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A systematic study of the host-guest complexation by alpha-, beta-, and gamma-cyclodextrin (CD) in either the free state or as substituents of poly(acrylic acid) (PAA) with the hydrophobic n-octadecyl groups, C18, substituted onto PAA (HMPAA) and its effect on polymer aggregation and network formation is reported. Free alpha-CD, beta-CD, and gamma-CD mask hydrophobic associations between the C18 substituent of HMPAA in aqueous solution and form host-guest complexes with a 1:1 or CD:C18 substituent stoichiometry at 0.5 wt % polymer concentration. For alpha-CD this host-guest stoichiometry changes to 2:1 or 2alpha-CD:C18 at > or =1 wt % polymer concentrations but not for beta-CD and gamma-CD. Shear-thickening occurs when gamma-CD complexes C18 HMPAA substituents. Upon addition of sodium dodecyl sulfate, SDS (SDS:CD = 1:1), the hydrophobic associations between C18 diminished by alpha-CD masking were fully restored, were only partly restored in the case of beta-CD, and not restored for gamma-CD. When alpha- and beta-CD substituted PAA (alpha-CDPAA and beta-CDPAA) were mixed with HMPAA polymer, networks formed. As for free beta-CD, the beta-CD substituents of beta-CDPAA also formed 1:1 or beta-CD:C18 stoichiometry host-guest complexes with the C18 substituents of HMPAA. The alpha-CD substituents of alpha-CDPAA also formed 1:1 or alpha-CD:C18 stoichiometry host-guest complexes with some indication of the formation of 2:1 or 2alpha-CD:C18 stoichiometry host-guest complexes at polymer concentrations > or =1 wt %. The polymer networks formed by beta-CDPAA with HMPAA are less viscous than those formed by alpha-CDPAA, for which shear-thickening occurs at polymer concentrations > or =2 wt %. It is evident that the difference in CD annular size and its match with the C18 of HMPAA control the diversity of the interactions of alpha-CD, beta-CD, gamma-CD, alpha-CDPAA, and beta-CDPAA with HMPAA.
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PMID:Complexation behavior of alpha-, beta-, and gamma-cyclodextrin in modulating and constructing polymer networks. 1857 Apr 48

Hollow microcapsules containing polymeric micelles in their walls were fabricated by alternating assembly of poly(allylamine hydrochloride) (PAH) and poly(styrene- b-acrylic acid) (PS- b-PAA) micelles on MnCO(3) microparticles followed by sacrificing the templates in acid solution. The successful formation of PAH/micelle multilayers on both planar and curved substrates was confirmed by UV-vis spectroscopy, ellipsometry, and xi-potential measurements. The PS- b-PAA micelles retained their structure during the whole assembly process. The as-prepared microcapsules showed extraordinary stability against concentrated HCl (37%) and 0.1 M NaOH solutions. No variation in capsule size or shape was observed in acidic solution, while slight swelling and distortion of the capsules took place in alkaline solution. However, these capsules completely recovered their original size and morphology after being incubated in acidic solution again. The microcapsules, in which large voids exist between the micelle grains on the walls, were totally permeable to fluorescein-tagged dextran with an M(w) of 2000 kDa. Assembly of additional PAH/poly(sodium 4-styrenesulfonate) multilayers could substantially reduce the permeation of the same molecules. These multicompartmental capsules combine polymeric micelles with multilayer polyelectrolyte microcapsules and could possibly be imparted with multifunctions, thus possibly finding diverse applications in the fields of drug delivery, biosensing, and nanobiotechnology.
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PMID:Assembly of polymeric micelles into hollow microcapsules with extraordinary stability against extreme pH conditions. 1859 Mar

We consider a symmetrical poly(styrene- stat-(acrylic acid))- block-poly(acrylic acid), i.e., PSAA- b-PAA, diblock copolymer, with a molar fraction phi AA = 0.42 of acrylic acid, in the more hydrophobic PSAA statistical first block. We investigate its structural behavior at constant concentration in water using small-angle neutron scattering (SANS) by varying (i) the ionization of its acrylic acid motives via the pH by adding NaOH and (ii) the ionic strength of the solution by increasing the NaCl salt concentration c S. We present the resulting morphological phase diagram {pH, c S}, in which we identified two different lamellar phases presenting a smectic long-range order at small-to-intermediate ionizations and a spherical phase with a liquid-like short-range order at larger ionization. In the low-ionization regime, the first lamellar phase comprises a water-free PSAA lamellar core surrounded by a dense poly(acrylic acid) brush swollen with water. Its mostly hydrophobic core still being glassy, this phase is unable to reorganize and is frozen in. A detailed analysis of the SANS data shows the osmotic nature of the polyelectrolyte brush, in which the Na+ counterions are confined so that local electroneutrality is satisfied. Above the pH at which the PSAA statistical block starts ionizing, the PSAA lamellar core melts. The second lamellar phase identified then comprises a PSAA core thinner than that of the frozen-in previous phase, implying a significant increase of the core/water interface and a decrease of the brush surface density. The transition from the first lamellar phase to the second one can be quantitatively shown to result from the balance between the two contributions: (i) the extra interfacial cost between the thinner core and water and (ii) the associated gain in entropy of mixing for the counterions confined inside the brush. At even higher ionization, the diblocks finally form spherical objects with a very small, pH-dependent aggregation number and reach an apparent onset of self-association. When the highest ionization investigated is reached, the cores of these final spherical core-shell objects are found to contain a significant amount of water. We thereby demonstrate that at constant concentration, pH, and ionic strength both trigger a transition from frozen to molten hydrophobic phases as well as unexpected morphological transitions.
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PMID:Double-polyelectrolyte, like-charged amphiphilic diblock copolymers: swollen structures and pH- and salt-dependent lyotropic behavior. 1859 8

Complexes of poly(diallyldimethylammonium chloride) (PDDA) and sodium silicate (PDDA-silicate) are alternately deposited with poly(acrylic acid) (PAA) to fabricate PAA/PDDA-silicate multilayer films. The removal of the organic components in the PAA/PDDA-silicate mulilayer films through calcination produces highly porous silica coatings with excellent mechanical stability and good adhesion to substrates. Quartz substrates covered with such porous silica coatings exhibit both antireflection and antifogging properties because of the reduced refractive index and superhydrophilicity of the resultant films. A maximum transmittance of 99.86% in the visible spectral range is achieved for the calcinated PAA/PDDA-silicate films deposited on quartz substrates. The wavelengths of maximum transmittance could be well tailored by simply changing the deposition cycles of multilayer films. The usage of PDDA-silicate complexes allows for the introduction of high porosity to the resultant silica coatings, which favors the fabrication of antireflection and antifogging coatings with enhanced performance. Meanwhile, PDDA-silicate complexes enable rapid fabrication of thick porous silica coatings after calcination because of the large dimensions of the complexes in solution. The easy availability of the materials and simplicity of this method for film fabrication might make the mechanically stable multifunctional antireflection and antifogging coatings potentially useful in a variety of applications.
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PMID:Mechanically stable antireflection and antifogging coatings fabricated by the layer-by-layer deposition process and postcalcination. 1876 28

The formation of binary and ternary complexes of poly(acrylic acid) (PAA) with N, N, N, N-dodecyltrimethylammonium chloride (DTAC) and/or Cu (2+) ions is investigated in dilute aqueous solution through turbidimetry, viscometry, and pyrene fluorescence probing. It is shown that the PAA-DTAC and PAA-Cu (2+) complexation as well as the formation of ternary PAA-DTAC-Cu (2+) complexes are controlled from the pH of the aqueous solution. A pronounced quenching of the emission of pyrene is observed when ternary PAA-DTAC-Cu (2+) complexes are formed, as a result of the close proximity of Cu (2+) ions (complexed along the polymer chain) and the probe (solubilized in the hydrophobic mixed polymer-surfactant aggregates), as indicated from the corresponding Stern-Volmer plots. A significant quenching is also observed when poly(sodium styrene sulfonate) is used instead of PAA, indicating that electrostatically bound Cu (2+) ions are still effective quenchers of the emission of the probes under similar conditions. Finally, it is demonstrated that the formation-deformation of the ternary PAA-DTAC-Cu (2+) complexes upon changing pH may act as a pH-controlled "on-off" switch of the emission of pyrene in aqueous solution.
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PMID:Formation of ternary poly(acrylic acid)-surfactant-Cu2+ complexes in aqueous solution: quenching of pyrene fluorescence and pH-controlled "on-off" emitting properties. 1881 24

The uptake of cesium, strontium and europium from dilute nitric acid solutions by a poly(sodium acrylate-acrylic acid) PAA hydrogel has been investigated. pH variations are consistent with cation exchange processes: COO(-), Na (+)H (+), COO(-), Na (+)M (m+) ( M (m+) = Cs (+)and Sr (2+)) and COOH Eu (3+). Saturation of the gel is achieved for metal/carboxylate ratios R = 0.5. The swelling ratios of gels loaded with metal cations are those of uncharged, shrunk gels (Sr, Eu) or of charged, swollen gels (Cs) in agreement with the formation of uncharged (COO)(2)Sr, (COO)(2)EuX (X = NO(3) or OH) type complexes and (COO(-), Cs(+)) ion pairs. The metal cations are extracted in the gels following the order of their affinities with carboxylic groups Eu(3+) > Sr(2+) > Cs(+). An increase of the ionic strength of the metal aqueous solution up to 0.5M NaNO(3) leads to slightly decrease the europium uptake by the PAA hydrogel, but 0.1M NaNO(3) is sufficient to prevent the Sr and Cs extractions.
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PMID:Uptake of cesium, strontium and europium by a poly(sodium acrylate-acrylic acid) hydrogel. 1896 96

Two types of polyelectrolyte multilayers were formed on both sides of a quartz crystal microbalance (QCM) substrate by a novel alternate drop coating process. In this study, poly(diallyldimethylammonium chloride) (PDDA) and poly(sodium 4-styrene sulfonate) (PSS) were used as strong-strong polyelectrolytes. On the other hand, PDDA and poly(acrylic acid) (PAA) were used as strong-weak polyelectrolytes. The novel alternate drop coating process can separately fabricate each polyelectrolyte multilayer on both sides of the substrate. The substrate provides dual biointerfaces, both sides of which comprise different multilayers, by employing a combination of polymers. The formation of the multilayer by alternate drop coating was evaluated in terms of changes in the frequency of the QCM and model protein adsorption for proteins such as bovine serum albumin, and their characteristics were investigated with those of the conventional alternate adsorption process by performing dip coating. There was no significant difference between the surface properties resulting from the two formation conditions. This result strongly supported the fact that the multilayers fabricated by alternate drop coating were similar in quality to those fabricated by conventional dip coating. The resulting dual biointerfaces with polyelectrolyte multilayers provide alternative biofunctions in terms of individual protein loading. In summary, the novel alternate drop coating process for substrates is a good candidate for the preparation of dual biointerfaces in the biomedical field.
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PMID:Alternate drop coating for forming dual biointerfaces composed of polyelectrolyte multilayers. 1898 56

Compression of the polyelectrolyte multilayers has been found previously when they were pressed by a poly(dimethylsiloxane) (PDMS) stamp under a small pressure (Macromolecules 2004, 37, 8836). In this work, we further found that the pattern formation of the poly(diallyldimethylammonium chloride) (PDADMAC) containing multilayers is dependent on the drying time of the multilayers prior to compression. After the poly(4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA)/PDADMAC multilayers were dried at 70% relative humidity and room temperature for 2, 6, and 12 h, compression of the multilayers by a PDMS stamp with linear patterns obtained double strips, high ridges and linear patterns on the multilayers, respectively. These phenomena were independent of the layer number and salt concentration and could be applied to other PDADMAC containing multilayer systems such as poly(styrene sulfonate) sodium salt (PSS)/PDADMAC and poly(acrylic acid, sodium salt) (PAA)/PDADMAC. A model was suggested to depict the process, and the influence of the water content on the multilayer structure and properties was discussed. The stability experiments revealed that the strips and high ridges obtained at shorter drying time could be erased by incubation in water for 5 h, while the compression created patterns were very stable.
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PMID:Influence of drying time of polyelectrolyte multilayers on the compression-induced pattern formation. 1905 63

Free-standing and supported films with a lateral gradient in composition were prepared using blends of poly(acrylic acid) (PAA)/sodium salt and its copolymers with acrylamide (AAm) in an applied electric field. The gradients were stabilized by complexation of carboxylate groups with metal species. To find the favorable conditions and components for successful blending and interaction with Fe and Ce species, we studied blending of the two PAA samples with molecular weights of 2000 and 15 000 Da with two copolymers of AA and AAm (with 10 and 70 wt % of AA units) and interaction of these blends with Fe(III) and Ce(IV) ions. The structure of the hybrid (blend) films was studied using differential scanning calorimetry (DSC), X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy, X-ray diffraction, and optical microscopy. To ensure blend miscibility and efficient interaction with metal ions, the copolymer containing 70 wt % AA units has been used. The surface enrichment with metal species was observed at all experimental conditions studied in this work. For lateral gradient film formation, 15 000 Da PAA has been used to avoid uneven distribution of the homopolymer in the film, observed for 2000 Da PAA. The gradient films were characterized by XPS. The lateral gradient of functionality such as COONa group or Fe content has been obtained at different strengths of electric field applied during film formation. The use of lower voltage allows one to prevent NaOH formation and creates more favorable conditions for development of a gradient polymer film. The Ce content gradient was not observed due to formation of large Ce oxide particles (> or = 750 nm), masking the gradient of functionality. For the first time, free-standing films with a lateral gradient in composition were prepared using an applied electric field.
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PMID:Bioinspired gradient materials via blending of polymer electrolytes and applying electric forces. 1910 43

Positively charged poly(allylamine hydrochloride) (PAH) and poly(acrylic acid) (PAA) complexes (noted as PAH-PAA) with a molar excess of PAH were layer-by-layer (LbL) assembled with polyanion poly(sodium 4-styrenesulfonate) (PSS) to produce multilayer films. The film structure and deposition behavior of the PAH-PAA/PSS films were influenced by the structure of PAH-PAA complexes in solution. For the PAH-PAA complexes with a low ratio of PAA to PAH the PAH-PAA complexes have low-level cross-linking and are flexible. The resultant PAH-PAA/PSS films have a thin film thickness and smooth surface and exhibit a nonlinear deposition behavior where the amount of PAH-PAA complexes and PSS deposited in each deposition cycle are larger than in its previous cycle. The PAH-PAA complexes with a high ratio of PAA to PAH have high-level cross-linking and are rigid. The PAH-PAA/PSS films constructed from the rigid PAH-PAA complexes have a large film thickness and rough surface and exhibit a linear deposition behavior. Deposition of the PAH-PAA/PSS films was well characterized by quartz crystal microbalance, atomic force microscopy, and scanning electron microscopy. The thermally cross-linked PAH-PAA/PSS films can be released from substrate to form stable free-standing films by an ion-triggered exfoliation method. Meanwhile, positively charged PAH-PAA complexes can be LbL assembled with negatively charged PAH-PAA complexes with a molar excess of PAA to produce multilayer films. Use of polyelectrolyte-polyelectrolyte complexes as building blocks for LbL fabrication provides a facile way to tailor the structures of the resultant films by simply changing the structure of the complexes in solution.
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PMID:Layer-by-layer deposition of polyelectrolyte-polyelectrolyte complexes for multilayer film fabrication. 1910 38


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