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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.
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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
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
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.
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Compostos Azo , Boro , Corantes , Diamante , Eletrodos , Oxirredução , Poluentes Químicos da Água , Corantes/química , Poluentes Químicos da Água/química , Boro/química , Compostos Azo/química , Diamante/química , Peróxido de Hidrogênio/química , Curtume , Técnicas Eletroquímicas , Fotólise , Raios Ultravioleta , Eliminação de Resíduos Líquidos/métodos , Ferro/químicaRESUMO
The combination of CRISPR technology and electrochemical sensors has sparked a paradigm shift in the landscape of point-of-care (POC) diagnostics. This review explores the dynamic convergence between CRISPR and electrochemical sensing, elucidating their roles in rapid and precise biosensing platforms. CRISPR, renowned for its remarkable precision in genome editing and programmability capability, has found a novel application in conjunction with electrochemical sensors, promising highly sensitive and specific detection of nucleic acids and biomarkers associated with diverse diseases. This article navigates through fundamental principles, research developments, and applications of CRISPR-based electrochemical sensors, highlighting their potential to revolutionize healthcare accessibility and patient outcomes. In addition, some key points and challenges regarding applying CRISPR-powered electrochemical sensors in real POC settings are presented. By discussing recent advancements and challenges in this interdisciplinary field, this review evaluates the potential of these innovative sensors as an alternative for decentralized, rapid, and accurate POC testing, offering some insights into their applications across clinical scenarios and their impact on the future of diagnostics.
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Técnicas Biossensoriais , Técnicas Eletroquímicas , Técnicas Biossensoriais/métodos , Humanos , Técnicas Eletroquímicas/métodos , Sistemas CRISPR-Cas/genética , Testes Imediatos , Sistemas Automatizados de Assistência Junto ao LeitoRESUMO
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
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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Foodborne pathogens are a grave concern for the for food, medical, environmental, and economic sectors. Their ease of transmission and resistance to treatments, such as antimicrobial agents, make them an important challenge. Food tainted with these pathogens is swiftly rejected, and if ingested, can result in severe illnesses and even fatalities. This review provides and overview of the current status of various pathogens and their metabolites transmitted through food. Despite a plethora of studies on treatments to eradicate and inhibit these pathogens, their indiscriminate use can compromise the sensory properties of food and lead to contamination. Therefore, the study of detection methods such as electrochemical biosensors has been proposed, which are devices with advantages such as simplicity, fast response, and sensitivity. However, these biosensors may also present some limitations. In this regard, it has been reported that nanomaterials with high conductivity, surface-to-volume ratio, and robustness have been observed to improve the detection of foodborne pathogens or their metabolites. Therefore, in this work, we analyze the detection of pathogens transmitted through food and their metabolites using electrochemical biosensors based on nanomaterials.
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Técnicas Biossensoriais , Técnicas Eletroquímicas , Contaminação de Alimentos , Microbiologia de Alimentos , Nanoestruturas , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Nanoestruturas/química , Microbiologia de Alimentos/métodos , Contaminação de Alimentos/análise , Doenças Transmitidas por Alimentos/microbiologia , Humanos , Bactérias/isolamento & purificaçãoRESUMO
Sulfuric acid anodizing assisted by a hydrothermal sealing with inhibitors [Ce3+-Mo6+] was used to prevent pitting corrosion on spray-deposited hypereutectic Al-Si alloy (A390). An investigation concerning the evaluation of pitting corrosion resistance on the anodic oxide thin film with ions incorporated was carried out in NaCl solution using electrochemical measurements (i.e., potentiodynamic polarization and electrochemical impedance spectroscopy, EIS). The influence of Si phase morphology and size on the growth mechanism of an anodic oxide film was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results were then compared with those for its equivalent IM390 alloy (Al-17Si-4.5Cu-0.6Mg) produced through a conventional process ingot metallurgy, IM. The electrochemical findings indicate that sulfuric acid anodizing followed by a simple hot water sealing treatment was ineffective. In this manner, an intense attack was localized by pitting corrosion that occurred on the anodic oxide film in less than three days, as denoted by characteristic changes in the EIS spectra at the lowest frequencies. Improved results were achieved for Ce-Mo surface modification, which can provide better corrosion resistance on the aluminum alloys because no signs of pits were observed during the corrosion testing.
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Foodborne diseases remain a worldwide concern, despite the advances made in sanitation, pathogen surveillance and food safety management systems. The methods routinely applied for detecting pathogens in foods are time consuming, labor intensive and usually require trained and qualified individuals. The objective of this review was to highlight the use of biosensors, with a focus on the electrochemical devices, as promising alternatives for detecting foodborne pathogens. These biosensors present high speed for obtaining results, with the possibility of evaluating foods in real time, at low cost, ease of use, in addition to being compact and portable. These aspects are considered advantageous and suitable for use in food safety management systems. This work also shows some limitations for the application of biosensors, and we present perspectives with the development and use of nanomaterials.
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Técnicas Biossensoriais , Técnicas Eletroquímicas , Microbiologia de Alimentos , Inocuidade dos Alimentos , Doenças Transmitidas por Alimentos , Técnicas Biossensoriais/instrumentação , Técnicas Biossensoriais/métodos , Inocuidade dos Alimentos/métodos , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Doenças Transmitidas por Alimentos/microbiologia , Doenças Transmitidas por Alimentos/prevenção & controle , Humanos , Microbiologia de Alimentos/métodos , Microbiologia de Alimentos/instrumentação , Bactérias/isolamento & purificação , Bactérias/classificação , Bactérias/genéticaRESUMO
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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Here, we report the preparation and evaluation of PVA/PEDOT:PSS-conducting hydrogels working as channel materials for OECT applications, focusing on the understanding of their charge transport and transfer properties. Our conducting hydrogels are based on crosslinked PVA with PEDOT:PSS interacting via hydrogen bonding and exhibit an excellent swelling ratio of ~180-200% w/w. Our electrochemical impedance studies indicate that the charge transport and transfer processes at the channel material based on conducting hydrogels are not trivial compared to conducting polymeric films. The most relevant feature is that the ionic transport through the swollen hydrogel is clearly different from the transport through the solution, and the charge transfer and diffusion processes govern the low-frequency regime. In addition, we have performed in operando Raman spectroscopy analyses in the OECT devices supported by first-principle computational simulations corroborating the doping/de-doping processes under different applied gate voltages. The maximum transconductance (gm~1.05 µS) and maximum volumetric capacitance (C*~2.3 F.cm-3) values indicate that these conducting hydrogels can be promising candidates as channel materials for OECT devices.
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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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Lung cancer is the leading cause of cancer death in both men and women. It represents a public health problem that must be addressed through the early detection of specific biomarkers and effective treatment. To address this critical issue, it is imperative to implement effective methodologies for specific biomarker detection of lung cancer in real clinical samples. Electrochemical methods, including microfluidic devices and biosensors, can obtain robust results that reduce time, cost, and assay complexity. This comprehensive review will explore specific studies, methodologies, and detection limits and contribute to the depth of the discussion, making it a valuable resource for researchers and clinicians interested in lung cancer diagnosis.
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This study investigates the tribocorrosion performance of a cast Co-Cr-Mo alloy prepared using casting and electromagnetic stirring (EMS) at specific frequencies. The tribocorrosion behaviour of the alloy was evaluated when exposed to Ringer's lactate solution to optimize the EMS parameters and improve its properties. The research focuses on biomedical implant applications and explores how EMS affects alloy wear and corrosion resistance. As did the friction coefficient and wear volume, the wear rate of samples produced with EMS frequencies of 75 Hz and 150 Hz decreased. These improvements are attributed to the ability of EMS to refine grain size and homogenize the microstructure, thereby increasing the resistance to tribocorrosion. Techniques such as scanning electron microscopy (SEM) and profilometry were used for surface and wear analysis, while mechanical properties were evaluated through instrumented indentation tests. The findings confirm that EMS improves the alloy's durability and tribocorrosion resistance, making it highly suitable for demanding biomedical applications such as joint replacements. This highlights the importance of advanced manufacturing techniques in optimizing biomedical alloys for simulated body conditions.
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Staphylococcus aureus is an important pathogen that causes nosocomial infections, resulting in unacceptable morbidity and mortality rates. In this work, we proposed the construction of a nanostructured ZnO-based electrochemical immunosensor for qualitative and semiquantitative detection of S. aureus using simple methods for growing zinc oxide nanorods (ZnO NRs) on a sensor board and immobilizing the anti-S. aureus antibody on ZnO NRs through cystamine and glutaraldehyde. The immunosensor detected S. aureus in the 103-107 colony-forming unit (CFU) mL-1 range and showed a limit of detection (LoD) around 0.792 × 103 CFU mL-1. Beyond a satisfactory LoD, the developed immunosensor presented other advantages, such as high versatility for point-of-care assays and a suitable selective factor that admits the detection of the S. aureus concentration range in human hand skin after washing. Moreover, the immunosensor showed the potential to be an excellent device to control nosocomial infection by detecting the presence of S. aureus in human hand skin.
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Técnicas Biossensoriais , Infecção Hospitalar , Técnicas Eletroquímicas , Sistemas Automatizados de Assistência Junto ao Leito , Pele , Staphylococcus aureus , Óxido de Zinco , Humanos , Staphylococcus aureus/isolamento & purificação , Infecção Hospitalar/prevenção & controle , Pele/microbiologia , Técnicas Biossensoriais/métodos , Óxido de Zinco/química , Imunoensaio/métodos , Técnicas Eletroquímicas/métodos , Infecções Estafilocócicas/diagnóstico , Infecções Estafilocócicas/microbiologia , Mãos/microbiologia , Limite de Detecção , Nanotubos/química , Anticorpos Imobilizados/químicaRESUMO
Dietary supplements are drastically growing as a category of consumer products all over the world. The abuse of supplements marketed for slimming purposes and physical fitness has been observed worldwide in recent years, which raises concerns in terms of public health. In this study, different types of dietary supplements marketed and delivered through the e-commerce were studied for the determination of thallium as a hazardous inorganic contaminant. The total content of thallium was determined by a sensitive voltammetric method after a microwave-assisted oxidative digestion of the sample. In addition, a comparative spectrometric method was applied for validation of the results in the samples. The maximum concentration found for thallium was found to be 2.89 mg kg-1, which well agree with the comparative measurement. Considering the 32 studied formulations, it can be pointed out that â¼24% of the of dietary supplements presented Tl concentrations at concentrations higher than 1 mg kg-1. The results permitted the assessment of the health risk related to thallium from contaminated samples, based on the calculation of the estimated daily intake (EDI) and the risk quotient (HQ). The highest daily intake of thallium was calculated as 82.0 µg day-1 in a protein-based supplement, which is equivalent to an EDI of 1.17 µg kg-1 day-1. This work highlights the need to develop regulations on the limits of toxic elements such as thallium in widely consumed dietary supplements, as well as an in-depth look at the adverse effects caused by this element in the human body.
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Suplementos Nutricionais , Contaminação de Alimentos , Tálio , Redução de Peso , Tálio/análise , Suplementos Nutricionais/análise , Humanos , Contaminação de Alimentos/análiseRESUMO
The native berries of South America present promising marketing opportunities owing to their high antioxidant content, notably rich in anthocyanin and phenolic compounds. However, Ecuador's endemic fruits, primarily found in the wild, lack comprehensive data regarding their phytochemical composition and antioxidant capacity, underscoring the need for research in this area. Accordingly, this study evaluated the total phenolic, anthocyanin, flavonoid, resveratrol, ascorbic acid, citric acid, sugars, and antioxidant content of three native Ecuadorian fruits: mora de monte (Rubus glabratus Kunth), mortiño (Vaccinium floribundum Kunth), and tuna de monte (Opuntia soederstromiana). Determination of resveratrol, ascorbic acid, citric acid, and sugars was determined by HPLC analysis, and UPLC analysis was used to determine tentative metabolites with nutraceutical properties. Antioxidant capacity was assessed using cyclic voltammetry and the DPPH method; differential pulse voltammetry was used to evaluate antioxidant power. Analysis of results through UPLC-QTOF mass spectrometry indicated that R. glabratus Kunth and V. floribundum Kunth are important sources of various compounds with potential health-promoting functions in the body. The DPPH results showed the following antioxidant capacities for the three fruits: R. glabratus Kunth > O. soederstromiana > V. floribundum Kunth; this trend was consistent with the antioxidant capacity results determined using the electrochemical methods.
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Lysergic acid diethylamide (LSD) and two phenethylamine classes (NBOHs and NBOMes) are the main illicit drugs found in seized blotter papers. The preliminary identification of these substances is of great interest for forensic analysis. In this context, this work constitutes the inaugural demonstration of an efficient methodology for the selective detection of LSD, NBOHs, and NBOMes, utilizing a fully 3D-printed electrochemical double cell (3D-EDC). This novel 3D-EDC enables the use of two working electrodes and/or two supporting electrolytes (at different pHs) in the same detection system, with the possibility of shared or individual auxiliary and pseudo-reference electrodes. Thus, the selective voltammetric detection of these substances is proposed using two elegant strategies: (i) utilizing the same 3D-EDC platform with two working electrodes (boron-doped diamond (BDD) and 3D-printed graphite), and (ii) employing two pH levels (4.0 and 12.0) with 3D-printed graphite electrode. This comprehensive framework facilitates a fast, robust, and uncomplicated electrochemical analysis. Moreover, this configuration enables a rapid and sensitive detection of LSD, NBOHs, and NBOMes in seized samples, and can also provide quantitative analysis. The proposed method showed good stability of the electrochemical response with RSD <9 % for Ip and <5 % for Ep, evaluating all oxidation processes observed for studied analytes (n = 7) at two pH levels, using the same and different (n = 3) working electrodes. It demonstrates a broad linear range (20-100 and 20-70 µmol L-1) and a low LOD (1.0 µmol L-1) for quantification of a model molecule (LSD) at the two pHs studied. Hence, the 3D-EDC combined with voltammetric techniques using BDD and 3D-printed graphite electrodes on the same platform, or only with this last sensor at two pH values, provide a practical and robust avenue for preliminary identification of NBOHs, NBOMes, and LSD. This method embodies ease, swiftness, cost-efficiency, robustness, and selectivity as an on-site screening tool for forensic analysis.