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1.
Mikrochim Acta ; 186(3): 174, 2019 02 15.
Artigo em Inglês | MEDLINE | ID: mdl-30771008

RESUMO

A carbon paste electrode (CPE) was modified with graphite oxide (GrO) and ß-cyclodextrin (CD) to obtain a sensor for simultaneous voltammetric determination of levodopa (LD), piroxicam (PRX), ofloxacin (OFX) and methocarbamol (MCB). The morphology, structure and electrochemical properties of the functionalized GrO were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, contact angle measurements and cyclic voltammetry. Under the optimal experimental conditions, the sensor is capable of detecting LD, PRX, OFX and MCB by square wave voltammetry (SWV) at working potentials of +0.40, +0.60, +1.03 and + 1.27 V (versus Ag/AgCl), respectively. Response is linear from 1.0 to 20 µM for LD, from 1.0 to 15 µM for PRX, from 1.0 to 20 µM for OFX, and from 1.0 to 50 µM for MCB. The respective limits of detection are 65, 105, 89 and 400 nM. The method was successfully applied to the simultaneous determination of LD, PRX, OFX and MCB in (spiked) real river water and synthetic urine samples, and the results were in agreement with those obtained using a spectrophotometric method, with recoveries close to 100%. Graphical abstract Schematic presentation of a novel electroanalytical method employing a carbon paste electrode modified with graphite oxide and ß-cyclodextrin for the simultaneous determination of levodopa, piroxicam, ofloxacin and methocarbamol in urine and river water samples by square wave voltammetry.


Assuntos
Grafite/química , Levodopa/urina , Metocarbamol/urina , Ofloxacino/urina , Piroxicam/urina , beta-Ciclodextrinas/química , Técnicas Eletroquímicas/métodos , Eletrodos , Levodopa/química , Limite de Detecção , Metocarbamol/química , Ofloxacino/química , Óxidos/química , Piroxicam/química , Reprodutibilidade dos Testes , Rios/química
2.
Mikrochim Acta ; 186(3): 148, 2019 02 02.
Artigo em Inglês | MEDLINE | ID: mdl-30712130

RESUMO

A glassy carbon electrode was modified with carbon black and CdTe quantum dots in a chitosan film to obtained a sensor for norfloxacin (NOR) in the presence of dopamine, caffeine, and uric acid. The morphological, structural and electrochemical characteristics of the nanostructured material were evaluated using spectrophotometry, X-ray diffraction, transmission electronic microscopy and voltammetry. The high electrochemical activity, fast electron transfer rate and high surface area enhanced the oxidation peak currents and shifted the peak potentials of NOR for more negative values (typically at 0.95 V vs. Ag/AgCl). Electrochemical determination of NOR was carried out using square-wave adsorptive anodic stripping voltammetry (SWAdASV). Response is linear in the 0.2 to 7.4 µmol L-1 NOR concentration range, and the detection limit is as low as 6.6 nmol L-1. The method was successfully applied to the determination of norfloxacin in pharmaceutical formulation, synthetic urine and spiked serum. Graphical abstract Schematic presentation of a voltammetric method using a glassy carbon electrode modified with carbon black and CdTe quantum dots in a chitosan film for the determination of norfloxacin in serum and urine samples.


Assuntos
Técnicas Eletroquímicas/métodos , Norfloxacino/análise , Pontos Quânticos/química , Compostos de Cádmio , Carbono/química , Quitosana , Eletrodos , Limite de Detecção , Norfloxacino/sangue , Norfloxacino/urina , Telúrio
3.
Biosensors (Basel) ; 13(9)2023 Sep 08.
Artigo em Inglês | MEDLINE | ID: mdl-37754111

RESUMO

This work reports the development and application of a highly selective core@shell-based quantum dot-molecularly imprinted polymer (QD@MIP) sensor for the detection of sulfadiazine (SDZ)-an antibiotic which belongs to the sulfonamide family. The synthesis of the smart material or MIP (molecularly imprinted polymer) was carried out by a precipitation method directly on the quantum dot surface, which played the role of a fluorescent probe in the optical sensor. The synthesized polymer was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. Fluorescence experiments were performed in order to evaluate the effects of pH, interaction time of the QD@MIP with the analyte and SDZ concentration in different matrices. Under optimized conditions, a linear concentration range of 10.0-60.0 ppm and a limit of detection of 3.33 ppm were obtained. The repeatability and reproducibility of the proposed QD@MIP were evaluated in terms of the RSD, where RSD values of less than 5% were obtained in both tests. Selectivity studies were carried out in the presence of four possible interfering substances with quenching properties, and the signals obtained for these interferents confirmed the excellent selectivity of the proposed sensor; the imprinting factor value obtained for SDZ was 1.64. Finally, the proposed sensor was applied in real animal-based food samples using a spiked concentration of SDZ, where the recovery values obtained were above 90% (experiments were performed in triplicate).


Assuntos
Compostos de Cádmio , Impressão Molecular , Pontos Quânticos , Animais , Antibacterianos , Polímeros Molecularmente Impressos , Pontos Quânticos/química , Compostos de Cádmio/química , Reprodutibilidade dos Testes , Impressão Molecular/métodos , Telúrio/química , Sulfanilamida , Sulfadiazina , Limite de Detecção
4.
Biomimetics (Basel) ; 8(1)2023 Feb 12.
Artigo em Inglês | MEDLINE | ID: mdl-36810408

RESUMO

This study investigates biomimetic sensors for the detection of methotrexate contaminants in environmental samples. Sensors inspired by biological systems are the focus of this biomimetic strategy. Methotrexate is an antimetabolite that is widely used for the treatment of cancer and autoimmune diseases. Due to the widespread use of methotrexate and its rampant disposal into the environment, the residues of this drug are regarded as an emerging contaminant of huge concern, considering that exposure to the contaminant has been found to lead to the inhibition of some essential metabolic processes, posing serious risks to humans and other living beings. In this context, this work aims to quantify methotrexate through the application of a highly efficient biomimetic electrochemical sensor constructed using polypyrrole-based molecularly imprinted polymer (MIP) electrodeposited by cyclic voltammetry on a glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNT). The electrodeposited polymeric films were characterized by infrared spectrometry (FTIR), scanning electron microscopy (SEM), and cyclic voltammetry (CV). The analyses conducted using differential pulse voltammetry (DPV) yielded a detection limit of 2.7 × 10-9 mol L-1 for methotrexate, a linear range of 0.01-125 µmol L-1, and a sensitivity of 0.152 µA L mol-1. The results obtained from the analysis of the selectivity of the proposed sensor through the incorporation of interferents in the standard solution pointed to an electrochemical signal decay of only 15.4%. The findings of this study show that the proposed sensor is highly promising and suitable for use in the quantification of methotrexate in environmental samples.

5.
Biosensors (Basel) ; 13(7)2023 Jun 29.
Artigo em Inglês | MEDLINE | ID: mdl-37504089

RESUMO

The present study reports the development and application of a flow injection analysis (FIA) system for the simultaneous determination of uric acid (UA) and caffeine (CAF) using cathodically pretreated boron-doped diamond electrode (CPT-BDD) and multiple-pulse amperometry (MPA). The electrochemical profiles of UA and CAF were analyzed via cyclic voltammetry in the potential range of 0.20-1.7 V using 0.10 mol L-1 H2SO4 solution as supporting electrolyte. Under optimized conditions, two oxidation peaks at potentials of 0.80 V (UA) and 1.4 V (CAF) were observed; the application of these potentials using multiple-pulse amperometry yielded concentration linear ranges of 5.0 × 10-8-2.2 × 10-5 mol L-1 (UA) and 5.0 × 10-8-1.9 × 10-5 mol L-1 (CAF) and limits of detection of 1.1 × 10-8 and 1.3 × 10-8 mol L-1 for UA and CAF, respectively. The proposed method exhibited good repeatability and stability, and no interference was detected in the electrochemical signals of UA and CAF in the presence of glucose, NaCl, KH2PO4, CaCl2, urea, Pb, Ni, and Cd. The application of the FIA-MPA method for the analysis of environmental samples resulted in recovery rates ranging between 98 and 104%. The results obtained showed that the BDD sensor exhibited a good analytical performance when applied for CAF and UA determination, especially when compared to other sensors reported in the literature.


Assuntos
Cafeína , Ácido Úrico , Cafeína/análise , Oxirredução , Eletrodos , Técnicas Eletroquímicas/métodos
6.
Polymers (Basel) ; 15(18)2023 Sep 08.
Artigo em Inglês | MEDLINE | ID: mdl-37765563

RESUMO

In this paper, we present an alternative technique for the removal of Brilliant Green dye (BG) in aqueous solutions based on the application of molecularly imprinted polymer (MIP) as a selective adsorbent for BG. The MIP was prepared by bulk radical polymerization using BG as the template; methacrylic acid (MAA) as the functional monomer, selected via computer simulations; ethylene glycol dimethacrylate (EGDMA) as cross-linker; and 2,2'-azobis(2-methylpropionitrile) (AIBN) as the radical initiator. Scanning electron microscopy (SEM) analyses of the MIP and non-molecularly imprinted polymer (NIP)-used as the control material-showed that the two polymers exhibited similar morphology in terms of shape and size; however, N2 sorption studies showed that the MIP displayed a much higher BET surface (three times bigger) compared to the NIP, which is clearly indicative of the adequate formation of porosity in the former. The data obtained from FTIR analysis indicated the successful formation of imprinted polymer based on the experimental procedure applied. Kinetic adsorption studies revealed that the data fitted quite well with a pseudo-second order kinetic model. The BG adsorption isotherm was effectively described by the Langmuir isotherm model. The proposed MIP exhibited high selectivity toward BG in the presence of other interfering dyes due to the presence of specific recognition sites (IF = 2.53) on its high specific surface area (112 m2/g). The imprinted polymer also displayed a great potential when applied for the selective removal of BG in real river water samples, with recovery ranging from 99 to 101%.

7.
Biosensors (Basel) ; 13(8)2023 Aug 19.
Artigo em Inglês | MEDLINE | ID: mdl-37622915

RESUMO

Nifedipine, a widely utilized medication, plays a crucial role in managing blood pressure in humans. Due to its global prevalence and extensive usage, close monitoring is necessary to address this widespread concern effectively. Therefore, the development of an electrochemical sensor based on a glassy carbon electrode modified with carbon nanofibers and gold nanoparticles in a Nafion® film was performed, resulting in an active electrode surface for oxidation of the nifedipine molecule. This was applied, together with a voltammetric methodology, for the analysis of nifedipine in biological and environmental samples, presenting a linear concentration range from 0.020 to 2.5 × 10-6 µmol L-1 with a limit of detection 2.8 nmol L-1. In addition, it presented a good recovery analysis in the complexity of the samples, a low deviation in the presence of interfering potentials, and good repeatability between measurements.


Assuntos
Nanopartículas Metálicas , Nanofibras , Humanos , Ouro , Nifedipino , Carbono , Eletrodos
8.
Food Chem ; 383: 132384, 2022 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-35176714

RESUMO

This paper reports the development of a voltammetric sensor using glassy carbon electrode based on hierarchical porous carbon (HPC) with silver sulfide nanoparticles (Ag2SNP), Nafion and fullerene (C60) for the determination of nitrite in foods. Raman spectroscopy, scanning electron microscopy, transmission electron microscopy and energy-dispersive X-ray were used to characterize the morphology and composition of the materials. The use of HPC and C60 in the construction of the electrode contributed toward the enlargement of the specific surface area and the improvement of the electrochemical performance of the device. The electrochemical behavior of nitrite in different electrodes was evaluated by cyclic voltammetry in the potential range of 0.4 - 1 V. Using the optimal conditions, a linear response ranges of 4.0- 148 µmol L-1, a limit of detection of 0.09 µmol L-1 and a sensitivity of 0.05 µAµmol L-1 cm-2 were obtained. The results showed that the proposed method can selectively detect nitrite in the presence of other compounds without interference and with good stability. The proposed method was successfully applied for the detection of nitrite in food samples where it demonstrated a good degree of accuracy and satisfactory efficiency.


Assuntos
Fulerenos , Nanopartículas , Carbono/química , Técnicas Eletroquímicas , Eletrodos , Limite de Detecção , Nanopartículas/química , Nitritos , Porosidade , Compostos de Prata
9.
Biosensors (Basel) ; 12(10)2022 Oct 12.
Artigo em Inglês | MEDLINE | ID: mdl-36290997

RESUMO

This work reports the development and application of a simple, rapid and low-cost voltammetric method for the determination of 3-methylmorphine at nanomolar levels in clinical and environmental samples. The proposed method involves the combined application of a glassy carbon electrode modified with reduced graphene oxide, chitosan and bismuth film (Bi-rGO-CTS/GCE) via square-wave voltammetry using 0.04 mol L-1 Britton-Robinson buffer solution (pH 4.0). The application of the technique yielded low limit of detection of 24 × 10-9 mol L-1 and linear concentration range of 2.5 × 10-7 to 8.2 × 10-6 mol L-1. The Bi-rGO-CTS/GCE sensor was successfully applied for the detection of 3-methylmorphine in the presence of other compounds, including paracetamol and caffeine. The results obtained also showed that the application of the sensor for 3-methylmorphine detection did not experience any significant interference in the presence of silicon dioxide, povidone, cellulose, magnesium stearate, urea, ascorbic acid, humic acid and croscarmellose. The applicability of the Bi-rGO-CTS/GCE sensor for the detection of 3-methylmorphine was evaluated using synthetic urine, serum, and river water samples through addition and recovery tests, and the results obtained were found to be similar to those obtained for the high-performance liquid chromatography method (HPLC)-used as a reference method. The findings of this study show that the proposed voltammetric method is a simple, fast and highly efficient alternative technique for the detection of 3-methylmorphine in both biological and environmental samples.


Assuntos
Quitosana , Grafite , Carbono/química , Bismuto , Acetaminofen , Substâncias Húmicas , Povidona , Cafeína , Limite de Detecção , Grafite/química , Eletrodos , Dióxido de Silício , Celulose , Ácido Ascórbico , Ureia , Água , Técnicas Eletroquímicas/métodos
10.
Anal Methods ; 14(39): 3859-3866, 2022 10 13.
Artigo em Inglês | MEDLINE | ID: mdl-36129055

RESUMO

A new electrode was prepared based on functionalized graphene and gold nanoparticles dispersed in a chitosan film. Such an electrochemical sensor determines ofloxacin in the presence of dopamine, paracetamol, and caffeine. Characterization (morphological and electrochemical) was done using scanning electron microscopy, electrochemical impedance spectroscopy, and cyclic voltammetry. The sensor design improved the analytical signal, the electrochemical activity, and the electron transfer rate. Ofloxacin was determined by square-wave voltammetry, with a linear concentration range of 0.10-4.9 µmol L-1 (r = 0.999, LOD = 12 nmol L-1). The proposed sensor showed good repeatability and selectivity and was applied successfully to the determination of ofloxacin in pharmaceutical formulations, synthetic urine, and water river samples. The proposed method proved to be excellent; therefore, it is an alternative method for the determination of ofloxacin.


Assuntos
Quitosana , Grafite , Nanopartículas Metálicas , Acetaminofen , Cafeína/química , Carbono/química , Dopamina , Eletrodos , Ouro/química , Grafite/química , Nanopartículas Metálicas/química , Ofloxacino , Preparações Farmacêuticas , Água
11.
ACS Appl Mater Interfaces ; 14(49): 54527-54538, 2022 Dec 14.
Artigo em Inglês | MEDLINE | ID: mdl-36454041

RESUMO

Low-cost, instrument-free colorimetric tests were developed to detect SARS-CoV-2 using plasmonic biosensors with Au nanoparticles functionalized with polyclonal antibodies (f-AuNPs). Intense color changes were noted with the naked eye owing to plasmon coupling when f-AuNPs form clusters on the virus, with high sensitivity and a detection limit of 0.28 PFU mL-1 (PFU stands for plaque-forming units) in human saliva. Plasmon coupling was corroborated with computer simulations using the finite-difference time-domain (FDTD) method. The strategies based on preparing plasmonic biosensors with f-AuNPs are robust to permit SARS-CoV-2 detection via dynamic light scattering and UV-vis spectroscopy without interference from other viruses, such as influenza and dengue viruses. The diagnosis was made with a smartphone app after processing the images collected from the smartphone camera, measuring the concentration of SARS-CoV-2. Both image processing and machine learning algorithms were found to provide COVID-19 diagnosis with 100% accuracy for saliva samples. In subsidiary experiments, we observed that the biosensor could be used to detect the virus in river waters without pretreatment. With fast responses and requiring small sample amounts (only 20 µL), these colorimetric tests can be deployed in any location within the point-of-care diagnosis paradigm for epidemiological control.


Assuntos
Técnicas Biossensoriais , COVID-19 , Nanopartículas Metálicas , Humanos , Colorimetria/métodos , Ouro/química , SARS-CoV-2 , Nanopartículas Metálicas/química , Ressonância de Plasmônio de Superfície/métodos , Smartphone , Teste para COVID-19 , COVID-19/diagnóstico , Técnicas Biossensoriais/métodos
12.
Anal Methods ; 13(4): 453-461, 2021 01 28.
Artigo em Inglês | MEDLINE | ID: mdl-33437979

RESUMO

This work describes a novel technique for the direct quantification of Acid Green 16 (AG16) adsorbed on a molecularly imprinted polymer (MIP) through the application of diffuse reflectance spectrophotometry (DRS) directly in a solid material. The MIP was synthesized by a bulk method using 1-vinylimidazole as the functional monomer. To conduct DRS analysis, adsorption assays were performed through the application of the MIP in a solution containing different concentrations of AG16 for 120 minutes; subsequently, the MIP was left to dry and a certain quantity of the polymer was analyzed. Under optimized conditions, a linear concentration range of 1.0 µmol L-1 to 10.0 µmol L-1 and limits of detection and quantification of 0.3 µmol L-1 and 1.0 µmol L-1, respectively, were obtained. The repeatability and reproducibility of the method were evaluated and RSD values lower than 4% were obtained. Selectivity studies allowed finding imprinting factor values of 1.9, 2.6, 1.1, and 1.1 for AG16, Direct yellow 50, Acid Blue 1, and Brilliant Green, respectively. The proposed method was applied toward the analysis of river water and textile industry effluents. The advantage and novelty of the technique lie in the fact that the amount of the analyte adsorbed on the selective polymer is directly measured on the solid material for AG16 and not indirectly via the remaining solution as it has always been carried out in previous studies reported in the literature. The findings show that the proposed technique is relatively simple, novel and highly versatile for the quantification of analytes adsorbed on MIPs, as well as for the analysis of the material of interest and quantification of diverse analytes in different matrices.

13.
J Pharm Anal ; 11(5): 646-652, 2021 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-34765278

RESUMO

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

14.
Front Chem ; 9: 615602, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-33816435

RESUMO

This work describes an electrochemical sensor for the selective recognition and quantification of amoxicillin and a ß-lactam antibiotic in real samples. This sensor consists of a carbon paste electrode (CPE) modified with mag-MIP (magnetic molecularly imprinted polymer), which was prepared by precipitation method via free radical using acrylamide (AAm) as functional monomer, N,N'-methylenebisacrylamide (MBAA) as a crosslinker, and potassium persulfate (KPS) as initiator, to functionalized magnetic nanoparticles. The magnetic non-imprinted polymers (mag-NIP) were prepared using the same experimental procedure without analyte and used for the preparation of a CPE for comparative studies. The morphological, structural, and electrochemical characteristics of the nanostructured material were evaluated using Field emission gun scanning electron microscopy (FEG-SEM), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Vibrating sample magnetometry (VSM), X-ray diffraction (XRD), and voltammetric technique. Electrochemical experiments performed by square wave voltammetry show that the mag-MIP/CPE sensor had a better signal response compared to the non-imprinted polymer-modified electrode (mag-NIP/CPE). The sensor showed a linear range from 2.5 to 57 µmol L-1 of amoxicillin (r 2 = 0.9964), with a limit of detection and a limit of quantification of 0.75 and 2.48 µmol L-1, respectively. No significant interference in the electrochemical signal of amoxicillin was observed during the testing experiments in real samples (skimmed milk and river water). The proposed mag-MIP/CPE sensor could be used as a good alternative method to confront other techniques to determine amoxicillin in different samples.

15.
Talanta ; 229: 122258, 2021 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-33838769

RESUMO

A new biomimetic sensor selective to folic acid based on a carbon paste modified with graphene oxide and Fe3O4 nanoparticles coated with molecularly imprinted polymer in the core@shell format (Fe3O4@MIPs) was obtained using the polyol method. The sensing phase was synthesized in a simple way and characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and Brunauer-Emmett-Teller (BET) surface area. In the binding experiments the selective material showed a high adsorption capacity (Q) of 30.4 mg g-1 for MMIP, while the Q value for MNIP (magnetic non-imprinted polymer) was 15.3 mg g-1 both of them following the Langmuir model to the adsorption procedure. After their efficiency was proven, these materials were used as modifiers in the electrochemical sensor (Fe3O4@MIP-GO/CPE). Under optimized conditions using the square-wave adsorptive voltammetry, the proposed sensor exhibited excellent response with a concentration linear range between 2.5 and 48 µmol L-1 and limit of detection of 0.65 µmol L-1 (S/σ = 3). The advantages obtained with the proposed method were high robustness, selectivity, and low cost being these characteristics due to the MIP; highly sensibility due to the high superficial area being the contribution of the magnetite in the core of material; and experimentally versatile since was possible carry out numerous reproductible analysis only make the renovation of the paste electrode surface by simple polishing. The sensor was applied successfully in pharmaceutical formulation and river water samples with recoveries percentages near 100%.

16.
Talanta ; 224: 121804, 2021 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-33379030

RESUMO

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


Assuntos
Grafite , Nanopartículas de Magnetita , Impressão Molecular , Pontos Quânticos , Técnicas Eletroquímicas , Eletrodos , Etinilestradiol , Limite de Detecção , Polímeros Molecularmente Impressos
17.
Talanta ; 222: 121539, 2021 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-33167247

RESUMO

The present study reports the development of graphite pencil electrode modified with palladium nanoparticles (PdNPs) and its application as an electrochemical sensor for the simultaneous detection of direct yellow 50, tryptophan, carbendazim and caffeine in river water and synthetic urine samples. The combination involving the conductive surface of the graphite pencil electrode (GPE) and the enlargement of the surface area caused by the use of palladium nanoparticles (PdNPs) led to the improvement of the analytical performance of the proposed device. The surface of the GPE-PdNPs was characterized by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The charge transfer kinetics of the electrode was evaluated based on the electrochemical analysis of the potassium ferricyanide redox probe. Using square wave voltammetry (SWV), well-defined and fully resolved anodic peaks were detected for the analytes, with peak-to-peak potential separation not less than 200 mV. Under optimised conditions, the following linear range concentrations were obtained: 0.99-9.9 µmol L-1 for direct yellow 50; 1.2-12 µmol L-1 for tryptophan; 0.20-1.6 µmol L-1 for carbendazim; and 25-190 µmol L-1 for caffeine. The sensor showed good sensitivity, repeatability, and stability. The device was successfully applied for the determination of analytes in urine and river water samples, where recovery rates close to 100% were obtained. Due to its low cost and reusability by simple polishing, the sensor has strong potential to be used as an electrochemical sensor for the determination of different analytes.


Assuntos
Grafite , Nanopartículas Metálicas , Compostos Azo , Benzimidazóis , Cafeína , Carbamatos , Técnicas Eletroquímicas , Eletrodos , Naftalenos , Paládio , Triptofano
18.
Talanta ; 209: 120588, 2020 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-31891996

RESUMO

The ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoroborate and carbon black (CB) nanoparticles were incorporated within a crosslinked chitosan film over the surface of a glassy carbon electrode, and the obtained architecture explored to the sensitive voltammetric sensing of Allura red colorant in soft drinking powders. The different electrodic surfaces were morphologically and electrochemically characterized. From the modification of glassy carbon electrode with IL and CB, a significantly enhanced voltammetric response was achieved toward the Allura red irreversible oxidation reaction. The type and amount of IL employed in the electrode modification step as well as all the others experimental parameters affecting the sensor response by square-wave adsorptive anodic stripping voltammetry (SWAdASV) were systematically optimized. Under the optimum experimental conditions, the proposed SWAdASV procedure provided a linear analytical curve in the concentration range of 3.98 × 10-8 to 9.09 × 10-7 mol L-1 and a low limit of detection of 9.1 × 10-10 mol L-1 (0.91 nmol L-1). The proposed sensor presented good precision and no matrice effects as shown from repeatability tests, concomitant studies and addition/recovery assays. The developed SWAdASV procedure was applied successfully in the determination of Allura red content in commercial soft drink powder samples, and the results were in close agreement with those obtained using a comparative spectrophotometric method at a confidence level of 95%.

19.
Talanta ; 206: 120252, 2020 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-31514822

RESUMO

A new electrochemical device based on a combination of nanomaterials such as Printex 6L Carbon and cadmium telluride quantum dots within a poly(3,4-ethylenedioxythiophene) polystyrene sulfonate film was developed for sensitive determination of amoxicillin. The morphological, structural and electrochemical characteristics of the nanostructured material were evaluated using X-ray diffraction, confocal microscopy, transmission electron microscopy and voltammetric techniques. The synergy between these materials increased the electrochemical activity, the electron transfer rate and the electrode surface area, leading to a high magnitude of the anodic peak current for the determination of amoxicillin. The electrochemical determination of the antibiotic was carried out using square-wave voltammetry. Under the optimised experimental conditions, the proposed sensor showed high sensitivity, repeatability and stability to amoxicillin determination, with an analytical curve in the amoxicillin concentration range from 0.90 to 69 µmol L-1, and a low detection limit of 50 nmol L-1. No significant interference in the electrochemical signal of amoxicillin was observed from potential biological interferences and drugs widely used, such as uric acid, paracetamol, urea, ascorbic acid and caffeine. It was demonstrated that without any sample pre-treatment and using a simple measurement device, the sensor could be an alternative method for not only the analysis of pharmaceutical products (commercial tablets) and clinical samples (urine), but also to examine food quality (milk samples).


Assuntos
Amoxicilina/análise , Antibacterianos/análise , Pontos Quânticos/química , Amoxicilina/urina , Animais , Antibacterianos/urina , Compostos Bicíclicos Heterocíclicos com Pontes/química , Compostos de Cádmio/química , Carbono/química , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Eletrodos , Contaminação de Alimentos/análise , Limite de Detecção , Leite/química , Polímeros/química , Poliestirenos/química , Telúrio/química
20.
Mater Sci Eng C Mater Biol Appl ; 103: 109825, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31349512

RESUMO

A new biomimetic sensor was prepared on carbon paste with magnetic molecularly imprinted polymer (mag-MIP) for sensitive and selective detection of methyl green dye. The mag-MIP was synthesized using a functional monomer that was selected before by computational simulation. A mag-NIP (magnetic non-imprinted polymer) control material was also prepared for comparative purposes. Modeling adsorption studied revealed that the dye-polymer interface followed pseudo-first order kinetics and that maximum adsorption (Qm) of the dye on mag-MIP was 3.13 mg g-1, while the value for mag-NIP was 1.58 mg g-1. The selective material was used as a sensing spot in fabrication of an electrochemical sensor based on modified carbon paste. For electrochemical analysis, the best achievement of the sensor was acquire by tack together a paste with 6.7% (w/w) of mag-MIP and using square-wave adsorptive anodic stripping voltammetry (SWAdASV) in 0.1 mol L-1 phosphate buffer (pH 7.0), with an applied potential (Eappl) of 0.3 V vs. Ag|AgClsat during an adsorption time (Tads) of 120 s. The results were obtained under optimized conditions in which sensor provided a linear concentration range of methyl green from 9.9 × 10-8 to 1.8 × 10-6 mol L-1, with a limit of detection (LOD) of 1.0 × 10-8 mol L-1 and a satisfactory relative standard deviation (RSD) of 4.3% (n = 15). The proposed sensor was applying using two spiked river water samples, obtaining recoveries ranging from 93% to 103%. The proposed method exhibits excellent precision also high reliability and proved to be an alternative method for the quantification of methyl green in real samples.


Assuntos
Materiais Biomiméticos/química , Técnicas Eletroquímicas , Fenômenos Magnéticos , Verde de Metila/análise , Impressão Molecular , Cinética
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