Speeding-up the Determination of Protein-Ligand Affinities by STD NMR: The Reduced Data Set STD NMR Approach (rd-STD NMR)

STD NMR spectroscopy is a powerful ligand-observed NMR tool for screening and characterizing the interactions of small molecules and low molecular weight fragments with a given macromolecule, identifying the main intermolecular contacts in the bound state. It is also a powerful analytical technique...

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Detalles Bibliográficos
Autores: Rocha, Gabriel, Ramírez-Cárdenas, Jonathan, Padilla-Pérez, M Carmen, Walpole, Samuel, Nepravishta, Ridvan, García-Moreno, M. Isabel, Sánchez-Fernández, Elena M., Ortiz-Mellet, Carmen, Angulo, Jesús, Muñoz-García, Juan C.
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2024
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/356374
Acceso en línea:http://hdl.handle.net/10261/356374
https://api.elsevier.com/content/abstract/scopus_id/85181558542
Access Level:acceso abierto
Palabra clave:Ligands
Magnetic Resonance Imaging
Magnetic Resonance Spectroscopy
Epitope
Mapping
Protein Binding Proteins
Descripción
Sumario:STD NMR spectroscopy is a powerful ligand-observed NMR tool for screening and characterizing the interactions of small molecules and low molecular weight fragments with a given macromolecule, identifying the main intermolecular contacts in the bound state. It is also a powerful analytical technique for the accurate determination of protein-ligand dissociation constants (KD) of medium-to-weak affinity, of interest in the pharmaceutical industry. However, accurate KD determination and epitope mapping requires a long series of experiments at increasing saturation times to carry out a full analysis using the so-called STD NMR build-up curve approach and apply the "initial slopes approximation". Here, we have developed a new protocol to bypass this important limitation, which allows us to obtain initial slopes by using just two saturation times and, hence, to very quickly determine precise protein-ligand dissociation constants by STD NMR.