Structural Characterization of Impurities in 3- Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR (CROSBI ID 672903)
Prilog sa skupa u zborniku | sažetak izlaganja sa skupa | međunarodna recenzija
Podaci o odgovornosti
Harča, Miroslava ; Habinovec, Iva ; Meštrović, Ernest ; Biljan, Ivana ; Novak, Predrag
engleski
Structural Characterization of Impurities in 3- Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR
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.
LC-SPE, NMR, Structural characterization, Impurities
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Podaci o prilogu
251-251.
2017.
objavljeno
Podaci o matičnoj publikaciji
25. hrvatski skup kemičara i kemijskih inženjera : Knjiga sažetaka
Šantić, Ana ; Đaković, Marijana
Zagreb: Hrvatsko kemijsko društvo
Podaci o skupu
25. hrvatski skup kemičara i kemijskih inženjera
poster
19.04.2017-22.04.2017
Poreč, Hrvatska