Premium
Applications of Two‐Dimensional 1 H NMR Methods to Photo‐Chemically Induced Dynamic Nuclear Polarisation Spectroscopy
Author(s) -
Stob Sijtze,
Scheek Ruud M.,
Boelens Rolf,
Dukstra Klaas,
Kaptein Robert
Publication year - 1988
Publication title -
israel journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.908
H-Index - 54
eISSN - 1869-5868
pISSN - 0021-2148
DOI - 10.1002/ijch.198800043
Subject(s) - cidnp , chemistry , two dimensional nuclear magnetic resonance spectroscopy , spectroscopy , pulse sequence , nuclear magnetic resonance spectroscopy , spectral line , lysozyme , nmr spectra database , nuclear overhauser effect , nuclear magnetic resonance , polarization (electrochemistry) , stereochemistry , physics , biochemistry , quantum mechanics , astronomy
Photo‐CIDNP is a useful technique to identify surface residues in proteins and to assign resonances in their 1 H NMR spectra by the spectral simplification that is obtained. In spite of this simplification, conventional photo‐CIDNP spectra can be quite complex due to spectral overlap. For this reason two‐dimensional (2D) methods are welcome. We present combinations of photo‐CIDNP with 2D J ‐correlated spectroscopy (CIDNP‐COSY) and with 2D NOE spectroscopy (CIDNP‐NOESY). In these experiments we insert a saturation pulse sequence and a short laser‐irradiation period at the beginning of the preparation period to generate CIDNP, leaving the remaining of the pulse scheme essentially unaltered. The CIDNP‐COSY and CIDNP‐NOESY spectra of a hen egg‐white (HEW) lysozyme are presented. The CIDNP‐NOESY spectrum of lysozyme is compared with the results from 1D cross‐polarisation experiments on the same protein. CIDNP‐NOESY spectra of lysozyme with and without inhibitor NAG are compared.