Molecular structure of crude beeswax studied by solid-state (13)C NMR

(13)C Solid-state NMR experiments were performed to investigate the structure of beeswax in the native state (crude beeswax) for the first time. From quantitative direct polarization (13)C MAS NMR spectrum, it was found that the fraction of internal-chain methylene (int-(CH(2))) component compared to other components of crude beeswax was over 95%. The line shape of the int-(CH(2)) carbon resonance region was comprehensively analyzed in terms of NMR chemical shift. The (13)C broad peak component covering from 31 to 35ppm corresponds to int-(CH(2)) carbons with trans conformation in crystalline domains, whereas the sharp signal at 30.3 ppm corresponds to gauche conformation in the non-crystalline domain. From peak deconvolution of the aliphatic region, it was found that over 85% of the int-(CH(2)) has a crystal structure and several kinds of molecular packing for int-(CH(2)), at least three, exist in the crystalline domain. Abbreviation: / NMR: nuclear magnetic resonance int-(CH(2)): internal-chain methylene CP: cross-polarization MAS: magic angle spinning