Preliminary communication

https://doi.org/10.5562/cca3042

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

Miroslava Harča ; PLIVA Croatia Ltd. Research and Development, Prilaz baruna Filipovića 25, HR-10000 Zagreb, Croatia
Iva Habinovec ; Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia
Ernest Meštrović ; PLIVA Croatia Ltd. Research and Development, Prilaz baruna Filipovića 25, HR-10000 Zagreb, Croatia
Ivana Biljan ; Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia
Predrag Novak ; Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia

Abstract

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.

Keywords

LC-SPE/NMR; impurities; identification; structure determination

Hrčak ID:

174780

URI

https://hrcak.srce.hr/174780

Publication date:

19.12.2016.

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