ABSTRACT
In this chapter, nuclear magnetic resonance (NMR) experiments related to structure elucidation are described, particularly as it relates to LC–NMR spectra. Typically, LC–NMR samples contain significant amounts of proteo solvent. Because these solvent signals are large relative to the peaks of interest, the solvent signals need to be suppressed. Solvent-suppression techniques, including WETDC, are described along with the fundamental NMR experiments used in structure elucidation. These NMR experiments include COSY, ROESY, NOESY, TOCSY, HSQC, HMQC, and HMBC. Decoupling techniques such as WALTZ and GARP are discussed along with relative preferences for use. Discussion of nuclear Overhauser effect (NOE) experiments and appropriate procedures for conducting and processing NOESY and ROESY experiments are presented. NOE analyses of conformational exchange, spin diffusion and conformational distance determination are presented.
