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Title: A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole

Journal Article · · Thermochimica Acta
 [1];  [2];  [3];  [4];  [5];  [4];  [6];  [2]
  1. Argonne National Lab. (ANL), Argonne, IL (United States); Arizona State Univ., Tempe, AZ (United States)
  2. Arizona State Univ., Tempe, AZ (United States)
  3. Univ. of Sheffield, Sheffield (United Kingdom)
  4. Argonne National Lab. (ANL), Argonne, IL (United States)
  5. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  6. Purdue Univ., West Lafayette, IN (United States)
+ Show Author Affiliations

Small and wide angle high energy x-ray scattering experiments were performed upon cooling itraconazole from the melt to investigate the structural origin of the two transitions at similar to 74 degrees C and similar to 90 degrees C observed in DSC measurements. Slight changes to the main WAXS peak at Q=1.33 +/- 0.01 angstrom(-1) were observed at 90 degrees C and are found to be inter-molecular in nature, suggesting a liquid to isotropic transition. This finding was supported by complementary wide angle neutron scattering measurements. For temperatures at and below similar to 74 degrees C two strong rings appear in the 2D-SAXS pattern at Q= 0.24 +/- 0.01 angstrom(-1) and 0,43 +/- 0.01 angstrom(-1). The SAXS spectra were further deconvoluted into sharp and broad components. A narrowing of the broad component is associated with only minor changes in the packing arrangements of the itraconazole molecules below 90 degrees C, while the appearance of the sharp component below similar to 74 degrees C is attributed to the formation of a polydomain lamellar phase.

Research Organization:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC05-00OR22725; AC02-06CH11357; AC02-06CH1135
OSTI ID:
1329117
Alternate ID(s):
OSTI ID: 1364641; OSTI ID: 1396821
Journal Information:
Thermochimica Acta, Vol. 644, Issue C; ISSN 0040-6031
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 11 works
Citation information provided by
Web of Science

References (9)

Investigation of thermal properties of glassy itraconazole: identification of a monotropic mesophase journal September 2001
Mesomorphous versus traces of crystallinity: The itraconazole example journal December 2013
Molecular dynamics of itraconazole at ambient and high pressure journal January 2013
Structural Characterization and Aging of Glassy Pharmaceuticals made Using Acoustic Levitation journal April 2013
The Nanoscale Ordered MAterials Diffractometer NOMAD at the Spallation Neutron Source SNS
  • Neuefeind, Jörg; Feygenson, Mikhail; Carruth, John
  • Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, Vol. 287 https://doi.org/10.1016/j.nimb.2012.05.037
journal September 2012
cis-2-sec-Butyl-4-{4-[4-(4-{[2-(2,4-dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy}phenyl)-1-piperazinyl]phenyl}-2,4-dihydro-3H-1,2,4-triazol-3-one (Itraconazole) journal September 1996
X-ray Intermolecular Structure Factor ( XISF ): separation of intra- and intermolecular interactions from total X-ray scattering data journal May 2015
A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques journal October 2013
The Measurement of the Nematic Order Parameter by X-ray Scattering Reconsidered journal January 1995

Cited By (2)

Organic glasses with tunable liquid-crystalline order through kinetic arrest of end-over-end rotation: the case of saperconazole journal January 2020
Vapor deposition of a nonmesogen prepares highly structured organic glasses journal September 2019

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