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Discrete EntityAnalysis via Microwave-Induced NitrogenPlasma–Mass Spectrometry in Single-Event Mode

Figshare 2025
Ana Rua-Ibarz (3131703), Flávio V. Nakadi (22426512), Eduardo Bolea-Fernandez (1770388), Antonio Bazo (21503549), Beatrice Battistella (8712789), Anna Matiushkina (22145922), Ute Resch-Genger (626347), Carlos Abad (11090249), Martín Resano (1770391)

Summary

Researchers evaluated single-event microwave-induced nitrogen plasma mass spectrometry (MINP-MS) for the first time to analyse discrete entities including iron oxide nanoparticles (20-70 nm), selenium nanoparticles, biological cells, and 2-3 µm polystyrene and PTFE microplastics. The nitrogen-based plasma overcame argon polyatomic interferences, achieved an iron detection limit of 8.6 ag (equivalent to 19 nm particle size), and successfully characterised multiple particle types in a single analytical framework.

Polymers

In this work, single-event microwave-induced nitrogen plasma–mass spectrometry (single-event MINP-MS) was evaluated for the first time for the analysis of discrete entities such as nanoparticles, biological cells, and microplastics. Nitrogen (N2) effectively overcomes Ar-based polyatomic interferences, enabling (ultra)trace element determination of Fe and Se using their most abundant isotopes, 56Fe (91.66%) and 80Se (49.82%). Iron oxide nanoparticles (Fe2O3 NPs) ranging from 20 to 70 nm were accurately characterized, with excellent agreement with established sizing techniques, such as transmission electron microscopy (TEM) and dynamic light scattering (DLS). A limit of detection (LoD) of 8.6 ag for Feequivalent to an LoDsize of 19 nm for Fe2O3was achieved, which is significantly lower than recent values reported for high-end quadrupole-based ICP-MS. Selenium nanoparticles (SeNPs) of 150 and 250 nm were also accurately characterized, without the N2-based plasma experiencing issues handling relatively large metallic NPs (linearity, R2 = 0.9994). Se-enriched yeast cells (SELM-1 certified reference material) were successfully analyzed via single-cell MINP-MS using external calibration based on SeNPs and a transport efficiency-independent approach. In addition, 2–3 μm polystyrene (PS) and polytetrafluoroethylene (PTFE) were accurately sized by monitoring 12C+, confirming the method’s suitability for handling micrometer-sized polymeric materials (microplastics). The average duration of individual events (680 ± 160 μs) suggests that the digestion of individual entities in N2-based plasmas is comparable to that in Ar-based plasmas. These results open new avenues for this instrumentation as an alternative to ICP ionization sources, also in the context of discrete entity analysis.

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