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Related Experiment Videos

The quantitative analysis of crystallinity using FT-Raman spectroscopy

L S Taylor1, G Zografi

  • 1School of Pharmacy, University of Wisconsin-Madison, 53706, USA.

Pharmaceutical Research
|June 10, 1998
PubMed
Summary

Fourier-transform Raman (FT-Raman) spectroscopy can accurately quantify the degree of crystallinity in indomethacin. This technique offers a sensitive method for detecting even small amounts of amorphous or crystalline content.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Pharmaceutical Analysis

Background:

  • Crystallinity significantly impacts drug properties, including solubility and bioavailability.
  • Accurate quantification of crystallinity is crucial for pharmaceutical development and quality control.
  • Existing methods for determining crystallinity may have limitations in certain applications.

Purpose of the Study:

  • To evaluate the efficacy of Fourier-transform Raman (FT-Raman) spectroscopy for the quantitative determination of the degree of crystallinity.
  • To establish a reliable method for quantifying amorphous and crystalline phases in a model compound, indomethacin.

Main Methods:

  • Preparation of indomethacin mixtures with varying proportions of amorphous and crystalline forms.
  • Utilizing the peak intensity ratio (1698 cm⁻¹ crystalline to 1680 cm⁻¹ amorphous) to construct a correlation curve.

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  • Validation of the correlation curve using samples of known composition and mechanically processed indomethacin.

    • Main Results:

    • A linear correlation was observed across the full spectrum of 0-100% crystallinity.
    • The method demonstrated sensitivity, detecting as little as 1% of either amorphous or crystalline content.
    • Inhomogeneities in sample mixing were identified as the primary source of error.
    • FT-Raman spectra of mechanically processed samples correlated well with calibration samples, allowing for crystallinity estimation.

    Conclusions:

    • FT-Raman spectroscopy presents a promising complementary technique for the quantitative analysis of crystallinity.
    • The method is sensitive and capable of quantifying crystallinity across a wide range.
    • Further refinement in sample preparation can minimize errors and enhance the reliability of the technique.