Implications of global and local mobility in amorphous excipients as determined by DSC and TM DSC
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DRANCĂ, Ion, LUPASCU, F. Implications of global and local mobility in amorphous excipients as determined by DSC and TM DSC . In: Chemistry Journal of Moldova, 2009, nr. 2(4), pp. 105-115. ISSN 1857-1727.
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Chemistry Journal of Moldova
Numărul 2(4) / 2009 / ISSN 1857-1727 /ISSNe 2345-1688

Implications of global and local mobility in amorphous excipients as determined by DSC and TM DSC

Pag. 105-115

Drancă Ion, Lupascu F
 
Institutul de Chimie al AŞM
 
 
Disponibil în IBN: 11 decembrie 2013


Rezumat

The paper explores the use of differential scanning calorimetry (DSC) and temperature modulated differential scanning calorimetry (TM DSC) to study α- and β- processes in amorphous sucrose and trehalose. Amorphous sucrose was prepared by lyophilization while amorphous trehalose was prepared by dehydration of trehalose dihydrate. The variation in the effective activation energy of α-relaxation through glass transition has been determined by applying an isoconversional method. β-relaxations were studied by annealing glassy samples at different temperatures and subsequently heating at different rates in a differential scanning calorimeter. The effect of heating rate on the β-relaxation peak temperature formed the basis for the calculation of the activation energy. The higher density of glassy trehalose resulted in larger activation energy of α-relaxation compared to sucrose. The effect of temperature on viscous flow was greater in trehalose which can have implications on lyophile collapse. The size of the cooperatively rearranging regions was about the same for sucrose and trehalose suggesting similar dynamic heterogeneity at their respective glass transition temperatures. The activation energy of β-relaxations increased with annealing temperature due to increasing cooperative motions and the increase was larger in sucrose. The temperature at which β-relaxation was detected for a given annealing time was much less in sucrose implying that progression of local motions to cooperative motions occurred at lower temperatures in sucrose.

Cuvinte-cheie
molecular mobility; excipients (sucrose & trehalose); α- and β-relaxations; activation energy; DSC & TM DSC