Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles

This paper presents a comprehensive investigation of the manufacturing of itraconazole (ITZ) amorphous solid dispersions (ASDs) with Kolllidon® VA64 (KVA64) using hot-melt extrusion (HME) and in-line process monitoring, employing a Quality by Design (QbD) approach. A sequential Design of Experiments...

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Main Authors: Hetvi Triboandas, Mariana Bezerra, Juan Almeida, Matheus de Castro, Bianca Aloise Maneira Corrêa Santos, Walkiria Schlindwein
Format: Article
Language:English
Published: Elsevier 2024-12-01
Series:International Journal of Pharmaceutics: X
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Online Access:http://www.sciencedirect.com/science/article/pii/S259015672400080X
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author Hetvi Triboandas
Mariana Bezerra
Juan Almeida
Matheus de Castro
Bianca Aloise Maneira Corrêa Santos
Walkiria Schlindwein
author_facet Hetvi Triboandas
Mariana Bezerra
Juan Almeida
Matheus de Castro
Bianca Aloise Maneira Corrêa Santos
Walkiria Schlindwein
author_sort Hetvi Triboandas
collection DOAJ
description This paper presents a comprehensive investigation of the manufacturing of itraconazole (ITZ) amorphous solid dispersions (ASDs) with Kolllidon® VA64 (KVA64) using hot-melt extrusion (HME) and in-line process monitoring, employing a Quality by Design (QbD) approach. A sequential Design of Experiments (DoE) strategy was utilized to optimize the manufacturing process, with in-line UV–Vis spectroscopy providing real-time monitoring. The first DoE used a fractional factorial screening design to evaluate critical process parameters (CPPs), revealing that ITZ concentration had the most significant impact on the product quality attributes. The second DoE, employing a central composite design, explored the interactions between feed rate and screw speed, using torque and absorbance at 370 nm as responses to develop a design space. Validation studies confirmed process robustness across multiple days, with stable in-line UV–Vis spectra and consistent product quality using 30 % ITZ, 300 rpm, 150 °C and 7 g/min as the optimized process conditions. Theoretical and experimental analyses indicated that shifts in UV–Vis spectra at different ITZ concentrations were due to conformational changes in ITZ, which were confirmed through density functional theory (DFT) calculations and infrared spectroscopy. This work offers novel insights into the production and monitoring of ITZ-KVA64-ASDs, demonstrating that in-line UV–Vis spectroscopy is a powerful tool for real-time process monitoring and/or control.
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issn 2590-1567
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publishDate 2024-12-01
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spelling doaj-art-8987fd4e4ae440e3a5039380239bb4572025-08-20T02:36:38ZengElsevierInternational Journal of Pharmaceutics: X2590-15672024-12-01810030810.1016/j.ijpx.2024.100308Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principlesHetvi Triboandas0Mariana Bezerra1Juan Almeida2Matheus de Castro3Bianca Aloise Maneira Corrêa Santos4Walkiria Schlindwein5Leicester School of Pharmacy, De Montfort University, Leicester LE1 9BH, UKGlaxoSmithKline, David Jack Centre, Harris Lane, Ware, Hertfordshire SG12 0GX, UKApplied Materials, Daresbury WA4 4AB, UKLeicester School of Pharmacy, De Montfort University, Leicester LE1 9BH, UKLeicester School of Pharmacy, De Montfort University, Leicester LE1 9BH, UKLeicester School of Pharmacy, De Montfort University, Leicester LE1 9BH, UK; Corresponding author at: Leicester School of Pharmacy, Leicester LE1 9BH, UK.This paper presents a comprehensive investigation of the manufacturing of itraconazole (ITZ) amorphous solid dispersions (ASDs) with Kolllidon® VA64 (KVA64) using hot-melt extrusion (HME) and in-line process monitoring, employing a Quality by Design (QbD) approach. A sequential Design of Experiments (DoE) strategy was utilized to optimize the manufacturing process, with in-line UV–Vis spectroscopy providing real-time monitoring. The first DoE used a fractional factorial screening design to evaluate critical process parameters (CPPs), revealing that ITZ concentration had the most significant impact on the product quality attributes. The second DoE, employing a central composite design, explored the interactions between feed rate and screw speed, using torque and absorbance at 370 nm as responses to develop a design space. Validation studies confirmed process robustness across multiple days, with stable in-line UV–Vis spectra and consistent product quality using 30 % ITZ, 300 rpm, 150 °C and 7 g/min as the optimized process conditions. Theoretical and experimental analyses indicated that shifts in UV–Vis spectra at different ITZ concentrations were due to conformational changes in ITZ, which were confirmed through density functional theory (DFT) calculations and infrared spectroscopy. This work offers novel insights into the production and monitoring of ITZ-KVA64-ASDs, demonstrating that in-line UV–Vis spectroscopy is a powerful tool for real-time process monitoring and/or control.http://www.sciencedirect.com/science/article/pii/S259015672400080XAmorphous Solid Dispersion (ASD)Hot-Melt Extrusion (HME)Itraconazole (ITZ)Quality by Design (QbD), In-line UV–Vis spectroscopyDensity Functional Theory (DFT)Design of Experiments (DoE)
spellingShingle Hetvi Triboandas
Mariana Bezerra
Juan Almeida
Matheus de Castro
Bianca Aloise Maneira Corrêa Santos
Walkiria Schlindwein
Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles
International Journal of Pharmaceutics: X
Amorphous Solid Dispersion (ASD)
Hot-Melt Extrusion (HME)
Itraconazole (ITZ)
Quality by Design (QbD), In-line UV–Vis spectroscopy
Density Functional Theory (DFT)
Design of Experiments (DoE)
title Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles
title_full Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles
title_fullStr Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles
title_full_unstemmed Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles
title_short Optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in-line UV–Vis spectroscopy and QbD principles
title_sort optimizing extrusion processes and understanding conformational changes in itraconazole amorphous solid dispersions using in line uv vis spectroscopy and qbd principles
topic Amorphous Solid Dispersion (ASD)
Hot-Melt Extrusion (HME)
Itraconazole (ITZ)
Quality by Design (QbD), In-line UV–Vis spectroscopy
Density Functional Theory (DFT)
Design of Experiments (DoE)
url http://www.sciencedirect.com/science/article/pii/S259015672400080X
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