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Espectroscopia de correlación heteronuclear mejorada en sensibilidad en RMN multidimensional en estado sólido de

T Gopinath¹, Nathaniel J Traaseth, Kaustubh Mote

¹Department of Biochemistry, Molecular Biology, and Biophysics, University of Minnesota, Minneapolis, Minnesota 55455, USA.

Journal of the American Chemical Society

|March 30, 2010

Resumen

Los nuevos métodos de RMN de estado sólido aumentan la sensibilidad para los experimentos de espectroscopia de correlación heteronuclear (HETCOR) hasta en un 180%. Estos avances aceleran la adquisición de datos para sistemas orientados como las proteínas de membrana y los cristales líquidos.

Área de la Ciencia:

Espectroscopia de resonancia magnética nuclear (RMN) en estado sólido.
Química biofísica es la química biofísica.
Ciencia de los materiales ciencia de los materiales.

Sus antecedentes:

La espectroscopia de correlación heteronuclear (HETCOR) es crucial para el esclarecimiento estructural de los sistemas orientados.
Las técnicas HETCOR actuales en RMN de estado sólido pueden estar limitadas por la sensibilidad, lo que requiere largos tiempos de adquisición.
Los sistemas orientados, incluidas las proteínas de membrana y los cristales líquidos, presentan desafíos únicos para el análisis de RMN.

Objetivo del estudio:

Introducir esquemas novedosos y de mayor sensibilidad para los experimentos HETCOR de RMN de estado sólido.
Mejorar la eficiencia y reducir los tiempos de adquisición para los experimentos multidimensionales HETCOR en muestras orientadas.
Proporcionar herramientas mejoradas para la caracterización estructural y dinámica de sistemas biológicos y materiales complejos.

Principales métodos:

Desarrollo de nuevas secuencias de pulsos para mejorar la sensibilidad en HETCOR.
Aplicación de los esquemas 2D SE-HETCOR y 3D SE-PISEMAI-HETCOR.
Validación experimental utilizando un único cristal de ((15) N) N-acetilleucina y la proteína de membrana sarcolipina orientada en las bicelas lipídicas.

Principales resultados:

Se logró una mejora de sensibilidad del 40% para los experimentos 2D SE-HETCOR.
Se ha demostrado hasta un 180% de mejora de sensibilidad para los experimentos 3D SE-PISEMAI-HETCOR.
Aplicó con éxito los esquemas mejorados tanto a pequeñas moléculas como a proteínas de membrana integral.

Conclusiones:

Los esquemas HETCOR mejorados de sensibilidad desarrollados mejoran significativamente la eficiencia experimental en RMN en estado sólido.
Estos métodos son ampliamente aplicables a varios sistemas orientados, incluidas las proteínas de membrana en bicapas lipídicas y materiales cristalinos líquidos.
Los tiempos de adquisición reducidos facilitarán estudios estructurales y dinámicos más profundos de sistemas desafiantes.

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