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Related Experiment Videos

Quantitative determination of polymorphic composition in intact compacts by parallel-beam X-ray powder

Wenjin Cao1, Simon Bates, Garnet E Peck

  • 1Department of Industrial and Physical Pharmacy, School of Pharmacy, 1336 Robert E. Heine Pharmacy Building, Purdue University, 47907-1336, West Lafayette, IN, USA.

Journal of Pharmaceutical and Biomedical Analysis
|November 1, 2002
PubMed
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This study introduces a new method using parallel-beam X-ray powder diffractometry to quantify crystal forms in intact compacts. This non-invasive technique accurately determines polymorphic composition without sample preparation.

Area of Science:

  • Pharmaceutical Sciences
  • Materials Science
  • Analytical Chemistry

Background:

  • Polymorphism significantly impacts drug properties and efficacy.
  • Accurate quantification of polymorphs in solid dosage forms is crucial for quality control.
  • Existing methods for polymorph analysis often require sample destruction or extensive preparation.

Purpose of the Study:

  • To develop and validate a novel, non-invasive method for determining polymorphic composition in intact pharmaceutical compacts.
  • To utilize parallel-beam X-ray powder diffractometry for quantitative analysis of co-existing polymorphs.
  • To establish a straightforward and reliable technique for polymorph quantitation in solid-state drug forms.

Main Methods:

  • Development of a parallel-beam X-ray powder diffractometry (PXRD) method.

Related Experiment Videos

  • Analysis of intact compacts of chlorpropamide and glycine polymorphic systems.
  • Quantification using the integrated intensity ratio of selected peaks and profile fitting.
  • Utilizing Shimadzu XRD-6000 software for data processing.
  • Main Results:

    • Excellent linear correlation was achieved for quantifying polymorphs in both chlorpropamide and glycine systems.
    • The method proved insensitive to the convex surface shape of the compacts.
    • This represents the first reported non-invasive X-ray diffraction quantitation of crystal forms in intact compacts.

    Conclusions:

    • Parallel-beam X-ray powder diffractometry offers a simple and effective non-invasive method for polymorph quantitation in intact compacts.
    • The technique eliminates the need for sample grinding or destruction, preserving sample integrity.
    • Further research is underway to apply this method to formulated tablets.