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Register a new userSelf-dispersion of Two Natural Polysaccharides for Granular Composites
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We envision that dispersion between two polymeric materials on mesoscales would create new composites with properties that are much more superior to the components alone. Here we elucidate the dispersion between two of most abundant natural polysaccharides, starch and chitosan, which form mesoscale composites that may promise many applications. By using X-ray microscopic imaging, small-angle X-ray scattering, and differential scanning calorimetry, we were able to characterize the interactions of chitosan and starch in the mesoscale composites. The morphology of the composite is far more complex from the simple mixture of starch granules with a nominal size of a few micrometers and chitosan microbundles of tens and hundreds of micrometers. This unique morphology can only be explained by the enhanced miscibility of chitosan in a starch granular matrix. It is evidenced that there is a possible ionic interaction between the amino group in chitosan and the hydroxyl groups in starch granules. Despite the limited solubility of chitosan in water, this ionic interaction allows for the disassembly of chitosan microbundles within the starch suspension. The result is a chemically stronger and more stable granular composite formed by two biocompatible and biodegradable polysaccharide polymers. The mechanism of chitosan to disperse throughout starch granules has implications for the application of chitosan in water and other solvents.
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EXSY, TOCSY and NOESY lie at the foundation of homonuclear NMR experiments in organic and pharmaceutical chemistry, as well as in structural biology. Limited magnetization transfer efficiency is an intrinsic downside of these methods, particularly when targeting rapidly exchanging species such as labile protons ubiquitous in polysaccharides, sidechains and backbones of proteins, and in bases and sugars of nucleic acids: the fast decoherence imparted on these protons through solvent exchanges, greatly reduces their involvement in homonuclear correlation experiments. We have recently discussed how these decoherences can be visualized as an Anti-Zeno Effect, that can be harnessed to enhance the efficiency of homonuclear transfers within Looped PROjected SpectroscopY (L-PROSY) leading to 200-300% enhancements in NOESY and TOCSY cross-peaks for amide groups in biomolecules. This study demonstrates that even larger sensitivity gains per unit time, equivalent to reductions by several hundred-folds in the duration of experiments, can be achieved by looping inversion or using saturation procedures. In the ensuing experiments a priori selected frequencies are encoded according to Hadamard recipes, and subsequently resolved along the indirect dimension via linear combinations. Magnetization-transfer (MT) processes reminiscent of those occurring in CEST provide significant enhancements in the resulting cross-peaks, in only a fraction of acquisition time of a normal 2D experiment. The effectiveness of the ensuing three-way polarization transfer interplay between water, labile and non-labile protons was corroborated experimentally for proteins, homo-oligosaccharides and nucleic acids. In all cases, cross-peaks barely detectable in conventional 2D NMR counterparts, were measured ca. 10-fold faster and with 200-600% signal enhancements by the Hadamard MT counterparts.
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