Nuclear magnetic resonance lipid phases

Fig. 5. The 13C nuclear magnetic resonance line widths of the (enriched) choline methyl resonances in dipalmitoylphosphatidylcholine (A) and in dielaidoylphosphatidylcholine (O), as a function of temperature. Spectra taken at 90.5 MHz similar results were also obtained at 25.2 MHz. Note that the higher-melting lipid, dipalmitoylphosphatidylcholine, shows a readily observable enhanced line broadening at temperatures TU 32°C, corresponding to the onset of the lateral phase separation. (Data from Ref. 4.) [Reprinted with permission from P. Brulet and H. M. McConnell, J. Am. Chem. Soc., 98, 1314 (1977). Copyright by American Chemical Society.]...

As mentioned in my report, in addition to large coexisting domains of solid and fluid phase lipids, there may be fluctuations of composition and density in the fluid-lipid phase that are not seen in the electron microscope but that may affect nuclear magnetic resonance spectra. 

Lewis RNAH, McElhaney RN (2000) Surface charge markedly attenuates the nonlamellar phase-forming propensities of lipid bilayer membranes calorimetric and P-31-nuclear magnetic resonance studies of mixtures of cationic, anionic, and zwitterionic lipids. Biophys J 79 1455-1464... 

From the analysis of the data in the LIPID AT database (41), more than 150 different methods and method modifications have been used to collect data related to the lipid phase transitions. Almost 90% of the data is accounted for by less than 10 methods. Differential scaiming calorimetry strongly dominates the field with two thirds of all phase transition records. From the other experimental techniques, various fluorescent methods account for 10% of the information records. X-ray diffraction, nuclear magnetic resonance (NMR), Raman spectroscopy, electron spin resonance (ESR), infrared (IR) spectroscopy, and polarizing microscopy each contribute to about or less than 2-3% of the phase transition data records in the database. Especially useful in gaining insight into the mechanism and kinetics of lipid phase transitions has been time-resolved synchrotron X-ray diffraction (62,78-81). 

Nuclear magnetic resonance (NMR) spectroscopy is at present one of the most widely applied physical techniques in biology, and its potential applications increase day by day, as more sophisticated instrumentation becomes available and deeper theoretical knowledge is obtained. The phenomenon of NMR was discovered simultaneously by Purcell and his associates at Harvard University and by Bloch and co-workers at Stanford University, for which they were jointly awarded the Nobel prize in physics in 1952. In the lipid field there are two main types of NMR spectroscopy that are of interest broad-line experiments, concerned mainly with the spectra obtained from samples in the solid state, or from oriented phases, and narrow-line, or high-resolution, experiments carried out with samples in the liquid, solution or gas phases. Both types of NMR spectroscopy are extremely useful in the study of the lipids. In addition, Fourier transform (FT) NMR has helped increase the sensitivity of the technique and the so-called pulse method of recording spectra has literally widened the prospect of NMR applications in the field of lipid research and industry. The application of NMR to solid fats is still in its infancy (Pines et aL, 1973 Schaefer and Stejskal, 1979 BocieketaL, 1985). 

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