Journal
STEROIDS
Volume 69, Issue 1, Pages 43-50Publisher
ELSEVIER SCIENCE INC
DOI: 10.1016/j.steroids.2003.09.012
Keywords
steroids; stigmasterol; 5,22-stigmastadien-3 beta-ol; NMR spectroscopy; selective NMR experiments; DPFGSE; COSY; TOCSY; NOESY
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The applicability of homonuclear gradient enhanced NMR experiments is demonstrated in the structure determination of steroid derivatives using stigmasterol as a model compound. High resolution H-1 NMR spectra of steroids very often display well resolved multiplets usually in the low-field region, and these signals can be used as starting points in several selective NMR experiments to study scalar (J coupling), and dipolar (NOE) interactions. Selective excitation was carried out using a double pulsed-field gradient spin-echo sequence (DPFGSE) in which 180degrees Gaussian pulses are sandwiched between sine shaped z-gradients. Scalar interactions were studied by homonuclear DPFGSE-COSY, DPFGSE-relay-COSY and DPFGSE-TOCSY experiments, while DPFGSE-NOESY was used to monitor spatial environment of the selectively excited proton. These methods provided unambiguous assignments for signals of the main skeleton and the side-chain of the steroid molecule. In addition, they allowed determination of the conformationally important homonuclear proton-proton coupling constants (J). (C) 2003 Elsevier Inc. All rights reserved.
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