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Journal of Biomolecular NMR

, Volume 30, Issue 3, pp 253–265 | Cite as

Probing membrane protein orientation and structure using fast magic-angle-spinning solid-state NMR

  • O. C. Andronesi
  • J. R. Pfeifer
  • L. Al-Momani
  • S. Özdirekcan
  • D. T. S. Rijkers
  • B. Angerstein
  • S. Luca
  • U. Koert
  • J. A. Killian
  • M. Baldus
Article

Abstract

One and two-dimensional solid-state NMR experiments are discussed that permit probing local structure and overall molecular conformation of membrane-embedded polypeptides under Magic Angle Spinning. The functional dependence of a series of anisotropic recoupling schemes is analyzed using theoretical and numerical methods. These studies lead to the construction of a set of polarization dephasing or transfer units that probe local backbone conformation and overall molecular orientation within the same NMR experiment. Experimental results are shown for a randomly oriented peptide and for two model membrane–peptides reconstituted into lipid bilayers and oriented on polymer films according to a method proposed by Bechinger etal. [J. Am. Chem. Soc., 124, (2002), 1146–1147].

Keywords

MAS membrane proteins NMR solid-state structure determination 

Abbreviations:

ssNMR

solid state NMR

MAS

Magic Angle Spinning

R.F.

Radio Frequency

CSA

Chemical Shift Anisotropy

CP

Cross Polarization

APHH-CP

Adiabatic-Passage Hartmann-Hahn Cross-Polarization

SPECIFIC-CP

Spectrally Induced Filtering In Combination with Cross-Polarization

TPPM

Two Pulse Phase Modulation

TPPI

Time Proportional Phase Incrementation

DQ

Double Quantum

SQ

Single Quantum

POST-C7

Permutationally Offset Stabilized C7

SPC-5

Supercycled POST-C5

SD

Spin Diffusion

AHT

Average Hamiltonian Theory

TFE

Trifluoroethanol

DMPC

1,2-Dimyristoyl-sn-glycero-3-Phosphocholine

WALP23

Trp-flanked poly(alanine-leucine) peptides

PEEK

Polyetheretherketone

PTFE

Polytetrafluoroethylene

Fmoc

9-Fluorenylmethoxycarbonyl

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Supplementary material

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Supplementary material (PDF 188 KB)

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Copyright information

© Kluwer Academic Publishers 2004

Authors and Affiliations

  • O. C. Andronesi
    • 1
  • J. R. Pfeifer
    • 2
  • L. Al-Momani
    • 2
  • S. Özdirekcan
    • 3
  • D. T. S. Rijkers
    • 4
  • B. Angerstein
    • 1
  • S. Luca
    • 1
  • U. Koert
    • 2
  • J. A. Killian
    • 3
  • M. Baldus
    • 1
  1. 1.Department of NMR-Based Structural BiologyMax-Planck-Institute for Biophysical ChemistryGöttingenGermany
  2. 2.Fachbereich ChemiePhilipps-Universität MarburgMarburgGermany
  3. 3.Department of Biochemistry of MembranesUtrecht UniversityUtrechtThe Netherlands
  4. 4.Department of Medicinal Chemistry, Utrecht Institute for Pharmaceutical Sciences, Faculty of PharmacyUtrecht UniversityUtrechtThe Netherlands

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