Laboratory Small-angle X-ray Scattering Research Articles

Small Angle X-Ray Scattering Data Analysis and Theoretical Modelling for the Size and Shape Characterization of Drug Delivery Systems Based on Vitamin E TPGS Micelles

We developed a simple two-dimensional/two-components theoretical model that describes the structure and functionality of a VitE-TPGS system of micelles assuming a hydrophobic inner core and an outer hydrated hydrophilic shell. We then conceptually applied the developed methodology to a simple system of VitE-TPGS micelles unloaded and loaded with an active pharmaceutical ingredient, eltrombopag, to verify if the model could reliably monitor the size change of the micelle upon loading. The fit of laboratory Small Angle X-Ray Scattering data against such model allows us to extract absolute values of the micelles size under a spherical shape hypothesis as well as the distribution within the system between components and level of hydration. The intensity scale of the SAXS experimental data needs to be normalized to a reference standard (pure water) to get absolute scattered intensities. The mathematical model which has been developed under a general hypothesis of ellipsoidal micelles, is applied to our experimental data under the simplified spherical assumption, which suitably fits our experimental data.

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

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.

Combining SAXS and DLS for simultaneous measurements and time-resolved monitoring of nanoparticle synthesis

Time-resolved characterization of nano-particle (NP) synthesis is a promising mean to produce NPs under controlled conditions. Here, an innovative experimental demonstration of a NP characterization tool which combines a laboratory Small Angle X-ray Scattering (SAXS) instrument, a new Dynamic Light Scattering (DLS) device and a microflow reactor is shown. The complementary SAXS and DLS techniques were designed and optimized to meet the ambitious requirements of time-resolved monitoring of NP suspensions while ongoing synthesis. For this purpose, SAXS instrument performance was enhanced by the implementation and optimization of a unique X-ray metal jet source. In parallel, an innovative DLS fiber remote probe head was developed specifically for in situ measurements. DLS measurements were performed directly inside a 2.0mm diameter glass capillary located inside the SAXS vacuum sample chamber. The combined SAXS and DLS devices were tested separately on commercially available gold NP suspensions of known size. Furthermore, simultaneous SAXS and DLS measurements were performed during the synthesis of silica NPs.

Setup for in situ WAXS/SAXS studies of the formation and growth of Bi nanodroplets and the melting of Bi nanocrystals using synchrotron radiation

The setup was designed for in situ studies of structural transformations in materials at high temperatures. It makes possible simultaneous recording of wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS) spectra from room temperature up to 1000 °C. The setup was installed in the National Synchrotron Light Laboratory SAXS beamline. It was applied to in situ studies of several structural transformations such as the formation and growth of liquid Bi nanodroplets embedded in a B 2O 3–Na 2O glass and the melting of Bi nanocrystals dispersed in the same glass matrix.