Artikel des Tages: Slow magic-angle coil spinning: A high-sensitivity and high-resolution NMR strategy for microscopic biological specimens

Der heutige Artikel des Tages widmet sich einer eher technischen Fragestellung.
Erschienen ist er im Februar 2010 in der Zeitschrift Magnetic Resonance in Medicine, Vol. 63, Teil 2, Seiten 269-274.

High-resolution magic-angle spinning has become a valuable tool to study biologic samples; however, there are only a few high-resolution magic-angle spinning methodologies that have been explored specifically to deal with small semisolid biomaterials such as tissues. Here, we report a novel high-resolution 1H NMR spectroscopic approach using magic-angle coil spinning. We demonstrate its potential for intact tissues by combining a resonant microcoil with a large-volume commercial magic-angle spinning rotor, where the microcoil offers incredible sensitivity and the large-volume magic-angle spinning rotor provides stable slow magic-angle spinning. This approach provides high-resolution spectra with high sensitivity and the preservation of living biologic specimens for an accurate chemical analysis.

Die Autoren sind Mitglieder des Commissariat à l'Énergie Atomique Saclay, in Gif-sur-Yvette, Frankreich.

Online abrufbar ist der Artikel über DOI 10.1002/mrm.22231.

Artikel des Tages: Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes

Nach eineinhalb Monaten Weihnachtspause gibt es hier auch endlich wieder einen Artikel des Tages.

Diesmal ist das Thema in der Festkörperphysik zu finden: es geht um NMR-Spektroskopie an DOPC-Membranen, unter der Anwendung der LG-HETCOR-LG-Methode.

Abstract:

Direct observation of J-couplings remains a challenge in high-resolution solid-state NMR. In some cases, it is possible to use Lee–Goldburg (LG) homonuclear decoupling during rare spin observation in MAS NMR correlation spectroscopy of lipid membranes to obtain J-resolved spectra in the direct dimension. In one simple implementation, a wide line separation-type
¹³C-¹H HETCOR can provide high-resolution ¹H/¹³C spectra, which are J-resolved in both dimensions. Coupling constants, ¹J_CH, obtained from ¹H doublets, can be compared with scaled ¹J^θ_CH obtained from the ¹³C multiplets to assess the LG-values efficiency and scaling factor. The use of homonuclear decoupling during proton evolution, LG-HETCOR-LG, can provide J-values, at least in the rare spin dimension, and allows measurements in less mobile membrane environments. The LG-decoupled spectroscopic approach is demonstrated on pure dioleoylphosphatidylcholine (DOPC) membranes and used to investigate lipid mixtures of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin.

Die Autoren sind Mitarbeiter der Universität von Nottingham in Großbritannien.

Erschienen ist der Artikel im Magazin Magnetic Resonance in Chemistry, Volume 48, Teil 12, Seiten 925–934. Online zu finden ist er außerdem unter DOI 10.1002/mrc.2690.