Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction

Time-resolved carbamazepine crystallization from wet ethanol has been monitored using a combination of cryoTEM and 3D electron diffraction. Carbamazepine is shown to crystallize exclusively as a dihydrate after 180 s. When the timescale was reduced to 30 s, three further polymorphs could be identifi...

Descripción completa

Detalles Bibliográficos
Autores principales: Broadhurst, Edward T., Xu, Hongyi, Parsons, Simon, Nudelman, Fabio
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2021
Materias:
Research Letters
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8562671/
https://www.ncbi.nlm.nih.gov/pubmed/34804540
http://dx.doi.org/10.1107/S2052252521010101
_version_ 1784593299878707200
author Broadhurst, Edward T.
Xu, Hongyi
Parsons, Simon
Nudelman, Fabio
author_facet Broadhurst, Edward T.
Xu, Hongyi
Parsons, Simon
Nudelman, Fabio
author_sort Broadhurst, Edward T.
collection PubMed
description Time-resolved carbamazepine crystallization from wet ethanol has been monitored using a combination of cryoTEM and 3D electron diffraction. Carbamazepine is shown to crystallize exclusively as a dihydrate after 180 s. When the timescale was reduced to 30 s, three further polymorphs could be identified. At 20 s, the development of early stage carbamazepine dihydrate was observed through phase separation. This work reveals two possible crystallization pathways present in this active pharmaceutical ingredient.
format Online
Article
Text
id pubmed-8562671
institution National Center for Biotechnology Information
language English
publishDate 2021
publisher International Union of Crystallography
record_format MEDLINE/PubMed
spelling pubmed-85626712021-11-18 Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction Broadhurst, Edward T. Xu, Hongyi Parsons, Simon Nudelman, Fabio IUCrJ Research Letters Time-resolved carbamazepine crystallization from wet ethanol has been monitored using a combination of cryoTEM and 3D electron diffraction. Carbamazepine is shown to crystallize exclusively as a dihydrate after 180 s. When the timescale was reduced to 30 s, three further polymorphs could be identified. At 20 s, the development of early stage carbamazepine dihydrate was observed through phase separation. This work reveals two possible crystallization pathways present in this active pharmaceutical ingredient. International Union of Crystallography 2021-10-30 /pmc/articles/PMC8562671/ /pubmed/34804540 http://dx.doi.org/10.1107/S2052252521010101 Text en © Edward T. Broadhurst et al. 2021 https://creativecommons.org/licenses/by/4.0/This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
spellingShingle Research Letters
Broadhurst, Edward T.
Xu, Hongyi
Parsons, Simon
Nudelman, Fabio
Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction
title Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction
title_full Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction
title_fullStr Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction
title_full_unstemmed Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction
title_short Revealing the early stages of carbamazepine crystallization by cryoTEM and 3D electron diffraction
title_sort revealing the early stages of carbamazepine crystallization by cryotem and 3d electron diffraction
topic Research Letters
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8562671/
https://www.ncbi.nlm.nih.gov/pubmed/34804540
http://dx.doi.org/10.1107/S2052252521010101
work_keys_str_mv AT broadhurstedwardt revealingtheearlystagesofcarbamazepinecrystallizationbycryotemand3delectrondiffraction
AT xuhongyi revealingtheearlystagesofcarbamazepinecrystallizationbycryotemand3delectrondiffraction
AT parsonssimon revealingtheearlystagesofcarbamazepinecrystallizationbycryotemand3delectrondiffraction
AT nudelmanfabio revealingtheearlystagesofcarbamazepinecrystallizationbycryotemand3delectrondiffraction

Ejemplares similares