Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR

A new impurity was detected during high performance liquid chromatographic (HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient. The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyze...

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Autores principales: Thomas, Saji, Paul, Saroj Kumar, Joshi, Subhash Chandra, Kumar, Vineet, Agarwal, Ashutosh, Vir, Dharam
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Xi'an Jiaotong University 2014
Materias:
Original Research Article
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5761219/
https://www.ncbi.nlm.nih.gov/pubmed/29403898
http://dx.doi.org/10.1016/j.jpha.2013.08.004
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author Thomas, Saji
Paul, Saroj Kumar
Joshi, Subhash Chandra
Kumar, Vineet
Agarwal, Ashutosh
Vir, Dharam
author_facet Thomas, Saji
Paul, Saroj Kumar
Joshi, Subhash Chandra
Kumar, Vineet
Agarwal, Ashutosh
Vir, Dharam
author_sort Thomas, Saji
collection PubMed
description A new impurity was detected during high performance liquid chromatographic (HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient. The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyzer (LC/ESI–IT/MS) analysis. Proposed structure of impurity was unambiguously confirmed by synthesis followed by characterization using (1)H, (13)C nuclear magnetic resonance spectrometry (NMR), (1)H–(1)H correlation spectroscopy (COSY) and infrared spectroscopy (IR). Based on the spectroscopic and spectrometric data, unknown impurity was characterized as 5-carbamoyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl propionate.
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spelling pubmed-57612192018-02-05 Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR Thomas, Saji Paul, Saroj Kumar Joshi, Subhash Chandra Kumar, Vineet Agarwal, Ashutosh Vir, Dharam J Pharm Anal Original Research Article A new impurity was detected during high performance liquid chromatographic (HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient. The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyzer (LC/ESI–IT/MS) analysis. Proposed structure of impurity was unambiguously confirmed by synthesis followed by characterization using (1)H, (13)C nuclear magnetic resonance spectrometry (NMR), (1)H–(1)H correlation spectroscopy (COSY) and infrared spectroscopy (IR). Based on the spectroscopic and spectrometric data, unknown impurity was characterized as 5-carbamoyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl propionate. Xi'an Jiaotong University 2014-10 2013-08-24 /pmc/articles/PMC5761219/ /pubmed/29403898 http://dx.doi.org/10.1016/j.jpha.2013.08.004 Text en © 2014 Xi’an Jiaotong University. Production and hosting by Elsevier B.V. http://creativecommons.org/licenses/by-nc-nd/3.0/ This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).
spellingShingle Original Research Article
Thomas, Saji
Paul, Saroj Kumar
Joshi, Subhash Chandra
Kumar, Vineet
Agarwal, Ashutosh
Vir, Dharam
Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR
title Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR
title_full Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR
title_fullStr Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR
title_full_unstemmed Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR
title_short Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI–IT/MS, (1)H, (13)C and (1)H–(1)H COSY NMR
title_sort identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by lc/esi–it/ms, (1)h, (13)c and (1)h–(1)h cosy nmr
topic Original Research Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5761219/
https://www.ncbi.nlm.nih.gov/pubmed/29403898
http://dx.doi.org/10.1016/j.jpha.2013.08.004
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