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• A microwave-assisted solvent extraction method was used to extract microplastics and additives. • The double-shot Py-GC–MS allowed us to analyze additives and microplastics in two different runs. • The validated method provided recoveries higher than 96 % for phthalates and polystyrene. • The method was used to analyze samples of sand collected from a shoreline in Tuscany. • Data were obtained regarding the presence of plastic oxidation products. Pollution from microplastics (MPs) needs to be evaluated by deploying reliable analytical techniques that provide qualitative and quantitative data on the extent of contamination in the various environmental matrices. Solvent extraction of MPs followed by pyrolysis-gas chromatography-mass spectrometry (Py-GC–MS) provides data that not only regard the soluble plastics, but also the organic additives contained in MPs and the low-molecular weight degradation products of insoluble plastics. In this study, the potential of microwave-assisted solvent extraction and double-shot Py-GC–MS was investigated in order to obtain quali-quantitative information on polystyrene and on phthalate plasticizers in environmental samples. The method was validated and provided recoveries higher than 96 %, and detection limits lower than 1 ng and 1 μg for phthalates and polystyrene, respectively. We used the method to analyze samples of sand collected from a shoreline in Tuscany (central Italy) and thereby determine the content of phthalates and polystyrene at different depths and distances from the coastline. Qualitative data were also obtained regarding the presence of oxidation products derived from polyethylene and polypropylene. The different contents of plasticizers, plastics, and degradation products in the investigated samples are discussed in relation to how environmental agents affect the leaching and degradation processes of the polymers. [ABSTRACT FROM AUTHOR]

In this study, the sources, abundance, and ecological implications of microplastic (MP) pollution in Volturno, one of the main rivers in southern Italy, were explored by investigating the MP concentration levels in sediments collected along the watercourse. The samples were sieved through 5- and 2-mm sieves and treated with selective organic solvents. The polymer classes polystyrene (PS), polyethylene (PE), polypropylene (PP), polyethylene terephthalate (PET), polycarbonate (PC), nylon 6 (PA6), and nylon 6,6 (PA66) were quantified using pyrolysis–gas chromatography–mass spectrometry (Py-GC/MS) and high-performance liquid chromatography (HPLC). Furthermore, a 16S rRNA metagenomic analysis was performed using next-generation sequencing in Ion Torrent™ to explore the bacterial taxonomy and ecological dynamics of sediment samples. The MPs were detected in all samples collected from the study area. PP and PET were the most abundant and frequently detected polymer types in the analysed samples. The total MP concentration ranged from 1.05 to 14.55 ppm (parts per million), identifying two distinct data populations: high- and low-MP-contaminated sediments. According to the Polymer Hazard Index (PHI), MP pollution was categorised as hazard levels III and IV (corresponding to the danger category). Metagenomic data revealed that the presence of MPs significantly affected the abundance of bacterial taxa; Flavobacteraceae and Nocardiaceae , which are known to degrade polymeric substances, were present in high-MP-contaminated sediments. This study provides new insights into the ecological relevance of MP pollution and suggests that microorganisms may serve as biomarkers of MP pollution. [Display omitted] • Microplastic (MP) quantification in sediments was achieved using Py-GC/MS and HPLC. • MP pollution was highly variable along the river continuum. • Bacterial taxonomic abundance in sediment was altered by MP contamination. • Microbial biomarkers of river sediment MP pollution dynamics were identified. [ABSTRACT FROM AUTHOR]

The environmental pollution by plastic debris directly dispersed in or eventually reaching marine habitats is raising increasing concern not only for the vulnerability of marine species to ingestion and entanglement by macroscopic debris, but also for the potential hazards from smaller fragments down to a few micrometer size, often referred to as "microplastics". A novel procedure for the selective quantitative and qualitative determination of organic solvent soluble microplastics and microplastics degradation products (<2 mm) in shoreline sediments was adopted to evaluate their concentration and distribution over the different sectors of a Tuscany (Italy) beach. Solvent extraction followed by gravimetric determination and chemical characterization by FT-IR, Pyrolysis-GC-MS, GPC and 1 H NMR analyses showed the presence of up to 30 mg microplastics in 1 kg sand, a figure corresponding to about 5.5 g of generally undetected and largely underestimated microplastics in the upper 10 cm layer of a square meter of sandy beach ! The extracted microplastic material was essentially polystyrene and polyolefin byproducts from oxidative degradation and erosion of larger fragments, with accumulation mainly above the storm berm. Chain scission and oxidation processes cause significant variations in the physical and chemical features of microplastics, promoting their adsorption onto sand particles and thus their persistence in the sediments.

Cereals were very important in ancient diets, however evidence from archaeological sites of the vessels used for processing or storing cereals is comparatively rare. Micro-organisms, as well as chemical-physical effects can easily degrade cereals during the burial period. This can lead to a complete cereal decay and to serious difficulties in estimating the intensity of use of the cereals by ancient populations. Here, we present a novel biomarker approach entailing the detection of secondary lipid metabolites produced by ergot fungi (genus Claviceps), which are common cereal pests. The aim was to identify the original presence of Gramineae and to indirectly establish if vessels were used for cereal storage/processing. The fatty acid and TAG-estolide profiles of the remains from more than 30 archaeological vessels were investigated by gas chromatography/mass spectrometry (GC/MS) and high performance liquid chromatography/high resolution mass spectrometry (HPLC/ESI-Q-ToF). The detection of lipids derived from ergot in archaeological and historic contexts rests on its complex chemistry, providing a unique and relatively recalcitrant chemical signature for cereals. This research demonstrated that the combination of our innovative biomarker approach along with environmental and archaeological evidence can provide unprecedented insights into the incidence of cereals and related processing activities in ancient societies.