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Dynamic Light Scattering on Nanoparticles in Microgravity in a Drop Tower

2022, Pyttlik, Andrea, Kuttich, Björn, Kraus, Tobias

Gravity affects colloidal dispersions via sedimentation and convection. We used dynamic light scattering (DLS) to quantify the mobility of nanoparticles on ground and in microgravity. A DLS instrument was adapted to withstand the accelerations in a drop tower, and a liquid handling set-up was connected in order to stabilize the liquid temperature and enable rapid cooling or heating. Light scattering experiments were performed in the drop tower at ZARM (Bremen, Germany) during a microgravity interval of 9.1 s and compared to measurements on ground. Particle dynamics were analyzed at constant temperature and after a rapid temperature drop using a series of DLS measurements with 1 s integration time. We observed nanoparticles with average gold core diameters of 7.8 nm and non-polar oleylamine shells that were dispersed in tetradecane and had an average hydrodynamic diameter of 21 nm. The particles did not change their diameter in the observed temperature range. The particle dynamics inferred from DLS on ground and in microgravity were in good agreement, demonstrating the possibility to perform reliable DLS measurements in a drop tower.

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Reliable release testing for nanoparticles with the NanoDis System, an innovative sample and separate technique

2021, Lombardo, Sonia M., Türeli, Nazende Günday, Koch, Marcus, Schneider, Marc, Türeli, Akif E.

One of the critical quality attributes of nanoparticle formulations is drug release. Their release properties should therefore be well characterized with predictive and discriminative methods. However, there is presently still no standard method for the release testing of extended release nanoformulations. Dialysis techniques are widely used in the literature but suffer from severe drawbacks. Burst release of formulations can be masked by slow permeation kinetics of the free drug through the dialysis membrane, saturation in the membrane, and absence of agitation in the membrane. In this study, the release profile of poly(lactic co-glycolic) (PLGA) nanocapsules loaded with all-trans retinoic acid was characterized using an innovative sample and separate set-up, the NanoDis System, and compared to the release profile measured with a dialysis technique. The NanoDis System showed clear superiority over the dialysis method and was able to accurately characterize the burst release from the capsules and furthermore discriminate between different all-trans retinoic acid nanoparticle formulations.

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High temporal-resolution scanning transmission electron microscopy using sparse-serpentine scan pathways

2021, Ortega, Eduardo, Nicholls, Daniel, Browning, Nigel D., de Jonge, Niels

Scanning transmission electron microscopy (STEM) provides structural analysis with sub-angstrom resolution. But the pixel-by-pixel scanning process is a limiting factor in acquiring high-speed data. Different strategies have been implemented to increase scanning speeds while at the same time minimizing beam damage via optimizing the scanning strategy. Here, we achieve the highest possible scanning speed by eliminating the image acquisition dead time induced by the beam flyback time combined with reducing the amount of scanning pixels via sparse imaging. A calibration procedure was developed to compensate for the hysteresis of the magnetic scan coils. A combination of sparse and serpentine scanning routines was tested for a crystalline thin film, gold nanoparticles, and in an in-situ liquid phase STEM experiment. Frame rates of 92, 23 and 5.8 s-1 were achieved for images of a width of 128, 256, and 512 pixels, respectively. The methods described here can be applied to single-particle tracking and analysis of radiation sensitive materials.