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1.
Chem Commun (Camb) ; 58(46): 6590-6593, 2022 Jun 08.
Artículo en Inglés | MEDLINE | ID: mdl-35611701

RESUMEN

Crystals of a metal-organic framework, UiO-66, are grown on electrospun crosslinked poly-cyclodextrin (poly-CD) fibrous membranes with an ultrahigh coverage, and polyaniline (PANI) is further confined within the MOF pores. The obtained PANI@UiO-66/poly-CD membranes are used as free-standing electrodes towards use in wearable energy-storage devices.


Asunto(s)
Ciclodextrinas , Estructuras Metalorgánicas , Ácidos Ftálicos , Compuestos de Anilina
2.
Chemosphere ; 296: 133997, 2022 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-35167833

RESUMEN

We report a highly selective and sensitive electrochemical sensor for the determination of nitrofurazone (NZ) based on sulfur-doped graphitic carbon nitride with copper tungstate hollow spheres (Sg-C3N4/CuWO4). Here, a Sg-C3N4/CuWO4 composite was synthesized by a facile ultrasonic method. The physicochemical properties of the composite were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). Then, the surface morphology of the composite material was investigated by field emission scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscopy (HR-TEM). Moreover, the electrochemical activity of the as-synthesized composite material was initially tested using electrochemical impedance spectroscopy (EIS). The electroanalytical techniques namely cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were carried out for the electrochemical studies. The proposed sensor exhibits lower LOD and good sensitivity of about 3 nM and 1.24 µAµM-1 cm-2 to NZ detection. In addition, the Sg-C3N4/CuWO4 modified electrode showed excellent repeatability, reproducibility, long-term storage stability and excellent selectivity. The developed sensor was successfully applied for the determination of NZ in human urine and serum samples and achieved good recovery results.


Asunto(s)
Grafito , Rubus , Antibacterianos , Técnicas Electroquímicas/métodos , Electrodos , Grafito/química , Humanos , Límite de Detección , Nitrofurazona , Reproducibilidad de los Resultados , Azufre/química
3.
Anal Chim Acta ; 1190: 339234, 2022 Jan 15.
Artículo en Inglés | MEDLINE | ID: mdl-34857130

RESUMEN

In this work, pyrochlore neodymium stannate nanoparticles (Nd2Sn2O7 NP) have been synthesized by a facile co-precipitation technique and employed as an electrode material on GCE for the determination of dimetridazole (DM) drug. The physical properties and texture of the Nd2Sn2O7 NP were characterized by PXRD, Raman spectroscopy, FE-SEM, EDX mapping, XPS, and HR-TEM analytical studies. The electrocatalytic investigation of Nd2Sn2O7 NP/GCE was carried out by CV, and DPV techniques. The fabricated Nd2Sn2O7 NP/GCE shows a lower LOD of 6 nm towards the determination of DM and the calculated sensitivity is 0.61 µA µM-1 cm-2. In addition to that, the constructed sensor delivers notable repeatability, reproducibility, and superior selectivity with the existence of metal ions, biological molecules, and nitro compounds, enabling the electrochemical detection of DM. Furthermore, Nd2Sn2O7 NP/GCE sensor displays acceptable recovery results in the real sample analysis in biological fluids such as human blood serum and human urine.


Asunto(s)
Dimetridazol , Nanopartículas , Técnicas Electroquímicas , Electrodos , Humanos , Límite de Detección , Neodimio , Reproducibilidad de los Resultados
4.
Materials (Basel) ; 14(21)2021 Nov 07.
Artículo en Inglés | MEDLINE | ID: mdl-34772226

RESUMEN

In this study, we synthesized heterostructured zinc stannate/tin oxide microparticles (ZTO/TO MPs) by a simple coprecipitation method and used them as an effective electrode material for the electrochemical detection of the antibacterial drug secnidazole (SCZ). The as-prepared ZTO/TO MPs were characterized by XRD, Raman, FE-SEM, HR-TEM, EDX, and XPS analyses. The physiochemical studies clearly proved that the fabricated ZTO/TO MPs were formed in a heterostructure phase without other impurities. A glassy carbon electrode modified with the synthesized ZTO/TO MPs showed an excellent and improved electrocatalytic activity in the electrochemical reduction of SCZ. Using differential pulse voltammetry (DPV), an impressive linear calibration range, extending from 0.01 to 193 µM, was observed, coupled with a detection limit of 0.0054 µM and a sensitivity of 0.055 µA/µM. In addition, the ZTO/TO MPs/GCE showed very good selectivity for the detection of SCZ in the presence of a number of biological, inorganic, and structurally related compounds. Finally, the ZTO/TO MPs/GCE was investigated for the analysis of SCZ in human blood serum samples. A very good recovery was obtained when spiking the blood serum with SCZ, highlighting the good applicability of the ZTO/TO MPs/GCE for the electrochemical analysis of SCZ in complex biological samples.

5.
Inorg Chem ; 60(4): 2464-2476, 2021 Feb 15.
Artículo en Inglés | MEDLINE | ID: mdl-33534999

RESUMEN

Apart from perovskites, the development of different types of pyrochlore oxides is highly focused on various electrochemical applications in recent times. Based on this, we have synthesized pyrochlore-type praseodymium stannate nanoparticles (Pr2Sn2O7 NPs) by using a coprecipitation method and further investigated by different analytical and spectroscopic techniques such as X-ray diffraction, Raman spectroscopy, field emission-scanning electron microscopy, high resolution-transmission electron microscopy, and X-ray photoelectron spectroscopy analysis. Followed by this, we have designed a unique and novel electrochemical sensor for nitrofurazone detection, by modifying the glassy carbon electrode (GCE) with the prepared Pr2Sn2O7 NPs. For that, the electrochemical experiments were performed by using cyclic voltammetry and differential pulse voltammetry techniques. The Pr2Sn2O7 NPs modified GCE exhibits high sensitivity (2.11 µA µM-1 cm-2), selectivity, dynamic linear ranges (0.01-24 µM and 32-332 µM), and lower detection limit (4 nM). Furthermore, the Pr2Sn2O7 NPs demonstrated promising real sample analysis with good recovery results in biological samples (human urine and blood serum) which showed better results than the noble metal catalysts. Based on these results, the present work gives clear evidence that the pyrochlore oxides are highly suitable electrode materials for performing outstanding catalytic activity toward electrochemical sensors.


Asunto(s)
Antiinfecciosos/administración & dosificación , Nanopartículas/química , Niobio/química , Nitrofurazona/análisis , Praseodimio/química , Compuestos de Estaño/química , Catálisis , Técnicas Electroquímicas/métodos , Humanos , Límite de Detección , Microscopía Electrónica de Rastreo , Espectroscopía de Fotoelectrones
6.
Chemosphere ; 273: 129665, 2021 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-33508687

RESUMEN

Nitroimidazole compounds are widely used antibiotics to encounter anaerobic bacterial and parasitic infections. The wide usage of antibiotic drugs became an ecological contaminant which in turn into potential monitoring. In this regards, we have designed and developed a new electrochemical sensing probe to monitor an antiprotozoal drug, ornidazole (ODZ), with the aid of a glassy carbon electrode (GCE) integrated with manganese molybdate nanorods (MnMoO4) decorated graphene nanosheets (GNS) hybrid materials that prepared by feasible probe sonochemical method (parameters: 2-4 W, 5 mV amp, 20 kHz). The electrochemical investigations of the developed probe were performed by using rapid scan electrochemical workstations namely cyclic voltammetry (CV) and amperometric (i-t) techniques. The as-prepared MnMoO4/GNS nanocomposite was characterized and its purity of nanocomposite formation was confirmed by various analytical techniques like X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and Raman spectroscopy. In addition to that, the textural morphology of the MnMoO4/GNS nanocomposite was examined with the aid of field emission scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscopy (HR-TEM). The MnMoO4/GNS nanocomposite rotating disk glassy carbon electrode (RDGCE) plays a crucial role in electrochemical detection of ODZ, which results in excellent anti-interference ability, a lower detection limit of 845 pM, massive linear ranges from 10 to 770 nM, and good sensitivity of about 104.62 µA µM-1 cm-2. From the acquired electrochemical studies, we have developed a disposable electrochemical sensor probe using a low-cost screen-printed carbon electrode (SPCE) with MnMoO4/GNS nanocomposite. The MnMoO4/GNS/SPCE are capably employed in real-time sensing of ODZ in water and urine samples. These electrochemical studies revealed the integral new vision on the electrocatalytic performance of the modified SPCE and also shown excellent amplification results in ultra-trace levels.


Asunto(s)
Contaminantes Ambientales , Grafito , Nanotubos , Ornidazol , Técnicas Electroquímicas , Espectroscopía Infrarroja por Transformada de Fourier , Agua
7.
RSC Adv ; 11(26): 15856-15870, 2021 Apr 26.
Artículo en Inglés | MEDLINE | ID: mdl-35481186

RESUMEN

A simple hydrothermal process has been used to prepare a carbon nanofiber/copper chromium dioxide (CNF/CuCrO2) composite for the selective detection of 4-nitrophenol (4-NP) and supercapacitor applications. The electrochemical sensor was developed with a glassy carbon electrode (GCE) modified with the CNF/CuCrO2 composite by the drop-casting method. The structural formation of the prepared materials was confirmed by infrared spectroscopy, electrochemical impedance spectroscopy, Raman spectroscopy, scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. To investigate the electrochemical efficiency of the electrode, various electroanalytical techniques, namely, differential pulse voltammetry (DPV), cyclic voltammetry (CV) and galvanostatic charge-discharge tests, were employed. The GCE/CNF/CuCrO2 modified electrode exhibited excellent electrocatalytic behavior for the detection of 4-NP under optimized conditions with a low detection limit (0.022 µM), long linear response range of 0.1-150 µM, and high sensitivity (20.02 µA µM-1 cm-2). The modified electrode was used for the detection of 4-NP in real samples with satisfactory results. In addition, the GCE/CNF/CuCrO2 electrode has advantages such as stability, reproducibility, repeatability, reliability, low cost, and practical application. The CNF/CuCrO2 composite coated Ni-foam electrodes also exhibited excellent supercapacitor efficiency, with a high specific capacitance of up to 159 F g-1 at a current density of 5 A g-1 and outstanding cycling stability. Hence, the CNF/CuCrO2 composite is a suitable material for 4-NP sensors and energy storage applications.

8.
Ultrason Sonochem ; 61: 104823, 2020 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-31669843

RESUMEN

Ultrasonication is one of the emerging probes for nanoparticles synthesis as well as promoting the material property by treasuring the precious time during a chemical reaction. In this present work, we successfully designed a cloud-like α-ZnMoO4 nanospheres (ZMNS) using ultrasound assistance (bath sonication with the power of 60 W and frequency of 37/80 kHz) hydrothermal method for catalyzing the effective electrochemical determination of anti-androgen drug candidate flutamide (FLT). The crystallinity and phase purity were investigated using powder X-ray diffractometric analysis. The FTIR and Raman spectra information were compared to detect the possible bonding in ZMNS. The texture and surface morphology were studied using Field emission scanning electron microscope and High-resolution Transmission electron microscope images. The presence of the elements (Zn, Mo and O) and the absence of any other impurities were monitored and confirmed using EDAX analysis. The fabrication of ZMNS modified GCE was performed carefully. Additionally, the ZMNS modified glassy carbon electrode (GCE) exhibits superior electrocatalytic activity by means of higher cathodic peak current towards the detection of FLT. The fashioned electrode attained two wide linear response ranges (0.1 to 73 µM; 111 to 1026 µM) with a lower detection limit of about 33 nM correspondingly. Furthermore, the fabricated sensor displayed excellent sensitivity of 1.095 µA µM-1 cm-2 and good selectivity for FLT sensing even in the existence of similar interfering compounds and biomolecules. Along with that, the designed sensor executed noticeable reproducibility, repeatability, and enduring stability.


Asunto(s)
Antagonistas de Andrógenos/análisis , Flutamida/análisis , Molibdeno/química , Nanosferas/química , Sonicación/métodos , Zinc/química , Técnicas Electroquímicas/métodos , Límite de Detección , Análisis Espectral/métodos
9.
ACS Appl Mater Interfaces ; 11(41): 38321-38335, 2019 Oct 16.
Artículo en Inglés | MEDLINE | ID: mdl-31549800

RESUMEN

Material combinations of semiconductor with conducting polymer are gaining growing interest due to their enhanced activities in photocatalysis as well as electrochemical sensing. In this present work, we report a facile in situ synthesis of polypyrrole (PPy) polymer-incorporated silver molybdate (Ag2MoO4) nanocomposite that is utilized as a photocatalyst and electrocatalyst for the degradation of pollutant heavy metals, namely, methylene blue (MB) and heavy metal (Cr(VI)), and ciprofloxacin (CIP) and for detection of the drug, azomycin. The synthesized nanocomposite was characterized by various theoretical, spectral, and microscopic studies. Matching of the powder X-ray diffraction pattern with JCPDS no. 76-1747 confirmed the formation of α-Ag2MoO4/PPy. The surface topography and spherical morphology of the nanocomposite were studied using field emission-scanning electron microscopy and transmission electron microscopy. Fourier transform infrared spectral detail expounds the smooth incorporation of PPy to Ag2MoO4. The as-synthesized nanocomposite performs as an efficient photocatalyst in the degradation of MB (99.9%), Cr(VI) (99%), and CIP drug (99.8%) within 10 min. In addition to this, the Ag2MoO4/PPy-modified glassy carbon electrode (GCE) demonstrated excellent electrocatalytic activity in terms of a higher cathodic peak current and lower peak potential when compared with other modified and unmodified GCEs for the detection of azomycin. The Ag2MoO4/PPy/GCE displayed a broader linear response range and lower detection limit of 0.5-499 µM and 65 nM, respectively. Moreover, other potentially co-interfering compounds, such as a similar functional group-containing biological substances and inorganic species, have no interference effect toward azomycin sensing.


Asunto(s)
Contaminantes Ambientales/química , Molibdeno/química , Nanocompuestos/química , Polímeros/química , Pirroles/química , Plata/química , Catálisis , Ciprofloxacina/química , Azul de Metileno/química , Nitroimidazoles/química
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