Comprehensive characterization of nanostructured lipid carriers using laboratory and synchrotron X-ray scattering and diffraction

Carolin Tetyczka, Aden Hodzic, Manfred Kriechbaum, Krunoslav Juraić, Christina Spirk, Sonja Hartl, Elisabeth Pritz, Gerd Leitinger, Eva Roblegg*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review


The development of lipid nanoparticles requires knowledge on the crystalline structure, polymorphic transitions and lipid-drug interactions. This study aimed at introducing advanced techniques to characterize nanostructured lipid carriers (NLC) comprising palmitic acid, oleic acid, stabilizer and Domperidone. Crystallinity of single components and mixtures was investigated by laboratory Small Angle X-ray Scattering (SAXS). NLC were studied with laboratory Small and Wide Angle X-ray Scattering (SWAXS). Photon Correlation Spectroscopy and Freeze Fracture Transmission Electron Microscopy were used to monitor particle size, zeta potential and shape. Stability of NLC was investigated using synchrotron X-ray Diffraction (XRD) and SAXS and laboratory SAXS. Palmitic acid showed a lamellar structure (polymorph C), which was still present after particle preparation. Spherical 300 nm-sized particles with zeta potential values above −30 mV were obtained and Domperidone was incorporated in its amorphous form. During storage, no differences in synchrotron XRD spectra were seen. However, laboratory SAXS measurements showed a second lamellar structure, identified as polymorph B. Synchrotron SAXS temperature scans confirmed that polymorph B did not affect the morphology of the encapsulated drug or the shape of NLC. These results highlight the unique capabilities of laboratory and synchrotron X-ray Scattering and Diffraction for improved structural characterization of lipid nanoparticles.
Original languageEnglish
Pages (from-to)153-160
Number of pages8
JournalEuropean Journal of Pharmaceutics and Biopharmaceutics
Publication statusPublished - 2019


  • Laboratory small and wide angle X-ray scattering
  • Nanostructured lipid carriers (NLC)
  • Palmitic acid
  • Synchrotron small angle X-ray scattering
  • Synchrotron X-ray diffraction

ASJC Scopus subject areas

  • Biotechnology
  • Pharmaceutical Science


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