The physicochemical properties of soft nanoparticles, most notably size, morphology, and ligand interactions, typically depend upon the solution environment in which they are suspended. Comprehensive characterization in a given environment is therefore essential. We have employed high-resolution solution nuclear magnetic resonance (NMR) spectroscopy, nuclear spin relaxation measurements, and diffusion ordered NMR spectroscopy (DOSY) techniques to thoroughly characterize polymeric nanoparticles formed by salt-induced collapse of a methacrylic acid–ethyl acrylate copolymer stabilized by ultraviolet (UV) irradiation. UV-dose-dependent production of new chemical species is apparent from 1H and 13C chemical shift patterns. 1H–13C correlation spectroscopy reveals that cross-linking is likely responsible for nanoparticle structural integrity. Paramagnetic relaxation enhancement (PRE) unambiguously shows protection of photochemically derived moieties from solvent, with a UV-dose-dependent decrease in particle siz...
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