Novel NMR tools to study structure and dynamics of biomembranes

Gawrisch, Klaus; Eldho, Nadukkudy V.; Polozov, Ivan V.

doi:10.1016/s0009-3084(02)00024-5

Cited by 76 publications

(82 citation statements)

References 46 publications

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“…Separated local-field spectroscopy (45)(46)(47) at natural 13 C abundance expands the range of applications of solid-state NMR in membrane biophysics in significant new ways. The development and use of biophysical methods for FIGURE 4 SLF 13 C NMR spectroscopy gives segmental jS CH j order parameters that agree with 2 H solid-state NMR-derived jS CD j order parameters.…”

Section: Discussionmentioning

confidence: 99%

“…This work is aimed at extending such investigations by using for the first time to our knowledge a combination of separated local-field (SLF) NMR spectroscopy (41,(46)(47)(48) and statistical mean-torque theory (35). Studies of natural lipids, as well as natural detergents (49), can benefit from extending methods originally developed for 2 H NMR spectroscopy (50) to cases where 2 H-isotope labeling is impractical.…”

Section: Introductionmentioning

confidence: 99%

“…Magic-angle spinning (MAS) NMR resolves site-specific details for individual lipid species in membranes (28,47,(53)(54)(55)(56), thus enabling a range of biologically significant applications. We show how the steric hydrocarbon thickness and average cross-sectional areas are derived from solid-state 13 C-1 H residual dipolar couplings (RDCs) for sphingolipids and phospholipids in singlecomponent and cholesterol-enriched binary mixtures.…”

Section: Introductionmentioning

confidence: 99%

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Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13 C NMR Spectroscopy

Leftin

Molugu

Job

et al. 2014

Biophysical Journal

111

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Investigations of lipid membranes using NMR spectroscopy generally require isotopic labeling, often precluding structural studies of complex lipid systems. Solid-state (13)C magic-angle spinning NMR spectroscopy at natural isotopic abundance gives site-specific structural information that can aid in the characterization of complex biomembranes. Using the separated local-field experiment DROSS, we resolved (13)C-(1)H residual dipolar couplings that were interpreted with a statistical mean-torque model. Liquid-disordered and liquid-ordered phases were characterized according to membrane thickness and average cross-sectional area per lipid. Knowledge of such structural parameters is vital for molecular dynamics simulations, and provides information about the balance of forces in membrane lipid bilayers. Experiments were conducted with both phosphatidylcholine (dimyristoylphosphatidylcholine (DMPC) and palmitoyloleoylphosphatidylcholine (POPC)) and egg-yolk sphingomyelin (EYSM) lipids, and allowed us to extract segmental order parameters from the (13)C-(1)H residual dipolar couplings. Order parameters were used to calculate membrane structural quantities, including the area per lipid and bilayer thickness. Relative to POPC, EYSM is more ordered in the ld phase and experiences less structural perturbation upon adding 50% cholesterol to form the lo phase. The loss of configurational entropy is smaller for EYSM than for POPC, thus favoring its interaction with cholesterol in raftlike lipid systems. Our studies show that solid-state (13)C NMR spectroscopy is applicable to investigations of complex lipids and makes it possible to obtain structural parameters for biomembrane systems where isotope labeling may be prohibitive.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13 C NMR Spectroscopy

Leftin

Molugu

Job

et al. 2014

Biophysical Journal

111

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“…The design of the actual rotor system used, on the other hand, is of major concern (see below). At a spinning speed of 8 kHz, a typical value employed in MAS experiments on biomembranes, 1,3,4 the temperature increase is 10°C.…”

Section: Thementioning

confidence: 99%

Heating caused by radiofrequency irradiation and sample rotation in ¹³C magic angle spinning NMR studies of lipid membranes

Dvinskikh

Castro

Sandström

2004

Magnetic Reson in Chemistry

103

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Application of rapid sample rotation and radiofrequency irradiation in magic angle spinning (MAS) NMR of lipid bilayers can significantly increase the sample temperature. In this work, we studied the extent of heating during the acquisition of 1H-decoupled 13C MAS spectra of hydrated dimyristoylphosphatidylcholine (DMPC) in the L(alpha) phase. First, we describe a simple procedure for determining the increase in temperature by observing the shift of the 1H water signal. The method is then used to identify and assess the various factors that contribute to the sample heating. The important factors discussed in this paper include: (i) the spinning speed, (ii) the variable-temperature gas pressure, (iii) the rotor geometry, (iv) the power, duration and frequency of the radiofrequency irradiation and (v) the hydration level. A comparison of different heteronuclear decoupling schemes in terms of their ability to produce highly resolved 13C spectra of DMPC is also reported.

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“…[1][2][3][4][5] For biological systems, temperature is one of the most important parameters for regulating various physiological functions such as intermolecular interactions, chemical reactions, lipid domain formation, and alteration of protein conformation. Therefore, to adequately investigate these phenomena, the in situ temperature of an NMR sample has to be accurately determined.…”

Section: Introductionmentioning

confidence: 99%

¹³C‐TmDOTA as versatile thermometer compound for solid‐state NMR of hydrated lipid bilayer membranes

Umegawa

Tanaka

Matsumori

et al. 2015

Magnetic Reson in Chemistry

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Recent advances in solid-state nuclear magnetic resonance (NMR) techniques, such as magic angle spinning and high-power decoupling, have dramatically increased the sensitivity and resolution of NMR. However, these NMR techniques generate extra heat, causing a temperature difference between the sample in the rotor and the variable temperature gas. This extra heating is a particularly crucial problem for hydrated lipid membrane samples. Thus, to develop an NMR thermometer that is suitable for hydrated lipid samples, thulium-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate (TmDOTA) was synthesized and labeled with (13) C (i.e., (13) C-TmDOTA) to increase the NMR sensitivity. The complex was mixed with a hydrated lipid membrane, and the system was subjected to solid-state NMR and differential scanning calorimetric analyses. The physical properties of the lipid bilayer and the quality of the NMR spectra of the membrane were negligibly affected by the presence of (13) C-TmDOTA, and the (13) C chemical shift of the complex exhibited a large-temperature dependence. The results demonstrated that (13) C-TmDOTA could be successfully used as a thermometer to accurately monitor temperature changes induced by (1) H decoupling pulses and/or by magic angle spinning and the temperature distribution of the sample inside the rotor. Thus, (13) C-TmDOTA was shown to be a versatile thermometer for hydrated lipid assemblies. Copyright © 2015 John Wiley & Sons, Ltd.

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Novel NMR tools to study structure and dynamics of biomembranes

Cited by 76 publications

References 46 publications

Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13 C NMR Spectroscopy

Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13 C NMR Spectroscopy

Heating caused by radiofrequency irradiation and sample rotation in ¹³C magic angle spinning NMR studies of lipid membranes

¹³C‐TmDOTA as versatile thermometer compound for solid‐state NMR of hydrated lipid bilayer membranes

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Novel NMR tools to study structure and dynamics of biomembranes

Cited by 76 publications

References 46 publications

Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13 C NMR Spectroscopy

Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13 C NMR Spectroscopy

Heating caused by radiofrequency irradiation and sample rotation in 13C magic angle spinning NMR studies of lipid membranes

13C‐TmDOTA as versatile thermometer compound for solid‐state NMR of hydrated lipid bilayer membranes

Contact Info

Product

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Heating caused by radiofrequency irradiation and sample rotation in ¹³C magic angle spinning NMR studies of lipid membranes

¹³C‐TmDOTA as versatile thermometer compound for solid‐state NMR of hydrated lipid bilayer membranes