The primary component of the amyloid plaques in Alzheimer's disease (AD) is a highly ordered fibril composed of the 39−43 amino acid peptide, β-amyloid (Aβ). The presence of this fibril has been correlated with both the onset and severity of the disease. Using a combination of synthetic model peptides, solid-state NMR, electron microscopy, and small angle neutron scattering (SANS), methods that allowed fibrils to be studied directly both in solution and in the solid state, the three-dimensional structure of fibrils formed from Aβ(10 - 35) is assigned. The structure consists of six laminated β-sheets propagating and twisting along the fibril axis. Each peptide strand is oriented perpendicular to the helical axis in a parallel β-sheet, with each like amino acid residue in register along the sheet. The six sheets are laminated, probably also in parallel arrays, to give a fibril with dimensions of about 60 × 80 Å. Both the methodology developed and the structural insight gained here lay the foundation for strategies to characterize and design materials capable of amyloid-like self-assembly.
We have measured both the static and dynamic structure factors of a single dendrimer with small-angle x-ray scattering ͑SAXS͒ and neutron spin-echo spectroscopy under good solvent conditions with the aim of finding a consistent correlation between the structural properties of dendrimers and their dynamic behavior. The samples under investigation were star-burst polyamidoamine dendrimers with generations gϭ0 to 8 in dilute methanol solutions. A model independent approach employing inverse Fourier transformation and square root deconvolution methods has been used to analyze the SAXS data to obtain the pair distance distribution function p(r) and the radial excess electron density profile ⌬ (r). In addition, we formulated a model that takes both the colloidal ͑globular, compact shape with form polydispersity or fuzzy surface͒ as well as the loose, polymeric ͑self-avoiding random walk͒ character of dendrimers into account. With this model we were able to describe the spectra of all dendrimer generations consistently. Parameters discussed as a function of the dendrimer generation are, among others, the correlation length of the density fluctuations ͑blob radius͒ , the radius of gyration R g , the sphere radius R s , the form polydispersity s or analogously, the width of the fuzzy surface region 2 f . Both the model-independent approach and the model fits reveal that at least down to the third generation the dendrimers exhibit a rather compact, globular shape. These findings are in agreement with the dynamic results obtained by NSE spectroscopy which probes length scales both larger and much smaller than the dimension of a single dendrimer. The method reveals that the dynamics throughout is dominated by the center-of-mass diffusion-the internal dynamics is suppressed. The diffusion coefficients obtained are close to the values calculated from the Stokes-Einstein relation using the sphere radius R s determined from the SAXS spectra. Dynamically, the dendrimers behave like ''hard'', solid spheres.
An efficient approach to the syntheses of amphiphilic rod-coil diblock and coil-rod-coil triblock copolymers was developed. Each diblock copolymer consists of a perfectly monodispersed oligo(phenylene vinylene) covalently bonded to a poly(ethylene glycol) block with a very low polydispersity (<1.05). The structure and basic physical properties of these copolymers were characterized by various spectroscopic techniques such as NMR, MALDI-TOF, GPC, DSC, UV/vis, and the fluorescence study. These diblock copolymers were shown to possess remarkable self-assembling abilities, and long cylindrical micelles (>1 µm) were formed. TEM, SANS, and AFM studies showed that the core of the micelles has a diameter of ∼8-10 nm and was composed of an OPV block. TEM and SANS studies revealed that these OPV-PEG micelles have a cylindrical OPV core surrounded by a PEG corona. Cryo-TEM and SANS studies indicate that fibers were formed even in very dilute THF/H 2 O solutions. Since the conjugated OPV blocks exhibit liquid crystallinity and electric and optical properties, these micelles are interesting for studying the electroactive effect in a nanometer scale.
The dynamics of phospholipids in unilamellar vesicles (ULVs) is of interest in biology, medical, and food sciences, since these molecules are widely used as biocompatible agents and a mimic of cell membrane systems. We have investigated the nanoscopic dynamics of 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) phospholipid in ULVs as a function of temperature using elastic and quasielastic neutron scattering (QENS). The dependence of the signal on the scattering momentum transfer, which is a critical advantage of neutron scattering techniques, allows the detailed analysis of the lipid motions that cannot be carried out by other means. In agreement with a differential scanning calorimetry measurement, a sharp rise in the elastic scattering intensity below ca. 296 K indicates a phase transition from the high-temperature fluid phase to the low-temperature solid gel phase. The microscopic lipid dynamics exhibits qualitative differences between the solid gel phase (in a measurement at 280 K) and the fluid phase (in a measurement at a physiological temperature of 310 K). The analysis of the data demonstrates the presence of two types of distinct motions: the entire lipid molecule motion within a monolayer, also known as lateral diffusion, and the relatively faster internal motion of the DMPC molecule. The lateral diffusion of the entire lipid molecule is Fickian in character, whereas the internal lipid motions are of localized character, which is consistent with the structure of the vesicles. The lateral motion slows down by an order of magnitude in the solid gel phase, whereas for the internal motion not only the time scale but also the character of the motion changes upon the phase transition. In the solid gel phase, the lipids are more ordered and undergo uniaxial rotational motion. However, in the fluid phase, the hydrogen atoms of the lipid tails undergo confined translation diffusion rather than uniaxial rotational diffusion. The translational, but spatially localized, diffusion of the hydrogen atoms of the lipid tails is a manifestation of the flexibility of the chains acquired in the fluid phase. Because of this flexibility, both the local diffusivity and the confinement volume for the hydrogen atoms increase in the linear fashion from near the lipid's polar headgroup to the end of its hydrophobic tail. Our results present a quantitative and detailed picture of the effect of the gel-fluid phase transition on the nanoscopic lipid dynamics in ULVs. The data analysis approach developed here has a potential for probing the dynamic response of lipids to the presence of additional cell membrane components.
The generation of bioethanol from lignocellulosic biomass holds great promise for renewable and clean energy production. A better understanding of the complex mechanisms of lignocellulose breakdown during various pretreatment methods is needed to realize this potential in a cost and energy efficient way. Here we use small-angle neutron scattering (SANS) to characterize morphological changes in switchgrass lignocellulose across molecular to submicrometer length scales resulting from the industrially relevant dilute acid pretreatment method. Our results demonstrate that dilute acid pretreatment increases the cross-sectional radius of the crystalline cellulose fibril. This change is accompanied by removal of hemicellulose and the formation of R(g) ∼ 135 A lignin aggregates. The structural signature of smooth cell wall surfaces is observed at length scales larger than 1000 A, and it remains remarkably invariable during pretreatment. This study elucidates the interplay of the different biomolecular components in the breakdown process of switchgrass by dilute acid pretreatment. The results are important for the development of efficient strategies of biomass to biofuel conversion.
Small-angle x-ray scattering (SAXS) patterns are recorded from thin breast tissue samples containing healthy and cancerous regions. The SAXS patterns are compared with histo-pathological observations. The information available from SAXS is reviewed, and a model for scattering from collagen is presented. Scattering patterns of collagen at regions far from the tumours are essentially different from those at tumours. The axial period of collagen fibrils is 65.0 +/- 0.1 nm in healthy regions, and 0.3 nm larger in cancer-invaded regions. The average intensity of scattering from cancerous regions is an order of magnitude higher than the intensity from healthy regions. This is interpreted to arise from an increase of the specific surface area of the scatterers, which is due to a disruption of the molecular and supra-molecular structures in cancerous regions and invasion of new types of cells. The differences of the SAXS patterns are large and distinctive enough to suggest that these phenomena may be utilized in mammography.
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