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PubMed2003

Preparation and drug release behaviors of nimodipine-loaded poly(caprolactone)-poly(ethylene oxide)-polylactide amphiphilic copolymer nanoparticles.

Amphiphilic block copolymers, poly(caprolactone)-poly(ethylene glycol)-poly(lactide) (PCELA), were synthesized by ring opening polymerization of caprolactone and lactide initiated with the hydroxyl groups of poly(ethylene glycol) (PEG). These copolymers could form micelle-like nanoparticles due to their amphiphilic characteristic. From the observation of transmission electron microscopy (TEM), the nanoparticles exhibited a regular spherical shape with core-shell structure. The critical micelle concentrations (CMC) of these nanoparticles in water were decreased as molecular weight of PEG decreased. The particle sizes obtained by dynamic light scattering of these nanoparticles were in the range of 100-200 nm, and increased as the hydrophobic property of the nanoparticles increased. Nimodipine as a model drug was loaded in these nanoparticles to investigate the drug release behavior. It was found that the chemical composition of the nanoparticles was a key factor in controlling nanoparticle size, nanoparticle yields, drug-entrapment efficiency, and drug release behavior. When the PEG content is about 2% (wt), the release profile of PCELA nanoparticles appeared to follow zero-order kinetics.

Absorbable Implants↗
PubMed2003

Intradermal immunization with novel plasmid DNA-coated nanoparticles via a needle-free injection device.

A high population of dendritic cells in the skin makes intradermal (ID) immunization an attractive route. We sought to further enhance immune responses from a previously reported novel nanoparticle-based DNA vaccine delivery system by administering the system intradermally into mouse skin using Biojector 2000, a needle-free jet injection device. Two mouse studies were carried out. Balb/C mice (n=5-6) were immunized on day 0, 7, and 14 by subcutaneous injection or via the Biojector 2000 with pDNA alone (CMV-beta-galactosidase, 5 micro g), pDNA-coated nanoparticles, or beta-galactosidase protein (10 micro g) adjuvanted with 'Alum' (15 micro g). On day 28, mice were sacrificed and specific serum IgG and IgA titer, in vitro cytokine release, and cell proliferation of isolated splenocytes were determined. Similar to previous reports, in both mouse studies, SC immunization with pDNA-coated nanoparticles led to over a log increase in specific serum IgG titer as compared to immunization with pDNA alone. For pDNA alone, jet and SC injection did not result in significant differences in IgG titer. In contrast, for pDNA-coated nanoparticles, jet injection led to as high as a 20-fold enhancement in IgG titer over SC injection. In addition, jet injection of pDNA-coated nanoparticles enhanced the IgG titer by more than 200-fold over jet injection of pDNA alone. Also, jet injection of pDNA-coated nanoparticles resulted in significantly enhanced specific serum IgA titer. For in vitro cytokine release, immunization with pDNA-coated nanoparticles by jet injection enhanced IFN-gamma and IL-4 release over pDNA alone by 6- and 5-fold, respectively. SC injection of pDNA-coated nanoparticles also resulted in enhanced IFN-gamma and IL-4 release over pDNA alone although with less magnitude. Finally, immunization with pDNA-coated nanoparticles, by both jet injection and SC injection, led to improved splenocyte proliferation over pDNA alone. In conclusion, a combination of a novel cationic nanoparticle-based DNA delivery system with ID jet injection led to enhanced antibody production, Th-1/Th-2 balanced cytokine release, and enhanced splenocyte proliferation.

Animals↗
PubMed2001

Chitosan-DNA nanoparticles as gene carriers: synthesis, characterization and transfection efficiency.

Chitosan-DNA nanoparticles were prepared using a complex coacervation process. The important parameters for the nanoparticle synthesis were investigated, including the concentrations of DNA, chitosan and sodium sulfate, temperature of the solutions, pH of the buffer, and molecular weights of chitosan and DNA. At an amino group to phosphate group ratio (N/P ratio) between 3 and 8 and a chitosan concentration of 100 microg/ml, the size of particles was optimized to approximately 100--250 nm with a narrow distribution, with a composition of 35.6 and 64.4% by weight for DNA and chitosan, respectively. The surface charge of these particles was slightly positive with a zeta potential of +12 to +18 mV at pH lower than 6.0, and became nearly neutral at pH 7.2. The chitosan-DNA nanoparticles could partially protect the encapsulated plasmid DNA from nuclease degradation as shown by electrophoretic mobility analysis. The transfection efficiency of chitosan-DNA nanoparticles was cell-type dependent. Typically, it was three to four orders of magnitude, in relative light units, higher than background level in HEK293 cells, and two to ten times lower than that achieved by LipofectAMINE-DNA complexes. The presence of 10% fetal bovine serum did not interfere with their transfection ability. Chloroquine could be co-encapsulated in the nanoparticles at 5.2%, but with negligible enhancement effect despite the fact that chitosan only showed limited buffering capacity compared with PEI. The present study also developed three different schemes to conjugate transferrin or KNOB protein to the nanoparticle surface. The transferrin conjugation only yielded a maximum of four-fold increase in their transfection efficiency in HEK293 cells and HeLa cells, whereas KNOB conjugated nanoparticles could improve gene expression level in HeLa cells by 130-fold. Conjugation of PEG on the nanoparticles allowed lyophilization without aggregation, and without loss of bioactivity for at least 1 month in storage. The clearance of the PEGylated nanoparticles in mice following intravenous administration was slower than unmodified nanoparticles at 15 min, and with higher depositions in kidney and liver. However, no difference was observed at the 1-h time point.

Animals↗
PubMed1999

Incorporation of polymeric nanoparticles into solid dosage forms.

Besides parenteral delivery, polymeric nanoparticles have been used for oral drug delivery. In this study, model polymeric nanoparticles (aqueous colloidal polymer dispersions: Eudragit(R) RL 30D, L 30D, NE 30D, or Aquacoat(R)) with different physicochemical properties were incorporated into various solid dosage forms (granules, tablets, pellets or films). The compatibility of the nanoparticles with commonly used tabletting excipients and the redispersibility of the nanoparticles after contact of the solid dosage forms with aqueous media were investigated. Ideally, the nanoparticles should be released from the solid dosage forms with their original properties. The addition of polymeric binders (e.g. polyvinylpyrrolidone, Na carboxymethylcellulose or hydroxypropyl methylcellulose) to the aqueous nanoparticle dispersions prior to wet granulation resulted in phase separation (depletion or bridging flocculation) for many nanoparticle/binder systems. Two critical parameters for the complete redispersibility/release of the nanoparticles with the original particle size properties from the solid dosage forms were a (1) high minimum film formation temperature (MFT) of the polymer dispersion and (2) a good wettability of the dried polymeric nanoparticles. Nanoparticle dispersions with a low MFT were not redispersible, they coalesced into larger agglomerates/films during the drying step. Contact angle measurements correlated well with the redispersibility of the nanoparticles, with ethylcellulose particles having high contact angles and poor redispersibility and Eudragit(R) RL, a polymer stabilized with quaternary ammonium groups, having low contact angles and good redispersibility.

Acrylic Resins↗
PubMed2003

Lattice measurement and alloy compositions in metal and bimetallic nanoparticles.

A new reliable method for determining the lattice spacings of metallic and bimetallic nanoparticles in phase contrast high resolution electron microscopy (HREM) images was developed. In this study, we discuss problems in applying HREM techniques to single metal (Pt and Au) and bimetallic (AuPd) nanoparticles of unknown shapes and random orientations. Errors arising from particle tilt and edge effects are discussed and analysis criteria are presented to reduce these errors in measuring the lattice parameters of nanoparticles. The accuracy of an individual particle lattice measurement is limited by an effective standard deviation which depends on the size of the individual nanoparticle. For example, the standard deviation for 20-30 A Pt or Au nanoparticles is about 1.5%. To increase the accuracy in determining the lattice spacings of nanoparticles, statistical methods have to be used to obtain the average lattice spacing of an ensemble of nanoparticles. We measured approximately 100 nanoparticles with sizes in the range of 20-30 A and found that the mean lattice spacing can be determined to within 0.2%. By applying Vegard's law to the AuPd bimetallic systems we successfully detected the presence of alloying. For 30 A nanoparticles, the estimated ultimate error in determining the composition of the AuPd alloy is about 3% provided that at least 100 particles are measured. Finally, the challenges in determining the presence of more than one alloy phases in bimetallic nanoparticle systems were also discussed.

Journal Article↗
PubMed2003

Nanoparticles bearing polyethyleneglycol-coupled transferrin as gene carriers: preparation and in vitro evaluation.

The aims of this work were to determine the stability of pDNA against various conditions during microencapsulation, prepare transferrin (TF)-conjugated PEGylated polycyanoacrylate nanoparticles (TF-PEG-nanoparticles), and assess its physicochemical characteristics and in vitro targeting cells association. The open circular forms of pDNA obviously increased when pDNA was emulsified into organic solution under sonification. When pDNA solution (pH 7.0) contained 1, 3 or 5% (w/v) PVA, after sonification, average 48.2, 59.4 and 62.1% of double-supercoiled DNA (dsDNA) were preserved, respectively. When medium of pDNA was 0.9% NaCl (pH 7.0), 0.1M NaHCO(3) (pH 8.0) or phosphate buffer (pH 8.0), average 53.1, 69.3 and 56.9% of dsDNA remained after sonification, respectively. Poly(aminopoly(ethylene glycol)cyanoacrylate-co-hexadecyl cyanoacrylate) (poly(H(2)NPEGCA-co-HDCA)) showed a slight influence on pDNA in 0.1M NaHCO(3) (pH 8.0) when its concentration increased from 0.5 to 4% (w/v). TF-PEG-nanoparticles loading pDNA were spherical in shape with size under 200nm and entrapment efficiency 35-50%. 0.1M NaHCO(3) with 3% PVA (w/v) could largely reduce the damage of pDNA during microencapsulation. TF-PEG-nanoparticles bore 1-3% of the total PEG chains conjugated to TF molecules, and exhibited the burst effect with over 30% drug release within 1 day. After the first phase, pDNA release profiles displayed a sustained release. The amount of cumulated pDNA release over 7 days was: 86.3, 81.5 and 74.4% for 1, 2 and 4% polymer nanoparticles, respectively. The degree of target K562 cell binding of TF-PEG-nanoparticles was greater than that of non-targeted PEG-nanoparticles at 4 degrees C. The presence of free TF decreased significantly the degree of cell binding of TF-PEG-nanoparticles, which revealed that the binding of TF-PEG-nanoparticles to K562 cells was indeed receptor specific. These results suggested that TF-PEG-nanoparticles were useful for delivery of pDNA to target cells.

Buffers↗
PubMed2004

Improving the signal sensitivity and photostability of DNA hybridizations on microarrays by using dye-doped core-shell silica nanoparticles.

The development of new highly sensitive and selective methods for microarray-based analysis is a great challenge because, for many bioassays, the amount of genetic material available for analysis is extremely limited. Currently, imaging and detection of DNA microarrays are based primarily on the use of organic dyes. To overcome the problems of photobleaching and low signal intensities of organic dyes, we developed a new class of silica core-shell nanoparticles that encapsulated with cyanine dyes and applied the dye-doped nanoparticles as labeling in the DNA microarray-based bioanalysis. The developed nanoparticles have core-shell structure containing 15-nm Au colloidal cores with 95 dye-alkanethiol (dT)20 oligomers chemisorbed on the each Au particle surface and 10-15-nm silica coatings bearing thiol functional groups. To be utilized for microarray detection, the dye-doped nanoparticles were conjugated with DNA signaling probes by using heterobifunctional cross-linker. The prepared nanoparticle conjugates are stable in both aqueous electrolytes and organic solvents. Two-color DNA microarray-based detection was demonstrated in this work by using Cy3- and Cy5-doped nanoparticles in sandwich hybridization. The use of the fluorophore-doped nanoparticles in high-throughput microarray detection reveals higher sensitivity with a detection limit of 1 pM for target DNA in sandwich hybridization and greater photostable signals than the direct use of organic fluorophore as labeling. A wide dynamic range of approximately 4 orders of magnitude was also found when the dye-doped nanoparticles were applied in microarray-based DNA bioanalysis. In addition, the use of these dye-doped nanoparticles as the labeling in hybridization also improved the differentiation of single-nucleotide polymorphisms. This work offers promising prospects for applying dye-doped nanoparticles as labeling for gene profiling based on DNA microarray technology.

Base Pairing↗
PubMed2005

Light emission of gold nanoparticles induced by the reaction of bis(2,4,6-trichlorophenyl) oxalate and hydrogen peroxide.

Light emission at approximately 415 nm was observed for gold particles with diameters of 2.6-6.0 nm dispersed in a solution containing bis(2,4,6-trichlorophenyl) oxalate and hydrogen peroxide. It was found that the light intensity was independent of the protecting reagents of the gold nanoparticles with similar size, the light intensity with gold nanoparticles of 5.0 and 6.0 nm in diameter was stronger than that with gold nanoparticles of 2.6 and 2.8 nm in diameter, and the light intensity increased linearly with the concentration of the gold nanoparticles using 6.0-nm gold nanoparticles. The gold nanoparticles were identified as emitting species, and the quantum yield was determined to be (2.8 +/- 0.3) x 10(-5) using 6.0-nm gold nanoparticles. The light emission is suggested to involve a sequence of steps: the oxidation reaction of bis(2,4,6-trichlorophenyl) oxalate with hydrogen peroxide yielding an energy-rich intermediate 1,2-dioxetanedione, the energy transfer from this intermediate to gold nanoparticles, and the radiative relaxation of the as-formed exited-state gold nanoparticles. The observed luminescence is expected to find applications in the field of bioanalysis owing to the excellent biocompatibility and relatively high stability of gold nanoparticles.

Journal Article↗
PubMed2006

Formation of silver nanoparticles in poly(perfluorosulfonic) acid membrane.

The formation of silver nanoparticles by chemical reduction of Ag+-loaded Nafion-117 membrane with NaBH4 was studied using radioactivity tagged ions. The counterion-exchange method (Ag(m)+ <--> Na(s)+) was used to obtain a membrane sample with a varying proportion of Ag+ ions. The X-ray elemental mapping across the thickness of the membrane by energy-dispersive X-ray spectrometer attached to the environmental scanning electron microscope (ESEM/EDAX) indicated that Na+ and Ag+ were uniformly distributed in the membrane samples before reduction. The average size of nanoparticles formed after reduction was found to be 15 +/- 3 nm, irrespective of the concentration of silver ions present in the membrane before reduction. Energy-dispersive X-ray fluorescence (EDXRF) analyses of the membrane samples, carried out before and after reduction, indicated that the Ag concentration on the membrane surface was considerably increased after reduction. EDXRF measurements of the membrane samples, obtained from reduction carried out in a dead end cell, indicated that Ag nanoparticles were formed only on the membrane surface exposed to NaBH4 solution. Reduction carried out with NaBH4 tagged with 22Na showed that the formation of Ag nanoparticles involved exchange of Ag+ ions from ion-exchange sites in the interior of the membrane with Na+ ions, followed by reduction of Ag+ ions with BH4- ions at the surface of membrane. The study of self-diffusion of water, Na+, and Cs+ ions in the membrane loaded with Ag nanoparticles indicated that formation of Ag nanoparticles did not affect the diffusional transport properties of the membrane. The ion-exchange capacity and water uptake capacity were also not affected by the formation of Ag nanoparticles in the membrane. The spatial distribution of Ag nanoparticles across the thickness of the membrane obtained by ESEM/EDAX showed that Ag nanoparticles were confined to a few-micrometer surface layer of the membrane. Based on these observations, an attempt has been made to explain the mechanism of the formation of Ag nanoparticles in the membrane.

Journal Article↗
PubMed2004

Real-time probing of membrane transport in living microbial cells using single nanoparticle optics and living cell imaging.

Membrane transport plays a leading role in a wide spectrum of cellular and subcellular pathways, including multidrug resistance (MDR), cellular signaling, and cell-cell communication. Pseudomonas aeruginosa is renowned for its intriguing membrane transport mechanisms, such as the interplay of membrane permeability and extrusion machinery, leading to selective accumulation of specific intracellular substances and MDR. Despite extensive studies, the mechanisms of membrane transport in living microbial cells remain incompletely understood. In this study, we directly measure real-time change of membrane permeability and pore sizes of P. aeruginosa at the nanometer scale using the intrinsic color index (surface plasmon resonance spectra) of silver (Ag) nanoparticles as the nanometer size index probes. The results show that Ag nanoparticles with sizes ranging up to 80 nm are accumulated in living microbial cells, demonstrating that these Ag nanoparticles transport through the inner and outer membrane of the cells. In addition, a greater number of larger intracellular Ag nanoparticles are observed in the cells as chloramphenicol concentration increases, suggesting that chloramphenicol increases membrane permeability and porosity. Furthermore, studies of mutants (nalB-1 and DeltaABM) show that the accumulation rate of intracellular Ag nanoparticles depends on the expression level of the extrusion pump (MexAB-OprM), suggesting that the extrusion pump plays an important role in controlling the accumulation of Ag nanoparticles in living cells. Moreover, the accumulation kinetics measured by Ag nanoparticles are similar to those measured using a small fluorescent molecule (EtBr), eliminating the possibility of steric and size effects of Ag nanoparticle probes. Susceptibility measurements also suggest that a low concentration of Ag nanoparticles (1.3 pM) does not create significant toxicity for the cells, further validating that single Ag nanoparticles (1.3 pM) can be used as biocompatible nanoprobes for the study of membrane transport kinetics in living microbial cells.

Anti-Bacterial Agents↗
PubMed2006

Hydrolytic and enzymatic degradation of nanoparticles based on amphiphilic poly(gamma-glutamic acid)-graft-L-phenylalanine copolymers.

Amphiphilic graft copolymers consisting of poly(gamma-glutamic acid) (gamma-PGA) as the hydrophilic backbone and L-phenylalanine ethylester (L-PAE) as the hydrophobic side chain were synthesized by grafting L-PAE to gamma-PGA. The nanoparticles were prepared by a precipitation method, and about 200 nm-sized nanoparticles were obtained due to their amphiphilic properties. The hydrolytic and enzymatic degradation of these gamma-PGA nanoparticles was studied by gel permeation chromatography (GPC), scanning electron microscopy (SEM), dynamic light scattering (DLS) and (1)H NMR measurements. The hydrolysis ratio of gamma-PGA and these hydrophobic derivatives was found to decrease upon increasing the hydrophobicity of the gamma-PGA derivates. The pH had an effect on the hydrolytic degradation of the polymer. The hydrolysis of the polymer could be accelerated by alkaline conditions. The degradation of the gamma-PGA backbone by gamma-glutamyl transpeptidase (gamma-GTP) resulted in a dramatic change in nanoparticle morphology. With increasing time, the gamma-PGA nanoparticles began to decrease in size and finally disappeared completely. Moreover, the gamma-PGA nanoparticles were degraded by four different enzymes (Pronase E, protease, cathepsin B and lipase) with different degradation patterns. The enzymatic degradation of the nanoparticles occurred via the hydrolysis of gamma-PGA as the main chain and L-PAE as the side chain. In the case of the enzymatic degradation of gamma-PGA nanoparticles with Pronase E, the size of the nanoparticles increased during the initial degradation stage and decreased gradually when the degradation time was extended. Nanoparticles composed of biodegradable amphiphilic gamma-PGA with reactive function groups can undergo further modification and are expected to have a variety of potential pharmaceutical and biomedical applications, such as drug and vaccine carriers.

Guanosine Triphosphate↗
PubMed2005

Preparation and characterization of a new class of starch-stabilized bimetallic nanoparticles for degradation of chlorinated hydrocarbons in water.

Dechlorination of TCE and PCBs using bimetallic nanoparticles has received increasing interest in recent years. However, due to the extremely high reactivity, nanoparticles prepared using current methods tend to either react with surrounding media or agglomerate, resulting in the formation of much larger flocs and significant loss in reactivity. To overcome these drawbacks, we developed a simple and green approach for synthesizing palladized iron (Fe-Pd) nanoparticles. We modified the conventional methods by applying a water-soluble starch as a stabilizer. The starched nanoparticles displayed much less agglomeration but greater dechlorination power than those prepared without a stabilizer. TEM analyses indicated that the starched nanoparticles were present as discrete particles as opposed to dendritic flocs for nonstarched particles. The mean particle size was estimated to be 14.1 nm with a standard deviation of 11.7 nm, which translated to a surface area of approximately 55 m2 g(-1). While starched nanoparticles remained suspended in water for days, nonstarched particles agglomerated and precipitated within minutes. The starched nanoparticles exhibited markedly greater reactivity when used for dechlorination of TCE or PCBs in water. At a dose of 0.1 g L(-1), the starched particles were able to destroy 98% of TCE (C0 = 25 mg L(-1)) within 1 h. While trace amounts (<25 microg L(-1)) of 1,1-DCE were detected in the initial stage (<20 min) of degradation, no other intermediate byproducts such as vinyl chloride, cis-, or trans-dichloroethene were detected. The starched nanoparticles at approximately 1 g L(-1) were able to transform over 80% of PCBs (C0 = 2.5 mg L(-1)) in less than 100 h, as compared to only 24% with nonstarched Fe-Pd nanoparticles. The application of an innocuous stabilizer may substantially enhance the performances of palladized iron nanoparticles for environmental applications.

Environmental Pollutants↗
PubMed2006

Rapid purification and size separation of gold nanoparticles via diafiltration.

Purification and size-based separation of nanoparticles remain significant challenges in the preparation of well-defined materials for fundamental studies and applications. Diafiltration shows considerable potential for the efficient and convenient purification and size separation of water-soluble nanoparticles, allowing for the removal of small-molecule impurities and for the isolation of small nanoparticles from larger nanostructures in a single process. Herein, we report studies aimed at assessing the suitability of diafiltration for (i) the purification of water-soluble thiol-stabilized 3-nm gold nanoparticles, (ii) the separation of a bimodal distribution of nanoparticles into the corresponding fractions, and (iii) the separation of a polydisperse sample into fractions of differing mean core diameter. NMR, thermogravimetric analysis (TGA), and X-ray photoelectron spectroscopy (XPS) measurements demonstrate that diafiltration produces nanoparticles with a much higher degree of purity than is possible by dialysis or a combination of solvent washes, chromatography, and ultracentrifugation. UV-visible spectroscopic and transmission electron microscopic (TEM) analyses show that diafiltration offers the ability to separate nanoparticles of disparate core size. These results demonstrate the applicability of diafiltration for the rapid and green preparation of high-purity gold nanoparticle samples and the size separation of heterogeneous nanoparticle samples. They also suggest the development of novel diafiltration membranes specifically suited to high-resolution nanoparticle size separation.

Journal Article↗
PubMed2004

Ethylene glycol monolayer protected nanoparticles: synthesis, characterization, and interactions with biological molecules.

The usefulness of the hybrid materials of nanoparticles and biological molecules on many occasions depends on how well one can achieve a rational design based on specific binding and programmable assembly. Nonspecific binding between nanoparticles and biomolecules is one of the major barriers for achieving their utilities in a biological system. In this paper, we demonstrate a new approach to eliminate nonspecific interactions between nanoparticles and biological molecules by shielding the nanoparticle with a monolayer of ethylene glycol. A direct synthesis of di-, tri-, and tetra(ethylene glycol)-protected gold nanoparticles (Au-S-EGn, n = 2, 3, and 4) was achieved under the condition that the water content was optimized in the range of 9-18% in the reaction mixture. With controlled ratio of [HAuCl4]/[EGn-SH] at 2, the synthesized particles have an average diameter of 3.5 nm and a surface plasma resonance band around 510 nm. Their surface structures were confirmed by 1H NMR spectra. These gold nanoparticles are bonded with a uniform monolayer with defined lengths of 0.8, 1.2, and 1.6 nm for Au-S-EG2, Au-S-EG3, and Au-S-EG4, respectively. They have great stabilities in aqueous solutions with a high concentration of electrolytes as well as in organic solvents. Thermogravimetric analysis revealed that the ethylene glycol monolayer coating is ca. 14% of the total nanoparticle weight. Biological binding tests by using ion-exchange chromatography and gel electrophoresis demonstrated that these Au-S-EGn (n = 2, 3, or 4) nanoparticles are free of any nonspecific bindings with various proteins, DNA, and RNA. These types of nanoparticles provide a fundamental starting material for designing hybrid materials composed of metallic nanoparticles and biomolecules.

Biocompatible Materials↗
PubMed2004

Nanoparticles of varying hydrophobicity at the emulsion droplet-water interface: adsorption and coalescence stability.

The coalescence stability of poly(dimethylsiloxane) emulsion droplets in the presence of silica nanoparticles ( approximately 50 nm) of varying contact angles has been investigated. Nanoparticle adsorption isotherms were determined by depletion from solution. The coalescence kinetics (determined under coagulation conditions at high salt concentration) and the physical structure of coalesced droplets were determined from optical microscopy. Fully hydrated silica nanoparticles adsorb with low affinity, reaching a maximum surface coverage that corresponds to a close packed monolayer, based on the effective particle radius and controlled by the salt concentration. Adsorbed layers of hydrophilic nanoparticles introduce a barrier to coalescence of approximately 1 kT, only slightly reduce the coalescence kinetics, and form kinetically unstable networks at high salt concentrations. Chemically hydrophobized silica nanoparticles, over a wide range of contact angles (25 to >90 degrees ), adsorb at the droplet interface with high affinity and to coverages equivalent to close-packed multilayers. Adsorption isotherms are independent of the contact angle, suggesting that hydrophobic attraction overcomes electrostatic repulsion in all cases. The highly structured and rigid adsorbed layers significantly reduce coalescence kinetics: at or above monolayer surface coverage, stable flocculated networks of droplets form and, regardless of their wettability, particles are not detached from the interface during coalescence. At sub-monolayer nanoparticle coverages, limited coalescence is observed and interfacial saturation restricts the droplet size increase. When the nanoparticle interfacial coverage is >0.7 and <1.0, mesophase-like microstructures have been noted, the physical form and stability of which depends on the contact angle. Adsorbed nanoparticle layers at monolayer coverage and composed of a mixture of nanoparticles with different hydrophobisation levels form stable networks of droplets, whereas mixtures of hydrophobized and hydrophilic nanoparticles do not effectively stabilize emulsion droplets.

Adsorption↗
PubMed2005

Nanoparticles of Mg(OH)2: synthesis and application to paper conservation.

We report an investigation on the effects of counterions of magnesium salts on the homogeneous phase precipitation reaction to yield nanoparticles. The results provide new parameters to guide the control of the size, monodispersity, crystallinity, and morphology of Mg(OH)(2) nanoparticles. Evidence emerged that magnesium counterions affect the size of crystallites. The particle size increases from about 50 to 200 nm and follows the Hofmeister anion series: sulfate < chloride < nitrate </= perchlorate. All of the results show that a proper choice of counterion and composition of reaction mixture allows one to modulate and set conditions that predetermine production of nanoparticles with desired size. The Mg(OH)(2) nanoparticles have been applied to the successful conservation of paper. To demonstrate the efficacy of nanoparticles as deacidifying agent and as protection against cellulose aging, some samples of paper from the 18th century were treated with the nanoparticles and artificially aged by subjecting them to hydrothermal and photooxidative degradation. The treatment with nanoparticles preserved the mechanical features of paper, and the deterioration was consistently reduced. The comparison with the Wei t'O method (based on magnesium alkoxides), one of the most common and largely used methods for paper deacidification, indicates the following: (1) nanoparticles present a higher efficacy in the deacidification treatment since they are much more reactive; (2) nanoparticles are less aggressive since they are easily converted into the carbonate form; (3) they present minor disadvantages related to the chemical nature of the solvent used in the Wei t'O (i.e., CFC); (4) papers/books can be treated with very simple procedures, and do not require any special apparatus; (5) nanoparticle treatments have substantial economic benefits.

Journal Article↗
PubMed1998

Pegylated nanoparticles from a novel methoxypolyethylene glycol cyanoacrylate-hexadecyl cyanoacrylate amphiphilic copolymer.

PURPOSE: The aim of this work was to develop PEGylated poly(alkylcyanoacrylate) nanoparticles from a novel methoxypolyethyleneglycol cyanoacrylate-co-hexadecyl cyanoacrylate copolymer. METHODS: PEGylated and non-PEGylated nanoparticles were formed by nanoprecipitation or by emulsion/solvent evaporation. Nanoparticles size, zeta potential and surface hydrophobicity were investigated. Surface chemical composition was determined by X-ray photoelectron spectroscopy. Nanoparticle morphology was investigated by transmission electron microscopy after freeze-fracture. Nanoparticles cytotoxicity was assayed in vitro, onto mouse peritoneal macrophages. Cell viability was determined through cell mitochondrial activity, by a tetrazolium-based colorimetric method (MTT test). Finally, the degradation of PEGylated and non-PEGylated poly(hexadecyl cyanoacrylate) nanoparticles was followed spectrophotometrically during incubation of nanoparticles in fetal calf serum. RESULTS: Monodisperse nanoparticles with a mean diameter ranging between 100 and 200 nm were obtained using nanoprecipitation or emulsion/solvent evaporation as preparation procedures. A complete physico-chemical characterization, including surface chemical analysis, allowed to confirm the formation of PEG-coated nanoparticles. The PEGylation of the cyanoacrylate polymer showed reduced cytotoxicity towards mouse peritoneal macrophages. Furthermore, the presence of the PEG segment increased the degradability of the poly(hexadecyl cyanoacrylate) polymer in presence of calf serum. CONCLUSIONS: We succeeded to prepare PEGylated nanoparticles from a novel poly(methoxypolyethyleneglycol cyanoacrylate-co-hexadecyl cyanoacrylate) by two different techniques. Physico-chemical characterization showed the formation of a PEG coating layer. Low cytotoxicity and enhanced degradation were also shown.

Animals↗
PubMed2002

Genetic immunization using nanoparticles engineered from microemulsion precursors.

PURPOSE: Genetic immunization using "naked" plasmid DNA (pDNA) has been shown to elicit broad humoral and cellular immune responses. However, more versatile and perhaps cell-targeted delivery systems are needed. To this end, a novel process to engineer cationic nanoparticles coated with pDNA for genetic immunization was explored. METHODS; Cationic nanoparticles were engineered from warm oil-in-water microemulsion precursors composed of emulsifying wax as the oil phase and cetyltrimethylammonium bromide (CTAB) as the cationic surfactant. Plasmid DNA was coated on the surface of the cationic nanoparticles to produce pDNA-coated nanoparticles. An endosomolytic lipid and/or a dendritic cell-targeting ligand (mannan) were incorporated in or deposited on the nanoparticles to enhance the in vitro cell transfection efficiency and the in vivo immune responses after subcutaneous injection to Balb/C mice. The IgG titer to expressed beta-galactosidase and the cytokine release from isolated splenocytes after stimulation were determined on 28 days. RESULTS: Cationic nanoparticles (around 100 nm) were engineered within minutes. The pDNA-coated nanoparticles were stable at 37 degrees C over 30 min in selected biologic fluids. Transmission electron microscopy showed the nanoparticles were spherical. Plasmid DNA-coated nanoparticles. especially those with both an endosomolytic lipid and dendritic cell-targeting ligand. resulted in significant enhancement in both IgG titer (over 16-fold) and T-helper type-1 (Th1-type) cytokine release (up to 300% increase) over "naked" pDNA. CONCLUSION: A novel method to engineer pDNA-coated nanoparticles for enhanced in vitro cell transfection and enhanced in vivo immune responses was reported.

Animals↗