RESUMEN

Growing demand for pesticides has created an environment prone to deceptive activities, where counterfeit or adulterated pesticide products infiltrate the market, often escaping rapid detection. This situation presents a significant challenge for sensor technology, crucial in identifying authentic pesticides and ensuring agricultural safety practices. Raman spectroscopy emerges as a powerful technique for detecting adulterants. Coupling the electrochemical techniques allows a more specific and selective detection and compound identification. In this study, we evaluate the efficacy of spectroelectrochemical measurements by coupling a potentiostat and Raman spectrograph to identify paraquat, a nonselective herbicide banned in several countries. Our findings demonstrate that applying -0.70 V during measurements yields highly selective Raman spectra, highlighting the primary vibrational bands of paraquat. Moreover, the selective Raman signal of paraquat was discernible in complex samples, including tap water, apple, and green cabbage, even in the presence of other pesticides such as diquat, acephate, and glyphosate. These results underscore the potential of this technique for reliable pesticide detection in diverse and complex matrices.

Asunto(s)

Malus , Paraquat , Espectrometría Raman , Espectrometría Raman/métodos , Paraquat/análisis , Malus/química , Herbicidas/análisis , Brassica/química , Técnicas Electroquímicas/métodos , Contaminación de Alimentos/análisis , Plaguicidas/análisis

RESUMEN

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.

Asunto(s)

Técnicas Biosensibles , COVID-19 , Espectroscopía Dieléctrica , Oro , SARS-CoV-2 , COVID-19/diagnóstico , COVID-19/virología , Técnicas Biosensibles/métodos , Técnicas Biosensibles/instrumentación , Humanos , SARS-CoV-2/aislamiento & purificación , SARS-CoV-2/inmunología , Espectroscopía Dieléctrica/instrumentación , Espectroscopía Dieléctrica/métodos , Oro/química , Electrodos , Técnicas Electroquímicas/métodos , Técnicas Electroquímicas/instrumentación , Inmunoensayo/métodos , Inmunoensayo/instrumentación , Proteínas de la Nucleocápside de Coronavirus/inmunología , Proteínas de la Nucleocápside de Coronavirus/análisis , Carbono/química , Fosfoproteínas/análisis

RESUMEN

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.

Asunto(s)

Antibacterianos , Técnicas Electroquímicas , Nanopartículas del Metal , Nanotubos de Carbono , Nitrofurazona , Nitrofurazona/análisis , Nitrofurazona/química , Técnicas Electroquímicas/métodos , Nanotubos de Carbono/química , Nanopartículas del Metal/química , Antibacterianos/análisis , Límite de Detección , Plata/química , Electrodos , Puntos Cuánticos/química

RESUMEN

A new type of buckypaper of MWCNT with entrapped Nimodipine (NMD) drug was constructed. NMD features a nitroaromatic group that is electroreducible, and a dihydropyridine ring that can be electrooxidized. From the perspective of the nitroaromatic group's reductive capability, we have devised amperometric and voltammetric analytical strategies, including both differential pulse and linear voltammetric techniques. These methods are implemented using glassy carbon electrodes (GCE) modified with buckypaper (BP) disks composed of multiwalled carbon nanotubes (MWCNT), which are capable of adsorbing NMD. Furthermore, by capitalizing on the oxidative capacity of the dihydropyridine ring, we have designed strategies that involve amperometry using screen-printed electrodes (SPE) modified with BP-MWCNT mini discs within a Batch Injection Analysis Cell (BIAS) designed for SPE. The developed sensor was applied successfully to determine the drug in commercial tablets. The analytical parameters of this sensor were adequate, with a recovery value of 98.24 % and detection and quantification limits of 7.01 mgL-1 and 23.35 mgL-1, respectively using the DPV method.

Asunto(s)

Nanotubos de Carbono , Nanotubos de Carbono/química , Nimodipina , Electrodos , Técnicas Electroquímicas , Límite de Detección

RESUMEN

Neglected tropical diseases are those caused by infectious agents or parasites and are considered endemic in low-income populations. These diseases also have unacceptable indicators and low investment in research, drug production, and control. Tropical diseases such as leishmaniasis are some of the main causes of morbidity and mortality around the globe. Electrochemical immunosensors are promising tools for diagnostics against these diseases. One such benefit is the possibility of assisting diagnosis in isolated regions, where laboratory infrastructure is lacking. In this work, different peptides were investigated to detect antibodies against Leishmania in human and canine serum samples. The peptides evaluated (395-KKG and 395-G) have the same recognition site but differ on their solid-binding domains, which ensure affinity to spontaneously bind to either graphene oxide (GO) or graphene quantum dots (GQD). Cyclic voltammetry and differential pulse voltammetry were employed to investigate the electrochemical behavior of each assembly step and the role of each solid-binding domain coupled to its anchoring material. The graphene affinity peptide (395-G) showed better reproducibility and selectivity when coupled to GQD. Under the optimized set of experimental conditions, negative and positive human serum samples responses were distinguished based on a cut-off value of 82.5% at a 95% confidence level. The immunosensor showed selective behavior to antibodies against Mycobacterium leprae and Mycobacterium tuberculosis, which are similar antibodies and potentially sources of false positive tests. Therefore, the use of the graphene affinity peptide as a recognition site achieved outstanding performance for the detection of Leishmania antibodies.

Asunto(s)

Técnicas Biosensibles , Grafito , Leishmaniasis , Animales , Perros , Humanos , Carbono/química , Grafito/química , Reproducibilidad de los Resultados , Inmunoensayo , Péptidos , Anticuerpos , Leishmaniasis/diagnóstico

RESUMEN

Fused deposition modeling (FDM) 3D printing is a promising additive manufacturing technique to produce low-cost disposable electrochemical devices. However, the print of devices like well-known screen-printed electrodes (all electrodes on the same device) is difficult using the available technology (few materials available for production of working electrodes). In this paper we present a procedure to produce disposable and robust electrochemical devices by FDM 3D printing that allows reproducible analysis of small volumes (50-2000 µL). The device consists of just two printed parts that allow easy coupling of different conductive materials for using as disposable or non-disposable working electrodes with reproducible geometric area. Printed counter and pseudo-reference electrodes can also be easily fitted into the microcell. Moreover, conventional counter (platinum wire) and mini reference electrodes can also be used. As a proof of concept, paracetamol, cocaine and uric acid were used as model analytes using different materials as working electrodes. Linear calibration curves (r > 0.99) with similar slopes (0.29 ± 0.01 µA µmol L-1; RSD = 3.4%) were obtained by square wave voltammetry (SWV) using a complete printed system and different volumes of standard solutions of paracetamol (50, 100, and 200 µL). For uric acid, a linear range of 10-125 µmol L-1 (r > 0.99), was obtained using differential pulse voltammetry as the electrochemical technique and a disposable laser-induced graphene base as the working electrode. With the coupling of boron-doped diamond working electrode, screening tests were successfully performed in seized cocaine samples with selective detection of cocaine in the presence of its most common adulterants. The production cost per unit of a complete electrochemical system is around US 5.00. In large-scale production, only the working electrode needs to be replaced while the microcell and counter/pseudo reference electrodes do not need to be discarded.

RESUMEN

This manuscript presents the design and facile production of screen-printed arrays (SPAs) for the internally validated determination of raised levels of serum procalcitonin (PCT). The screen-printing methodology produced SPAs with six individual working electrodes that exhibit an inter-array reproducibility of 3.64% and 5.51% for the electrochemically active surface area and heterogenous electrochemical rate constant respectively. The SPAs were modified with antibodies specific for the detection of PCT through a facile methodology, where each stage simply uses droplets incubated on the surface, allowing for their mass-production. This platform was used for the detection of PCT, achieving a linear dynamic range between 1 and 10 ng mL-1 with a sensor sensitivity of 1.35 × 10-10 NIC%/ng mL-1. The SPA produced an intra- and inter-day %RSD of 4.00 and 5.05%, with a material cost of £1.14. Internally validated human serum results (3 sample measurements, 3 control) for raised levels of PCT (>2 ng mL-1) were obtained, with no interference effects seen from CRP and IL-6. This SPA platform has the potential to offer clinicians vital information to rapidly begin treatment for "query sepsis" patients while awaiting results from more lengthy remote laboratory testing methods. Analytical ranges tested make this an ideal approach for rapid testing in specific patient populations (such as neonates or critically ill patients) in which PCT ranges are inherently wider. Due to the facile modification methods, we predict this could be used for various analytes on a single array, or the array increased further to maintain the internal validation of the system.

Asunto(s)

Técnicas Biosensibles , Sepsis , Recién Nacido , Humanos , Polipéptido alfa Relacionado con Calcitonina , Reproducibilidad de los Resultados , Sepsis/diagnóstico , Anticuerpos

RESUMEN

To help meet the global demand for reliable and inexpensive COVID-19 testing and environmental analysis of SARS-CoV-2, the present work reports the development and application of a highly efficient disposable electrochemical immunosensor for the detection of SARS-CoV-2 in clinical and environmental matrices. The sensor developed is composed of a screen-printed electrode (SPE) array which was constructed using conductive carbon ink printed on polyethylene terephthalate (PET) substrate made from disposable soft drink bottles. The recognition site (Spike S1 Antibody (anti-SP Ab)) was covalently immobilized on the working electrode surface, which was effectively modified with carbon black (CB) and gold nanoparticles (AuNPs). The immunosensing material was subjected to a multi-technique characterization analysis using X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) with elemental analysis via energy dispersive spectroscopy (EDS). The electrochemical characterization of the electrode surface and analytical measurements were performed using cyclic voltammetry (CV) and square-wave voltammetry (SWV). The immunosensor was easily applied for the conduct of rapid diagnoses or accurate quantitative environmental analyses by setting the incubation period to 10 min or 120 min. Under optimized conditions, the biosensor presented limits of detection (LODs) of 101 fg mL-1 and 46.2 fg mL-1 for 10 min and 120 min incubation periods, respectively; in addition, the sensor was successfully applied for SARS-CoV-2 detection and quantification in clinical and environmental samples. Considering the costs of all the raw materials required for manufacturing 200 units of the AuNP-CB/PET-SPE immunosensor, the production cost per unit is 0.29 USD.

RESUMEN

A poly(thiophene acetic acid)/Au/poly(methylene blue) nanostructured interface was electrochemically assembled step-by-step on screen-printed carbon electrodes (SPCE) for label-free detection of p53 protein. The initial electrical conductive properties of the polymeric interface were increased with an additional layer of poly(methylene blue) electropolymerized in the presence of gold nanoparticles. The nano-immunosensing architecture was prepared by covalent immobilization of anti-p53 antibodies as bioreceptors through the poly(thiophene acetic acid) moieties. The nano-immunosensor assembly was extensively characterized by ultraviolet-visible spectrophotometry, dynamic and electrophoretic light scattering, scanning electron microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, atomic force microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. Under optimal conditions, p53 was specifically and selectively detected by square wave voltammetry in a linear range between 1 and 100 ng mL-1 with a limit of detection of 0.65 ng mL-1. In addition, the electrochemical nano-immunosensor detected p53 in spiked human serum samples and colorectal cancer cell lysates, and the results were validated with a standard spectrophotometric method using a paired samples t test, which did not exhibit significant differences between both methods. The resultant p53 nano-immunosensor is simple to assemble, robust, and has the potential for point-of-care biomarker detection applications.

Asunto(s)

Ácido Acético , Nanopartículas del Metal , Humanos , Técnicas Electroquímicas/métodos , Oro/química , Nanopartículas del Metal/química , Azul de Metileno , Tiofenos

RESUMEN

A label-free nanoimmunosensor is reported based on p53/CeO2/PEDOT nanobiocomposite-decorated screen-printed gold electrodes (SPAuE) for the electrochemical detection of anti-p53 autoantibodies. CeO2 nanoparticles (NPs) were synthesized and stabilized with cyanopropyltriethoxysilane by a soft chemistry method. The nanoimmunosensing architecture was prepared by in situ electropolymerization of 3,4-ethylenedioxythiophene (EDOT) on SPAuE in the presence of CeO2 NPs. The CeO2 NPs and Ce/PEDOT/SPAuE were characterized by scanning and transmission electron microscopy, dynamic and electrophoretic light scattering, ultraviolet-visible spectrophotometry, X-ray diffraction, Fourier-transform infrared spectroscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. Ce/PEDOT/SPAuE was biofunctionalized with p53 antigen by covalent bonding for the label-free determination of anti-p53 autoantibodies by differential pulse voltammetry. The nanobiocomposite-based nanoimmunosensor detected anti-p53 autoantibodies in a linear range from 10 to 1000 pg mL-1, with a limit of detection (LOD) of 3.2 pg mL-1. The nanoimmunosensor offered high specificity, selectivity, and long-term storage stability with great potential to detect anti-p53 autoantibodies in serum samples. Overall, incorporating organo-functional nanoparticles into polymeric matrices can provide a simple-to-assemble, rapid, and ultrasensitive approach for on-site screening of anti-p53 autoantibodies and other disease-related biomarkers with low sample volumes.

Asunto(s)

Técnicas Biosensibles , Nanopartículas del Metal , Nanocompuestos , Autoanticuerpos , Técnicas Biosensibles/métodos , Compuestos Bicíclicos Heterocíclicos con Puentes , Cerio , Nanopartículas del Metal/química , Nanocompuestos/química , Polímeros

RESUMEN

Smart electronic devices based on micro-controllers, also referred to as fashion electronics, have raised wearable technology. These devices may process physiological information to facilitate the wearer's immediate biofeedback in close contact with the body surface. Standard market wearable devices detect observable features as gestures or skin conductivity. In contrast, the technology based on electrochemical biosensors requires a biomarker in close contact with both a biorecognition element and an electrode surface, where electron transfer phenomena occur. The noninvasiveness is pivotal for wearable technology; thus, one of the most common target tissues for real-time monitoring is the skin. Noninvasive biosensors formats may not be available for all analytes, such as several proteins and hormones, especially when devices are installed cutaneously to measure in the sweat. Processes like cutaneous transcytosis, the paracellular cell-cell unions, or even reuptake highly regulate the solutes content of the sweat. This review discusses recent advances on wearable devices based on electrochemical biosensors for biomarkers with a complex blood-to-sweat partition like proteins and some hormones, considering the commented release regulation mechanisms to the sweat. It highlights the challenges of wearable epidermal biosensors (WEBs) design and the possible solutions. Finally, it charts the path of future developments in the WEBs arena in converging/emerging digital technologies.

Asunto(s)

Técnicas Biosensibles , Dispositivos Electrónicos Vestibles , Biomarcadores/análisis , Hormonas/análisis , Sudor/química

RESUMEN

Monitoring the concentration of antibiotics in body fluids is essential to optimizing the therapy and minimizing the risk of bacteria resistance, which can be made with electrochemical sensors tailored with appropriate materials. In this paper, we report on sensors made with screen-printed electrodes (SPE) coated with fullerene (C60), reduced graphene oxide (rGO) and Nafion (NF) (C60-rGO-NF/SPE) to determine the antibiotic metronidazole (MTZ). Under optimized conditions, the C60-rGO-NF/SPE sensor exhibited a linear response in square wave voltammetry for MTZ concentrations from 2.5 × 10-7 to 34 × 10-6 mol/L, with a detection limit of 2.1 × 10-7 mol/L. This sensor was also capable of detecting MTZ in serum and urine, with recovery between 94% and 100%, which are similar to those of the standard chromatographic method (HPLC-UV). Because the C60-rGO-NF/SPE sensor is amenable to mass production and allows for MTZ determination with simple principles of detection, it fulfills the requirements of therapeutic drug monitoring programs.

RESUMEN

Multiplex detection of emerging pollutants is essential to improve quality control of water treatment plants, which requires portable systems capable of real-time monitoring. In this paper we describe a flexible, dual electrochemical sensing device that detects nonylphenol and paroxetine in tap water samples. The platform contains two voltammetric sensors, with different working electrodes that were either pretreated or functionalized. Each working electrode was judiciously tailored to cover the concentration range of interest for nonylphenol and paroxetine, and square wave voltammetry was used for detection. An electrochemical pretreatment with sulfuric acid on the printed electrode enabled a selective detection of nonylphenol in 1.0-10 × 10-6 mol L-1 range with a limit of detection of 8.0 × 10-7 mol L-1. Paroxetine was detected in the same range with a limit of detection of 6.7 × 10-7 mol L-1 using the printed electrode coated with a layer of carbon spherical shells. Simultaneous detection of the two analytes was achieved in tap water samples within 1 min, with no fouling and no interference effects. The long-term monitoring capability of the dual sensor was demonstrated in phosphate buffer for 45 days. This performance is statistically equivalent to that of high-performance liquid chromatography (HPLC) for water analysis. The dual-sensor platform is generic and may be extended to other water pollutants and clinical biomarkers in real-time monitoring of the environment and health conditions. Silver pseudo-reference electrodes for paroxetine (REP) and nonylphenol (REN), working electrodes for paroxetine (WP) and nonylphenol (WN), and auxiliary electrode (AE). USP refers to the University of Sao Paulo. "Red" is reduced form and "Oxi" is oxidized form of analytes.

RESUMEN

Human immunodeficiency virus (HIV) is still considered a pandemic, and the detection of p24-HIV protein has an important role in the early diagnosis of HIV in adults and newborns. The accessibility of these trials depends on the price and execution difficulty of the method, which can be reduced using electrochemical methods by using enzymeless approaches, disposable and accurate devices. In this work, graphene quantum dots were acquired by a simple synthesis and employed as an electrochemical signal amplifier and support for the aptamer immobilization through a feasible and stable modification of disposable screen-printed electrodes. The device has been easily assembled and used to detect p24-HIV protein without the interference of similar proteins or sample matrix. Using the best set of experimental conditions, a linear correlation between analytical signal and log of p24-HIV concentration from 0.93 ng mL-1 to 93 µg mL-1 and a limit of detection of 51.7 pg mL-1 were observed. The developed device was applied to p24 determination in spiked human serum and provided distinct levels of signal for positive and negative samples, successfully identifying real samples with the target protein. This sensor is a step towards the development of point-of-care devices and the popularization of electrochemical methods for trials and diagnostics of relevant diseases.

Asunto(s)

Aptámeros de Nucleótidos , Técnicas Biosensibles , Grafito , Infecciones por VIH , Puntos Cuánticos , Adulto , Técnicas Electroquímicas , Electrodos , Infecciones por VIH/diagnóstico , Proteínas del Virus de la Inmunodeficiencia Humana , Humanos , Recién Nacido , Límite de Detección

RESUMEN

Currently, the detection of pathogens such as Escherichia coli through instrumental alternatives with fast response and excellent sensitivity and selectivity are being studied. Biosensors are systems consisting of nanomaterials and biomolecules that exhibit remarkable properties such as simplicity, portable, affordable, user­friendly, and deliverable to end­users. For this, in this work we report for the first time, to our knowledge, the bioinformatic design of a new peptide based on TIR protein, a receptor of Intimin membrane protein which is characteristic of E. coli. This peptide (named PEPTIR­1.0) was used as recognition element in a biosensor based on AuNPs­modified screen­printed electrodes for the detection of E. coli. The morphological and electrochemical characteristics of the biosensor obtained were studied. Results show that the biosensor can detect the bacteria with limits of detection and quantification of 2 and 6 CFU/mL, respectively. Moreover, the selectivity of the system is statistically significant towards the detection of the pathogen in the presence of other microorganisms such as P. aeruginosa and S. aureus. This makes this new PEPTIR­1.0 based biosensor can be used in the rapid, sensitive, and selective detection of E. coli in aqueous matrices.

Asunto(s)

Técnicas Biosensibles , Técnicas Electroquímicas , Escherichia coli O157/química , Proteínas de Escherichia coli/química , Péptidos/química , Receptores de Superficie Celular/química , Microbiología del Agua , Secuencia de Aminoácidos , Biología Computacional/métodos , Microbiología de Alimentos , Oro/química , Ligandos , Nanopartículas del Metal/química , Nanopartículas del Metal/ultraestructura , Modelos Moleculares , Péptidos/análisis , Conformación Proteica , Sensibilidad y Especificidad

RESUMEN

Breast cancer remains one of the leading causes of women death. The development of more sensitive diagnostic tests, which could present a faster response, lower cost, and could promote early diagnosis would increase the chances of survival. This study reports the development and optimization of an electrochemical aptasensor for the detection of HER2 protein, a breast cancer biomarker. Two sensing platforms were developed on gold screen-printed electrodes. The first platform is composed of self-assembled monolayer (SAM) made from mixture of thiolated DNA aptamers specific for HER2 and 1-mercapto-6-hexanol (MCH), while the second one is a ternary SAM composed of the same aptamer and 1,6-hexanethiol (HDT). Both platforms were further passivated with MCH and blocked with bovine serum albumin. The biosensors were characterized using electrochemical impedance spectroscopy to detect the target protein from 1 pg/mL to 1 µg/mL in phosphate buffered saline, diluted and undiluted human serum through charge transfer resistance value. The ternary SAM architecture shows a reduction of non-specific attachment to the electrode surface due to the HDT antifouling properties. In addition, this platform exhibits 172 pg/mL as limit of detection and a sensitivity of 4.12% per decade for undiluted serum compared with SAM architecture with the 179 pg/mL and 4.32% per decade, respectively. Electrochemical aptasensors are highly promising for medical diagnostic and ternary layers could improve the limit of detection.

Asunto(s)

Aptámeros de Nucleótidos/química , Neoplasias de la Mama/diagnóstico , Técnicas Electroquímicas/instrumentación , Electrodos , Biomarcadores de Tumor , Técnicas Biosensibles/métodos , Neoplasias de la Mama/sangre , Femenino , Genes erbB-2 , Humanos , Límite de Detección

RESUMEN

The present work reports the development of a sensitive and selective method for ethinylestradiol detection using screen-printed electrode (SPE) modified with functionalized graphene (FG), graphene quantum dots (GQDs) and magnetic nanoparticles coated with molecularly imprinted polymers (mag@MIP). The performance of the mag@MIP sensor was compared with that of a non-molecularly imprinted sensor (mag@NIP). Chemical and physical characterizations of the mag@NIP and mag@MIP sensors were performed using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and Brunauer-Emmett-Teller (BET) techniques. The electrochemical behavior of the electrodes investigated, which included (mag@MIP)-GQDs-FG-NF/SPE, (mag@NIP)-GQDs-FG-NF/SPE, GQDs-FG-NF/SPE and FG-NF/SPE, was evaluated by cyclic voltammetry. The results obtained show a significant increase in peak current magnitude for (mag@MIP)-GQDs-FG-NF/SPE. Using square wave voltammetry experiments, the efficiency of the (mag@MIP)-GQDs-FG-NF/SPE sensor was also tested under optimized conditions. The linear response range obtained for ethinylestradiol concentration was 10 nmol L-1 to 2.5 µmol L-1, with limit of detection of 2.6 nmol L-1. The analytical signal of the (mag@MIP)-GQDs-FG-NF/SPE sensor suffered no interference from different compounds and the sensor exhibited good repeatability. The proposed sensor was successfully applied for ethynilestradiol detection in river water, serum and urine samples, where recovery rates between 96 to 105% and 97-104% were obtained for environmental and biological samples, respectively.

Asunto(s)

Grafito , Nanopartículas de Magnetita , Impresión Molecular , Puntos Cuánticos , Técnicas Electroquímicas , Electrodos , Etinilestradiol , Límite de Detección , Polímeros Impresos Molecularmente

RESUMEN

Detection and quantification of diverse analytes such as molecules, cells receptor and even particles and nanoparticles, play an important role in biomedical research, particularly in electrochemical sensing platform technologies. In this study, gold nanoparticles (AuNPs) prepared by green synthesis from Sargassum sp. were characterized using ultraviolet-visible (UV-Vis) and Fourier transform-infrared (FT-IR) spectroscopies, X-ray diffraction (XRD), scanning electron microscopy (SEM), dynamic light scattering (DLS) and zeta potential (ζ) obtaining organic capped face-centered cubic 80-100 nm AuNPs with an excellent stability in a wide range of pH. The AuNPs were used to modify a carbon nanotubes-screen printed electrode (CNT-SPE), through the drop-casting method, to assemble a novel portable electrochemical sensing platform for glucose, using a novel combination of components, which together have not been employed. The ability to sense and measure glucose was demonstrated, and its electrochemical fundamentals was studied using cyclic voltammetry (CV). The limits of detection (LOD) and quantification (LOQ) to glucose were 50 µM and 98 µM, respectively, and these were compared to those of other sensing platforms.

Asunto(s)

Electrodos , Nanopartículas del Metal , Nanotubos de Carbono , Sargassum/química , Oro , Tecnología Química Verde , Espectroscopía Infrarroja por Transformada de Fourier

RESUMEN

The need for agile and proper identification of drugs of abuse has encouraged the scientific community to improve and to develop new methodologies. The drug lysergic acid diethylamide (LSD) is still widely used due to its hallucinogenic effects. The use of voltammetric methods to analyze narcotics has increased in recent years, and the possibility of miniaturizing the electrochemical equipment allows these methods to be applied outside the laboratory; for example, in crime scenes. In addition to portability, the search for affordable and sustainable materials for use in electroanalytical research has grown in recent decades. In this context, employing paper substrate, graphite pencil, and silver paint to construct paper-based electrodes is a great alternative. Here, a paper-based device comprising three electrodes was drawn on 300 g/m2 watercolor paper with 8B pencils, and its efficiency was compared to the efficiency of a commercially available screen-printed carbon electrode. Square wave voltammetry was used for LSD analysis in aqueous medium containing 0.05 mol/L LiClO4 . The limits of detection and quantification were 0.38 and 1.27 µmol/L, respectively. Both electrodes exhibited a similar voltammetric response, which was also confirmed during analysis of a seized LSD sample, with recovery of less than 10%. The seized samples were previously analyzed by GCMS technique, employing the full scan spectra against the software spectral library. The electrode selectivity was also tested against 3,4-methylenedioxymethamphetamine (MDMA) and methamphetamine. It was possible to differentiate these compounds from LSD, indicating that the developed paper-based device has potential application in forensic chemistry analyses.

Asunto(s)

Electroquímica/instrumentación , Electrodos , Alucinógenos/análisis , Dietilamida del Ácido Lisérgico/análisis , Papel , Toxicología Forense/instrumentación , Humanos , Límite de Detección , Metanfetamina/aislamiento & purificación , N-Metil-3,4-metilenodioxianfetamina/aislamiento & purificación

RESUMEN

Electrochemical immunosensors have been developed to determine the carbohydrate antigen 19-9 (CA19-9). They are based on screen-printed carbon electrodes (SPCEs) coated with layer-by-layer (LbL) films of carbon black (CB) and polyelectrolytes. Owing to a suitable choice of LbL film architecture, the procedures for immobilization of anti-CA19-9 antibodies on the electrode surfaces were straightforward. Mechanically flexible immunosensors were capable of detecting CA19-9 within a dynamic range of 0.01 to 40 U mL-1 and a limit of detection of 0.07 U mL-1 using differential pulse voltammetry. In addition to detecting CA19-9 at clinically relevant concentrations for pancreatic cancer in standard solutions, the immunosensors provide the determination of CA19-9 on cell lysate and human serum samples. Using LbL films led to immunosensors with superior performance compared to similar systems obtained by drop casting. The fabrication of this relatively simple, inexpensive platform is a demonstration that SPCEs modified with cost-effective materials are able to detect cancer biomarkers and may be adapted to other disposable immunosensors. Graphical abstract Schematic representation of assembly and characterization of electrochemical immunosensors for the determination of carbohydrate antigen 19-9 based on printed electrodes modified with composites of carbon black and polyelectrolyte films.

Asunto(s)

Antígenos de Carbohidratos Asociados a Tumores/sangre , Biomarcadores de Tumor/sangre , Técnicas Electroquímicas/métodos , Inmunoensayo/métodos , Polielectrolitos/química , Hollín/química , Anticuerpos Inmovilizados/inmunología , Antígenos de Carbohidratos Asociados a Tumores/inmunología , Biomarcadores de Tumor/inmunología , Técnicas Electroquímicas/instrumentación , Electrodos , Humanos , Límite de Detección