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


Harča, Miroslava; Habinovec, Iva; Meštrović, Ernest; Novak, Predrag; Biljan, Ivana
LC-SPE/NMR analysis of process impurities of 3-bromo-5-(trifluormethyl)aniline // Adriatic NMR Book of Abstracts / Namjesnik, Danijel ; Novak, Predrag ; Parlov Vuković, Jelena (ur.).
Zagreb, 2019. str. 51-51 (poster, međunarodna recenzija, sažetak, znanstveni)


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 Book of Abstracts / Namjesnik, Danijel ; Novak, Predrag ; Parlov Vuković, Jelena - Zagreb, 2019, 51-51

ISBN
978-953-6076-56-7

Skup
Adriatic NMR conference

Mjesto i datum
Mali Ston, Hrvatska, 06-09.06.2019

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



POVEZANOST RADA


Projekt / tema
Met4Pharm

Ustanove
Prirodoslovno-matematički fakultet, Zagreb

Profili:

Avatar Url Predrag Novak (autor)

Avatar Url Ernest Meštrović (autor)

Avatar Url Ivana Biljan (autor)

Citiraj ovu publikaciju

Harča, Miroslava; Habinovec, Iva; Meštrović, Ernest; Novak, Predrag; Biljan, Ivana
LC-SPE/NMR analysis of process impurities of 3-bromo-5-(trifluormethyl)aniline // Adriatic NMR Book of Abstracts / Namjesnik, Danijel ; Novak, Predrag ; Parlov Vuković, Jelena (ur.).
Zagreb, 2019. str. 51-51 (poster, međunarodna recenzija, sažetak, znanstveni)
Harča, M., Habinovec, I., Meštrović, E., Novak, P. & Biljan, I. (2019) LC-SPE/NMR analysis of process impurities of 3-bromo-5-(trifluormethyl)aniline. U: Namjesnik, D., Novak, P. & Parlov Vuković, J. (ur.)Adriatic NMR Book of Abstracts.
@article{article, year = {2019}, pages = {51-51}, keywords = {LC-SPE, NMR, Impurities, Structural characterization}, isbn = {978-953-6076-56-7}, title = {LC-SPE/NMR analysis of process impurities of 3-bromo-5-(trifluormethyl)aniline}, keyword = {LC-SPE, NMR, Impurities, Structural characterization}, publisherplace = {Mali Ston, Hrvatska} }