Naslov
Structural Characterization of Impurities in 3- Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR

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

Vrsta, podvrsta i kategorija rada
Sažeci sa skupova, sažetak, znanstveni

Izvornik
25. hrvatski skup kemičara i kemijskih inženjera : Knjiga sažetaka / Šantić, Ana ; Đaković, Marijana - Zagreb : Hrvatsko kemijsko društvo, 2017, 251-251

Skup
25. hrvatski skup kemičara i kemijskih inženjera

Mjesto i datum
Poreč, Hrvatska, 19.04.2017. - 22.04.2017

Vrsta sudjelovanja
Poster

Vrsta recenzije
Međunarodna recenzija

Ključne riječi
LC-SPE, NMR, Structural characterization, Impurities

Sažetak
Impurities define the quality of a chemical entity so their unambiguous structure determination is essential part of the pharmaceutical development. Liquid chromatography (LC) – solid-phase extraction (SPE) / nuclear magnetic resonance (NMR) methodology with cryoprobe was developed and applied 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 to show that the impurities in question are di-bromo derivatives of 3- (trifluoromethyl)aniline. The results 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