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Approaches for the preparation and evaluation of hydrophilic polyethylene and polyethylene terephthalate microplastic particles suited for toxicological effect studies

Analytical and Bioanalytical Chemistry 2025 8 citations ? Citation count from OpenAlex, updated daily. May differ slightly from the publisher's own count. Score: 53 ? 0–100 AI score estimating relevance to the microplastics field. Papers below 30 are filtered from public browse.
Seghers John, Claudia Cella, Emmy Pequeur, Rita La Spina, Francesco Roncari, Andrea Valsesia, Dóra Méhn, Douglas Gilliland, Stefanie Trapmann, Håkan Emteborg

Summary

Researchers developed methods to create large quantities of artificially aged, hydrophilic microplastic particles from PET and polyethylene, eliminating the need for surfactants in toxicity experiments. Using alkaline and acidic treatments, they produced particles smaller than 5 micrometers with significantly increased water compatibility. These standardized, aged particles better represent real-world microplastics and could improve the consistency and relevance of laboratory toxicity studies.

When performing effect studies to investigate the impact of microplastic (MP) on cell lines, algae, or daphnia, it is advantageous if such experiments can be performed without the use of surfactants. The need for surfactants arises from the fact that finely milled pristine MP particles generally are hydrophobic. Methods for the preparation of larger amounts of hydrophilic and hence artificially aged MP particles and approaches for their characterization are of high importance. Here we present methods to artificially age polyethylene terephthalate (PET) and low-density polyethylene (PE) using alkaline and acidic treatments that reproducibly result in large quantities of particles below 5 µm with considerably increased hydrophilicity. The artificially aged MP particles were characterized using particle counting by single-particle extinction and scattering (SPES), particle size by laser diffraction measurements, zeta potential using electrophoretic light scattering, hydrophobicity index (Hy) through dark-field (DF) microscopy, chemical composition by inductively coupled plasma-mass spectrometry (ICP-MS), Fourier transform infrared (FTIR) microscopy, and Raman microscopy. The hydrophobicity index values obtained should allow the aged MP particles to be characterized as qualitative reference materials (RMs) with an ordinal property. Evidence for the maintained integrity and hydrophilicity of the artificially aged MP particles (in powder form) over time was obtained by measurements of zeta potential with a 33-month interval. Uniformity of subsampling with respect to particle number concentration in suspensions within a 10-day period was also investigated. It provided evidence for the possibility of reproducible spiking of a specific number of hydrophilic MP particles with relative standard deviations (RSDs) from 6.2 to 13.6%. For the development of future reference materials of artificially aged microplastics, they should be characterized for an ordinal property (artificial age as Hy-index) and nominal property (identity of PET or PE based on spectral matching).

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