganism with application in innovative bioelectrochemical processes, and highlighting its role in sustainable strategies for environmental remediation.
Assuntos
Biodegradação Ambiental , Fontes de Energia Bioelétrica , Glifosato , Serratia , Serratia/metabolismo , Herbicidas/metabolismo , Glicina/análogos & derivados , Glicina/metabolismo , Glicina/química , Poluentes Químicos da Água/metabolismo , EletrodosRESUMO
This work comprehends the development and characterization of a carbon black-based electrode modified with Au microflowers to increase its effect as a capacitance biosensor for the determination of PARK7/DJ-1. Due to its high surface-to-volume ratio and biocompatibility, Au particles are suitable for antibody binding, and by monitoring surface capacitance, it is possible to identify the immune-pair interaction. Au microflowers allowed the adequate immobilization of Parkinsonian-related proteins: PARK7/DJ-1 and its antibody. The protein is associated with several antioxidant mechanisms, but its abnormal concentrations or mutations can be the cause of the loss of dopaminergic neurons, leading to Parkinson's disease. The device was characterized by scanning electron microscopy and cyclic voltammetry, revealing the flower-like structures and the electrochemically-interest enhancements they provide, such as increased heterogeneous electron transfer rate coefficient and electroactive area. The self-assembled monolayers of different molecules were optimized with the aid of 22 central composite experiments and a linear calibration curve was obtained between 0.700 and 120 ng mL-1 of PARK7/DJ-1, with a limit of detection of 0.207 ng mL-1. The data confirms that the addition of Au microflowers enhanced the electrochemical signal of the device, as well as allowed for the determination of an early stage Parkinson's disease biomarker with appreciable analytical performance.
Assuntos
Técnicas Biossensoriais , Capacitância Elétrica , Técnicas Eletroquímicas , Ouro , Doença de Parkinson , Proteína Desglicase DJ-1 , Ouro/química , Técnicas Biossensoriais/métodos , Doença de Parkinson/diagnóstico , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Humanos , Imunoensaio/métodos , Biomarcadores/análise , Anticorpos Imobilizados/imunologia , Limite de Detecção , EletrodosRESUMO
This study introduces a cost-effective approach for quantifying uric acid (UA), the main antioxidant species in human physiology and implicated in inflammatory regulation. Using a PVC substrate and pencil drawing technique, electrodes were fabricated and modified with niobium oxide and graphene oxide via a straightforward "drop casting" method. The nanostructures of the substrate, electrode, and modified electrode were evaluated using SEM images. The synergistic effect between these materials significantly facilitated the uric acid oxidation process with a 400 mV peak potential shift and 45% current increase. The evaluation of the electrode's response to common blood and urine components showed minimal deviation. Among the components tested-ascorbic acid, glucose, nitrate, nitrite, cysteine, urea, creatinine, and ammonium ion-only the ammonium ion exhibited a 10% interference at concentrations commonly found in urine. The sensors showed a good detection limit of 8.7 µmol L-1, with a wide linear range from 8.7 to 2000 µmol L-1 with a correlation factor of 0.9993 for five different sensors. The reproducibility and repeatability of the produced sensors were estimated by the RSD at 4% and 1%, respectively. Synthetic urine samples spiked exhibited reliable analysis, with recovery values within a 5% error margin. This work presents a practical, simple, and affordable sensor platform for rapid and accurate UA quantification.
Assuntos
Eletrodos , Grafite , Limite de Detecção , Nióbio , Óxidos , Ácido Úrico , Grafite/química , Ácido Úrico/urina , Ácido Úrico/química , Humanos , Nióbio/química , Óxidos/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Cloreto de Polivinila/química , Reprodutibilidade dos Testes , Análise Custo-Benefício , OxirreduçãoRESUMO
Laser scribing is a promising technology for the rapid and large-scale production of low-cost electrochemical sensors from diverse substrates. Polyimide has been the most popular so far because of its low cost, flexibility and capability of generating high-quality porous graphene films, known as laser-induced graphene (LIG). Herein we report the electrochemistry of chloramphenicol (CAP) on LIG electrodes and its determination in honey samples. LIG electrodes were fabricated by the photothermal conversion of sp3 carbon within the polymeric matrix into sp2 carbon using a CO2 laser cutter. The LIG electrode associated with differential pulse voltammetry (DPV) showed good linearity (R2 > 0.99) in the range from 10 to 160 µmol L-1 with a limit of detection of 1.0 µmol L-1 and good precision (RSD < 5%) for the electrochemical reduction of CAP species. Detection was possible free from the interference of other antibiotics, such as amoxicillin, tetracycline, sulfanilamide, and sulfamethoxazole. Spiked honey samples were analyzed by the standard-addition method and recovery values between 86 and 109% were obtained, which confirmed the absence of sample matrix effects. Therefore, the proposed sensor is an alternative, feasible, low-cost, and powerful analytical tool for the determination of CAP in honey.
Assuntos
Cloranfenicol , Técnicas Eletroquímicas , Eletrodos , Grafite , Mel , Mel/análise , Grafite/química , Cloranfenicol/análise , Cloranfenicol/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Lasers , Antibacterianos/análise , Antibacterianos/química , Limite de DetecçãoRESUMO
Rapid virus identification is crucial for preventing outbreaks. The COVID-19 pandemic has highlighted the critical nature of rapid virus detection. Here, we designed a label-free electrochemical biosensor modified with gold nanoparticles (AuNPs) to detect IgG antibodies from human serum, enabling rapid point-of-care diagnostics. AuNPs were synthesized and characterized. A multivariate optimization was carried out to determine the optimal condition for functionalizing AuNPs with anti-IgG. Subsequently, using a glassy carbon electrode (GCE), a modified AuNPs/GCE electrochemical biosensor was developed for IgG detection. The results indicated that AuNPs displayed a spherical morphology with a size distribution of 19.54 nm. Additionally, the zeta potential was recorded at -7.84 mV. Central composite design (CCD) analysis determined the optimal conditions for functionalizing AuNPs to be an anti-IgG concentration of 320 µg mL-1, a temperature of 25 °C, and pH of 7.4. The characterization study confirmed the successful synthesis and functionalization of AuNPs. Through electrochemical impedance spectroscopy measurement, the biosensor demonstrated a limit of detection (LOD) of 0.2 ng mL-1 and limit of quantification (LOQ) of 0.8 ng mL-1. Furthermore, tests in real samples showed the interaction between IgG antibodies in serum samples and AuNPs/GCE, confirming the biosensor's ability to detect and quantify IgG in clinical samples.
Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Ouro , Imunoglobulina G , Limite de Detecção , Nanopartículas Metálicas , SARS-CoV-2 , Humanos , Técnicas Biossensoriais/métodos , Ouro/química , Nanopartículas Metálicas/química , Técnicas Eletroquímicas/métodos , Imunoglobulina G/sangue , SARS-CoV-2/imunologia , SARS-CoV-2/isolamento & purificação , COVID-19/diagnóstico , COVID-19/sangue , COVID-19/virologia , Anticorpos Antivirais/sangue , Anticorpos Antivirais/imunologia , EletrodosRESUMO
The oil industry is facing substantial environmental challenges, especially in managing waste streams such as Oilfield Produced Water (OPW), which represents a significant component of the industrial ecological footprint. Conventional treatment methods often fail to effectively remove dissolved oils and grease compounds, leading to operational difficulties and incomplete remediation. Electrochemical oxidation (EO) has emerged as a promising alternative due to its operational simplicity and ability to degrade pollutants directly and indirectly, which has already been applied in treating several effluents containing organic compounds. The application of EO treatment for OPW is still in an initial stage, due to the intricate nature of this matrix and scattered information about it. This study provides a technological overview of EO technology for OPW treatment, from laboratory scale to the development of large-scale prototypes, identifying design and process parameters that can potentially permit high efficiency, applicability, and commercial deployment. Research in this domain has demonstrated notable rates of removal of recalcitrant pollutants (>90%), utilizing active and non-active electrodes. Electro-generated active species, primarily from chloride, play a pivotal role in the oxidation of organic compounds. However, the highly saline conditions in OPW hinder the complete mineralization of these organics, which can be improved by using non-active anodes and lower salinity levels. The performance of electrodes greatly influences the efficiency and effectiveness of OPW treatment. Various factors must be considered when selecting the electrode material, such as its conductivity, stability, surface area, corrosion resistance, and cost. Additionally, the specific contaminants present in the OPW, and their electrochemical reactivity must be considered to ensure optimal treatment outcomes. Balancing these considerations can be challenging, but it is crucial for achieving successful OPW treatment. Active electrode materials exhibit a high affinity for chloride molecules, generating more active species than non-active materials, which exhibit more significant degradation potential due to the production of hydroxyl radicals. Regarding scale-up, key challenges include low current efficiency, the formation of by-products, electrode deactivation, and limitations in mass transfer. To address these issues, enhanced mass transfer rates and appropriate residence times can be achieved using flow-through mesh anodes and moderate current densities, which have proven to be the optimal configuration for this process.
Assuntos
Oxirredução , Poluentes Químicos da Água/química , Eliminação de Resíduos Líquidos/métodos , Eletrodos , Campos de Petróleo e GásRESUMO
Cotton fabrics with zinc oxide (ZnO) coating are of significant interest due to their excellent antibacterial performance. Thus, they are widely in demand in the textile industry due to their medical and hygienic properties. However, conventional techniques used to deposit ZnO on fabric require long processing times in deposition, complex and expensive equipment, and multiple steps for deposition, such as a separate process for nanoparticle synthesis and subsequent deposition on fabric. In this study, we proposed a new method for the deposition of ZnO on fabric, using cathodic cage plasma deposition (CCPD), which is commonly used for coating deposition on conductor materials and is not widely used for fabric due to the temperature sensitivity of the fabric. The effect of gas composition, including argon and a hydrogen-argon mixture, on the properties of ZnO deposition is investigated. The deposited samples are characterized by XRD, SEM, EDS, photocatalytic, and antibacterial performance against Staphylococcus aureus and Pseudomonas aeruginosa bacteria. It is observed that ZnO-deposited cotton fabric exhibits excellent photocatalytic degradation of methylene blue and antibacterial performance, specifically when a hydrogen-argon mixture is used in CCPD. The results demonstrate that CCPD can be used effectively for ZnO deposition on cotton fabric; this system is already used in industrial-scale applications and is thus expected to be of significant interest to garment manufacturers and hospitals.
Assuntos
Antibacterianos , Fibra de Algodão , Staphylococcus aureus , Óxido de Zinco , Óxido de Zinco/química , Óxido de Zinco/farmacologia , Antibacterianos/farmacologia , Antibacterianos/química , Antibacterianos/síntese química , Catálise , Staphylococcus aureus/efeitos dos fármacos , Pseudomonas aeruginosa/efeitos dos fármacos , Eletrodos , Gases em Plasma/química , Gases em Plasma/farmacologia , Processos FotoquímicosRESUMO
This paper presents a new application of a lanthanum oxide (III)-modified carbon paste electrode (LaOX/CPE) for dopamine (DP) detection in the presence of ascorbic acid (AA). The presence of cetyl trimethyl ammonium bromide (CTAB) facilitated the LaOX/CPE electrode's ability to detect DP amidst AA interference, resulting in a substantial 70.0% increase in the anodic peak current for DP when compared to the unmodified carbon paste electrode (CPE). CTAB enabled clear separation of the anodic peaks for DP and AA by nearly 0.2 V, despite their initially overlapping potential values, through the ion-dipole interaction of AA and CTAB. The electrode was characterized using cyclic voltammetry (CV) and energy-dispersive spectroscopy (EDS). The method demonstrated a detection limit of 0.06 µmol/L with a relative standard deviation (RSD) of 6.0% (n = 15). Accuracy was assessed through the relative error and recovery percent, using urine samples spiked with known quantities of DP.
Assuntos
Carbono , Cetrimônio , Dopamina , Técnicas Eletroquímicas , Eletrodos , Lantânio , Óxidos , Tensoativos , Lantânio/química , Carbono/química , Dopamina/urina , Dopamina/análise , Dopamina/química , Óxidos/química , Tensoativos/química , Cetrimônio/química , Técnicas Eletroquímicas/métodos , Ácido Ascórbico/química , Ácido Ascórbico/análise , Limite de Detecção , HumanosRESUMO
Hydrochlorothiazide is an extremely important diuretic that regulates body functions, which can prevent several diseases. However, the abuse of this diuretic is concerning since it does not require a medical prescription, particularly for aesthetic purposes such as weight loss, which can lead to various health problems, including ventricular arrhythmia. The present work aims to use a glassy carbon electrode modified with Super P carbon black (SPCB/GCE) to quantify hydrochlorothiazide through Linear Sweep Adsorptive Stripping Voltammetry (LSAdSV). The modification of the GCE with SPCB significantly improved the response of hydrochlorothiazide. Furthermore, due to the adsorptive nature of charge transport, applying preconcentration time enhanced sensitivity. The optimized system provided a linear range of 0.5 to 30.0 µmol L-1 with a detection limit of 0.083 µmol L-1. Pharmaceutical tablet analyses indicated approximately 25 mg per tablet, which was confirmed by the UV-vis and in agreement with that indicated by the manufacturer. Furthermore, analyses of the tea, synthetic urine, tap water and lake water samples indicated recovery values close to 100%, demonstrating that there was no matrix effect. Therefore, it is possible to infer that the proposed method together with the sensor modified with carbon black nanoparticles presented excellent results, demonstrating that it can be an alternative method of monitoring this drug in different samples.
Assuntos
Técnicas Eletroquímicas , Eletrodos , Hidroclorotiazida , Nanopartículas , Fuligem , Hidroclorotiazida/análise , Hidroclorotiazida/urina , Hidroclorotiazida/química , Nanopartículas/química , Fuligem/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Carbono/química , Limite de Detecção , Comprimidos , Diuréticos/urina , Diuréticos/análise , Diuréticos/químicaRESUMO
The potential impact on human health and the environment has spurred significant interest in detecting and quantifying pharmaceutical compounds across various matrices, from environmental to biological samples. Here, we present an electrochemical approach for determining levofloxacin in drug, synthetic urine, water, and breast milk samples. An affordable sensor was constructed using 3D printing and composite material based on nail polish, graphite, and aluminum oxide. The conductive composite material was characterized spectroscopically, electrochemically, and by imaging techniques. Subsequently, an electrochemical method based on square wave voltammetry was optimized and applied. The method exhibited good sensitivity (5.11 ± 0.0912 µA L µmol-1 cm-2) and enhanced stability (RSD = 7.2%), with electrochemical responses correlating with the concentration of levofloxacin in the samples tested, yielding recovery values in the range of 98 to 111%. The developed method demonstrated a robust linear working range from 2 to 100 µmol L-1 and a nanomolar detection limit of 128 nmol L-1, rendering it suitable for quantitative analysis. The sensor also shows promise as a platform for the sensitive detection of pharmaceutical compounds, contributing to greater safety and sustainability in these domains.
Assuntos
Óxido de Alumínio , Técnicas Eletroquímicas , Eletrodos , Grafite , Levofloxacino , Grafite/química , Levofloxacino/análise , Humanos , Óxido de Alumínio/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Limite de Detecção , Análise Custo-Benefício , Impressão Tridimensional , Unhas/química , Antibacterianos/análiseRESUMO
Electrophoretic deposition is a straightforward method for synthesizing high-quality photoanodes. We present a protocol for synthesizing a TiO2-modified boron-doped diamond photoanode (BDD/TiO2) via electrophoretic deposition, detailing the chemical and electrochemical treatments applied to the bare BDD electrode prior to use. We provide a step-by-step guide for performing photoelectrochemical characterization under both dark and light conditions and describe an optical technique for investigating band-gap energy. For complete details on the use and execution of this protocol, please refer to Quilumbaquin et al.1.
Assuntos
Boro , Diamante , Técnicas Eletroquímicas , Eletrodos , Titânio , Titânio/química , Boro/química , Diamante/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Processos Fotoquímicos , Eletroforese/métodosRESUMO
An innovative supramolecular architecture is reported for bienzymatic glucose biosensing based on the use of a nanohybrid made of multi-walled carbon nanotubes (MWCNTs) non-covalently functionalized with a Schiff base modified with two phenylboronic acid residues (SB-dBA) as platform for the site-specific immobilization of the glycoproteins glucose oxidase (GOx) and horseradish peroxidase (HRP). The analytical signal was obtained from amperometric experiments at - 0.050 V in the presence of 5.0 × 10-4 M hydroquinone as redox mediator. The concentration of GOx and HRP and the interaction time between the enzymes and the nanohybrid MWCNT-SB-dBA deposited at glassy carbon electrodes (GCEs) were optimized through a central composite design (CCD)/response surface methodology (RSM). The optimal concentrations of GOx and HRP were 3.0 mg mL-1 and 1.50 mg mL-1, respectively, while the optimum interaction time was 3.0 min. The bienzymatic biosensor presented a sensitivity of (24 ± 2) × 102 µA dL mg-1 ((44 ± 4) × 102 µA M-1), a linear range between 0.06 mg dL-1 and 21.6 mg dL-1 (3.1 µM-1.2 mM) (R2 = 0.9991), and detection and quantification limits of 0.02 mg dL-1 (1.0 µM) and 0.06 mg dL-1 (3.1 µM), respectively. The reproducibility for five sensors prepared with the same MWCNT-SB-dBA nanohybrid was 6.3%, while the reproducibility for sensors prepared with five different nanohybrids and five electrodes each was 7.9%. The GCE/MWCNT-SB-dBA/GOx-HRP was successfully used for the quantification of glucose in artificial human urine and commercial human serum samples.
Assuntos
Técnicas Biossensoriais , Ácidos Borônicos , Enzimas Imobilizadas , Glucose Oxidase , Peroxidase do Rábano Silvestre , Nanotubos de Carbono , Bases de Schiff , Nanotubos de Carbono/química , Bases de Schiff/química , Técnicas Biossensoriais/métodos , Ácidos Borônicos/química , Glucose Oxidase/química , Glucose Oxidase/metabolismo , Peroxidase do Rábano Silvestre/química , Peroxidase do Rábano Silvestre/metabolismo , Humanos , Enzimas Imobilizadas/química , Enzimas Imobilizadas/metabolismo , Glucose/análise , Eletrodos , Limite de Detecção , Técnicas Eletroquímicas/métodos , Glicemia/análiseRESUMO
Transition metal oxides are a great alternative to less expensive hydrogen evolution reaction (HER) catalysts. However, the lack of conductivity of these materials requires a conductor material to support them and improve the activity toward HER. On the other hand, carbon paste electrodes result in a versatile and cheap electrode with good activity and conductivity in electrocatalytic hydrogen production, especially when the carbonaceous material is agglomerated with ionic liquids. In the present work, an electrode composed of multi-walled carbon nanotubes (MWCNTs) and cobalt ferrite oxide (CoFe2O4) was prepared. These compounds were included on an electrode agglomerated with the ionic liquid N-octylpyridinium hexafluorophosphate (IL) to obtain the modified CoFe2O4/MWCNTs/IL nanocomposite electrode. To evaluate the behavior of each metal of the bimetallic oxide, this compound was compared to the behavior of MWCNTs/IL where a single monometallic iron or cobalt oxides were included (i.e., α-Fe2O3/MWCNTs/IL and Co3O4/MWCNTs/IL). The synthesis of the oxides has been characterized by X-ray diffraction (XRD), RAMAN spectroscopy, and field emission scanning electronic microscopy (FE-SEM), corroborating the nanometric character and the structure of the compounds. The CoFe2O4/MWCNTs/IL nanocomposite system presents excellent electrocatalytic activity toward HER with an onset potential of -270 mV vs. RHE, evidencing an increase in activity compared to monometallic oxides and exhibiting onset potentials of -530 mV and -540 mV for α-Fe2O3/MWCNTs/IL and Co3O4/MWCNTs/IL, respectively. Finally, the system studied presents excellent stability during the 5 h of electrolysis, producing 132 µmol cm-2 h-1 of hydrogen gas.
Assuntos
Cobalto , Compostos Férricos , Hidrogênio , Líquidos Iônicos , Nanocompostos , Nanotubos de Carbono , Óxidos , Cobalto/química , Nanotubos de Carbono/química , Líquidos Iônicos/química , Nanocompostos/química , Catálise , Hidrogênio/química , Compostos Férricos/química , Óxidos/química , Eletrodos , Técnicas Eletroquímicas/métodos , Difração de Raios X , Análise Espectral RamanRESUMO
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.
Assuntos
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
With the evolution of energy storage, Thermal Runaway (TR) stands out as the most critical safety concern for Lithium-Ion Batteries (LIBs). This study employs a prismatic lithium battery with a nominal capacity of 40Ah, featuring Li(Ni0.6Co0.2Mn0.2)O2 as the cathode material. The investigation delves into the thermal runaway characteristics of the battery at 25%, 50%, 75%, and 100% State of Charge (SOC) in a nitrogen environment. The findings indicate: 1) an ascending trend in the highest temperatures at various points within the battery as SOC increases, accompanied by a declining trend in normalized gas production and a non-linear relationship between the heat released during TR and the stored electrochemical energy; 2) the highest temperature point within the battery consistently resides at the surface, offering insights for the temperature monitoring of the Battery Thermal Management System (BTMS); 3) a direct correlation between higher SOC and increased material ejection, with a mass loss rate of 25.8% at 100% SOC, a static total gas production of 2.45 mol, and a maximum explosion index of 0.2886 kPaâ mâ s⻹.
Assuntos
Fontes de Energia Elétrica , Lítio , Lítio/análise , Temperatura Alta , Temperatura , EletrodosRESUMO
An epicardial approach is often used in radiofrequency (RF) catheter ablation to ablate ventricular tachycardia when an endocardial approach fails. Our objective was to analyze the effect of the position of the dispersive patch (DP) on lesion size using computer modeling during epicardial approach. We compared the posterior position (patient's back), commonly used in clinical practice, to the anterior position (patient's chest). The model considered ventricular wall thicknesses between 4 and 8 mm, and electrode insertion depths between .3 and .7 mm. RF pulses were simulated with 20 W of power for 30 s duration. Statistically significant differences (P < .001) were found between both DP positions in terms of baseline impedance, RF current (at 15 s) and thermal lesion size. The anterior position involved lower impedance (130.8 ± 4.7 vs. 146.2 ± 4.9 Ω) and a higher current (401.5 ± 5.6 vs. 377.5 ± 5.1 mA). The anterior position created lesion sizes larger than the posterior position: 8.9 ± 0.4 vs. 8.4 ± 0.4 mm in maximum width, 8.6 ± 0.4 vs. 8.1 ± 0.4 mm in surface width, and 4.5 ± 0.4 vs. 4.3 ± 0.4 mm in depth. Our results suggest that: (1) the redirection of the RF currents due to repositioning the PD has little impact on lesion size and only affects baseline impedance, and (2) the differences in lesion size are only 0.5 mm wider and 0.2 mm deeper for the anterior position, which does not seem to have a clinical impact in the context of VT ablation.
Assuntos
Ablação por Cateter , Simulação por Computador , Eletrodos , Ventrículos do Coração , Humanos , Ventrículos do Coração/cirurgia , Ablação por Cateter/métodos , Ablação por Radiofrequência/métodos , Modelos Cardiovasculares , Pericárdio/cirurgia , Taquicardia Ventricular/cirurgia , Taquicardia Ventricular/fisiopatologiaRESUMO
Electrochemical oxidation (EO), electro-Fenton (EF), and photoelectro-Fenton (PEF) with a BDD anode have been comparatively assessed to remediate solutions of Red CL and/or Red WB azo dyes from real raw water. For the EO process in 50 mM Na2SO4 at pH 3.0, the main oxidant was the heterogeneous â¢OH generated at the anode, whereas in EF and PEF, the cathodic production of H2O2 and the addition of 0.50 mM Fe2+ catalyst additionally originated homogeneous â¢OH that enhanced the oxidation of organics. In PEF, the solution was illuminated with a 6 W UVA light. An almost total discoloration was always found operating with a 1:1 mixture of 200 mg L-1 of both dyes in 60 min, whose efficiency increased in the order of EO < EF < PEF. The HPLC analysis of the dye mixture treated by PEF disclosed that its degradation process agreed with its discoloration. A high 74% of COD was reduced due to the oxidative action of hydroxyl radicals and the photolysis of final Fe(III)-carboxylate species with UVA irradiation. The process was accompanied by an energy consumption of 0.76 kWh (g COD)-1, a value similar to the energy consumed by the applied UVA light.