Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction
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Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction. / Karjalainen, Milja; Airaksinen, Sari; Rantanen, Jukka; Aaltonen, Jaakko; Yliruusi, Jouko.
In: Journal of Pharmaceutical and Biomedical Analysis, Vol. 39, No. 1-2, 01.09.2005, p. 27-32.Research output: Contribution to journal › Journal article › Research › peer-review
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TY - JOUR
T1 - Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction
AU - Karjalainen, Milja
AU - Airaksinen, Sari
AU - Rantanen, Jukka
AU - Aaltonen, Jaakko
AU - Yliruusi, Jouko
PY - 2005/9/1
Y1 - 2005/9/1
N2 - The aim of this study was to use variable temperature X-ray powder diffraction (VT-XRPD) to understand the solid-state changes in the pharmaceutical materials during heating. The model compounds studied were sulfathiazole, theophylline and nitrofurantoin. This study showed that the polymorph form of sulfathiazole SUTHAZ01 was very stable and SUTHAZ02 changed as a function of temperature to SUTHAZ01. Theophylline monohydrate changed via its metastable form to its anhydrous form during heating and nitrofurantoin monohydrate changed via amorphous form to its anhydrous form during heating. The crystallinity of SUTHAZ01, SUTHAZ02 and theophylline monohydrate were very high and stable. Nitrofurantoin monohydrate was also very crystalline at room temperature but during heating at lower temperatures the crystallinity decreased and started to increase strongly at the temperature where the sample had changed to the anhydrous form. The average crystallite size of sulfathiazole samples varied only a little during heating. The average crystallite size of both theophylline and nitrofurantoin monohydrate decreased during heating. However, the average crystallite size of nitrofurantoin monohydrate returned back to starting size at higher temperatures. These analyses showed that VT-XRPD can be used to effectively characterize polymorphic changes during heating.
AB - The aim of this study was to use variable temperature X-ray powder diffraction (VT-XRPD) to understand the solid-state changes in the pharmaceutical materials during heating. The model compounds studied were sulfathiazole, theophylline and nitrofurantoin. This study showed that the polymorph form of sulfathiazole SUTHAZ01 was very stable and SUTHAZ02 changed as a function of temperature to SUTHAZ01. Theophylline monohydrate changed via its metastable form to its anhydrous form during heating and nitrofurantoin monohydrate changed via amorphous form to its anhydrous form during heating. The crystallinity of SUTHAZ01, SUTHAZ02 and theophylline monohydrate were very high and stable. Nitrofurantoin monohydrate was also very crystalline at room temperature but during heating at lower temperatures the crystallinity decreased and started to increase strongly at the temperature where the sample had changed to the anhydrous form. The average crystallite size of sulfathiazole samples varied only a little during heating. The average crystallite size of both theophylline and nitrofurantoin monohydrate decreased during heating. However, the average crystallite size of nitrofurantoin monohydrate returned back to starting size at higher temperatures. These analyses showed that VT-XRPD can be used to effectively characterize polymorphic changes during heating.
KW - Nitrofurantoin
KW - Powder Diffraction
KW - Temperature
KW - Theophylline
KW - X-Ray Diffraction
U2 - 10.1016/j.jpba.2005.02.036
DO - 10.1016/j.jpba.2005.02.036
M3 - Journal article
C2 - 16085131
VL - 39
SP - 27
EP - 32
JO - Journal of Pharmaceutical and Biomedical Analysis
JF - Journal of Pharmaceutical and Biomedical Analysis
SN - 0731-7085
IS - 1-2
ER -
ID: 140622016