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  • Title: Synthesis and solid state NMR characterization of novel peptide/silica hybrid materials.
    Author: Werner M, Heil A, Rothermel N, Breitzke H, Groszewicz PB, Thankamony AS, Gutmann T, Buntkowsky G.
    Journal: Solid State Nucl Magn Reson; 2015 Nov; 72():73-8. PubMed ID: 26411982.
    Abstract:
    The successful synthesis and solid state NMR characterization of silica-based organic-inorganic hybrid materials is presented. For this, collagen-like peptides are immobilized on carboxylate functionalized mesoporous silica (COOH/SiOx) materials. A pre-activation of the silica material with TSTU (O-(N-Succinimidyl)-N,N,N',N'-tetramethyluronium tetrafluoroborate) is performed to enable a covalent binding of the peptides to the linker. The success of the covalent immobilization is indicated by the decrease of the (13)C CP-MAS NMR signal of the TSTU moiety. A qualitative distinction between covalently bound and adsorbed peptide is feasible by (15)N CP-MAS Dynamic Nuclear Polarization (DNP). The low-field shift of the (15)N signal of the peptide's N-terminus clearly identifies it as the binding site. The DNP enhancement allows the probing of natural abundance (15)N nuclei, rendering expensive labeling of peptides unnecessary.
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