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A polyelectrolyte nanogel (PENG) particle consisting of lightly cross-linked terpolymer chains of N-isopropylacrylamide, acrylic acid, and 1-vinylimidazole has positive charges in an aqueous medium at pH 3 due to protonation of the imidazole groups, and thereby forms a polyelectrolyte complex with the linear polyanion, potassium poly(vinyl alcohol) sulfate (KPVS). It has been demonstrated that the hydrodynamic radius (Rh), by dynamic light scattering (DLS), and the radius of gyration (Rg), by static light scattering (SLS), of the complex particles are smallest at approximately 1:1 mixing ratio (rm) of anions to cations, in the absence of simple salts such as KCl (Langmuir 2005, 21, 4830). Here, we aimed to study the nature of the complex formed at rm=1 and examined the complex formation process by electrophoretic light scattering (ELS). It was found that the mobility of the cationic PENG with a stoichiometric amount of bound KPVS anions (i.e., the complex formed at rm=1) is positive but not zero at 25 degrees C. This was also the case when the complex was examined by ELS at 45 degrees C, where DLS and SLS show a temperature-driven collapse of the complex. We thus assumed that (a) electroneutrality is maintained in the complex particle with the aid of counterions, but (b) the complex is highly polarizable, and hence (c) during ELS the KPVS anions would dissociate in part from the complex. This hypothesis was supported by the following results: (i) Mixing complexed and uncomplexed PENG particles at different ratios brings about an increase in Rh and a decrease in the light scattering intensity of the complex at the same time, suggesting a polyelectrolyte exchange reaction. (ii) The same phenomenon is seen when poly(diallyldimethylammonium chloride) (PDDA as a polysalt) is added to the complex dispersion, meaning that the PDDA takes out the KPVS from the complex to form a stable PDDA-KPVS complex. (iii) Upon addition of KCl, the complex undergoes little change in Rh (62-67 nm) at a salt concentration (Cs)<or=0.02 M, aggregates with each other at Cs from 0.03 to 0.2 M, and becomes water-soluble at Cs>0.2 M. (iv) The Rh (78 nm) of the soluble complex at Cs from 0.3 to 0.5 M is larger than that at Cs<0.02 M, suggesting dissociation of the KPVS ions. (v) Complexation between KPVS and PDDA as mentioned in (ii) is facilitated in the presence of 0.01 M KCl.
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PMID:On an intraparticle complex of cationic nanogel with a stoichiometric amount of bound polyanions. 1727

Narrowly distributed polystyrene-b-poly(N-isopropylacrylamide)-b-polystyrene (PS-b-PNIPAM-b-PS) triblock copolymer with trithiocarbonate group in the middle of PNIPAM block was synthesized by using reversible addition fragmentation chain transfer (RAFT) polymerization. Such copolymer chains form a micelle-like aggregate with PNIPAM interlocking rings and associating PS blocks as the core and PNIPAM rings as the corona. The hydrolysis of the trithiocarbonate group leads the rings in the corona to be cut into open linear coils. Using laser light scattering, we have investigated the temperature-induced collapse of the aggregates with the rings and coils in the corona. Our results reveal that the former shrink much less than the latter due to the topological effect of PNIPAM blocks in the corona. On the other hand, the aggregates with long coils exhibit a sharper collapse transition than those with shorter coils.
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PMID:Thermoresponsive triblock copolymer aggregates investigated by laser light scattering. 1743 94

Micrometer-scale poly(N-isopropylacrylamide) (poly-NIPAAm) hydrogel monolith patterns were fabricated on solid surfaces using soft lithography. At sufficiently high aspect ratios, the hydrogel monoliths swell and contract laterally with temperature. The spaces between the monoliths form a series of trenches that catch, hold, and release appropriately sized targets. A series of poly-NIPAAm monoliths were fabricated with dry dimensions of 40 microm height, 12 microm diameter, and a spacing of 12 microm between monoliths. Above the lower critical solution temperature (LCST), the monoliths collapse to their dry dimensions and the spacing between monoliths is 12 microm. Below the LCST, the monoliths swell by 70% in the lateral direction, reducing the gap size between monoliths to 3 microm. The potential use of the hydrogel monoliths as size-selective "catch and release" structures was demonstrated with a mixture of 6 and 20 microm polystyrene microspheres, where the 6 microm diameter particles were selectively concentrated and separated from the larger particles.
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PMID:Size-Exclusion "capture and release" separations using surface-patterned poly(N-isopropylacrylamide) hydrogels. 1744 45

Nanoparticles and in particular gold nanorods have interesting optical properties arising from two well-differentiated plasmon modes. The frequency of such modes can be altered by their chemical environment and coupling with neighboring rods. This study investigates new composite materials made of gold nanorods adsorbed on thermoresponsive poly(N-isopropylacrylamide) (PNIPAM) microgels. It is shown that the thermally induced collapse of the polymer network inside the particles leads to a red shift of the longitudinal plasmon band of the gold rods, which is found to be fully reversible.
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PMID:Nanorod-coated PNIPAM microgels: thermoresponsive optical properties. 1748 99

Metal nanoparticles combined with environmentally sensitive polymers can lead to enhanced nanometer-sized switches. We present a silver nanoparticle synthesis method that uses poly(N-isopropylacrylamide) (PNIPAM) as the nucleating, capping, and stabilizing agent. The synthesis is performed at room temperature by sodium borohydride-mediated reduction of silver nitrate in the presence of a fully hydrated polymer. The resulting metal nanoparticles have a narrow size distribution comparable to or better than those achieved with other synthesis methods. The silver particles can be thermally precipitated by the collapse of the PNIPAM shell and resolubilized with fast response times, as shown by surface plasmon spectroscopy. The silver-PNIPAM composite allows for combined surface plasmon and thermal switching applications.
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PMID:Environmentally sensitive silver nanoparticles of controlled size synthesized with PNIPAM as a nucleating and capping agent. 1759 29

A novel magnetic drug-targeting carrier consisting of magnetic nanoparticles encapsulated with a smart polymer with characteristics of controlled drug release is described. The carrier is characterized by functionalized magnetite (Fe(3)O(4)) and conjugated therapeutic agent doxorubicin, which is encapsulated with the thermosensitive polymer, dextran-g-poly(N-isopropylacrylamide-co-N,N-dimethylacrylamide) [dextran-g-poly(NIPAAm-co-DMAAm)]. The surface of magnetite nanoparticles was functionalized by chemical bonding with 3-mercaptopropionic acid hydrazide (HSCH(2)CH(2)CONHNH(2)) via Fe-S covalent bonds. The anticancer therapeutic drug, doxorubicin, was attached to the surface of the functionalized magnetic nanoparticles through an acid-labile hydrazone-bond, formed by the reaction of hydrazide group of HSCH(2)CH(2)CONHNH(2) with the carbonyl group of doxorubicin. The dextran-g-poly(NIPAAm-co-DMAAm) smart polymer exhibits a lower critical solution temperature (LCST) of approximately 38 degrees C, which is representative of a phase transition behavior. This behavior allows for an on-off trigger mechanism. At an experimental temperature lower than LCST, the drug release was very low. However, at a temperature greater than LCST, there was an initially rapid drug release followed by a controlled released in the second stage, especially, in the mild acidic buffer solution of pH 5.3. The release of drug is envisaged to occur by the collapse of the encapsulated thermosensitive polymer and cleavage of the acid-labile hydrazone linkage. The proposed carrier is appropriately suitable for magnetic targeting drug delivery system with longer circulation time, reduced side effects and controlled drug release in response to the change in external temperature.
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PMID:Magnetic drug-targeting carrier encapsulated with thermosensitive smart polymer: core-shell nanoparticle carrier and drug release response. 1763 99

A double hydrophilic ABC triblock copolymer, poly(2-(diethylamino)ethyl methacrylate)-b-poly(2-(dimethylamino)ethyl methacrylate)-b-poly(N-isopropylacrylamide) (PDEA-b-PDMA-b-PNIPAM), containing the well-known pH-responsive PDEA block and thermoresponsive PNIPAM block, was synthesized by atom transfer radical polymerization via sequential monomer addition using ethyl 2-chloropropionate as the initiator. The obtained triblock copolymer exhibits interesting "schizophrenic" micellization behavior in aqueous solution, and supramolecularly self-assembles into three-layer "onion-like" PNIPAM-core micelles at acidic pH's and elevated temperatures and PDEA-core micelles with "inverted" structures at alkaline pH's and room temperature. In both cases, dynamic laser light scattering (LLS) and optical transmittance reveal the presence of near-monodisperse micelles, and the micelle formation/inversion process is fully reversible. Novel shell cross-linked (SCL) micelles with pH-responsive PDEA cores and thermoresponsive PNIPAM coronas were then facilely fabricated from the PDEA-b-PDMA-b-PNIPAM triblock copolymer by cross-linking the PDMA inner shells with 1,2-bis(2-iodoethoxy)ethane. The reversible pH-dependent swelling/shrinking of PDEA cores and thermosensitive collapse/aggregation of PNIPAM coronas of the obtained SCL micelles were investigated in detail by dynamic LLS, optical transmittance, and transmission electron microscopy. As the structurally stable SCL micelles possess pH-controllable core swellability and thermo-tunable corona permeability, the release profile of a model hydrophobic drug, dipyridamole, initially loaded within the hydrophobic PDEA core, can be dually controlled by both the solution pH and the temperature. This represents the first report of SCL micelles with multiresponsive cores and coronas, which may find practical applications in fields such as drug delivery and smart release.
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PMID:Fabrication of multiresponsive shell cross-linked micelles possessing pH-controllable core swellability and thermo-tunable corona permeability. 1788 94

The temperature-induced structural changes of a thermo-responsive poly(N-isopropylacrylamide) (PNIPAM) layer grafted onto a silica substrate were investigated in aqueous solution using an atomic force microscope (AFM) and a quartz crystal microbalance with dissipation (QCM-D). A PNIPAM layer was grafted onto the silicon wafer surface by free radical polymerization of NIPAM to obtain a high molecular weight polymer layer with low-grafting density overall. By AFM imaging, the transition of the grafted PNIPAM chains from a brush-like to a mushroom-like state was clearly visualized: The surface images of the plate were featureless at temperatures below the LCST commensurate with a brush-like layer, whereas above the LCST, a large number of domain structures with a characteristic size of approximately 100 nm were seen on the surface. Both frequency and dissipation data obtained using QCM-D showed a significant change at the LCST. Analysis of these data confirmed that the observed PNIPAM structural transition was caused by a collapse of the brush-like structure as a result of dehydration of the polymer chains.
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PMID:Direct observation of the phase transition for a poly(N-isopropylacryamide) layer grafted onto a solid surface by AFM and QCM-D. 1790 14

Synthesis of novel double-hydrophilic diblock copolypeptides (BCPs), poly(l-glutamic acid)-block-poly(N-isopropylacrylamide) (PLGnPNm), and their thermoresponsive properties in aqueous solutions at different pH values are described. The diblock copolypeptides were synthesized by a combination of ring-opening polymerization (ROP) of gamma-benzyl-l-glutamate N-carboxyanhydrides (BLG-NCA) and reversible addition-fragmentation chain transfer (RAFT) polymerization of N-isopropylacrylamide (NiPAM). A new class of RAFT agents (CTA-2 and CTA-3) with amino-functional groups was designed for this purpose. Two different strategies, i.e., macrochain transfer agent (CTA) and macroinitiator routes, were utilized and compared on the control of the chemical structures of the resulting BCPs. Their block ratios and lengths are broadly varied (n = 21-600 and m =180-442). Their thermally switchable aggregation behaviors in aqueous solutions were investigated at the microscopic level by 1H NMR spectroscopy and at the macroscopic level by turbidity measurements using UV/vis spectroscopy. The latter was also utilized for their lower critical aggregation temperature (LCAT) determination. The effects of block lengths and ratios as well as solution pH values on the collapse of NiPAM chain and aggregation process of BCPs were examined. This aggregation process was also followed by dynamic light scattering (DLS) measurements, and the thermally induced aggregate structures were investigated by transmission electron microscopy (TEM).
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PMID:Synthesis and characterization of thermo- and pH-responsive double-hydrophilic diblock copolypeptides. 1791 95

Silica-gold (SiO(2)-Au) nanoshells are a new class of nanoparticles that consist of a silica dielectric core that is surrounded by a gold shell. These nanoshells are unique because their peak extinctions are very easily tunable over a wide range of wavelengths particularly in the near infrared (IR) region of the spectrum. Light in this region is transmitted through tissue with relatively little attenuation due to absorption. In addition, irradiation of SiO(2)-Au nanoshells at their peak extinction coefficient results in the conversion of light to heat energy that produces a local rise in temperature. Thus, to develop a photothermal modulated drug delivery system, we have fabricated nanoshell-composite hydrogels in which SiO(2)-Au nanoshells of varying concentrations have been embedded within temperature-sensitive hydrogels, for the purpose of initiating a temperature change with light. N-isopropylacrylamide-co-acrylamide (NIPAAm-co-AAm) hydrogels are temperature-sensitive hydrogels that were fabricated to exhibit a lower critical solution temperature (LCST) slightly above body temperature. The resulting composite hydrogels had the extinction spectrum of the SiO(2)-Au nanoshells in which the hydrogels collapsed reversibly in response to temperature (50 degrees C) and laser irradiation. The degree of collapse of the hydrogels was controlled by the laser fluence as well as the concentration of SiO(2)-Au nanoshells. Modulated drug delivery profiles for methylene blue, insulin, and lysozyme were achieved by irradiation of the drug-loaded nanoshell-composite hydrogels, which showed that drug release was dependent upon the molecular weight of the therapeutic molecule.
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PMID:Temperature-sensitive hydrogels with SiO2-Au nanoshells for controlled drug delivery. 1792 Jan 54


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