title: Synthesis and solid state NMR characterization of novel peptide/silica hybrid materials.
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.
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Mayke
authors.initials: M
authors.lastname: Werner
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Andreas
authors.initials: A
authors.lastname: Heil
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Niels
authors.initials: N
authors.lastname: Rothermel
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Hergen
authors.initials: H
authors.lastname: Breitzke
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Pedro Braga
authors.initials: PB
authors.lastname: Groszewicz
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
authors.forename: Aany Sofia
authors.initials: AS
authors.lastname: Thankamony
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany. Electronic address: gutmann@chemie.tu-darmstadt.de.
authors.forename: Torsten
authors.initials: T
authors.lastname: Gutmann
authors.affiliation: Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany. Electronic address: gerd.buntkowsky@chemie.tu-darmstadt.de.
authors.forename: Gerd
authors.initials: G
authors.lastname: Buntkowsky
mesh_terms: D002264:Carboxylic Acids / Q000737:chemistry; D060326:Chemistry Techniques, Synthetic; D003094:Collagen / Q000737:chemistry; D055767:Immobilized Proteins / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy; D009842:Oligopeptides / Q000138:chemical synthesis* / Q000737:chemistry*; D016062:Porosity; D012822:Silicon Dioxide / Q000737:chemistry*
chemical_list: D002264:Carboxylic Acids; D055767:Immobilized Proteins; D009842:Oligopeptides; D012822:Silicon Dioxide; D003094:Collagen
keywords: (15)N CP-MAS NMR; Bio-active silica; Collagen; Collagen-like peptides; DNP; Grafting; Immobilization; Natural abundance; SBA-15