Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR

Autor:	Iva Habinovec, Predrag Novak, Ernest Meštrović, Miroslava Harča, Ivana Biljan
Jazyk:	angličtina
Rok vydání:	2016
Předmět:	Chromatography Trifluoromethyl Chemistry Elution General Chemistry LC-SPE/NMR Impurities Identification Structure determination NMR spectra database chemistry.chemical_compound impurities identification structure determination Aniline Heteronuclear molecule Deuterium Impurity Acetonitrile
Zdroj:	Croatica Chemica Acta Volume 89 Issue 4
ISSN:	1334-417X 0011-1643
Popis:	Identification of unknown pharmaceutical impurities is an essential part in the drug development process. In the present study, we developed and applied liquid chromatography (LC) – solid-phase extraction (SPE) / nuclear magnetic resonance (NMR) methodology with cryoprobe for identification and structural characterization of unknown impurities in 3-bromo-5-(trifluoromethyl)aniline. The three main impurities were separated and isolated by LC-SPE system. After multiple trapping, isolated impurities were eluted from the SPE cartridges with deuterated acetonitrile and one- and two-dimensional homo- and heteronuclear NMR spectra were recorded. The structures of the unknown impurities were determined by detailed inspection of NMR spectra and by mass spectrometric (MS) analysis. The results of the present preliminary study demonstrated that LC-SPE/NMR can be used for rapid impurity profiling of 3-bromo-5-(trifluoromethyl)aniline. This work is licensed under a Creative Commons Attribution 4.0 International License.
Databáze:	OpenAIRE
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