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1.
Mikrochim Acta ; 191(4): 208, 2024 Mar 19.
Article in English | MEDLINE | ID: mdl-38499898

ABSTRACT

The identification and correction of negative factors, such as 4-ethylphenol and ethanethiol, is important to comply with food safety regulations and avoid economic losses to wineries. A simple amperometric measurement procedure that facilitates the simultaneous quantification of both compounds in the gas phase has been developed using fullerene and cobalt (II) phthalocyanine-modified dual screen-printed electrodes coated with a room temperature ionic liquid-based gel polymer electrolyte. The replacement of the typical aqueous supporting electrolyte by low-volatility ones improves both operational and storage lifetime. Under the optimum conditions of the experimental variables, Britton Robinson buffer pH 5 and applied potentials of + 0.86 V and + 0.40 V for each working electrode (vs. Ag ref. electrode), reproducibility values of 7.6% (n = 3) for 4-ethylphenol and 6.6% (n = 3) for ethanethiol were obtained, as well as capability of detection values of 23.8 µg/L and decision limits of 1.3 µg/L and 9.2 µg/L (α = ß = 0.05), respectively. These dual electrochemical devices have successfully been applied to the headspace detection of both compounds in white and red wines, showing their potential to be routinely used for rapid analysis control in wineries.

2.
Talanta ; 272: 125761, 2024 May 15.
Article in English | MEDLINE | ID: mdl-38364564

ABSTRACT

The biggest allure of heterogeneous electro-Fenton (HEF) processes largely fails on its high efficiency for the degradation of a plethora of hazardous compounds present in water, but still challenging to search for good and cost-effective electrocatalyst. In this work, carbon black (CB) and oxidised carbon black (CBox) materials were investigated as cathodes in the electrochemical production of hydrogen peroxide involved in HEF reaction for the degradation of 2-phenylphenol (2PP) as a target pollutant. The electrodes were fabricated by employing carbon cloth as support, and the highest H2O2 production yields were obtained for the CBox, pointing out the beneficial effect of the hydrophilic character of the electrode and oxygen-type functionalization of the carbonaceous surface. HEF degradation of 2PP was explored at -0.7 V vs. Ag/AgCl exhibiting the best conversion rates and degradation grade (total organic carbon) for the CBox-based cathode. In addition, the incorporation of an electrochemical sensor of 2PP in line with the HEF reactor was accomplished by the use of screen-printed electrodes (SPE) in order to monitor the pollutant degradation. The electrochemical sensor performance was evaluated from the oxidation of 2PP in the presence of Fe2+ ions by using square wave voltammetry (SWV) technique. The best electrochemical sensor performance was based on SPE modified with Meldola Blue showing a high sensitivity, low detection limit (0.12 ppm) and wide linear range (0.5-21 ppm) with good reproducibility (RSD 2.3 %). The all-in-one electrochemical station has been successfully tested for the degradation and quantification of 2PP, obtaining good recoveries analysing spiked waters from different water matrices origins.

3.
Mikrochim Acta ; 191(2): 112, 2024 01 29.
Article in English | MEDLINE | ID: mdl-38286966

ABSTRACT

For the first time, a tumour hypoxia marker detection has been developed using two-dimensional layered composite modified electrodes in biological and environmental samples. The concept of TaB2 and V4C3-based MXene composite materials is not reported hitherto using ball-milling and thermal methods and it remains the potentiality of the present work. The successful formation is confirmed through various characterisation techniques like X-ray crystallography, scanning electron microscopy photoelectron, and impedance spectroscopy. A reliable and repeatable electrochemical sensor based on TaB2@V4C3/SPCE was developed for quick and extremely sensitive detection of pimonidazole by various electroanalytical methods. It has been shown that the modified electrode intensifies the reduction peak current and causes a decrease in the potential for reduction, in comparison with the bare electrode. The proposed sensor for pimonidazole reduction has strong electrocatalytic activity and high sensitivity, as demonstrated by the cyclic voltammetry approach. Under the optimal experimental circumstances, differential pulse voltammetry techniques were utilised for generating the wide linear range (0.02 to 928.51 µM) with a detection limit of 0.0072 µM. The resultant data demonstrates that TaB2@V4C3/SPCE nano-sensor exhibits excellent stability, reliability, and repeatability in the determination of pimonidazole. Additionally, the suggested sensor was successfully used to determine the presence of pimonidazole in several real samples, such as human blood serum, urine, water, and drugs.


Subject(s)
Carbon , Nitroimidazoles , Tantalum , Humans , Carbon/chemistry , Vanadium , Reproducibility of Results , Limit of Detection , Electrodes , Boron Compounds
4.
Chemosphere ; 337: 139315, 2023 Oct.
Article in English | MEDLINE | ID: mdl-37392799

ABSTRACT

Since bisphenol A (BPA) and dimethyl bisphenol A (DM-BPA) are human endocrine disruptors (EDCs) with tiny potential differences (44 mV) and widespread applications, there is a lack of published reports on their simultaneous detection. Therefore, this study reports a novel electrochemical detection system capable of simultaneous direct detection of BPA and DM-BPA using screen-printed carbon electrodes (SPCE) as a sensing platform. To improve the electrochemical performance of the SPCE, the SPCE was modified by using a combination of Pt nanoparticles modified with single-walled carbon nanotubes (Pt@SWCNTs), MXene (Ti3C2), and graphene oxide (GO). In addition, the GO in Pt@SWCNTs-MXene-GO was reduced to reduced graphene oxide (rGO) by the action of electric field (-1.2 V), which significantly improved the electrochemical properties of the composites and effectively solved the problem of dispersion of the modified materials on the electrode surface. Under optimal experimental conditions, Pt@SWCNTs-Ti3C2-rGO/SPCE exhibited a suitable detection range (0.006-7.4 µmol L-1) and low detection limits (2.8 and 3 nmol L-1, S/N = 3) for the simultaneous detection of BPA (0.392 V vs. Ag/AgCl) and DM-BPA (0.436 V vs. Ag/AgCl)). Thus, this study provides new insights into detecting compounds with similar structures and slight potential differences. Finally, the developed sensor's reproducibility, stability, interference resistance and accuracy were demonstrated with satisfactory results.


Subject(s)
Graphite , Nanotubes, Carbon , Humans , Nanotubes, Carbon/chemistry , Reproducibility of Results , Graphite/chemistry , Electrochemical Techniques/methods , Electrodes
5.
ADMET DMPK ; 11(2): 151-173, 2023.
Article in English | MEDLINE | ID: mdl-37325116

ABSTRACT

Various applications of electrochemical sensors and biosensors have been reported in many fields. These include pharmaceuticals, drug detection, cancer detection, and analysis of toxic elements in tap water. Electrochemical sensors are characterised by their low cost, ease of manufacture, rapid analysis, small size and ability to detect multiple elements simultaneously. They also allow the reaction mechanisms of analytes, such as drugs, to be taken into account, giving a first indication of their fate in the body or their pharmaceutical preparation. Several materials are used in the construction of sensors, such as graphene, fullerene, carbon nanotubes, carbon graphite, glassy carbon, carbon clay, graphene oxide, reduced graphene oxide, and metals. This review covers the most recent progress in electrochemical sensors used to analyze drugs and metabolites in pharmaceutical and biological samples. We have highlighted carbon paste electrodes (CPE), glassy carbon electrodes (GCE), screen-printed carbon electrodes (SPCE) and reduced graphene oxide electrodes (rGOE). The sensitivity and analysis speed of electrochemical sensors can be improved by modifying them with conductive materials. Different materials used for modification have been reported and demonstrated, such as molecularly imprinted polymers, multiwalled carbon nanotubes, fullerene (C60), iron(III) nanoparticles (Fe3O4NP), and CuO micro-fragments (CuO MF). Manufacturing strategies and the detection limit of each sensor have been reported.

6.
Talanta ; 260: 124583, 2023 Aug 01.
Article in English | MEDLINE | ID: mdl-37105081

ABSTRACT

The formation of thiols has a notable and detrimental sensory impact, especially in the aroma of bottled wines. Their detection in wine is of great interest to avoid important economic and image losses for wineries. This work reports the study of different cobalt phthalocyanine/nanomaterials-based sensors for the headspace detection of volatile thiols. The amperometric procedure based on the use of carbon sensors simply modified with cobalt phthalocyanine showed the best performance. Under the optimum conditions of applied potential, +0.8 V, and pH of the supporting electrolyte, 2.6, this procedure shows a reproducibility of 7% (n = 5) in terms of relative standard deviation of the slopes of calibration curves built in the concentration range from 9.9 to 82.6 µg/L, a capability of detection of 12.5 µg/L and a decision limit of 6.5 µg/L (α = ß = 0.05). The use of this electrocatalytic material and the headspace measurements reduce interferents, increasing the selectivity of the procedure, which allows the easy and successful quantification of ethanethiol in white and red wines.

7.
Biosensors (Basel) ; 13(1)2023 Jan 12.
Article in English | MEDLINE | ID: mdl-36671965

ABSTRACT

In this study, a screen-printed carbon electrode (SPCE) based on in situ deposition modification was developed for the sensitive, rapid, easy and convenient determination of As(III) in water and tea by linear sweep anodic stripping voltammetry (LSASV). The screen-printed carbon electrodes were placed in a solution consisting of As(III) solution, chlorauric acid and L-cysteine. Under certain electrical potential, the chloroauric acid was reduced to gold nanoparticles (AuNPs) on the SPCE. L-cysteine was self-assembled onto AuNPs and promoted the enrichment of As(III), thus enhancing the determination specificity and sensitivity of As(III). The method achieved a limit of determination (LOD) of 0.91 ppb (µg L-1), a linear range of 1~200 µg L-1, an inter-assay coefficient of variation of 5.3% and good specificity. The developed method was successfully applied to the determination of As(III) in tap water and tea samples, with a recovery rate of 93.8%~105.4%, and further validated by inductively coupled plasma mass spectrometry (ICP-MS). The developed method is rapid, convenient and accurate, holding great promise in the on-site determination of As(III) in tap water and tea leaves, and it can be extended to the detection of other samples.


Subject(s)
Gold , Metal Nanoparticles , Gold/chemistry , Carbon/chemistry , Cysteine , Water , Electrochemical Techniques/methods , Metal Nanoparticles/chemistry , Electrodes , Tea
8.
Small ; 19(51): e2207216, 2023 Dec.
Article in English | MEDLINE | ID: mdl-36703534

ABSTRACT

Tackling the current problem of antimicrobial resistance (AMR) requires fast, inexpensive, and effective methods for controlling and detecting antibiotics in diverse samples at the point of interest. Cost-effective, disposable, point-of-care electrochemical biosensors are a particularly attractive option. However, there is a need for conductive and versatile carbon-based materials and inks that enable effective bioconjugation under mild conditions for the development of robust, sensitive, and selective devices. This work describes a simple and fast methodology to construct an aptasensor based on a novel graphene derivative equipped with alkyne groups prepared via fluorographene chemistry. Using click chemistry, an aptamer is immobilized and used as a successful platform for the selective determination of ampicillin in real samples in the presence of interfering molecules. The electrochemical aptasensor displayed a detection limit of 1.36 nM, high selectivity among other antibiotics, the storage stability of 4 weeks, and is effective in real samples. Additionally, structural and docking simulations of the aptamer shed light on the ampicillin binding mechanism. The versatility of this platform opens up wide possibilities for constructing a new class of aptasensor based on disposable screen-printed carbon electrodes usable in point-of-care devices.


Subject(s)
Aptamers, Nucleotide , Biosensing Techniques , Graphite , Graphite/chemistry , Click Chemistry , Alkynes , Aptamers, Nucleotide/chemistry , Electrochemical Techniques/methods , Carbon/chemistry , Biosensing Techniques/methods , Electrodes , Gold/chemistry , Ampicillin , Anti-Bacterial Agents , Limit of Detection
9.
Biosens Bioelectron ; 221: 114907, 2023 Feb 01.
Article in English | MEDLINE | ID: mdl-36444798

ABSTRACT

Measuring glucose together with glycated hemoglobin (HbA1c) could provide short-term and long-term information of blood glycemic condition after a single treatment. However, it has been a challenge to quantify glucose and HbA1c from single sample drop and strip of electrodes with suitable sensitivity, selectivity, and efficiency. In this paper, we demonstrated a label free & single sample drop electrochemical detection method of glucose and HbA1c by modifying carbon electrodes. Glucose oxidase and capture antibodies (C-Ab) against HbA1c were immobilized onto the first working electrode (WE1) and the second working electrode (WE2) of dual working screen-printed carbon electrodes (DWSPCEs), respectively. WE2 was modified with Gold Nano Flower. After that, 3-mercaptopropionic acid was coated as a linker. Finally, C-Ab was bonded by the linker. The relationship between gold surface area and concentration of HgAuCl4 was evaluated to optimize HbA1c incubation time. Linear calibration curves for glucose concentration (0.02-35 mM), HbA1c concentration (0.01 to 1mgml-1), and HbA1c percentage solution (0-14%) were obtained, with correlation coefficients of 0.99. Sensitivities of the biosensor for glucose and HbA1c were 0.5 µAmm-2mM-1 and 0.09 µAmm-2µg-1ml, respectively. The biosensor also showed proper stability (>93%, 45days) and selectivity (>92%). The efficiency of the proposed biosensor was also compared with those of commercial kits using whole blood samples of diabetic and normal cases. Results of this study demonstrate that this biosensor can measure both glucose and HbA1c electrochemically using label-free methods to overview glycemic conditions of blood samples using cheap and commercially viable dual carbon electrode-based biosensors.


Subject(s)
Biosensing Techniques , Glucose , Glycated Hemoglobin , Blood Glucose , Carbon , Gold , Antibodies
10.
Molecules ; 27(23)2022 Nov 24.
Article in English | MEDLINE | ID: mdl-36500293

ABSTRACT

Rapid and highly sensitive quantitative analysis of chlorpromazine (CPZ) in human whole blood is of great importance for human health. Herein, we utilize the screen-printed carbon electrodes (SPCE) as the electrode substrates for growth of highly electroactive and antifouling nanocomposite materials consisting of vertically ordered mesoporous silica films (VMSF) and electrochemically reduced graphene oxide (ErGO) nanosheets. The preparation of such VMSF/ErGO/SPCE could be performed by using an electrochemical method in a few seconds and the operation is controllable. Inner ErGO layer converted from graphene oxide (GO) in the growth process of VMSF provides oxygen-containing groups and two-dimensional π-conjugated planar structure for stable fabrication of outer VMSF layer. Owing to the π-π enrichment and excellent electrocatalytic abilities of ErGO, electrostatic preconcentration and antifouling capacities of VMSF, and inherent disposable and miniaturized properties of SPCE, the proposed VMSF/ErGO/SPCE sensor could be applied for quantitative determination of CPZ in human whole blood with high accuracy and sensitivity, good stability, and low sample consumption.


Subject(s)
Carbon , Graphite , Humans , Carbon/chemistry , Chlorpromazine , Oxides/chemistry , Silicon Dioxide , Electrodes , Graphite/chemistry , Electrochemical Techniques
11.
Environ Pollut ; 307: 119524, 2022 Aug 15.
Article in English | MEDLINE | ID: mdl-35636716

ABSTRACT

Current synthesis routes of bismuth oxide nanosheets (BiONS) are relatively complicated, requiring the use of halogens or metalloids. Herein, a facile method to synthesize BiONS without the addition of halogens or other metalloids was developed. The synthesized BiONS were identified to have flake-shaped structures (300-1000 nm in width) with the thickness of 6-10 nm, which were predominantly made of ß-Bi2O3. Such BiONS were applied to modify the surface of screen-printed carbon electrodes (BiONS-SPCEs) for the development of a robust palladium (Pd2+) sensor. After optimizing the electrochemical parameters of the sensor, it was found that the linear sensor response range and limit of detection for Pd2+ were 40-400 and 1.4 ppb, respectively. The electrocatalytic activity of the Pd2+-sensor was validated in the competing environment of other metal and metalloid ions. Real samples collected during a Pd recovery process from pharmaceutical wastewater were used to verify the application of BiONS-SPCEs in control of palladium recovery process. The quantitative results of post recovery palladium concentrations obtained using BiONS-SPCEs in treated pharmaceutical wastewater samples were in good agreement with those obtained by inductively coupled plasma-optical emission spectrometry (ICP-OES). Thus, such Pd2+-sensor provided the possibility of on-site process control of complex industrial samples for obtaining near-instant information that would lead to better management of resources used in the process, and same time assure environmental standards for both recovered products and processed discharge.


Subject(s)
Metalloids , Palladium , Bismuth/chemistry , Electrochemical Techniques/methods , Electrodes , Halogens , Palladium/chemistry , Pharmaceutical Preparations , Wastewater
12.
J Forensic Sci ; 67(4): 1450-1460, 2022 Jul.
Article in English | MEDLINE | ID: mdl-35490301

ABSTRACT

Analysis of gunshot residue currently lacks effective screening methods that can be implemented in real time at the crime scene. Historically, SEM-EDS has been the standard for analysis; however, advances in technology have brought portable instrumentation to the forefront of forensic science disciplines, including the screening of GSR. This study proposes electrochemical methods with disposable screen-printed carbon electrodes for GSR screening at the laboratory and points of care due to their rapid, cost-efficient, and compact platform. GSR residues were extracted from typical aluminum/carbon adhesive collection stubs and analyzed via square-wave anodic stripping voltammetry. Benchtop and portable electrochemical instruments were compared for the assessment and classification of authentic shooter samples by monitoring a panel of inorganic and organic GSR elements and compounds including lead, antimony, copper, 2,4-dinitrotoluene, diphenylamine, nitroglycerin, and ethyl centralite. The evaluation included the assessment of figures of merit and performance measures from quality controls, nonshooter, and shooter data sets. Samples collected from the hands of 200 background individuals (nonshooters), and shooters who fired leaded ammunition (100) and lead-free ammunition (50) were analyzed by the benchtop and portable systems with accuracies of 95.7% and 96.5%, respectively. The findings indicate that electrochemical methods are fast, sensitive, and specific for the identification of inorganic and organic gunshot residues. The portable potentiostat provided results comparable with the benchtop system, serving as a proof-of-concept to transition this methodology to crime scenes for a practical and inexpensive GSR screening that could reduce backlogs, improve investigative leads, and increase the impact of gunshot residues in forensic science.


Subject(s)
Wounds, Gunshot , Antimony/analysis , Carbon , Forensic Sciences , Hand , Humans
13.
Food Chem ; 383: 132598, 2022 Jul 30.
Article in English | MEDLINE | ID: mdl-35255369

ABSTRACT

This study aimed to devise a nontoxic electrochemical immunosensor to quantitatively determine aflatoxin M1 by chronoamperometry with novel anti-idiotypic nanobody-functionalized screen-printed carbon electrodes (SPCEs). Anti-idiotype nanobodies (AIdnb) were developed to replace the high toxic chemically synthesized antigen. AIdnb was immobilized on the surface of SPCE via covalent coupling as capture reagent. The functionalized SPCEs were followed by characterization using electrochemical impedance spectroscopy, fourier-transform infrared spectroscopy, transmission electron microscopy mapping, and atomic force microscopy. After optimizing experimental parameters, the assembled immunosensor exhibited a good linearity range of 0.25-5.0 ng/mL, with the limit of detection of 0.09 ng/mL. The immunosensor showed a satisfactory selectivity to AFM1, without interference from analogs, including zearalenone, ochratoxin, and fumonisin B1. For practical application, the developed immunosensor was validated using real spiked samples with the recovery range 82.0%-108.0% and relative standard deviation (RSD) 10.1%-13.0%, indicating that it could be used in milk samples.


Subject(s)
Aflatoxin M1 , Biosensing Techniques , Aflatoxin M1/analysis , Animals , Biosensing Techniques/methods , Carbon/chemistry , Electrochemical Techniques , Electrodes , Immunoassay/methods , Limit of Detection , Milk/chemistry
14.
Mikrochim Acta ; 188(10): 359, 2021 10 01.
Article in English | MEDLINE | ID: mdl-34599426

ABSTRACT

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.

15.
J Hazard Mater ; 418: 126267, 2021 09 15.
Article in English | MEDLINE | ID: mdl-34111746

ABSTRACT

Heavy metal ions (HMIs) pollution is always a serious issue worldwide. Therefore, monitoring HMIs in environmental water is an important and challenging step to ensure environmental health and human safety. In this study, we spotlight an effortless, single-step in-situ electrochemical polymerization deposition technique to fabricate a novel, low-cost, efficient, nano-engineered poly(melamine)/graphitic-carbon nitride nanonetwork (PM/g-C3N4) modified screen-printed carbon electrode (SPE) for sensitive, selective, and simultaneous electrochemical monitoring of toxic HMIs in environmental waters. g-C3N4 nanomaterial was prepared using melamine as a precursor via pyrolysis technique. As-prepared g-C3N4 and melamine monomer were electrochemically in-situ polymerized/deposited over pre-anodized SPE (ASPE) using cyclic voltammetry technique. XRD, XPS, and SEM were engaged to characterize the developed electrode. The fabricated PM/g-C3N4/ASPE was applied as an environmental sensor to selective and simultaneous electrochemical detection of Pb2+ and Cd2+ ions using differential pulse voltammetry technique. The developed sensor displayed excellent selectivity and sensitivity towards Pb2+ and Cd2+ with limit of detections of 0.008 µM and 0.02 µM, respectively. The fabricated PM/g-C3N4/ASPE sensor exhibits superior stability, repeatability, good anti-interference, and applicability for recognition of Pb2+ and Cd2+ ions in real water samples. These results proved that developed environmental sensor is low-cost, efficient, practical platform for rapid, selective, simultaneous monitoring of HMIs in the environment.


Subject(s)
Metals, Heavy , Nitriles , Electrochemical Techniques , Electrodes , Humans
16.
Food Chem ; 358: 129894, 2021 Oct 01.
Article in English | MEDLINE | ID: mdl-33933968

ABSTRACT

Listeria monocytogenes is an important foodborne pathogen, which imposes great burdens on public health. The current methods for detecting L. monocytogene are limited in several ways such as time consuming and lab equipment dependent. In this study, we developed a new electrochemical assay to improve the efficacy. This assay allows us to generate numerous G-quadruplex sequences while loop-mediated isothermal amplification happens. Then, these G-quadruplex sequences form DNAzyme to produce a color change and an electrochemical signal by oxidizing tetramethylbenzidine. This assay could be finished in 2 h, which significantly reduced the detection time. Also, we confirmed the limit of detection of this assay at 6.8 CFU/mL according to 3σ criterion. Our assay shows good sensitivity to detect bacteria range from 52.5 to 5.25 × 104 CFU/mL. This assay's reliability was also confirmed by detecting artificially contaminated pork samples. Thus, we propose this electrochemical assay for rapid and sensitive detection of L. monocytogenes in food.


Subject(s)
Electrochemical Techniques/methods , Food Microbiology/methods , Listeria monocytogenes/genetics , Molecular Diagnostic Techniques/methods , Nucleic Acid Amplification Techniques/methods , Pork Meat/microbiology , Animals , Benzidines/chemistry , DNA, Catalytic/chemistry , DNA, Catalytic/metabolism , G-Quadruplexes , Reproducibility of Results , Sensitivity and Specificity
17.
Front Chem ; 9: 782813, 2021.
Article in English | MEDLINE | ID: mdl-35252124

ABSTRACT

Polyamic acid (PAA) nanofibers produced by using the electrospinning method were fully characterized in terms of morphology and spectroscopy. A PAA nanofiber-modified screen-printed carbon electrode was applied to the detection of selected sulfonamides by following an electroanalytical protocol. The polyamic acid (PAA) nanofibers were characterized using Fourier transform infrared (FTIR) spectroscopy to study the integrity of polyamic acid functional groups as nanofibers by comparing them to chemically synthesized polyamic acid. A scanning electron microscope (SEM) was used to confirm the morphology of the produced nanofibers and 3D arrangement at the electrode interface. The Brunauer-Emmett-Teller (BET) method was used to determine the surface area of the nanofibers. Atomic force microscopy (AFM) was used to study the porosity and surface roughness of the nanofibers. Electrochemical evaluation based on diffusion-controlled kinetics was applied to determine the number of electrons transferred in the system, the surface concentration of the deposited PAA thin film (2.14 × 10-6 mol/cm2), and the diffusion coefficient (De) for the PAA nanofiber-modified screen-printed carbon electrode (9.43 × 10-7 cm-2/s). The reported LODs for sulfadiazine and sulfamethazine detection are consistent with requirements for trace-level monitoring by early warning diagnostic systems.

18.
Talanta ; 223(Pt 2): 121702, 2021 Feb 01.
Article in English | MEDLINE | ID: mdl-33298256

ABSTRACT

A electrochemical biosensor for As(III) determination has been developed by immobilization of the Alcaligenis faecalis bacteria on gold nanoparticle-modified screen-printed carbon electrode (AuNPs-SPCE). The detection of As(III) is due to the catalytic activity of arsenite oxidase enzyme which oxidizes As(III) to As(V) producing an analytical signal. To enhance the performance of the biosensor, was optimized the amount of bacteria, amount of glutaraldehyde and incubation time applied in the preparation of the electrode, in addition to the effect of pH and applied potential. The analytical application was carried out applying 300 mV (pH = 7) obtaining a LOD of 6.61 µmol L-1 (R = 0.9975) and 700 mV (pH = 12) obtaining a LOD of 1.84 µmol L-1 (R = 0.9983). AF/AuNPs-SPCE was applied to the determination of total arsenic in Loa river water samples after reduction, with satisfactory results.


Subject(s)
Alcaligenes faecalis , Biosensing Techniques , Metal Nanoparticles , Carbon , Electrochemical Techniques , Electrodes , Gold
19.
Talanta ; 219: 121247, 2020 Nov 01.
Article in English | MEDLINE | ID: mdl-32887138

ABSTRACT

This paper describes the first biosensor reported to date for the determination of mustard seed traces. The biosensor consists of an amperometric immunosensing platform able to sensitively and selectively determine Sin a 1 content, the major allergen of yellow mustard and the most abundant protein of these seeds. The immunosensing platform exploits the coupling of magnetic microbeads (MBs) modified with sandwich-type immune complexes, comprising polyclonal and monoclonal antibodies, selective to the target protein for its capturing and detection, respectively. In addition, a HRP-conjugated secondary antibody was used for enzymatic labelling of the monoclonal antibody, and amperometric transduction was made at screen-printed carbon electrodes (SPCEs) using the hydroquinone (HQ)/H2O2 system. The electrochemical immunosensor allows the simple and fast detection (a single 1-h incubation step) of Sin a 1 with a limit of detection of 0.82 ng mL-1 (20.5 pg of protein in 25 µL of sample) with high selectivity against structurally similar non-target allergenic proteins (such as Pin p 1 from pine nut). The developed immunoplatform was successfully used for the analysis of peanut, rapeseed, cashew, pine nut and yellow mustard extracts, giving only positive response for the yellow mustard extract with a Sin a 1 content, in full agreement with that provided by conventional ELISA methodology.


Subject(s)
Biosensing Techniques , Mustard Plant , Electrochemical Techniques , Electrodes , Food , Hydrogen Peroxide , Immunoassay , Limit of Detection , Plant Extracts , Seeds
20.
J Forensic Sci ; 65(6): 1935-1944, 2020 Nov.
Article in English | MEDLINE | ID: mdl-32841369

ABSTRACT

The increasing demand for rapid methods to identify both inorganic and organic gunshot residues (IGSR and OGSR) makes electrochemical methods, an attractive screening tool to modernize current practice. Our research group has previously demonstrated that electrochemical screening of GSR samples delivers a simple, inexpensive, and sensitive analytical solution that is capable of detecting IGSR and OGSR in less than 10 min per sample. In this study, we expand our previous work by increasing the number of GSR markers and applying machine learning classifiers to the interpretation of a larger population data set. Utilizing bare screen-printed carbon electrodes, the detection and resolution of seven markers (IGSR; lead, antimony, and copper, and OGSR; nitroglycerin, 2,4-dinitrotoluene, diphenylamine, and ethyl centralite) was achieved with limits of detection (LODs) below 1 µg/mL. A large population data set was obtained from 395 authentic shooter samples and 350 background samples. Various statistical methods and machine learning algorithms, including critical thresholds (CT), naïve Bayes (NB), logistic regression (LR), and neural networks (NN), were utilized to calculate the performance and error rates. Neural networks proved to be the best predictor when assessing the dichotomous question of detection of GSR on the hands of shooter versus nonshooter groups. Accuracies for the studied population were 81.8 % (CT), 88.1% (NB), 94.7% (LR), and 95.4% (NN), respectively. The ability to detect both IGSR and OGSR simultaneously provides a selective testing platform for gunshot residues that can provide a powerful field-testing technique and assist with decisions in case management.

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