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1.
Molecules ; 28(22)2023 Nov 09.
Artigo em Inglês | MEDLINE | ID: mdl-38005229

RESUMO

The leaves of the Aegle marmelos plant were used for the green synthesis of copper oxide nanoparticles and further characterized by different techniques, including (Ultra Violet-Visible) UV-Vis, Scanning electron microscopy (SEM), Energy dispersive X-ray (EDX), Transmission electron microscopy (TEM) and X-ray diffraction (XRD). The UV-Vis showed a peak at 330 nm, which may be due to the Surface Plasmon Resonance phenomenon. XRD analysis showed the crystalline nature of copper oxide nanoparticles (CuO NPs). In contrast, SEM showed that nanoparticles were not aggregated or clumped, EDX showed the presence of elemental copper., and further, the TEM analysis revealed the average particle size of copper oxide nanoparticles to be 32 nm. The Minimum Inhibitory Concentration (MIC) for Escherichia coli (E. coli) and Staphylococcusaureus (S. aureus) was found to be 400 µg/mL, whereas for Candida albicans (C. albicans) and Candida dubliniensis (C. dubliniensis) it was 800 µg/mL. The zone of inhibition in the well diffusion assay showed the antimicrobial activity of copper oxide nanoparticles, and it also showed that as the concentration of copper oxide nanoparticles increased, the zone of inhibition also increased. Further, the electron microscopic view of the interaction between copper oxide nanoparticles and C. albicans cells showed that CuO NPs were internalized and attached to the cell membrane, which caused changes in the cellular structure and caused deformities which eventually led to cell death. The prepared CuO NPs showed significant photocatalytic degradation of organic dyes in the presence of sunlight.


Assuntos
Aegle , Nanopartículas Metálicas , Antibacterianos/química , Cobre/química , Nanopartículas Metálicas/química , Escherichia coli , Staphylococcus aureus , Extratos Vegetais/química , Óxidos , Testes de Sensibilidade Microbiana , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios X
2.
Molecules ; 28(1)2022 Dec 27.
Artigo em Inglês | MEDLINE | ID: mdl-36615419

RESUMO

Recently, the simulation of perovskite solar cells (PSCs) via SCAPS-1D has been widely reported. In this study, we adopted SCAPS-1D as a simulation tool for the numerical simulation of lead-free (Pb-free) PSCs. We used methyl ammonium germanium iodide (MAGeI3) as a light absorber, zinc oxysulphide (ZnOS) as an electron transport layer (ETL), and spiro-OMeTAD as a hole transport layer. Further, the thickness of the ZnOS, MAGeI3, and spiro-OMeTAD layers was optimized. The optimal thicknesses of the ZnOS, MAGeI3, and spiro-OMeTAD layers were found to be 100 nm, 550 nm, and 100 nm, respectively. The optimized MAGeI3-based PSCs exhibited excellent power conversion efficiency (PCE) of 21.62%, fill factor (FF) of 84.05%, and Jsc of 14.51 mA/cm2. A fantastic open circuit voltage of 1.77 V was also obtained using SCAPS-1D. We believe that these theoretically optimized parameters and conditions may help improve the experimental efficiency of MAGeI3-based PSCs in the future.

3.
Molecules ; 27(21)2022 Oct 28.
Artigo em Inglês | MEDLINE | ID: mdl-36364154

RESUMO

The new 3D coordination polymer (CP) [Mn(L)(HCOO)]n (Mn-CP) [L = 4-(pyridin-4-ylcarbamoyl)benzoate] was synthesised via a hydrothermal reaction using the pyridyl amide functionalized benzoic acid HL. It was characterized by elemental, FT-IR spectroscopy, single-crystal and powder X-ray diffraction (PXRD) analyses. Its structural features were disclosed by single-crystal X-ray diffraction analysis, which revealed a 3D structure with the monoclinic space group P21/c. Its performance as an electrocatalyst for oxygen reduction (ORR), oxygen evolution (OER), and hydrogen evolution (HER) reactions was tested in both acidic (0.5 M H2SO4) and alkaline (0.1 M KOH) media. A distinct reduction peak was observed at 0.53 V vs. RHE in 0.1 M KOH, which corresponds to the oxygen reduction, thus clearly demonstrating the material's activity for the ORR. Tafel analysis revealed a Tafel slope of 101 mV dec-1 with mixed kinetics of 2e- and 4e- pathways indicated by the Koutecky-Levich analysis. Conversely, the ORR peak was not present in 0.5 M H2SO4 indicating no activity of Mn-CP for this reaction in acidic media. In addition, Mn-CP demonstrated a noteworthy activity toward OER and HER in acidic media, in contrast to what was observed in 0.1 M KOH.


Assuntos
Amidas , Polímeros , Espectroscopia de Infravermelho com Transformada de Fourier , Oxigênio , Hidrogênio
4.
Molecules ; 26(6)2021 Mar 14.
Artigo em Inglês | MEDLINE | ID: mdl-33799355

RESUMO

Biocompatible tryptophan-derived copper (1) and zinc (2) complexes with norharmane (ß-carboline) were designed, synthesized, characterized, and evaluated for the potential anticancer activity in vitro and in vivo. The in vitro cytotoxicity of both complexes 1 and 2 were assessed against two cancerous cells: (human breast cancer) MCF7 and (liver hepatocellular cancer) HepG2 cells with a non-tumorigenic: (human embryonic kidney) HEK293 cells. The results exhibited a potentially decent selectivity of 1 against MCF7 cells with an IC50 value of 7.8 ± 0.4 µM compared to 2 (less active, IC50 ~ 20 µM). Furthermore, we analyzed the level of glutathione, lipid peroxidation, and visualized ROS generation to get an insight into the mechanistic pathway and witnessed oxidative stress. These in vitro results were ascertained by in vivo experiments, which also supported the free radical-mediated oxidative stress. The comet assay confirmed the oxidative stress that leads to DNA damage. The histopathology of the liver also ascertained the low toxicity of 1.


Assuntos
Antineoplásicos/farmacologia , Neoplasias da Mama/tratamento farmacológico , Carbolinas/farmacologia , Cobre/farmacologia , Triptofano/farmacologia , Animais , Neoplasias da Mama/metabolismo , Linhagem Celular , Linhagem Celular Tumoral , Ensaio Cometa/métodos , Dano ao DNA/efeitos dos fármacos , Feminino , Glutationa/metabolismo , Células HEK293 , Células Hep G2 , Humanos , Peroxidação de Lipídeos/efeitos dos fármacos , Células MCF-7 , Estresse Oxidativo/efeitos dos fármacos , Ratos , Espécies Reativas de Oxigênio/metabolismo , Zinco/farmacologia
5.
Microb Pathog ; 144: 104172, 2020 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-32224208

RESUMO

Antimicrobial resistance among pathogenic bacteria has become a global threat to human health. Due to poor progress in development of new antimicrobial drugs, there is a need for the development of novel alternative strategies to combat the problem of multidrug resistance. Moreover, there is focus on ecofriendly approach for the synthesis nanoparticles having efficient medicinal properties including antivirulence properties to tackle the emergence of multi-drug resistance. Targeting quorum sensing controlled virulence factors and biofilms has come out to be a novel anti-infective drug target. The silver nanoparticles (Ag@CC-NPs) were synthesized from aqueous extract of Carum copticum and characterized using UV-vis absorption spectroscopy, fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Ag@CC-NPs were checked for its ability to inhibit quorum sensing-mediated virulence factors and biofilms against three test pathogens at sub-MIC values. There was ~75% inhibition of violacein production by Ag@CC-NPs against C. violaceum. The P. aeruginosa virulence factors such as pyocyanin production, pyoverdin production, exoprotease activity, elastase activity, swimming motility and rhamnolipid production were inhibited by 76.9, 49.0, 71.1, 53.3, 89.5, and 60.0% at sub-MIC. Moreover, virulence factors of S. marcescens viz. prodigiosin production, exoprotease activity, and swarming motility was reduced by 78.4, 67.8, and 90.7%. Ag@CC-NPs also exhibited broad-spectrum antibiofilm activity with 77.6, 86.3, and 75.1% inhibition of biofilms of P. aeruginosa, S. marcescens, and C. violaceum respectively. The biofilm formation on glass coverslip was reduced remarkably as evident from SEM and CLSM analysis. The findings revealed the in vitro efficacy of Ag@CC-NPs against bacterial pathogens and can be exploited in the development of alternative therapeutic agent in management of bacterial infections for topical application, mainly wound infection, or coating of surfaces to prevent bacterial adherence on medical devices.


Assuntos
Antibacterianos/farmacologia , Biofilmes/efeitos dos fármacos , Nanopartículas Metálicas/química , Percepção de Quorum/efeitos dos fármacos , Prata/farmacologia , Fatores de Virulência/antagonistas & inibidores , Carum/metabolismo , Chromobacterium/efeitos dos fármacos , Farmacorresistência Bacteriana Múltipla/fisiologia , Indóis/metabolismo , Locomoção/efeitos dos fármacos , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Prodigiosina/biossíntese , Pseudomonas aeruginosa/efeitos dos fármacos , Piocianina/biossíntese , Serratia marcescens/efeitos dos fármacos , Infecção dos Ferimentos/tratamento farmacológico , Infecção dos Ferimentos/microbiologia
6.
Molecules ; 25(22)2020 Nov 13.
Artigo em Inglês | MEDLINE | ID: mdl-33202876

RESUMO

Seeking to enrich the yet less explored field of scorpionate complexes bearing antioxidant properties, we, here, report on the synthesis, characterization and assessment of the antioxidant activity of new complexes derived from three scorpionate ligands. The interaction between the scorpionate ligands thallium(I) hydrotris(5-methyl-indazolyl)borate (TlTp4Bo,5Me), thallium(I) hydrotris(4,5-dihydro-2H-benzo[g]indazolyl)borate (TlTpa) and potassium hydrotris(3-tert-butyl- pyrazolyl)borate (KTptBu), and metal(II) chlorides, in dichloromethane at room temperature, produced a new family of complexes having the stoichiometric formula [M(Tp4Bo,5Me)2] (M = Cu, 1; Zn, 4; Cd, 7), [M(Tpa)2] (M = Cu, 2; Zn, 5; Cd, 8), [Cu(HpztBu)3Cl2] (3), [Zn(TptBu)Cl] (6) and [Cd(BptBu)(HpztBu)Cl] (9). The obtained metal complexes were characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance and elemental analysis, highlighting the total and partial hydrolysis of the scorpionate ligand TptBu during the synthesis of the Cu(II) complex 3 and the Cd(II) complex 9, respectively. An assessment of the antioxidant activity of the obtained metal complexes was performed through both enzymatic and non-enzymatic assays against 1,1-diphenyl-2-picryl- hydrazyl (DPPH·), 2,2'-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS+·), hydroxyl (HO·), nitric oxide (NO·), superoxide (O2-) and peroxide (OOH·) radicals. In particular, the complex [Cu(Tpa)2]⋅0.5H2O (2) exhibited significant antioxidant activity, as good and specific activity against superoxide (O2-·), (IC50 values equal to 5.6 ± 0.2 µM) and might be identified as auspicious SOD-mimics (SOD = superoxide dismutase).


Assuntos
Antioxidantes/análise , Cádmio/análise , Cobre/análise , Zinco/análise , Benzotiazóis/química , Compostos de Bifenilo/química , Radical Hidroxila/química , Concentração Inibidora 50 , Ligantes , Espectroscopia de Ressonância Magnética , Óxido Nítrico/química , Peróxidos/química , Picratos/química , Espectroscopia de Infravermelho com Transformada de Fourier , Ácidos Sulfônicos/química , Superóxidos/química , Temperatura , Tálio/química
7.
Molecules ; 25(24)2020 Dec 17.
Artigo em Inglês | MEDLINE | ID: mdl-33348597

RESUMO

Epoxy resins (EP) have been used as a thermos-setting material in the field of coating, casting, bonding agent, and laminating. However, a major drawback associated with its use is the lack of good flaming properties, and it is responsible for heavy smoke along with hazardous gases considerably limiting its uses in various fields. In this study, N-ethanolamine triazine-piperizine, a melamine polymer (ETPMP), was established as a new charring-foaming agent and was successfully synthesized with ethanolamine, piperizine, cyanuric chloride, and melamine as precursor molecules via the nucleophilic substitution reaction method. Elemental analysis and Fourier transform infrared (FTIR) spectroscopy analysis were applied to approve the synthesis of ETPMP and confirmation of its structure and characterization. The epoxy coating of intumescent flame retardant (IFR) was equipped by introducing ETPMP, ammonium polyphosphate (APP), and copper oxide (CuO) in multiple composition ratios. CuO was loaded at various amounts into the IFR-coating system as a synergistic agent. The synergistic action of CuO on IFR coatings was scientifically examined by using different analytical tests such as vertical burning test (UL-94V), limited oxygen index (LOI), thermal gravimetric analysis (TGA), cone calorimeter, and scanning electron microscope (SEM). The results showed that small changes in the amount of CuO expressively amplified the LOI results and enhanced the V-0 ratings in the UL-94V test. The TGA data clearly demonstrate that the inclusion of CuO can transform the thermal deprivation behavior of coatings with a growing char slag proportion with elevated temperatures. Information from cone calorimeter data affirmed that CuO can decrease the burning factors by total heat release (THR) together with peak heat release rate (PHRR). The SEM images indicated that CuO can enrich the power and compression of the intumescent char that restricts the movement of heat and oxygen. Our results demonstrate a positive influence of CuO on the epoxy-headed intumescent flame retardant coatings.


Assuntos
Cobre/química , Resinas Epóxi/química , Retardadores de Chama/síntese química , Piperazinas/síntese química , Polímeros/química , Compostos Benzidrílicos/química , Calorimetria , Análise Diferencial Térmica , Fenóis/química , Piperazinas/química , Espectroscopia de Infravermelho com Transformada de Fourier , Triazinas/química
8.
J Fluoresc ; 29(4): 1029-1037, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31327088

RESUMO

A novel coumarin based Schiff base sensor probe 1, was synthesized and structural elucidation was carried out by FTIR, UV-vis, 1H and 13C NMR and MS spectroscopy. The optical properties of the sensor probe were investigated by employing absorption and fluorescence titrations which showed specific recognition behaviour being highly selective towards Cd2+ over the other 3d transition metal ions. The strong fluorometric response of probe 1 towards Cd2+ ion is attributed to inhibition of C=N isomerization effect upon coordination of the metal ion. The binding stoichiometry was determined by Job's plot and the probable sensing mechanism of the probe towards Cd2+ was investigated by employing FTIR spectra analysis and 1H NMR titration experiments. Computational validation of the sensing mechanism in various modes towards Cd2+ was also performed by carrying out the DFT studies which were found to be in good concordance with the experimental results. The reversible nature of the probe was studied by EDTA titration indicating that it can be reused. Interaction studies of the sensor probe with the BSA showed the practical applicability for the quantitative determination of Cd2+ concentration in the blood plasma. The lower detection limit of the probe upto 0.114 µM further proves its practical application in the sensing phenomenon.

9.
Int J Mol Sci ; 19(5)2018 May 16.
Artigo em Inglês | MEDLINE | ID: mdl-29772746

RESUMO

Herein, we have synthesized and characterized a new benzimidazole-derived "BnI" ligand and its copper(II) complex, [Cu(BnI)2], 1, and zinc(II) complex, [Zn(BnI)2], 2, using elemental analysis and various spectroscopic techniques. Interaction of complexes 1 and 2 with the biomolecules viz. HSA (human serum albumin) and DNA were studied using absorption titration, fluorescence techniques, and in silico molecular docking studies. The results exhibited the significant binding propensity of both complexes 1 and 2, but complex 1 showed more avid binding to HSA and DNA. Also, the nuclease activity of 1 and 2 was analyzed for pBR322 DNA, and the results obtained confirmed the potential of the complexes to cleave DNA. Moreover, the mechanistic pathway was studied in the presence of various radical scavengers, which revealed that ROS (reactive oxygen species) are responsible for the nuclease activity in complex 1, whereas in complex 2, the possibility of hydrolytic cleavage also exists. Furthermore, the cytotoxicity of the ligand and complexes 1 and 2 were studied on a panel of five different human cancer cells, namely: HepG2, SK-MEL-1, HT018, HeLa, and MDA-MB 231, and compared with the standard drug, cisplatin. The results are quite promising against MDA-MB 231 (breast cancer cell line of 1), with an IC50 value that is nearly the same as the standard drug. Apoptosis was induced by complex 1 on MDA-MB 231 cells predominantly as studied by flow cytometry (FACS). The adhesion and migration of cancer cells were also examined upon treatment of complexes 1 and 2. Furthermore, the in vivo chronic toxicity profile of complexes 1 and 2 was also studied on all of the major organs of the mice, and found them to be less toxic. Thus, the results warrant further investigations of complex 1.


Assuntos
Antineoplásicos/química , Antineoplásicos/farmacologia , Benzimidazóis/química , Benzimidazóis/farmacologia , Técnicas de Química Sintética , Cobre/química , Desenho de Fármacos , Zinco/química , Antineoplásicos/síntese química , Apoptose/efeitos dos fármacos , Benzimidazóis/síntese química , Adesão Celular/efeitos dos fármacos , Linhagem Celular Tumoral , Movimento Celular/efeitos dos fármacos , DNA/genética , DNA/metabolismo , Clivagem do DNA , Transferência Ressonante de Energia de Fluorescência , Humanos , Ligantes , Modelos Moleculares , Conformação Molecular , Conformação de Ácido Nucleico , Albumina Sérica/química , Albumina Sérica/metabolismo , Termodinâmica
10.
Molecules ; 23(5)2018 05 21.
Artigo em Inglês | MEDLINE | ID: mdl-29883398

RESUMO

Three new transition metal complexes, Cu(II) 1, Co(II) 2, and Zn(II) 3 with ligand "bimnap" derived from 1-methyl-2-aminobenzimidazole and 2-hydroxynapthaldehyde were synthesized and characterized. The structure of the ligand was determined by single X-ray crystallography. All the three complexes, 1⁻3, were examined for the mode of interaction with biomolecule viz., calf thymus-DNA (CT-DNA) using various spectroscopic methods. The nuclease activity was performed against pBR322 DNA that exhibited concentration-dependent degradation of the nucleic acid. The mechanism of DNA cleavage was studied by the electrophoretic pattern in the presence of the radical scavengers. Also, the complexes 1⁻3 were analyzed for groove binding affinity. Moreover, in vitro cytotoxicities of the complexes 1⁻3 were tested against the five human cancer cell lines, i.e., HeLa, SK-MEL-1, HepG2, HT108, and MDA-MB 231. Also, the cell adhesion and migration properties upon treatment of cell lines with complexes 1⁻3, and consequently, their cell death pathway via apoptosis and necrosis were analyzed. Further, complexes 1⁻3 were studied in vivo for their toxicities and tolerabilities in mice. In sum, the complexes 1⁻3 showed merits of an effective anticancer agent in cell lines⁻based study while minor side effects were observed in vivo.A green solvent extraction technology involving a microwave processing method was used to increase the content of minor ginsenosides from Panax notoginseng. This article aims to investigate the optimization of preparation of the minor ginsenosides by this microwave processing method using single-factor experiments and response surface methodology (RSM), and discuss the blood-enriching activity and hemostatic activity of the extract of microwave processed P. notoginseng (EMPN) The RSM for production of the minor ginsenosides was based on a three-factor and three-level Box-Behnken design. When the optimum conditions of microwave power, temperature and time were 495.03 W, 150.68 °C and 20.32 min, respectively, results predicted that the yield of total minor ginsenosides (Y9) would be 93.13%. The actual value of Y9 was very similar to the predicted value. In addition, the pharmacological results of EMPN in vivo showed that EMPN had the effect of enriching blood in N-acetylphenylhydrazine (APH) and cyclophosphamide (CTX)-induced blood deficient mice because of the increasing content of white blood cells (WBCs) and hemoglobin (HGB) in blood. Hemostatic activity in vitro of EMPN showed that it had significantly shortened the clotting time in PT testing (p < 0.05). The hemostatic effect of EMPN was mainly caused by its components of Rh4, 20(S)-Rg3 and 20(R)-Rg3. This microwave processing method is simple and suitable to mass-produce the minor ginsenosides from P. notoginseng.


Assuntos
Antineoplásicos/síntese química , Benzimidazóis/síntese química , Complexos de Coordenação/síntese química , Animais , Antineoplásicos/farmacologia , Apoptose/efeitos dos fármacos , Benzimidazóis/farmacologia , Adesão Celular/efeitos dos fármacos , Linhagem Celular Tumoral , Movimento Celular/efeitos dos fármacos , Sobrevivência Celular/efeitos dos fármacos , Cobalto/química , Complexos de Coordenação/farmacologia , Cobre/química , Cristalografia por Raios X , DNA/química , Clivagem do DNA , Ensaios de Seleção de Medicamentos Antitumorais , Feminino , Sequestradores de Radicais Livres/química , Humanos , Ligantes , Masculino , Camundongos , Estrutura Molecular , Relação Estrutura-Atividade , Zinco/química
11.
Micromachines (Basel) ; 15(8)2024 Aug 18.
Artigo em Inglês | MEDLINE | ID: mdl-39203698

RESUMO

L-tryptophan is an amino acid that significantly impacts metabolic activity in both humans and herbivorous animals. It is also known as a precursor for melatonin and serotonin, and its levels must be regulated in the human body. Therefore, there is a need to develop a cost-effective, simple, sensitive, and selective method for detecting L-tryptophan. Herein, we report the fabrication of an L-tryptophan sensor using a nickel-doped tungsten oxide ceramic-modified electrode. The Ni-WO3 was synthesized using simple strategies and characterized by various advanced techniques such as powder X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and photoelectron X-ray spectroscopy. Furthermore, a glassy carbon electrode was modified with the synthesized Ni-WO3 and explored as the L-tryptophan (L-TRP) sensor. Cyclic voltammetry and differential pulse voltammetry were used to investigate the sensing ability of the modified electrode (Ni-WO3/GC). The Ni-WO3/GC exhibited an excellent limit of detection of 0.4 µM with a good dynamic linear range. The Ni-WO3/GC also demonstrated excellent selectivity in the presence of various electroactive molecules. The Ni-WO3/GC also showed decent reproducibility, repeatability, stability, and storage stability. This work proposes the fabrication of novel Ni-WO3/GC for the sensing of L-tryptophan. So far, no report is available on the use of Ni-WO3/GC for the sensing of L-TRP. This is the first report on the use of Ni-WO3/GC for the sensing of L-TRP sensing applications.

12.
Micromachines (Basel) ; 15(5)2024 May 09.
Artigo em Inglês | MEDLINE | ID: mdl-38793207

RESUMO

Hydrazine is considered a powerful reducing agent and catalyst, showing diverse applications in agricultural industries, toxic degradation research, and wastewater management. Additionally, hydrazine can trigger some specific reactions when combined with suitable oxidants. Due to its highly polar nature, hydrazine can easily dissolve in alcohol, water, and various other polar solvents. Therefore, it can be extensively utilized in different areas of application and industries such as rocketry and various chemical applications. Despite its beneficial properties, hydrazine is unstable, posing significant risk due to its highly toxic nature. It is extremely hazardous to both human health and the environment. It can cause various illnesses and symptoms such as dizziness, temporary blindness, damage to the central nervous system, and even death when inhaled in sufficient quantities. Therefore, it is highly important to monitor the level of hydrazine to prevent its toxic and hazardous effects on human beings and the environment. In the present study, we discuss the simple fabrication of a disposable cost-effective and eco-friendly hydrazine sensor. We used a screen-printed carbon electrode, i.e., SPCE, as a base for the construction of a hydrazine sensor. The Ti3AlC2 MAX has been used as a suitable and efficient electrode material for the fabrication of disposable hydrazine sensors. We modified the active surface of the SPCE using a drop-casting approach. The resulting Ti3AlC2 MAX modified SPCE (Ti3AlC2@SPCE) has been utilized as an efficient and low-cost hydrazine sensor. Cyclic voltammetry, i.e., CV, and linear sweep voltammetry, viz., LSV, was employed as a sensing technique in this study. The optimization of pH and electrode material loading was conducted. The Ti3AlC2@SPCE exhibited excellent sensing performance toward hydrazine oxidation. A reasonable detection limit (0.01 µM) was achieved for hydrazine sensing. The fabricated sensor also demonstrated a reasonable linear range of 1-50 µM. This work provides the design and fabrication of simple disposable Ti3AlC2@SPCE as a suitable electrode for the determination of hydrazine using LSV technology.

13.
ACS Omega ; 9(1): 1620-1626, 2024 Jan 09.
Artigo em Inglês | MEDLINE | ID: mdl-38222511

RESUMO

Graphitic carbon nitride nanosheets were synthesized onto cellulose nanofiber surfaces utilizing an eco-friendly salt melt approach. The fabricated material CNF@C3N4 selectively removes Ni(II) and Cu(II) from electroplating wastewater samples. The immobilization of g-C3N4 on solid substrates eases handling of nanomaterial in a flow-through approach and mitigates sorbent loss during column operations. Characterization techniques such as scanning electron microscopy, tunneling electron microscopy, and X-ray photoelectron microscopy were employed to analyze the surface morphology and chemical bonding within the synthesized material. Selective Cu(II) and Ni(II) sorption predominantly arises from the soft-soft interaction between metal ions and associated nitrogen groups. An inner-sphere surface complexation mechanism effectively elucidated the interaction dynamics between the metal and CNF@C3N4. Experimental findings demonstrated satisfactory separation of Ni(II) and Cu(II) ions, with the extraction of 340.0 and 385.0 mg g-1 of material, respectively. Additionally, the devised technique was executed for the preconcentration and quantification of trace metals ions in water samples with a detection limit and limit of quantification of 0.06 and 0.20 µg L-1, respectively.

14.
RSC Adv ; 14(47): 34556-34564, 2024 Oct 29.
Artigo em Inglês | MEDLINE | ID: mdl-39479489

RESUMO

Porous materials play a crucial role in the extraction of trace analytes; yet, the attainment of high selectivity and efficient regeneration continues to pose a considerable problem. In this study, we employed a green method to synthesize porous carbon microspheres. These microspheres were subsequently functionalized with aminophosphonic acid to facilitate the extraction of heavy metal ions from real samples. A comprehensive analysis of the aminomethylphosphorylated carbon microspheres was conducted using FTIR, SEM, EDX, TEM, BET and water contact angle measuring techniques. The potential optimization of analyte enrichment can be accomplished by the proposed solid-phase extraction (SPE) approach, which notably reduces spectrum interferences following sample purification. Following the IUPAC equation, the detection limit of the proposed method was found to be 0.04 ng mL-1, after running 20 replicate blank tests. The primary focus of sequestration of trace metal ions is the formation of metal-ligand chelates within the carbon spheres, resulting in enhanced selectivity and extraction rates exceeding 99.9% from samples with low concentrations. The present studies show a significant preconcentration limit of 0.4 ng mL-1 and a substantial preconcentration factor of 500. The method was implemented to examine real food and water samples, and the obtained data exhibit significant accuracy with a relative standard deviation (RSD) of less than 5%.

15.
RSC Adv ; 14(3): 1593-1601, 2024 Jan 03.
Artigo em Inglês | MEDLINE | ID: mdl-38179094

RESUMO

In this study, we successfully synthesized polymeric graphitic carbon nitride (g-C3N4) nanosheets through thermal means and proposed their application in solid-phase extraction (SPE) for the enrichment of trace Hg(ii). The nanosheets underwent characterization using scanning electron microscopy, tunnelling electron microscopy, and energy-dispersive X-ray spectroscopy. The column packed with polymeric carbon nitride nanosheets demonstrated effective extraction of trace Hg(ii) ions from complex samples. The g-C3N4 nanosheets possess a zeta potential value of -20 mV, enabling strong interaction with positively charged divalent Hg(ii) ions. This interaction leads to the formation of stable chelates with the nitrogen atoms present in the polytriazine and heptazine units of the material. The proposed method exhibited a high preconcentration limit of 0.33 µg L-1, making it suitable for analysing trace amounts of Hg(ii) ions. Moreover, the method's applicability was confirmed through successful analysis of real samples, achieving an impressive preconcentration factor of 200. The detection limit for trace Hg(ii) ions was determined to be 0.6 µg L-1. To assess the accuracy of the method, we evaluated its performance by recovering spiked amounts of Hg(ii) and by analysing certified reference materials. The results indicated excellent precision, with RSD consistently below 5% for all the analyses conducted. In conclusion, the thermally synthesized polymeric carbon nitride nanosheets present a promising approach for solid-phase extraction and preconcentration of trace Hg(ii) from real samples. The method showcases high efficiency, sensitivity, and accuracy, making it a valuable tool for environmental and analytical applications.

16.
Chemosphere ; 364: 143001, 2024 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-39121961

RESUMO

Three novel coordination polymers (CPs), namely [Cu(µ-1κO,2κN-L)2]n (1), [Zn (µ-1κO,2κN-L)2(H2O)2]n (2) and [Cd (µ-1κOO',2κN-L)2]n (3) [where HL = 4-(pyrimidin-5-ylcarbamoyl)benzoic acid], were synthesized and characterized by elemental analysis, ATR-IR, TGA, XPS and single-crystal X-ray diffraction. Despite having the same organic ligand, the various metal cations had an impact in the subsequent frameworks. Hirshfeld surface analysis was performed to investigate the intermolecular interactions and to examine the stability of the crystal structures of the three polymers. Their catalytic performances were screened for the peroxidative oxidation of Volatile Organic Compounds (VOCs), with toluene and p-xylene selected as model substrates. Tert-butyl hydroperoxide (t-BuOOH or TBHP) (aq. 70 %) was employed as the oxidant. The catalytic oxidation of toluene yielded benzyl alcohol, benzaldehyde and benzoic acid. The copper CP 1 exhibited the highest total yield for toluene oxidation, reaching approximately 36% in an aqueous medium. For p-xylene oxidation, tolualdehyde, methylbenzyl alcohol, and toluic acid were produced as the primary products, accompanied by minor ones. The experiments were conducted under diverse conditions, manipulating key parameters such as the choice of solvent (water or acetonitrile), type of oxidant (t-BuOOH or H2O2), the concentration of the oxidant and reaction temperature. In the presence of catalyst 1, a maximum total yield of ca. 80% was achieved for p-xylene oxidation.


Assuntos
Cobre , Oxirredução , Polímeros , Compostos Orgânicos Voláteis , Cobre/química , Catálise , Polímeros/química , Compostos Orgânicos Voláteis/química , Complexos de Coordenação/química , Tolueno/química
17.
Biosensors (Basel) ; 13(11)2023 Nov 02.
Artigo em Inglês | MEDLINE | ID: mdl-37998142

RESUMO

L-tryptophan (L-TRP) is an essential amino acid responsible for the establishment and maintenance of a positive nitrogen equilibrium in the nutrition of human beings. Therefore, it is vital to quantify the amount of L-tryptophan in our body. Herein, we report the MoS2/S@g-CN-modified glassy carbon electrode for the electrochemical detection of L-tryptophan (L-TRP). The MoS2/S@g-CN composite was successfully synthesized using an efficient and cost-effective hydrothermal method. The physical and chemical properties of the synthesized composite were analyzed using powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and energy-dispersive X-ray analysis (EDX). The crystallite size of the composite was calculated as 39.4 nm, with porous balls of MoS2 decorated over the S@g-CN surface. The XPS spectrum confirmed the presence of Mo, S, O, C, and N elements in the sample. The synthesized nanocomposite was further used to modify the glassy carbon (GC) electrode (MoS2/S@g-CN/GC). This MoS2/S@g-CN/GC was used for the electrochemical detection of L-TRP using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques. For the purpose of comparison, the effects of the scanning rate and the concentration of L-TRP on the current response for the bare GC, S@g-CN/GC, MoS2/GC, and MoS2/S@g-CN/GC were studied in detail. The MoS2/S@g-CN-modified GC electrode exhibited a rational limit of detection (LoD) of 0.03 µM and a sensitivity of 1.74 µA/ µMcm2, with excellent stability, efficient repeatability, and high selectivity for L-TRP detection.


Assuntos
Grafite , Humanos , Grafite/química , Triptofano/análise , Molibdênio , Carbono/química , Eletrodos , Técnicas Eletroquímicas/métodos
18.
Biosensors (Basel) ; 13(11)2023 Nov 16.
Artigo em Inglês | MEDLINE | ID: mdl-37998161

RESUMO

Azithromycin (AZY) is a well-known top-prioritized antibiotic and is used by humans in strong concentrations. However, the side effects of the AZY antibiotic may cause some serious and significant damage to humans and the environment. Thus, there is a need to develop effective and sensitive sensors to monitor accurate concentrations of AZY. In the last decade, electrochemistry-based sensors have received enormous attention from the scientific community because of their high sensitivity, selectivity, cost-effectiveness, fast response, rapid detection response, simple fabrication, and working principle. It is important to mention that electrochemical sensors rely on the properties of electrode modifiers. Hence, the selection of electrode materials is of great significance when designing and developing efficient and robust electrochemical sensors. In this study, we fabricated an AZY sensor by utilizing a molybdenum disulfide/titanium aluminum carbide (MoS2@Ti3AlC2) composite as the electrode material. The MoS2@Ti3AlC2 composite was synthesized via a simple sonication process. The synthesized MoS2@Ti3AlC2 composite was characterized using a powder X-ray diffraction (XRD) method to examine the phase purity and formation of the MoS2@Ti3AlC2 composite. Scanning electron microscopy (SEM) was used to study the surface morphological features of the prepared MoS2@Ti3AlC2 composite, whereas energy dispersive X-ray spectroscopy (EDAX) was adopted to determine the elemental composition of the prepared MoS2@Ti3AlC2 composite. The glassy carbon (GC) electrode was modified with the prepared MoS2@Ti3AlC2 composite and applied as the AZY sensor. The sensing performance of the MoS2@Ti3AlC2 composite-modified GC electrode was studied using linear sweep voltammetry. The sensor demonstrated excellent performance when determining AZY and showed a good detection limit of 0.009 µM with a sensitivity of 6.77 µA/µM.cm2.


Assuntos
Azitromicina , Molibdênio , Humanos , Molibdênio/química , Carbono/química , Microscopia Eletrônica de Varredura , Antibacterianos , Eletrodos , Limite de Detecção , Técnicas Eletroquímicas/métodos
19.
RSC Adv ; 13(42): 29632-29644, 2023 Oct 04.
Artigo em Inglês | MEDLINE | ID: mdl-37822660

RESUMO

Iron-nickel bimetallic nanoparticles (Fe-Ni BMNPs) are prepared by combining two different metals by using the bottom-up approach. The resulting material has entirely different properties as compared to both the metals. The product is examined by using different analytical instruments such as.; scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), MDIJADE, ORIGIN pro to characterize their morphology, crystallinity and elemental composition and the final data has been statistically analyzed. SEM findings show that most nanoparticles are irregular in form and range in size from 10 nm to 100 nm. The findings of the TEM verified that the particles between 10 nm and 50 nm are irregular in size shape. The products acquired utilized as a fuel additive to monitor oil effectiveness by studying various parameters. The degradation of methylene blue dye depends directly on the concentration of the nanocatalyst. Different parameters also use the freshly prepared bimetallic nanocatalyst to investigate the efficacy of the kerosene fuel. By adding a tiny quantity of the nanocatalyst, the value of the flash point and fire point is significantly reduced. The nanocatalyst does not affect the cloud point and pour point to a large extent. The bimetallic nanocatalyst therefore has very excellent catalytic characteristics.

20.
RSC Adv ; 12(55): 35712-35721, 2022 Dec 12.
Artigo em Inglês | MEDLINE | ID: mdl-36545069

RESUMO

Zirconium oxide (ZrO2) nanoparticles were introduced onto cellulose nanofibers after being covalently functionalized with mercaptoacetic acid. We experimentally demonstrate that the nanocomposite is capable of selectively capturing Hg(ii) from aqueous samples down to trace level concentrations. Density functional theory (DFT) calculations indicate that energetically favorable R-S → Hg ← O-R bidentate complex formation enhances the rapid adsorption, leading to selective extraction of Hg(ii). Furthermore, the loss of ZrO2 particles during flow-through studies is controlled and restricted after binding to CNF rather than being used directly in the column. The Hg(ii) selectivity is primarily due to the Lewis soft-soft acid-base chelation of Hg(ii) with the mercapto functionalities of the adsorbent. The experimental observations depict a high sorption capacity of 280.5 mg g-1 for Hg(ii). The limit of detection and quantification of the proposed approach were found to be 0.04 µg L-1 and 0.15 µg L-1, respectively. Analytical method accuracy and validity were determined by analyzing Standard Reference Materials and by the standard addition method (recovery > 95% with a 5% RSD). The findings of a Student's t-test were found to be lower than the critical Student's t value. Real water samples were successfully analyzed using the developed procedure.

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