Band-selective 3D NOESY-TOCSY: measurement of through-space correlations between aliphatic protons of membrane peptides and proteins in non-deuterated detergents.
Recently the use of band-selective excitation to obtain 1H 2D NMR spectra of membrane peptides and proteins in non-deuterated detergents has been demonstrated [Seigneuret, M. and Levy, D. (1995) J. Biomol. NMR, 5, 345-352]. A limitation of the method was the inability to obtain through-space correlation between aliphatic protons. Here, a 3D F3-band-selective NOESY-TOCSY experiment is described that allows such correlations to be observed in the presence of an excess of non-deuterated detergent. Application to the measurement of proximities between aliphatic protons of the membrane peptide mastoparan X solubilized in non-deuterated n-octylglucoside is presented. With this additional experiment, it is now possible to obtain the same amount of structural constraints on membrane peptides and protein in non-deuterated detergent as in deuterated detergent and therefore to perform complete structural studies.
Le Guernevé
C
C
Laboratoire de Biophysique Cellulaire et RMN, Université Paris, France.
Seigneuret
M
M
D003902:Detergents / Q000737:chemistry; D005960:Glucosides / Q000737:chemistry; D036341:Intercellular Signaling Peptides and Proteins; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008565:Membrane Proteins / Q000737:chemistry*; D010455:Peptides / Q000737:chemistry*; D011522:Protons
D003902:Detergents; D005960:Glucosides; D036341:Intercellular Signaling Peptides and Proteins; D008565:Membrane Proteins; D010455:Peptides; D011522:Protons; C018619:octyl-beta-D-glucoside; C071123:mastoparan X