The three-dimensional structure of A-amylose crystals, as a model of the crystal domains of A-starch granules, was revised using synchrotron radiation microdiffraction data collected from individual micron-sized single crystals. The resulting datasets allowed a determination of the structure with conventional X-ray structure determination techniques normally used for small molecules and not for polymers. Whereas the gross features of this improved structure do not differ extensively from previous structure determination, the high resolution of the diffraction diagrams, which is unusual for a crystalline polymer, allowed the resolution of important new fine details. These include a distortion of the amylose double helices resulting from the occurrence of two intracrystalline molecules of water and a tight network of hydrogen bonds involving each of the primary and secondary hydroxyl groups of the glucosyl moieties. Pairs of water molecules are located in discrete pockets that do not interfere with one another. In addition, the refinement of the new structure indicates a "parallel-down" organization of the amylose molecules within the unit cell as opposed to the previous "parallel-up" model. This new feature indicates that within the crystals, the nonreducing ends of the amylose molecules are oriented toward the c-axis direction of the unit cell. The description of this geometry is important to correlate the crystallography of the granules of A-starch with their ultrastructure and their mode of biosynthesis.Here, we present for the first time the resolution of the structure of a polymer crystal from a full X-ray dataset collected on micron-sized polymer single crystals using synchrotron radiation microdiffraction. This achievement is a substantial advance, which opens the way to many more studies since the technique of growing polymer and biopolymer single crystals is well established.3
The structure of short dough and biscuit has been characterized at a macroscopic level (dimensions, bulk structure) and a microscopic level (starch damage, protein aggregates, microstructure) by physical and biochemical methods. The baking process of short dough induces a large decrease of the product bulk density from 1.26 to 0. 42 (+/-0.01) g.cm(-)(3) for final biscuit, leading to a cellular solid with a thin colored surface and a porous inner structure. Proteins appear aggregated in biscuit when compared to short dough, whereas starch granules remain almost intact in biscuits. The components which are involved in the cohesiveness of short dough and biscuit final structure have been identified. They suggest that short dough is a suspension of solid particles in a liquid phase being an emulsion of lipids in a concentrated sugar solution. The role of sugars in biscuit structure suggest that biscuit structure is a composite matrix of protein aggregates, lipids and sugars, embedding starch granules.
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