PURPOSE: To study the solid-state and phase transitions of glycine, (i) in frozen aqueous solutions, and (ii) during freeze-drying. METHODS: X-ray powder diffractometry (XRD) and differential scanning calorimetry (DSC) were used to analyze the frozen systems. In situ freeze-drying in the sample chamber of the diffractometer enabled characterization of phase transitions during freeze-drying. RESULTS: Transitions in frozen systems. Rapid (20 degrees C/min) or slow (2 degrees C/min) cooling of aqueous solutions of glycine (15% w/w) to -70 degrees C resulted in crystallization of beta-glycine. Annealing at -10 degrees C led to an increase in the amount of the crystalline phase. When quench-cooled by immersing in liquid nitrogen, glycine formed an amorphous freeze-concentrate. On heating, crystallization of an unidentified phase of glycine occurred at approximately -65 degrees C which disappeared at approximately -55 degrees C, and the peaks of beta-glycine appeared. Annealing caused a transition of beta- to the -gamma- form. The extent of this conversion was a function of the annealing temperature. Slower cooling rates and annealing in frozen solutions increased the crystalline beta-glycine content in the Iyophile. Freeze-drying of quench-cooled solutions led to the formation of gamma-glycine during primary drying resulting in a lyophile consisting of a mixture of beta- and -gamma-glycine. The primary drying temperature as well as the initial solute concentration significantly influenced the solidstate of freeze-dried glycine only in quench-cooled systems. CONCLUSIONS: The cooling rate, annealing conditions and the primary drying temperature influenced the solid-state composition of freeze-dried glycine.
PURPOSE: To study the solid-state and phase transitions of glycine, (i) in frozen aqueous solutions, and (ii) during freeze-drying. METHODS: X-ray powder diffractometry (XRD) and differential scanning calorimetry (DSC) were used to analyze the frozen systems. In situ freeze-drying in the sample chamber of the diffractometer enabled characterization of phase transitions during freeze-drying. RESULTS: Transitions in frozen systems. Rapid (20 degrees C/min) or slow (2 degrees C/min) cooling of aqueous solutions of glycine (15% w/w) to -70 degrees C resulted in crystallization of beta-glycine. Annealing at -10 degrees C led to an increase in the amount of the crystalline phase. When quench-cooled by immersing in liquid nitrogen, glycine formed an amorphous freeze-concentrate. On heating, crystallization of an unidentified phase of glycine occurred at approximately -65 degrees C which disappeared at approximately -55 degrees C, and the peaks of beta-glycine appeared. Annealing caused a transition of beta- to the -gamma- form. The extent of this conversion was a function of the annealing temperature. Slower cooling rates and annealing in frozen solutions increased the crystalline beta-glycine content in the Iyophile. Freeze-drying of quench-cooled solutions led to the formation of gamma-glycine during primary drying resulting in a lyophile consisting of a mixture of beta- and -gamma-glycine. The primary drying temperature as well as the initial solute concentration significantly influenced the solidstate of freeze-dried glycine only in quench-cooled systems. CONCLUSIONS: The cooling rate, annealing conditions and the primary drying temperature influenced the solid-state composition of freeze-dried glycine.
Authors: Dushyant B Varshney; Satyendra Kumar; Evgenyi Y Shalaev; Shin-Woong Kang; Larry A Gatlin; Raj Suryanarayanan Journal: Pharm Res Date: 2006-08-23 Impact factor: 4.200
Authors: João Paulo T Baú; Cristine E A Carneiro; Antônio Carlos S da Costa; Daniel F Valezi; Eduardo di Mauro; Eduardo Pilau; Dimas A M Zaia Journal: Orig Life Evol Biosph Date: 2022-01-22 Impact factor: 1.120
Authors: Edward T Broadhurst; Hongyi Xu; Max T B Clabbers; Molly Lightowler; Fabio Nudelman; Xiaodong Zou; Simon Parsons Journal: IUCrJ Date: 2020-01-01 Impact factor: 4.769