Werner Mayke, Heil Andreas, Rothermel Niels, Breitzke Hergen, Groszewicz Pedro Braga, Thankamony Aany Sofia, Gutmann Torsten, Buntkowsky Gerd
Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
Eduard-Zintl-Institute of Inorganic and Physical Chemistry, Technical University of Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
Solid State Nucl Magn Reson. 2015 Nov;72:73-8. doi: 10.1016/j.ssnmr.2015.09.008. Epub 2015 Sep 18.
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.
本文介绍了基于二氧化硅的有机-无机杂化材料的成功合成及固态核磁共振表征。为此，将类胶原肽固定在羧基官能化的介孔二氧化硅（COOH/SiOx）材料上。用TSTU（O-(N-琥珀酰亚胺基)-N,N,N',N'-四甲基脲四氟硼酸盐）对二氧化硅材料进行预活化，以使肽与连接体共价结合。TSTU部分的(13)C CP-MAS NMR信号降低表明共价固定成功。通过(15)N CP-MAS动态核极化（DNP）可以对共价结合的肽和吸附的肽进行定性区分。肽N端的(15)N信号的低场位移清楚地将其识别为结合位点。DNP增强使得能够探测天然丰度的(15)N核，无需对肽进行昂贵的标记。
