In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine

The objective of this work was to study the polymorphic transformation of carbamazepine from Form II to Form III in 1-propanol during seeded isothermal batch crystallization. First, the pure Form II and Form III were obtained and characterized. Then their solubilities and metastable zone limits were...

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Main Authors: Sohrab Rohani, Yingying Zhao, Ying Bao, Jingkang Wang
Format: Article
Language:English
Published: MDPI AG 2012-02-01
Series:Pharmaceutics
Subjects:
Online Access:http://www.mdpi.com/1999-4923/4/1/164/
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author Sohrab Rohani
Yingying Zhao
Ying Bao
Jingkang Wang
author_facet Sohrab Rohani
Yingying Zhao
Ying Bao
Jingkang Wang
author_sort Sohrab Rohani
collection DOAJ
description The objective of this work was to study the polymorphic transformation of carbamazepine from Form II to Form III in 1-propanol during seeded isothermal batch crystallization. First, the pure Form II and Form III were obtained and characterized. Then their solubilities and metastable zone limits were measured by in-situ attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy and focused beam reflectance measurement (FBRM). A transition temperature at about 34.2 °C was deduced suggesting the enantiotropic nature of this compound over the studied temperature range. To quantify the polymorph ratio during the transformation process, a new in-situ quantitative method was developed to measure the fraction of Form II by Raman spectroscopy. Successful tracking of the nucleation of the stable form and the transformation from Form II to Form III during isothermal crystallization was achieved by Raman spectroscopy and FBRM. The results from these three in-situ techniques, FBRM, FTIR and Raman were consistent with each other. The results showed a strong dependency on the amount of seeds added during isothermal crystallization.
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spelling doaj.art-495005d664164150a8f4085a865387122022-12-22T04:19:46ZengMDPI AGPharmaceutics1999-49232012-02-014116417810.3390/pharmaceutics4010164In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of CarbamazepineSohrab RohaniYingying ZhaoYing BaoJingkang WangThe objective of this work was to study the polymorphic transformation of carbamazepine from Form II to Form III in 1-propanol during seeded isothermal batch crystallization. First, the pure Form II and Form III were obtained and characterized. Then their solubilities and metastable zone limits were measured by in-situ attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy and focused beam reflectance measurement (FBRM). A transition temperature at about 34.2 °C was deduced suggesting the enantiotropic nature of this compound over the studied temperature range. To quantify the polymorph ratio during the transformation process, a new in-situ quantitative method was developed to measure the fraction of Form II by Raman spectroscopy. Successful tracking of the nucleation of the stable form and the transformation from Form II to Form III during isothermal crystallization was achieved by Raman spectroscopy and FBRM. The results from these three in-situ techniques, FBRM, FTIR and Raman were consistent with each other. The results showed a strong dependency on the amount of seeds added during isothermal crystallization.http://www.mdpi.com/1999-4923/4/1/164/carbamazepinepolymorph transformationin-situ quantitative methodin-situ analytical techniques
spellingShingle Sohrab Rohani
Yingying Zhao
Ying Bao
Jingkang Wang
In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine
Pharmaceutics
carbamazepine
polymorph transformation
in-situ quantitative method
in-situ analytical techniques
title In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine
title_full In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine
title_fullStr In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine
title_full_unstemmed In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine
title_short In Situ Focused Beam Reflectance Measurement (FBRM), Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Raman Characterization of the Polymorphic Transformation of Carbamazepine
title_sort in situ focused beam reflectance measurement fbrm attenuated total reflectance fourier transform infrared atr ftir and raman characterization of the polymorphic transformation of carbamazepine
topic carbamazepine
polymorph transformation
in-situ quantitative method
in-situ analytical techniques
url http://www.mdpi.com/1999-4923/4/1/164/
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