Elizaveta Maksimova, David Wang, Megan Stierli, Nikolina Veljancic, Oya Tagit, Jörg Huwyler, Anne Bonnin, Jonathan De Roo. “Neutral ligands, distinct zeta potentials: consequences for hafnium oxide nanoparticles biodistribution.” ChemRxiv (). https://doi.org/10.26434/chemrxiv.15003826/v2

The main paper refers to supporting information, but no separate supporting information file was available on the ChemRxiv article page

HfO₂ nanoparticles
TEM, ellipsoidal dimensions (μ ± σ) Major axis: 3.8 ± 0.6 nm; Minor axis: 2.4 ± 0.4 nm
Main, p. 7
HfO₂ nanoparticles capped with NDA-PEG₁₀₀, NDA-ZW or NDA-PEG₂₀₀₀
¹H NMR NDA-PEG₁₀₀ and NDA-ZW showed broadened resonances; NDA-PEG₂₀₀₀ showed sharp signals for the PEG chains and especially for the terminal methoxy group
DOSY NMR NDA-PEG₂₀₀₀ had a lower diffusion coefficient than the free ligand
TGA, weight loss NDA-PEG₂₀₀₀ nanoparticles showed a larger weight loss than the nanoparticles with the two short ligands
DLS, hydrodynamic diameter at pH 7.4 NDA-PEG₁₀₀: 7.7 nm; NDA-ZW: 6.3 nm; NDA-PEG₂₀₀₀: 13.5 nm
DLS, pH-dependent Z-average All three formulations had a low Z-average in the physiological pH range and above; below pH 5, aggregation and an increase in the Z-average were observed
Zeta potential NDA-PEG₁₀₀ and NDA-ZW nanoparticles had substantially negative zeta potentials over the full investigated pH range; NDA-PEG₂₀₀₀ nanoparticles had a significantly less negative zeta potential over the investigated pH range and a zeta potential of −8 mV at pH 7
DLS in PBS over 24 h The Z-average did not increase; NDA-ZW and NDA-PEG₁₀₀ had slightly higher Z-averages than NDA-PEG₂₀₀₀; the nanoparticles with short chains had smaller hydrodynamic diameters
¹H NMR, TGA, DLS and zeta-potential plots Image data were not transcribed
Main, pp. 8–11
HfO₂ nanoparticles capped with NDA-PEG₁₀₀ and 10, 20 or 40 % NDA
DLS The zeta potential became progressively less negative and the Z-average increased with increasing amounts of NDA
Main, p. 10
HfO₂ nanoparticles after incubation with BSA
DLS, Z-average NDA-PEG₁₀₀ showed a slight but clear increase after 30 min and a further increase after 24 h; the increase for NDA-ZW was comparable to the BSA control; NDA-PEG₂₀₀₀ remained constant
SEC (Superose 6 column, HEPES buffer, pH 7.4), elution volume before incubation BSA: 16.8 mL, with a small native-aggregate peak at 15.7 mL; NDA-PEG₁₀₀: 17.2 mL; NDA-ZW: 17.0 mL; NDA-PEG₂₀₀₀: 14.4 mL
SEC after incubation The NDA-PEG₁₀₀ peak shifted completely toward a lower elution volume; NDA-ZW showed only a minimal change in its original elution volume; NDA-PEG₂₀₀₀ showed two distinct peaks corresponding to nanoparticles and free BSA
DLS of SEC fractions, NDA-PEG₁₀₀ Size increased slightly, up to 18 nm
Bradford assay of SEC fractions, NDA-PEG₂₀₀₀ No adsorbed BSA was detected
DLS and SEC plots Image data were not transcribed
Main, pp. 11–13
HfO₂ nanoparticles after incubation with FBS
DLS, Z-average The Z-average was dominated by proteins in the FBS mixture and could not be interpreted unambiguously
SEC with UV detection at 280 nm FBS had a dominant BSA peak at 16.8 mL and additional small peaks at 12.8, 21, 22 and 24 mL; NDA-PEG₁₀₀ showed a significant amount of larger aggregates; NDA-ZW showed a small amount of aggregates; NDA-PEG₂₀₀₀ showed little to no hard protein corona formation
DLS and SEC plots Image data were not transcribed