title: Exploring uncharted terrain in nature's structure space using capillary NMR spectroscopy: 13 steroids from 50 fireflies.
abstract: Capillary NMR spectroscopy (CapNMR) was used to characterize 13 new cardenolides and related steroids from a severely mass-limited natural products sample derived from a rare firefly, Lucidota atra. These analyses were carried out on only partially purified samples, each containing 20-100 mug of up to three steroids. Compared to other NMR spectroscopic techniques, CapNMR provided an up to 3-fold gain in sensitivity while maintaining very high spectral quality, which was essential for the identification of the L. atra steroids. We show that CapNMR allows for routine 1H and 13C NMR spectroscopic characterization of small molecule samples containing as little as 40 nmol of material.
authors.affiliation: Department of Chemistry, State University of New York at Cortland, Cortland, NY 13045, USA.
authors.forename: Matthew
authors.initials: M
authors.lastname: Gronquist
authors.forename: Jerrold
authors.initials: J
authors.lastname: Meinwald
authors.forename: Thomas
authors.initials: T
authors.lastname: Eisner
authors.forename: Frank C
authors.initials: FC
authors.lastname: Schroeder
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid; D001517:Coleoptera / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D013256:Steroids / Q000737:chemistry*
chemical_list: D013256:Steroids