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1.
Mikrochim Acta ; 191(5): 280, 2024 04 22.
Artigo em Inglês | MEDLINE | ID: mdl-38649540

RESUMO

An interfacial galvanic replacement strategy to controllable synthesize palladium nanoparticles (Pd NPs)-modified NiFe MOF nanocomposite on nickel foam, which served as an efficient sensing platform for quantitative determination of dopamine (DA). Pd NPs grown in situ on the nanosheets of NiFe MOF via self-driven galvanic replacement reaction (GRR) and well uniform distribution was achieved. This method effectively reduced the aggregation of metallic nanoparticles and significantly promoted the electron transfer rate during the electrochemical process, leading to improved electrocatalytic activity for DA oxidation. Remarkably, the precisely constructed biosensor achieved a low detection limit (LOD) of 0.068 µM and recovery of 94.1% (RSD 6.7%, N = 3) for simulated real sample detection and also exhibited superior selectivity and stability. The results confirmed that the as-fabricated Pd-NiFe/NF composite electrode could realize the quantitative determination of DA and showed promising prospects in real sample biosensing.


Assuntos
Técnicas Biossensoriais , Dopamina , Estruturas Metalorgânicas , Nanoestruturas , Dopamina/análise , Nanoestruturas/química , Nanoestruturas/ultraestrutura , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/normas , Níquel/química , Eletrodos/normas , Paládio/química , Técnicas Biossensoriais/instrumentação , Técnicas Biossensoriais/métodos , Microscopia Eletrônica de Varredura , Estruturas Metalorgânicas/síntese química , Estruturas Metalorgânicas/ultraestrutura , Sensibilidade e Especificidade , Condutividade Elétrica , Microscopia Eletrônica de Transmissão , Ferro/química , Reprodutibilidade dos Testes
2.
Food Chem ; 338: 127851, 2021 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-32836002

RESUMO

Trans-resveratrol (TRA) possesses a variety of pharmacological activities, making important to explore simple, inexpensive, and reliable analytical methods for identification and quantification of it. We report on the synergistic effects originated from layer-by-layer films of graphene (Gr)-gold nanoparticles (Au) and molecularly imprinted polymers (MIPs) modified glassy carbon electrode (GCE) for electrochemical detection of TRA. To construct the TRA electrochemical sensor (GCE|Gr-Au/MIPs), the films of Gr-Au, MIPs were step by step formed onto GCE via in-situ and controllable electrodeposition and polymerization processes. The compositions, morphologies, and electrochemical properties of obtained films were investigated by various methods. Under the optimized experimental conditions, the electrochemical sensor showed superior performance toward selective and sensitive determination of TRA with K3[Fe(CN)6] as electrochemical signal probe. The electrochemical sensor was applied to determine TRA in real samples with good accuracy and recovery, verifying the broad and practical application prospects for foods and medicines analysis.


Assuntos
Técnicas Eletroquímicas/métodos , Resveratrol/análise , Calibragem , Carbono/química , Técnicas Eletroquímicas/normas , Eletrodos , Ferricianetos/química , Análise de Alimentos , Ouro/química , Grafite/química , Isomerismo , Nanopartículas Metálicas/química , Impressão Molecular , Reprodutibilidade dos Testes , Resveratrol/normas
3.
Sci Rep ; 10(1): 21077, 2020 12 03.
Artigo em Inglês | MEDLINE | ID: mdl-33273679

RESUMO

The tellurium doped zinc imidazole framework (Te@ZIF-8) is prepared by a two-step hydrothermal strategy for the electrochemical sensing of hydrogen peroxide. Material is characterized by transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The electrochemical characterization of the MOF modified electrode is done by a three-electrode system. Electrochemical sensing of hydrogen peroxide is made by cyclic voltammetry, amperometry, and impedance measurements. Results demonstrate that Te@ZIF-8 shows a detection limit of 60 µM with linearity up to 0.98855. Material is stable to 1000 cycles with no significant change in electrochemical response. Amperometry depicts the recovery of hydrogen peroxide from human serum up to 101%. Impedance curve reveals the surface of Te@ZIF-8-GCE (glassy carbon electrode) as porous and rough and an interface is developed between analyte ions and the sensing material. Finally, the modified electrode is used for the quantitative determination of hydrogen peroxide from serum samples of pancreatic cancer patients, diagnosed with CA 19-9.


Assuntos
Técnicas Eletroquímicas/métodos , Peróxido de Hidrogênio/sangue , Estruturas Metalorgânicas/química , Neoplasias Pancreáticas/sangue , Telúrio/química , Zinco/química , Análise Química do Sangue/instrumentação , Análise Química do Sangue/métodos , Análise Química do Sangue/normas , Células Cultivadas , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/normas , Eletrodos , Humanos , Imidazóis/química , Limite de Detecção
4.
Mikrochim Acta ; 187(4): 239, 2020 03 18.
Artigo em Inglês | MEDLINE | ID: mdl-32189141

RESUMO

In order to overcome the antibody-based sensor's shortcomings, an electrochemical aptamer (Apt)-based sensor was developed for amyloid-ß40 oligomer (Aß40-O). The aptasensor was constructed by locating Apt and ferrocence (Fc) on streptavidin-modified gold (SA-gold) nanoparticles. The obtained AptFc@SA-gold nanoparticles were linked onto the Au electrode via the connection of double-stranded DNA (dsDNA) as a "conductive spring." The determination of Aß40-O was performed with square-wave voltammetry (SWV). Upon bio-recognition between Apt and Aß40-O, the conformation of Apt changed and the formed Apt/Aß40-O complex separated from the SA-gold surface. As a result, the surface charge of SA-gold positively shifted, weakening the electrostatic attraction between the SA-gold and the positively charged Au electrode surface (at potential range of 0.1~0.5 V, corresponding to the Fc redox transformation), and stretching the dsDNA chain. Based on the exponential decay of dsDNA's electron transfer efficiency on its chain stretching, the oxidation current density from Fc decreased and displayed linear correlation to the concentration of Aß40-O. A wide linear range of 0.100 nM to 1.00 µM with a low detection limit of 93.0 pM was obtained. The aptasensor displayed excellent selectivity toward Aß40-O in contrast to other possible interfering analogs (Aß40 monomer, Aß42 monomer, and oligomer) at × 100 higher concentrations. The recoveries for Aß40-O-spiked artificial cerebrospinal fluid and healthy human serum were 94.0~104% and 92.8~95.4%, respectively. The electrochemical aptasensor meets the demands of clinic determination of Aß40-O, which is significant for the early diagnosis of AD. Graphical abstract Schematic representation of the electrochemical aptasensor for amyloid-ß oligomer based on the surface charge change induced by target binding.


Assuntos
Peptídeos beta-Amiloides/análise , Aptâmeros de Nucleotídeos/química , DNA/química , Técnicas Eletroquímicas/métodos , Doença de Alzheimer/diagnóstico , Técnicas Eletroquímicas/normas , Ouro , Humanos , Limite de Detecção , Nanopartículas Metálicas/química , Oxirredução
5.
Biosens Bioelectron ; 155: 112093, 2020 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-32217332

RESUMO

Biosensor development exploiting various transduction principles is characterized by a strong competition to reach high detectability, portability and robustness. Nevertheless, a literature-based comparison is not possible, as different conditions are employed in each paper. Herein, we aim at evaluating which measurement, photons or electrons, yields better biosensor performance. Upon outlining an update in recent achievements to boost analytical performance, amperometry and chemiluminescence (CL)-based biosensors are directly compared employing the same biospecific reagents and analytical formats. Horseradish peroxidase (HRP) and hydrogen peroxide concentrations were directly measured, while glucose and mouse IgG were detected employing an enzyme paper-based biosensor and an immunosensor, respectively. Detectability was down to picomoles of hydrogen peroxide (4 pmol for CL and 210 pmol for amperometry) and zeptomoles of HRP (45 zmol for CL and 20 zmol for amperometry); IgG was detected down to 12 fM (CL) and 120 fM (amperometry), while glucose down to 17 µM (CL) and 40 µM (amperometry). Results showed that amperometric and CL biosensors offered similar detectability and analytical performance, with some peculiarities that suggest complementary application fields. As they generally provided slightly higher detectability and wider dynamic ranges, CL-based biosensors appear more suitable for point-of-care testing of clinical biomarkers, where detectability is crucial. Nevertheless, as high detectability in CL biosensors usually requires longer acquisition times, their rapidity will allocate electrochemical biosensors in real-time monitoring and wearable biosensors. The analytical challenge demonstrated that these biosensors have competitive and similar performance, and between photons and electrons the competition is still open.


Assuntos
Técnicas Biossensoriais/métodos , Técnicas Biossensoriais/normas , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/normas , Eletroquímica/métodos , Eletroquímica/normas , Elétrons , Medições Luminescentes/métodos , Medições Luminescentes/normas , Fótons , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
6.
Biosens Bioelectron ; 155: 112111, 2020 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-32217334

RESUMO

Electrochemical biosensors possess numerous desirable qualities for target detection, such as portability and ease of use, and are often considered for point-of-care (POC) development. Label-free affinity electrochemical biosensors constructed with semiconductor manufacturing technology (SMT)-produced electrodes and a streptavidin biomediator currently display the highest reproducibility, accuracy, and stability in modern biosensors. However, such biosensors still do not meet POC guidelines regarding these three characteristics. The purpose of this research was to resolve the limitations in reproducibility and accuracy caused by problems with production of the biosensors, with the aim of developing a platform capable of producing devices that exceed POC standards. SMT production settings were optimized and bioreceptor immobilization was improved through the use of a unique linker, producing a biosensor with exceptional reproducibility, impressive accuracy, and high stability. Importantly, the three characteristics of the sensors produced using the proposed platform all meet POC standards set by the Clinical and Laboratory Standards Institute (CLSI). This suggests possible approval of the biosensors for POC development. Furthermore, the detection range of the platform was demonstrated by constructing biosensors capable of detecting common POC targets, including circulating tumor cells (CTCs), DNA/RNA, and curcumin, and the devices were optimized for POC use. Overall, the platform developed in this study shows high potential for production of POC biosensors.


Assuntos
Técnicas Biossensoriais/normas , Técnicas Eletroquímicas/normas , Testes Imediatos/normas , Técnicas Biossensoriais/instrumentação , Técnicas Biossensoriais/métodos , Curcumina/análise , DNA/análise , Eletrodos , Humanos , RNA/análise , Reprodutibilidade dos Testes
7.
Mikrochim Acta ; 187(4): 245, 2020 03 24.
Artigo em Inglês | MEDLINE | ID: mdl-32211982

RESUMO

A disposable screen-printed carbon electrode (SPCE) modified with an ionic liquid/graphene composite (IL/G) exhibits a wider potential window, excellent conductivity, and specific surface area for the improvement in the voltammetric signal of rapamycin detection. The modified composite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). The electrochemical behavior of rapamycin at the modified SPCE was investigated by cyclic and square wave voltammetry in 60:40 EtOH: 0.1 M LiClO4 at pH 5.0. A high reproducible and well-defined peak with a high peak current were obtained for rapamycin detection at a position potential of + 0.98 V versus Ag/AgCl. Under the optimized conditions, the rapamycin concentration in the range 0.1 to 100 µM (R2 = 0.9986) had a good linear relation with the peak current. The detection limit of this method was 0.03 µM (3SD/slope). The proposed device can selectively detect rapamycin in the presence of commonly interfering compounds. Finally, the proposed method was successfully applied to determine rapamycin in urine and blood samples with excellent recoveries. These devices are disposable and cost-effective and might be used as an alternative tool for detecting rapamycin in biological samples and other biological compounds. Graphical abstract Schematic presentation of wide electrochemical window and disposable screen-printed sensor using ionic liquid/graphene composite for the determination of rapamycin. This composite can enhance the oxidation current and expand the potential for rapamycin detection.


Assuntos
Técnicas Eletroquímicas/métodos , Sirolimo/análise , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/normas , Eletrodos , Grafite , Líquidos Iônicos , Limite de Detecção , Sirolimo/sangue , Sirolimo/urina
8.
Mikrochim Acta ; 187(1): 79, 2020 01 02.
Artigo em Inglês | MEDLINE | ID: mdl-31897733

RESUMO

A copper(II) benzene-1,3,5-tricarboxylate (BTC) metal-organic framework (MOF) was modified with poly(acrylic acid) (PAA) and then used in an electrochemical sensor for vancomycin. The MOF, synthesized via a single-pot method, has enhanced solubility and dispersibility in water as compared to HKUST-1 but without compromising its crystallinity and porosity. The MOF was placed on a glassy carbon electrode (GCE) where it shows enhanced electrocatalytic properties. This is assumed to be due to the presence of the poly(acrylic acid) that forms a network between various HKUST-1 crystals through dimer formation between the carboxy groups of BTC and PAA. This also led to better dispersion of the MOF and to improved interaction between MOF and vancomycin. The structural, spectral and electrochemical properties of the MOFs and their vancomycin complexes was characterized. The modified GCE is shown to be a viable tool for electrochemical determination (best at a working potential of 784 mV vs. Ag/AgCl) of the antibiotic vancomycin in spiked urine and serum samples. Response is linear in the 1-500 nM vancomycin concentration range, and the detection limit is 1 nM, with a relative standard deviation of ±4.3%. Graphical abstractSchematic representation of a method for determination of vancomycin. Poly(acrylic acid) modified HKUST-1 (P-HKUST-1) forms a complex with vancomycin [Van-P-HKUST-1] which is coated over glassy carbon electrode (GCE). The decrease in peak current is recorded as response to vancomycin via cyclic voltammetry.


Assuntos
Resinas Acrílicas/química , Cobre/química , Técnicas Eletroquímicas/métodos , Estruturas Metalorgânicas/química , Vancomicina/análise , Carbono , Técnicas Eletroquímicas/normas , Eletrodos , Solubilidade , Vancomicina/sangue , Vancomicina/urina
9.
Mikrochim Acta ; 187(1): 80, 2020 01 02.
Artigo em Inglês | MEDLINE | ID: mdl-31897753

RESUMO

Multiwalled carbon nanotubes coated with cobalt(II) sulfide nanoparticles were prepared and used for immobilization of glucose oxidase (GOx) to obtain an electrochemical glucose biosensor. The nanocomposite was synthesized through an in-situ hydrothermal method and characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and electrochemical impedance spectroscopy. The results show that the nanocomposite possesses a large specific surface area and apparently enhances the direct electron transfer between GOx and the surface of the electrode, best at a potential near -0.43 V (vs. SCE). The immobilized GOx retains its good bioactivity even at a high surface coverage of 30 pmol cm-2. Under the optimum conditions. The biosensor exhibits a wide linear range (from 8 µM to 1.5 mM), a high sensitivity (15 mA M -1 cm-2), and a 5 µM detection limit (at S/N = 3). The sensor is selective, acceptably repeatable, specific and stable. Graphical abstractMultiwalled carbon nanotubes coated with cobalt(II) sulfide nanoparticles (CoS-MWCNTs) were synthesized through in situ hydrothermal method for the construction of a sensitive electrochemical glucose biosensor.


Assuntos
Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Glucose Oxidase/metabolismo , Glucose/análise , Nanotubos de Carbono/química , Técnicas Biossensoriais/normas , Cobalto , Técnicas Eletroquímicas/normas , Elétrons , Enzimas Imobilizadas/metabolismo , Nanopartículas/química
10.
Mikrochim Acta ; 187(1): 92, 2020 01 03.
Artigo em Inglês | MEDLINE | ID: mdl-31900660

RESUMO

A facile and highly sensitive biosensor was developed for the determination of hydrogen peroxide (H2O2) via electrochemical catalytic reduction of H2O2 by hemoglobin (Hb). Hb was enriched and immobilized simply in a chitosan (Chit) membrane on a magnetic electrode to construct an enzyme-like biosensor. The biosensor catalyzes the electrochemical reduction of H2O2 under an external magnetic field. The response improved roughly twice as Hb was adsorbed by Chit in an alkaline medium. The response of the biosensor under the magnetic field increased by 16% owing to the paramagnetism of Hb. The effect of pH values on Hb adsorption by Chit, as well as the effect of an external magnetic field on Hb configuration were investigated by UV-vis spectroscopy. The reduction peak current has linear and log-linear relationships with H2O2 concentration in the range of 5-250 µmol∙L-1 and 0.01-1 µmol∙L-1, respectively. The detection limit was 0.003 µmol∙L-1, with a good sensitivity of 0.227 µA∙µM-1∙cm-2. The biosensor was successfully applied to the determination of H2O2 in milk samples and in disinfectant solutions. Recoveries ranged from 96.3 to 105.4%, and from 95.3 to 107.7%, respectively. Graphical abstractConstruction of the biosensor, and principle of H2O2 determination based on Hb bioelectrocatalysis.


Assuntos
Técnicas Biossensoriais/métodos , Hemoglobinas/química , Peróxido de Hidrogênio/análise , Animais , Técnicas Biossensoriais/normas , Desinfetantes/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/normas , Eletrodos , Magnetismo , Leite/química , Oxirredução , Espectrofotometria Ultravioleta
11.
Mikrochim Acta ; 187(1): 95, 2020 01 06.
Artigo em Inglês | MEDLINE | ID: mdl-31903507

RESUMO

To increase the sensitivity of electrochemical sensor, Fe-MIL-88B-NH2 (Fe-MOF) with peroxidase-like activity is designed for the construction of immunoprobe. The Fe-MOF was prepared by one-step hydrothermalf method using 2-aminoterephthalic acid and iron(III) chloride. For the immunoprobe, it was fabricated by gold nanocomposite/Fe-MOF (Au/Fe-MOF) for the immobilization of labeling antibody (the antibody was used to conjuncting with label materials). The thin layer of Methylene Blue (MB) covered by reduced graphene oxide-gold nanocomposites (Au-rGO) serves as a substrate to covalently fix coating antibodies. The MB as a redox-active species was modified on the glass carbon electrode that can give a strong amperometric signal at 0.18 V (vs. Ag/AgCl). With the participation of H2O2, Fe-MOF can induce the Fenton reaction which degrades MB covered by Au-rGO on the substrate. The rest of MB on the surface of electrode becomes oxidized thereby generating a current signal. Square wave voltammetry (SWV) was used to quantify PSA. Under optimal conditions, the immunoassay is stable, specific and reproducible. It has a lower detection limit of 0.13 pg mL-1 (S/N = 3) and a wide analytical range that extends from 0.001 to 100 ng mL-1. Graphical abstractA sandwich-type amperometric immunoassay based on Fe-MOF-induced Fenton reaction was designed for sensitive determination of prostate specific antigen.


Assuntos
Técnicas Eletroquímicas/métodos , Calicreínas/análise , Estruturas Metalorgânicas/química , Nanocompostos/química , Peroxidase/metabolismo , Antígeno Prostático Específico/análise , Anticorpos Imobilizados/imunologia , Técnicas Eletroquímicas/normas , Eletrodos , Ouro , Humanos , Peróxido de Hidrogênio/química , Ferro , Calicreínas/imunologia , Azul de Metileno/química , Mimetismo Molecular , Oxirredução , Antígeno Prostático Específico/imunologia
12.
Mikrochim Acta ; 187(1): 94, 2020 01 04.
Artigo em Inglês | MEDLINE | ID: mdl-31902014

RESUMO

Poly(3,4-ethylenedioxythiophene) (PEDOT) films were electrodeposited by cyclic voltammetry on a glassy carbon electrode (GCE) in aqueous solution. Three kinds of supporting electrolytes were used, viz. graphene oxide (GO), phosphate buffered saline (PBS), and GO in PBS, respectively. The surface morphology of the modified electrodes was characterized by scanning electron microscopy. The electrochemical performance of the modified electrodes was investigated by cyclic voltammetry and electrochemical impedance spectroscopy by using the hexacyanoferrate redox system. The results demonstrate that the PEDOT-GO/GCE, which was electropolymerized in aqueous solutions containing EDOT and GO, shows the best electrochemical activities compared with other modified electrodes. The electrochemical behaviors of ascorbic acid (AA), dopamine (DA) and uric acid (UA) were investigated by cyclic voltammetry. The PEDOT-GO/GCE exhibits enhanced electrocatalytic activities towards these important biomolecules. Under physiological pH conditions and in the mixed system of AA, DA and UA, the modified GCE exhibits the following figures of merit: (a) a linear voltammetric response in the concentration ranges of 100-1000 µM for AA, 6.0-200 µM for DA, and 40-240 µM for UA; (b) well separated oxidation peaks near 31, 213 and 342 mV (vs. saturated Ag/AgCl) for AA, DA and UA, respectively; and (c) detection of limits (at S/N = 3) of 20, 2.0 and 10 µM. The results demonstrate that GO, based on its relatively large number of anionic sites, can be used as the sole weak electrolyte and charge balance dopant for the preparation of functionally doped conducting polymers by electrodeposition. Graphical abstractSchematic representation of a nanostructure composed of hybrid conducting polymer PEDOT-GO nanocomposites, and its application to simultaneous determination of ascorbic acid, dopamine and uric acid.


Assuntos
Ácido Ascórbico/análise , Dopamina/análise , Técnicas Eletroquímicas/métodos , Ácido Úrico/análise , Compostos Bicíclicos Heterocíclicos com Pontes , Técnicas Eletroquímicas/normas , Eletrodos , Galvanoplastia/métodos , Ferrocianetos/química , Grafite , Oxirredução , Polímeros
13.
Mikrochim Acta ; 187(1): 97, 2020 01 06.
Artigo em Inglês | MEDLINE | ID: mdl-31907624

RESUMO

A stable and enzyme-free method is described for highly sensitive determination of telomerase activity. It is based on the use of a framework nucleic acid (FNA) nanomachine and doxorubicin-spherical nucleic acid (DSNA) tags. Upon incubation with telomerase, the primer-tetrahedron becomes elongated to form the handed swing arm. The extended swing arm autonomously moves along the predefined track consisting of entropy-tetrahedron by consecutive strand displacement under the aid of fuel-tetrahedron. As a result, many (entropy-tetrahedron)-(fuel-tetrahedron) complexes are assembled for combining the DSNA tags. This results in an amplified electrochemical signal, typically measured at around -0.63 V (Ag/AgCl). The use of an enzyme-free FNA nanomachine and of DSNA tags warrants outstandingly high stability and sensitivity. The method shows a broad dynamic correlation of telomerase activity in cell extracts. The analytical range extends from 10 to 1.0 × 104 HeLa cells mL-1 with a lower detection limit of 2 cells mL-1. The differences in telomerase activity between different cancer cells can be easily evaluated. The method was further verified by quantifying telomerase activity of cancer cells in accumulated normal cells. Therefore, the sensing method has great potential for clinical application. Graphical abstractSchematic representation of the electrochemical biosensor based on target induced framework nucleic acid nanomachine with doxorubicin-spherical nucleic acids (DSNA) tags, which can be used to the determination of telomerase activity in accumulated normal cells. dNTP: Deoxynucleotide triphosphates; FT: Fuel-tetrahedron.


Assuntos
Doxorrubicina/química , Técnicas Eletroquímicas/métodos , Ácidos Nucleicos/química , Telomerase/análise , Linhagem Celular Tumoral , Técnicas Eletroquímicas/normas , Células HeLa , Humanos , Nanomedicina/métodos , Neoplasias/diagnóstico , Neoplasias/enzimologia , Neoplasias/patologia , Telomerase/metabolismo
14.
Mikrochim Acta ; 187(1): 98, 2020 01 06.
Artigo em Inglês | MEDLINE | ID: mdl-31907634

RESUMO

Porous Co3S4 was synthesized by a two-step hydrothermal method, and its morphology and structure were characterized by transmission electron microscopy and X-ray diffraction. Electrochemical investigations showed that a glassy carbon electrode modified with Co3S4 exhibits high electrocatalytic activity toward glucose in 0.2 M NaOH solution. Figures of merit for this sensor include (i) a wide linear range (2.0 µM to 1.1 mM), (ii) a working potential near 0.52 V (vs. Ag/AgCl), (iii) high sensitivity (346.7 µA mM-1 cm-2), and (iv) a 0.17 µM detection limit. Graphical abstractPorous Co3S4 was explored as electrocatalyst for glucose oxidation. It exhibits distinctly higher electrocatalytic activity toward glucose oxidation than Co3O4.


Assuntos
Cobalto/química , Técnicas Eletroquímicas/métodos , Glucose/análise , Técnicas Eletroquímicas/normas , Eletrodos , Oxirredução , Porosidade , Hidróxido de Sódio , Soluções
15.
Chemosphere ; 238: 124669, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-31524613

RESUMO

Sugar production is a water intensive process that produces a large amount of wastewaters with high concentration of chemical oxygen demand (COD), mostly consists of organic carbon compounds. Conventional treatment methods are limited to provide the necessary treatment of effluent COD to meet the regulatory limits prior to discharge. The treatment performance of electrooxidation (EO) and electrochemical peroxidation (ECP) for organic removal were investigated in a laboratory scale study. The experimental conditions were optimized for both EO and ECP using Box-Behnken Design (BBD) and the models provided highly significant quadratic models for both treatment methods. The effects of pH, H2O2 dosage, current density, and operation time were investigated using BBD. The results showed that EO could remove 75% of organics at optimum conditions of pH 5.3; current density of 48.5 mA cm-2; and operation time of 393 min. The predicted values were in reasonable agreement with measured values. ECP could remove total and soluble COD and total and dissolved organic carbon by 65, 64, 66, and 63%, respectively at optimum conditions of H2O2 dosage of 21 mL L-1; current density of 48 mA cm-2; and operation time of 361 min. The methods were compared based on removal efficiency and energy consumption during operation.


Assuntos
Beta vulgaris/química , Técnicas Eletroquímicas/métodos , Eliminação de Resíduos Líquidos/métodos , Águas Residuárias/química , Purificação da Água/métodos , Análise da Demanda Biológica de Oxigênio , Técnicas Eletroquímicas/normas , Peróxido de Hidrogênio , Indústrias , Compostos Orgânicos , Oxirredução , Açúcares , Eliminação de Resíduos Líquidos/normas , Poluentes Químicos da Água/química , Purificação da Água/normas
16.
Mikrochim Acta ; 186(8): 573, 2019 07 24.
Artigo em Inglês | MEDLINE | ID: mdl-31342189

RESUMO

An electrochemical sensor is described for simultaneous voltammetric determination of dopamine (DA) and uric acid (UA). It is based on the use of a nanomaterial composed of gold nanoparticles and 3-dimensional graphene (Au NP@3D GR). The 3D GR was prepared by chemical vapor deposition using nickel nanoparticles as the template at a temperature of around 900 °C. The surface of 3D GR contains oxygen-functional groups after treatment with acid. Carboxylated Au NP were self-assembled and anchored onto the surface of 3D GR. The nanomaterial was placed on a ITO electrode. The few-layer graphene on the ITO glass has a porous structure and the distribution of Au NP is uniform. The electrode shows a high sensitivity and a low detection limit for DA and UA. Figures of merit include detection limits of 0.1 M for DA and of 0.1 µM for UA, and well separated peaks at potentials of 0.18 and 0.30 V (vs. Ag/AgCl), respectively, at pH 7.0. The electrode has good repeatability and stability. Graphical abstract Carboxylated gold nanoparticles were self-assembled and immobilized on 3-dimensional graphene by chemical vapor deposition for simultaneous determination of dopamine (DA) and uric acid (UA).


Assuntos
Dopamina/análise , Técnicas Eletroquímicas/métodos , Grafite/química , Nanopartículas Metálicas/química , Ácido Úrico/análise , Animais , Técnicas Eletroquímicas/normas , Eletrodos/normas , Ouro/química , Humanos , Limite de Detecção , Reprodutibilidade dos Testes
17.
Sci Rep ; 9(1): 6642, 2019 04 30.
Artigo em Inglês | MEDLINE | ID: mdl-31040350

RESUMO

The SELEX (Systematic Evolution of Ligands by EXponential enrichment) method has been used successfully since 1990, but work is still required to obtain highly specific aptamers. Here, we present a novel approach called 'Competitive non-SELEX' (and termed as 'SELCOS' (Systematic Evolution of Ligands by COmpetitive Selection)) for readily obtaining aptamers that can discriminate between highly similar targets. This approach is based on the theoretical background presented here, in which under the co-presence of two similar targets, a specific binding type can be enriched more than a nonspecifically binding one during repetitive steps of partitioning with no PCR amplification between them. This principle was experimentally confirmed by the selection experiment for influenza virus subtype-specific DNA aptamers. Namely, the selection products (pools of DNA aptamers) obtained by SELCOS were subjected to a DEPSOR-mode electrochemical sensor, enabling the method to select subtype-specific aptamer pools. From the clonal analysis of these pools, only a few rounds of in vitro selection were sufficient to achieve the surprisingly rapid enrichment of a small number of aptamers with high selectivity, which could be attributed to the SELCOS principle and the given selection pressure program. The subtype-specific aptamers obtained in this manner had a high affinity (e.g., KD = 82 pM for H1N1; 88 pM for H3N2) and negligible cross-reactivity. By making the H1N1-specific DNA aptamer a sensor unit of the DEPSOR electrochemical detector, an influenza virus subtype-specific and portable detector was readily constructed, indicating how close it is to the field application goal.


Assuntos
Aptâmeros de Nucleotídeos , Técnicas Biossensoriais , Técnicas Eletroquímicas , Técnica de Seleção de Aptâmeros , Técnicas Biossensoriais/métodos , Técnicas Biossensoriais/normas , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/normas , Conformação de Ácido Nucleico
18.
J Immunol Methods ; 470: 6-14, 2019 07.
Artigo em Inglês | MEDLINE | ID: mdl-31004579

RESUMO

Enterotoxigenic Escherichia coli (ETEC) is a leading cause of bacterial diarrhea both among children in low and middle income countries and in travelers to these regions. Although there are several approaches to develop an effective vaccine for ETEC, no licensed vaccines are currently available. The most advanced ETEC vaccine candidates include multiple colonization factors along with the heat labile toxin B subunit. In the absence of known correlates of protection, and to understand the mechanism of protection, monitoring immune responses to a majority of the vaccine associated antigens using various types of samples is needed. Unfortunately, a traditional ELISA is time consuming, labor intensive and requires substantial amounts of antigens and sample volumes. To address these constraints, we developed and validated a novel high throughput electrochemiluminescent (ECL) - based multiplex immunoassay using Meso Scale Discovery (MSD) platform for analyzing immune responses to ETEC antigens. The ETEC multiplex ECL assay is an 8-plex assay which includes the ETEC colonization factor antigens (CFA/I, CS1, CS2, CS3, CS5 and CS6) along with the two subunits of heat labile toxin (LTA and LTB). Our data suggested that a single dilution of sample provides a quantifiable result for a wide range of sample titers. To compare ETEC multiplex ECL with ELISA, we carried out assays using the same antigens with the two immunoassay platforms using a common sample set of serum and ALS (antibodies in lymphocyte supernatant) specimens. The MSD platform achieved excellent correlations with ELISA for the antigens tested, consistently detecting comparable antibody levels in the samples. The ETEC multiplex ECL can serve as a fundamental platform in evaluating performances of candidate ETEC vaccines in future field trials.


Assuntos
Anticorpos Antibacterianos/sangue , Técnicas Eletroquímicas/métodos , Escherichia coli Enterotoxigênica/imunologia , Vacinas contra Escherichia coli/análise , Imunoensaio/métodos , Medições Luminescentes/métodos , Antígenos de Bactérias/química , Antígenos de Bactérias/imunologia , Toxinas Bacterianas/química , Toxinas Bacterianas/imunologia , Técnicas Eletroquímicas/normas , Infecções por Escherichia coli/imunologia , Infecções por Escherichia coli/microbiologia , Infecções por Escherichia coli/prevenção & controle , Proteínas de Escherichia coli/química , Proteínas de Escherichia coli/imunologia , Humanos , Soros Imunes/química , Imunoensaio/normas , Luminescência , Medições Luminescentes/normas , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
19.
J Immunol Methods ; 470: 55-58, 2019 07.
Artigo em Inglês | MEDLINE | ID: mdl-31034878

RESUMO

FMS related tyrosine kinase 3 (FLT-3) is a tyrosine kinase expressed in early hematopoietic precursor cells and has roles in survival, proliferation, and differentiation. Bone marrow expression and mutagenic analysis of FLT-3 in Acute Myeloid Leukemia (AML) patients is well-characterized. However, the levels of circulating FLT-3 in serum have not been previously described. In this study we describe a quantitative electrochemiluminescent immunoassay that detects FLT-3 in human serum. Using this method we find that AML patients have elevated levels of circulating FLT-3 and these levels correlated to the percent blast counts in the bone marrow (BM).


Assuntos
Biomarcadores Tumorais/sangue , Técnicas Eletroquímicas/métodos , Imunoensaio/métodos , Leucemia Mieloide Aguda/diagnóstico , Medições Luminescentes/métodos , Tirosina Quinase 3 Semelhante a fms/sangue , Adulto , Idoso , Idoso de 80 Anos ou mais , Biomarcadores Tumorais/genética , Medula Óssea/enzimologia , Medula Óssea/patologia , Técnicas Eletroquímicas/normas , Feminino , Expressão Gênica , Humanos , Imunoensaio/normas , Leucemia Mieloide Aguda/sangue , Leucemia Mieloide Aguda/genética , Leucemia Mieloide Aguda/patologia , Luminescência , Medições Luminescentes/normas , Masculino , Pessoa de Meia-Idade , Variações Dependentes do Observador , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Tirosina Quinase 3 Semelhante a fms/genética
20.
Anal Chem ; 91(5): 3754-3758, 2019 03 05.
Artigo em Inglês | MEDLINE | ID: mdl-30761889

RESUMO

For the screening of novel toxic-element-free and biocompatible electrochemiluminophores, electrochemiluminescence (ECL) of multinary nanocrystals (NCs) was investigated for the first time with Zn-Ag-In-S (ZAIS) NCs as model. Aqueous soluble ZAIS NCs could bring out efficient reductive-oxidation ECL with tri- n-propylamine as coreactant, while coating the ZAIS NCs with a ZnS shell could reduce the surface defects of ZAIS NCs, and enable 6.7-fold enhanced ECL of ZAIS/ZnS NCs as compared to ZAIS NCs. ECL of ZAIS/ZnS NCs was about 4.2-fold that of ternary CuInS2/ZnS NCs, spectrally similar to that of Ru(bpy)32+ with maximum emission around 605 nm, and favorable for less electrochemical interference with a lowered triggering potential (∼0.95 V) than that of Ru(bpy)32+. An ultrasensitive ECL microRNA sensor was fabricated with ZAIS/ZnS NCs as tags, which could sensitively and selectively determine microRNA-141 with a wide linearity range from 0.1 fmol/L to 20 pmol/L and a low limit of detection at 50 amol/L ( S/ N = 3). Multinary NCs might provide a promising alternative to the traditional binary NCs for both electrochemiluminophore screening and NC ECL modulating.


Assuntos
Técnicas Eletroquímicas/métodos , Medições Luminescentes/métodos , MicroRNAs/análise , Animais , Técnicas Eletroquímicas/normas , Humanos , Limite de Detecção , Medições Luminescentes/normas , Nanopartículas/química , Propilaminas , Prata , Sulfetos , Compostos de Zinco
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