AbstractIn this paper HRMAS NMR was used to investigate whether peptides on a peptidyl resin swollen in aqueous solution can adopt an intramolecular β‐sheet structure. A model peptide YQNPDGSQA, that was previously shown to adopt such a secondary structure in solution, (Blancoet 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. Copyright © 2003 European Peptide Society and John Wiley&Sons,