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1.
Mikrochim Acta ; 191(2): 112, 2024 01 29.
Artigo em Inglês | MEDLINE | ID: mdl-38286966

RESUMO

For the first time, a tumour hypoxia marker detection has been developed using two-dimensional layered composite modified electrodes in biological and environmental samples. The concept of TaB2 and V4C3-based MXene composite materials is not reported hitherto using ball-milling and thermal methods and it remains the potentiality of the present work. The successful formation is confirmed through various characterisation techniques like X-ray crystallography, scanning electron microscopy photoelectron, and impedance spectroscopy. A reliable and repeatable electrochemical sensor based on TaB2@V4C3/SPCE was developed for quick and extremely sensitive detection of pimonidazole by various electroanalytical methods. It has been shown that the modified electrode intensifies the reduction peak current and causes a decrease in the potential for reduction, in comparison with the bare electrode. The proposed sensor for pimonidazole reduction has strong electrocatalytic activity and high sensitivity, as demonstrated by the cyclic voltammetry approach. Under the optimal experimental circumstances, differential pulse voltammetry techniques were utilised for generating the wide linear range (0.02 to 928.51 µM) with a detection limit of 0.0072 µM. The resultant data demonstrates that TaB2@V4C3/SPCE nano-sensor exhibits excellent stability, reliability, and repeatability in the determination of pimonidazole. Additionally, the suggested sensor was successfully used to determine the presence of pimonidazole in several real samples, such as human blood serum, urine, water, and drugs.


Assuntos
Carbono , Nitroimidazóis , Tantálio , Humanos , Carbono/química , Vanádio , Reprodutibilidade dos Testes , Limite de Detecção , Eletrodos , Compostos de Boro
2.
Chemosphere ; 321: 138008, 2023 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-36731664

RESUMO

Alizarin red S (ARS) extraction from aqueous medium was carried out using hydrophobic ionic liquids (ILs) containing trioctylammonium cation paired with 4-tert-butylbenzoate ([TOA][Butbenz] (IL1), 4-phenylbutanoate ([TOA][PheBut] (IL2), 3-4-dimethylbenzoate ([TOA][DMbenz] (IL3), naphthoate, ([TOA][Naph]) (IL4), salicylate ([TOA][Sali]) (IL5) and nonanedioate ([TOA]2[Nona]) (IL6). The findings demonstrated that all of the tested ILs were efficient for extracting ARS, however, [TOA]2[Nona] was more effective than others. For the extraction of ARS from the aqueous phase, the effects of various parameters including the initial pH of the dye solution, contact time, ILs to dye volume ratio (VIL:VW), dye concentration, temperature, and salt effect were investigated. The spontaneity of the liquid-liquid extraction of ARS from the aqueous phase to the IL phase was confirmed by thermodynamic parameters. More than 90% of the ARS was extracted from the aqueous phase to the IL phase throughout all experiments. Interaction of selected IL with dyes were confirmed using FTIR analysis. The standard bacterial strains of Escherichia coli (E. coli) ATCC BAA-2471 (gram negative) and Methicillin-resistant Staphylococcus (MRSA) ATCC 43300 (gram positive) were used for evaluating antibacterial activity. The lower dose (250 ppm), the ILs1, 2, 3, 4, 5, and 6 inhibited 0.40, 1.50, 6.50, 1.50, 2.50, and 0.50 mm growth of E. coli, and 4.0, 2.0, 16.50, 0.40, 5.0, and 3.50 mm growth of MRSA, respectively. The experimental findings confirmed that the present ILs can be utilized as an effective solvent for ARS and other dyes extraction from aqueous media.


Assuntos
Compostos de Amônio , Líquidos Iônicos , Staphylococcus aureus Resistente à Meticilina , Líquidos Iônicos/química , Escherichia coli , Água/química , Antibacterianos , Corantes , Têxteis
3.
Chemosphere ; 321: 138077, 2023 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-36758812

RESUMO

This work successfully utilised eco-friendly green synthesis to produce Ag-TiO2 nanofibers (NFs). As pollution and energy limitations have become global issues, there is an ongoing need to develop more effective catalysts through straightforward and environmentally friendly methods. The Ag-TiO2 nanofibers (NFs) XRD pattern exhibits an anatase TiO2 and FCC crystal structure of Ag nanoparticles. The SEM investigation revealed a nanofiber-like surface morphology. The Ag-TiO2 nanofibers (NFs) exhibits an optical band gap energy is 2.5 eV. Methylene blue (MB), malachite green (MG), Congo red (CR), and crystal violet (CV) dye aqueous solutions were used to evaluate the photocatalytic performance of the synthesized Ag-modified TiO2 nanofibers (NFs) under direct sunlight irradiation. The effects of catalyst size on the efficient breakdown of MB dye were also investigated. The optimum catalyst concentration was found to be at 0.02 mg/mL. At 120 min of direct sunlight, the highest photosynthetic degradation efficiency (DE percentage) of 94% was achieved for MB dye. Ag-TiO2 nanofibers (NFs) have been demonstrated to have exceptional antibacterial activity against Gram-positive bacteria such as Staphylococcus aureus and Gram-negative bacteria E-Coli. Because of these great qualities, it seems likely that the Ag-TiO2 nanofibers (NFs) made could be a great photocatalyst for getting dye pollutants out of wastewater.


Assuntos
Nanopartículas Metálicas , Nanofibras , Nanofibras/química , Nanopartículas Metálicas/química , Prata/química , Titânio/química , Antibacterianos/química
4.
Chemosphere ; 322: 138078, 2023 May.
Artigo em Inglês | MEDLINE | ID: mdl-36754302

RESUMO

Conventional homogeneous-based catalyzed transesterification for the production of biodiesel can be replaced with a membrane reactor that has an immobilized heterogeneous catalyst. Combining reaction with separation while utilizing membranes with a certain pore size might boost conversion process. this investigation to study the effectiveness of membrane reactor in combination with heterogeneous green nano catalysis of MnO2. Techniques such as XRD, EDX, FTIR, SEM, and TGA were used to characterize the synthesized MnO2 nano catalyst. The highest conversion of around 94% Trachyspermum ammi oil was obtained by MnO2. The optimum process variables for maximum conversion were catalyst loading of 0.26 (wt.%), 8:1 M ratio, 90 °C reaction temperature, and time 120 min. The green nano catalyst of MnO2 was reusable up to five cycles with minimum loss in conversion rate of about 75% in the fifth cycle. Nuclear magnetic resonance validated the synthesis of methyl esters. It was concluded that membrane reactor a promising technique to efficiently transesterify triglycerides into methyl esters and enable process intensification uses MnO2 as a catalyst.


Assuntos
Ammi , Óxidos , Compostos de Manganês , Biocombustíveis , Esterificação , Ésteres , Óleos de Plantas
5.
Chemosphere ; 313: 137426, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36470356

RESUMO

Natural gas is the cleanest form of fossil fuel that needs to be purified from CO2 and H2S to diminish harmful emissions and provide feasible processing. The conventional chemical and physical solvents used for this purpose have many drawbacks, including corrosion, solvent loss, high energy requirement, and the formation of toxic compounds, which ultimately disrupt the process and affect the environment. Hybrid solvents have lately been researched to cater to these liabilities and enhance process economics. This study screened eight solvents based on CO2 selectivity viscosity, absorption enthalpy, corrosivity, working capacity, specific heat, and vapor pressure. From the screened solvents, ten cases of hybrid solvents are simulated and optimized on Aspen HYSYS®. Furthermore, 5Es (Energy, Exergy, Economic, Environmental, and Exergy-environmental) analyses were performed on optimized cases, and results were compared with the base case, MEA (30 wt%). The hybrid blend of Sulfolane and MDEA with weight percentages of 6% and 24%, respectively, showed the highest energy savings of 20% concerning the base case. In addition, it offered 93% savings in exergy destruction and 17.26% in the total operating cost of the process. It is also promising to the environment due to reduced entropy sent to the ecosystem and controlled CO2 emissions. Therefore, the blend of Sulfolane and MDEA is proposed to Supersede the conventional solvent MEA for the natural gas sweetening process.


Assuntos
Aminas , Gás Natural , Solventes/química , Dióxido de Carbono/análise , Ecossistema
6.
Environ Res ; 216(Pt 3): 114665, 2023 01 01.
Artigo em Inglês | MEDLINE | ID: mdl-36334828

RESUMO

In the present work, mixed-spinel ferrite anchored onto graphitic carbon nitride (GCN) was synthesized for mineralization of antibiotic pollutant from waste water. A Z-scheme g-C3N4/Ni0.5Zn0.5Fe2O4 nano heterojunction was fabricated by three step procedure: pyrolysis, solution combustion and mechanical grinding followed by annealing. The prepared photocatlyst was tested for degradation of Doxycycline (DC) drug under the natural sun light. Results revealed that the prepared heterojunction has maximum degradation efficiency of 97.10% pollutant in 60 min experiment. The Z-scheme heterojunction between g-C3N4 and Ni-Zn ferrite improves the photoinduced charges separation and protection of redox capability and therby increases the photo degradation efficiency. The scavenging experiments suggested that O2-● and h+ as main active species responsible for degradation of the antibiotic. In addition, the dopant variation can drive the shists in band gap and energy band positiong too which makes then excellent candidates for synthesizing tunable heterostructures with organic semiconductors. The work focusses on designing and developing of saimpler but efficient magnetic heterojunctions with superior redox capability for solar powered waste water treatment.


Assuntos
Doxiciclina , Poluentes Ambientais , Catálise , Luz , Antibacterianos , Zinco
7.
Molecules ; 27(24)2022 Dec 09.
Artigo em Inglês | MEDLINE | ID: mdl-36557859

RESUMO

In this study, chloride (Cl−) ions were successfully doped into ZnO nanostructures by the solvothermal method. The effect of various Cl− concentrations on the photocatalytic activity of ZnO towards the photodegradation of methylene blue (MB) under the illumination of ultraviolet light was studied. The as-prepared Cl−-doped ZnO nanostructures were analyzed in terms of morphology, structure, composition and optical properties. XRD data revealed an average crystallite size of 23 nm, and the XRD patterns were assigned to the wurtzite structure of ZnO even after doping with Cl−. Importantly, the optical band gap of various Cl ion-doped ZnO nanostructures was successively reduced from 3.42 to 3.16 eV. The photodegradation efficiency of various Cl− ion-doped ZnO nanostructures was studied for MB in aqueous solution, and the relative performance of each Cl ion-doped ZnO sample was as follows: 20% Cl−-doped ZnO > 15% Cl−-doped ZnO > 10% Cl−-doped ZnO > 5% Cl−-doped ZnO > pristine ZnO. Furthermore, the correlation of the pH of the MB solution and each Cl ion dopant concentration was also investigated. The combined results of varying dopant levels and the effect of the pH of the MB solution on the photodegradation process verified the crucial role of Cl− ions in activating the degradation kinetics of MB. Therefore, these newly developed photocatalysts could be considered as alternative materials for practical applications such as wastewater treatment.


Assuntos
Nanoestruturas , Óxido de Zinco , Óxido de Zinco/química , Azul de Metileno , Cloretos , Raios Ultravioleta
8.
Mikrochim Acta ; 189(5): 210, 2022 05 03.
Artigo em Inglês | MEDLINE | ID: mdl-35503583

RESUMO

A novel electrochemical method has been developed for determination of nitrite using La-based perovskite-type lanthanum aluminate nanorod-incorporated graphene oxide nanosheets (LaAlO3@GO). Morphological and structural analyses of the prepared perovskite-type electrocatalyst, with and without a glassy carbon electrode (GCE) surface, were performed using various techniques, including transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffractometry, Raman spectroscopy, and electrochemical impedance spectroscopy. Under optimal conditions, the LaAlO3@GO composite-modified GCE (LaAlO3@GO/GCE) exhibited excellent electrocatalytic performance toward the electrooxidation of nitrite (pH = 7.0), with a significant increase in anodic peak currents compared with the bare GCE. Using amperometry, the fabricated sensor exhibited a wide nitrite determination range from 0.01 to 1540.5 µM, with a detection limit of 0.0041 µM. Notably, the proposed LaAlO3@GO/GCE electrode demonstrated a good nitrite detection performance in different meat and water samples. In addition, the LaAlO3@GO/GCE electrode displayed excellent selectivity, repeatability, reproducibility, storage, and operational stability toward nitrite detection.


Assuntos
Água Potável , Nitritos , Compostos de Cálcio , Carbono/química , Água Potável/análise , Grafite , Lantânio , Limite de Detecção , Carne/análise , Nitritos/análise , Óxidos , Extratos Vegetais , Reprodutibilidade dos Testes , Titânio
9.
Biosensors (Basel) ; 13(1)2022 Dec 29.
Artigo em Inglês | MEDLINE | ID: mdl-36671889

RESUMO

High concentrations of nicotine (40 to 60 mg) are more dangerous for adults who weigh about 70 kg. Herein, we developed an electrochemical transducer using an MXene (Ti3C2Tx)/palladium hydroxide-supported carbon (Pearlman's catalyst) composite (MXene/Pd(OH)2/C) for the identification of nicotine levels in human sweat. Firstly, the MXene was doped with Pd(OH)2/C (PHC) by mechanical grinding followed by an ultrasonication process to obtain the MXene/PHC composite. Secondly, XRD, Raman, FE-SEM, EDS and E-mapping analysis were utilized to confirm the successful formation of MXene/PHC composite. Using MXene/PHC composite dispersion, an MXene/PHC composite-modified glassy carbon electrode (MXene/PHC/GCE) was prepared, which showed high sensitivity as well as selectivity towards nicotine (300 µM NIC) oxidation in 0.1 M phosphate buffer (pH = 7.4) by cyclic voltammetry (CV) and amperometry. The MXene/PHC/GCE had reduced the over potential of nicotine oxidation (about 200 mV) and also enhanced the oxidation peak current (8.9 µA) compared to bare/GCE (2.1 µA) and MXene/GCE (5.5 µA). Moreover, the optimized experimental condition was used for the quantification of NIC from 0.25 µM to 37.5 µM. The limit of detection (LOD) and sensitivity were 27 nM and 0.286 µA µM-1 cm2, respectively. The MXene/PHC/GCE was also tested in the presence of Na+, Mg2+, Ca2+, hydrogen peroxide, acetic acid, ascorbic acid, dopamine and glucose. These molecules were not interfered during NIC analysis, which indicated the good selectivity of the MXene/PHC/GCE sensor. In addition, electrochemical determination of NIC was successfully carried out in the human sweat samples collected from a tobacco smoker. The recovery percentage of NIC in the sweat sample was 97%. Finally, we concluded that the MXene/PHC composite-based sensor can be prepared for the accurate determination of NIC with high sensitivity, selectivity and stability in human sweat samples.


Assuntos
Nicotina , Paládio , Humanos , Suor , Titânio/química , Carbono/química , Eletrodos , Técnicas Eletroquímicas
10.
Materials (Basel) ; 16(1)2022 Dec 29.
Artigo em Inglês | MEDLINE | ID: mdl-36614665

RESUMO

Herein, a unique synthetic approach called microemulsion is used to create nickel nanoparticles (Ni-NPs). SEM, TEM, EDX, and XRD techniques were employed for the investigation of morphology and structures of the synthesized material. Electrons from electroactive components are transferred to external circuits by Ni-NPs' superior electrical conductivity and interconnected nanostructures, which also provide a large number of channels for ion diffusion and additional active sites. The experimental findings showed that as a positive electrode for supercapacitors (SC), Ni-NPs had an outstanding ability to store charge, with a dominant capacitive charge storage of 72.4% when measured at 10 mV/s. Furthermore, at 1 A/g, Ni-NP electrodes exhibit a maximum capacitance of 730 F/g. Further, the Ni-NP electrode retains 92.4% of its capacitance even for 5000 cycles, highlighting possible applications for it in the developing field of renewable energy. The current study provides a new method for producing high-rate next-generation electrodes for supercapacitors.

11.
Mikrochim Acta ; 188(4): 131, 2021 03 19.
Artigo em Inglês | MEDLINE | ID: mdl-33742263

RESUMO

An electrocatalyst modified electrode has been investigated to develop the rapid detection of antibiotics. The modified electrocatalyst was intended for the determination of sulfadiazine (SFZ) in biological fluids by electrochemical methods. Nanocube of zinc manganite (ZnMn2O4-NC) is prepared by hydrothermal method and a glassy carbon electrode (GCE) has been modified with the zinc manganite. The ZnMn2O4/GCE exhibit enhanced detection performances towards SFZ drug owing to their selective adsorption ability and the combination of electrostatic attraction of nanocube with SFZ. The modified electrocatalyst shows excellent electrocatalytic interactions with antibiotic drug. Besides, the modified sensors exhibit nanomolar detection limit (0.0021 µM) in 0.05 M phosphate buffer (pH = 7.0) using differential pulse voltammetric method. The working range of the modified electrode is 0.008-1264 µM, and the sensitivity of the SFZ sensor is 11.44 µA µM-1 cm-2. The modified sensor stability and reproducibility performances have been examined by electrochemical method. In addition, the obtained results of real sample analysis with different concentrations of SFZ in biological fluids are satisfactory with good recovery.

12.
J Hazard Mater ; 413: 125265, 2021 07 05.
Artigo em Inglês | MEDLINE | ID: mdl-33588330

RESUMO

The design and fabrication of effective electrochemical sensor for ultrasensitive detection of feed additive and multidrug are highly significant in food analysis. In this work, we explored to develop the possibility for rapid detection of feed additive drug using bismuth telluride (Bi2Te3) decorated graphitic carbon nitrides (GCN) nanostructures as a modified electrode for electrochemical sensing. Herein, the modified electrode was focused on the development of electrocatalytic performances for the determination of salbutamol in food products. The electrochemical sensors are developed by bismuth telluride sheets interconnected with graphitic carbon nitrides sheets (Bi2Te3/GCN) on to a screen-printed carbon electrode. The binary nanosheets of Bi2Te3/GCN exhibited an enhanced electrocatalytic ability towards salbutamol detection owing to their selective adsorption, by the combination of electrostatic interaction of binary nanosheets and the formation of charge assisted interactions between salbutamol and Bi2Te3/GCN surfaces. A nanomolar limit of detection (1.36 nM) was calculated in 0.05 M phosphate buffer (PB) supporting electrolyte (pH 7.0) using differential pulse voltammetry. The linear dynamic ranges with respect to salbutamol concentration were 0.01-892.5 µM, and the sensitivity of the sensor was 36.277 µA µM-1 cm-2. The sensor stability and reproducibility performances were observed. However, the obtained results are highly satisfactory which suggest the application of binary nanosheets in real-time food analysis.


Assuntos
Albuterol , Técnicas Eletroquímicas , Bismuto , Eletrodos , Grafite , Carne/análise , Compostos de Nitrogênio , Reprodutibilidade dos Testes , Telúrio
13.
Colloids Surf B Biointerfaces ; 200: 111577, 2021 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-33524698

RESUMO

In this work, we report a novel preparation of selenium nanorods (Se) doped cobalt oxide (Co3O4) nanoflowers encapsulated with graphene oxide (GO) nanocomposite (NC). Se nanorods were successfully decorated on Co3O4 nanoflowers and an increase in electrical conductivity was observed in Se-Co3O4@GO-NC. The as-prepared Se-Co3O4@GO-NC was utilized as an effective nanocomposite for the electrochemical detection of dimetridazole (DMZ) for the first time in the field of electrochemical sensors. Se-Co3O4@GO-NC modified glassy carbon electrode (GCE) which showed an excellent cathodic current response (17.6 µA) at the lower potential at -0.7314 V upon DMZ sensing. With the various optimized conditions, Se-Co3O4@GO-NC based electrochemical sensor displayed a lengthy linear range of 0.02-83.72 µM, limit of detection 3.4 nM and sensitivity of 1.898 µA.µM-1. cm-2 for DMZ detection. In addition, Se-Co3O4@GO-NC revealed fabulous catalytic reduction activity for DMZ, when compared to GO and Se-Co3O4 modified GCE. Additionally, Se-Co3O4@GO-NC is applied in real sample analysis of pigeon egg, milk and pigeon meat. The results illustrated that Se-Co3O4@GO-NC can be a promising nanocomposite for the electrocatalytic reduction of DMZ in clinical samples in biomedical field.


Assuntos
Grafite , Nanotubos , Animais , Columbidae , Técnicas Eletroquímicas , Carne , Leite
14.
Ecotoxicol Environ Saf ; 208: 111701, 2021 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-33396032

RESUMO

Harmful chemicals are always found in the environment and it is necessary to construct a viable sensor to detect those chemicals. In order to construct an electrochemical sensing platform, designing an electrode using bismuth mixed oxides are more important and which grabbed more attention due to its high electrocatalytic ability and conductivity. In this literature, we report a facile synthesis of thorn apple like structured pure bismuth molybdate (Bi2MoO6) using a simple hydrothermal assisted one-step calcination method and we report a facile method to sense 4-cyanophenol by electrochemical technique. Bi2MoO6 modified (Glassy Carbon electrode) GCE possess two linear ranges 0.1-39.1 µM and 46.6-110.1 µM with excellent detection limit 0.008297 µM and 0.01097 µM. Also, this novel sensor is steady with good stability, repeatability, and reproducibility. Successfully, the environmental water sample is analyzed as a real sample with a feasible and quantification results which were compared with HPLC analysis.


Assuntos
Bismuto/química , Técnicas Eletroquímicas , Monitoramento Ambiental/métodos , Molibdênio/química , Fenóis/análise , Poluentes Químicos da Água/análise , Carbono/química , Eletrodos , Limite de Detecção , Fenóis/química , Reprodutibilidade dos Testes , Água/química , Poluentes Químicos da Água/química
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