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PubMed2005

Small-angle neutron scattering and theoretical investigation of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) stabilized oil-in-water microemulsions.

The aim of this study is to determine the effects of oil solutes and alcohol cosolvents on the structure of oil-in-water microemulsions stabilized by poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) triblock copolymers. The systems investigated involved the solubilization of 1,3,5-trimethylbenzene or 1,2-dichlorobenzene by P123 (EO(20)-PO(70)-EO(20)) pluronic surfactant micelles in water and water + ethanol solvents. The structures of these swollen micelles were determined by small-angle neutron scattering (SANS). A thermodynamic model was employed to interpret the characterization data. The results of the thermodynamic model for micellization agreed well with the SANS data from samples of micelles swollen by both oils. The model predicted the size of the micelles within 5% accuracy using only one fitting parameter, the micelle polydispersity. Ethanol had significantly different effects on the polymer micelles that contained solubilized oil compared to pure polymer micelles. For pure polymer micelles, the addition of ethanol increased the solubility of the polymer and, therefore, decreased the total volume fraction of micelles, while for polymer-oil aggregates, ethanol tended to have a positive effect on the volume fraction of micelles. SANS results showed that the greatest divergence from pure aqueous solvent results occurred at oil concentrations above the microemulsion stability limit.

Journal Article↗

PubMed2003

Neutron reflection and small-angle neutron scattering studies of a fluorocarbon telomer surfactant.

Dilute aqueous phase behavior of a novel tris(hydroxymethyl)acrylamidomethane (THAM)-derived telomer bearing a perfluorohexyl hydrophobic chain, F6THAM6, has been investigated. Fluorinated polyhydroxy surfactants of this kind find use in emerging biomedical applications. Neutron reflection (NR) and drop volume surface tension (DVT) methods have been used to determine the critical micelle concentration (cmc=4.7 x 10(-4) mol x dm(-3)) and surface adsorption parameters (at the cmc NR gives a molecular area a(cmc)=67.4 and 62 A(2) and surface excess gamma(cmc)=2.46 x 10(-6) mol x m(-2)). The aggregation structures were determined by small-angle neutron scattering (SANS), indicating globular (polydisperse spheres) micelles of radius approximately 30 A are present. These findings are compared with literature on surfactants with related structures, to identify how the unusual molecular structure of F6THAM6 affects surfactant properties.

Journal Article↗

PubMed2000

Critical role of micelles in pancreatic lipase activation revealed by small angle neutron scattering.

In the duodenum, pancreatic lipase (PL) develops its activity on triglycerides by binding to the bile-emulsified oil droplets in the presence of its protein cofactor pancreatic colipase (PC). The neutron crystal structure of a PC-PL-micelle complex (Hermoso, J., Pignol, D., Penel, S., Roth, M., Chapus, C., and Fontecilla-Camps, J. C. (1997) EMBO J. 16, 5531-5536) has suggested that the stabilization of the enzyme in its active conformation and its adsorption to the emulsified oil droplets are mediated by a preformed lipase-colipase-micelle complex. Here, we correlate the ability of different amphypathic compounds to activate PL, with their association with PC-PL in solution. The method of small angle neutron scattering with D(2)O/H(2)O contrast variation was used to characterize a solution containing PC-PL complex and taurodeoxycholate micelles. The resulting radius of gyration (56 A) and the match point of the solution indicate the formation of a ternary complex that is similar to the one observed in the neutron crystal structure. In addition, we show that either bile salts, lysophospholipids, or nonionic detergents that form micelles with radii of gyration ranging from 13 to 26 A are able to bind to the PC-PL complex, whereas smaller micelles or nonmicellar compounds are not. This further supports the notion of a micelle size-dependent affinity process for lipase activation in vivo.

Animals↗

PubMed1991

Conformation of Lys-plasminogen and the kringle 1-3 fragment of plasminogen analyzed by small-angle neutron scattering.

Native human Glu-plasminogen (Glu1-Asn791) was previously shown to have a radius of gyration of 39 A and a shape best described by a prolate ellipsoid [Mangel, W. F., Lin, B., & Ramakrishnan, V. (1990) Science 248, 69-73]. Upon occupation of a weak lysine-binding site, the shape reversibly changes to that best described by a Debye random coil with a radius of gyration of 56 A. Conversion from the closed to the open form is not accompanied by any change in secondary structure, hence the closed conformation is formed by interaction between domains, the five kringles and the protease domain, and this is abolished upon conversion to the open form. Here we analyzed by small-angle neutron scattering the conformations of human Lys-plasminogen (Lys78-Asn791) and the fragment K1-3 that contains the first three kringles of plasminogen (Tyr80-Val338 or Tyr80-Val354). The shape of Lys-plasminogen was best described by a Debye random coil with a radius of gyration of 51 A, and occupation of its lysine-binding sites by 6-aminohexanoic acid did not dramatically alter its conformation. Thus Lys-plasminogen was in the open form, similar to that of Glu-plasminogen with its lysine-binding sites occupied. The fragment K1-3 in the absence or presence of 6-aminohexanoic acid had a shape best described equally either by an elongated prolate ellipsoid or by a Debye random coil, with a radius of gyration of 29 A. Our model for the two forms of plasminogen is that, in the closed form, domain interaction generates a compact, almost globular, structure.(ABSTRACT TRUNCATED AT 250 WORDS)

Amino Acid Sequence↗

PubMed1983

Optical properties and small-angle neutron scattering of bovine heart mitochondrial oligomycin sensitivity conferring protein.

The mitochondrial oligomycin sensitivity conferring protein (OSCP) was isolated from beef heart mitochondria according to Senior (1979) [Senior, A.E. (1979) Methods Enzymol. 55,391-397] with a supplementary step of Sephadex chromatography for more extensive purification. The ultraviolet and fluorescence spectra of OSCP were consistent with the presence of tyrosyl residues and the absence of tryptophanyl residues. From the circular dichroism spectrum of OSCP, 43% alpha-helical structure was calculated; the dichroism spectra of OSCP in H2O and D2O were identical. A molecular weight (Mr) of 22 000 for OSCP was determined by sodium dodecyl sulfate gel electrophoresis at different concentrations of the polyacrylamide gel. The radius of gyration (Rg) and the shape of OSCP in H2O and D2O were studied by small-angle neutron scattering. The experimentally determined Rg value of OSCP in H2O was 24 +/- 1 A, and its Mr was 25 000 +/- 3000. Comparison of the experimental Rg value with that expected for a compact globular protein of the same molecular weight (17 A) led to the conclusion that OSCP is a considerably elongated molecule protein with an axial ratio higher than 3. In D2O buffer, the Rg value was higher than that in H2O, a situation in contrast with that observed for most globular hydrophilic proteins; this might be due to a preferential location of the positively charged lysine residues.

Adenosine Triphosphatases↗

PubMed2004

Organic spin clusters. A dendritic-macrocyclic poly(arylmethyl) polyradical with very high spin of S = 10 and its derivatives: synthesis, magnetic studies, and small-angle neutron scattering.

Synthesis and characterization of organic spin clusters, high-spin poly(arylmethyl) polyradicals with 24 and 8 triarylmethyls, are described. Polyether precursors to the polyradicals are prepared via modular, multistep syntheses, culminating in Negishi cross-couplings between four monofunctional branch (dendritic) modules and the tetrafunctional calix[4]arene-based macrocyclic core. The corresponding carbopolyanions are prepared and oxidized to polyradicals in tetrahydrofuran-d(8). The measured values of S, from numerical fits of magnetization vs magnetic field data to Brillouin functions at low temperatures (T = 1.8-5 K), are S = 10 and S = 3.6-3.8 for polyradicals with 24 and 8 triarylmethyls, respectively. Magnetizations at saturation (M(sat)) indicate that 60-80% of unpaired electrons are present at T = 1.8-5 K. Low-resolution shape reconstructions from the small-angle neutron scattering (SANS) data indicate that both the polyradical with 24 triarylmethyls and its derivatives have dumbbell-like shapes with overall dimensions 2 x 3 x 4 nm, in agreement with the molecular shapes of the lowest energy conformations obtained from Monte Carlo conformational searches. On the basis of these shapes, the size of the magnetic anisotropy barrier in the polyradical, originating in magnetic shape anisotropy, is estimated to be in the milliKelvin range, consistent with the observed paramagnetic behavior at T >or= 1.8 K. For macromolecular polyradicals, with the elongated shape and the spin density similar to the polyradical with 24 triarylmethyls, it is predicted that the values of S on the order of 1000 or higher may be required for "single-molecule-magnet" behavior, i.e., superparamagnetic blocking (via coherent rotation of magnetization) at the readily accessible temperatures T > 2 K.

Journal Article↗

PubMed1999

Acoustic Spectroscopy for Characterizing Heptane/H(2)O/AOT Reverse Microemulsions.

Acoustic spectroscopy was used to monitor the droplet size distribution in a classic three component system of heptane, water, and aerosol-OT (AOT). The size of the reverse microemulsion drops was varied by changing the molar ratio of water to AOT surfactant. The acoustic results for this transparent microemulsion were found to be in close agreement with literature results obtained with small angle neutron scattering and small angle X-ray scattering. The system was investigated well into the turbid region where microemulsion changes to macroemulsion. The droplet size distribution was found to shift to a bimodal form due to this transition. Copyright 1999 Academic Press.

Journal Article↗

PubMed2006

Influence of conformational asymmetry on the phase behavior of ternary homopolymer/block copolymer blends around the bicontinuous microemulsion channel.

We have developed a new ternary polymeric system, poly(ethylene-alt-propylene) (PEP)/poly(butylene oxide) (PBO)/PEP-PBO, to study the complex phase behavior near the bicontinuous microemulsion phase channel. The molecular weights of the PEP and PBO homopolymers are 2600 and 3050 g/mol, respectively, and the copolymer is 23.4 kg/mol with volume fraction composition fPBO=0.49. A combination of small-angle neutron scattering, small-angle X-ray scattering, rheology, optical microscopy, and visual oil bath measurements was employed to map out the phase diagrams at five fixed homopolymer PBO/PEP ratios, ranging from 40/60 to 60/40 by volume, with copolymer concentrations ranging from 0 to 100%. It was found that the bicontinuous microemulsion channel is consistently cut off at low temperature by a hexagonal phase. We attribute this phenomenon to the effect of the conformational asymmetry between the PEP and PBO species, whereby the more flexible PBO component induces a spontaneous curvature toward the PBO domains. These findings complement previous descriptions of the isopleth phase diagrams for A/B/A-B systems and identify a new design variable for preparing bicontinuous phases.

Journal Article↗

PubMed2004

Association behavior of fluorine-containing and non-fluorine-containing methacrylate-based amphiphilic diblock copolymer in aqueous media.

Fluorine-containing amphiphilic block copolymers, poly(sodium methacrylate)-block-poly(nonafluorohexyl methacrylate) (NaMAm-b-NFHMAn) (m:n = 61:12, 72:33, 64:57), and the corresponding non-fluorine-containing amphiphilic block copolymer, poly(sodium methacrylate)-block-poly(hexyl methacrylate) (NaMAm-b-HMAn) (m:n = 64:10, 69:37, 67:50), were synthesized. Both polyNaMA-b-polyNFHMA and polyNaMA-b-polyHMA formed micelles above critical micelle concentrations, (cmc's), around 3 x 10(-5) to 1 x 10(-4) mol/L, while neither polymer decreased surface tension of aqueous solutions. The size and shape of the micelles were examined by dynamic light scattering, small-angle neutron scattering, and small-angle X-ray scattering. PolyNaMA-b-polyHMA appeared to form only spherical micelles, while polyNaMA-b-polyNFHMA with a long NFHMA segment formed both spherical and rodlike micelles. The micelles of fluorine-containing block copolymers were obviously larger than those of non-fluorine-containing block copolymers with the same chain length and the same hydrophilic/hydrophobic chain ratio. The fluorine-containing block copolymer selectively solubilized fluorinated dye into the water phase when a mixture of decafluorobiphenyl and 2,6-dimethylnaphthalene was added to the micelle solution.

Journal Article↗

PubMed2006

Structural and dynamical properties of ribbonlike self-assemblies of a fluorinated cationic surfactant.

The structural and dynamic properties of low ionic strength micellar solutions of the cationic surfactant perfluorooctylbutane trimethylammonium bromide have been investigated by cryo-TEM, small-angle neutron scattering, small-angle X-ray scattering, T-jump and rheological experiments. The surfactant molecules self-assemble into narrow ribbons with average dimensions on the order of 4 nm x 3 nm, either under salt-free conditions or in the presence of up to 30 mM KBr or NaF. Cryo-TEM also reveals in the salt-free systems the presence of networks of multiconnected micelles. Rheological experiments showed that these surfactant systems exhibit a strong shear-thickening effect even in the presence of up to 30 mM KBr. The T-jump response of the micellar solutions was found to be multiexponential. This observation rules out the presence of only linear micelles with an exponential length distribution and suggests more complex topologies of the micellar aggregates. The relaxation time associated with the predominant process in the T-jump relaxation is strongly correlated to the critical shear rate beyond which shear thickening occurs, thus indicating that this critical shear rate is controlled by the micellar kinetics.

Journal Article↗

PubMed2005

Behavior of tri(n-butyl)ammonium bis[citrato(3-)-O1,O3,O6]silicate in aqueous solution: analysis of a sol-gel process by small-angle neutron scattering.

The racemic hexacoordinate silicon(IV) complex tri(n-butyl)ammonium bis[citrato(3-)-O1,O3,O6]silicate (1) was synthesized by treatment of Si(OMe)4 with 2 molar equiv of citric acid and 2 molar equiv of N(n-Bu)3. The corresponding germanium analogue, tri(n-butyl)ammonium bis[citrato(3-)-O1,O3,O6]germanate (5; structurally characterized by single-crystal X-ray diffraction), was obtained analogously, starting from Ge(OMe)4. Upon dissolution in water, the lambda6Si-silicate dianion of 1 hydrolyzes spontaneously (formation of Si(OH)4 and citric acid), whereas the lambda6Ge-germanate dianion of 5 was found to be stable in water. Aqueous "solutions" of 1, with concentrations that are significantly higher than the saturation concentration of Si(OH)4, look absolutely clear over a period of several weeks; however, in reality, these solutions are sols with very small particles that slowly grow with time and finally form a gel that precipitates. This sol-gel process was monitored by small-angle neutron scattering (SANS). For reasons of comparison, an aqueous solution of the hydrolytically stable germanium compound 5 was also studied by the SANS technique.

Journal Article↗

PubMed2005

Binding of sodium dodecyl sulfate and hexaethylene glycol mono-n-dodecyl ether to the block copolymer L64: electromotive force, microcalorimetry, surface tension, and small angle neutron scattering investigations of mixed micelles and polymer/micellar surfactant complexes.

The interactions of sodium dodecyl sulfate (SDS) with the triblock copolymer L64 (EO13-PO30-EO13) and hexaethylene glycol mono-n-dodecyl ether (C12EO6) were studied using electromotive force, isothermal titration microcalorimetry, differential scanning microcalorimetry, and surface tension measurements. In certain regions of binding, mixed micelles are formed, and here we could evaluate an interaction parameter using regular solution theory. The mixed micelles of L64 with both SDS and C12EO6 exhibit synergy. When L64 is present in its nonassociated state, it forms polymer/micellar SDS complexes at SDS concentrations above the critical aggregation concentration (cac). The cac is well below the critical micellar concentration (cmc) of pure SDS, and a model suggesting how bound micelles are formed at the cac in the presence of a polymer is described. The interaction of nonassociated L64 with C12EO6 is a very rare example of strong binding between a nonionic surfactant and a nonionic polymer, and C12EO6/L64 mixed micelles are formed. We also carried out small angle neutron scattering measurement to determine the structure of the monomeric polymer/micellar SDS complex, as well as the mixed L64/C12EO6 aggregates. In these experiments, contrast matching was achieved by using the h and d forms of SDS, as well as C12EO6. During the early stages of the formation of polymer-bound SDS micelles, SDS aggregates with aggregation numbers of approximately 20 were found and such complexes contain 4-6 bound L64 monomers. The L64/C12EO6 data confirmed the existence of mixed micelles, and structural information involving the composition of the mixed micelle and the aggregation numbers were evaluated.

Journal Article↗

PubMed2004

Nanostructure in block copolymer solutions: rheology and small-angle neutron scattering.

Triblock copolymers composed of poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO) present an amphiphilic character in aqueous solutions. Since PPO is less hydrophilic than PEO and since their solubilities decrease when the temperature increases, the copolymers self-assemble spontaneously, forming micelles at moderate temperatures. For higher temperatures or concentrations, the copolymers or the micelles are ordered because of repulsive interactions and form lyotropic liquid crystalline phases. These are phases of very great viscosity with the aspect of gels, and transitions between different crystalline phases can occur at fixed concentration during an increase of temperature. We studied solutions of three different copolymers. The first two have a star structure. They are both composed of four branches (EO)x (PO)y fixed on an ethylene diamine, but differ by the values of x and y . Their commercial name is Tetronic 908 (x=114, y=21) and Tetronic 704 (x=16, y=18) . The third copolymer (EO)37(PO)56(EO)37 is linear and is known under the name of Pluronic P105 . The measurements of the shear complex elastic modulus according to the temperature is used to determine the temperatures of the different transitions. Then, small-angle neutron scattering on samples under flow and true crystallographic arguments make it possible to identify the nature of the crystalline phases. For the systems studied, we show that the branched copolymers form only one type of liquid crystalline phase, which is bcc for the T908 and lamellar for the T704 . For the linear copolymer, it is possible to identify three transitions: micellar solution to hexagonal phase, hexagonal phase to body-centered cubic phase, and finally body-centered cubic phase to lamellar phase.

Journal Article↗

PubMed1986

Deuterium incorporation into Escherichia coli proteins. A neutron-scattering study of DNA-dependent RNA polymerase.

Neutron small-angle scattering studies of single protein subunits in a protein-DNA complex require the adjustment of the neutron scattering-length densities of protein and DNA, which is attainable by specific deuteration of the protein. The neutron scattering densities of unlabelled DNA and DNA-dependent RNA polymerase of Escherichia coli match when RNA polymerase is isolated from cells grown in a medium containing 46% D2O and unlabelled glucose as carbon source. Their contrasts vanish simultaneously in a dialysis buffer containing 65% D2O. An expression was evaluated which allows the calculation of the degree of deuteration and match point of any E. coli protein from the D2O content of the growth medium, taking the 2H incorporation into RNA polymerase amino acids to be representative for all amino acids in E. coli proteins. The small-angle scattering results, on which the calculation of the degree of deuteration is based, were confirmed by mass spectrometric measurements.

DNA-Directed RNA Polymerases↗

PubMed2004

Binding of sodium dodecyl sulfate to linear and star homopolymers of the nonionic poly(methoxyhexa(ethylene glycol) methacrylate) and the polycation poly(2-(dimethylamino)ethyl methacrylate): electromotive force, isothermal titration calorimetry, surface tension, and small-angle neutron scattering measurements.

We investigated the binding of sodium dodecyl sulfate (SDS) to various linear and star polymers of the nonionic methoxyhexa(ethylene glycol) methacrylate (PMHEGMA) and the ionic 2-(dimethylamino)ethyl methacrylate (PDMAEMA), the latter being a polycation at low pH. The dodecyl sulfate ion selective electrode (EMF), isothermal titration calorimetry (ITC), and surface tension (ST) were applied to gain detailed information about interactions. In all cases there is evidence of significant binding of SDS over an extensive SDS concentration range spanning from ca. 10(-6) to 0.1 mol dm(-3). At pH 3, the polymer PDMAEMA is a strong polycation and here the binding is dominated by electrostatic 1:1 charge neutralization with the anionic surfactant. At their natural pH of 8.6, PMHEGMA and PDMAEMA polymers are essentially nonionic and bind SDS in the form of polymer-bound aggregates in the concentration range of ca. 1 x 10(-3) to 3 x 10(-2) mol dm(-3). All the polymers also bind SDS to a lesser extent at concentrations below 1 x 10(-3) mol dm(-3) reaching as low as 10(-7) mol dm(-3). This low concentration binding process involves the polymer and nonassociated SDS monomers. As far as we are aware, this is the first example that such a low concentration noncooperative binding process could be observed in SDS/neutral polymer systems by EMF and ST. We also showed that the nonionic surfactant hexa(ethylene glycol) mono-n-dodecyl ether (C12EO6) and the cationic cetyltrimethylammonium bromide (C16TAB) interact with star PDMAEMA. We believe that the interaction of C12EO6 and CTAB is of similar noncooperative type as the first SDS binding process in the range from ca. 10(-5) to 0.3 x 10(-3) mol dm(-3). At the high concentration binding limit Csat of SDS, the above polymers become fully saturated with bound SDS micelles. We applied small angle neutron scattering (SANS) to determine the structure and aggregation numbers of the star polymer/bound SDS micelles and calculated the stoichiometry of such supramolecular complexes. The SANS data on PDMAEMA star polymers in the presence of C12EO6 showed only a limited monomer binding in contrast to linear PDMAEMA, which showed monomer C12EO6 binding at low concentrations but micellar aggregates at 6 x 10(-3) mol dm(-3).

Journal Article↗

PubMed1988

Temperature dependence of the structure of aggregates of tobacco mosaic virus protein at pH 7.2. Static synchrotron small-angle X-ray scattering.

The small-angle X-ray scattering (SAXS) method using a synchrotron radiation source was applied to the study of the self-aggregation process of tobacco mosaic virus protein (TMVP) at a concentration of 5.0 or 12.0 mg ml-1 in 50 mM or 100 mM-phosphate buffer (ionic strengths approx. 0.1 and 0.2, respectively) at pH 7.2 in the temperature region of 4.8 to 25.0 degrees C. This paper presents the results of static measurements of SAXS. Sedimentation velocity experiments were performed simultaneously under the same conditions. These results are qualitatively parallel to those of the SAXS measurements, although the size of stacked disks derived from the SAXS measurements is larger than that derived from the sedimentation experiments, suggesting a change in the equilibrium conditions in the centrifugal field. Qualitative analysis of the SAXS data with model simulation calculations implies that the aggregation of TMVP consists of two steps: (1) the aggregation of A-protein comprising a few subunits to form double-layered disks; and (2) the random polymerization of double-layered disks by disk-stacking. Increase in temperature, ionic strength or protein concentration induced TMVP to polymerize to form a double-layered disk or a quadruple-layered short rod with consumption of A-proteins, accompanied by a small number of multi-layered short rods. The SAXS results indicate that the A-protein and the multilayered short rods are polydisperse with respect to size and shape, i.e. the mixture of A-protein, double-layered disks and multi-layered short rods coexists in the equilibrium state without pressure-induced partial dissociation of TMPV as observed during normal ultracentrifugation, and even under solution conditions in which the formation of double-layered disks or higher-order aggregates is favored.

Capsid Proteins↗

PubMed1984

A study of an infected bone tissue (osteomyelitis) by small-angle X-ray scattering.

The small-angle X-ray scattering method has been applied to evaluate various macromolecular parameters such as the specific inner surface, the transversal lengths, the length of crystallinity, the range of amorphous zone and the percentage of porosity in pure human bone and osteomyelitis, an infection of bone tissue. The hydroxyapatite crystals of bone being uniformly dispersed throughout the hydrated collagenous matrix creating a large mineral matrix interface, we found the bone samples to behave as a densely packed two phase system. The theories of Kratky and Porod have been utilized to evaluate the macromolecular parameters. These findings may shed light on tertiary structural deformation of human bone when it is infected.

Bone and Bones↗

PubMed1988

Micellar structure of beta-casein observed by small-angle X-ray scattering.

The small-angle X-ray scattering was observed from beta-casein micelles in 0.2 M phosphate buffer (pH 6.7) with varying temperatures. An oblate ellipsoid of a rigid core with a thin soft layer was proposed as a probable model of the beta-casein micellar structure, according to the results of the model optimization with simple triaxial bodies. Here the axial ratio was found to decrease and the micelle to become spherical when the polymerization proceeds with temperature. The consistency of the present model was examined with the results of hydrodynamic measurements published previously.

Algorithms↗