Applications of two-dimensional 1H nuclear magnetic resonance methods in photochemically induced dynamic nuclear polarisation spectroscopy

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Abstract
Photochemically induced dynamic nuclear polarisation (photo-CIDNP) has been widely used to identify surface residues in proteins and to assign resonances in their 1H n.m.r. spectra by the spectral simplification that is obtained. Welcome as this simplification may be in many cases, it also presents a limitation to the technique. We have increased the information content of photo-CIDNP spectra using pulse sequences analogous to INEPT (CIDNPT and refocused CIDNPT). Furthermore, we present combinations of photo-CIDNP with two-dimensional (2D)J-correlated spectroscopy (CIDNP-COSY) and with 2D nuclear Overhauser effect 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 remainder of the pulse scheme essentially unaltered. The CIDNPT technique has been applied to N-acetyl tyrosine and to N-acetyl tryptophan. The CIDNP-COSY spectrum of the lac-repressor headpiece is presented. The CIDNP-NOESY spectrum of hen egg-white lysozyme is compared with 1 D cross-polarisation spectra of the same protein.

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