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Quantitative Analysis by X-Ray Diffraction of the Inclusion Complex Formed by d-Limonene in a

H Yoshii1, T Furuta1,2, M Asada1

  • 1a Department of Biochemical Engineering , Toyama National College of Technology , Toyama 939 , Japan.

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|June 21, 2016
PubMed
Summary
This summary is machine-generated.

X-ray diffraction and NMR accurately measured d-Limonene and beta-Cyclodextrin (β-CD) inclusion complex levels in powders. Results correlated with d-Limonene molar fraction in beta-CD and maltodextrin mixtures.

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Area of Science:

  • Supramolecular Chemistry
  • Materials Science
  • Analytical Chemistry

Background:

  • Beta-Cyclodextrin (β-CD) is a cyclic oligosaccharide used for encapsulating guest molecules.
  • d-Limonene is a natural compound with various applications, often requiring stabilization.
  • Formation of inclusion complexes enhances the stability and bioavailability of guest molecules.

Purpose of the Study:

  • To quantify the inclusion complex formation between β-CD and d-Limonene.
  • To investigate the effect of maltodextrin as a co-former on complexation.
  • To validate analytical methods for complex characterization.

Main Methods:

  • X-ray diffraction (XRD) was employed to analyze the crystalline structure and complex formation.
  • Solid-state Carbon-13 Cross-Polarization Magic Angle Spinning Nuclear Magnetic Resonance ((13)C-CP/MAS NMR) was used for structural elucidation.
  • Relative integral intensities in XRD patterns were correlated with molar fractions.

Main Results:

  • XRD analysis showed a strong correlation between relative integral intensities (at 2θ=5-7° and 11-12°) and the molar fraction of d-Limonene.
  • The presence of maltodextrin in mixed powders did not hinder the accurate measurement of complex levels.
  • (13)C-CP/MAS NMR results corroborated the findings obtained by X-ray diffraction.

Conclusions:

  • X-ray diffraction is a reliable method for quantifying β-CD/d-Limonene inclusion complex levels in both pure β-CD and β-CD/maltodextrin systems.
  • Solid-state NMR provides complementary structural information that aligns with XRD data.
  • The study confirms the utility of these techniques for characterizing cyclodextrin inclusion complexes.