Two-dimensional heteronuclear 13C 1H chemical-shift correlation spectra were obtained for bovine high-density lipoprotein (HDL). The 13C and 1H shifts of the lipid components are assigned. No evidence for dynamic equilibration of lipid classes between different structure environments was found at this limited resolution. Heteronuclear correlation spectroscopy can be effectively applied to macromolecular complexes as large as HDLs.