Naslov
LC-SPE/NMR analysis of process impurities of 3- bromo-5-(trifluormethyl)aniline

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

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

Izvornik
Adriatic NMR Conference 2019 : Book of abstracts / Namjesnik, Danijel ; Novak, Predrag ; Parlov Vuković, Jelena - Zagreb, 2019, 51-51

ISBN
978-953-6076-56-7

Skup
Adriatic NMR 2019

Mjesto i datum
Mali Ston, Hrvatska, 06.06.2019. - 09.06.2019

Vrsta sudjelovanja
Poster

Vrsta recenzije
Međunarodna recenzija

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

Sažetak
As impurities define the quality of a chemical entity, their identification is an essential part in the drug development process. 3-Bromo-5- (trifluoromethyl)aniline is used as a starting material in the synthesis of active pharmaceutical ingredients (APIs). In the present work, we developed and applied liquid chromatography (LC) – solid-phase extraction (SPE) / nuclear magnetic resonance (NMR) methodology with cryoprobe for separation, isolation, trapping and structural characterization of process impurities of 3-bromo- 5-(trifluoromethyl)aniline. More than fifteen analytes were separated and isolated by using LC- SPE, and structural characterization was performed on ten isolated impurities. The structures of isolated impurities were elucidated by interpretation of their one-dimensional (1H and 19F) and two-dimensional homo- and heteronuclear (COSY, 1H-13C HSQC and 1H-13C HMBC) NMR spectra and mass spectrometry (MS) data. The results demonstrated that LC-SPE/NMR system with cryoprobe can be used successfully for rapid isolation and identification of impurities of 3-bromo-5- (trifluoromethyl)aniline.

Izvorni jezik
Engleski

Znanstvena područja
Kemija

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