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Use of dynamic mechanical analysis (DMA) to determine critical transition temperatures in frozen bio.pdf

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Use of dynamic mechanical analysis (DMA) to determine critical transition temperatures in frozen bio

Cryobiology 61 (2010) 27–32Contents lists available at ScienceDirect Cryobiology journal homepage: www.elsevier .com/locate /ycryoUse of dynamic mechanical analysis (DMA) to determine critical transition temperatures in frozen biomaterials intended for lyophilizationq John Gearing a,1, Kiran P. Malik b, Paul Matejtschuk b,* aGearing Scientific Ltd., 4 Springhead, Ashwell, Hertfordshire, SG7 5LL, United Kingdom bNational Institute for Biological Standards and Control, Health Protection Agency, South Mimms, Potters Bar, Hertfordshire, EN6 3QG, United Kingdom a r t i c l e i n f oArticle history: Received 7 November 2009 Accepted 22 April 2010 Available online 27 April 2010 Keywords: Dynamic mechanical analysis Glass transition Frozen state Lyophilization Freeze drying Trehalose0011-2240/$ - see front matter 2010 Elsevier Inc. A doi:10.1016/j.cryobiol.2010.04.002 q No grants supported the work described which wa pursuance of their respective core business activities. * Corresponding author. Fax: +44 (0) 1707 641 520 E-mail addresses: gearingsci@ (J. Gearing .uk (P. Matejtschuk). 1 Fax: +44 (0) 1462 742 565.a b s t r a c t Dynamic mechanical analysis is widely used to determine glass transitions in solid state materials. How- ever, here we demonstrate the application of DMA for the determination of glass transitions (Tg’) in the frozen liquid state by means of a steel sample pocket. The use of the pocket allows frozen material to be analysed and glass transition events demonstrated. In addition, it allows weak glass transitions to be detected clearly in some complex formulations where they can be obscured by eutectic and other strong thermal events when other methods such as DSC or DTA are used. Classical excipients (trehalose, lactose, dextran) were analysed and shown to give reproducible Tg’ values, though with values slightly higher than those obtained by DSC. Finally, several complex real biological materials, typical of those encoun- tered when freeze drying biol