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1.
Anal Chem ; 94(4): 2263-2270, 2022 02 01.
Artigo em Inglês | MEDLINE | ID: mdl-35050594

RESUMO

Here, we present a wearable potentiometric ion sensor for real-time monitoring of sodium ions (Na+) in human sweat samples using Na0.44MnO2 as the sensing material. Na0.44MnO2 is an attractive material for developing wearable electrochemical sensors due to its good Na+ incorporation ability, electrical conductivity, stability, and low fabrication cost. In the first step, the analytical performance of the electrode prepared using Na0.44MnO2 is presented. Then, a miniaturized potentiometric cell integrated into a wearable substrate is developed, which reveals a Nernstian response (58 mV dec-1). We achieved the detection of Na+ in the linear ranges of 0.21-24.54 mmol L-1, which is well within the physiological range of Na+. Finally, for on-body sweat analysis, the potentiometric sensor is fully integrated into a headband textile. This platform can be employed for non-invasive analysis of Na+ in human sweat for healthcare and disease diagnosis.


Assuntos
Técnicas Biossensoriais , Dispositivos Eletrônicos Vestíveis , Humanos , Íons , Compostos de Manganês , Óxidos , Sódio , Suor
2.
Mikrochim Acta ; 190(1): 37, 2022 12 26.
Artigo em Inglês | MEDLINE | ID: mdl-36571644

RESUMO

It was demonstrated that the mechanism of the inner filter effect (IFE) can emerge well in the resonance Rayleigh scattering (RRS) technique and be utilized as a new analytical method in the design of innovative IFE-based sensors. To prove this process, silver nanocubes (Ag NCs) with tunable extinction spectra were selected as RRS probes, and three analytes, doxorubicin (DOX), sunitinib (SUN), and Alizarin Red S (ARS), were considered as the typical absorbers. In addition, in the presence of SUN as a typical analyte, the quenching of the RRS signal of Ag NCs, with λmax of 419 nm, was linear in the range 0.01 to 2.5 µM of SUN. The limit of detection (LOD) was 0.0025 µM. The introduced method was then used to develop a dual-signal assay for the ratiometric determination of Al3+ ions. The suggested dual-signal assay was based on the color changes of ARS caused by Al3+ and the IFE between ARS and Ag NCs. The obtained results showed that the two characteristics of response sensitivity and linear dynamic range are very satisfactory for sensing Al3+ ions. The findings of this study demonstrate that the newly developed IFE mechanism can be employed as an attractive and highly efficient analytical technique for measuring different analytes.


Assuntos
Prata , Espalhamento de Radiação , Limite de Detecção , Íons
3.
Analyst ; 146(15): 4865-4872, 2021 Jul 26.
Artigo em Inglês | MEDLINE | ID: mdl-34231570

RESUMO

Achieving efficient chiral discrimination by a convenient method remains a challenge in pharmaceutical and biotechnology industries. Our aim in this paper was to develop a dual-signaling enantioselective sensing strategy based on the competitive binding assay. A combination of ß-cyclodextrin (ß-CD) and methylene blue (MB) was used as an enantioselective discrimination probe to develop a straightforward electrochemical chiral sensor using the drug naproxen (R-and S-NaX) as the representative enantiomers. The principle relied on the difference between two enantiomers in the ability to replace a pre-binding redox probe, which in turn resulted in different dual signals for the two enantiomers. The applicability of the optimized procedure was demonstrated by the analysis of NaX enantiomers in the range of 0.4-6.0 µM. Featuring both signal-on and signal-off elements, the electrode presented significantly enhanced electrochemical activity with a low limit of detection (LOD) of 0.07 µM. We expect that our work will inspire interesting engineering strategies for developing novel enantioselective electrochemical sensors.


Assuntos
Técnicas Eletroquímicas , Azul de Metileno , Eletrodos , Limite de Detecção , Estereoisomerismo
4.
Ecotoxicol Environ Saf ; 209: 111807, 2021 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-33360291

RESUMO

In the present study, both gaseous and particulate (PM with dae <2.5 µm) phases of polycyclic aromatic hydrocarbons (PAHs) were measured in the ambient air of Hamadan city, Iran. For this reason, two low-volume samplers equipped with glass fiber filters were used for sampling of particulate phase (N = 30) and XAD-2 sorbent tubes were applied for sampling gaseous phase of PAHs (N = 30). The sampling was conducted during warm and cold seasons in 2019. The average of cold/warm season ratios for Σ16PAH and PM concentrations were 1.14 and 0.62, respectively. Summed PAHs concentration were determined to be in the range 0.008-59.46 (mean: 11.61) ng/m3 and 0.05-40.83 (mean: 10.22) ng/m3 for the cold and warm seasons, respectively. A negative Pearson correlation coefficient was obtained for wind speed and relative humidity. The average Benzo (a) Pyrene equivalent carcinogenic (BaPeq) levels in the cold season were lower than the maximum permissible risk level of 1 ng/m3 for BaP. The BaP toxicity equivalency (ΣBaPTEQ) and BaP mutagenicity equivalency (ΣBaPMEQ) appeared to be significantly higher in the cold season (averaging 0.35 and 1.65 ng/m3, respectively) than those in warm season. Health risk assessment was performed for children and adults based on BaPeq, inhalation cancer risk. The diagnostic ratios of individual PAHs concentration showed that the significant sources of PAH emissions may be related to light duty vehicles (LDVs) in Hamadan. Although, some other sources such as pyrogenic source and petrol combustion were also suggested.


Assuntos
Poluentes Atmosféricos/análise , Exposição Ambiental/estatística & dados numéricos , Hidrocarbonetos Policíclicos Aromáticos/análise , Adulto , Benzo(a)pireno/análise , Carcinógenos , Criança , Cidades , Carvão Mineral , Monitoramento Ambiental , Gases , Humanos , Irã (Geográfico) , Mutagênicos , Material Particulado/análise , Medição de Risco , Estações do Ano , Vento
5.
Mikrochim Acta ; 188(9): 305, 2021 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-34448045

RESUMO

Metal-organic frameworks (MOFs) have received extensive attention in adsorption applications owing to their high surface area. However, some MOFs do not perform well as the extraction medium when used under aqueous conditions. The low hydrostability of MOFs limits the practical application of these materials in solid-phase microextraction (SPME). Here, the fabrication of a water resistance SPME fiber coating is introduced based on the crystal violet (CV)-modified HKUST-1 framework on copper (Cu@HKUST-1@CV). The HKUST-1 was prepared by the in situ growth method, followed by post-synthetic modification of HKUST-1 with the CV layer. The preparation of the modified HKUST-1 was characterized by FESEM, XRD, FTIR, and DFT approaches. The prepared SPME coating was successfully employed for the quantification of anthracene (AN), as a model analyte, in water samples. The limit of detection was 0.8 ng mL-1. The developed method will open up a new door towards searching for promising materials in SPME applications.


Assuntos
Antracenos/isolamento & purificação , Violeta Genciana/química , Estruturas Metalorgânicas/química , Microextração em Fase Sólida/métodos , Poluentes Químicos da Água/isolamento & purificação , Adsorção , Antracenos/química , Cobre/química , Água Potável/química , Limite de Detecção , Espectrometria de Fluorescência , Água/química , Poluentes Químicos da Água/química
6.
Int J Mol Sci ; 22(22)2021 Nov 19.
Artigo em Inglês | MEDLINE | ID: mdl-34830361

RESUMO

The iontophoresis delivery of insulin (INS) remains a serious challenge due to the low permeability of the drug through the skin. This work aims to investigate the potential of water-soluble polypyrrole nanoparticles (WS-PPyNPs) as a drug donor matrix for controlled transdermal iontophoresis of INS. WS-PPyNPs have been prepared via a simple chemical polymerization in the presence of sodium dodecyl sulfate (SDS) as both dopant and the stabilizing agent. The synthesis of the soluble polymer was characterized using field emission scanning electron microscopy (FESEM), dynamic light scattering (DLS), fluorescence spectroscopy, and Fourier transform infrared (FT-IR) spectroscopy. The loading mechanism of INS onto the WS-PPyNPs is based on the fact that the drug molecules can be replaced with doped dodecyl sulfate. A two-compartment Franz-type diffusion cell was employed to study the effect of current density, formulation pH, INS concentration, and sodium chloride concentration on anodal iontophoresis (AIP) and cathodal iontophoresis (CIP) of INS across the rat skin. Both AIP and CIP delivery of INS using WS-PPyNPs were significantly increased compared to passive delivery. Furthermore, while the AIP experiment (60 min at 0.13 mA cm-2) show low cumulative drug permeation for INS (about 20.48 µg cm-2); the CIP stimulation exhibited a cumulative drug permeation of 68.29 µg cm-2. This improvement is due to the separation of positively charged WS-PPyNPs and negatively charged INS that has occurred in the presence of cathodal stimulation. The obtained results confirm the potential applicability of WS-PPyNPs as an effective approach in the development of controlled transdermal iontophoresis of INS.


Assuntos
Insulina/farmacologia , Iontoforese/métodos , Nanopartículas/química , Pele/efeitos dos fármacos , Administração Cutânea , Animais , Portadores de Fármacos/química , Portadores de Fármacos/farmacologia , Humanos , Microscopia Eletrônica de Varredura , Polímeros/química , Polímeros/farmacologia , Pirróis/química , Pirróis/farmacologia , Coelhos , Pele/ultraestrutura , Dodecilsulfato de Sódio/química , Dodecilsulfato de Sódio/farmacologia , Solubilidade , Espectroscopia de Infravermelho com Transformada de Fourier , Água/química
7.
Anal Chem ; 92(6): 4209-4216, 2020 03 17.
Artigo em Inglês | MEDLINE | ID: mdl-32066241

RESUMO

Significant levels of infectious diseases caused by pathogenic bacteria are nowadays a worldwide matter, carrying considerable public health care challenges and huge economic concerns. Because of the rapid transmission of these biothreat agents and the outbreak of diseases, a rapid detection of pathogens in early stages is crucial, particularly in low-resources settings. To this aim, we developed for the first time a new sensing approach carried out in a single step for Escherichia coli O157:H7 detection. The detection principle is based on Förster resonance energy transfer using gold nanoclusters as a signal reporter and gold nanoparticles conjugated with antibodies as a quencher. The sensing platform includes an ultraviolet-light-emitting diode to provide the proper excitation and consists of a microtube containing two pieces of fiber glass; one of them is embedded with label-free gold nanoclusters and the other one with gold nanoparticles conjugated with antibodies. Upon the addition of the sample containing bacteria, the florescence of gold nanoclusters is recovered. The assay was evaluated by the naked eye (on/off) and quantitatively with use of a smartphone camera. The biosensor proved to be highly specific and sensitive, achieving a limit of detection as low as 4.0 cfu mL-1. Additionally, recoveries of 110% and 95% were obtained when the platforms in spiked river and tap water, respectively, were evaluated.


Assuntos
Técnicas Biossensoriais , Escherichia coli O157/isolamento & purificação , Sistemas Automatizados de Assistência Junto ao Leito , Ouro/química , Humanos , Nanopartículas Metálicas/química
8.
Anal Chem ; 92(16): 11405-11412, 2020 08 18.
Artigo em Inglês | MEDLINE | ID: mdl-32687322

RESUMO

This work presents an effective strategy for the well-oriented immobilization of antibodies in which boronic acid is directly attached to the surface and with no need of the long and flexible spacer. A magnetic graphene nanoribbon-boronic-acid-based immunosensor was developed and tested for the impedimetric detection of lymphoma cancer cells, a blood cancer biomarker. Magnetic graphene nanoribbons (MGNRs) were modified with boronic acid (BA) to create a supporting matrix that is utilized by immobilizing anti-CD20 antibodies with good orientation. The prepared biosensing layer (MGNR/BA/Ab) with well-oriented antibodies was premixed into whole blood samples to interact with lymphoma cancer cell receptors. In the presence of target cell receptors, an immunocomplex was formed between anti-CD20 antibodies and lymphoma cancer cell receptors. Then, the biosensing layer was magnetically collected on a screen-printed carbon electrode (SPCE) and placed in a homemade electrochemical cell configuration to measure impedimetric signals. The fabrication steps of the immunosensor were characterized by various techniques, such as resonance light scattering, fluorescence, electrochemical impedance spectroscopy, and cyclic voltammetry. The assay is highly sensitive: the calculated limit of detection of lymphoma cancer cells was as low as 38 cells/mL, and the detection was linear from 100 to 1 000 000 cells/mL. The specificity of the immunosensor is also very high, and there is no interference effect with several potential interferents, such as the breast cancer (MCF-7), human embryonic kidney (HEK293), and leukemia (HL-60 and KCL-22) cell lines. The performance of the immunosensor for lymphoma cancer cells in clinical blood samples is consistent with that of commercial flow cytometric assays.


Assuntos
Anticorpos Imobilizados/imunologia , Biomarcadores Tumorais/sangue , Separação Celular/métodos , Imunoensaio/métodos , Linfoma/sangue , Nanotubos de Carbono/química , Anticorpos Imobilizados/química , Biomarcadores Tumorais/imunologia , Ácidos Borônicos/química , Linhagem Celular Tumoral , Técnicas Eletroquímicas , Células HEK293 , Humanos , Limite de Detecção , Linfoma/patologia , Fenômenos Magnéticos , Rituximab/química , Rituximab/imunologia
9.
Anal Bioanal Chem ; 412(7): 1629-1637, 2020 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-31965245

RESUMO

A new magnetic molecularly imprinted nanofiber (MMIN) nanocomposite was prepared and used to the selective extraction of nilotinib. MMIN was constructed using a novel and general method including a combination of molecular imprinting and electrospinning technology. By electrospun precursor nanofibers containing polyacrylonitrile, Fe3O4 magnetic nanoparticles, and nilotinib as the template, molecularly imprinted nanofibers were produced with a mean diameter of 500 nm and lengths up to several millimeters. The microstructure and morphology of the prepared MMIN were thoroughly investigated using techniques such as X-ray diffraction (XRD) and scanning electron microscopy (SEM). The MMIN was then used to the extraction of nilotinib. The extracted nilotinib was re-extracted and determined spectrofluorimetrically at the excitation and emission wavelengths of 271 and 335 nm, respectively. The relation between fluorescence signal for the re-extracted solution and nilotinib concentration was linear in the range 0.01-10.0 mg L-1 (n = 9) and the RSD for the determination of 1.0 and 5.0 mg L-1 nilotinib 2.75% and 1.09% (n = 3), respectively. The detection limit of the method was obtained as 0.002 mg L-1 nilotinib. The results indicated that the proposed method can be successfully applied to the determination of nilotinib in human serum samples. Graphical abstract.


Assuntos
Magnetismo , Impressão Molecular , Nanofibras , Pirimidinas/isolamento & purificação , Resinas Acrílicas/química , Humanos , Limite de Detecção , Microscopia Eletrônica de Varredura , Pirimidinas/sangue , Reprodutibilidade dos Testes , Espectrometria de Fluorescência
10.
Anal Chem ; 91(9): 6383-6390, 2019 05 07.
Artigo em Inglês | MEDLINE | ID: mdl-30987423

RESUMO

A sensitive prostate-specific antigen (PSA) detection method using a visual-readout closed bipolar electrode (BPE) system has been introduced by integration of hydrogen evolution reaction (HER) in cathodic pole and electrochemiluminescence (ECL) of luminol loaded within the MIL-53(Fe)-NH2 (L@MIL-53(Fe)-NH2) in the anodic pole. The cathode of the BPE was electrochemically synthesized by 3D porous copper foam, followed by decorating with nitrogen-doped graphene nanosheet and ruthenium nanoparticles. As an alternative, we employed carboxylate-modified magnetic nanoparticles (MNPs) for immobilization of the primary antibody (Ab1) and utilized the L@MIL-53(Fe)-NH2 conjugated to secondary antibody (Ab2) as a signaling probe and coreaction accelerator. After sandwiching the target PSA between Ab1 and Ab2, the MNP/Ab1-PSA-Ab2/L@MIL-53(Fe) were introduced to a gold anodic BPE. Finally, the resulting ECL of luminol and H2O2 at the anodic poles was monitored using a photomultiplier tube (PMT) or digital camera. The PMT and visual (camera)-based detections showed linear responses from 1 pg mL-1 to 300 ng mL-1 (limit of detection 0.2 pg mL-1) and 5 pg mL-1 to 200 ng mL-1 (limit of detection 0.1 pg mL-1), respectively. This strategy provides an effective method for high-performance bioanalysis and opens a new door toward the development of the highly sensitive and user-friendly device.


Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , Luminescência , Medições Luminescentes , Antígeno Prostático Específico/análise , Anticorpos/química , Técnicas Biossensoriais/instrumentação , Técnicas Eletroquímicas/instrumentação , Hidrogênio/química , Medições Luminescentes/instrumentação , Luminol/química , Nanopartículas de Magnetita/química , Estruturas Metalorgânicas/química , Tamanho da Partícula , Porosidade , Propriedades de Superfície
11.
Mikrochim Acta ; 186(3): 205, 2019 02 26.
Artigo em Inglês | MEDLINE | ID: mdl-30806793

RESUMO

The fluorescence of ZnS quantum dots in colloidal water solution changes very slightly on addition of glutathione (GSH) but is strongly enhanced in the presence of Zn(II) even in concentrations as low as 10 µM. The resulting Zn(II)-enhanced fluorescence is found to be quenched by GSH. In contrast to GSH, cysteine does not cause an effect. Response surface methodology was applied to optimize the experimental parameters. The best data can be obtained at 305/427 nm as excitation/emission wavelengths. These findings were used to design an indirect method for the fluorometric determination of GSH that has a 0.9 µM detection limit and a response that is linear in the 2.0-104.0 µM GSH concentration range. The relative standard deviation at a level of 65 µM of GSH (for n = 5) is 1.9%. Graphical abstract Schematic presentation of the detection strategy for glutathione and the influence of the mediator (Zn2+). Direct pathway shows that the glutathione cannot cause a change in the blue fluorescence of ZnS QDs. The presence of Zn2+ causes the enhancement of the fluorescence intensity, and this generates the indirect pathway to glutathione detection.

12.
Anal Bioanal Chem ; 410(16): 3683-3691, 2018 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-29627893

RESUMO

Sensitive detection of biomarkers will mean accurate and early diagnosis of diseases. A tissue plasminogen activator (tPA) has a crucial role in many cardiovascular diseases and it is related to many processes such as angiogenesis in cancer cells. Therefore, sensitive determination of tPA is important in diagnosis and clinical research. tPA monoclonal antibody was covalently attached onto single-wall carbon nanotubes (SWCNTs) using diimide-activated imidation coupling. Functionalized SWCNTs were immobilized onto a glassy carbon electrode and the modification process was investigated by sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), SEM, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). Cyclic voltammograms (CVs) in a scan rate of 100 mVs-1 was studied and comparisons were made between the modified glassy carbon electrodes (immobilized with antibodies) as a working electrode before and after the formation of tPA-antibody complex. Results of the SDS-PAGE demonstrated that the antibody was covalently and site directly attached to the SWCNTs. The fabricated biosensor provided a good linear response range from 0.1 to 1.0 ng mL-1 with a low detection limit of 0.026 ng mL-1. The immunosensor showed selectivity, reproducibility, good sensitivity, and acceptable stability. Satisfactory results were observed for early and sensitive determination of tPA in human serum samples. For the first time, such specific biosensor is currently being fabricated for tPA in our laboratories and successfully could determine tPA in myocardial infraction and breast cancer patients. Graphical abstract Fabricated biosensor for determination of tPA.


Assuntos
Anticorpos Imobilizados/química , Técnicas Biossensoriais/métodos , Neoplasias da Mama/sangue , Infarto do Miocárdio/sangue , Nanotubos de Carbono/química , Ativador de Plasminogênio Tecidual/sangue , Biomarcadores Tumorais/sangue , Neoplasias da Mama/diagnóstico , Detecção Precoce de Câncer/métodos , Técnicas Eletroquímicas/métodos , Feminino , Humanos , Imunoensaio/métodos , Limite de Detecção , Pessoa de Meia-Idade , Modelos Moleculares , Infarto do Miocárdio/diagnóstico , Nanotubos de Carbono/ultraestrutura , Reprodutibilidade dos Testes
13.
Arch Toxicol ; 92(1): 213-222, 2018 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-28871328

RESUMO

Mandelic acid (MA) is a major metabolite of ethylbenzene and styrene. For the first time, a selective, fast, and easy-to-use procedure was developed for the determination of MA in urine samples. The new procedure is based on MIMEPS, the combination of a molecularly imprinted polymer (MIP) and microextraction by packed sorbent (MEPS). High-performance liquid chromatography with ultraviolet detection (HPLC-UV) was used for the separation and determination of MA. The bulk polymerization method was used to synthesize the MIP, and the MIP and non-imprinted polymer (NIP) were characterized by Fourier transform infrared spectroscopy. The selectivity of the MIP was investigated in the presence of interferents. In addition, we investigated the various parameters that affect the performance of the MEPS, including the pH of the sample, the number of extraction cycles, sample volume, and the types and volumes of the washing and elution solvents. A six-point calibration curve was obtained in the range of 0.2-20 µg/mL (R 2 = 0.9994). The extraction recovery was more than 88.8%. The limit of detection and the limit of quantitation were 0.06 and 0.2 µg/mL, respectively. The intra- and inter-day precisions were in the range of 3.6-4.7% and 3.8-5.1%, respectively. The accuracy was -8.4 to -11.1%. The optimized procedure was selective, sensitive, and rapid, and it was both user friendly and environmentally friendly. The sample preparation process took only about 5 min, so the MIMEPS-HPLC-UV procedure is recommended as an alternative for the biomonitoring of workers exposed to ethylbenzene and/or styrene.


Assuntos
Derivados de Benzeno , Ácidos Mandélicos/urina , Impressão Molecular/métodos , Exposição Ocupacional/análise , Derivados de Benzeno/toxicidade , Calibragem , Cromatografia Líquida de Alta Pressão , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Microextração em Fase Líquida/instrumentação , Microextração em Fase Líquida/métodos , Masculino , Polímeros/química , Reprodutibilidade dos Testes , Solventes/química , Espectroscopia de Infravermelho com Transformada de Fourier , Raios Ultravioleta
14.
Arch Toxicol ; 92(1): 223, 2018 01.
Artigo em Inglês | MEDLINE | ID: mdl-29308533

RESUMO

In the original publication of the article, there is an error in Fig. 2c. The authors would like to correct this error and the corrected version of Fig. 2c is as follow.

15.
Mikrochim Acta ; 185(6): 296, 2018 05 11.
Artigo em Inglês | MEDLINE | ID: mdl-29752544

RESUMO

A nanostructured material of the type Au-ZnO-SiO2 is described that consists of ZnO and gold nanoparticles (NPs) dispersed into a silica matrix and used to construct a voltammetric sensor for 4-nitrophenol. The AuNPs and ZnO NPs are anchored onto the silica network which warrants the nanostructures to be stable in various environments. It also facilitates the electron transfer between the electrolyte and the glassy carbon electrode (GCE). The properties of the nanostructure as a modifier for the GCE were investigated by energy dispersive spectrometry, X-ray diffraction spectroscopy, and transmission electron microscopy. It is shown that the nanostructure increases the surface area. Hence, the cathodic and anodic current in differential pulse voltammetry of 4-nitrophenol are considerably enhanced in comparison to a bare GCE. Under optimum conditions, the currents for oxidation and reduction are proportional to the concentration of 4-nitrophenol in the 0.05-3.5 µM and 0.01-1.2 µM concentration ranges, with 13.7 and 2.8 nM detection limits, respectively. The sensor has excellent sensitivity, fast response, long-term stability, and good reproducibility. It is perceived to be a valuable tool for monitoring 4-nitrophenol in real water samples. Graphical abstract Schematic of voltammetric sensor for 4-nitrophenol. It is based on GCE modified with gold-ZnO-SiO2 nanostructure. It exhibited the improvement in performance for both oxidation and reduction peaks in terms of linearity, concentration range, detection limit, and sensitivity.

16.
Anal Bioanal Chem ; 409(22): 5269-5278, 2017 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-28667386

RESUMO

Vinblastine (VLB) is prescribed for a wide variety of cancers. Therefore, development of sensitive methods for early diagnosis is urgently required. In this work, a highly sensitive and label-free impedimetric biosensor was fabricated for the electrochemical detection of VLB. First, the gold nanoparticles (AuNPs) were electrodeposited on the surface of a glassy carbon electrode (GCE). 3-Mercaptopropionic acid (MPA) was self-assembled over the AuNPs. Then, tubulin (TUB), as a receptor, was covalently immobilized at the AuNPs/GCE surface via carbodiimide coupling reaction using N-(3 dimethylaminopropyl)-N'-ethyl carbodiimide (EDC) and N-hydroxy succinimide (NHS). The step-by-step modification process was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in the presence of a redox probe [Fe(CN)6]3-/4-. The VLB concentration was measured through the increase of impedance values in the corresponding specific binding of VLB and TUB. The increased electron-transfer resistance (R et) values were proportional to the value of VLB concentrations in the range of 0.4 to 65.0 nmol L-1 with a detection limit of 8.4 × 10-2 nmol L-1 (SN-1 = 3). The practical analytical performance of the proposed method was demonstrated by determination of VLB in plant extracts and human serum samples with satisfactory recoveries.


Assuntos
Técnicas Biossensoriais , Eletrodos , Vidro/química , Ouro/química , Nanopartículas Metálicas/química , Tubulina (Proteína)/química , Vimblastina/análise , Catharanthus/química , Técnicas Eletroquímicas/instrumentação , Humanos , Limite de Detecção , Microscopia Eletrônica de Varredura , Extratos Vegetais/química , Vimblastina/sangue , Vimblastina/química
17.
Sensors (Basel) ; 17(5)2017 May 09.
Artigo em Inglês | MEDLINE | ID: mdl-28486408

RESUMO

In this work, a novel nanocomposite consisting of electrosynthesized gold nanodendrites and chitosan nanoparticles (AuNDs/CSNPs) has been prepared to fabricate an impedimetric immunosensor based on a screen printed carbon electrode (SPCE) for the rapid and sensitive immunoassay of botulinum neurotoxin A (BoNT/A). BoNT/A polyclonal antibody was immobilized on the nanocomposite-modified SPCE for the signal amplification. The structure of the prepared nanocomposite was investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The charge transfer resistance (RCT) changes were used to detect BoNT/A as the specific immuno-interactions at the immunosensor surface that efficiently limited the electron transfer of Fe(CN)63-/4- as a redox probe at pH = 7.4. A linear relationship was observed between the %∆RCT and the concentration logarithm of BoNT/A within the range of 0.2 to 230 pg·mL-1 with a detection limit (S/N = 3) of 0.15 pg·mL-1. The practical applicability of the proposed sensor was examined by evaluating the detection of BoNT/A in milk and serum samples with satisfactory recoveries. Therefore, the prepared immunosensor holds great promise for the fast, simple and sensitive detection of BoNT/A in various real samples.


Assuntos
Nanoestruturas , Técnicas Biossensoriais , Quitosana , Eletrodos , Ouro , Imunoensaio , Limite de Detecção , Nanopartículas Metálicas , Neurotoxinas , Sorogrupo
18.
Anal Bioanal Chem ; 408(10): 2577-86, 2016 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-26873212

RESUMO

A facile and effective approach of fabricating oxidized multiwalled carbon nanotube/glassy carbon electrode (OMWCNT/GCE) is herein reported. The OMWCNT/GCE was prepared by electrochemical oxidation method in basic media (0.5 mol L(-1) NaOH solution) and used as a sensor for simultaneous determination of dopamine (DA) and doxorubicin (DOX). Scanning electron microscopy, energy dispersive X-ray spectroscopy and cyclic voltammetry were used for characterization and performance study of the OMWCNT/GCE. The modified electrode exhibited good electrocatalytic properties toward the oxidation of DA and DOX. Peaks potential difference of 240 mV between DA and DOX was large enough to determine DA and DOX individually and simultaneously. Square wave voltammetry (SWV) was used for the simultaneous determination of DA and DOX in their binary mixture. Under the optimum conditions, the linear concentration dependences of SW peak current responses were observed for DA and DOX in the concentration ranges of 0.03-55 µmol L(-1) and 0.04-90 µmol L(-1), respectively. The detection limits (S/N = 3) were 8.5 × 10(-3) µmol L(-1), and 9.4 × 10(-3) µmol L(-1) for DA and DOX, respectively. The analytical utility of OMWCNT/GCE was also successfully demonstrated for the simultaneous determination of DA and DOX in human blood serum and urine samples. Graphical Abstract Fabrication of new oxidized multiwalled carbon nanotube/glassy carbon electrode for simultaneous determination of dopamine and doxorubicin.


Assuntos
Carbono/química , Dopamina/análise , Doxorrubicina/análise , Nanotubos de Carbono , Técnicas Eletroquímicas/métodos , Humanos , Concentração de Íons de Hidrogênio , Limite de Detecção , Microscopia Eletrônica de Varredura , Oxirredução , Reprodutibilidade dos Testes
19.
Luminescence ; 30(5): 576-82, 2015 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-25377137

RESUMO

A sensitive spectrofluorimetric method using constant-energy synchronous fluorescence technique is proposed for the determination of human albumin without separation. In this method, no reagent was used for enhancement of the fluorescence signal of albumin in the solution. Effects of some parameters, such as energy difference between excitation and emission monochromators (ΔE), emission and excitation slit widths and scan rate of wavelength were studied and the optimum conditions were established. For this purpose factorial design and response surface method were employed for optimization of the effective parameters on the fluorescence signal. The results showed that the scan rate of the wavelength has no significant effect on the analytical signal. The calibration curve was linear in the range 0.1-220.0 µg mL(-1) of albumin with a detection limit of 7.0 × 10(-3) µg mL(-1). The relative standard deviations (RSD) for six replicate measurements of albumin were calculated as 2.2%, 1.7% and 1.3% for 0.5, 10.0 and 100.0 µg mL(-1) albumin, respectively. Furthermore the proposed method has been employed for the determination of albumin in human serum and urine samples.


Assuntos
Albumina Sérica/análise , Espectrometria de Fluorescência/métodos , Albuminúria/diagnóstico , Calibragem , Humanos , Limite de Detecção
20.
Talanta ; 274: 126041, 2024 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-38581854

RESUMO

This paper presents the development and optimization of a cost-effective paper electrochemical sensor for the detection of TNT using Fe3O4-Au core-shell nanoparticles modified with cysteamine (Fe3O4@Au/CA). The sensor was constructed by modifying a graphite paste with the aforementioned nanoparticles, which facilitated the formation of a Meisenheimer complex between cysteamine and TNT as an electron donor and an electron acceptor, respectively. The central composite design was employed to optimize four key parameters pH, modifier percentage, contact time, and buffer type to enhance the performance of the sensor. The detection limit was found to be 0.5 nM of TNT, while the linear range of the electrode response spanned from 0.002 µM to 10 µM. The simplicity and low cost of the sensor make it highly attractive for practical applications, particularly in scenarios where rapid and on-site TNT detection is required.

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