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Phase transitions in frozen systems and during freeze-drying: quantification using synchrotron X-ray diffractometry.

Dushyant B Varshney1, Prakash Sundaramurthi, Satyendra Kumar

  • 1Department of Pharmaceutics, College of Pharmacy, University of Minnesota, Minneapolis, Minnesota 55455, USA. dushamaya@gmail.com

Pharmaceutical Research
|March 28, 2009
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Synchrotron X-ray diffraction (SXRD) monitored phase transitions during freeze-drying. Disodium hydrogen phosphate dodecahydrate (DHPD) crystallized and dehydrated incompletely during primary drying, with complete dehydration occurring during secondary drying.

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Area of Science:

  • Pharmaceutical Sciences
  • Materials Science

Background:

  • Freeze-drying (lyophilization) is a critical process for stabilizing pharmaceuticals.
  • Understanding phase transitions during freeze-drying is essential for optimizing product stability and formulation.

Purpose of the Study:

  • Develop a synchrotron X-ray diffraction (SXRD) method to monitor phase transitions throughout the entire freeze-drying cycle.
  • Investigate the influence of initial solute concentration on glycine and phosphate buffer salt crystallization during lyophilization.

Main Methods:

  • Utilized aqueous sodium phosphate buffered glycine solutions with varying molar ratios (1:3, 1:1, 3:1).
  • Employed a custom-designed sample cell for freeze-drying under controlled cooling, annealing, and vacuum conditions.
  • Acquired time-resolved 2D SXRD patterns using synchrotron X-ray radiation at different freeze-drying stages.

Main Results:

  • Observed ice formation followed by disodium hydrogen phosphate dodecahydrate (DHPD) crystallization upon cooling and annealing.
  • DHPD showed incomplete dehydration to amorphous disodium hydrogen phosphate during primary drying, with complete dehydration during secondary drying.
  • Higher initial buffer concentration relative to glycine inhibited glycine crystallization during freeze-drying.

Conclusions:

  • A sensitive SXRD method was successfully developed to simultaneously monitor all crystalline phases during freeze-drying.
  • The study quantified the impact of initial solute concentration on phase composition throughout the freeze-drying process.
  • DHPD crystallization and dehydration behavior were elucidated, highlighting the distinct roles of primary and secondary drying stages.