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Related Experiment Videos

Characterization of monoclinic crystals in tablets by pattern-fitting procedure using X-ray powder diffraction data.

Shigeo Yamamura1, Yasunori Momose

  • 1School of Pharmaceutical Sciences, Toho University, Miyama 2-2-1, Funabashi, Chiba 274-8510, Japan. yamamura@phar.toho-u.ac.jp

International Journal of Pharmaceutics
|June 6, 2003
PubMed
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This study used X-ray powder diffraction to analyze monoclinic crystals in tablets, revealing acetaminophen consolidates via fragmentation and benzoic acid via plastic deformation during compression. Pattern fitting is superior for characterizing crystalline drugs.

Area of Science:

  • Crystallography
  • Materials Science
  • Pharmaceutical Sciences

Background:

  • Understanding crystal deformation during tablet compression is crucial for drug formulation.
  • Monoclinic crystals present unique challenges in characterization due to their complex structures.

Purpose of the Study:

  • To characterize monoclinic crystals (acetaminophen, benzoic acid) in tablets using X-ray powder diffraction.
  • To evaluate crystal deformation during compression.
  • To compare the effectiveness of different functions for preferred orientation correction.

Main Methods:

  • X-ray powder diffraction (XRPD) data acquisition.
  • Fitting observed diffraction intensities to analytic expressions using non-linear least-squares.
  • Optimization of lattice parameters, peak-width, preferred orientation, and asymmetry parameters.

Related Experiment Videos

  • Application of Gauss and March distribution functions for preferred orientation correction.

    • Main Results:

    • The March function demonstrated superior performance in correcting preferred orientation effects, indicating fiber texture with axial orientation in crystallites.
    • Acetaminophen tablets showed significant peak broadening with increased compression pressure, suggesting consolidation by fragmentation.
    • Benzoic acid tablets exhibited minimal peak broadening, indicating consolidation by plastic deformation and molecular rearrangement.

    Conclusions:

    • Pattern fitting is a superior method for characterizing monoclinic crystalline drugs in tablets.
    • Acetaminophen consolidates via fragmentation, while benzoic acid consolidates via plastic deformation during compression.
    • The study provides insights into the distinct deformation mechanisms of crystalline materials under compression.