PMID: 12751637May 20, 2003Paper

Crystalline to amorphous transition of disodium hydrogen phosphate during primary drying

Pharmaceutical Research
Abira PyneRaj Suryanarayanan

Abstract

To monitor the phase transitions during freeze-drying of disodium hydrogen phosphate. The variable temperature sample stage of the X-ray diffractometer (XRD) was attached to a vacuum pump, which enabled the entire freeze-drying process to be carried out in the sample chamber. The phase transitions during the freeze-drying cycle were monitored in real time by XRD. Aqueous buffer solution (containing disodium hydrogen phosphate and sodium dihydrogen phosphate) was cooled at 2 degrees C/min from room temperature to -70 degrees C. It was then heated to -25 degrees C and subjected to primary drying for 2 h at a chamber pressure of approximately 100 mTorr, followed by secondary drying at -10 degrees C. In the frozen solution, disodium hydrogen phosphate had crystallized as the dodecahydrate (Na2HPO4 x 12H2O) as was evident from its characteristic lines at approximately 5.37, 4.27, and 2.81 angstroms. Primary drying for 2 h resulted in ice sublimation, and the complete disappearance of the dodecahydrate peaks. The dehydration of the crystalline dodecahydrate resulted in an amorphous anhydrate. Thus the amorphous nature of the end product is a result of phase transitions during the process and do not reflect the solid-state of the ingr...Continue Reading

Citations

Aug 24, 2006·Pharmaceutical Research·Dushyant B VarshneyRaj Suryanarayanan
Dec 21, 2006·Pharmaceutical Research·Xiangmin LiaoRaj Suryanarayanan
Mar 24, 2005·Pharmaceutical Research·Koustuv ChatterjeeRaj Suryanarayanan
Sep 3, 2010·Pharmaceutical Research·Prakash SundaramurthiRaj Suryanarayanan
Apr 7, 2011·Archives of Pharmacal Research·Jung-Soon Song, Young-Taek Sohn
May 31, 2012·Archives of Pharmacal Research·Ji Yoon Ryu, Young-Taek Sohn
Jul 24, 2014·Archives of Pharmacal Research·In Jeong BangYoung Taek Sohn
Dec 31, 2010·Archives of Pharmacal Research·Hyun-Ok Song, Young-Taek Sohn
May 16, 2019·Pharmaceutical Research·Alpana A Thorat, Raj Suryanarayanan
Mar 24, 2011·European Journal of Pharmaceutics and Biopharmaceutics : Official Journal of Arbeitsgemeinschaft Für Pharmazeutische Verfahrenstechnik E.V·Julia Christina Kasper, Wolfgang Friess

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