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Preliminary communication
https://doi.org/10.5562/cca3042

Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR

Miroslava Harča ; PLIVA Croatia Ltd. Research and Development, Prilaz baruna Filipovića 25, HR-10000 Zagreb, Croatia
Iva Habinovec ; Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia
Ernest Meštrović ; PLIVA Croatia Ltd. Research and Development, Prilaz baruna Filipovića 25, HR-10000 Zagreb, Croatia
Ivana Biljan ; Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia
Predrag Novak ; Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, HR-10000 Zagreb, Croatia

Fulltext: english, pdf (913 KB) pages 543-547 downloads: 568* cite
APA 6th Edition
Harča, M., Habinovec, I., Meštrović, E., Biljan, I. & Novak, P. (2016). Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR. Croatica Chemica Acta, 89 (4), 543-547. https://doi.org/10.5562/cca3042
MLA 8th Edition
Harča, Miroslava, et al. "Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR." Croatica Chemica Acta, vol. 89, no. 4, 2016, pp. 543-547. https://doi.org/10.5562/cca3042. Accessed 22 Feb. 2020.
Chicago 17th Edition
Harča, Miroslava, Iva Habinovec, Ernest Meštrović, Ivana Biljan and Predrag Novak. "Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR." Croatica Chemica Acta 89, no. 4 (2016): 543-547. https://doi.org/10.5562/cca3042
Harvard
Harča, M., et al. (2016). 'Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR', Croatica Chemica Acta, 89(4), pp. 543-547. https://doi.org/10.5562/cca3042
Vancouver
Harča M, Habinovec I, Meštrović E, Biljan I, Novak P. Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR. Croatica Chemica Acta [Internet]. 2016 [cited 2020 February 22];89(4):543-547. https://doi.org/10.5562/cca3042
IEEE
M. Harča, I. Habinovec, E. Meštrović, I. Biljan and P. Novak, "Rapid Identification of Unknown Impurities in 3-Bromo-5-(trifluoromethyl)aniline by LC-SPE/NMR", Croatica Chemica Acta, vol.89, no. 4, pp. 543-547, 2016. [Online]. https://doi.org/10.5562/cca3042

Abstracts
Identification of unknown pharmaceutical impurities is an essential part in the drug development process. In the present study, we developed and applied liquid chromatography (LC) – solid-phase extraction (SPE) / nuclear magnetic resonance (NMR) methodology with cryoprobe 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. The results of the present preliminary study demonstrated that LC-SPE/NMR can be used for rapid impurity profiling of 3-bromo-5-(trifluoromethyl)aniline.

Creative Commons License This work is licensed under a Creative Commons Attribution 4.0 International License.

Keywords
LC-SPE/NMR; impurities; identification; structure determination

Hrčak ID: 174780

URI
https://hrcak.srce.hr/174780

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