Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools

<b>Background:</b> Active pharmaceutical ingredient (API) content is a critical quality attribute (CQA) of amorphous solid dispersions (ASDs) prepared by spraying a solution of APIs and polymers onto the excipients in fluid bed granulator. This study presents four methods for quantifying...

Full description

Saved in:
Bibliographic Details
Main Authors: Sandi Svetič, Laura Medved, Klemen Korasa, Franc Vrečer
Format: Article
Language:English
Published: MDPI AG 2024-12-01
Series:Pharmaceutics
Subjects:
Online Access:https://www.mdpi.com/1999-4923/16/12/1538
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1846103187163971584
author Sandi Svetič
Laura Medved
Klemen Korasa
Franc Vrečer
author_facet Sandi Svetič
Laura Medved
Klemen Korasa
Franc Vrečer
author_sort Sandi Svetič
collection DOAJ
description <b>Background:</b> Active pharmaceutical ingredient (API) content is a critical quality attribute (CQA) of amorphous solid dispersions (ASDs) prepared by spraying a solution of APIs and polymers onto the excipients in fluid bed granulator. This study presents four methods for quantifying API content during ASD preparation. <b>Methods:</b> Raman and three near-infrared (NIR) process analysers were utilized to develop methods for API quantification. Four partial least squares (PLS) models were developed using measurements from three granulation batches, with an additional batch used to evaluate model predictability. Models performance was assessed using metrics such as root mean square error of prediction (RMSEP), root mean square error of cross-validation (RMSECV), residual prediction deviation (RPD), and others. <b>Results:</b> Off-line and at-line NIR models were identified as suitable for process control applications. Additionally, at-line Raman measurements effectively predicted the endpoint of the spraying phase. <b>Conclusions:</b> To the best of authors’ knowledge, this is the first study focused on monitoring API content during fluidized bed granulation (FBG) used for ASD preparation. The findings provide novel insights into the application of Raman and NIR process analysers with PLS modelling for monitoring and controlling ASD preparation processes.
format Article
id doaj-art-1a04571de8fd44768d56db433edffca8
institution Kabale University
issn 1999-4923
language English
publishDate 2024-12-01
publisher MDPI AG
record_format Article
series Pharmaceutics
spelling doaj-art-1a04571de8fd44768d56db433edffca82024-12-27T14:46:25ZengMDPI AGPharmaceutics1999-49232024-12-011612153810.3390/pharmaceutics16121538Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology ToolsSandi Svetič0Laura Medved1Klemen Korasa2Franc Vrečer3KRKA, d. d., 8501 Novo Mesto, SloveniaKRKA, d. d., 8501 Novo Mesto, SloveniaKRKA, d. d., 8501 Novo Mesto, SloveniaFaculty of Pharmacy, University of Ljubljana, 1000 Ljubljana, Slovenia<b>Background:</b> Active pharmaceutical ingredient (API) content is a critical quality attribute (CQA) of amorphous solid dispersions (ASDs) prepared by spraying a solution of APIs and polymers onto the excipients in fluid bed granulator. This study presents four methods for quantifying API content during ASD preparation. <b>Methods:</b> Raman and three near-infrared (NIR) process analysers were utilized to develop methods for API quantification. Four partial least squares (PLS) models were developed using measurements from three granulation batches, with an additional batch used to evaluate model predictability. Models performance was assessed using metrics such as root mean square error of prediction (RMSEP), root mean square error of cross-validation (RMSECV), residual prediction deviation (RPD), and others. <b>Results:</b> Off-line and at-line NIR models were identified as suitable for process control applications. Additionally, at-line Raman measurements effectively predicted the endpoint of the spraying phase. <b>Conclusions:</b> To the best of authors’ knowledge, this is the first study focused on monitoring API content during fluidized bed granulation (FBG) used for ASD preparation. The findings provide novel insights into the application of Raman and NIR process analysers with PLS modelling for monitoring and controlling ASD preparation processes.https://www.mdpi.com/1999-4923/16/12/1538amorphous solid dispersionprocess analytical technologynear-infrared spectroscopyRaman spectroscopyfluidized bed granulationmultivariate analysis
spellingShingle Sandi Svetič
Laura Medved
Klemen Korasa
Franc Vrečer
Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools
Pharmaceutics
amorphous solid dispersion
process analytical technology
near-infrared spectroscopy
Raman spectroscopy
fluidized bed granulation
multivariate analysis
title Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools
title_full Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools
title_fullStr Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools
title_full_unstemmed Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools
title_short Quantification of Amlodipine Maleate Content in Amorphous Solid Dispersions Produced by Fluidized Bed Granulation Using Process Analytical Technology Tools
title_sort quantification of amlodipine maleate content in amorphous solid dispersions produced by fluidized bed granulation using process analytical technology tools
topic amorphous solid dispersion
process analytical technology
near-infrared spectroscopy
Raman spectroscopy
fluidized bed granulation
multivariate analysis
url https://www.mdpi.com/1999-4923/16/12/1538
work_keys_str_mv AT sandisvetic quantificationofamlodipinemaleatecontentinamorphoussoliddispersionsproducedbyfluidizedbedgranulationusingprocessanalyticaltechnologytools
AT lauramedved quantificationofamlodipinemaleatecontentinamorphoussoliddispersionsproducedbyfluidizedbedgranulationusingprocessanalyticaltechnologytools
AT klemenkorasa quantificationofamlodipinemaleatecontentinamorphoussoliddispersionsproducedbyfluidizedbedgranulationusingprocessanalyticaltechnologytools
AT francvrecer quantificationofamlodipinemaleatecontentinamorphoussoliddispersionsproducedbyfluidizedbedgranulationusingprocessanalyticaltechnologytools