利用毛细管核磁共振波谱探索自然界结构空间中的未知领域：从50只萤火虫中获取的13种甾体化合物

Exploring uncharted terrain in nature's structure space using capillary NMR spectroscopy: 13 steroids from 50 fireflies.

作者信息

Gronquist Matthew, Meinwald Jerrold, Eisner Thomas, Schroeder Frank C

机构信息

Department of Chemistry, State University of New York at Cortland, Cortland, NY 13045, USA.

出版信息

J Am Chem Soc. 2005 Aug 10;127(31):10810-1. doi: 10.1021/ja053617v.

DOI:10.1021/ja053617v

PMID:16076169

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.

摘要

毛细管核磁共振波谱法（CapNMR）用于对从珍稀萤火虫 Lucidota atra 获得的严重受限的天然产物样品中的 13 种新强心苷及相关甾体进行表征。这些分析仅在部分纯化的样品上进行，每个样品含有 20 - 100 微克多达三种甾体。与其他核磁共振波谱技术相比，CapNMR 在保持非常高的光谱质量的同时，灵敏度提高了多达 3 倍，这对于鉴定 Lucidota atra 甾体至关重要。我们表明，CapNMR 能够对仅含 40 纳摩尔物质的小分子样品进行常规的 1H 和 13C 核磁共振波谱表征。