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Quantifying API polymorphs in formulations using X-ray powder diffraction and multivariate standard addition method

Alessandro Zappi1, Lucia Maini1, Giuliano Galimberti2

  • 1Department of Chemistry "G. Ciamician", University of Bologna, Bologna, Italy.

European Journal of Pharmaceutical Sciences : Official Journal of the European Federation for Pharmaceutical Sciences
|January 18, 2019
PubMed
Summary

This study introduces a novel method using X-ray Powder Diffraction and multivariate analysis for accurate quantification of active pharmaceutical ingredients in solid formulations. The technique overcomes matrix effects, enabling rapid analysis without sample pre-treatment.

Keywords:
ChemometricsDirect analysisNASRootProfSAMXRPD

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Pharmaceutical Sciences

Background:

  • Direct quantification of active pharmaceutical ingredients (APIs) in solid formulations presents significant challenges.
  • X-ray Powder Diffraction (XRPD) is a definitive technique for identifying polymorphs and crystal phases but faces limitations in quantitative analysis due to matrix effects.
  • Existing quantitative methods like Rietveld refinement and univariate calibration struggle with incomplete sample knowledge and the presence of amorphous phases.

Purpose of the Study:

  • To develop and validate a novel quantitative method for API polymorphs in solid formulations using XRPD.
  • To address the limitations of traditional quantitative XRPD methods, particularly matrix effects and the need for analytical blanks.
  • To enable rapid, pre-treatment-free analysis of polymorphic forms in pharmaceutical products.

Main Methods:

  • Application of a multivariate standard addition method (SAM) combined with the net analyte signal (NAS) procedure.
  • Utilizing X-ray Powder Diffraction (XRPD) for data acquisition.
  • Bypassing the need for a complete sample composition knowledge or an analytical blank.

Main Results:

  • Successfully quantified polymorphic forms of APIs in solid formulations without sample pre-treatment.
  • Demonstrated the efficacy of the multivariate SAM combined with NAS for overcoming matrix effects in XRPD.
  • Validated the method through two case studies: piracetam polymorphs (II and III) in binary mixtures and paracetamol (form I) in Tachifludec®.

Conclusions:

  • The developed method provides a reliable and rapid approach for the quantitative analysis of API polymorphs in solid formulations using XRPD.
  • This technique effectively overcomes the challenges posed by matrix effects and amorphous content, offering an advancement over existing methods.
  • The combined multivariate standard addition and net analyte signal procedure represents a significant step forward in quantitative XRPD for pharmaceutical analysis.