title: Centerband-only analysis of rotor-unsynchronized spin echo for measurement of lipid (31) P chemical shift anisotropy.
abstract: Structural diversity and molecular flexibility of phospholipids are essential for biological membranes to play key roles in numerous cellular processes. Uncovering the behavior of individual lipids in membrane dynamics is crucial for understanding the molecular mechanisms underlying biological functions of cell membranes. In this paper, we introduce a simple method to investigate dynamics of lipid molecules in multi-component systems by measuring the (31) P chemical shift anisotropy (CSA) under magic angle spinning (MAS) conditions. For achieving both signal separation and CSA determination, we utilized a centerband-only analysis of rotor-unsynchronized spin echo (COARSE). This analysis is based on the curve fitting of periodic modulation of centerband intensity along the interpulse delay time in rotor-unsynchronized spin-echo experiments. The utility of COARSE was examined by using phospholipid vesicles, a three-component lipid raft model system, and archaeal purple membranes. We found that the apparent advantages of this method are high resolution and high sensitivity given by the moderate MAS speed and the one-dimensional acquisition with short spin-echo delays. COARSE provides an alternative method for CSA measurement that is effective in the investigation of lipid polymorphologies.
authors.affiliation: JST ERATO, Lipid Active Structure Project, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Project Research Centre for Fundamental Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.
authors.forename: Yuichi
authors.initials: Y
authors.lastname: Umegawa
authors.affiliation: JST ERATO, Lipid Active Structure Project, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Project Research Centre for Fundamental Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.
authors.forename: Toshiyuki
authors.initials: T
authors.lastname: Yamaguchi
authors.affiliation: JST ERATO, Lipid Active Structure Project, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Project Research Centre for Fundamental Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.
authors.forename: Michio
authors.initials: M
authors.lastname: Murata
authors.affiliation: JST ERATO, Lipid Active Structure Project, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Department of Chemistry, Graduate School of Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.|Project Research Centre for Fundamental Science, Osaka University, 1-1 Machikaneyama, Toyonaka, Osaka Prefecture, 560-0043, Japan.
authors.forename: Shigeru
authors.initials: S
authors.lastname: Matsuoka
mesh_terms: D016880:Anisotropy; D008051:Lipid Bilayers / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000592:standards; D015394:Molecular Structure; D010743:Phospholipids / Q000032:analysis*; D010758:Phosphorus / Q000737:chemistry*; D012015:Reference Standards
chemical_list: D008051:Lipid Bilayers; D010743:Phospholipids; D010758:Phosphorus
keywords: 31P and 13C; CSA recoupling under MAS; lipid polymorphism; solid-state NMR