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1.
Mikrochim Acta ; 191(9): 535, 2024 08 14.
Article in English | MEDLINE | ID: mdl-39141139

ABSTRACT

Photoelectrochemical (PEC) nanobiosensors integrate molecular (bio)recognition elements with semiconductor/plasmonic photoactive nanomaterials to produce measurable signals after light-induced reactions. Recent advancements in PEC nanobiosensors, using light-matter interactions, have significantly improved sensitivity, specificity, and signal-to-noise ratio in detecting (bio)analytes. Tunable nanomaterials activated by a wide spectral radiation window coupled to electrochemical transduction platforms have further improved detection by stabilizing and amplifying electrical signals. This work reviews PEC biosensors based on nanomaterials like metal oxides, carbon nitrides, quantum dots, and transition metal chalcogenides (TMCs), showing their superior optoelectronic properties and analytical performance for the detection of clinically relevant biomarkers. Furthermore, it highlights the innovative role of red light and NIR-activated PEC nanobiosensors in enhancing charge transfer processes, protecting them from biomolecule photodamage in vitro and in vivo applications. Overall, advances in PEC detection systems have the potential to revolutionize rapid and accurate measurements in clinical diagnostic applications. Their integration into miniaturized devices also supports the development of portable, easy-to-use diagnostic tools, facilitating point-of-care (POC) testing solutions and real-time monitoring.


Subject(s)
Biosensing Techniques , Electrochemical Techniques , Infrared Rays , Biosensing Techniques/methods , Electrochemical Techniques/methods , Electrochemical Techniques/instrumentation , Humans , Nanostructures/chemistry , Quantum Dots/chemistry , Quantum Dots/radiation effects , Animals , Photochemical Processes , Biomarkers/analysis
2.
Bioelectrochemistry ; 160: 108795, 2024 Dec.
Article in English | MEDLINE | ID: mdl-39146929

ABSTRACT

E6 and E7 oncogenes are pivotal in the carcinogenic transformation in HPV infections and efficient diagnostic methods can ensure the detection and differentiation of HPV genotype. This study describes the development and validation of an electrochemical, label-free genosensor coupled with a microfluidic system for detecting the E6 and E7 oncogenes in cervical scraping samples. The nanostructuring employed was based on a cysteine and graphene quantum dots layer that provides functional groups, surface area, and interesting electrochemical properties. Biorecognition tests with cervical scraping samples showed differentiation in the voltammetric response. Low-risk HPV exhibited a lower biorecognition response, reflected in ΔI% values of 82.33 % ± 0.29 for HPV06 and 80.65 % ± 0.68 for HPV11 at a dilution of 1:100. Meanwhile, high-risk, HPV16 and HPV18, demonstrated ΔI% values of 96.65 % ± 1.27 and 93 % ± 0.026, respectively, at the same dilution. Therefore, the biorecognition intensity followed the order: HPV16 >HPV18 >HPV06 >HPV11. The limit of detection and the limit of quantification of E6E7 microfluidic LOC-Genosensor was 26 fM, and 79.6 fM. Consequently, the E6E7 biosensor is a valuable alternative for clinical HPV diagnosis, capable of detecting the potential for oncogenic progression even in the early stages of infection.


Subject(s)
Biosensing Techniques , Oncogene Proteins, Viral , Biosensing Techniques/methods , Humans , Oncogene Proteins, Viral/genetics , Female , Limit of Detection , Papillomavirus E7 Proteins/genetics , Cervix Uteri/virology , Graphite/chemistry , Papillomavirus Infections/diagnosis , Papillomavirus Infections/virology , Electrochemical Techniques/methods , Repressor Proteins/genetics , Microfluidic Analytical Techniques/methods , Microfluidic Analytical Techniques/instrumentation , Quantum Dots/chemistry , Lab-On-A-Chip Devices , Papillomaviridae/genetics , Papillomaviridae/isolation & purification
3.
STAR Protoc ; 5(3): 103259, 2024 Sep 20.
Article in English | MEDLINE | ID: mdl-39128006

ABSTRACT

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.


Subject(s)
Boron , Diamond , Electrochemical Techniques , Electrodes , Titanium , Titanium/chemistry , Boron/chemistry , Diamond/chemistry , Electrochemical Techniques/methods , Electrochemical Techniques/instrumentation , Photochemical Processes , Electrophoresis/methods
4.
Appl Spectrosc ; 78(9): 912-921, 2024 Sep.
Article in English | MEDLINE | ID: mdl-39090839

ABSTRACT

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.


Subject(s)
Malus , Paraquat , Spectrum Analysis, Raman , Spectrum Analysis, Raman/methods , Paraquat/analysis , Malus/chemistry , Herbicides/analysis , Brassica/chemistry , Electrochemical Techniques/methods , Food Contamination/analysis , Pesticides/analysis
5.
Anal Methods ; 16(28): 4827-4834, 2024 Jul 18.
Article in English | MEDLINE | ID: mdl-38967314

ABSTRACT

A cloud point method was developed and applied for the first time to extract and preconcentrate thiabendazole (TBZ) from commercial whole grape juice samples, with determination by high performance liquid chromatography coupled to electrochemical detection (HPLC/EC), using a cathodically pretreated boron-doped diamond electrode (BDD). The best conditions for extraction and preconcentration of TBZ by cloud point extraction (CPE) were performed at pH 6.0, by adding 1 mL of the surfactant Tergitol TMN-6 at 10% (mass-to-mass ratio), without heating (at 27 °C) and ultrasonic stirring time of (20 kHz) for 60 min. The HPLC/EC determination was duly validated in a C8 column, in mobile phase with a 69 : 31 ratio (V/V) of phosphate buffer (pH 7.0):ACN, at a flow rate of 1.2 mL min-1 and electrochemical detection with BDD electrode by applying 1.40 V × Ag/AgCl (3.0 mol L-1). Under these conditions, the procedure showed a preconcentration factor (FC) of 21.7, and limits of detection (LOD) and quantification (LOQ) of 6.64 × 10-9 mol L-1 (or 1.33 µg L-1) and 1.66 × 10-8 mol L-1 (or 3.34 µg L-1), respectively. The method provided a percent recovery of 81% to 98%, with a coefficient of variation between 3% and 15%.


Subject(s)
Electrochemical Techniques , Fruit and Vegetable Juices , Thiabendazole , Vitis , Chromatography, High Pressure Liquid/methods , Thiabendazole/analysis , Thiabendazole/isolation & purification , Fruit and Vegetable Juices/analysis , Vitis/chemistry , Electrochemical Techniques/methods , Limit of Detection , Electrodes , Pesticides/analysis , Food Contamination/analysis
6.
Int J Mol Sci ; 25(13)2024 Jun 27.
Article in English | MEDLINE | ID: mdl-39000155

ABSTRACT

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.


Subject(s)
Cobalt , Ferric Compounds , Hydrogen , Ionic Liquids , Nanocomposites , Nanotubes, Carbon , Oxides , Cobalt/chemistry , Nanotubes, Carbon/chemistry , Ionic Liquids/chemistry , Nanocomposites/chemistry , Catalysis , Hydrogen/chemistry , Ferric Compounds/chemistry , Oxides/chemistry , Electrodes , Electrochemical Techniques/methods , X-Ray Diffraction , Spectrum Analysis, Raman
7.
Mikrochim Acta ; 191(8): 492, 2024 07 27.
Article in English | MEDLINE | ID: mdl-39066907

ABSTRACT

The development and application of an electrochemical sensor is reported for detection of poly(3-hydroxybutyrate) (P3HB) - a bioplastic derived from agro-industrial residues. To overcome the challenges of molecular imprinting of macromolecules such as P3HB, this study employed methanolysis reaction to break down the P3HB biopolymer chains into methyl 3-hydroxybutyrate (M3HB) monomers. Thereafter, M3HB were employed as the target molecules in the construction of molecularly imprinted sensors. The electrochemical device was then prepared by electropolymerizing a molecularly imprinted poly (indole-3-acetic acid) thin film on a glassy carbon electrode surface modified with reduced graphene oxide (GCE/rGO-MIP) in the presence of M3HB. Electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), scanning electron microscopy with field emission gun (SEM-FEG), Raman spectroscopy, attenuated total reflection Fourier-transform infrared (ATR-FTIR) and X-ray Photoelectron Spectroscopy (XPS) were employed to characterize the electrode surface. Under ideal conditions, the MIP sensor exhibited a wide linear working range of 0.1 - 10 nM and a detection limit of 0.3 pM (n = 3). The sensor showed good repeatability, selectivity, and stability over time. For the sensor application, the bioproduction of P3HB was carried out in a bioreactor containing the Burkholderia glumae MA13 strain and sugarcane byproducts as a supplementary carbon source. The analyses were validated through recovery assays, yielding recovery values between 102 and 104%. These results indicate that this MIP sensor can present advantages in the monitoring of P3HB during the bioconversion process.


Subject(s)
Burkholderia , Electrochemical Techniques , Electrodes , Graphite , Hydroxybutyrates , Molecularly Imprinted Polymers , Polyesters , Graphite/chemistry , Polyesters/chemistry , Hydroxybutyrates/chemistry , Burkholderia/chemistry , Burkholderia/metabolism , Electrochemical Techniques/methods , Electrochemical Techniques/instrumentation , Molecularly Imprinted Polymers/chemistry , Limit of Detection , Oxidation-Reduction , Polyhydroxybutyrates
8.
Chemosphere ; 363: 142771, 2024 Sep.
Article in English | MEDLINE | ID: mdl-38969219

ABSTRACT

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.


Subject(s)
Diazepam , Electrochemical Techniques , Nanotubes, Carbon , Nitrophenols , Wearable Electronic Devices , Nanotubes, Carbon/chemistry , Nitrophenols/analysis , Electrochemical Techniques/instrumentation , Electrochemical Techniques/methods , Diazepam/analysis , Electrodes , Humans , Limit of Detection , Explosive Agents/analysis , Polymers/chemistry , Picrates
9.
Chemosphere ; 363: 142825, 2024 Sep.
Article in English | MEDLINE | ID: mdl-38996982

ABSTRACT

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 •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 •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.


Subject(s)
Azo Compounds , Boron , Coloring Agents , Diamond , Electrodes , Oxidation-Reduction , Water Pollutants, Chemical , Coloring Agents/chemistry , Water Pollutants, Chemical/chemistry , Boron/chemistry , Azo Compounds/chemistry , Diamond/chemistry , Hydrogen Peroxide/chemistry , Tanning , Electrochemical Techniques , Photolysis , Ultraviolet Rays , Waste Disposal, Fluid/methods , Iron/chemistry
10.
Anal Biochem ; 693: 115600, 2024 Oct.
Article in English | MEDLINE | ID: mdl-38964698

ABSTRACT

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.


Subject(s)
Biosensing Techniques , Electrochemical Techniques , Food Contamination , Food Microbiology , Nanostructures , Biosensing Techniques/methods , Electrochemical Techniques/methods , Nanostructures/chemistry , Food Microbiology/methods , Food Contamination/analysis , Foodborne Diseases/microbiology , Humans , Bacteria/isolation & purification
11.
Talanta ; 278: 126467, 2024 Oct 01.
Article in English | MEDLINE | ID: mdl-38968657

ABSTRACT

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.


Subject(s)
Biosensing Techniques , Electrochemical Techniques , Biosensing Techniques/methods , Humans , Electrochemical Techniques/methods , CRISPR-Cas Systems/genetics , Point-of-Care Testing , Point-of-Care Systems
12.
Talanta ; 278: 126513, 2024 Oct 01.
Article in English | MEDLINE | ID: mdl-38970965

ABSTRACT

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.


Subject(s)
Electrochemical Techniques , Kaempferols , Oxidation-Reduction , Kaempferols/chemistry , Kaempferols/analysis , Electrochemical Techniques/methods , Glycosylation , Electrodes , Bauhinia/chemistry , Quantum Theory , Flavonoids/chemistry , Flavonoids/analysis , Limit of Detection , Diamond/chemistry
13.
Sensors (Basel) ; 24(12)2024 Jun 10.
Article in English | MEDLINE | ID: mdl-38931556

ABSTRACT

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.


Subject(s)
Biosensing Techniques , COVID-19 , Dielectric Spectroscopy , Gold , SARS-CoV-2 , COVID-19/diagnosis , COVID-19/virology , Biosensing Techniques/methods , Biosensing Techniques/instrumentation , Humans , SARS-CoV-2/isolation & purification , SARS-CoV-2/immunology , Dielectric Spectroscopy/instrumentation , Dielectric Spectroscopy/methods , Gold/chemistry , Electrodes , Electrochemical Techniques/methods , Electrochemical Techniques/instrumentation , Immunoassay/methods , Immunoassay/instrumentation , Coronavirus Nucleocapsid Proteins/immunology , Coronavirus Nucleocapsid Proteins/analysis , Carbon/chemistry , Phosphoproteins/analysis
14.
Biosensors (Basel) ; 14(6)2024 Jun 10.
Article in English | MEDLINE | ID: mdl-38920608

ABSTRACT

Agricultural products are vitally important for sustaining life on earth and their production has notably grown over the years worldwide in general and in Brazil particularly. Elevating agricultural practices consequently leads to a proportionate increase in the usage of pesticides that are crucially important for enhanced crop yield and protection. These compounds have been employed excessively in alarming concentrations, causing the contamination of soil, water, and air. Additionally, they pose serious threats to human health. The current study introduces an innovative tool for producing appropriate materials coupled with an electrochemical sensor designed to measure carbendazim levels. The sensor is developed using a molecularly imprinted polymer (MIP) mounted on a glassy carbon electrode. This electrode is equipped with multi-walled carbon nanotubes (MWCNTs) for improved performance. The combined system demonstrates promising potential for accurately quantifying carbendazim. The morphological characteristics of the synthesized materials were investigated using field emission scanning electron microscopy (FESEM) and the Fourier-transform infrared (FTIR) technique. The analytical curve was drawn using the electrochemical method in the range of 2 to 20 ppm while for HPLC 2-12 ppm; the results are presented as the maximum adsorption capacity of the MIP (82.4%) when compared with NIP (41%) using the HPLC method. The analysis conducted using differential pulse voltammetry (DPV) yielded a limit of detection (LOD) of 1.0 ppm and a repeatability of 5.08% (n = 10). The results obtained from the analysis of selectivity demonstrated that the proposed electrochemical sensor is remarkably efficient for the quantitative assessment of carbendazim, even in the presence of another interferent. The sensor was successfully tested for river water samples for carbendazim detection, and recovery rates ranging from 94 to 101% were obtained for HPLC and 94 to 104% for the electrochemical method. The results obtained show that the proposed electrochemical technique is viable for the application and quantitative determination of carbendazim in any medium.


Subject(s)
Benzimidazoles , Carbamates , Electrochemical Techniques , Nanotubes, Carbon , Pesticides , Carbamates/analysis , Benzimidazoles/analysis , Pesticides/analysis , Nanotubes, Carbon/chemistry , Biosensing Techniques , Electrodes , Biomimetic Materials/chemistry , Limit of Detection
15.
Biosensors (Basel) ; 14(6)2024 May 29.
Article in English | MEDLINE | ID: mdl-38920582

ABSTRACT

Glucosamine-chitosan synthesized by the Maillard reaction was combined with montmorillonite to obtain a nanohybrid composite to immobilize horseradish peroxidase. The material combines the advantageous properties of clay with those of the chitosan derivative; has improved water solubility and reduced molecular weight and viscosity; involves an eco-friendly synthesis; and exhibits ion exchange capacity, good adhesiveness, and a large specific surface area for enzyme adsorption. The physicochemical characteristics of the composite were analyzed by infrared spectroscopy and X-ray diffraction to determine clay-polycation interactions. The electrochemical response of the different polyphenols to glassy carbon electrodes modified with the composite was evaluated by cyclic voltammetry. The sensitivity and detection limit values obtained with the biosensor toward hydroquinone, chlorogenic acid, catechol, and resorcinol are (1.6 ± 0.2) × 102 µA mM-1 and (74 ± 8) nM; (1.2 ± 0.1) × 102 µA mM-1 and (26 ± 3) nM; (16 ± 2) µA mM-1 and (0.74 ± 0.09) µM; and (3.7± 0.3) µA mM-1 and (3.3 ± 0.2) µM, respectively. The biosensor was applied to quantify polyphenols in pennyroyal and lemon verbena extracts.


Subject(s)
Bentonite , Biosensing Techniques , Chitosan , Electrochemical Techniques , Enzymes, Immobilized , Glucosamine , Horseradish Peroxidase , Polyphenols , Bentonite/chemistry , Polyphenols/analysis , Chitosan/chemistry , Horseradish Peroxidase/chemistry , Enzymes, Immobilized/chemistry , Glucosamine/analysis , Electrodes
16.
Talanta ; 277: 126391, 2024 Sep 01.
Article in English | MEDLINE | ID: mdl-38861764

ABSTRACT

An edible Mushroom-Nafion modified glassy carbon electrode (M2N5-GCE) was prepared using a homogeneous mixture varying the concentrations of these, in addition to the origin of the mushroom (Shiitake, Lentinula edodes, M1 and Abrantes, Agariscus bisporus, M2) and applied to the As(III) determination by anodic stripping voltammetry. After choosing the optimal conditions in the preparation of the electrode, the second stage was to study the effects of various parameters such as supporting electrolyte, pH, accumulation potential, and time (Eacc, tacc). The optimum experimental conditions chosen were Britton Robinson buffer 0.01 mol L-1 pH:4.6; Eacc: -1.0 and tacc: 60 s obtaining a signal of oxidation of As(0) to As(III) about 0.08 V. Peak current was proportional to arsenic concentration over the 19.6-117.6 µg L-1 range, with a 3σ detection limit of 13.4 µg L-1. The method was validated using As(III) spiked tap water from the laboratory with satisfactory results (RE:3.0 %). Finally, the method was applied to the determination of As(III) in water samples from the Loa River (Northern Chile) in the presence of As(V) in a concentration >20 times higher (RE: 2.3 %).


Subject(s)
Agaricales , Arsenic , Carbon , Electrodes , Fluorocarbon Polymers , Fluorocarbon Polymers/chemistry , Carbon/chemistry , Arsenic/analysis , Arsenic/chemistry , Agaricales/chemistry , Electrochemical Techniques/methods , Limit of Detection , Hydrogen-Ion Concentration , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry , Electrochemistry
17.
Mikrochim Acta ; 191(7): 425, 2024 06 27.
Article in English | MEDLINE | ID: mdl-38926184

ABSTRACT

A solvothermal synthesis of ultrasmall cerium oxide nanoparticles (USCeOxNPs) with an average size of 0.73 ± 0.07 nm using deep eutectic solvent (DES) as a stabilizing medium at a temperature of 90 ºC is reported. Transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) were used to morphologically characterize the USCeOxNPs. These revealed approximately spherical shapes with emission lines characteristic of cerium. Selected area electron diffraction (SAED) was used to determine the crystalline structure of the cerium oxide nanoparticles (CeO2NPs), revealing the presence of crystalline cubic structures. The USCeOxNPs-DES/CB film was characterized by scanning electron microscopy (SEM), which demonstrated the spherical characteristic of CB with layers slightly covered by DES residues. DES was characterized by Fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR), indicating its formation through hydrogen bonds between the precursors. An electrochemical sensor for dopamine (DA) determination in biological fluids was developed using the USCeOxNPs together with carbon black (CB). An enhanced current response was observed on DA voltammetric determination, and this can be attributed to the USCeOxNPs. This sensor displayed linear responses for DA in the range 5.0 × 10-7 mol L-1 to 3.2 × 10-4 mol L-1, with a limit of detection of 80 nmol L-1. Besides detectability, excellent performances were verified for repeatability and anti-interference. The sensor based on USCeOxNPs synthesized in DES in a simpler and environmentally friendly way was successfully applied to determine DA in biological matrix.


Subject(s)
Cerium , Dopamine , Electrochemical Techniques , Cerium/chemistry , Dopamine/analysis , Dopamine/blood , Electrochemical Techniques/methods , Humans , Deep Eutectic Solvents/chemistry , Nanoparticles/chemistry , Limit of Detection , Metal Nanoparticles/chemistry , Particle Size
18.
Anal Methods ; 16(25): 4136-4142, 2024 Jun 27.
Article in English | MEDLINE | ID: mdl-38860551

ABSTRACT

The ivermectin (IVM), as a broad-spectrum antiparasitic drug, was widely prescribed to treat COVID-19 during the pandemic, despite lacking proven efficacy in combating this disease. Therefore, it is important to establish affordable devices in laboratories with minimal infrastructure. The laser engraving technology has been revolutionary in sensor manufacturing, primarily attributed to the diversity of substrates that can be employed and the freedom it provides in creating sensor models. In this work, electrochemical sensors based on graphene were developed using the laser engraving technology for IVM sensing. Through, the studies that used the techniques of cyclic voltammetry and differential pulse voltammetry, following parameter optimization, for the laser-induced graphene electrode demonstrated a mass transport governed by adsorption of the species and exhibited a linear working range of 10-100 (µmol L-1), a limit of detection (LOD) of 1.6 × 10-6 (mol L-1), a limit of quantification (LOQ) of 4.8 × 10-6 (mol L-1), and a sensitivity of 0.139 (µA µmol L-1). The developed method was successfully applied to direct analysis of pharmaceutical tablets, tap water (recovery of 94%) and synthetic urine samples (recovery between 97% and 113%). These results demonstrate the feasibility of the method for routine analyses involving environmental samples.


Subject(s)
Electrochemical Techniques , Graphite , Ivermectin , Lasers , Ivermectin/analysis , Ivermectin/chemistry , Electrochemical Techniques/methods , Electrochemical Techniques/instrumentation , Graphite/chemistry , Humans , Limit of Detection , Antiparasitic Agents/urine , Antiparasitic Agents/analysis , Antiparasitic Agents/chemistry , Electrodes , COVID-19 , SARS-CoV-2
19.
Anal Methods ; 16(24): 4002-4009, 2024 Jun 20.
Article in English | MEDLINE | ID: mdl-38855859

ABSTRACT

This study presents the first insights into vinpocetine (VIN) behavior, a nootropic compound, on a glassy carbon electrode (GCE). Cyclic voltammetry (CV) revealed an irreversible oxidation peak at +1.0 V (vs. Ag/AgCl), with pH dependency indicating proton involvement in the electrochemical reaction. Density functional theory (DFT) optimized VIN's molecular geometry, while Fukui functions and dual descriptors elucidated its reactivity for a more straightforward exploration of the complete electrooxidation mechanism. Differential pulse voltammetry (DPV) demonstrated VIN sensing capabilities within a concentration range of 0.20 to 12.8 mg L-1, with a theoretical limit of detection (LOD) at 0.07 mg L-1, using optimized conditions of supporting electrolyte. The method showed selectivity in the presence of excipients and interfering species commonly found in pharmaceutical formulations. Recovery tests yielded 95.5% (n = 3), and quantification in pharmaceutical formulations showed no significant differences compared to the reference method based on HPLC DAD. This novel electroanalytical method holds promise for VIN nootropic sensing and routine pharmaceutical analysis.


Subject(s)
Electrochemical Techniques , Oxidation-Reduction , Vinca Alkaloids , Vinca Alkaloids/chemistry , Vinca Alkaloids/analysis , Electrochemical Techniques/methods , Electrodes , Limit of Detection
20.
Chemosphere ; 361: 142481, 2024 Aug.
Article in English | MEDLINE | ID: mdl-38823428

ABSTRACT

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.


Subject(s)
Anti-Bacterial Agents , Electrochemical Techniques , Metal Nanoparticles , Nanotubes, Carbon , Nitrofurazone , Nitrofurazone/analysis , Nitrofurazone/chemistry , Electrochemical Techniques/methods , Nanotubes, Carbon/chemistry , Metal Nanoparticles/chemistry , Anti-Bacterial Agents/analysis , Limit of Detection , Silver/chemistry , Electrodes , Quantum Dots/chemistry
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