Ti3AlC2 MAX Phase Modified Screen-Printed Electrode for the Fabrication of Hydrazine Sensor.

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.

Preconcentration and selective extraction of trace Hg(ii) by polymeric g-C3N4 nanosheet-packed SPE column.

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.

In Situ Fabrication and Characterization of g-C3N4 onto Cellulose Nanofibers and Selective Separation of Heavy Metal Ions.

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.

MoS2/S@g-CN Composite Electrode for L-Tryptophan Sensing.

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.

Fabrication of an Azithromycin Sensor.

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.

Green Synthesis of Copper Oxide Nanoparticles from the Leaves of Aegle marmelos and Their Antimicrobial Activity and Photocatalytic Activities.

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.

Recent advances in synthesis and characterization of iron-nickel bimetallic nanoparticles and their applications as photo-catalyst and fuel additive.

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.

Covalently linked mercaptoacetic acid on ZrO2 coupled cellulose nanofibers for solid phase extraction of Hg(ii): experimental and DFT studies.

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.

Electrocatalytic Behavior of an Amide Functionalized Mn(II) Coordination Polymer on ORR, OER and HER.

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.

Numerical Simulation of NH3(CH2)2NH3MnCl4 Based Pb-Free Perovskite Solar Cells Via SCAPS-1D.

Recently, the design and fabrication of lead (Pb)-free perovskite or perovskite-like materials have received great interest for the development of perovskite solar cells (PSCs). Manganese (Mn) is a less toxic element, which may be an alternative to Pb. In this work, we explored the role of NH3(CH2)2NH3MnCl4 perovskite as a light absorber layer via SCAPS-1D. A Pb-free PSC device (FTO/TiO2/NH3(CH2)2NH3MnCl4/spiro-OMeTAD/Au) was simulated via SCAPS-1D software. The simulated Pb-free PSCs (FTO/TiO2/NH3(CH2)2NH3MnCl4/spiro-OMeTAD/Au) showed decent power conversion efficiency (PCE) of 20.19%. Further, the impact of the thickness of absorber (NH3(CH2)2NH3MnCl4), electron transport (TiO2), and hole-transport (spiro-OMeTAD) layers were also investigated. Subsequently, various electron transport layers (ETLs) were also introduced to investigate the role of ETL. In further studies, an NH3(CH2)2NH3MnCl4-based PSC device (FTO/TiO2/NH3(CH2)2NH3MnCl4/spiro-OMeTAD/Au) was also developed (humidity = ~30-40%). The fabricated PSCs displayed an open circuit voltage (Voc) of 510 mV with a PCE of 0.12%.

Fabrication of CeO2/GCE for Electrochemical Sensing of Hydroquinone.

Hydroquinone is a widely used derivative of phenol which has a negative influence on human beings and the environment. The determination of the accurate amount of hydroquinone is of great importance. Recently, the fabrication of an electrochemical sensing device has received enormous attention. In this study, we reported on the facile synthesis of cerium dioxide (CeO2) nanoparticles (NPs). The CeO2 NPs were synthesized using cerium nitrate hexahydrate as a precursor. For determining the physicochemical properties of synthesized CeO2 NPs, various advanced techniques, viz., powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS), were studied. Further, these synthesized CeO2 NPs were used for the modification of a glassy carbon electrode (CeO2/GCE), which was utilized for the sensing of hydroquinone (HQ). A decent detection limit of 0.9 µM with a sensitivity of 0.41 µA/µM cm2 was exhibited by the modified electrode (CeO2/GCE). The CeO2/GCE also exhibited good stability, selectivity, and repeatability towards the determination of HQ.

Design and Fabrication of α-MnO2-Nanorods-Modified Glassy-Carbon-Electrode-Based Serotonin Sensor.

Serotonin is a very important monoamine neurotransmitter, which takes part in biological and psychological processes. In the present scenario, design and fabrication of a serotonin electrochemical sensor is of great significance. In this study, we have synthesized α-MnO2 via a hydrothermal synthesis method using potassium permanganate as a precursor. The physiochemical properties, such as structural and phase-purity of the prepared α-MnO2, were investigated by various characterization techniques and methods (powder X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy). Furthermore, the serotonin sensor was fabricated using α-MnO2 as an electrode modifier or electro-catalyst. The bare glassy carbon electrode (GCE) was adopted as a working substrate, and its active carbon surface was modified with the synthesized α-MnO2. This modified GCE (α-MnO2/GCE = MGCE) was explored as a serotonin sensor. The electrochemical investigations showed that the MGCE has excellent electro-catalytic properties towards determination of serotonin. The MGCE exhibits an excellent detection limit (DL) of 0.14 µM, along with good sensitivity of 2.41 µAµM-1 cm-2. The MGCE also demonstrated excellent selectivity for determination of serotonin in the presence of various electro-active/interfering molecules. The MGCE also exhibits good cyclic repeatability, stability, and storage stability.

Systematic study of physicochemical and electrochemical properties of carbon nanomaterials.

Carbon nanomaterials exhibit exceptional properties and broad horizon applications, where graphene is one of the most popular allotropes of this family due to its astounding performance in every stratum vis-à-vis other classical materials. The large surface area of 2630 m2 g-1, high electrical conductivity, and electron mobility of non-toxic graphene nanomaterials serve as the building blocks for supercapacitor studies. In this article, comparative studies are carried out between electrochemically exfoliated graphene sheets (GSs), solvothermally synthesized graphene quantum dots (GQDs) and acid refluxed carbon nanotubes (CNTs) as an energy storage electrode nanomaterial through cyclic voltammetry (CV). The electrochemical properties of the materials are well correlated with the physicochemical characteristics obtained from Raman, Fourier-transform infrared, and absorption spectroscopy. Thin GSs (0.8-1 nm) and small size (6-10 nm) GQDs fabricated by using laboratory-grade 99% purity graphite rods resulted in promising low-cost materials at mass scale as compared to conducting CNTs. The 0D graphene quantum dots proved to be an excellent energy electrode material in an alkaline electrolyte solution compared to other carbon nanomaterials. The distinct characteristic features of GQDs, like superior electrical properties, large surface area, and abundant active sites make them an ideal candidate for utilization in supercapacitors. The GQDs exhibited an enhanced specific capacitance of 113 F g-1 in 6 mol L-1 KOH through cyclic voltammetry.

Selective Extraction of Trace Arsenite Ions Using a Highly Porous Aluminum Oxide Membrane with Ordered Nanopores.

Metal ion extraction and determination at trace level concentration are challenging due to sample complexity or spectral interferences. Herein, we prepared a through-hole aluminum oxide membrane (AOM) by electrochemical anodization of aluminum substrates. The prepared AOM was characterized by scanning electron microscopy, surface area analysis, porosity measurements, and X-ray photoelectron spectroscopy. The AOM with ordered nanopores was highly porous and possess inherent binding sites for selective arsenite sorption. The AOM was used as a novel sorbent for solid-phase microextraction and preconcentration of arsenite ions in water samples. The AOM's sub-micrometer thickness allows water molecules to flow freely across the pores. Before instrumental determination, the suggested microextraction approach removes spectral interferents and improves the analyte ion concentration, with a detection limit of 0.02 µg L-1. Analyzing a standard reference material was used to validate the procedure. Student's t-test value was less than critical Student's t-value of 4.303 at a 95% confidence level. With coefficients of variation of 3.25%, good precision was achieved.

Optimization of Photovoltaic Performance of Pb-Free Perovskite Solar Cells via Numerical Simulation.

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.

Coumarin Exhibits Broad-Spectrum Antibiofilm and Antiquorum Sensing Activity against Gram-Negative Bacteria: In Vitro and In Silico Investigation.

Quorum sensing (QS) and biofilm inhibition are recognized as the novel drug targets for the broad-spectrum anti-infective strategy to combat the infections caused by drug-resistant bacterial pathogens. Many compounds from medicinal plants have been found to demonstrate anti-infective activity. However, broad-spectrum anti-QS and antibiofilm efficacy and their mode of action are poorly studied. In this study, the efficacy of coumarin was tested against QS-regulated virulent traits of Gram-negative bacteria. Coumarin inhibited the production of violacein pigment in Chromobacterium violaceum 12472 by 64.21%. Similarly, there was 87.25, 70.05, 76.07, 58.64, 48.94, and 81.20% inhibition of pyocyanin, pyoverdin, and proteolytic activity, lasB elastase activity, swimming motility, and rhamnolipid production, respectively, in Pseudomonas aeruginosa PAO1. All tested virulence factors of Serratia marcescens MTCC 97 were also suppressed by more than 50% at the highest sub-minimum inhibitory concentration. Moreover, the biofilms of bacterial pathogens were also inhibited in a dose-dependent manner. Molecular docking and molecular dynamics (MD) simulation gave insights into the possible mode of action. The binding energy obtained by docking studies ranged from -5.7 to -8.1 kcal mol-1. Coumarin was found to be docked in the active site of acylhomoserine lactone (AHL) synthases and regulatory proteins of QS. MD simulations further supported the in vitro studies where coumarin formed a stable complex with the tested proteins. The secondary structure of all proteins showed a negligible change in the presence of coumarin. Computational studies showed that the possible mechanisms of anti-QS activity were the inhibition of AHL synthesis, antagonization of QS-regulatory proteins, and blocking of the receptor proteins. The findings of this study clearly highlight the potency of coumarin against the virulence factors of Gram-negative bacterial pathogens that may be developed as an effective inhibitor of QS and biofilms.

Bioactive Tryptophan-Based Copper Complex with Auxiliary ß-Carboline Spectacle Potential on Human Breast Cancer Cells: In Vitro and In Vivo Studies.

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.

A novel biocompatible formate bridged 1D-Cu(ii) coordination polymer induces apoptosis selectively in human lung adenocarcinoma (A549) cells.

Copper compounds are promising candidates for next-generation metal anticancer drugs. Therefore, we synthesized and characterized a formate bridged 1D coordination polymer [Cu(L)(HCOO)2]n, (L = 2-methoxy-6-methyl-3-((quinolin-8-ylimino)methyl)chroman-4-ol), PCU1, wherein the Cu(ii) center adopts a square pyramidal coordination environment with adjacent CuCu distances of 5.28 Å. Primarily, in vitro DNA interaction studies revealed a metallopolymer which possesses high DNA binding propensity and cleaves DNA via the oxidative pathway. We further analysed its potential on cancerous cells MCF-7, HeLa, A549, and two non-tumorigenic cells HEK293 and HBE. The selective cytotoxicity potential of PCU1 against A549 cells driven us to examine the mechanistic pathways comprehensively by carrying out various assays viz, cell cycle arrest, Annexin V-FTIC/PI assay, autophagy, intercellular localization, mitochondrial membrane potential 'MMP', antiproliferative assay, and gene expression of TGF-ß and MMP-2.

Graphene oxide lamellar membrane with enlarged inter-layer spacing for fast preconcentration and determination of trace metal ions.

We report a graphene oxide (GO) lamellar membrane with increased inter-layer spacing for efficient permeation of water molecules and heavy metal ions through nanoporous graphene oxide. The inter-layer spacing of the GO sheets in the lamellar structure was increased by introducing poly-aminophosphonic acid (APA) in between the GO sheets. We demonstrate experimentally, the use of a prepared membrane (GO-APA) by a SPE technique for the preconcentration and extraction of heavy metal ions by chelate formation and their determination by ICP-OES. We found that this sub-micrometer-thick membrane allows unimpeded permeation of water molecules through two-dimensional capillaries formed across the pores and by closely spaced graphene sheets. Compared to the bulk GO sorbent, GO-APA membrane offers enhanced sensitivity and permeability for heavy metal ions due to relatively large inter-layer spacing and high surface area (extraction phase) with a high number of active functional groups. The potential of this technique for the preconcentration and extraction of Pb(ii), Cd(ii) and Cu(ii) is illustrated with the contaminated ground water and industrial waste water analysis. The detection limit achieved for studied ions was 1.1 ng L-1, under optimized experimental conditions. The co-existing ions did not hinders the extraction of trace heavy metal ions. Accuracy of the developed method was assessed by analyzing Standard Reference Materials. The Student's t test values were found to less than the critical Student's t value of 4.303 at the 95% confidence level. The method shows good precision as coefficients of variation for five replicate measurements were found to be 4-5%.

Preconcentration and determination of trace Hg(ii) using ultrasound-assisted dispersive solid phase microextraction.

Defect rich molybdenum disulfide (MoS2) nanosheets were hydrothermally synthesized and their potential for ultrasound assisted dispersive solid phase microextraction of trace Hg(ii) ions was assessed. Ultrasonic dispersion allows the MoS2 nanosheets to chelate rapidly and evenly with Hg(ii) ions and results in improving the precision and minimizing the extraction time. The multiple defect rich surface was characterized by X-ray diffraction and high-resolution transmission electron microscopy. The surface charge of intrinsically sulfur rich MoS2 nanosheets and their elemental composition was characterized by zeta potential measurements, energy dispersive spectroscopy, and X-ray photoelectron spectroscopy. The cracks and holes on the basal planes of MoS2 led to diffusion of the Hg(ii) ions into the interior channels. Inner-sphere chelation along with outer-sphere electrostatic interaction were the proposed mechanism for the Hg(ii) adsorption onto the MoS2 surface. The experimental data showed good selectivity of MoS2 nanosheets towards Hg(ii) adsorption. The systematic and constant errors of the proposed method were ruled out by the analysis of the Standard Reference Material (>95% recovery with <5% RSD). The Student's t-test values for the analyzed Standard Reference Material were found to be less than the critical Student's t value at 95% confidence level. The limit of detection (3S) was found to be 0.01 ng mL-1. The MoS2 nanosheets were successfully employed for the analysis of Hg(ii) in environmental water samples.