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PubMed2006

Adsorption of sodium dodecyl sulfate at the hydrophobic solid/aqueous solution interface in the presence of poly(ethylene glycol): dependence upon polymer molecular weight.

The polar orientation and degree of conformational order of sodium dodecyl sulfate (SDS) adsorbed at the hydrophobic octadecanethiol/aqueous solution interface in the presence of poly(ethylene glycol) (PEG) has been investigated as a function of the surfactant concentration and the molecular weight of the polymer. Sum frequency generation (SFG) vibrational spectroscopy was employed to obtain spectra of interfacial surfactant; weak SFG signals from interfacial polymer were also detected for polymer molecular weights of 900 and above. The phase of the SFG spectra indicated that both the surfactant and polymer had a net orientation of their CH2 and/or CH3 groups toward the hydrophobic surface. Spectra of SDS in the presence of mixed polymer/surfactant solutions showed increasing conformational order as the surfactant concentration was raised. At the lowest surfactant concentrations, the spectra of SDS were weaker in the presence of the polymer than in its absence. All PEG molecular weights investigated, with the exception of PEG 400, gave rise to significant inhibition of ordered surfactant adsorption below the critical micelle concentration. The greatest inhibitory effect was noted for PEG 900. Probing interfacial PEG specifically through the use of perdeuterated SDS revealed that the polymer spectral intensity decreased monotonically as the surfactant concentration was increased for all polymer molecular weights where a PEG spectrum was apparent. These findings are interpreted in terms of the displacement of preadsorbed polymer as the surfactant concentration increases. This result is compatible with observations of adsorption from SDS/PEG solutions at solid/solution and solution/air interfaces made using other techniques.

Adsorption↗

PubMed2006

Nanoparticles in solutions of adsorbing polymers: pair interactions, percolation, and phase behavior.

We study the polymer adsorption characteristics, pair-interaction potentials, and phase and percolation behavior in nanoparticle-polymer mixtures. We propose a "saturable" adsorption model to capture the effect of the finite surface saturation capacity for adsorption, and use polymer self-consistent field theory in combination with a McMillan-Mayer framework [McMillan, W. G., Jr.; Mayer, J. E. J. Chem. Phys. 1945, 13, 276] to compute the pair-interaction potentials. Our results demonstrate novel size effects that distinguish the adsorption characteristics of nanoparticles from that of larger particles. Specifically, we predict that the nanoparticle regime is characterized by a significant adsorbance of polymers, albeit distributed predominantly in the form of tails. We also demonstrate that an interplay between the surface saturation, polymer-to-particle size ratios, and the polymer concentrations governs the overall effective interactions between nanoparticles in the presence of an adsorbing polymer. We use simple, mean-field models to relate these characteristics to the phase and percolation behavior in such systems. Our results show that the percolation thresholds for smaller particles are significantly smaller (and, overall, correspond only to a few volume percent) compared to that of the larger particles. Further, with a decrease in the size of the particles, we also predict a considerable increase in the miscibility of the polymer-particle mixtures. Our results are qualitatively in accord with many experimental observations in the nanoparticle regime.

Journal Article↗

PubMed2006

Fluorometric and isothermal titration calorimetric studies on binding interaction of a telechelic polymer with sodium alkyl sulfates of varying chain length.

Steady-state fluorescence measurements and isothermal titration calorimetric experiments have been performed to study the interaction between a telechelic polymer, pyrene-end-capped poly(ethylene oxide) (PYPY), and sodium alkyl sulfate surfactants having decyl, dodecyl, and tetradecyl hydrocarbon tails. Fluorometric results suggest polymer-surfactant interaction in the very low range of polymer concentrations. The relative variation in the excimer to monomer pyrene emission intensities with varying surfactant concentration reveals that initial addition of surfactant favors intramolecular preassociation until the surfactant molecules start binding with the ethylene oxide (EO) chain. With the growing number of surfactant aggregates along the EO chain, the association becomes hindered due to the polyelectrolyte effect. The results from microcalorimetric titrations in the low concentration range of PYPY solution (approximately 10(-6) M) with alkyl sulfates suggest two kinds of surfactant-polymer interactions, one with the polymer hydrophobic end groups and the other with the ethylene oxide backbone. The overall polymer-surfactant interaction starts at a much lower surfactant concentration for the hydrophobically modified polymers compared to that in the case of unsubstituted poly(ethylene oxide) homopolymer. From the experiments critical aggregation concentration values and the second critical concentration where free micelles start forming have been determined. An endeavor has been made to unveil the mechanism underlying the corresponding associations of the surfactants with the polymer.

Journal Article↗

PubMed2007

Synthesis and characterization of variable-architecture thermosensitive polymers for complexation with DNA.

Copolymers of N-isopropylacrylamide with a fluorescent probe monomer were grafted to branched poly(ethyleneimine) to generate polycations that exhibited lower critical solution temperature (LCST) behavior. The structures of these polymers were confirmed by spectroscopy, and their phase transitions before and after complexation with DNA were followed using ultraviolet and fluorescence spectroscopy and light scattering. Interactions with DNA were investigated by ethidium bromide displacement assays, while temperature-induced changes in structure of both polymers and polymer-DNA complexes were evaluated by fluorescence spectroscopy, dynamic light scattering, laser Doppler anemometry, and atomic force microscopy (AFM) in water and buffer solutions. The results showed that changes in polymer architecture were mirrored by variations in the architectures of the complexes and that the overall effect of the temperature-mediated changes was dependent on the graft polymer architecture and content, as well as the solvent medium, concentrations, and stoichiometries of the complexes. Furthermore, AFM indicated subtle changes in polymer-DNA complexes at the microstructural level that could not be detected by light scattering techniques. Uniquely, variable-temperature aqueous-phase AFM was able to show that changes in the structures of these complexes were not uniform across a population of polymer-DNA condensates, with isolated complexes compacting above LCST even though the sample as a whole showed a tendency for aggregation of complexes above LCST over time. These results indicate that sample heterogeneities can be accentuated in responsive polymer--DNA complexes through LCST-mediated changes--a factor that is likely to be important in cellular uptake and nucleic acid transport.

Acrylamides↗

PubMed1998

Polymer Brushes: From Self-Consistent Field Theory to Classical Theory.

We consider planar brushes formed by end-grafted polymers with moderate to strong excluded-volume interactions. We first rederive the mean-field theory and solve the resulting self-consistent equations numerically. In the continuum limit, the results depend sensitively on a single parameter, beta, whose square is the ratio of the scaling prediction for the brush height to the unperturbed polymer radius of gyration, and which measures therefore the degree to which the polymers are stretched. For large values of beta, the density profile is close to parabolic, as predicted by the infinite-stretching theory of Zhulina et al. and of Milner et al. As beta decreases, the profile deviates strongly from a parabolic one. By calculating the most probable paths and comparing their contribution to various properties with those obtained from the full self-consistent theory, we determine the effect of the fluctuations about such paths. At large values of beta, these effects are very small everywhere. As beta decreases, fluctuation effects on the density profile become increasingly important near the grafting surface, but remain small far from it. For all values of beta, we find that polymer paths which begin far from the grafting surface are strongly, and almost uniformly, stretched throughout their length, including their free end points. Paths which begin close to the grafting surface are also stretched, but they initially move away from the grafting surface before reaching a maximum height and then returning to it. The classical theory is then derived from the self-consistent field equations by retaining, for each end point location, only that single trajectory which minimizes the free energy of the system. This free energy contains an entropy, of relative weight beta-1, which arises from the distribution of end points. Even for brushes which are only moderately stretched, the results of the classical theory for the brush profile and polymer end point distribution agree well with those of the full self-consistent theory except near the grafting surface itself. There the density profile as calculated in the self-consistent theory shows a characteristic decrease which is not captured by the classical theory. However it does capture the fact that the individual polymer paths are stretched in general throughout their length, including the end points, and yields nonmonotonic paths for polymers whose end points are close to the grafting surface. In addition, it reproduces extremely well the form of the density distribution far from the grafting surface, which is essentially Gaussian. This results from the fact that the stretching energy dominates the interaction energy of those polymers which extend far from the grafting surface, so that their behavior is nearly ideal. In the limit of infinite stretching, beta --> infinity, the theory reduces to that of Zhulina et al. and of Milner et al.

Journal Article↗

PubMed2000

Freeze-concentration separates proteins and polymer excipients into different amorphous phases.

PURPOSE: To study the miscibility of proteins and polymer excipients in frozen solutions and freeze-dried solids as protein formulation models. METHODS: Thermal profiles of frozen solutions and freeze-dried solids containing various proteins (lysozyme, ovalbumin, BSA), nonionic polymers (Ficoll, polyvinylpyrrolidone [PVP]), and salts were analyzed by differential scanning calorimetry (DSC). The polymer miscibility was determined from the glass transition temperature of maximally freeze-concentrated solute (Tg') and the glass transition temperature of freeze-dried solid (Tg). RESULTS: Frozen Ficoll or PVP 40k solutions showed Tg' at -22 degrees C, while protein solutions did not show an apparent Tg'. All the protein and nonionic polymer combinations (5% w/w, each) were miscible in frozen solutions and presented single Tg's that rose with increases in the protein ratio. Various salts concentration-dependently lowered the single Tg's of the proteins and Ficoll combinations maintaining the mixed amorphous phase. In contrast, some salts induced the separation of the proteins and PVP combinations into protein-rich and PVP-rich phases among ice crystals. The Tg's of these polymer combinations were jump-shifted to PVP's intrinsic Tg' at certain salt concentrations. Freeze-dried solids showed varied polymer miscibilities identical to those in frozen solutions. CONCLUSIONS: Freeze-concentration separates some combinations of proteins and nonionic polymers into different amorphous phases in a frozen solution. Controlling the polymer miscibility is important in designing protein formulations.

Calorimetry, Differential Scanning↗

PubMed2000

Collapse of stiff conjugated polymers with chemical defects into ordered, cylindrical conformations

The optical, electronic and mechanical properties of synthetic and biological materials consisting of polymer chains depend sensitively on the conformation adopted by these chains. The range of conformations available to such systems has accordingly been of intense fundamental as well as practical interest, and distinct conformational classes have been predicted, depending on the stiffness of the polymer chains and the strength of attractive interactions between segments within a chain. For example, flexible polymers should adopt highly disordered conformations resembling either a random coil or, in the presence of strong intrachain attractions, a so-called 'molten globule'. Stiff polymers with strong intrachain interactions, in contrast, are expected to collapse into conformations with long-range order, in the shape of toroids or rod-like structures. Here we use computer simulations to show that the anisotropy distribution obtained from polarization spectroscopy measurements on individual poly[2-methoxy-5-(2'-ethylhexyl)oxy-1,4-phenylenevinylene] polymer molecules is consistent with this prototypical stiff conjugated polymer adopting a highly ordered, collapsed conformation that cannot be correlated with ideal toroid or rod structures. We find that the presence of so-called 'tetrahedral chemical defects', where conjugated carbon-carbon links are replaced by tetrahedral links, divides the polymer chain into structurally identifiable quasi-straight segments that allow the molecule to adopt cylindrical conformations. Indeed, highly ordered, cylindrical conformations may be a critical factor in dictating the extraordinary photophysical properties of conjugated polymers, including highly efficient intramolecular energy transfer and significant local optical anisotropy in thin films.

Journal Article↗

PubMed2001

Epitaxial nucleation of crystallization at polymer-filler interfaces.

In polymer composites the interaction between polymer matrix and filler particles often results in nucleation of spherulites. The principles of polymer crystal nucleation and spherulite growth are investigated using scanning transmission electron microscopy (STEM) and microdiffraction techniques in combination with polarized light microscopy. Simultaneous diffraction patterns from the interface of the filler and the polymer were obtained. Special precautions for successful recording of the diffraction patterns were used to overcome the rapid loss of polymer crystallinity, resulting from electron beam damage. Analysis of the diffraction patterns has shown that partial epitaxial correlation between the atomic periodicity of the particle surface and the molecular periodicity of polymer chains is always present when spherulites are nucleated. STEM images show that only large particles, with well developed facets (cleavage planes), are nucleating. The nucleating efficiency of the filler is therefore dependent on the size as well as on the crystallographic orientation of the facet. Small particles, or those with no suitable facets, do not affect the crystalline structure of the polymer. It is also shown that anisotropic polymer structures can be formed by inhomogeneous dispersion of nucleating filler particles.

Journal Article↗

PubMed2001

Studies of the microstructure of polymer-modified bitumen emulsions using confocal laser scanning microscopy.

Polymer-modified bitumen emulsions present a safer and more environmentally friendly binder for enhancing the properties of roads. Cationic bitumen emulsion binders containing polymer latex were investigated using confocal laser scanning microscopy. The latex was incorporated into the bitumen emulsion by using four different addition methods and all emulsions were processed with a conventional colloid mill. The emulsion binder films were studied after evaporation of the emulsion aqueous phase. We show how the microstructure and distribution of the polymer varies within the bitumen binder depending on latex addition method, and that the microstructure of the binder remains intact when exposed to elevated temperature. It was found that a distinctly fine dispersion of polymer results when the polymer is blended into the bitumen before the emulsifying process (a monophase emulsion). In contrast, bi-phase emulsion binders produced by either post-adding the latex to the bitumen emulsion, or by adding the latex into the emulsifier solution phase before processing, or by comilling the latex with the bitumen, water and emulsifier all resulted in a network formation of bitumen particles surrounded by a continuous polymer film. The use of emulsified binders appears to result in a more evenly distributed polymer network compared to the use of hot polymer-modified binders, and they therefore have greater potential for consistent binder cohesion strength, stone retention and therefore improved pavement performance.

Journal Article↗

PubMed2000

Non-hydrolysable GTP-gamma-S stabilizes the FtsZ polymer in a GDP-bound state.

FtsZ, a tubulin homologue, forms a cytokinetic ring at the site of cell division in prokaryotes. The ring is thought to consist of polymers that assemble in a strictly GTP-dependent way. GTP, but not guanosine-5'-O-(3-thiotriphosphate) (GTP-gamma-S), has been shown to induce polymerization of FtsZ, whereas in vitro Ca2+ is known to inhibit the GTP hydrolysis activity of FtsZ. We have studied FtsZ dynamics at limiting GTP concentrations in the presence of 10 mM Ca2+. GTP and its non-hydrolysable analogue GTP-gamma-S bind FtsZ with similar affinity, whereas the non-hydrolysable analogue guanylyl-imidodiphosphate (GMP-PNP) is a poor substrate. Preformed FtsZ polymers can be stabilized by GTP-gamma-S and are destabilized by GDP. As more than 95% of the nucleotide associated with the FtsZ polymer is in the GDP form, it is concluded that GTP hydrolysis by itself does not trigger FtsZ polymer disassembly. Strikingly, GTP-gamma-S exchanges only a small portion of the FtsZ polymer-bound GDP. These data suggest that FtsZ polymers are stabilized by a small fraction of GTP-containing FtsZ subunits. These subunits may be located either throughout the polymer or at the polymer ends, forming a GTP cap similar to tubulin.

Bacterial Proteins↗

PubMed2005

Phase behavior of a blend of polymer-tethered nanoparticles with diblock copolymers.

Using the self-consistent field theory (SCFT), we investigate the phase behavior of a mixture of diblock copolymers and nanoparticles with monodisperse polymer chains tethered to their surfaces. We assume the size of the nanoparticles to be much smaller than that of the attached polymer chains and therefore model the particles with their grafted polymer "shell" as star polymers. The polymer chains attached to the particles are of the same species as one of the blocks of the symmetric diblock copolymer. Of primary interest is how to tune the shell of the particle by changing both the length and number of tethered polymers in order to achieve higher loading of nanoparticles within an ordered structure without macrophase separation occurring. We find that the phase behavior of the system is very sensitive to the size of the particle including its tethered shell. The region of microphase separation is increased upon decreasing the star polymer size, which may be achieved by shortening and/or removing tethered polymer chains. To explore the possible structures in these systems we employ SCFT simulations that provide insight into the arrangement of the different species in these complex composites.

Journal Article↗

PubMed2006

Shear thinning in dilute polymer solutions.

We use bead-spring models for a polymer coupled to a solvent described by multiparticle collision dynamics to investigate shear thinning effects in dilute polymer solutions. First, we consider the polymer motion and configuration in a shear flow. For flexible polymer models we find a sharp increase in the polymer radius of gyration and the fluctuations in the radius of gyration at a Weissenberg number approximately 1. We then consider the polymer viscosity and the effect of solvent quality, excluded volume, hydrodynamic coupling between the beads, and finite extensibility of the polymer bonds. We conclude that the excluded volume effect is the major cause of shear thinning in polymer solutions. Comparing the behavior of semiflexible chains, we find that the fluctuations in the radius of gyration are suppressed when compared to the flexible case. The shear thinning is greater and, as the rigidity is increased, the viscosity measurements tend to those for a multibead rod.

Journal Article↗

PubMed2001

Antibacterial efficacy of triclosan-incorporated polymers.

Triclosan (2, 4, 4'-trichloro-2'-hydroxydiphenyl ether) is a broad-spectrum antimicrobial agent, routinely used in various personal care products.(1) It is also incorporated into polymers through melt-mixing, with the aim of providing persistent antibacterial action on the surface of the polymer.(2,3) Such triclosan-incorporated polymers can be promoted for hospital use as fabric seat covers, tables, chairs, and clothing. We assessed the antibacterial efficacy of triclosan-incorporated polymer disks against 2 bacteria cultured in liquids in contact with the polymer. In spite of the relatively high concentrations of triclosan in the polymer, only some initial slowing of the bacterial growth rates was observed, followed by the absence of an antibacterial effect over extended periods. The triclosan at the surface of the disks dissolves into the liquids, and the rest of the triclosan, immobilized in the disks, does not contribute to the antibacterial effectiveness of triclosan-incorporated polymer. In light of recent studies, which have shown that triclosan acts on a specific target within the bacterial lipid synthesis pathway, triclosan-incorporated polymers may provide the ideal setting for resistant strains of bacteria to grow and thus should be used selectively in hospital environments.

Anti-Infective Agents, Local↗

PubMed1995

Carbon monoxide religation kinetics to hemoglobin S polymers following ligand photolysis.

The re-equilibration rate of carbon monoxide binding to hemoglobin S polymers is determined by time-resolved measurements of linear dichroism spectra. Linear dichroism is used to detect religation to hemoglobin in the polymer in the presence of rebinding to free hemoglobin S tetramers. Measurement of the linear dichroism resulting from photolysis of the small percentage of ligand bound to the polymer is accomplished through the use of an ultrasensitive, ellipsometric linear dichroism technique developed for this purpose. The major finding is that the return of the polymer phase to its equilibrium ligation state is much slower than that of the solution phase hemoglobin tetramers. Assuming all hemes in the polymer are equally likely to participate in rebinding, the re-equilibration rate for carbon monoxide religation to hemoglobin S polymers is found to be 0.14 +/- 0.07 (s-1 mM-1), about 1000 times slower than the rebinding rate of carbon monoxide to T-state monomer hemoglobin. Several interpretations of this result are discussed. An understanding of the ligand binding kinetics to hemoglobin S polymers could have pathophysiological significance in its relevance to polymer formation and melting during red blood cell circulation.

Anemia, Sickle Cell↗

PubMed2004

Synchronized chemoenzymatic synthesis of monodisperse hyaluronan polymers.

The length of the hyaluronan (HA) polysaccharide chain dictates its biological effects in many cellular and tissue systems. Long and short HA polymers often appear to have antagonistic or inverse effects. However, no source of very defined, uniform HA polymers with sizes greater than 10 kDa is currently available. We present a method to produce synthetic HA with very narrow size distributions in the range of approximately 16 kDa to approximately 2 MDa. The Pasteurella HA synthase enzyme, pmHAS, catalyzes the synthesis of HA polymer utilizing monosaccharides from UDP-sugar precursors. Recombinant pmHAS will also elongate exogenously supplied HA oligosaccharide acceptors in vitro in a nonprocessive fashion. As a result of bypassing the slow initiation step in vitro, the elongation process is synchronized in the presence of acceptor; thus all of polymer products are very similar in length. In contrast, without the use of an acceptor, the final polymer size range is difficult to predict and the products are more polydisperse. HA polymers of a desired size are constructed by controlling the reaction stoichiometry (i.e. molar ratio of precursors and acceptor molecules). The use of modified acceptors allows the synthesis of HA polymers containing tags (e.g. fluorescent, radioactive). In this scheme, each molecule has a single foreign moiety at the reducing terminus. Alternatively, the use of radioactive UDP-sugar precursors allows the synthesis of uniformly labeled native HA polymers. Overall, synthetic HA reagents with monodisperse size distributions and defined structures should assist in the elucidation of the numerous roles of HA in health and disease.

Glucuronosyltransferase↗

PubMed2001

Interaction of verapamil hydrochloride with carbopol 934P and its effect on the release rate of the drug and the water uptake of the polymer matrix.

In the present study, investigation of the possibility of interaction of verapamil hydrochloride with Carbopol 934P using differential scanning calorimetric analysis and Fourier transform infrared analysis was performed. The effect of the drug-to-polymer ratio, the electrolyte concentration, and the pH of the medium on the extent of interaction of the drug with the polymer using 2(3) factorial design was investigated. The study also investigated the effect of this interaction on the rate of water uptake of the matrix or the rate of release of verapamil hydrochloride from the swelling polymer matrix. Results revealed that the drug-to-polymer ratio had the most influential effect on both the extent of interaction between the drug and the polymer and the rate of water uptake of the polymer matrix. On the other hand, the pH of the medium had the most significant effect on the rate of drug release. Interaction of the tertiary amine nitrogen of the drug with the anionic carboxyl group on the polymer, forming an insoluble complex, reduced the rate of drug release. This interaction also led to neutralization of the carboxyl group and suppression of the electrostatic repulsion between the anionic groups, which reduced the uncoiling and chain relaxation of the polymer and consequently decreased the swelling of the matrix. The application of the designed experiment allowed the quantification of the effect of each of the studied variables on the investigated responses through the calculation of their coefficient in the response suface equation and checking of their significance.

Acrylates↗

PubMed1998

Interferon-containing controlled-release polymers for localized cerebral immunotherapy.

Controlled-release ethylene-vinyl acetate copolymers (EVAc), which were used previously for the in vivo intracerebral delivery of chemotherapeutics, were evaluated as a possible route of localized intracerebral delivery of interferon (IFN). Natural mouse IFN-alpha/beta (Mu-IFN-alpha/beta) was incorporated into polymers at 5% or 10% by weight with 2 x 10(4) U or 4 x 10(4) U, respectively. In vitro and in vivo studies of the release of Mu-IFN-alpha/beta from EVAc polymers showed the released IFN to be biologically active, as determined by the inhibition assay of viral cytopathic effect (CPE). Evaluation of the in vitro kinetics of release showed that most of the IFN activity was released in the first 4 days, with the rest being released thereafter. The in vivo kinetic release of Mu-IFN-alpha/beta from intracerebrally implanted polymers showed that most of the IFN activity was released within 24 h after polymer implantation in the hemisphere ipsilateral to the polymer. This IFN activity gradually decreased over the next 72 h, with a significant linear trend (p < 0.0001). The hemisphere contralateral to the implanted polymer showed no significant levels of IFN activity throughout the 4 days of evaluation. By contrast, blood levels of IFN increased from day 1 to day 4, showing a significant linear trend (p = 0.0125), with IFN levels on day 4 being significantly higher (p < 0.05) than on day 1 after polymer implant. This study demonstrates the feasibility of intracranial controlled local delivery of IFN using a polymer delivery device.

Animals↗

PubMed1985

Enhancement of calcium absorption in rats by coadministration of glucose polymer.

Glucose polymer derived from corn starch is widely used in infant formula and nutritional supplements as a readily digestible, low osmolarity source of calories. We have previously observed that glucose polymer causes a marked increase in intestinal calcium absorption in patients with intestinal malabsorption and in normal subjects. The present study investigates the effect of concurrently administered glucose polymer on intestinal 45calcium absorption in rats. The effect of glucose polymer on calcium absorption was compared to that of equivalent doses of dextrose or lactose. Femur radioactivity was determined as an index of calcium absorption. Carbohydrates were prepared at doses of 0.5, 2.0 and 4.0 mg/g body weight and administered with 45Ca by stomach gavage. Control rats received 45Ca in water alone. Coadministration of glucose polymer resulted in a dose-dependent increase in calcium absorption. At the highest dose of polymer studied calcium absorption was 75% greater than in control animals. Administration of lactose and dextrose also resulted in a dose-dependent increase in calcium absorption. Calcium absorption was 122 and 67% greater than controls when 4 mg/g BW lactose and dextrose were given with the 45Ca. We conclude that glucose polymer stimulates calcium absorption in rats similar to lactose and glucose. These results suggest that glucose polymer may be a useful therapeutic adjunct in patient groups in which there is a desire to increase intestinal calcium absorption.

Animals↗