Solid-state C-13{F-19} rotational-echo double-resonance (REDOR) NMR was used to locate [24-C-13]cholic acid that had been absorbed by nanoparticles with a core-shell morphology. The nanoparticles were composed of poly(4-fluorostyrene)-block-poly(acrylic acid) copolymers in which 15% of the poly(acrylic acid) shell functionality had been cross-linked with 2,2'-(ethylenedioxy)bis(ethylamine). The REDOR data were consistent with no cholic acid in the core, approximately 28% located at or near the core-shell interface, and the remaining 72% of the cholic acid farther than 25 Angstrom from the interface.