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Related Concept Videos

Polymer Classification: Crystallinity01:21

Polymer Classification: Crystallinity

Unlike ionic or small covalent molecules, polymers do not form crystalline solids due to the diffusion limitations of their long-chain structures. However, polymers contain microscopic crystalline domains separated by amorphous domains.
Crystalline domains are the regions where polymer chains are aligned in an orderly manner and held together in proximity by intermolecular forces. For example, chains in the crystalline domains of polyethylene and nylon are bound together by van der Waals...
Factors Affecting Dissolution: Polymorphism, Amorphism and Pseudopolymorphism01:21

Factors Affecting Dissolution: Polymorphism, Amorphism and Pseudopolymorphism

Polymorphism refers to the existence of a drug substance in multiple crystalline forms, known as polymorphs. Recently, this term has been expanded to include solvates (forms containing a solvent), amorphous forms (non-crystalline forms), and desolvated solvates (forms from which the solvent has been removed).
Some polymorphic crystals possess lower aqueous solubility than their amorphous counterparts, leading to incomplete absorption. For instance, the oral suspension of Chloramphenicol, which...
Ionic Crystal Structures02:42

Ionic Crystal Structures

Ionic crystals consist of two or more different kinds of ions that usually have different sizes. The packing of these ions into a crystal structure is more complex than the packing of metal atoms that are the same size.
Most monatomic ions behave as charged spheres, and their attraction for ions of opposite charge is the same in every direction. Consequently, stable structures for ionic compounds result (1) when ions of one charge are surrounded by as many ions as possible of the opposite...
Molecular and Ionic Solids02:54

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Crystalline solids are divided into four types: molecular, ionic, metallic, and covalent network based on the type of constituent units and their interparticle interactions.
Molecular Solids
Molecular crystalline solids, such as ice, sucrose (table sugar), and iodine, are solids that are composed of neutral molecules as their constituent units. These molecules are held together by weak intermolecular forces such as London dispersion forces, dipole-dipole interactions, or hydrogen bonds, which...
Pharmaceutical Alternatives: Polymorphic Form-Related and Particle Size-Related Therapeutic Nonequivalence01:27

Pharmaceutical Alternatives: Polymorphic Form-Related and Particle Size-Related Therapeutic Nonequivalence

Changes in polymorphic forms can significantly influence the bioavailability of poorly soluble drugs. Although the FDA defines pharmaceutical equivalence based on having the same active ingredient, dosage form, and route of administration, it does not automatically disqualify products with different polymorphic forms. This means two products with different polymorphs can still be deemed pharmaceutically equivalent. However, polymorphic differences can affect properties like wettability,...
Physical Properties of Carboxylic Acid Derivatives01:19

Physical Properties of Carboxylic Acid Derivatives

Intermolecular forces dictate several physical properties such as boiling points, melting points, solubilities, and so forth. They are classified into four types: ionic forces, hydrogen bonds, dipole–dipole forces, and dispersion forces. Ionic forces are the strongest, while dispersion forces are the weakest.
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Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses
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Solid-state characterization of amorphous and mesomorphous calcium ketoprofen.

Faraj Atassi1, Chen Mao, Ahmad S Masadeh

  • 1Eli Lilly and Company, Indianapolis, Indiana, USA.

Journal of Pharmaceutical Sciences
|September 26, 2009
PubMed
Summary

Pair distribution function (PDF) analysis reveals structural differences between crystalline, amorphous, and mesomorphous calcium ketoprofen. PDF and solid-state NMR (SSNMR) confirm partial molecular ordering in non-crystalline phases, with amorphous forms being more disordered than mesomorphous ones.

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Area of Science:

  • Pharmaceutical analysis
  • Solid-state chemistry
  • Materials science

Background:

  • Characterizing the solid-state forms of pharmaceuticals is crucial for drug development and formulation.
  • Amorphous and mesomorphous (liquid crystalline) phases present unique structural challenges compared to crystalline forms.
  • Pair distribution function (PDF) analysis offers a powerful tool for probing local atomic arrangements in disordered materials.

Purpose of the Study:

  • To explore the application of pair distribution function (PDF) analysis in pharmaceutical solid-state characterization.
  • To compare the structures of amorphous and mesomorphous calcium ketoprofen with its crystalline phase.
  • To develop optimal experimental parameters and peak assignment methods for PDF analysis of organic materials.

Main Methods:

  • X-ray powder diffraction (XRPD) and single crystal X-ray diffraction.
  • Spectroscopic techniques: Raman spectroscopy and solid-state Nuclear Magnetic Resonance (SSNMR), including variable-temperature SSNMR.
  • Pair distribution function (PDF) analysis.

Main Results:

  • Raman and SSNMR identified crystalline phases but struggled to differentiate amorphous and mesomorphous phases, indicating minimal differences in major chemical group environments.
  • Peak broadening in Raman and SSNMR spectra for non-crystalline phases suggested increased disorder.
  • PDF analysis showed that calcium-calcium and calcium-oxygen distances remained intact upon transformation from crystalline to disordered states, while other molecular parts became disordered. Variable-temperature SSNMR indicated the amorphous phase was more disordered than the mesomorphous phase.

Conclusions:

  • SSNMR and PDF analysis support the hypothesis that anhydrous calcium ketoprofen retains partial molecular order in non-crystalline states.
  • The amorphous phase exhibits greater disorder than the mesomorphous phase.
  • PDF analysis is a valuable technique for characterizing disordered pharmaceutical solids and understanding structural changes.