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Current Research on HRMAS:

J Pept Sci. 2003 Jan;9(1):47-53. Related Articles, Links

HRMAS NMR observation of beta-sheet secondary structure on a water swollen solid support.

Rousselot-Pailley P, Boutillon C, Wieruszeski JM, Lippens G.

UMR 8525 CNRS-Institut de Biologie de Lille-Universite de Lille II and Institut Pasteur de Lille, 1 rue du Professeur Calmette, BP447, 59021 Lille Cedex, France.

In this paper HRMAS NMR was used to investigate whether peptides on a peptidyl resin swollen in aqueous solution can adopt an intramolecular beta-sheet structure. A model peptide YQNPDGSQA, that was previously shown to adopt such a secondary structure in solution, (Blanco et al, J. Am. Chem. Soc., 1993) was grafted onto three different solid supports that swell in aqueous solution to examine the influence of the resin on the structure. Both parameters of resin loading and pH inside the swollen peptidyl resin proved to be important for the physicochemical behaviour of the peptide on the support.

Proceedings of the 15th European Experimental NMR Conference (EENC 2000)

12-17 June 2000, University of Leipzig, Germany

Using HRMAS in mesoporous materials

Christina Sizun*a, Jésus Rayaa, Karim Elbayeda, Anne Boosb, Amarawan Intasirib aInstitut Le Bel, UMR 7510 CNRS-Bruker-Université Louis Pasteur, Strasbourg bLaboratoire de Chimie Analytique et Minérale, UMR 7512, Ecole de Chimie des Polymères et Matériaux, Strasbourg


High Resolution Magic Angle Spinning (HRMAS) provides a powerful tool for the study of molecules bound to solid supports like resins or polymers, or soft materials such as lipids or physiological tissues. The averaging of the residual dipole interactions leads to spectra are of nearly liquid state quality. We show that HRMAS can also be applied in the case of the template surfactants in mesoporous silica gels before the final calcination step. Leaving the surfactants inside the pores could provide new applications in the domain of mesoporous materials, linked to the chemical properties of the organic part of the gels. HRMAS could help to fully characterize those materials during the various steps of synthesis. 29Si, 13C or 1H MAS NMR are valuable characterization methods for calcined and non-calcined silica materials. However, solid state MAS NMR yields limited information about the surfactants or adsorbed molecules, owing to non-quantitative low-resolution spectra. High resolution spectra have been obtained by adding an appropriate solvent. 1D and 2D NMR experiments allowed a more detailed investigation of the surfactants and their interactions with the silica surface. Recoupling of the static dipolar interaction by rotational resonance experiments was performed between protons belonging to different types of surfactants. The results obtained by HRMAS for two types of silica gels will be presented.

Ex vivo HRMAS MRS Analysis of Intact Tissue at Slow Sample Spinning Rates

Jennifer L. Taylor, A. Bielecki, C-L. Wu, R. G. Gonzalez, L. L. Cheng

Massachusetts General Hospital, Harvard Medical School, Massachusetts Institute of Technology, Boston, MA, USA


Photo by Shaoxiong Wu, Lake Taheo, CA,  October,  2003

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