A comprehensive physicochemical characterization of heterogeneous nanoplastic (NPL) samples remains an analytical challenge requiring a combination of orthogonal measurement techniques to improve the accuracy and robustness of the results. Here, batch methods, including dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), tunable resistive pulse sensing (TRPS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM), as well as separation/fractionation methods such as centrifugal liquid sedimentation (CLS) and field-flow fractionation (FFF)–multi-angle light scattering (MALS) combined with pyrolysis gas chromatography mass spectrometry (pyGC–MS) or Raman microspectroscopy (RM) were evaluated for NPL size, shape, and chemical composition measurements and for quantification. A set of representative/test particles of different chemical natures, including (i) polydisperse polyethylene (PE), (ii) (doped) polystyrene (PS) NPLs, (iii) titanium dioxide, and (iv) iron oxide nanoparticles (spherical and elongated), was used to assess the applicability and limitations of the selected methodologies. Particle sizes and number-based concentrations obtained by orthogonal batch methods (DLS, NTA, TRPS) were comparable for monodisperse spherical samples, while higher deviations were observed for polydisperse, agglomerated samples and for non-spherical particles, especially for light scattering methods. CLS and TRPS offer further insight with increased size resolution, while detailed morphological information can be derived by electron microscopy (EM)–based approaches. Combined techniques such as FFF coupled to MALS and RM can provide complementary information on physical and chemical properties by online measurements, while pyGC–MS analysis of FFF fractions can be used for the identification of polymer particles (vs. inorganic particles) and for their offline (semi)quantification. However, NPL analysis in complex samples will continue to present a serious challenge for the evaluated techniques without significant improvements in sample preparation. Graphical abstract

In single particle inductively coupled plasma mass spectrometry (spICP-MS), the transport efficiency is fundamental for the correct determination of both particle number concentration and size. In the present study, transport efficiency was systematically determined on three different days with six carefully characterised gold nanoparticle (AuNP) suspensions and in seven European and US expert laboratories using different ICP-MS instruments and spICP-MS software. Both particle size—(TES)—and particle frequency—(TEF)—methods were applied. The resulting transport efficiencies did not deviate much under ideal conditions. The TEF method however systematically resulted in lower transport efficiencies. The extent of this difference (0–300% rel. difference) depended largely on the choice and storage conditions of the nanoparticle suspensions used for the determination. The TES method is recommended when the principal measurement objective is particle size. If the main aim of the measurement is the determination of the particle number concentration, the TEF approach could be preferred as it might better account for particle losses in the sample introduction system.

Biocompatible coating based on bovine serum albumin (BSA) was applied on two different TiO₂ nanoparticles (aeroxide P25 and food grade E171) to investigate properties and stability of resulting TiO₂@BSA composites, under the final perspective to create a "Safe-by-Design" coating, able to uniform, level off and mitigate surface chemistry related phenomena, as naturally occurring when nano-phases come in touch with proteins enriched biological fluids. The first step towards validating the proposed approach is a detailed characterization of surface chemistry with the quantification of amount and stability of BSA coating deposited on nanoparticles' surfaces. At this purpose, we implemented an orthogonal multi-techniques characterization platform, providing important information on colloidal behavior, particle size distribution and BSA-coating structure of investigated TiO₂ systems. Specifically, the proposed orthogonal approach enabled the quantitative determination of bound and free (not adsorbed) BSA, a key aspect for the design of intentionally BSA coated nano-structures, in nanomedicine and, overall, for the control of nano-surface reactivity. In fact, the BSA-coating strategy developed and the orthogonal characterisation performed can be extended to different designed nanomaterials in order to further investigate the protein-corona formation and promote the implementation of BSA engineered coating as a strategy to harmonize the surface reactivity and minimize the biological impact.

Zinc oxide nanoparticles (ZnO NPs) exhibit diverse morphologies and sizes, influencing their functional properties. However, the relationship between their morphology and behavior under varying conditions remains poorly understood. This study provides novel insights by linking ZnO NPs shape to generation of reactive oxygen species (ROS), and to antimicrobial efficacy under varying temperatures. ROS generation was confirmed via electron paramagnetic resonance, although no antioxidant activity was observed. Antibacterial tests against Escherichia coli and Staphylococcus aureus at different temperatures (4–22 °C) revealed that sheet-shaped NPs achieved complete bacterial reduction (7.5 log CFU mL⁻¹ for E. coli at 4 and 22 °C; 6.8 log CFU mL⁻¹ for S. aureus at 22 °C). Flower-shaped NPs were less effective due to larger size and reduced surface area. Zeta potential ranged from −44 to −58 mV, indicating high stability, with sheet-shaped particles being the most dispersed. Scanning electron microscopy confirmed closer interaction between sheet-shaped NPs and E. coli in agreement with the higher activity. Antibacterial efficacy decreased at 4 °C, highlighting implications for cold storage. The Weibull model successfully described E. coli reduction. These aspects were not previously addressed in the published work. The effect of temperature on the activity and its modeling are new insights into the morphology-dependent antimicrobial activity of ZnO NPs, supporting their integration into packaging materials for food applications.

Nanocellulose has attracted significant attention in recent years due to its distinctive properties and vast potential applications across various fields. This study encompasses two distinct yet interconnected activities: the characterisation of eight different types of nanocellulose test materials, including crystalline, fibrillated, and bacterial nanocellulose, using a range of analytical techniques such as dynamic light scattering (DLS), asymmetric flow field-flow fractionation (AF4) coupled to multi-angle light scattering (MALS) and DLS, and transmission electron microscopy (TEM), and a focused case study employing a tiered analytical approach to identify bacterial nanocellulose in commercially available food products like pudding and drinks with nata de coco, SCOBY, and kombucha. The results demonstrate that different types of nanocellulose can be distinguished by their unique physicochemical properties using a combination of analytical techniques. This finding was used for the identification of bacterial nanocellulose in food products by combining pyGC-MS for cellulose identification, TEM for nanosize range determination, and XRD for crystallinity analysis to distinguish between bacterial and fibrillated nanocellulose. The study advances fundamental understanding of nanocellulose and provides tools to facilitate potential future regulatory compliance.