Magnetic resonance imaging of glioma with novel APTS-coated superparamagnetic iron oxide nanoparticles

We report in vitro and in vivo magnetic resonance (MR) imaging of C6 glioma cells with a novel acetylated 3-aminopropyltrimethoxysilane (APTS)-coated iron oxide nanoparticles (Fe₃O₄ NPs). In the present study, APTS-coated Fe₃O₄ NPs were formed via a one-step hydrothermal approach and then chemically modified with acetic anhydride to generate surface charge-neutralized NPs. Prussian blue staining and transmission electron microscopy (TEM) data showed that acetylated APTS-coated Fe₃O₄ NPs can be taken up by cells. Combined morphological observation, cell viability, and flow cytometric analysis of the cell cycle indicated that the acetylated APTS-coated Fe₃O₄ NPs did not significantly affect cell morphology, viability, or cell cycle, indicating their good biocompatibility. Finally, the acetylated APTS-coated Fe₃O₄ nanoparticles were used in magnetic resonance imaging of C6 glioma. Our results showed that the developed acetylated APTS-coated Fe₃O₄ NPs can be used as an effective labeling agent to detect C6 glioma cells in vitro and in vivo for MR imaging. The results from the present study indicate that the developed acetylated APTS-coated Fe₃O₄ NPs have a potential application in MR imaging.     

Surface enhanced fluorescence of anti-tumoral drug emodin adsorbed on silver nanoparticles and loaded on porous silicon

Fluorescence spectra of anti-tumoral drug emodin loaded on nanostructured porous silicon have been recorded. The use of colloidal nanoparticles allowed embedding of the drug without previous porous silicon functionalization and leads to the observation of an enhancement of fluorescence of the drug. Mean pore size of porous silicon matrices was 60 nm, while silver nanoparticles mean diameter was 50 nm. Atmospheric and vacuum conditions at room temperature were used to infiltrate emodin-silver nanoparticles complexes into porous silicon matrices. The drug was loaded after adsorption on metal surface, alone, and bound to bovine serum albumin. Methanol and water were used as solvents. Spectra with 1 μm spatial resolution of cross-section of porous silicon layers were recorded to observe the penetration of the drug. A maximum fluorescence enhancement factor of 24 was obtained when protein was loaded bound to albumin, and atmospheric conditions of inclusion were used. A better penetration was obtained using methanol as solvent when comparing with water. Complexes of emodin remain loaded for 30 days after preparation without an apparent degradation of the drug, although a decrease in the enhancement factor is observed. The study reported here constitutes the basis for designing a new drug delivery system with future applications in medicine and pharmacy.     

Formation and characterization of iron oxide nanoparticles loaded on self-organized TiO2 nanotubes

The iron oxide nanoparticles were loaded onto self-organized TiO₂ nanotube layers grown by anodization of Ti in fluoride containing electrolytes. The nanoparticles were obtained by electrodepositing method in glycerol/water/FeCl₃·6H₂O electrolytes at room temperature. The X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) measurements showed that the nanoparticles consisted of iron nanocrystalline (Fe) and magnetite (Fe₃O₄). The hematite (α-Fe₂O₃) structure was obtained by annealing in air at 450 °C. The growth mechanism of the nanoparticles and their morphology were also described. Furthermore, the nanoparticles exhibited good ferromagnetic properties at room temperature.     

Magnetic properties and hyperfine interactions of Co1-2xNixMnxFe2O4 nanoparticles

Co1-2xNixMnxFe2O4 (0.0≤x≤0.5) nanoparticles (NPs) were prepared via citrate assisted microwave combustion route. XRD analysis confirmed the cubic structure (spinel) of all samples. Average crystallite size of products (obtained from (311) diffraction line) was in the range of 32.9–43.4 nm. The intense peak appearing at around 531 cm⁻¹ in FT-IR was attributed to the formation of a spinel ferrite. Magnetic properties of the products were investigated by room temperature vibrating sample magnetometer and Mössbauer spectroscopy. The magnetic parameters have been found to strongly depend on the Ni and Mn concentrations. The saturation magnetization continuously decreases with the increasing of the concentration (x). We found that Ni_0.5Mn_0.5Fe₂O₄ NP has superparamagnetic character at room temperature. This result was also verified by Mössbauer analysis. Scanning electron microscopic analysis revealed the cubic morphology of all products, EDX and elemental mapping analyses confirmed the expected composition of each product.     

Green facile synthesis of low-toxic superparamagnetic iron oxide nanoparticles (SPIONs) and their cytotoxicity effects toward Neuro2A and HUVEC cell lines

Superparamagnetic iron oxide (Fe₃O₄) nanoparticles (SPIONs) were synthesized by co-precipitation using polyvinyl alcohol (PVA) as a capping agent under alkaline condition. The produced X-ray diffraction (XRD) pattern evidenced the presence of peaks corresponding to the inverse spinel structure of the prepared SPIONs. Debye-Scherrer and field emission scanning microscopy (FESEM) showed the prepared SPIONs to be well-defined with about <?50?nm size. Likewise, the superparamagnetic properties of the SPIONs measured by Vibrating Sample Magnetometer (VSM) showed high saturation magnetization (~ 65.36?emu/g). The in vitro cytotoxicity studies on Neuro2A and HUVEC cells have mentioned low toxic and non-toxic SPIONs, respectively in a range of concentrations (1.17–150?μg/ml), thus, we reckon that the synthesized SPIONs will have persistent utilization in different fields of medical applications.     

Electric relaxation of superparamagnetic Gd-doped lead molybdato-tungstates

Tetragonal, scheelite-type Pb_1–3x□_xGd_2x(MoO₄)_1–3x(WO₄)_3x materials (x?=?0.0455, 0.0839, 0.1154, 0.1430, 0.1667 and 0.1774, where □ denotes vacancies) synthesized via solid state reaction route were magnetically and electrically examined. The ac and dc magnetic measurements as well as the Brillouin fitting procedure showed paramagnetic state with characteristic superparamagnetic-like behaviour and a spin-only contribution to the paramagnetic moment. Broadband dielectric spectroscopy studies exhibited existence in the loss spectra the faster and slower relaxation processes with various time scales for the gadolinium-poorer samples with the x vacancy parameter up to 0.1154. For samples with higher Gd content, i.e. when x?>?0.1154, no signs of any relaxation processes was observed. This phenomenon has been explained by a smaller number of structural and spin defects as opposed to the samples poorer in gadolinium ions.     

Iron oxide-based superparamagnetic polymeric nanomaterials: Design, preparation, and biomedical application

Recent advances in the development and biological applications of polymeric nanomaterials embedded with superparamagnetic iron oxide nanoparticles (SIONPs) are summarized. Novel SIONP-polymer hybrid nanoparticles are prepared by various methods, including direct modification with polymers, surface-initiated controlled polymerization, inorganic silica/polymer hybridization, self-assembly, self-association, and various heterogeneous polymerization methods. They have potential for various biomedical applications, including magnetic resonance imaging (MRI) contrast enhancement, targeted drug delivery, hyperthermia, biological separation, protein immobilization, and biosensors.     

Synthesis and characterization of Sr2+ and Gd3+ doped magnetite nanoparticles for magnetic hyperthermia and drug delivery application

Commendable efforts have been gingered towards the fight against cancer. Nevertheless, it remains a major public health concern due to its predominant cause of death globally. Given this, we synthesized two different nanoparticles, Sr²⁺ and Gd³⁺ doped magnetite for magnetic hyperthermia and drug delivery application. Based on the characterization, the diffractogram shows that only one phase related to magnetite with a crystallite size of 10 nm was formed. TEM images revealed nanoparticles of spherical shapes of approximately 12 nm. There is no difference in magnetic saturation of the as-received synthesized samples (Fe₃O₄@Sr and Fe₃O₄@Gd), while the BET-specific surface area of Fe₃O₄@Gd is 8 m² g⁻¹ higher than Fe₃O₄@Sr. The heat generation in alternating magnetic field (the magnetic hyperthermia) of Fe₃O₄@Sr functionalized with citric acid and loaded with 5- fluorouracil (Fe₃O₄@Sr@CA@5-flu) is slower than Fe₃O₄@Gd@CA@5-flu. The specific absorption rate (SAR) of Fe₃O₄@Gd@CA@5-flu, 112.0 ± 10.4 W g⁻¹ was found to be higher than that of Fe₃O₄@Sr@CA@5-flu. The thermogram shows that 11% of the drug was successfully loaded on Fe₃O₄@Gd@CA@5-flu. The release of the antitumor drug by the synthesized nanoparticle drug carriers for ovarian cancer (SKOV-3 cells) therapy showed that more than 50% of the cancer cell’s viability was reduced after 72 h of incubation. The synthesized nanoparticles demonstrated a promising drug carrier for the treatment of SKOV-3 cells.     

Nitric oxide-releasing porous silicon nanoparticles

In this study, the ability of porous silicon nanoparticles (PSi NPs) to entrap and deliver nitric oxide (NO) as an effective antibacterial agent is tested against different Gram-positive and Gram-negative bacteria. NO was entrapped inside PSi NPs functionalized by means of the thermal hydrocarbonization (THC) process. Subsequent reduction of nitrite in the presence of d-glucose led to the production of large NO payloads without reducing the biocompatibility of the PSi NPs with mammalian cells. The resulting PSi NPs demonstrated sustained release of NO and showed remarkable antibacterial efficiency and anti-biofilm-forming properties. These results will set the stage to develop antimicrobial nanoparticle formulations for applications in chronic wound treatment.     

Anti-CEA-functionalized superparamagnetic iron oxide nanoparticles for examining colorectal tumors in vivo

Although the biomarker carcinoembryonic antigen (CEA) is expressed in colorectal tumors, the utility of an anti-CEA-functionalized image medium is powerful for in vivo positioning of colorectal tumors. With a risk of superparamagnetic iron oxide nanoparticles (SPIONPs) that is lower for animals than other material carriers, anti-CEA-functionalized SPIONPs were synthesized in this study for labeling colorectal tumors by conducting different preoperatively and intraoperatively in vivo examinations. In magnetic resonance imaging (MRI), the image variation of colorectal tumors reached the maximum at approximately 24 h. However, because MRI requires a nonmetal environment, it was limited to preoperative imaging. With the potentiality of in vivo screening and intraoperative positioning during surgery, the scanning superconducting-quantum-interference-device biosusceptometry (SSB) was adopted, showing the favorable agreement of time-varied intensity with MRI. Furthermore, biological methodologies of different tissue staining methods and inductively coupled plasma (ICP) yielded consistent results, proving that the obtained in vivo results occurred because of targeted anti-CEA SPIONPs. This indicates that developed anti-CEA SPIONPs owe the utilities as an image medium of these in vivo methodologies.     

Growth of silicon carbide nanotubes in arc plasma treated silicon carbide grains and their microstructural characterizations

Silicon carbide nanotubes were found to grow in straight as well as curved configurations by treating silicon carbide grains in an arc plasma reactor/furnace followed by 3 h of cooling (in air). By increasing the plasma treatment time from 16 min to 20 min, multi-wall tubes were found to change to single wall tubes with reduction in diameter from few nm to sub-nm. Typical in situ grown nanotubes were characterized by XRD, TEM, SAED, HRTEM, EDS and micro Raman spectroscopy, and it is established from these evaluations that the nanotubes are made up of silicon carbide and not carbon. A possible mechanism, involving reaction between the plasma dissociated carbon (solid) forming carbon nanotube and the left-out silicon (existing in vapour state) during the cooling period (3000–2680 °C), is suggested to be responsible for silicon carbide nanotube formation in the plasma assisted process.     

The cytotoxicity evaluation of magnetic iron oxide nanoparticles on human aortic endothelial cells

One major obstacle for successful application of nanoparticles in medicine is its potential nanotoxicity on the environment and human health. In this study, we evaluated the cytotoxicity effect of dimercaptosuccinic acid-coated iron oxide (DMSA-Fe₂O₃) using cultured human aortic endothelial cells (HAECs). Our results showed that DMSA-Fe₂O₃ in the culture medium could be absorbed into HAECs, and dispersed in the cytoplasm. The cytotoxicity effect of DMSA-Fe₂O₃ on HAECs was dose-dependent, and the concentrations no more than 0.02 mg/ml had little toxic effect which were revealed by tetrazolium dye assay. Meanwhile, the cell injury biomarker, lactate dehydrogenase, was not significantly higher than that from control cells (without DMSA-Fe₂O₃). However, the endocrine function for endothelin-1 and prostacyclin I-2, as well as the urea transporter function, was altered even without obvious evidence of cell injury in this context. We also showed by real-time PCR analysis that DMSA-Fe₂O₃ exposure resulted in differential effects on the expressions of pro- and anti-apoptosis genes of HAECs. Meanwhile, it was noted that DMSA-Fe₂O₃ exposure could activate the expression of genes related to oxidative stress and adhesion molecules, which suggested that inflammatory response might be evoked. Moreover, we demonstrated by in vitro endothelial tube formation that even a small amount of DMSA-Fe₂O₃ (0.01 and 0.02 mg/ml) could inhibit angiogenesis by the HAECs. Altogether, these results indicate that DMSA-Fe₂O₃ have some cytotoxicity that may cause side effects on normal endothelial cells.     

The Effect of Iron Oxide Magnetic Nanoparticles on Smooth Muscle Cells

Recently, magnetic nanoparticles of iron oxide (Fe₃O₄, γ-Fe₂O₃) have shown an increasing number of applications in the field of biomedicine, but some questions have been raised about the potential impact of these nanoparticles on the environment and human health. In this work, the three types of magnetic nanoparticles (DMSA-Fe₂O₃, APTS-Fe₂O₃, and GLU-Fe₂O₃) with the same crystal structure, magnetic properties, and size distribution was designed, prepared, and characterized by transmission electronic microscopy, powder X-ray diffraction, zeta potential analyzer, vibrating sample magnetometer, and Fourier transform Infrared spectroscopy. Then, we have investigated the effect of the three types of magnetic nanoparticles (DMSA-Fe₂O₃, APTS-Fe₂O₃, and GLU-Fe₂O₃) on smooth muscle cells (SMCs). Cellular uptake of nanoparticles by SMC displays the dose, the incubation time and surface property dependent patterns. Through the thin section TEM images, we observe that DMSA-Fe₂O₃ is incorporated into the lysosome of SMCs. The magnetic nanoparticles have no inflammation impact, but decrease the viability of SMCs. The other questions about metabolism and other impacts will be the next subject of further studies. Song Zhang and Xiangjian Chen contributed equally to this work.     

Effect of carbon nanotubes decorated with silver nanoparticles as hybrid filler on properties of natural rubber nanocomposites

Decoration of carbon nanotube (CNT) surfaces with silver nanoparticles (AgNPs) was performed using N,N-dimethylformamide reducing agent. The CNT-decorated with AgNP (CNT-AgNP) was then used to prepare natural rubber (NR) nanocomposites via latex mixing method. Cure characteristics, mechano-thermal relaxation, electrical conductivity, and thermal properties of the composites were investigated. It was found that the CNT-AgNP gave cure properties improved over plain NR compounds in terms of scorch time, degree of vulcanization, and activation energy. In addition, temperature scanning stress relaxation measurement revealed stronger network formation after incorporation of AgNP into the NR matrix due to the interaction among CNT and AgNP particles. This also provided high conductivity and low percolation threshold concentration for the CNT-AgNP filled NR, relative to plain CNT filled NR composites. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47281.     

Broadband antireflective silicon nanostructures produced by spin-coated Ag nanoparticles

We report the fabrication of broadband antireflective silicon (Si) nanostructures fabricated using spin-coated silver (Ag) nanoparticles as an etch mask followed by inductively coupled plasma (ICP) etching process. This fabrication technique is a simple, fast, cost-effective, and high-throughput method, making it highly suitable for mass production. Prior to the fabrication of Si nanostructures, theoretical investigations were carried out using a rigorous coupled-wave analysis method in order to determine the effects of variations in the geometrical features of Si nanostructures to obtain antireflection over a broad wavelength range. The Ag ink ratio and ICP etching conditions, which can affect the distribution, distance between the adjacent nanostructures, and height of the resulting Si nanostructures, were carefully adjusted to determine the optimal experimental conditions for obtaining desirable Si nanostructures for practical applications. The Si nanostructures fabricated using the optimal experimental conditions showed a very low average reflectance of 8.3%, which is much lower than that of bulk Si (36.8%), as well as a very low reflectance for a wide range of incident angles and different polarizations over a broad wavelength range of 300 to 1,100 nm. These results indicate that the fabrication technique is highly beneficial to produce antireflective structures for Si-based device applications requiring low light reflection.     

Enhanced photoluminescence of porous silicon nanoparticles coated by bioresorbable polymers

A significant enhancement of the photoluminescence (PL) efficiency is observed for aqueous suspensions of porous silicon nanoparticles (PSiNPs) coated by bioresorbable polymers, i.e., polylactic-co-glycolic acid (PLGA) and polyvinyl alcohol (PVA). PSiNPs with average size about 100 nm prepared by mechanical grinding of electrochemically etched porous silicon were dispersed in water to prepare the stable suspension. The inner hydrophobic PLGA layer prevents the PSiNPs from the dissolution in water, while the outer PVA layer makes the PSiNPs hydrophilic. The PL quantum yield of PLGA/PVA-coated PSiNPs was found to increase by three times for 2 weeks of the storage in water. The observed effect is explained by taking into account both suppression of the dissolution of PSiNPs in water and a process of the passivation of nonradiative defects in PSiNPs. The obtained results are interesting in view of the potential applications of PSiNPs in bioimaging.     

Decorated carbon nanotubes by silicon deposition in fluidized bed for Li-ion battery anodes

Multi-walled carbon nanotubes Graphistrength^® were decorated with silicon by Fluidized Bed Chemical Vapor Deposition. The ability to fluidize of these nanotubes forming ball-shaped jumbles of several hundreds of microns in diameter and that of the final CNT-Si balls was first studied. These balls reveal to fluidize with characteristics of Geldart's group A particles, i.e. without bubbles and with high bed expansion. Coating experiments from silane SiH₄ were performed at 500 °C in the 30–60 wt.% range of silicon deposited. SEM and TEM imaging reveals that the nanotubes are coated by silicon nanoparticles uniformly distributed from the periphery to the center of the balls for the whole conditions tested. On-line acquisition of key process parameters evolution shows that the material remains fluidizable, even for large proportions of silicon deposited. The Sauter diameter and the tapped, untapped and skeleton densities of balls increase with the percentage of silicon deposited, whereas their specific surface area decreases due to the progressive filling of the pores by the deposit. This composite material is a promising candidate as anode to replace graphite in lithium-ion batteries.     

Luminescence nanothermometry with alkyl-capped silicon nanoparticles dispersed in nonpolar liquids

Silicon nanoparticles (Si NPs) with a diameter size ranging from 4 to 8 nm were successfully fabricated. They exhibit a visible photoluminescence (PL) due to the quantum confinement effect. Chemical functionalization of these Si NPs with alkyl groups allowed to homogeneously disperse them in nonpolar liquids (NPLs). In comparison to most of literature results for Si NPs, an important PL peak position variation with temperature (almost 1 meV/K) was obtained from 303 to 390 K. The influence of the liquid viscosity on the peak positions is also presented. These variations are discussed considering energy transfer between nanoparticles. The high PL thermal sensitivity of the alkyl-capped Si NPs paves the way for their future application as nanothermometers.     

Magnetic separation of Fe catalyst from single-walled carbon nanotubes in an aqueous surfactant solution

We report an efficient technique to separate ferromagnetic catalyst particles from an aqueous surfactant solution of single-walled carbon nanotubes (SWNTs) by the use of a 1.3 T permanent magnet. High resolution transmission electron microscopy (HRTEM) demonstrates that SWNTs are coated with a surfactant layer that stabilises the aqueous dispersions of SWNTs. The residual quantities of Fe catalyst (∼3%) can be effectively removed from a colloid solution of SWNTs in a magnetic field while absorbance spectra of the initial and purified solutions show that the nanotube diameter distribution remains unchanged.     

Effects of irradiation energy and nanoparticle concentrations on the structure and morphology of laser sintered magnesia with alumina and iron oxide nanoparticles

The laser sintering mechanism of composites based on magnesia and oxide nanoparticles was studied in terms of nanoparticle concentration and laser energy fluence. Iron oxide and aluminum oxide nanoparticles were mechanically mixed with magnesia (MgO) powder (5, 7 and 10 wt%) and the compacted pellets were irradiated with the fundamental output (1064 nm) of a pulsed Nd:YAG laser at 2.5 and 3.0 J/cm². Crystal structure, elemental composition and morphology were characterized by X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy. X-ray diffraction results confirmed the crystalline phases and spinel formation by addition of oxide nanoparticles and laser sintering. X-ray photoelectron spectroscopy analysis confirmed their surface composition and chemical states of the corresponding elements. Morphological changes were observed due to the laser fluence and the oxide nanoparticle concentrations. Results show that a coarsening mechanism was predominant with a high energy fluence and concentration of oxide nanoparticles.