EC-SPE-stripline-NMR analysis of reactive products: a feasibility study.
Anal Bioanal Chem
; 405(21): 6711-20, 2013 Aug.
Article
em En
| MEDLINE
| ID: mdl-23812883
ABSTRACT
Flow-through electrochemical conversion (EC) of drug-like molecules was hyphenated to miniaturized nuclear magnetic resonance spectroscopy (NMR) via on-line solid-phase extraction (SPE). After EC of the prominent p38α mitogen-activated protein kinase inhibitor BIRB796 into its reactive products, the SPE step provided preconcentration of the EC products and solvent exchange for NMR analysis. The acquisition of NMR spectra of the mass-limited samples was achieved in a stripline probe with a detection volume of 150 nL offering superior mass sensitivity. This hyphenated EC-SPE-stripline-NMR setup enabled the detection of the reactive products using only minute amounts of substrate. Furthermore, the integration of conversion and detection into one flow setup counteracts incorrect assessments caused by the degradation of reactive products. However, apparent interferences of the NMR magnetic field with the EC, leading to a low product yield, so far demanded relatively long signal averaging. A critical assessment of what is and what is not (yet) possible with this approach is presented, for example in terms of structure elucidation and the estimation of concentrations. Additionally, promising routes for further improvement of EC-SPE-stripline-NMR are discussed.
Texto completo:
1
Base de dados:
MEDLINE
Assunto principal:
Espectroscopia de Ressonância Magnética
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Análise de Injeção de Fluxo
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Proteína Quinase 14 Ativada por Mitógeno
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Eletroquímica
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Extração em Fase Sólida
Tipo de estudo:
Diagnostic_studies
Idioma:
En
Ano de publicação:
2013
Tipo de documento:
Article