NDLI: Phase Transitions in Frozen Systems and During Freeze–Drying: Quantification Using Synchrotron X-Ray Diffractometry

Content Provider	Springer Nature Link
Author	Varshney, Dushyant B. Sundaramurthi, Prakash Kumar, Satyendra Shalaev, Evgenyi Y. Kang, Shin Woong Gatlin, Larry A. Suryanarayanan, Raj
Copyright Year	2009
Abstract	(1) To develop a synchrotron X-ray diffraction (SXRD) method to monitor phase transitions during the entire freeze–drying cycle. Aqueous sodium phosphate buffered glycine solutions with initial glycine to buffer molar ratios of 1:3 (17:50 mM), 1:1 (50 mM) and 3:1 were utilized as model systems. (2) To investigate the effect of initial solute concentration on the crystallization of glycine and phosphate buffer salt during lyophilization.Phosphate buffered glycine solutions were placed in a custom-designed sample cell for freeze–drying. The sample cell, covered with a stainless steel dome with a beryllium window, was placed on a stage capable of controlled cooling and vacuum drying. The samples were cooled to −50°C and annealed at −20°C. They underwent primary drying at −25°C under vacuum until ice sublimation was complete and secondary drying from 0 to 25°C. At different stages of the freeze–drying cycle, the samples were periodically exposed to synchrotron X-ray radiation. An image plate detector was used to obtain time-resolved two-dimensional SXRD patterns. The ice, β-glycine and DHPD phases were identified based on their unique X-ray peaks.When the solutions were cooled and annealed, ice formation was followed by crystallization of disodium hydrogen phosphate dodecahydrate (DHPD). In the primary drying stage, a significant increase in DHPD crystallization followed by incomplete dehydration to amorphous disodium hydrogen phosphate was evident. Complete dehydration of DHPD occurred during secondary drying. Glycine crystallization was inhibited throughout freeze–drying when the initial buffer concentration (1:3 glycine to buffer) was higher than that of glycine.A high-intensity X-ray diffraction method was developed to monitor the phase transitions during the entire freeze–drying cycle. The high sensitivity of SXRD allowed us to monitor all the crystalline phases simultaneously. While DHPD crystallizes in frozen solution, it dehydrates incompletely during primary drying and completely during secondary drying. The impact of initial solute concentration on the phase composition during the entire freeze–drying cycle was quantified.
Starting Page	1596
Ending Page	1606
Page Count	11
File Format	PDF
ISSN	07248741
Journal	Pharmaceutical Research
Volume Number	26
Issue Number	7
e-ISSN	1573904X
Language	English
Publisher	Springer US
Publisher Date	2009-03-27
Publisher Place	Boston
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	disodium hydrogen phosphate dodecahydrate glycine in situ freeze–drying phase transitions phosphate buffer synchrotron X-ray diffraction Biomedical Engineering Medical Law Biochemistry Pharmacy Pharmacology/Toxicology
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Pharmacology Molecular Medicine Pharmacology (medical) Biotechnology Pharmaceutical Science

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