Preparation,Characterization and Optimization of Egg Albumin Nanoparticles as Low Molecular‐Weight Drug Delivery Vehicle

Protein nanoparticles have been recognized as carriers to deliver low molecular‐weight drugs, anticancer drug, DNA, vaccines, oligonucleotides, peptides and etc. The purpose of this research was preparation of Egg Albumin (EA) nanoparticle with suitable size/size distribution and good surface properties for drug delivery application based on simple coacervation method along with optimization of the nanoparticles by employing Taguchi method. Several synthesis parameters were examined to characterize their impacts on nanoparticle size and topography. These variables were including temperature, EA concentration, desolvating agent volume, pH value and agitation speed. In addition, size and morphology of prepared nanoparticles were analyzed by photon correlation spectroscopy (PCS) as well as atomic force microscopy (AFM). As result of Taguchi analysis in this research, desolvating agent volume and pH were most influencing factors on particle size. The minimum size of nanoparticles (～51 nm) were obtained at Temperature 55 °C, 30 mg/ml EA concentration, desolvating agent volume 50 ml, agitation speed of 500 rpm and pH 4. The mechanistic of optimum conditions for preparing protein nanoparticles from Egg Albumin for the first time and their characterization as delivering nano system are discussed.     

Particle size effect on phase and magnetic properties of polymer-coated magnetic nanoparticles

Polymer-coated magnetic nanoparticles are hi-tech materials with ample applications in the field of biomedicine for the treatment of cancer and targeted drug delivery. In this study, magnetic nanoparticles were synthesized by chemical reduction of FeCl₂ solution with sodium borohydride and coated with amine-terminated polyethylene glycol (aPEG). By varying the concentration of the reactants, the particle size and the crystallinity of the particles were varied. The particle size was found to increase from 6 to 20 nm and the structure becomes amorphous-like with increase in the molar concentration of the reactant. The magnetization at 1 T field (M_1T) for all samples is > 45 emu/g while the coercivity is in the range of 100-350 Oe. When the ethanol-suspended particles are subjected to an alternating magnetic field of 4 Oe at 500 kHz, the temperature is increased to a maximum normalized temperature (3.8 °C/mg) with decreasing particle size.     

Optimization and characterization of ultrasound assisted preparation of curcumin-loaded solid lipid nanoparticles: Application of central composite design,thermal analysis and X-ray diffraction techniques

This study is devoted to preparation of novel solid lipid nanoparticles (SLNs) for the encapsulation of curcumin which is produced by micro-emulsion and ultrasonication using stearic acid and tripalmitin as solid lipids, tween80 and span80 as surfactants. The relation between particle size and entrapment efficiency of the produced SLNs was operated by central composite design (CCD) under response likes surface method (RSM). The variables including the ratio of lipids (X₁), the ratio of surfactants (X₂), drug/lipid ratio (X₃), time of sonication (X₄) and time of homogenization (X₅). Particle size and entrapment efficiency of the loaded curcumin was justified according to the minimum particle size and maximum entrapment efficiency. The curcumin loaded SLNs presented fairly spherical shape with the mean diameter and entrapment efficiency of 112.0 ± 2.6 nm and 98.7 ± 0.3%, respectively. The optimized SLNs were characterized by X-ray diffraction analysis (XRD), differential scanning calorimetry (DSC), photon correlation spectroscopy (PCS) and field emission scanning electron microscopy (FESEM). The drug release profile of the optimal formulated material was examined in aqueous media and almost 30% of the curcumin loaded in SLNs was gradually released during 48 h, which reveals efficient prolonged release of the drug.     

Clustering of magnetic nanoparticles using a double hydrophilic block copolymer, poly(ethylene oxide)-b-poly(acrylic acid)

The use of a double hydrophilic block copolymer (DHBC), poly(ethylene oxide)-block-poly(acrylic acid) (PEO-b-PAA) to prepare magnetic nanoparticle (MNP) clusters was investigated. In this one-pot synthesis method, the DHBC controlled the particle growth and served as both stabilizer and clustering agent. Depending on the iron-to-polymer ratio, the synthesized particles can be in the form of colonies of small iron oxide particles or clusters of these particles with size larger than 100 nm. Compared to the previous reported result using random copolymers, the clusters prepared with DHBC were more compact and homogeneous. The yield of clusters increased when the amount of polymer added was limiting. Insufficient amounts of polymer resulted in the formation of bare patches on the magnetite surface, and the strong van der Waals attraction induced cluster formation.     

Details of crystalline growth in co-deposited electroplated nickel films with hard (nano)particles

Electroplated nickel dispersion films with incorporated hard particles, primarily titanium oxide, were studied. A sufficient dispersion of nanometre-scaled particles in Watts solution was reached by application of ultrasonic energy to the galvanic bath. Crystal morphology, mean grain size and formation of textures were examined by electron backscattering diffraction (EBSD), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The typical columnar structure of pure Ni films was refined by means of ultrasound. Incorporation of micron-sized TiO₂ particles generates additional nucleation surfaces in contrast to SiC particles. Textures of the subsequent columnar nickel crystals change from 〈2 1 1〉 (silent condition) or 〈1 1 0〉 (ultrasonic condition) fibre textures in growth direction to 〈1 0 0〉 and 〈1 1 1〉 textures under the influence of nanoparticle incorporation. Moreover, nanoparticles remarkably decrease the grain size and grain aspect ratio. Their incorporation takes place inside the crystals as well as between grains.     

Modifier effects on chemical reduction synthesis of nanostructured copper

Size-controlled chemical reduction synthesis of nanostructured Cu was studied in the presence of a single modifier such as polyethylene glycols, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate or a mixture of two different types of modifiers. The Cu nanoparticles were characterized by powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction and Fourier transform infrared spectroscopy. The average particle size and particle size distribution of the nanostructured Cu depend upon the type of modifiers and the modifier effect follows the order: PEG-2000 > SDBS > PEG-600 > SDS > PEG-6000. The experimental results indicate that due to the existence of a synergistic action, a mixture of two types of modifiers has a significant effect on the particle size and the size distribution of Cu nanoparticles.     

Folate-decorated chitosan/doxorubicin poly(butyl)cyanoacrylate nanoparticles for tumor-targeted drug delivery

A novel chitosan coated poly(butyl cyanoacrylate) (PBCA) nanoparticles loaded doxorubicin (DOX) were synthesized and then conjugated with folic acid to produce a folate-targeted drug carrier for tumor-specific drug delivery. Prepared nanoparticles were surface modified by folate for targeting cancer cells, which is confirmed by FTIR spectroscopy and characterized for shape, size, and zeta potential measurements. The size and zeta potential of prepared DOX-PBCA nanoparticles (DOX-PBCA NPs) were almost 174 ± 8.23 nm and +23.14 ± 4.25 mV, respectively with 46.8 ± 3.32% encapsulation capacity. The transmission electron microscopy study revealed that preparation allowed the formation of spherical nanometric and homogeneous. Fluorescent microscopy imaging and flow cytometry analysis revealed that DOX-PBCA NPs were endocytosed into MCF-7 cells through the interaction with overexpressed folate receptors on the surface of the cancer cells. The results demonstrate that folate-conjugated DOX-PBCA NPs drug delivery system could provide increased therapeutic benefit by delivering the encapsulated drug to the folate receptor positive cancer cells.     

Challenge of ultra high frequency limit of permeability for magnetic nanoparticle assembly with organic polymer—Application of superparamagnetism

Permeability and its upper limitation frequency of superparamagnetic nanoparticle type magneto-dielectric hybrid material were theoretically and experimentally investigated. The Landau-Lifschitz-Gilbert equation without any interaction between nanoparticles revealed that the blocking resonance frequency was able to exceed the ferromagnetic resonance frequency originating from the intrinsic magnetocrystalline anisotropy field by decreasing particle size, resulting in ultra fast switching of superparamagnetic moment in GHz range. In the case of Fe nanoparticles, the blocking resonance frequency can be increased to 130 GHz by reducing particle size to 1 nm. The experiment results for Fe₃O₄ and Fe nanoparticle assemblies supported the validity of our calculation results. Thus, superparamagnetic nanoparticle assembly could be promising material for high frequency use over 10 GHz range.     

In vitro study of magnetic nanoparticles as the implant for implant assisted magnetic drug targeting

Magnetic nanoparticle (MNP) seeds were studied in vitro for use as an implant in implant assisted-magnetic drug targeting (IA-MDT). The magnetite seeds were captured in a porous polymer, mimicking capillary tissue, with an external magnetic field (70 mT) and then used subsequently to capture magnetic drug carrier particles (MDCPs) (0.87 μm diameter) with the same magnetic field. The effects of the MNP seed diameter (10, 50 and 100 nm), MNP seed concentration (0.25-2.0 mg/mL), and fluid velocity (0.03-0.15 cm/s) on the capture efficiency (CE) of both the MNP seeds and the MDCPs were studied. The CE of the 10 nm MNP seeds was never more than 30%, while those of the 50 and 100 nm MNP seeds was always greater than 80% and in many cases exceeded 90%. Only the MNP seed concentration affected its CE. The 10 nm MNP seeds did not increase the MDCP CE over that obtained in the absence of the MNP seeds, while the 50 and 100 nm MNP seeds increased significantly, typically by more than a factor of two. The 50 and 100 nm MNP seeds also exhibited similar abilities to capture the MDCPs, with the MDCP CE always increasing with decreasing fluid velocity and generally increasing with increasing MNP seed concentration. The MNP seed size, magnetic properties, and capacity to self-agglomerate and form clusters were key properties that make them a viable implant in IA-MDT.     

Enhanced photoluminescence of ZnO-SiO2 nanocomposite particles and the analyses of structure and composition

Stable blue-green photoluminescent ZnO-SiO₂ nanocomposite particles exhibiting quantum efficiency as high as 34.8% under excitation at 360 nm were prepared using a spray-drying process from a feed solution that contained both luminescent ZnO nanoparticles synthesized by a sol-gel method and commercially-available SiO₂ nanoparticles. The effects of silica nanoparticle size and SiO₂-to-ZnO concentration ratio on the PL properties of the composite particles were investigated. The internal structure and chemical composition were investigated in detail using elemental mapping, which revealed that ZnO nanoparticles were well-dispersed within silica nanoparticle matrix. At a LiOH concentration of 0.23 M, the predicted ZnO crystallite diameter before and after spray drying was approximately constant at 3.3 and 3.6 nm, respectively. This result indicates that ZnO particle growth was inhibited and therefore the PL property of ZnO nanoparticles was stably preserved in the composite.     

Reactively sputtered Ni, Ni(N) and Ni3N films: Structural, electrical and magnetic properties

Nickel thin films were deposited on glass substrates at different N₂ gas contents using a dc triode sputtering deposition system. Triode configuration was used to deposit nanostructured thin films with preferred orientation at lower gas pressure and at lower substrate temperature compared to the dc diode sputtering system. A gradual evolution in the composition of the films from Ni, Ni(N), to Ni₃N was found by X-ray diffraction analysis. The preferred growth orientation of the nanostructured Ni films changed from (1 1 1) to (1 0 0) for 9% N₂ at 100 °C. Ni₃N films were formed at 23% N₂ with a particle size of about 65 nm, while for 0% and 9% of nitrogen, the particles sizes were 60 nm, and 37 nm, respectively, as obtained by atomic force microscopy. Magnetic force microscopy imaging showed that the local magnetic structure changed from disordered stripe domains of about 200 nm for Ni and Ni(N) to a structure without a magnetic contrast, indicating the paramagnetic state of this material, which confirmed the structural transformation from Ni to Ni₃N.     

Surface-modified zeolite-filled chitosan membranes for pervaporation dehydration of ethanol

Surface-modified zeolite-filled chitosan (CS) membranes were prepared by incorporating 3-mercaptopropyltrimethoxysilane (MPTMS)-modified H-ZSM-5 zeolite into chitosan for pervaporation dehydration of aqueous ethanol solution. The physicochemical characterization by XPS, FT-IR, XRD, DMA and SEM showed that -SO₃H group was readily grafted on the surface of H-ZSM-5 with the mediation of MPTMS and hydrogen peroxide, and the accompanying ion-ion interaction between -SO₃H group on surface-modified H-ZSM-5 and -NH₃⁺ group on chitosan substantially eliminated the nonselective voids at the chitosan-H-ZSM-5 interface of the filled membranes. The experimental results also revealed that H-ZSM-5 exhibited desirable size-selective and preferential adsorption effects for aqueous ethanol solution. As a result, modified H-ZSM-5 filled membranes showed higher swelling degree and permeation flux, and improved selectivity for aqueous ethanol solution. In comparison between chitosan control membrane (permeation flux 54.18 g/(m² h) and separation factor 158.02 for 90 wt.% aqueous ethanol solution at 80 °C), the modified H-ZSM-5 filled membrane with 8 wt.% filling content exhibited a remarkably improved pervaporation performance with permeation flux 278.54 g/(m² h) and separation factor 274.46 under the identical experimental condition.     

Nanoparticle composites: FePt with wide-band-gap semiconductor

We present a simple way to synthesize FePt and ZnO (wide-band-gap semiconductor) nanoparticle composites. The FePt nanoparticles were fabricated using the method reported by Sun et al. By controlling the heating rate, 3 nm FePt nanoparticles were synthesized. Well-dispersed FePt and ZnO nanoparticle composites were prepared by further adding zinc acetate and oleyl amine into the 3 nm FePt nanoparticle dispersion. By controlling the molar ratio of the FePt and zinc acetate, FePt and ZnO nanoparticle composites with different FePt particle fractions were obtained. The intensity of photo luminescence spectra of the nanoparticle composites increases very much with decreasing FePt particle fraction, whereas the peak position shifts a little. After annealing at 550 °C for half an hour, the nanoparticle composites become magnetically hard or semi-hard with coercivity much dependent on the FePt particle volume fraction. The coercivity of the composites increases with annealing temperature. The composites hold the promise of applications in new generation recording and/or optical devices.     

Surface-enhanced Raman scattering effect of gold nanoparticle arrays: The influence of annealing temperature,excitation power and array thickness

Gold nanoparticle arrays are fabricated for surface-enhanced Raman scattering (SERS) and the effect of the annealing temperature, the thickness of nanoparticle array and the exciting power on the SERS signals are investigated. The particle distribution and particle size are dense and uniform on the glass substrate when the 10 nm gold film was annealed at 250 °C and strong SERS signals for Rhodamine 6G were achieved via a 532 nm excitation with a 10 mW power. The SERS signal at 1650 cm⁻¹ is enhanced more than 10 times as compared to that of the gold film without annealing. The strong SERS behavior of gold nanoparticle arrays may broaden the SERS applications in biomedical and analytical chemistry.     

The effect of target size on α-Fe nanoparticle preparation by?pulsed laser ablation

Two methods of preparing Fe nanoparticles at atmospheric pressure were conducted using pulsed laser ablation of a 0.5-mm-diameter Fe wire and a bulk Fe target. Passivated α-Fe nanoparticles covered with a shell of γ-Fe₂O₃ were prepared at different process parameters. The influences of average laser power, repetition rate, pulse duration and carrier-gas pressure on the mean particle size for two laser ablation methods were investigated, respectively. The results show that the target size has a large effect on the nanoparticle preparation though we have the same range of laser process parameters. Except the carrier-gas pressure, the influence of the laser parameters on the mean particle size is almost opposite for the two laser ablation methods. Besides, the ablation mechanisms were discussed to understand the variation of mean particle sizes with target size.     

Growth of Ni-Al alloys on Ni(1 1 1), from Al deposits of various thicknesses: (II) Formation of NiAl over a Ni3Al interfacial layer

This paper describes the second part of a study devoted to the growth of thin Ni-Al alloys after deposition of Al on Ni(1 1 1). In the previous paper [S. Le Pévédic, D. Schmaus, C. Cohen, Surf. Sci. 600 (2006) 565] we have described the results obtained for ultra-thin Al deposits, leading, after annealing at 750 K, to an epitaxial layer of Ni₃Al(1 1 1). In the present paper we show that this regime is only observed for Al deposits smaller than 8 × 10¹⁵ Al/cm² and we describe the results obtained for Al deposits exceeding this critical thickness, up to 200 × 10¹⁵ Al/cm². Al deposition was performed at low temperature (around 130 K) and the alloying process was followed in situ during subsequent annealing, by Auger electron spectroscopy, low energy electron diffraction and ion beam analysis-channeling measurements, in an ultra-high vacuum chamber connected to a Van de Graaff accelerator. We evidence the formation, after annealing at 750 K, of a crystallographically and chemically well-ordered NiAl(1 1 0) layer (whose thickness depends on the deposited Al amount), over a Ni₃Al “interfacial” layer (whose thickness—about 18 (1 1 1) planes—is independent of the deposited Al amount). The NiAl overlayer is composed of three variants, at 120° from each other in the surface plane, in relation with the respective symmetries of NiAl(1 1 0) and Ni₃Al(1 1 1). The NiAl layer is relaxed (the lattice parameters of cc-B2 NiAl and fcc-L1₂ Ni₃Al differ markedly), and we have determined its epitaxial relationship. In the case of the thickest alloyed layer formed the results concerning the structure of the NiAl layer have been confirmed and refined by ex situ X-ray diffraction and information on its grain size has been obtained by ex situ Atomic Force Microscopy. The kinetics of the alloying process is complex. It corresponds to an heterogeneous growth leading, above the thin Ni₃Al interfacial layer, to a mixture of Al and NiAl over the whole Al film, up to the surface. The atomic diffusion is very limited in the NiAl phase that forms, and thus the progressive enrichment in Ni of the Al film, i.e. of the mean Ni concentration, becomes slower and slower. As a consequence, alloying is observed to take place in a very broad temperature range between 300 K and 700 K. For annealing temperatures above 800 K, the alloyed layer is decomposed, Al atoms diffusing in the bulk of the substrate.     

Photochemical synthesis of copper nanoparticles incorporated in poly(vinyl pyrrolidone)

The effect of the presence of poly(vinyl pyrrolidone) (PVP) on the copper nanoparticle formation, obtained by UV irradiation of ethanol solution of Cu(acac)₂ (acac = 2,4-pentanedionato), was investigated. At 254 nm, in conditions of light completely absorbed by complex, the PVP exhibited protective and stabilizing effects, as shown by the formation of a colloidal copper solution and by a block of the heterogeneous process, which leads to thin film formation on the quartz walls. The colloidal solution was tested for several months by plasmon position and it was found that it remained unaltered in inert atmosphere, but returned to the starting complex on contact with air. The PVP ability to control the particle size was investigated by carrying out photoreduction sensitized by Hacac at 254 and 300 nm, in the presence of PVP concentration varying from 0 to 0.2 M. In this range it was possible to obtain copper nanoparticles of dimensions decreasing from 30 to 4 nm. Besides this, the PVP (0.005–0.05 M) role as sensitizer was investigated by irradiating solutions of Cu(acac)₂ at 300 nm which is an inactive wavelength for copper reduction by direct light absorption. It was found that the PVP was an efficient sensitizer of the copper photoreduction. The nanoparticles were characterized by plasmon band, Trasmission Electron Microscope (TEM) as well as Dynamic Light Scattering (DSL) analysis. The overall results evidence the advantages of the PVP use in the nanoparticle copper formation through the photochemical technique such as the exclusive formation of colloidal copper, their size control, stable colloidal solution and complete return to the starting complex.     

Upon a magnetic composite preparation based on magnetite and poly(succinimide)-b-poly(ethylene glycol) shell

Taking into account that magnetic particles with suitable surface characteristics have a high potential for the use in a lot of in vitro and in vivo applications, in the study is presented the in situ preparation of a core-shell magnetic composite based on the magnetite core and the shell composed from the poly(succinimide)-b-poly(ethylene glycol) copolymer. The average particle size of the synthesized magnetic microspheres is in the range of 6.5-8.8 μm with a magnetite content of around 11%. The saturation magnetization of the microspheres was found 26.8 emu/g, the magnetic microspheres being characterized by superparamagnetic properties. The particles have combined properties of high magnetic saturation and biocompatibility and interactive functions at the surface through the block copolymer shell. The surface of the magnetic particles has also the possibility for further functionalization or the attachment of various bioactive molecules after the hydrolysis of the succinimide cycle and the resulting carboxylic group.     

Synthesis, characterization and analytical applications of Ni(II)-ion imprinted polymer

Ion recognition-based separation techniques have received much attention because of their high selectivity for target ions. In this study, we have prepared a novel ion imprinted polymer (IIP) to remove nickel ions with high selectivity. The imprinted polymer was prepared by copolymerization of 2-hydroxy ethyl methacrylate (HEMA) with nickel vinylbenzoate complex in the presence of ethylene glycol dimethacrylate (EGDMA) as a crosslinker. The polymerization was carried out in bulk with free radical initiation using 2-methoxy ethanol as a solvent and porogen. The adsorbed nickel was completely eluted with 15 mL of 1 M HCl. Control polymer was also prepared by similar experimental conditions without using imprint ion. The above synthesized polymers were characterized by surface area measurements, FT-IR, microanalysis and SEM analysis. The adsorption capacity of IIP and CP was found to be 1.51 and 0.65 mmol g⁻¹, respectively. The optimal pH for quantitative enrichment was 6.5. Nature of eluent, eluent concentration and eluent volume were also studied. The relative selectivity factor (α_r) values of Ni(II)/Zn(II), Ni(II)/Cu(II) and Ni(II)/Co(II) were 78.6, 111.1 and 91.6, respectively. Five replicate determinations of 30 μg L⁻¹ of Ni(II) gave a mean absorbance of 0.067 with a relative standard deviation of 1.06%. The lowest concentration determined by GTA-AAS below which the recovery becomes non-quantitative is 6 μg L⁻¹. IIP was tested for removal of Ni(II) from sea water sample.     

Preparation and performance of polysulfone-sulfonated poly(ether ether ketone) blend ultrafiltration membranes. Part I

Ultrafiltration membranes were prepared from blends with polysulfone (PSf) and sulfonated poly(ether ether ketone) (SPEEK) by phase inversion technique. The blend membranes were prepared with polymer composition from 0 to15 wt%. Sulfonated poly(ether ether ketone) was used to improve the performance and permeability of blended membranes. The effects of polymer composition on compaction, pure water flux, water content, and membrane hydraulic resistance were studied. The membranes were also subjected to the determination of pore statistics and molecular weight cut-off (MWCO) determination studies by using different molecular weight of proteins. The porosity, pore size of the membranes increased with increasing concentrations of SPEEK in the casting solution. Similarly, the MWCOs of the blend membranes ranged from 20 to 45 kDa, depending on the various polymer blend compositions. The pure water flux of the PSf/SPEEK blend membranes increases from 16.7 to 61.5 l m⁻² h, when the concentration of SPEEK increased from 0 to 15 wt%. Scanning electron microscope (SEM) results qualitative evidence for the trends observed for the pore statistics and MWCO studies.