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Solvent-Free Bubbling Extraction Mass Spectrometryfor Ultrasensitive, Size-Independent Detection of Microplastics inWater

Analytical Chemistry 2026
Yupeng Li, Sining Li, Yuxin Leng, Min Zhang, Feng Yuan, Xinyue Li, Meiling Liu, Xingyu Li, Yi He, Yuanji Gao

Summary

Scientists developed a new, super-sensitive method to detect tiny microplastic particles in water, even ones far too small and too rare for older tests to catch. Using this tool, they found that plastic cups (like those made from polystyrene or "biodegradable" PLA) can shed microplastics into hot or cold liquids depending on temperature, which matters because it means everyday food packaging could be a hidden source of plastic exposure. This more precise detection method could help researchers better measure real-world microplastic contamination and its potential risks to human health.

Polymers

Abstract Ultratrace microplastics (MPs) in aquatic environments are a growing problem for ecosystems and human health, yet their reliable detection at subng/L levels with sub-100 nm particle sizes remains a substantial analytical challenge. Herein, we introduce a solvent-free and interface-driven bubbling extraction solid-phase microextraction gas chromatography mass spectrometry (BE−SPME−GC−MS) platform that enables ultrasensitive and size-independent detection of representative MPs (poly(methyl methacrylate) (PMMA), polystyrene (PS), and poly(lactic acid) (PLA)). The method combines bubble bursting−induced aerosol enrichment with the adsorptive microstructures of SPME coatings to achieve a dual solvent-free preconcentration pathway, facilitating the selective release of diagnostic volatile markers (methyl methacrylate, styrene, and lactide). The optimized system achieved limits of detection (LODs) of 80−180 pg/L, which are 3−6 orders of magnitude lower than those of conventional spectroscopic and pyrolysis-based approaches. The method exhibited excellent reproducibility (relative standard deviation <5%) and linearity, with correlation coefficients >0.999 over a broad concentration range. Field application to surface waters in Chengdu revealed MP concentrations below the LODs. Release tests revealed that PS cups exhibit temperature-dependent MP emissions, whereas PLA cups exhibit a nonmonotonic profile characterized by low-temperature brittleness, glass transition behavior, and high-temperature hydrolysis. Overall, this solvent-free, size-independent, and ultrasensitive analytical platform provides a robust tool for elucidating MP release behaviors and assessing real environmental exposure to ultratrace MPs in natural waters.

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