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Pharmaceutical Research

, Volume 24, Issue 5, pp 880–887 | Cite as

Crystallization Kinetics of Amorphous Griseofulvin by Pattern Fitting Procedure Using X-Ray Diffraction Data

  • Shigeo Yamamura
  • Rieko Takahira
  • Yasunori Momose
Research Paper

Abstract

Purpose

A pattern fitting procedure using X-ray powder diffraction patterns was applied to study the crystallization kinetics of amorphous griseofulvin. From the optimized parameters obtained by pattern fitting, a change in the quantity and quality of griseofulvin crystals with crystallization was also investigated.

Materials and Methods

Amorphous griseofulvin was prepared by cooling the melts followed by pulverization. X-ray diffraction patterns of amorphous griseofulvin were repeatedly measured every 20 h. The observed pattern was separated into crystalline diffraction intensity and amorphous scattering intensity by the nonlinear least-squares procedure.

Results

The fitting between the observed and simulated diffraction patterns was satisfactorily independent of the degree of crystallinity. Since a good linear relationship was found in a plot of amorphous scattering intensity against crystalline diffraction intensity, the degree of crystallinity can be determined according to Hermans’ method. The diffraction peak width increased with higher diffraction angles with crystallization. The crystallization was biphasic: fast and slow crystallization with the growth of low disordered crystals and disordered crystals, respectively.

Conclusion

The pattern fitting procedure is a powerful tool to analyze the X-ray diffraction patterns of semicrystalline materials. This procedure can simultaneously analyze the degree of crystallinity and crystal disorder in semicrystalline samples during crystallization.

Key words

crystallinity crystallization pattern fitting powder X-ray diffraction 

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Copyright information

© Springer Science+Business Media, LLC 2007

Authors and Affiliations

  • Shigeo Yamamura
    • 1
  • Rieko Takahira
    • 1
  • Yasunori Momose
    • 1
  1. 1.School of Pharmaceutical SciencesToho UniversityChibaJapan

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