engleski

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

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.

LC-SPE ; NMR ; Impurities ; Structural characterization

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