Abstract
Membrane organization, including the presence of domains, can be characterized by measuring lateral diffusion rates of lipids and membrane-bound substances. Magic angle spinning (MAS) yields well-resolved proton nuclear magnetic resonance (NMR) of lipids in biomembranes. When combined with pulsed-field gradient NMR (rendering what is called “pulsed magnetic field gradients-MAS-NMR”), it permits precise diffusion measurements on the micrometer lengths scale for any substance with reasonably well-resolved proton MAS-NMR resonances, without the need of preparing oriented samples. Sample preparation procedures, the technical requirements for the NMR equipment, and spectrometer settings are described. Additionally, equations for analysis of diffusion data obtained from unoriented samples, and a method for correcting the data for liposome curvature are provided.
This is a preview of subscription content, log in via an institution to check access.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Holte, L. L. and Gawrisch, K. (1997) Determining ethanol distribution in phospholipid multilayers with MAS-NOESY spectra. Biochemistry 36, 4669–4674.
Eldho, N. V., Feller, S. E., Tristram-Nagle, S., Polozov, I. V., and Gawrisch, K. (2003) Polyunsaturated docosahexaenoic vs docosapentaenoic acid—Differences in lipid matrix properties from the loss of one double bond. J. Am. Chem. Soc. 125, 6409–6421.
Gaede, H. C. and Gawrisch, K. (2003) Lateral diffusion rates of lipid, water, and a hydrophobic drug in a multilamellar liposome. Biophys. J. 85, 1734–1740.
Gaede, H. C. and Gawrisch, K. (2004) Multidimensional PFG-MAS-NMR experiments on membranes. Magn. Reson. Chem. 42, 115–122.
Scheidt, H. A., Huster, D., and Gawrisch, K. (2005) Diffusion of cholesterol and its precursors in lipid membranes studied by 1H pulsed field gradient magic angle spinning NMR. Biophys. J. 89, 2504–2512.
Wattraint, O. and Sarazin, C. (2005) Diffusion measurements of water, ubiquinone and lipid bilayer inside a cylindrical nanoporous support: A stimulated echo pulsed-field gradient MAS-NMR investigation. Biochim. Biophys. Acta 1713, 65–72.
Pampel, A., Zick, K., Glauner, H., and Engelke, F. (2004) Studying lateral diffusion in lipid bilayers by combining a magic angle spinning NMR probe with a microimaging gradient system. J. Am. Chem. Soc. 126, 9534–9535.
Pampel, A., Michel, D., and Reszka, R. (2002) Pulsed field gradient MAS-NMR studies of the mobility of carboplatin in cubic liquid-crystalline phases. Chem. Phys. Lett. 357, 131–136.
Pampel, A., Kärger, J., and Michel, D. (2003) Lateral diffusion of a transmembrane peptide in lipid bilayers studied by pulsed field gradient NMR in combination with magic angle sample spinning. Chem. Phys. Lett. 379, 555–561.
Polozov, I. V. and Gawrisch, K. (2004) Domains in binary SOPC/POPE lipid mixtures studied by pulsed field gradient H-1 MAS NMR. Biophys. J. 87, 1741–1751.
Cotts, R. M., Hoch, M. J. R., sun, T., and markert, J. T. (1989) pulsed field gradient stimulated echo methods for improved NMR diffusion measurements in heterogeneous systems. J. Magn. Reson. 83, 252–266.
Fordham, E. J., Mitra, P. P., and Latour, L. L. (1996) Effective diffusion times in multiple-pulse PFG diffusion measurements in porous media. J. Magn. Reson. A. 121, 187–192.
Callaghan, P. T. and söderman, O. (1983) examination of the lamellar phase of aerosol OT-water using pulsed field gradient nuclear magnetic-resonance. J. Phys. Chem. 87, 1737–1744.
Lindblom, G., Wennerström, H., and Arvidson, G. (1977) translational diffusion in model membranes studied by nuclear magnetic resonance. int. J. quant. chem. 12, 153–158.
Nagle, J. F., Liu, Y. F., Tristram-Nagle, S., Epand, R. M., and Stark, R. E. (1999) Re-analysis of magic angle spinning nuclear magnetic resonance determination of interlamellar waters in lipid bilayer dispersions. Biophys. J. 77, 2062–2065.
Huster, D., Arnold, K., and Gawrisch, K. (1999) Investigation of lipid organization in biological membranes by two-dimensional nuclear Overhauser enhancement spectroscopy. J. Phys. Chem. B. 103, 243–251.
Mills, R. (1973) self-diffusion in normal and heavy-water in range 1–45 degrees. J. phys. chem. 77, 685–688.
Author information
Authors and Affiliations
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2007 Humana Press Inc.
About this protocol
Cite this protocol
Gawrisch, K., Gaede, H.C. (2007). Measurement of Lateral Diffusion Rates in Membranes by Pulsed Magnetic Field Gradient, Magic Angle Spinning-Proton Nuclear Magnetic Resonance. In: Dopico, A.M. (eds) Methods in Membrane Lipids. Methods in Molecular Biology™, vol 400. Humana Press. https://doi.org/10.1007/978-1-59745-519-0_17
Download citation
DOI: https://doi.org/10.1007/978-1-59745-519-0_17
Publisher Name: Humana Press
Print ISBN: 978-1-58829-662-7
Online ISBN: 978-1-59745-519-0
eBook Packages: Springer Protocols