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Apparatus for rapid adjustment of the degree of alignment of NMR samples in aqueous media: Verification with residual quadrupolar splittings in Na-23 and (CS)-C-133 spectra

Philip W. Kuchel
Organization: The University of Sydney
Department: Department of Biochemistry
B. E. Chapman
N Muller
Journal / Anthology

Year: 2006
Volume: 180
Issue: 2
Page range: 256-265

NMR spectra of Na-23(+) and Cs-133(+) in gelatine in a silicone rubber tube that was stretched to various extents showed remarkably reproducible resonance multiplicity. The relative intensities of the components of the split peaks had ratios, 3:4:3, and 7:12:15:16:15:12:7, respectively, that conformed with those predicted using a Mathematica program. The silicone-rubber tube was sealed at its lower end by a small rubber stopper and placed inside a thick-walled glass tube. Gelatine was injected in solution into the silicone tube and 'set' by cooling below 30 degrees C. A plastic thumb-screw held the silicone tube at various degrees of extension, up to similar to 2-fold. After constituting the gel in buffers containing NaCl and CsCl, both Na-23 and Cs-113 NMR spectroscopy revealed that after stretching the initial single Lorentzian line was split into a well-resolved triplet and a heptet, respectively. This was interpreted as being due to coupling between the electric quadrupoles of the nuclei and the average electric field gradient tensor of the collagen molecules of gelatine; these molecules became progressively more aligned in the direction of the main magnetic field, B-0, of the vertical bore magnet, as the gel was stretched. This apparatus provides a simple way of demonstrating fundamental physical characteristics of quadrupolar cations, some characteristics of gelatine under stretching, and a way to invoke static distortion of red blood cells. It should be useful with these and other cell types, for studies of metabolic and membrane transport characteristics that may change when the cells are distorted, and possibly for structural studies of macromolecules.

*Science > Chemistry

alignment tensor, electric field tensor, quadropolar splitting, gelatine, erythrocytes, 133-caesium, 23-sodium