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PubMed2006

Cosolvent effects on the micellization of oxyphenyl(copoly)ethylene oxide copolymers in aqueous solution.

In the present paper, we have analyzed how the presence of ethanol affects the micellization process of two structurally related polyoxyethylene block copolymers with diblock and triblock architectures (diblock, S15E63; triblock, E67S15E67) and the same hydrophobic block length, formed by oxyphenylethylene units, through surface tension, static and dynamic light scattering, density, ultrasound velocity, transmission electron microscopy, and steady-state fluorescence techniques. E and S denote the oxyethylene (-OCH2CH2) and oxyphenylethylene (-OCH2CH(C6H5)) units, respectively, and the subscripts the block length. The effect of increasing amounts of ethanol in solution gives rise to a progressive disruption of the micelle structures formed by these copolymers, with an increase in the critical micelle concentration (cmc) values and a decrease in the micellar aggregation number. This originated from the deswelling of the poly(ethylene oxide) (PEO) chains due to a decrease of the water content, accompanied by a reduction of the solvophobicity and an increase of the solubility of the S blocks, causing the lowering of the interfacial tension between the polyoxyphenylethylene core and the solvent, and favoring the swelling of hydrophobic blocks. Therefore, to achieve thermodynamic equilibrium, the micelle size should be smaller. A model derived from small angle neutron scattering (SANS) data is also applied to get extra information on micelle structure. With the aim of obtaining information about the hydration of micellar solutions of these block copolymers, compressibility and fluorescence data were collected. The increase of compressibility with ethanol addition confirms the swelling of the hydrophobic polyoxyphenylethylene chains. Fluorescence data show that the addition of ethanol to the solution decreases the polarity, favoring the solubilization of the oxyphenylethylene chains in the mixed solvent as single monomers. Aggregation data derived from this technique are in fair agreement with those obtained from light scattering.

Journal Article↗

PubMed2002

Complexities in ETS-domain transcription factor function and regulation: lessons from the TCF (ternary complex factor) subfamily. The Colworth Medal Lecture.

The ETS-domain transcription factor family can be divided into a series of subfamilies. Elk-1 represents the founding member of the ternary complex factor (TCF) subfamily. By focusing on the TCF subfamily, we can demonstrate the complexities that exist in the function and regulation of ETS-domain transcription factors. This article focuses on Elk-1 in detail and summarizes the functions of other TCFs. The key themes covered include the domain structure of the TCFs, the mechanisms of complex formation with serum response factor, regulation of TCFs by mitogen-activated protein kinase cascades, and transcriptional regulatory properties of the TCFs. Finally, the emerging role of the TCFs in vivo is discussed. A picture is developing indicating that, while these proteins exhibit significant sequence and functional conservation, key differences in their structure and regulation are being identified which may relate to unique functions of these proteins in vivo.

Amino Acid Sequence↗

PubMed1994

Structural characterization of the micelle-vesicle transition in lecithin-bile salt solutions.

Small-angle neutron scattering (SANS) and dynamic light scattering (QLS) are used to characterize the aggregates found upon dilution of mixed lecithin-bile salt micelles. Molar ratios of lecithin (L) to taurocholate (TC) studied varied from 0.1 to 1, and one series contained cholesterol (Ch). Mixed aggregates of L and taurodeoxycholate (TDC) at ratios of 0.4 and 1 were also examined. In all cases the micelles are cylindrical or globular and elongate upon dilution. The radius of the mixed micelles varies only slightly with the overall composition of lecithin and bile salt which indicates that the composition of the cylindrical micelle body is nearly constant. The transition from micelles to vesicles is a smooth transformation involving a region where micelles and vesicles coexist. SANS measurements are more sensitive to the presence of two aggregate populations than QLS. Beyond the coexistence region the vesicle size and degree of polydispersity decrease with dilution. Incorporation of a small amount of cholesterol in the lipid mixture does not affect the sequence of observed aggregate structures.

Bile Acids and Salts↗

PubMedDate not supplied

[Structural polymorphism of the liquid-crystalline dispersions formed from the double-stranded DNA molecules complexed with synthetic polycations].

The double-stranded, linear DNA molecules form the liquid-crystalline dispersions (LCD) in water-salt solutions containing positively charged polyconidin molecules. It was established from the analysis of the absorption spectra of the LCDs formed from (DNA-polyconidin) complexes, that the mean size of the particles of these dispersions is equal to -6000 angstroms. The small-angle X-ray data show, that in the LCD particles different density of packing of the (DNA-polycation) complexes is realized. The comparison of the X-ray data of the liquid-crystalline phases of (DNA-polyconidin) complexes formed under various conditions with the phase diagram, that reflects the polymorphism of the linear double-stranded DNA liquid crystals, demonstrates that the hexagonal mode of the LCD packing is existing in 0.15-0.4 M NaCl solutions, whereas in 0.4-0.55 M NaCl solutions-- the cholesteric one. As a result of specific spatial organization the cholesteric LCD possesses of an abnormal optical activity in the CD spectrum. The similar situation takes place in the case of another synthetic polycation--poly(2,5-ionen), whose chemical structure differs from that of polyconidin. Thus, the structural polymorphism of the (DNA-polyconidine) LCDs was evidenced. It means that change of NaCl concentration opens a gate to control the spatial packing of the molecules of (DNA-polycation) complexes in the particles of LCDs. The supposition about mechanism of formation of the DNA cholesteric liquid-crystalline state in the narrow interval of NaCl concentrations was suggested.

DNA↗

PubMed1996

Probing self assembly in biological mixed colloids by SANS, deuteration, and molecular manipulation.

Small-angle neutron scattering was used to obtain information on the form and molecular arrangement of particles in mixed colloids of bile salts with phosphatidylcholine, and bile salts with monoolein. Both types of systems showed the same general characteristics. The particle form was highly dependent on total lipid concentration. At the highest concentrations the particles were globular mixed micelles with an overall size of 50A. As the concentration was reduced the mixed micelles elongated, becoming rodlike with diameter about 50A. The rods had a radial core-shell structure in which the phosphatidylcholine or monoolein fatty tails were arranged radially to form the core with the headgroups pointing outward to form the shell. The bile salts were at the interface between the shell and core with the hydrophilic parts facing outward as part of the shell. The lengths of the rods increased and became more polydispersed with dilution. At sufficiently low concentrations the mixed micelles transformed into single bilayer vesicles. These results give insight on the physiological function of bile and on the rules governing the self assembly of bile particles in the hepatic duct and the small intestine.

Bile Acids and Salts↗

PubMed2006

Adsorption of simple gases in MCM-41 materials: the role of surface roughness.

This paper reports the development and testing of atomistic models of silica MCM-41 pores. Model A is a regular cylindrical pore having a constant section. Model B has a surface disorder that reproduces the morphological features of a pore obtained from an on-lattice simulation that mimics the synthesis process of MCM-41 materials. Both models are generated using a similar procedure, which consists of carving the pore out of an atomistic silica block. The differences between the two models are analyzed in terms of small angle neutron scattering spectra as well as adsorption isotherms and isosteric heat curves for Ar at 87 K and Xe at 195 K. As expected for capillary condensation in regular nanopores, the Ar and Xe adsorption/desorption cycles for model A exhibit a large hysteresis loop having a symmetrical shape, i.e., with parallel adsorption and desorption branches. The features of the adsorption isotherms for model B strongly depart from those observed for model A. Both the Ar and Xe adsorption branches for model B correspond to a quasicontinuous pore filling that involves coexistence within the pore of liquid bridges and gas nanobubbles. As in the case of model A, the Ar adsorption isotherm for model B exhibits a significant hysteresis loop; however, the shape of the loop is asymmetrical with a desorption branch much steeper than the adsorption branch. In contrast, the adsorption/desorption cycle for Xe in model B is quasicontinuous and quasireversible. Comparison with adsorption and neutron scattering experiments suggests that model B is too rough at the molecular scale but reproduces reasonably the surface disorder of real MCM-41 at larger length scales. In contrast, model A is smooth at small length scales in agreement with experiments but seems to be too ordered at larger length scales.

Journal Article↗

PubMed2006

Distinct kinetic pathways generate organogel networks with contrasting fractality and thixotropic properties.

The kinetics of the isothermal transformation of sols, comprised of a low molecular-mass organogelator (LMOG) and an organic liquid, to their organogel phases have been followed by circular dichroism (CD), fluorescence, small angle neutron scattering (SANS), and rheological methods. The thixotropic properties (in the sense that severe shearing followed by rest lead to reestablishment of viscoelasticity) of the gels have been examined as well by rheological measurements. The compositions of the samples were either 5alpha-cholestan-3beta-yl N-(2-naphthyl) carbamate (CNC) in an n-alkane (n-octane or n-dodecane) or 3beta-cholesteryl N-(2-naphthyl) carbamate (CeNC) in ethyl acetate. Values of Df, the mass fractal dimension of the microcrystalline self-assembled fibrillar networks (SAFINs) in the gels, have been extracted from the kinetic data using a model developed by Dickinson (J. Chem. Soc., Faraday Trans. 1997, 93, 111). The Df values, 1.1-1.3 for the CeNC gels and 1.3-1.4 or 1.6-1.8 (depending on the temperature of incubation of the sol phase) for CNC gels, are consistent with the gel network structures observed by optical microscopy. In addition, comparison of the temperature dependence of both n (the Avrami component) and K (the Avrami "rate constant") for CeNC/ethyl acetate gelation with those reported previously for gelation of CNC/n-alkane sols demonstrate that the very small change of a single bond in CNC to a double bond in CeNC causes significant differences in their gelation abilities and gel properties. The rheological measurements on CNC/n-alkane gels with spherulitic SAFIN units, formed by incubation of their sols at < or =28 degrees C, indicate that they are thixotropic. Gels with the same chemical composition but formed by incubation of their sols at > or =30 degrees C, leading to fiberlike SAFIN units, remain liquidlike after shearing regardless of the periods they are at rest. The time-dependent viscoelastic properties of the gel networks are treated according to a stretched exponential model. The observations from these studies provide detailed insights into the mechanisms of formation of molecular organogel phases and demonstrate the extreme sensitivity of the SAFINs and viscoelastic properties of such organogels to slight modifications in LMOG structure or sample history.

Journal Article↗

PubMed2001

Clipped random wave analysis of anisometric lamellar microemulsions.

Small-angle neutron scattering experiments were performed on C10E4-D2O-octane (where C10E4 is tetraethylene glycol monodecyl ether) anisometric microemulsions in the lamellar phase at a constant surfactant volume fraction of 20% and at the hydrophile-lipophile balance temperature of 22.5 degrees C. The results were analyzed using a clipped random wave model with a specific spectral distribution function developed by us previously. This enabled us to generate three-dimensional morphologies of the microemulsions, which showed clearly that in sufficiently anisometric microemulsions the oil-water interface was no longer connected. At large anisometry isolated regions of oil or water were found, and the transition from a bicontinuous structure at isometry to these isolated micelles far from isometry goes through an intermediate cylindrical morphology when the oil-to-water or water-to-oil ratio is around 4 to 1. We further computed the joint distribution function of the mean curvature H and Gaussian curvature K of the entire oil-water interface for each anisometric microemulsion. In particular, we show the distribution of , , and - (2) for different isolated regions within an oil-rich microemulsion at an oil-to-water ratio of 85% to 15%. These distributions allowed us to prove that the isolated regions formed in highly anisometric microemulsions were small and had spherical topology.

Journal Article↗

PubMed1999

Quantification of the fiber architecture and biaxial mechanical behavior of porcine intestinal submucosa.

Porcine small intestinal submucosa (SIS) has been shown to serve as a remodelable tissue scaffold in a wide range of applications. Despite the large number of experimental studies, there is a lack of fundamental information on SIS anisotropic mechanical behavior and how this behavior changes postimplantation. As a first step in our study of remodeling biomaterials, we performed biaxial mechanical testing to quantify the anisotropic mechanical behavior and used small-angle light scattering (SALS) to quantify the gross fiber structure of fresh, unimplanted SIS. Structural results indicate that SIS displays primarily a single, continuous preferred fiber direction oriented parallel to the long axis of the intestine. Occasionally, two distinct fiber populations oriented at approximately +/-28 degrees with respect to the longitudinal axis could be distinguished. Consistent with this structure, SIS exhibited a nonlinear, anisotropic mechanical response with higher stresses along the longitudinal axis. Further, the circumferential stress-strain response was strongly affected by the maximum longitudinal strain level, but the maximum circumferential strain level only weakly affected the longitudinal stress-strain response. This asymmetric mechanical coupling suggests strong mechanical interactions on a fiber level. SIS stress-strain response also was similar to glutaraldehyde-treated bovine pericardium, attesting to the substantial strength of SIS in the fresh, untreated state. The results of this study will provide a basis for a future analysis of the structural and mechanical changes during the remodeling process.

Algorithms↗

PubMed2006

Further characterization of theobroma oil-beeswax admixtures as lipid matrices for improved drug delivery systems.

There is an increasing interest in lipid based drug delivery systems due to factors such as better characterization of lipidic excipients and formulation versatility and the choice of different drug delivery systems. It is important to know the thermal characteristics, crystal habit, texture, and appearance of a new lipid matrix when determining its suitability for use in certain pharmaceutical application. It is line with this that this research was embarked upon to characterize mixtures of beeswax and theobroma oil with a view to applying their admixtures in drug delivery systems such as solid lipid nanoparticles and nanostructured lipid carriers. Admixtures of theobroma oil and beeswax were prepared to contain 25% w/w, 50% w/w, and 75% w/w of theobroma oil. The admixtures were analyzed by differential scanning calorimetry (DSC), small angle X-ray diffraction (SAXD), wide angle X-ray diffraction (WAXD), and isothermal heat conduction microcalorimetry (IMC). The melting behavior and microstructures of the lipid admixtures were monitored by polarized light microscopy (PLM). Transmission electron microscopy (TEM) was used to study the internal structures of the lipid bases. DSC traces indicated that the higher melting peaks were roughly constant for the different admixtures, but lower melting peaks significantly increased (p < 0.05). The admixture containing 25% w/w of theobroma oil possessed highest crystallinity index of 95.6%. WAXD studies indicated different reflections for the different lipid matrices. However, new interferences were detected for all the lipid matrix admixtures between 2theta = 22.0 degrees and 2theta = 25.0 degrees. The lipid matrices containing 50% w/w and 25% w/w of theobroma oil showed absence of the weak reflection characteristic of pure theobroma oil, while there was disappearance of the strong intensity reflection of beeswax in all the lipid matrix admixtures at all stages of the study. PLM micrographs revealed differences with regard to the thermal and optical behaviors depending on the composition of the matrix. The lipid matrix consisting of 75% w/w of theobroma oil showed a spherulite texture after 4 weeks of isothermal storage. Crystallization exotherms of lipid matrices containing 50% w/w and 25% w/w of theobroma oil showed change in modification after 30 min with the latter having a greater time-dependent crystallization. Generally, low non-integral Avrami exponents and growth rate constants were obtained for all the lipid matrices, with the admixture containing 25% w/w theobroma oil having the lowest Avrami exponent and growth rate constant. Based on the results obtained, admixtures containing 50% w/w and 75% w/w of theobroma oil could be applied in the formulation of solid lipid nanoparticles and nanostructured lipid carriers as these lipid matrices possessed crystal characteristics that favour such drug delivery systems.

Cacao↗

PubMed1985

Characterization of a half-molecular fragment obtained by reduction of human alpha 2-macroglobulin with dithiothreitol. A small-angle X-ray and neutron scattering investigation.

A half-molecular fragment of alpha 2-macroglobulin has been prepared by reducing and alkylating the inter-subunit disulfide bonds in the tetrameric alpha 2-macroglobulin molecule with 1 mM dithiothreitol (40 min) and 3 mM iodoacetamide (40 min). Further purification was made by gel chromatography and the homogeneous population of half-molecules has been characterized by the techniques of small-angle X-ray and neutron scattering. The radii of gyration found by the two methods are 57.0 and 58.0 A, respectively. The match point, obtained by neutron scattering from solutions with different H2O/D2O ratios, is at 43% D2O; the data are consistent with a particle having a higher scattering density at large distances from the particle centre. From the X-ray and neutron intensities scattered at zero angle, the specific volume was determined to be 0.73 cm3/g at +5 degrees C and the molecular weight to be 390,000; the latter value is associated with a relatively large error due to the uncertainty in the concentration determination. Shape analysis indicates that the best-fitting scattering-equivalent three-axial bodies are oblate shaped, with two of their axial dimensions about three to four times larger than the third one. From the volume of the best-fitting scattering-equivalent three-axial bodies, 0.72 X 10(6) A3, we obtain a water content equal to 0.38 g H2O/g protein (dry weight).

Dithiothreitol↗

PubMed1999

Association behavior of native beta-lactoglobulin.

The association behavior of beta-lactoglobulin has been studied by small-angle neutron scattering as a function of protein concentration, temperature, pH, and NaCl concentration of the solution. By indirect Fourier transformation of the spectra, pair-distance distribution functions for the various samples were obtained. These functions provided information on the maximum size, the weight-averaged molecular mass, and the z-averaged radius of gyration of the beta-lactoglobulin particles. At room temperature and pH values below 4 and above 5.2 the protein consists predominantly of monomers and dimers, consistent with literature. In these pH regimes the formation of dimers is favored upon increasing ionic strength and decreasing protein charge (pH values closer to the isoelectric point of the protein). Around pH 4.7, larger oligomeric structures are formed, enhanced by a decrease in temperature and a decrease in ionic strength. beta-Lactoglobulin A associates more strongly than beta-lactoglobulin B. Surprisingly, at pH 6.9 larger structures than dimers seem to be formed at high protein concentrations (> 30 mg mL-1).

Animals↗

PubMed1998

Optimal bovine pericardial tissue selection sites. I. Fiber architecture and tissue thickness measurements.

Use of bovine pericardium as an engineered biomaterial in the fabrication of bioprosthetic heart valves is limited, in part, by substantial intra- and intersac variations in its fibrous structure. To quantitatively assess this variability, we determined the fiber architecture of 20 whole BP sacs. Each sac was mounted on a prolate spheroidal mold, cleared and preserved in 100% glycerol, then sectioned into four equisized quadrants. This preparation method allowed for accurate intersac comparisons and minimized tissue distortions. The fiber architecture was evaluated by small-angle light scattering (SALS) using a 2.54-mm rectilinear grid resulting in approximately 1200 SALS measurements per quadrant, along with tissue thickness measured at 55 locations per quadrant. The fiber architecture was described in terms of fiber preferred directions, degree of orientation, and asymmetry of the fiber angular distribution. The BP sac fiber architecture demonstrated substantial intra- and intersac variability, with local fiber preferred directions changing by as much as 90 degrees within approximately 5 mm. Overall, most sacs revealed potential selection areas in the apex region characterized by a high degree of orientation, high uniformity in fiber preferred directions, and uniform tissue thickness. However, the size, location, and fiber orientation of these potential selection areas varied sufficiently from sac-to-sac to question whether anatomic location alone is sufficient for consistent localization of regions of high structural uniformity suitable for improved BHV design.

Animals↗

PubMed1998

Optimal bovine pericardial tissue selection sites. II. Cartographic analysis.

In Part I of this work we used small-angle light scattering (SALS) to quantify the fiber architecture of 20 bovine pericardial sacs, along with corresponding tissue-thickness measurements, to determine optimal material selection sites. In order to determine the anatomic consistency of these sites, the fiber architecture and thickness data from all 20 sacs were averaged together using a cartographic analysis method that took advantage of the geometry of the prolate spheroid mold used to process the sacs. Optimal selection sites were determined based on a local criteria where all fiber preferred directions within a 2.54-cm circular area were within +/- 10 degrees. The largest contiguous area (LCA) for the entire BP sac was 20.54 cm2, located in the vicinity of the left ventricle of the heart. The LCA tissue thicknesses were also relatively uniform, further supporting the use of these areas. However, even within these optimal areas there was a +/- 20 degrees standard deviation in local fiber preferred directions, resulting in at best a 40 degrees spread in local preferred directions. The observed structural variability may be due to regionally heterogeneous physiologic loadings induced by the ligamentous attachments. These attachments may alter the regional fiber preferred orientation to support local mechanical loadings. Overall, given the inherent structural variability of the BP sac, we conclude that use of anatomic location alone will not consistently guarantee the selection of tissue specimens with a highly homogeneous and predictable fibrous structure. It is thus suggested that a direct fiber measurement presorting method be employed when selecting BP specimens for bioprosthetic applications where tissue structural homogeneity and uniformity is critical.

Animals↗

PubMed1998

The aortic valve microstructure: effects of transvalvular pressure.

We undertook this study to establish a more quantitative understanding of the microstructural response of the aortic valve cusp to pressure loading. Fresh porcine aortic valves were fixed at transvalvular pressures ranging from 0 mmHg to 90 mmHg, and small-angle light scattering (SALS) was used to quantify the gross fiber structure of the valve cusps. At all pressures the fiber-preferred directions coursed along the circumferential direction. Increasing transvalvular pressure induced the greatest changes in fiber alignment between 0 and 1 mmHg, with no detectable change past 4 mmHg. When the fibrosa and ventricularis layers of the cusps were re-scanned separately, the fibrosa layer revealed a higher degree of orientation while the ventricularis was more randomly oriented. The degree of fiber orientation for both layers became more similar once the transvalvular pressure exceeded 4 mmHg, and the layers were almost indistinguishable by 60 mmHg. It is possible that, in addition to retracting the aortic cusp during systole, the ventricularis mechanically may contribute to the diastolic cuspal stiffness at high transvalvular pressures, which may help to prevent over distention of the cusp. Our results suggest a complex, highly heterogeneous structural response to transvalvular pressure on a fiber level that will have to be duplicated in future bioprosthetic heart valve designs.

Animals↗

PubMed2000

Mechanical evaluation and design of a multilayered collagenous repair biomaterial.

One method of fabricating implantable biomaterials is to utilize biologically derived, chemically modified tissues to form constructs that are both biocompatible and remodelable. Rigorous mechanical characterization is a necessary component in material evaluation to ensure that the constructs will withstand in vivo loading. In this study we performed an in-depth biaxial mechanical and quantitative structural analysis of GraftPatch (GP), a biomaterial constructed by assembling chemically treated layers of porcine small intestinal submucosa (SIS). The mechanical behavior of GP was compared to both native SIS and to glutaraldehyde-treated bovine pericardium (GLBP) as a reference biomaterial. Under biaxial loading, GP was found to be stiffer than native SIS and mechanically anisotropic, with the preferred fiber direction demonstrating greater stiffness. Quantitative structural analysis using small-angle light scattering indicated a uniform fiber structure similar to GLBP and SIS. To enable test-protocol-independent quantitative comparisons, the biaxial mechanical data were fit to an orthotropic constitutive model, which indicated a similar degree of mechanical anisotropy between the three groups. We also demonstrate how the constitutive model can be used to design layered biocomposite materials that can undergo large deformations.

Animals↗

PubMed2004

Dendrimers in solution: insight from theory and simulation.

A variety of experimental and theoretical approaches show that, akin to linear polymers, dendrimers in good solvent conditions are best described as flexible macromolecular aggregates with a dense core and fluctuating monomer groups. We present theoretical and simulational evidence of how the shape and inner structure of dendrimers depends on the generation number as well as the effective interactions that exist between dendrimers in solution. These approaches based on simplified dendritic structures show there is a tunable and ultrasoft interaction between the centers of the solublized dendrimers. Results from small-angle neutron scattering data confirm the theory and indicate that dendrimers are model systems of ultrasoft colloids that bridge the gap between polymers and hard spheres. Dendrimers can form a class of materials analogous to the related systems of star polymers and block copolymer micelles which exhibit special properties.

Journal Article↗

PubMed2004

Supramolecular self-assembly of conjugated diblock copolymers.

This paper describes the synthesis and characterization of a novel series of copolymers with different lengths of oligo(phenylene vinylene) (OPV) as the rod block, and poly(propylene oxide) as the coil block. Detailed characterization by means of transmission electron microscopy (TEM), atomic force microscopy (AFM), and small-angle neutron scattering (SANS) revealed the strong tendency of these copolymers to self-assemble into cylindrical micelles in solution and as-casted films on a nanometer scale. These micelles have a cylindrical OPV core surrounded by a poly(propylene glycol) (PPG) corona and readily align with each other to form parallel packed structures when mica is used as the substrate. A packing model has been proposed for these cylindrical micelles.

Journal Article↗