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1.
Talanta ; 278: 126510, 2024 Jul 04.
Article in English | MEDLINE | ID: mdl-38981154

ABSTRACT

A novel and robust electrochemical sensing tool for the determination of vismodegib (VIS), an anticancer drug, has been developed by integrating the selective recognition capabilities of molecularly imprinted polymer (MIP) and the sensitivity enhancement capability of metal-organic framework (MOF). Prior to this step, the electrochemical behavior of VIS was investigated using a bare glassy carbon electrode (GCE). It was observed that in 0.5 M H2SO4 solution as electrolyte, VIS has an oxidation peak around 1.3 V and the oxidation mechanism is diffusion controlled. The determination of VIS in a standard solution using a bare GCE showed a linear response in the concentration range from 2.5 µM to 100 µM, with a limit of detection (LOD) of 0.75 µM. Since sufficient sensitivity and selectivity could not be achieved with bare GCE, a MIP sensor was developed in the next step of the study. For this purpose, the GCE surface was first modified by drop casting with as-synthesized Co-MOF. Subsequently, a MIP network was synthesized via a thermal polymerization approach using 2-acrylamido-2-methylpropanesulfonic acid (AMPS) as monomer and VIS as template. MOFs are ideal electrode materials due to their controllable and diverse morphologies and modifiable surface properties. These characteristics enable the development of MIPs with more homogeneous binding sites and high affinity for target molecules. Integrating MOFs could help the performance of sensors with the desired stability and reproducibility. Electrochemical analysis revealed an observable enhancement of the output signal by the incorporation of MOF molecules, which is consistent with the sensitivity-enhancing role of MOF by providing more anchoring sites for the attachment of the polymer texture to the electrode surface. This MOF-MIP sensor exhibited impressive linear dynamic ranges ranging from 0.1 to 1.0 pM for VIS, with detection limits in the low picomolar range. In addition, the MOF-MIP sensor offers high accuracy, selectivity and precision for the determination of VIS, with no interference observed from complex media of serum samples. Additionally, in this study, Analytical GREEnness metric (AGREE), Analytical GREEnness preparation (AGREEprep) and Blue Applicability Grade Index (BAGI) were used to calculate the green profile score.

2.
Food Chem ; 458: 140275, 2024 Jun 28.
Article in English | MEDLINE | ID: mdl-38964102

ABSTRACT

Enzyme-inhibited electrochemical sensor is a promising strategy for detecting organophosphorus pesticides (OPs). However, the poor stability of enzymes and the high oxidation potential of thiocholine signal probe limit their potential applications. To address this issue, an indirect strategy was proposed for highly sensitive and reliable detection of chlorpyrifos by integrating homogeneous reaction and heterogeneous catalysis. In the homogeneous reaction, Hg2+ with low oxidation potential was employed as signal probe for chlorpyrifos detection since its electroactivity can be inhibited by thiocholine, which was the hydrolysate of acetylthiocholine catalyzed by acetylcholinesterase. Additionally, Co,N-doped hollow porous carbon nanocage@carbon nanotubes (Co,N-HPNC@CNT) derived from ZIF-8@ZIF-67 was utilized as high-performance electrode material to amplify the stripping voltammetry signal of Hg2+. Thanks to their synergistic effect, the sensor exhibited outstanding sensing performance, excellent stability and good anti-interference ability. This strategy paves the way for the development of high-performance OP sensors and their application in food safety.

3.
J Colloid Interface Sci ; 675: 84-93, 2024 Jul 02.
Article in English | MEDLINE | ID: mdl-38964127

ABSTRACT

In this study, we innovatively synthesized nitrogen-doped carbon microspheres (NCS) derived from oatmeal. By utilizing polyoxometalates (POM) as both reducing and linking agents, we achieved uniform loading of platinum nanoparticles (Pt NPs) onto the surface of the NCS. The composite nanoparticles constructed from Pt/polyoxometalate/nitrogen-doped carbon microspheres (Pt/POM/NCS) fully exploit the synergistic catalytic effect, demonstrating superior performance in adrenaline detection. The method has a linear range of 2.59 to 1109.59 µM, a detection limit as low as 0.25 µM (S/N = 3), and a sensitivity of 0.74 µA µM-1 cm-2. Additionally, it exhibits high stability and strong anti-interference ability. The recoveries in human serum were 98.51 % to 101.25 %.

4.
J Pharm Biomed Anal ; 249: 116334, 2024 Jul 03.
Article in English | MEDLINE | ID: mdl-38976964

ABSTRACT

This work presents the modification of glassy carbon electrodes (GCE) by using a dispersion resulting from the non-covalent functionalization of multi-walled carbon nanotubes (MWCNT) with polyarginine (polyArg). MWCNT-polyArg is used for the quantification of ascorbic acid (AA) in the presence of acetaminophen (APAP) and viceversa. Since ascorbic acid and acetaminophen are strongly absorbed on GCE/MWCNT-polyArg, they can be detected in the presence of 4.0×10-5 M acetaminophen (and 3.0×10-5 M ascorbic acid) by using adsorptive stripping with media exchange and differential pulse voltammetry. Using water as the solvent for the MWCNT dispersion, the result was Z-potential of 0.053 ± 0.006 V. The developed sensor showed excellent specificity, sensitivity, stability and reproducibility compared to previously published sensors. The GCE/MWCNT-polyArg sensor shows a fast response time of ∼5 minutes, low limits of detection and quantification for AA (0.95 and 2.9 µM respectively) and APAP (0.27 and 0.82µM, respectively), high sensitivity of 0.0616 µA/M for AA or APAP 0.240µA/M. It was used to test its practicability by determining the concentration of AA or APAP (AA and APAP) in pharmaceutical samples. Finally, the simultaneous measurement of ascorbic acid and acetaminophen in pharmaceuticals showed a good correlation, with a maximum error and RSD of 4.5 and 5.1 %, respectively.

5.
Anal Biochem ; : 115597, 2024 Jul 03.
Article in English | MEDLINE | ID: mdl-38969155

ABSTRACT

Vibrio parahaemolyticus (V. parahaemolyticus) is a major foodborne pathogen, which can cause serious foodborne illnesses like diarrhoea. Rapid on-site detection of foodborne pathogens is an ideal way to respond to foodborne illnesses. Herein, we provide an electrochemical sensor for rapid on-site detection. This sensor utilized a pH-sensitive metal-oxide material for the concurrent isothermal amplification and label-free detection of nucleic acids. Based on a pH-sensitive hydrated iridium oxide oxyhydroxide film (HIROF), the electrode transforms the hydrogen ion compound generated during nucleic acid amplification into potential, so as to achieve a real-time detection. The results can be transmitted to a smartphone via Bluetooth. Moreover, HIROF was applied in nucleic acid device detection, with a super-Nernst sensitivity of 77.6 mV/pH in the pH range of 6.0-8.5, and the sensitivity showed the best results so far. Detection of V. parahaemolyticus by this novel method showed a detection limit of 1.0×103 CFU/mL, while the time consumption was only 30 min, outperforming real-time fluorescence loop-mediated isothermal amplification (LAMP). Therefore, the characteristics of compact, portable, and fast make the sensor more widely used in on-site detection.

6.
Chemosphere ; : 142771, 2024 Jul 03.
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% to 4.61% using 7 different wearable devices (n=7) and stability in the range of 4.86% to 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.

7.
Anal Chim Acta ; 1316: 342879, 2024 Aug 08.
Article in English | MEDLINE | ID: mdl-38969416

ABSTRACT

BACKGROUND: Chirality is a ubiquitous phenomenon in nature, but enantiomers exhibit different pharmacological activities and toxicological effects. Therefore, Chiral recognition plays a pivotal role in various fields such as life sciences, chemical synthesis, drug development, and materials science. The synthesis of novel chiral composites with well-defined loading capabilities and ordered structures holds significant potential for electrochemical chiral recognition applications. However, the design of selective and stable electrochemical chiral recognition materials remains a challenging task. RESULT: In this work, we construct a simple and rapid electrochemical sensing platform for tryptophan (Trp) enantiomer recognition using cyclodextrin-modified microporous organic network as chiral recognition agent. CD-MON with chiral microenvironment was prepared by Sonogashira-Hagihara coupling reaction of the chiral molecule heptyl-6-iodo-6-deoxyß-cyclodextrin and 1, 4-Diethynylbenzene. The adhesion of BSA makes CD-MON firmly fixed on the electrode surface, and as a chiral protein, it can improve the chiral recognition ability through synergistic effect. Chiral amino acids are in full contact with the chiral microenvironment during pore conduction of MON, and L-Trp is more stably bound to CD-MON/BSA due to steric hindrance, host-guest recognition and hydrogen bonding. Therefore, the electrochemical sensor can effectively identify tryptophan enantiomers (IL-Trp/ID-Trp = 2.02), and it exhibits a detection limit of 2.6 µM for L-Trp. UV-Vis spectroscopy confirmed the adsorption capacity of CD-MON towards tryptophan enantiomers in agreement with electrochemistry results. SIGNIFICANCE: The prepared chiral sensor has excellent stability, reproducibility (RSD = 3.7%) and selectivity, realizes the quantitative detection of single isomer in tryptophan racemic and quantitative analysis in real samples with 94.0%-101.0% recovery. This work represents the first application of MON in chiral electrochemistry which expands the application scope of chiral sensors and holds great significance in separation science and electrochemical sensing.


Subject(s)
Cyclodextrins , Electrochemical Techniques , Stereoisomerism , Electrochemical Techniques/methods , Cyclodextrins/chemistry , Porosity , Tryptophan/analysis , Tryptophan/chemistry , Amino Acids/analysis , Amino Acids/chemistry , Limit of Detection , Animals , Electrodes , Serum Albumin, Bovine/chemistry
8.
Anal Chim Acta ; 1316: 342837, 2024 Aug 08.
Article in English | MEDLINE | ID: mdl-38969427

ABSTRACT

Monitoring the levels of L-Tryptophan (L-Trp) in body fluids is crucial due to its significant role in metabolism and protein synthesis, which ultimately affects neurological health. Herein, we have developed a novel magneto-responsive electrochemical enantioselective sensor for the recognition of L-Trp based on oriented biochar derived from Loofah, Fe3O4 nanoparticles, and molecularly imprinted polydopamine (MIPDA) in xanthan hydrogel. The successful synthesis of these materials has been confirmed through physicochemical and electrochemical characterization. Various operational factors such as pH, response time, loading sample volume, and loading of active materials were optimized. As a result, the sensor exhibited an affordable linear range of 1.0-60.0 µM, with a desirable limit of detection of 0.44 µM. Furthermore, the proposed electrochemical sensor demonstrated good reproducibility and desirable selectivity for the determination of L-Trp, making it suitable for analyzing L-Trp levels in human plasma and serum samples. The development presented offers an appealing, easily accessible, and efficient strategy. It utilizes xanthan hydrogel to improve mass transfer and adhesion, biochar-stabilized Fe3O4 to facilitate magnetic orientation and accelerate mass transfer and sensitivity, and polydopamine MIP to enhance selectivity. This approach enables on-site evaluation of L-Trp levels, which holds significant value for healthcare monitoring and early detection of related conditions.


Subject(s)
Electrochemical Techniques , Hydrogels , Polysaccharides, Bacterial , Tryptophan , Tryptophan/chemistry , Tryptophan/blood , Polysaccharides, Bacterial/chemistry , Hydrogels/chemistry , Stereoisomerism , Humans , Molecular Imprinting , Polymers/chemistry , Molecularly Imprinted Polymers/chemistry , Indoles/chemistry , Biopolymers/chemistry , Limit of Detection , Magnetite Nanoparticles/chemistry
9.
Anal Chim Acta ; 1316: 342875, 2024 Aug 08.
Article in English | MEDLINE | ID: mdl-38969433

ABSTRACT

BACKGROUND: Indole-3-acetic acid (IAA) and salicylic acid (SA), pivotal regulators in plant growth, are integral to a variety of plant physiological activities. The ongoing and simultaneous monitoring of these hormones in vivo enhances our comprehension of their interactive and regulatory roles. Traditional detection methods, such as liquid chromatography-mass spectrometry, cannot obtain precise and immediate information on IAA and SA due to the complexity of sample processing. In contrast, the electrochemical detection method offers high sensitivity, rapid response times, and compactness, making it well-suited for in vivo or real-time detection applications. RESULTS: A microneedle electrochemical sensor system crafted from disposable stainless steel (SS) wire was specifically designed for the real-time assessment of IAA and SA in plant in situ. This sensor system included a SS wire (100 µm diameter) coated with carbon cement and multi-walled carbon nanotubes, a plain platinum wire (100 µm diameter), and an Ag/AgCl wire (100 µm diameter). Differential pulse voltammetry and amperometry were adopted for detecting SA and IAA within the range of 0.1-20 µM, respectively. This sensor was applied to track IAA and SA fluctuations in tomato leaves during PstDC3000 infection, offering continuous data. Observations indicated an uptick in SA levels following infection, while IAA production was suppressed. The newly developed disposable SS wire-based microneedle electrochemical sensor system is economical, suitable for mass production, and inflicts minimal damage during the monitoring of SA and IAA in plant tissues. SIGNIFICANCE: This disposable microneedle electrochemical sensor facilitates in vivo detection of IAA and SA in smaller plant tissues and allows for long-time monitoring of their concentrations, which not only propels research into the regulatory and interaction mechanisms of IAA and SA but also furnishes essential tools for advancing precision agriculture.


Subject(s)
Electrochemical Techniques , Indoleacetic Acids , Plant Leaves , Salicylic Acid , Solanum lycopersicum , Stainless Steel , Solanum lycopersicum/chemistry , Indoleacetic Acids/analysis , Salicylic Acid/analysis , Plant Leaves/chemistry , Plant Leaves/metabolism , Stainless Steel/chemistry , Electrochemical Techniques/instrumentation , Needles , Plant Diseases/microbiology
10.
Luminescence ; 39(7): e4825, 2024 Jul.
Article in English | MEDLINE | ID: mdl-38961763

ABSTRACT

Herein, we have reported a red-emitting 4-methyl coumarin fused barbituric acid azo dye (4-MCBA) synthesized by conventional method. Density functional theory (DFT) studies of tautomer compounds were done using (B3LYP) with a basis set of 6-31G(d,p). NLO analysis has shown that tautomer has mean first-order hyperpolarisabilities (ß) value of 1.8188 × 10-30 esu and 1.0470 × 10-30 esu for azo and hydrazone forms, respectively, which is approximately nine and five times greater than the magnitude of urea. 4-MCBA exhibited two absorption peaks in the range of 290-317 and 379-394 nm, and emission spectra were observed at 536 nm. CV study demonstrated that the modified 4-MCBA/MGC electrode exhibited excellent electrochemical sensitivity towards the detection of catechol and the detection limit is 9.39 µM under optimum conditions. The 4-MCBA employed as a fluorescent probe for the visualisation of LFPs on various surfaces exhibited Level-I to level-II LFPs, with low background interference.


Subject(s)
Barbiturates , Catechols , Coumarins , Electrochemical Techniques , Barbiturates/chemistry , Catechols/chemistry , Catechols/analysis , Electrochemical Techniques/instrumentation , Coumarins/chemistry , Fluorescent Dyes/chemistry , Fluorescent Dyes/chemical synthesis , Molecular Structure , Density Functional Theory , Electrodes
11.
Talanta ; 278: 126513, 2024 Jul 05.
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.

12.
Environ Res ; 259: 119500, 2024 Jun 29.
Article in English | MEDLINE | ID: mdl-38950814

ABSTRACT

Monitoring fenitrothion (FNT) residues in food and the environment is crucial due to its high environmental toxicity. In this study, we developed a sensitive, reliable electrochemical method for detecting FNT by using screen-printed carbon electrodes (SPCE) modified with porous graphene oxide (PGO) nanosheets. PGO surface properties have been meticulously characterized using advanced spectroscopic techniques. Electrochemical impedance spectroscopy and cyclic voltammetry were used to test the electrochemical properties of the PGO-modified sensor. The PGO-modified sensor exhibited remarkable sensitivity, achieving a detection limit as low as 0.061 µM and a broad linear range of 0.02-250 µM. Enhanced performance is due to PGO's high surface area and excellent electrocatalytic properties, which greatly improved electron transfer. Square wave voltammetry was used to demonstrate the sensor's efficacy as a real-time, on-site monitoring tool for FNT residues in fruit and water. The outstanding performance of the PGO/SPCE sensor underscores its applicability in ensuring food safety and environmental protection.

13.
Food Chem ; 457: 140071, 2024 Jun 13.
Article in English | MEDLINE | ID: mdl-38905827

ABSTRACT

In this study, we have developed a novel, hypersensitive, and ultraselective electrochemical sensor containing thermally annealed gold-silver alloy nanoporous matrices (TA-Au-Ag-ANpM) integrated with f-MWCNTs-CPE and poly(l-serine) nanocomposites for the simultaneous detection of sulfathiazole (SFT) and sulfamethoxazole (SFM) residues in honey, beef, and egg samples. TA-Au-Ag-ANpM/f-MWCNTs-CPE/poly(l-serine) was characterized using an extensive array of analytical (UV-Vis, FT-IR, XRD, SEM, and EDX), and electrochemical (EIS, CV and SWV) techniques. It exhibited outstanding performance over a wide linear range, from 4.0 pM to 490 µM for SFT and 4.0 pM to 520 µM for SFM, with picomolar detection and quantification limits (0.53 pM and 1.75 pM for SFT, 0.41 pM and 1.35 pM for SFM, respectively). The sensor demonstrated exceptional repeatability, reproducibility, and anti-interference capability, with percentage recovery of 95.6-102.4% in food samples and RSD below 5%. Therefore, the developed sensor is an ideal tool to address the current antibiotic residue crisis in food sources.

14.
Bioresour Technol ; 406: 130985, 2024 Jun 15.
Article in English | MEDLINE | ID: mdl-38885731

ABSTRACT

Microbial electrochemical sensor (MES) using electroactive biofilm (EAB) as the sensing element represents a broad-spectrum technology for early warning of biotoxicity of water samples. However, its commercial application is impeded by limited sensitivity and repeatability. Here, we proposed a layered standardized EAB (SEAB) with enriched Geobacter anodireducens SD-1 in the inner layer and self-matched outer layer. The SEAB sensors showed a 2.3 times higher sensitivity than conventional EAB acclimated directly from wastewater (WEAB). A highly repeatable response sensitivity was concentrated at 0.011 ± 0.0006 A/m2/ppm in 4 replicated batches of SEAB sensors (R2 > 0.95), highlighting their potential for reliable toxicity monitoring in practical applications. In contrast, the sensing performance of all WEAB sensors was unpredictable. SEAB also exhibited a better tolerance towards low concentration of formaldehyde, with only a 4 % loss in viability. Our findings improved the sensitivity and reproducibility of standardized MES for toxicity early warning.

15.
Polymers (Basel) ; 16(11)2024 Jun 04.
Article in English | MEDLINE | ID: mdl-38891543

ABSTRACT

Electrochemical sensors play a pivotal role in various fields, such as biomedicine and environmental detection, due to their exceptional sensitivity, selectivity, stability, rapid response time, user-friendly operation, and ease of miniaturization and integration. In addition to the research conducted in the application field, significant focus is placed on the selection and optimization of electrode interface materials for electrochemical sensors. The detection performance of these sensors can be significantly enhanced by modifying the interface of either inorganic metal electrodes or printed electrodes. Among numerous available modification materials, conductive polymers (CPs) possess not only excellent conductivity exhibited by inorganic conductors but also unique three-dimensional structural characteristics inherent to polymers. This distinctive combination allows CPs to increase active sites during the detection process while providing channels for rapid ion transmission and facilitating efficient electron transfer during reaction processes. This review article primarily highlights recent research progress concerning CPs as an ideal choice for modifying electrochemical sensors owing to their remarkable features that make them well-suited for biomedical and environmental applications.

16.
Molecules ; 29(11)2024 May 21.
Article in English | MEDLINE | ID: mdl-38893303

ABSTRACT

In this study, we designed a novel electrochemical sensor by modifying a glass carbon electrode (GCE) with Pd confined mesoporous carbon hollow nanospheres (Pd/MCHS) for the simultaneous detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA). The structure and morphological characteristics of the Pd/MCHS nanocomposite and the Pd/MCHS/GCE sensor are comprehensively examined using SEM, TEM, XRD and EDX. The electrochemical properties of the prepared sensor are investigated through CV and DPV, which reveal three resolved oxidation peaks for AA, DA, and UA, thereby verifying the simultaneous detection of the three analytes. Benefiting from its tailorable properties, the Pd/MCHS nanocomposite provides a large surface area, rapid electron transfer ability, good catalytic activity, and high conductivity with good electrochemical behavior for the determination of AA, DA, and UA. Under optimized conditions, the Pd/MCHS/GCE sensor exhibited a linear response in the concentration ranges of 300-9000, 2-50, and 20-500 µM for AA, DA, and UA, respectively. The corresponding limit of detection (LOD) values were determined to be 51.03, 0.14, and 4.96 µM, respectively. Moreover, the Pd/MCHS/GCE sensor demonstrated outstanding selectivity, reproducibility, and stability. The recovery percentages of AA, DA, and UA in real samples, including a vitamin C tablet, DA injection, and human urine, range from 99.8-110.9%, 99.04-100.45%, and 98.80-100.49%, respectively. Overall, the proposed sensor can serve as a useful reference for the construction of a high-performance electrochemical sensing platform.


Subject(s)
Ascorbic Acid , Carbon , Dopamine , Electrochemical Techniques , Limit of Detection , Nanospheres , Palladium , Uric Acid , Ascorbic Acid/analysis , Ascorbic Acid/urine , Uric Acid/urine , Uric Acid/analysis , Dopamine/analysis , Dopamine/urine , Nanospheres/chemistry , Electrochemical Techniques/methods , Carbon/chemistry , Palladium/chemistry , Porosity , Humans , Electrodes , Biosensing Techniques/methods , Reproducibility of Results
17.
J Pharm Biomed Anal ; 248: 116283, 2024 Jun 04.
Article in English | MEDLINE | ID: mdl-38850885

ABSTRACT

This study presented a new method to design a MIP-based electrochemical sensor that could improve the selective and sensitive detection of ipratropium bromide (IPR). The polymeric film was designed using 2-hydroxyethyl methacrylate (HEMA) as the basic monomer, 2-hydroxy-2-methylpropiophenone as the initiator, ethylene glycol dimethacrylate (EGDMA) as the crosslinking agent, and N-methacryloyl-L-aspartic acid (MAAsp) as the functional monomer. The presence of MAAsp results in the functional groups in imprinting binding sites, while the presence of poly(vinyl alcohol) (PVA) allows the generation of porous materials not only for sensitive sensing but also for avoiding electron transport limitations. Electrochemical characterizations of the changes at each stage of the MIP preparation process were confirmed using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). In addition, morphological characterizations of the developed sensor were performed using scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), and contact angle measurements. Theoretical calculations were also performed to explain/confirm the experimental results better. It was found that the results of the calculations using the DFT approach agreed with the experimental data. The MAAsp-IPR@MIP/GCE sensor was developed using the photopolymerization method, and the sensor surface was obtained by exposure to UV lamp radiation at 365 nm. The improved MIP-based electrochemical sensor demonstrated the ability to measure IPR for standard solutions in the linear operating range of 1.0 × 10-12-1.0 × 10-11 M under optimized conditions. For standard solutions, the limit of detection (LOD) and limit of quantification (LOQ) were obtained as 2.78 × 10-13 and 9.27 × 10-13 M, respectively. The IPR recovery values for the inhalation form were calculated as 101.70 % and 100.34 %, and the mean relative standard deviations (RSD) were less than 0.76 % in both cases. In addition, the proposed modified sensor demonstrated remarkable sensitivity and selectivity for rapid assessment of IPR in inhalation forms. The sensor's unique selectivity is demonstrated by its successful performance even in the presence of IPR impurities.

18.
Food Chem ; 456: 140007, 2024 Jun 07.
Article in English | MEDLINE | ID: mdl-38861864

ABSTRACT

Developing an efficient method for screening Ochratoxin A (OTA) in agriculture products is vital to ensure food safety and human health. However, the complex food matrix seriously affects the sensitivity and accuracy. To address this issue, we designed a novel molecularly imprinted polymer (MIP) electrochemical sensor based on multiwalled carbon nanotube-modified niobium carbide (Nb2C-MWCNTs) with the aid of the density functional theory (DFT). In this design, a glassy carbon electrode (GCE) was first modified by Nb2C-MWCNTs heterostructure. Afterward, the MIP layer was prepared, with ortho-toluidine as a functional monomer selected via DFT and OTA acting as a template on the surface of Nb2C-MWCNTs/GCE using in-situ electropolymerization. Electrochemical tests and physical characterization revealed that Nb2C-MWCNTs improved the sensor's active surface area and electron transmission capacity. Nb2C-MWCNTs had a good synergistic effect on MIP, endowing the sensor with high sensitivity and specific recognition of OTA in complex food matrix systems. The MIP sensor showed a wide linear range from 0.04 to 10.0 µM with a limit of detection (LOD) of 3.6 nM. Moreover, it presented good repeatability and stability for its highly antifouling effect on OTA. In real sample analysis, the recoveries, ranging from 89.77% to 103.70%, agreed well with the results obtained by HPLC methods, suggesting the sensor has good accuracy and high potential in practical applications.

19.
Nanomaterials (Basel) ; 14(11)2024 May 21.
Article in English | MEDLINE | ID: mdl-38869524

ABSTRACT

The chemical stability of azithromycin (AZM) may be compromised depending on the imposed thermo-oxidative conditions. This report addresses evidence of this process under varying conditions of temperature (20-80 °C), exposure time to UV radiation (1-3 h irradiation at 257 nm), and air saturation (1-3 h saturation with atmospheric air at 1.2 L min-1 and 15 kPa) through electrochemical measurements performed with a thermoactivated cerium molybdate (Ce2(MoO4)3)/multi-walled carbon nanotubes (MWCNT)-based composite electrode. Thermal treatment at 120 °C led to coordinated water elimination in Ce2(MoO4)3, improving its electrocatalytic effect on antibiotic oxidation, while MWCNT were essential to reduce the charge-transfer resistance and promote signal amplification. Theoretical-experimental data revealed remarkable reactivity for the irreversible oxidation of AZM on the working sensor using phosphate buffer (pH = 8) prepared in CH3OH/H2O (10:90%, v/v). Highly sensitive (230 nM detection limit) and precise (RSD < 4.0%) measurements were recorded under these conditions. The results also showed that AZM reduces its half-life as the temperature, exposure time to UV radiation, and air saturation increase. This fact reinforces the need for continuous quality control of AZM-based pharmaceuticals, using conditions closer to those observed during their transport and storage, reducing impacts on consumers' health.

20.
Nanomaterials (Basel) ; 14(11)2024 May 28.
Article in English | MEDLINE | ID: mdl-38869573

ABSTRACT

This study addresses the necessity to monitor the presence of glyphosate (Gly) in waters, highlighting the need for on-site detection of Gly by using electrochemical sensors in environmental and agricultural monitoring programs. Two approaches were employed: (1) modification with graphene decorated with gold nanoparticles (AuNPs-Gr) and dispersed in either dimethylformamide (DMF) or a solution containing Nafion and isopropanol (NAF), and (2) molecularly imprinted polymers (MIPs) based on polypyrrole (PPy) deposited on gold SPEs (AuSPE). Electrochemical characterization revealed that sensors made of AuNPs-Gr/SPCE exhibited enhanced conductivity, larger active area, and improved charge transfer kinetics compared to unmodified SPEs and SPEs modified with graphene alone. However, the indirect detection mechanism of Gly via complex formation with metallic cations in AuNPs-Gr-based sensors introduces complexities and compromises sensitivity and selectivity. In contrast, MIPPy/AuSPE sensors demonstrated superior performance, offering enhanced reliability and sensitivity for Gly analysis. The MIPPy/AuSPE sensor allowed the detection of Gly concentrations as low as 5 ng/L, with excellent selectivity and reproducibility. Moreover, testing in real surface water samples from the Olt River in Romania showed recovery rates ranging from 90% to 99%, highlighting the effectiveness of the detection method. Future perspectives include expanding the investigation to monitor Gly decomposition in aquatic environments over time, providing insights into the decomposition's long-term effects on water quality and ecosystem health, and modifying regulatory measures and agricultural practices for mitigating its impact. This research contributes to the development of robust and reliable electrochemical sensors for on-site monitoring of Glyphosate in environmental and agricultural settings.

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