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X-ray Crystallography

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Discriminating the Interaction Anisotropy in Polymorphs Using Powder Brillouin Light Scattering.

Beth A Young¹, Lewis L Stevens¹

¹Department of Pharmaceutical Sciences and Experimental Therapeutics, University of Iowa, College of Pharmacy, Iowa City, IA 52241, United States.

Journal of Pharmaceutical Sciences

|September 13, 2021

Summary

This summary is machine-generated.

Powder Brillouin light scattering (p-BLS) reliably distinguishes drug polymorphs by analyzing sound velocities, offering a new non-destructive method for manufacturing quality control. This technique monitors intermolecular forces, crucial for ensuring final product performance.

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Area of Science:

Materials Science
Solid-State Chemistry
Analytical Chemistry

Background:

Drug product performance is critically dependent on solid-state form (polymorphism).
Current methods like Powder X-ray Diffraction (PXRD) are effective but not always suitable for continuous manufacturing.
There is a need for advanced Process Analytical Technologies (PATs) for real-time, non-destructive polymorph monitoring.

Purpose of the Study:

To introduce and validate powder Brillouin light scattering (p-BLS) as a novel PAT for discriminating between polymorphic forms of molecular solids.
To investigate the relationship between intermolecular forces and acoustic properties measurable by p-BLS.
To demonstrate the potential of p-BLS for in situ monitoring of solid-state transformations in pharmaceutical manufacturing.

Main Methods:

Application of powder Brillouin light scattering (p-BLS) to three model compounds (resorcinol, sulfamerazine, furosemide).
Analysis of anisotropic sound velocities and acoustic frequency distributions obtained from p-BLS spectra.
Interpretation of p-BLS data using hydrogen-bond analysis and computational energy frameworks (CrystalExplorer).

Main Results:

Distinct, polymorph-specific acoustic frequency distributions were successfully obtained using p-BLS.
The observed sound frequencies directly correlated with the strength and orientation of intermolecular forces within the crystal structures.
p-BLS demonstrated a reliable capability for discriminating between different polymorphic forms.

Conclusions:

p-BLS is a novel optical technique sensitive to intermolecular interaction forces in molecular solids.
p-BLS can reliably discriminate between polymorphs, offering a valuable alternative to traditional methods.
The technique holds significant potential for monitoring various pharmaceutically relevant processes like hydrate formation and co-crystallization in real-time.