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

Autori
Harča, Miroslava ; Habinovec, Iva ; Meštrović, Ernest ; Biljan, Ivana ; Novak, Predrag

Izvornik
Croatica chemica acta (0011-1643) 89 (2016), 4; 543-547

Vrsta, podvrsta i kategorija rada
Radovi u časopisima, prethodno priopćenje, znanstveni

Ključne riječi
LC-SPE/NMR ; Impurities ; Identification ; Structure determination

Sažetak
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.

Izvorni jezik
Engleski

Znanstvena područja
Kemija

POVEZANOST RADA