Controlling microencapsulation and release of micronized proteins using poly(ethylene glycol) and electrospraying

The fabrication of tailored microparticles for delivery of therapeutics is a challenge relying upon a complex interplay between processing parameters and materials properties. The emerging use of electrospraying allows better tailoring of particle morphologies and sizes than current techniques, critical to reproducible release profiles. While dry encapsulation of proteins is essential for the release of active therapeutics from microparticles, it is currently uncharacterized in electrospraying. To this end, poly(ethylene glycol) (PEG) was assessed as a micronizing and solubilizing agent for dry protein encapsulation and release from electrosprayed particles made from polycaprolactone (PCL). The physical effect of PEG in protein-loaded poly(lactic-co-glycolic acid) (PLGA) particles was also studied, for comparison. The addition of 5–15 wt% PEG 6 kDa or 35 kDa resulted in reduced PCL particle sizes and broadened distributions, which could be improved by tailoring the electrospraying processing parameters, namely by reducing polymer concentration and increasing flow rate. Upon micronization, protein particle size was reduced to the micrometer domain, resulting in homogenous encapsulation in electrosprayed PCL microparticles. Microparticle size distributions were shown to be the most determinant factor for protein release by diffusion and allowed specific control of release patterns.

Experimental and numerical analysis of the relationship between indoor and outdoor airborne particles in an operating room

This work investigated the impact of the HVAC filtration system and indoor particle sources on the relationship between indoor and outdoor airborne particle size and concentrations in an operating room. Filters with efficiency between 65% and 99.97% were used in the investigation and indoor and outdoor particle size and concentrations were measured. A balance mass model was used for the simulation of the impact of the surgical team, deposition rate, HVAC exhaust and air change rates on indoor particle concentration. The experimental results showed that high efficiency filters would not be expected to decrease the risk associated with indoor particles larger than approximately 1 µm in size because normal filters are relatively efficient for these large particles. A good fraction of outdoor particles were removed by deposition on the HVAC system surfaces and this deposition increased with particle size. For particles of 0.3-0.5 µm in diameter, particle reduction was about 23%, while for particles >10 µm the loss was about 78%. The modelling results showed that depending on the type of filter used, the surgical team generated between 93-99% of total particles, while the outdoor air contributed only 1-6%.

Synthesis and characterization of titanium sol–gels in varied gravity

Two unique test systems were designed and built to allow the effects of varied gravity (high, normal, reduced) during synthesis of titanium sol–gels to be studied. A centrifuge capable of providing high gravity environments of up to 70 g for extended periods while applying a 100 mbar vacuum and a temperature of 40–50 °C to the reaction chambers was developed. The second system was used in the QUT Microgravity Drop Tower Facility also provided the same thermal and vacuum conditions used in the centrifuge, but was required to operate autonomously during free fall. Through the use of post synthesis instrumental characterization, it was found that increased gravity levels during synthesis, had the greatest effect on the final products. Samples produced in reduced and normal gravity appeared to form amorphous gels containing very small particles with moderate surface areas. Whereas crystalline anatase (TiO2), was found to form in samples synthesized above 5 g with significant increases in crystallinity, particle size and surface area observed when samples were produced at gravity levels up to 70 g. It is proposed that for samples produced in higher gravity, an increased concentration gradient of water is forms at the bottom of the reacting film due to forced convection. The particles formed in higher gravity diffuse downward toward this excess of water, which favors the condensation reaction of remaining sol–gel precursors with the particles promoting increased particle growth. Due to the removal of downward convection in reduced gravity, particle growth due to condensation reaction processes are physically hindered hydrolysis reactions favored instead. Another significant finding from this work was that anatase could be produced at relatively low temperatures of 40–50 °C instead of the conventional method of calcination above 450 °C solely through sol–gel synthesis at higher gravity levels.

Recycling concrete: An undiscovered source of ultrafine particles

While concrete recycling is practiced worldwide, there are many unanswered questions in relation to ultrafine particle (UFP; Dp<100nm) emissions and exposure around recycling sites. In particular: (i) Does recycling produce UFPs and in what quantities? (ii) How do they disperse around the source? (iii) What impact does recycling have on ambient particle number concentrations (PNCs) and exposure? (iv) How effective are commonly used dust respirators to limit exposure? We measured size-resolved particles in the 5-560 nm range at five distances from a simulated concrete recycling source and found that: (i) the size distributions were multimodal, with up to ~93% of total PNC in the UFP size range; and (ii) dilution was a key particle transformation mechanism. UFPs showed a much slower decay rate, requiring ~62% more distance to reach 10% of their initial concentration compared with their larger counterparts. Compared with typical urban exposure during car journeys, exposure decay profiles showed up to ~5 times higher respiratory deposition within 10 m of the source. Dust respirators were found to remove half of total PNC; however the removal factor for UFPs was only ~57% of that observed in the 100-560 nm size range. These findings highlight a need for developing an understanding of the nature of the particles as well as for better control measures to limit UFP exposure.

Microstructure and electromagnetic characteristics of Ni nanoparticle film coated carbon microcoils

Carbon microcoils (CMCs) have been coated with a Ni nanoparticle film using an electroless plating process. The morphology, the elemental composition and the phases in the coating layer, complex permittivity and permeability of the CMCs and Ni-coated CMCs were, respectively, investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and microwave vector network analysis at room temperature. A homogeneous dispersion of Ni nanoparticles on the outer surface of the CMCs was obtained, with a mean particle size of ∼34.4 nm and the phosphorus content of about 8.5 wt%. When comparing the coated and uncoated CMC samples, the real (ε′) and imaginary (ε″) part of the complex permittivity as well as dielectric dissipation factor (tgδε = ε″/ε′) of the Ni-coated CMCs were much smaller, while the real (μ′) and imaginary (μ″) part of the complex permeability and the magnetic dissipation factor (t g σμ = μ″ / μ′) were larger. The enhanced microwave absorption of Ni-coated CMCs resulted from stronger dielectric and magnetic losses. In contrast, the microwave absorption of uncoated CMCs was mainly attributed to the dielectric rather than magnetic losses.

Low-phosporous nickel-coated carbon microcoils : Controlling microstructure through an electroless plating process

Carbon microcoils (CMCs) have been coated with a nickel-phosphorus (Ni-P) film using an electroless plating process, with sodium hypophosphite as a reducing agent in an alkaline bath. CMC composites have potential applications as microwave absorption materials. The morphology, elemental composition and phases in the coating layer of the CMCs and Ni-coated CMCs were investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD), respectively. The effects of process parameters such as pH, temperature and coating time of the plating bath on the phosphorus content and deposition rate of the electroless Ni-P coating were studied. The results revealed that a continuous, uniform and low-phosphorous nickel coating was deposited on the surface of the CMCs for 20 min at pH 9.0, plating bath temperature 70 °C. The as-deposited coatings with approximately 4.5 wt.% phosphorus were found to consist of a mix of nano- and microcrystalline phases. The mean particle size of Ni-P nanoparticles on the outer surface of the CMCs was around 11.9 nm. The deposition rate was found to moderately increase with increasing pH, whereas, the phosphorous content of the deposit exhibited a significant decrease. Moreover, the material of the coating underwent a phase transition between an amorphous and a crystalline structure. The thickness of the deposit and the deposition rate may be controlled through careful variation of the coating time and plating bath temperature.

Steady state and transient dynamometer vehicle emission measurements using a DiSC

Analysis of the particulate size and number concentration emissions from a fleet of inner city medium duty CNG buses was conducted using the newly available Diffusion Size Classifier in comparison with more traditional SMPS's and CPC's. Studies were conducted at both steady state and transient driving modes on a vehicle dynamometer utilising a CVS dilution system. Comparative analysis of the results showed that the DiSC provided equivalent information during steady state conditions and was able to provide additional information during transient conditions, namely, the modal diameter of the particle size distribution.

High-yield atmospheric-pressure CVD of highly-uniform carbon nanocoils using Co–P catalyst nanoparticles prepared by electroless plating

A simple, fast and low-cost atmospheric-pressure chemical vapor deposition technique is developed to synthesize high-yield carbon nanocoils (CNCs) using amorphous Co–P alloy as catalyst and thiophene as nucleation agent. The uniform catalyst pattern with the mean particle size of 350 nm was synthesized using a simple electroless plating process. This uniformity of the Co–P nanoparticles results in a high yield, very uniform size/shape distribution and regular structure of CNCs at the optimum growth temperature of 800 ◦C. The yield of CNCs reaches ∼76%; 70% of the CNCs have fiber diameters approximately 250 nm. The CNC coil diameters and lengths are 450–550nm and 0.5–2mm, respectively. The CNC nucleation and growth mechanism are also discussed.

Colloidal semiconductor nanocrystals : controlled synthesis and surface chemistry in organic media

Colloidal semiconductor nanocrystals (CS-NCs) possess compelling benefits of low-cost, large-scale solution processing, and tunable optoelectronic properties through controlled synthesis and surface chemistry engineering. These merits make them promising candidates for a variety of applications. This review focuses on the general strategies and recent developments of the controlled synthesis of CS-NCs in terms of crystalline structure, particle size, dominant exposed facet, and their surface passivation. Highlighted are the organic-media based synthesis of metal chalcogenide (including cadmium, lead, and copper chalcogenide) and metal oxide (including titanium oxide and zinc oxide) nanocrystals. Current challenges and thus future opportunities are also pointed out in this review.

Synthesis, characterization and organic field effect transistor performance of a diketopyrrolopyrrole-fluorenone copolymer

A diketopyrrolopyrrole (DPP) with fluorenone (FN) based low band gap alternating copolymer (PDPPT-alt-FN) has been synthesized via Suzuki coupling. PDPPT-alt-FN exhibits a deep HOMO level with a lower band gap. Fabricated organic thin film transistors using PDPPT-alt-FN as a channel semiconductor show p-channel behaviour with the highest hole mobility of 0.083 cm2 V-1 s-1 measured in air.

Hydrothermal synthesis and characterisation of Cu2ZnSnS4 light absorbers for solar cells

This project has extended the knowledge in the hydrothermal synthesis of copper zinc tin sulphide (CZTS) semiconductor material which is regarded as one of the most promising light absorbing material for PV technologies. The investigation of various reaction parameters on the controlled synthesis of CZTS compound has provided important insight into the formation mechanism as well as the crystal growth behaviour of the material. CZTS nanocrystals with different crystal structure and particle size were synthesised throughout this project. The growth mechanism of CZTS crystals through a high temperature annealing treatment was also explored.

Polymer-mediated synthesis of γ-Fe2O3 nano-particles

Nano-particles of γ-Fe2O3 were synthesized by reacting polyethylene oxide–FeCl3 complex with NH4OH. These were characterized by X-ray diffraction (XRD), scanning electron miscroscopy (SEM), selected area electron diffraction (SAED) and transmision electron microscopy (TEM). The average particle size was found to be 10 nm, as determined from the line broadening of the main XRD peak. The crystalline phase was a spinel-type tetragonal structure, which was confirmed from the electron diffraction pattern. The zero field cooled magnetization of samples with varying γ-Fe2O3 content as a function of temperature was measured using a vibrating sample magnetometer. The magnetization curves show a peak at low temperature (15 K) corresponding to the blocking temperature TB. The value of TB was found to decrease with decreasing particle size. The magnetization measurements with respect to field at 5 and 170 K confirmed the transition from superparamagnetic to spin-glass state at TB, as evidenced from the remanence and hysteresis. These results can be explained on the basis of Néel's theory of superparamagnetism as applied to nano-particles.

N,N'-Carbonyldiimidazole-mediated functionalization of superparamagnetic nanoparticles as vaccine carrier

Particulates with specific sizes and characteristics can induce potent immune responses by promoting antigen uptake of appropriate immuno-stimulatory cell types. Magnetite (Fe3O4) nanoparticles have shown many potential bioapplications due to their biocompatibility and special characteristics. Here, superparamagnetic Fe3O4 nanoparticles (SPIONs) with high magnetization value (70emug-1) were stabilized with trisodium citrate and successfully conjugated with a model antigen (ovalbumin, OVA) via N,N'-carbonyldiimidazole (CDI) mediated reaction, to achieve a maximum conjugation capacity at approximately 13μgμm-2. It was shown that different mechanisms governed the interactions between the OVA molecules and magnetite nanoparticles at different pH conditions. We evaluated as-synthesized SPION against commercially available magnetite nanoparticles. The cytotoxicity of these nanoparticles was investigated using mammalian cells. The reported CDI-mediated reaction can be considered as a potential approach in conjugating biomolecules onto magnetite or other biodegradable nanoparticles for vaccine delivery.

Microparticle-mediated gene delivery for the enhanced expression of a 19-KDa fragment of merozoite surface protein 1 of Plasmodium falciparum

The 19 kDa carboxyl-terminal fragment of merozoite surface protein 1 (MSP119) is a major component of the invasion-inhibitory response in individual immunity to malaria. A novel ultrasonic atomization approach for the formulation of biodegradable poly(lactic-co-glycolic acid) (PLGA) microparticles of malaria DNA vaccines encoding MSP119 is presented here. After condensing the plasmid DNA (pDNA) molecules with a cationic polymer polyethylenimine (PEI), a 40 kHz ultrasonic atomization frequency was used to formulate PLGA microparticles at a flow rate of 18 mL h1. High levels of gene expression and moderate cytotoxicity in COS-7 cells were achieved with the condensed pDNA at a nitrogen to phosphate (N/P) ratio of 20, thus demonstrating enhanced cellular uptake and expression of the transgene. The ability of the microparticles to convey pDNA was examined by characterizing the formulated microparticles. The microparticles displayed Z-average hydrodynamic diameters of 1.50-2.10 lm and zeta potentials of 17.8-23.2 mV. The encapsulation efficiencies were between 78 and 83%, and 76 and 85% of the embedded malaria pDNA molecules were released under physiological conditions in vitro. These results indicate that PLGA-mediated microparticles can be employed as potential gene delivery systems to antigen-presenting cells in the prevention of malaria.

Synthesis of biodegradable polymer-mesoporous silica composite microspheres for DNA prime-protein boost vaccination

DNA vaccines or proteins are capable of inducing specific immunity; however, the translation to the clinic has generally been problematic, primarily due to the reduced magnitude of immune response and poor pharmacokinetics. Herein we demonstrate a composite microsphere formulation, composed of mesoporous silica spheres (MPS) and poly(d,l-lactide-co-glycolide) (PLGA), enables the controlled delivery of a prime-boost vaccine via the encapsulation of plasmid DNA (pDNA) and protein in different compartments. Method with modified dual-concentric-feeding needles attached to a 40 kHz ultrasonic atomizer was studied. These needles focus the flow of two different solutions, which passed through the ultrasonic atomizer. The process synthesis parameters, which are important to the scale-up of composite microspheres, were also studied. These parameters include polymer concentration, feed flowrate, and volumetric ratio of polymer and pDNA-PEI/MPS-BSA. This fabrication technique produced composite microspheres with mean D[4,3] ranging from 6 to 34 μm, depending upon the microsphere preparation. The resultant physical morphology of composite microspheres was largely influenced by the volumetric ratio of pDNA-PEI/MPS-BSA to polymer, and this was due to the precipitation of MPS at the surface of the microspheres. The encapsulation efficiencies were predominantly in the range of 93-98% for pDNA and 46-68% for MPS. In the in vitro studies, the pDNA and protein showed different release kinetics in a 40 day time frame. The dual-concentric-feeding in ultrasonic atomization was shown to have excellent reproducibility. It was concluded that this fabrication technique is an effective method to prepare formulations containing a heterologous prime-boost vaccine in a single delivery system.