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Application of capillary‐scale NMR for the structure determination of phytochemicals
Author(s) -
Hu JinFeng,
Garo Eliane,
Yoo HyeDong,
Cremin Peadar A.,
Zeng Lu,
Goering Matt G.,
O'NeilJohnson Mark,
Eldridge Gary R.
Publication year - 2005
Publication title -
phytochemical analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.574
H-Index - 72
eISSN - 1099-1565
pISSN - 0958-0344
DOI - 10.1002/pca.831
Subject(s) - chemistry , homonuclear molecule , natural product , dept , heteronuclear single quantum coherence spectroscopy , two dimensional nuclear magnetic resonance spectroscopy , nmr spectra database , carbon 13 nmr , proton nmr , analytical chemistry (journal) , nuclear magnetic resonance spectroscopy , chromatography , stereochemistry , spectral line , organic chemistry , molecule , physics , astronomy
Employing a capillary‐scale NMR probe enables the miniaturisation of structure determination and de‐replication of purified natural products from plants using only 5–100 µg of material. Approximately 5 µg are required to perform one‐dimensional proton and two‐dimensional homonuclear (COSY and NOESY) NMR experiments; some 30 µg are needed to acquire HMQC‐ or HSQC‐NMR spectra; ca. 75–100 µg are necessary to measure HMBC‐NMR spectra; and around 200 µg of a compound are needed to perform 13 C‐ and DEPT‐NMR experiments. In order to illustrate the integration of the outputs from high‐throughput natural product chemistry methods with the capabilities of the state‐of‐the‐art CapNMR™ technology, the preparation of a natural product library from the extract of Penstemon centranthifolius , and the subsequent isolation, purification and structure determination of six known iridoid glycosides with 25–300 µg of material are presented. Copyright © 2005 John Wiley & Sons, Ltd.

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