Insights into phase stability of anhydrous/hydrate systems: a Raman-based methodology
authors Nolasco, MM; Amado, AM; Ribeiro-Claro, PJA
nationality International
journal JOURNAL OF RAMAN SPECTROSCOPY
author keywords Raman spectroscopy; hydration/dehydration; kinetics; phase stability; caffeine
keywords RAY-POWDER-DIFFRACTION; SOLID-STATE REACTIONS; CRYSTALLINE CAFFEINE HYDRATE; X-RAY; PSEUDOPOLYMORPHIC TRANSITIONS; POLYMORPHIC TRANSFORMATION; PHARMACEUTICAL SOLIDS; QUANTITATIVE-ANALYSIS; MOLECULAR-CRYSTALS; PHYSICAL STABILITY
abstract FT-Raman spectroscopy turns out to be a powerful technique to evaluate the amount of polymorphic and pseudopolymorphic forms in crystalline samples - which is particularly relevant in pharmaceutical sciences. This paper presents a methodology that allows successful quantitative evaluation of the solid-state hydration and dehydration processes, using FT-Raman spectroscopy. All the steps required for a reliable evaluation of the hydration/dehydration process are illustrated for the caffeine system, a particularly challenging system presenting limited spectral differences between the pseudopolymorphs. The hydration process of caffeine was found to occur in a single-step process with a half-life time of ca 13 h, while the dehydration occurs through a two-step mechanism. The critical relative humidity was found to be at ca 81 and 42% for anhydrous and hydrate caffeine forms, respectively. Copyright (C) 2009 John Wiley & Sons, Ltd.
publisher JOHN WILEY & SONS LTD
issn 0377-0486
year published 2010
volume 41
issue 3
beginning page 340
ending page 349
digital object identifier (doi) 10.1002/jrs.2453
web of science category Spectroscopy
subject category Spectroscopy
unique article identifier WOS:000276649900013
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