Characterization and quantification of microplastics and organic pollutants in mussels by microwave-assisted sample preparation and analytical pyrolysis

Sampling, separation, detection, and characterization of micro- and nanoplastic pollutants is a critical goal to assess their amount, fate, and the related hazards for ecosystems. There is still a major lack of understanding of the most relevant mechanisms of interaction and exchange of this class of pollutants with the environment and with organisms. In the last few years a number of studies highlighted the importance of the evaluation of the chemical species associated with the presence of microplastics in the environment, such as plasticizers, low-molecular weight degradation products, and different kinds of organic contaminants. In this work we combined microwave-assisted extraction and digestion, together with analytical pyrolysis coupled with gas chromatography and mass spectrometry (Py-GC-MS), to quantify microplastics together with different classes of associated pollutants. This method was developed using mussels as a matrix and it can be potentially applied to characterize and quantify, together with microplastics, polymer additives (phthalate plasticizers, UV stabilizers, etc.), polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and emerging contaminants like anti-inflammatory drugs. This method allowed the quantification of more than 40 different contaminants in a single chromatographic run, with recoveries higher that 87% in most cases and limits of detection/quantitation in the nanogram range. The method was also tested on a standard microplastic calibration mixture containing 11 different polymers, and recoveries higher than 84% were obtained in most cases. We developed a method to isolate and quantify various classes of both non-polymeric contaminants and polymers from mussel flour using microwave-assisted extraction/digestion and analytical pyrolysis-GC-MS.