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Hydration and dehydration of crystalline and amorphous forms of raffinose

✍ Scribed by Azita Saleki-Gerhardt; Joseph G. Stoweell; Stephen R. Byrn; George Zografi


Book ID
102916596
Publisher
John Wiley and Sons
Year
1995
Tongue
English
Weight
564 KB
Volume
84
Category
Article
ISSN
0022-3549

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✦ Synopsis


The trisaccharide raffinose was prepared in its crystal pentahydrate, anhydrous methanolate, and amorphous forms and evaluated with regard to dehydration and hydration properties at various temperatures and relative humidities. The pentahydrate, when stored at relative humidities (RHs) of <60% but >lo%, showed no loss of water after 3 months of storage at 30 "C. When stored below 10% RH, only one water molecule could be removed over a period of 3 months, whereas within 24 h at 30 "C in a vacuum oven, two water molecules were removed with no change in crystal structure. Increasing the temperature to 60 "C progressively removed the remaining three molecules, causing the crystal, however, to collapse into an amorphous form identical to one prepared by lyophilization. Rehydration at 30 "C, which was sufficient to reduce the glass transition temperature to <30 "C, rapidly restored the pentahydrate crystal structure. Rehydration of the methanolate also restored the pentahydrate structure. The significant amount of water accommodated by raff inose in both the crystalline and amorphous forms would appear to make it a potentially useful water scavenger in certain types of dosage forms.


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Assessment of defects and amorphous stru
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The progressive conversion of crystalline raffinose pentahydrate to its amorphous form by dehydration at 608C, well below its melting temperature, was monitored by X-ray powder diffraction over a period of 72 h. The presence of defects within the crystal structure and any amorphous structure created