Photo-irradiation coupled biosynthesis of magnesium oxide nanoparticles for antibacterial application.

In recent times, magnesium oxide (MgO) nanoparticles are proven to be an excellent antibacterial agent which inhibits the growth of bacteria by generating reactive oxygen species (ROS). Release of ROS by nanoparticles will damage the cell membrane of bacteria and leads to the leakage of bacterial internal components and cell death. However, chemically synthesized MgO nanoparticles may possess toxic functional groups which may inhibit healthy human cells along with bacterial cells. Thus, the aim of the present study is to synthesize MgO nanoparticles using leaf extracts of Amaranthus tricolor and photo-irradiation of visible light as a catalyst, without addition of any chemicals. Optimization was performed using Box-Behnken design (BBD) to obtain the optimum condition required to synthesize smallest nanoparticles. The parameters such as time of reaction, the concentration of precursor, and light intensity have been identified to affect the size of biosynthesized nanoparticles and was optimized. The experiment performed with optimized conditions such as 0.001 M concentration of magnesium acetate as precursor, 5 cm distance of light (intensity), and 15 min of reaction time (light exposure) has led to the formation of 74.6 nm sized MgO nanoparticles. The antibacterial activities of MgO nanoparticles formed via photo-irradiation and conventional biosynthesis approach were investigated and compared. The lethal dosage of E. coli for photo-irradiated and conventional biosynthesis MgO nanoparticles was 0.6 ml and 0.4 ml, respectively. Likewise, the lethal dosage of S. aureus for both biosynthesis approaches was found to be 0.4 ml. The results revealed that the antibacterial activity of MgO nanoparticles from both biosynthesis approaches was similar. Thus, photo-irradiated MgO nanoparticles were beneficial over heat-mediated conventional method due to the reduced synthesis duration.

Formation of Mo5Si3/Mo3Si-MgAl2O4 Composites via Self-Propagating High-Temperature Synthesis.

In situ formation of intermetallic/ceramic composites composed of molybdenum silicides (Mo5Si3 and Mo3Si) and magnesium aluminate spinel (MgAl2O4) was conducted by combustion synthesis with reducing stages in the mode of self-propagating high-temperature synthesis (SHS). The SHS process combined intermetallic combustion between Mo and Si with metallothermic reduction of MoO3 by Al in the presence of MgO. Experimental evidence showed that combustion velocity and temperature decreased with increasing molar content of Mo5Si3 and Mo3Si, and therefore, the flammability limit determined for the reaction at Mo5Si3 or Mo3Si/MgAl2O4 = 2.0. Based upon combustion wave kinetics, the activation energies, Ea = 68.8 and 63.8 kJ/mol, were deduced for the solid-state SHS reactions producing Mo5Si3- and Mo3Si-MgAl2O4 composites, respectively. Phase conversion was almost complete after combustion, with the exception of trivial unreacted Mo existing in both composites and a minor amount of Mo3Si in the Mo5Si3-MgAl2O4 composite. Both composites display a dense morphology formed by connecting MgAl2O4 crystals, within which micro-sized molybdenum silicide grains were embedded. For equimolar Mo5Si3- and Mo3Si-MgAl2O4 composites, the hardness and fracture toughness are 14.6 GPa and 6.28 MPa m1/2, and 13.9 GPa and 5.98 MPa m1/2, respectively.

Mechanochemical Synthesis of CuO/MgAl2O4 and MgFe2O4 Spinels for Vanillin Production from Isoeugenol and Vanillyl Alcohol.

CuO/MgAl2O4 and CuO/MgFe2O4 catalysts were successfully synthesized with the use of spinel supports by a very simple and low-cost mechanochemical method. High-speed ball-milling was used to synthesize these catalyst supports for the first time. Materials were subsequently characterized by using XRD, FESEM, TEM, EDS-Dot mapping, XPS, BET-BJH, and Magnetic Susceptibility to investigate the physical-chemical characteristics of the catalysts. Acidity evaluation results indicated that the catalyst with the Mg-Al spinel support had more acid sites. XRD results showed a successful synthesis of the catalysts with large crystal sizes. Both catalysts were used in isoeugenol oxidation and vanillyl alcohol to vanillin reactions, with the CuO/MgAl2O4 showing optimum results. This catalyst provided 67% conversion (74% selectivity) after 2 h and this value improved to 81% (selectivity 100%) with the second reaction after 8 h. The CuO/MgFe2O4 catalyst in the first reaction after five hours revealed 53% conversion (47% selectivity) and after eight hours with the second reaction, the conversion value improved to 64% (100% selectivity). In terms of reusability, CuO/MgAl2O4 showed better results than the CuO/MgFe2O4 catalyst, for both reactions.

Biosynthesis and characterization of magnesium oxide and manganese dioxide nanoparticles using Matricaria chamomilla L. extract and its inhibitory effect on Acidovorax oryzae strain RS-2.

Bacterial brown stripe (BBS) is one of the most economically important diseases of rice caused by Acidovorax oryzae (Ao). In order to ensure food security and safe consumption, the use of non-chemical approach is necessary. In this study, MgO and MnO2 were synthesized using chamomile flower extract. The synthesized MgO and MnO2 nanoparticles were characterized by UV-Visible spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction, transmission/scanning electron microscopy. The sizes were 18.2 and 16.5 nm for MgO and MnO2 nanoparticles, respectively. The MgO and MnO2 nanoparticles reduced the growth of Ao strain RS-2 by 62.9 and 71.3%, respectively. Also, the biofilm formation and swimming motility were significantly reduced compared to the control. The antibacterial mechanisms of MgO and MnO2 nanoparticles against RS-2 reveals that MgO and MnO2 nanoparticles penetrated the cells and destroyed the cell membrane leading to leakage of cytoplasmic content. Also, the flow cytometry observation reveals that the apoptotic cell ratio of RS-2 increased from 0.97% to 99.52 and 99.94% when treated with MgO and MnO2 nanoparticles, respectively. Altogether, the results suggest that the synthesized MgO and MnO2 nanoparticles could serve as an alternative approach method for the management of BBS.

Facile synthesis of hollow mesoporous MgO spheres via spray-drying with improved adsorption capacity for Pb(II) and Cd(II).

Spherical-like MgO nanostructures have been synthesized efficiently via spray-drying combined with calcination using magnesium acetate as magnesium source. The products were characterized by means of X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and the specific surface areas were calculated using the Brunauer-Emmett-Teller (BET) method. The obtained spherical-like MgO nanostructures exhibit uniform pore sizes (7.7 nm) and high specific surface areas (180 m2 g-1). The adsorption kinetics and isotherm data agree well with pseudo-second-order model and Langmuir model, indicating the monolayer chemisorption of heavy metal ions. The spherical-like MgO nanostructures exhibited high adsorption performance for Pb(II) and Cd(II) ions, and the maximum adsorption capacities were up to 5214 mg g-1 and 4187 mg g-1, respectively. These values are much higher than those reported MgO-based adsorbents. Moreover, in less than 10 min, Pb(II) and Cd(II) ions in solution can be almost removed, which means that the spherical-like MgO possesses a high adsorption rate. XRD and FTIR analysis revealed the adsorption mechanism of Pb(II) and Cd(II) ions on MgO, which was mainly due to hydroxyl functional groups and ion exchange between Mg and heavy metal ions on the surface of MgO. These favorable performances recommend that the synthesized spherical-like MgO nanostructures would be a potential adsorbent for rapid removal of heavy metal ions from wastewater.

Antibacterial, antibiofilm, and photocatalytic activities of metals-substituted spinel cobalt ferrite nanoparticles.

This study reports the photocatalytic degradation of Methylene Blue (MB) dye (a class of dyestuffs that are resistant to biodegradation) under the influence of UV-light irradiation. Antibacterial and antibiofilm activities of ferrite nanoparticles (FO NPs) were examined against some pathogenic bacteria isolated from the medical operating room surfaces. In the same context, metals-substituted spinel cobalt ferrite nanoparticles with nominal composition [MxCo1-xFe2O4 NPs; (M = Zn, Cu, Mn; x = 0.0, 0.25, 0.5 and 0.75)] were synthesized by citrate sol-gel method. Also, the structures of the synthesized FO NPs were characterized by X-ray diffraction, and Williamson-Hall (WH) method was used to determine the crystallite size. The estimated specific surface area is found in the range from 37.99 to 107.05 m2/g, between the synthesized ferrites, Zn0.5Co0.5Fe2O4 NPs have average pore radius 1.84 nm and the pore volume was 0.136 ml/g. SEM images revealed that, the synthesized FO NPs have an unique pores and uniformly distribution, while EDX spectra shows the elemental composition for the synthesized FO NPs. The elastic properties of FO NPs have been estimated using FTIR data, whereas (M - H) hysteresis loops revealed that, by replacing cobalt ions with Zn, Cu, and Mn ions the magnetic behaviour changed from ferromagnetic to paramagnetic. Results obtained from the photocatalysis indicated that Mn0.75Co0.25Fe2O4 NPs (30.0 mg) were a promising photocatalyst achieving 96.0% removal of MB after 100 min of UV-light exposure in the alkaline solution. Antibacterial results showed that the most effective combination was Zn0.75Co0.25Fe2O4 NPs (20.0 ppm) displaying activity against Staphylococcus aureus, Enterococcus columbae, and Aerococcus viridians by 15.0, 13.0, and 12.0 mm ZOI, respectively. Additionally, Zn0.75Co0.25Fe2O4 NPs were active as antibiofilm factors producing activity by 63.7, 57.9, and 45.5% towards S. aureus, A. viridians, and E. columbae, respectively. Accordingly, Zn0.75Co0.25Fe2O4 and Mn0.75Co0.25Fe2O4 NPs can be utilized in industrial, biological and medical applications.

Characterization of the surface properties of MgO using paper spray mass spectrometry.

RATIONALE: Significant advances have been made in the preparation of different morphologies of magnesium oxide (MgO), but the relationship between MgO morphology and its interactions with therapeutic drugs is rarely studied. Herein, we investigated the interactions between different morphologies of MgO and therapeutic drugs using paper spray mass spectrometry. METHODS: Different morphologies of MgO including trapezoidal, needle-like, flower-like and nest-like structures were prepared through a facile precipitation method. The as-obtained MgO particles were then coated onto the surface of filter paper via vacuum filtration strategy. The coated papers with different morphologies of MgO were used as the substrates for paper spray mass spectrometry to explore the interactions between different MgO and therapeutic drugs. RESULTS: Through investigating the interactions between different morphologies of MgO coated papers and therapeutic drugs, it demonstrated that, in contrast to the trapezoidal, needle-like and nest-like MgO coated papers, different drugs in dried blood spots (DBS) were more favourably eluted off from the paper coated with flower-like MgO due to its weaker surface basicity. Also, the signal intensities of different drugs during paper spray were highly dependent on their elution behaviours. CONCLUSIONS: Paper spray mass spectrometry (MS) provides an avenue to elaborate the surface properties of MgO with different structures. The surface basicity of MgO played a crucial role in determining the elution behaviours of therapeutic drugs in DBS, and a more favourable elution behaviour tended to result in a higher MS signal. Copyright © 2016 John Wiley & Sons, Ltd.

In vitro cytotoxic evaluation of MgO nanoparticles and their effect on the expression of ROS genes.

Water-dispersible MgO nanoparticles were tested to investigate their cytotoxic effects on oxidative stress gene expression. In this in vitro study, genes related to reactive oxygen species (ROS), glutathione S-transferase (GST) and catalase, were quantified using real-time polymerase chain reactions (molecular level) and molecular beacon technologies (cellular level). The monodispersed MgO nanoparticles, 20 nm in size, were used to treat human cancer cell lines (liver cancer epithelial cells) at different concentrations (25, 75 and 150 µg/mL) and incubation times (24, 48 and 72 h). Both the genetic and cellular cytotoxic screening methods produced consistent results, showing that GST and catalase ROS gene expression was maximized at 150 µg/mL nanoparticle treatment with 48 h incubation. However, the genotoxic effect of MgO nanoparticles was not significant compared with control experiments, which indicates its significant potential applications in nanomedicine as a diagnostic and therapeutic tool.

Fe3-xCuxO4 as highly active heterogeneous Fenton-like catalysts toward elemental mercury removal.

A series of novel spinel Fe3-xCuxO4 (0

A comparative study on properties of synthesized MgO with different templates.

Magnesium oxide powders have been prepared by simple method using different templates as Hexamine (T1), alkylate-hexamine salt (T2) and alkylate-dihexamine salt (T3). The annealed products were systematically investigated by using X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM) and UV-Visible absorption. It was found that the formation of nanoparticle could involved the role of performed "nucleus" and used template to control the growth rate of nucleuses. The results were shown that different templates affect on the size and species of particles. In this study, the crystallite size of the MgO products were in a range from 4 to 7 nm. The optical band gap of MgO nanoparticles was in the range 4.27-4.77 eV. The morphology of MgO was nanospheres or nanokongelemere-like. In this investigation photocatalytic degradation of Indigo carmine (IC) in water was studied. The effects of some parameters such as pH, amount of catalyst, initial concentration of dye were examined.

Synthesis, structural and luminescence studies of magnesium oxide nanopowder.

Nanoparticles of magnesium oxide (MgO) have been prepared by low temperature solution combustion and hydrothermal method respectively. Powder X-ray diffraction (PXRD) patterns of MgO samples prepared by both the methods show cubic phase. The Scanning Electron Microscopy (SEM) studies reveal, the combustion derived product show highly porous, foamy and fluffy in nature than hydrothermally derived sample. The optical absorption studies of MgO show surface defects in the range 250-300 nm. The absorption peak at ∼290 nm might be due to F-centre. Photoluminescence (PL) studies were carried upon exciting at 290 nm. The sample prepared via combustion method show broad emission peak centred at ∼395 nm in the bluish-violet (3.14 eV) region. However, in hydrothermal prepared sample show the emission peaks at 395 and 475 nm. These emission peaks were due to surface defects present in the sample since nanoparticles exhibits large surface to volume ratio and quantum confinement effect.

High-pressure combinatorial process integrating hot isostatic pressing.

A high-pressure combinatorial process integrating hot isostatic pressing (HIP) was developed by providing a reaction vessel with a high-pressure tightness based on a commercial flange. The reaction vessel can be used up to 200 MPa and 500 °C under HIP processing condition. Preparation of spinel-type MgAl2O4 from Mg(OH)2, Al(OH)3 and AlOOH was performed using the reaction vessel under 200 MPa and 500 °C as demonstration. The entire powder library was characterized using powder X-ray diffraction patterns, and the single phase of spinel-type MgAl2O4 was obtained from Mg(OH)2+Al(OH)3. These assessments corresponded with previously published data.

Mesoporous carbon stabilized MgO nanoparticles synthesized by pyrolysis of MgCl2 preloaded waste biomass for highly efficient CO2 capture.

Anthropogenic CO2 emission makes significant contribution to global climate change and CO2 capture and storage is a currently a preferred technology to change the trajectory toward irreversible global warming. In this work, we reported a new strategy that the inexhaustible MgCl2 in seawater and the abundantly available biomass waste can be utilized to prepare mesoporous carbon stabilized MgO nanoparticles (mPC-MgO) for CO2 capture. The mPC-MgO showed excellent performance in the CO2 capture process with the maximum capacity of 5.45 mol kg(-1), much higher than many other MgO based CO2 trappers. The CO2 capture capacity of the mPC-MgO material kept almost unchanged in 19-run cyclic reuse, and can be regenerated at low temperature. The mechanism for the CO2 capture by the mPC-MgO was investigated by FTIR and XPS, and the results indicated that the high CO2 capture capacity and the favorable selectivity of the as-prepared materials were mainly attributed to their special structure (i.e., surface area, functional groups, and the MgO NPs). This work would open up a new pathway to slow down global warming as well as resolve the pollution of waste biomass.

Biotemplated hierarchical porous material: the positively charged leaf.

Addressing the problem of pathogenic bacteria in human health remains a great challenge. We have prepared MgO, replicated from the leaf template, for efficient bacterial removal. The synthesis method perfectly inherits the advantage of the hierarchical three-level micro-meso-macroporous structure from the leaf template. The final product has the integrated advantages of a positively charged property, hierarchical three-level micro-meso-macroporous microstructure and sterilization property so that it could be named "the positively charged leaf". The positively charged leaf with the microstructure, which is bestowed by Nature, could be utilized in water purification for dye removal and could be extended to pollutant removal, especially of harmful bacteria. The positively charged leaf, as the leaf shield, could be useful in protecting human health. The concept of this work could be applied to the synthesis of different functional metal oxides with hierarchical porous structures, and the products could be utilized in efficient bacterial removal.

Electrochemical insertion of lithium in mechanochemically synthesized Zn2SnO4.

We studied the electrochemical insertion of Li in mechanochemically prepared Zn(2)SnO(4). The mechanism of the electrochemical reaction was investigated by using X-ray diffraction, nuclear magnetic resonance spectroscopy, and Mössbauer spectroscopy. Changes in the morphology of the Zn(2)SnO(4) particles were studied by in situ scanning electron microscopy. The results were compared with mixtures of SnO(2) + ZnO and with Zn(2)SnO(4) prepared by conventional solid-state synthesis and showed that the mechanochemically prepared Zn(2)SnO(4) exhibits the best cyclic stability of these samples.

Preparation, characterization and application of octadecyl modified magnesium oxide microspheres.

A new solid-phase extraction sorbent, octadecyl modified magnesium oxide (C18-MgO) microspheres, was successfully prepared in the present work. Its composition, morphology and structure were studied by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), N(2) adsorption-desorption technique, and solid-state nuclear magnetic resonance (NMR). The as-synthesized C18-MgO was employed as a solid-phase extraction sorbent for the enrichment of polycyclic aromatic hydrocarbons (PAHs) in aqueous solutions. Several factors affecting the extraction efficiency of PAHs, including the type and concentration of organic modifiers, flow rate, sample volume, and the types of rinsing solvents and eluting solvents, were investigated systematically. The results demonstrated that C18-MgO was superior to MgO in terms of large volume in loading samples. In comparison with MgO and Sep-Pak C18, C18-MgO exhibited excellent extraction efficiency (>91% except for naphthalene) in respect of high recoveries under the optimized conditions. The limits of detection varied from 0.001 to 0.603 ng mL(-1) for 15 PAHs using high-performance liquid chromatography coupled with a fluorescence detector, indicating that the analytical method was highly sensitive. The proposed method was applied to enrich PAHs in tap water and acceptable recoveries (18-96%) were obtained.

Rapid room-temperature synthesis of nanocrystalline spinels as oxygen reduction and evolution electrocatalysts.

Spinels can serve as alternative low-cost bifunctional electrocatalysts for oxygen reduction/evolution reactions (ORR/OER), which are the key barriers in various electrochemical devices such as metal-air batteries, fuel cells and electrolysers. However, conventional ceramic synthesis of crystalline spinels requires an elevated temperature, complicated procedures and prolonged heating time, and the resulting product exhibits limited electrocatalytic performance. It has been challenging to develop energy-saving, facile and rapid synthetic methodologies for highly active spinels. In this Article, we report the synthesis of nanocrystalline M(x)Mn(3-x)O(4) (M = divalent metals) spinels under ambient conditions and their electrocatalytic application. We show rapid and selective formation of tetragonal or cubic M(x)Mn(3-x)O(4) from the reduction of amorphous MnO(2) in aqueous M(2+) solution. The prepared Co(x)Mn(3-x)O(4) nanoparticles manifest considerable catalytic activity towards the ORR/OER as a result of their high surface areas and abundant defects. The newly discovered phase-dependent electrocatalytic ORR/OER characteristics of Co-Mn-O spinels are also interpreted by experiment and first-principle theoretical studies.

Surface-step-terrace-induced anomalous transport properties in highly epitaxial La0.67Ca0.33MnO3 thin films.

La0.67Ca0.33MnO3 thin films were epitaxially grown on miscut MgO(001) substrates by pulsed laser ablation. Electrical transport properties were studied by using an ultra high vacuum, four-probe STM system at different temperatures. Anomalous resistivity behavior and metal-insulator transition temperatures were found, both of which are highly dependent upon the miscut angle (1, 3, and 5°). These phenomena are attributed to the difference in residual strain that results from the difference in terrace widths of the vicinal surfaces.

High yield combustion synthesis of nanomagnesia and its application for fluoride removal.

We describe a novel combustion synthesis for the preparation of Nanomagnesia (NM) and its application in water purification. The synthesis is based on the self-propagated combustion of the magnesium nitrate trapped in cellulose fibers. Various characterization studies confirmed that NM formed is crystalline with high phase purity, and the particle size varied in the range of 3-7nm. The fluoride scavenging potential of this material was tested as a function of pH, contact time and adsorbent dose. The result showed that fluoride adsorption by NM is highly favorable and the capacity does not vary in the pH range usually encountered in groundwater. The effects of various co-existing ions usually found in drinking water, on fluoride removal were also investigated. Phosphate was the greatest competitor for fluoride followed by bicarbonate. The presence of other ions studied did not affect the fluoride adsorption capacity of NM significantly. The adsorption kinetics followed pseudo-second-order equation and the equilibrium data are well predicted by Frendlich equation. Our experimental evidence shows that fluoride removal happened through isomorphic substitution of fluoride in brucite. A batch household defluoridation unit was developed using precipitation-sedimentation-filtration techniques, addressing the problems of high fluoride concentration as well as the problem of alkaline pH of the magnesia treated water. The method of synthesis reported here is advantageous from the perspectives of small size of the nanoparticle, cost-effective recovery of the material and improvement in the fluoride adsorption capacity.

Synthesis of nanocrystalline (Co, Ni)Al2O4 spinel powder by mechanical milling of quasicrystalline materials.

In the present study, attempts have been made to synthesize the nano-crystalline (Co, Ni)Al2O4 spinel powders by ball milling and subsequent annealing. An alloy of Al70Co15Ni15, exhibiting the formation of a complex intermetallic compound known as decagonal quasicrystal is selected as the starting material for mechanical milling. It is interesting to note that this alloy is close to the stoichiometry of aluminum and transition metal atoms required to form the aluminate spinel. The milling was carried out in an attritor mill at 400 rpm for 40 hours with ball to powder ratio of 20 : 1 in hexane medium. Subsequent to this annealing was performed in an air ambience for 10, 20, and 40 h at 600 degrees C in side the furnace in order to oxidize the decagonal phase and finally to form the spinel structure. The X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the formation of nano-sized decagonal phase after milling and then (Co, Ni)Al2O4 spinel type phase after annealing. The XRD studies reveal the lattice parameter to be 8.075 angstroms and the lattice strain as 0.6%. The XRD and TEM explorations of spinel phase indicate the average grain size to be approximately 40 nm.