LnDOTA-d8 , a versatile chemical-shift thermometer for 2 H solid-state NMR

© 2022 John Wiley & Sons Ltd.

Bibliographische Detailangaben
Veröffentlicht in:Magnetic resonance in chemistry : MRC. - 1985. - 60(2022), 10 vom: 17. Okt., Seite 1005-1013
1. Verfasser: Umegawa, Yuichi (VerfasserIn)
Weitere Verfasser: Shimonishi, Takeshi, Tsuchikawa, Hiroshi, Murata, Michio
Format: Online-Aufsatz
Sprache:English
Veröffentlicht: 2022
Zugriff auf das übergeordnete Werk:Magnetic resonance in chemistry : MRC
Schlagworte:Journal Article Research Support, Non-U.S. Gov't 2H chemical-shift thermometer lanthanide complex lipid bilayers segmental melting solid-state NMR Ligands Lipid Bilayers Membrane Lipids
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520 |a 2 H solid-state nuclear magnetic resonance (NMR) is a method for examining the mobility and orientation of molecules in the field of biophysics. In studies on lipid bilayer membranes, 2 H NMR is often adopted to detect a phase transition from the gel to the liquid-crystal phase, which is observed as a change in spectral shape, and to evaluate the ordering of lipid alkyl chains using quadrupole coupling values. Because the mobility of membrane lipids is highly temperature dependent, precise temperature control is a prerequisite for evaluating the physical properties of membranes. Generally, NMR instruments monitor the temperature of the variable temperature (VT) gas. The temperature inside the sample tube and the VT gas match only when the heat generated by the radio frequency (rf) pulse emitted from the coil or magic angle spinning is significantly lower than the cooling capacity of the VT gas. In other words, the sample temperature inside the tube depends on the measurement method. Therefore, in this study, we took advantage of temperature-dependent changes in the chemical shift of a paramagnetic metal-ligand complex. We designed and synthesized a deuterated ligand complex and evaluated its temperature dependence as a thermometer for 2 H solid-state NMR spectroscopy. We chose Tb, Dy, Ho, and Er as the paramagnetic central metals. We then measured the 2 H NMR spectrum of each metal complex and confirmed the 2 H chemical shift to be temperature dependent. Furthermore, with the use of the thermometer molecule with Er, we succeeded in accurately evaluating the segmental melting of an alkyl chain in lipid bilayers with 0.1°C accuracy 
650 4 |a Journal Article 
650 4 |a Research Support, Non-U.S. Gov't 
650 4 |a 2H 
650 4 |a chemical-shift thermometer 
650 4 |a lanthanide complex 
650 4 |a lipid bilayers 
650 4 |a segmental melting 
650 4 |a solid-state NMR 
650 7 |a Ligands  |2 NLM 
650 7 |a Lipid Bilayers  |2 NLM 
650 7 |a Membrane Lipids  |2 NLM 
700 1 |a Shimonishi, Takeshi  |e verfasserin  |4 aut 
700 1 |a Tsuchikawa, Hiroshi  |e verfasserin  |4 aut 
700 1 |a Murata, Michio  |e verfasserin  |4 aut 
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