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Related Experiment Videos

Quantitative analysis of mannitol polymorphs. X-ray powder diffractometry--exploring preferred orientation effects.

Sarra N Campbell Roberts1, Adrian C Williams, Ian M Grimsey

  • 1Drug Delivery Group, School of Pharmacy, University of Bradford, West Yorkshire Bradford, UK.

Journal of Pharmaceutical and Biomedical Analysis
|June 7, 2002
PubMed
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Quantitative X-ray powder diffractometry (XRPD) of mannitol polymorphs is challenging due to preferred orientation effects. Reducing particle size and rotating samples significantly improves assay accuracy for detecting low levels of delta-mannitol.

Area of Science:

  • Pharmaceutical Sciences
  • Materials Science
  • Analytical Chemistry

Background:

  • Mannitol, a pharmaceutical excipient, exhibits polymorphism with alpha, beta, and delta forms.
  • Needle-like crystal morphology of mannitol polymorphs causes preferred orientation effects in X-ray powder diffractometry (XRPD).
  • Preferred orientation complicates accurate quantitative analysis using XRPD.

Purpose of the Study:

  • To investigate methods for minimizing preferred orientation effects in quantitative XRPD analysis of mannitol polymorphs.
  • To assess the impact of particle size reduction and sample rotation on assay accuracy.
  • To determine the limit of detection and quantitation for delta-mannitol in binary mixtures with beta-mannitol.

Main Methods:

  • Preparation of binary mixtures of beta and delta mannitol using particle size ranges <125 microm and 125-500 microm.

Related Experiment Videos

  • Quantitative analysis using X-ray powder diffractometry (XRPD) with static and rotating sample holders.
  • Investigation of various sources of assay error, including sample packing and mixing.

    • Main Results:

    • Reducing particle size to <125 microm and employing sample rotation halved the limits of detection and quantitation for delta-mannitol to 1% and 3.6%, respectively.
    • Sample rotation effectively minimized preferred orientation effects across both particle size ranges.
    • Sample packing and mixing were identified as significant contributors to assay variation, but rotation reduced most examined errors.

    Conclusions:

    • Combining sample rotation with particle size reduction is crucial for minimizing preferred orientation effects in XRPD.
    • This approach enhances assay accuracy, enabling the discrimination of similar mannitol polymorphs at low concentrations (around 1%).
    • The optimized method improves the reliability of quantitative XRPD analysis for polymorphic pharmaceutical excipients.