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Sol LeWitt, a pioneer of conceptual art, created during his career over 1350 wall drawings, including the Wall Drawing #736 (1993) at the Center for Contemporary Art Luigi Pecci in Prato (Prato, Italy). The painting, executed by Andrea Marescalchi and Antony Sansotta under LeWitt's instructions, features a grid of coloured rectangles obtained by overlapping different layers of inks. During a 2021 restoration by the Wall Paintings and Stuccoes Department of the Opificio delle Pietre Dure (Firenze, Italy), an in-depth investigation of the composition and the materials used by LeWitt's assistants in producing Wall Drawing #736 was performed. A multi-analytical approach entailing Raman spectroscopy, high-performance liquid chromatography coupled to diode array and high-resolution mass spectrometry, gas chromatography–mass spectrometry (GC–MS), and pyrolysis coupled with GC–MS was applied. Our results revealed the use of animal glue, shellac resin, paraffin wax, linseed oil, and various organic pigments. The binder in the preparation layer was identified as poly(vinyl acetate), while poly(n-butyl methacrylate) was determined as a fixative. This research provided valuable insights into LeWitt's techniques. The acquired knowledge on the paint technique is highly relevant in supporting conservators in restoration and consolidating the many wall drawings produced exploiting the same technique all over the world. [ABSTRACT FROM AUTHOR]

Recently, a notable change has occurred in how street art murals are perceived by art history and the general public, with a growing recognition of their social and cultural significance and a new focus on preserving the most representative modern urban murals for future generations. An interesting case study is constituted by the "UBUNTU" mural (Ivan Pontevia and Daniele Castagnetti, Reggio Emilia, 2018), whose appearance has radically changed in a few years. Indeed, the intense and direct exposure to sunlight as well as the environmental and polluting agents have induced the bleaching and fading of the original highly fluorescent hues. To investigate the degradation processes that are occurring, five micro-samples were collected from different fluorescent-coloured areas and analysed by a combined approach based on µ-Raman and Surface Enhanced Raman Spectroscopy (SERS), High Performance Liquid Chromatography coupled with Diode Array Detector and mass spectrometry (HPLC-DAD and HPLC-MS), and Pyrolysis Gas Chromatography coupled with Mass Spectrometry (Py-GC-MS). The analytical protocol applied allowed us to disclose the painting materials used by the artist and fully characterise the ageing phenomena occurring in the mural that are possibly responsible for its colour ephemerality. [ABSTRACT FROM AUTHOR]

Lipid characterization in art and archeology, together with the study of lipid degradation processes, is an important research area in heritage science. Lipid‐based materials have been used as food since ancient times, but also employed as illuminants and as ingredients in cosmetic, ritual, and pharmaceutical preparations. Both animal and plant lipids have also been processed to produce materials used in art and crafts, such as paint binders, varnishes, waterproofing agents, and coatings. Identifying the origin of the lipid materials is challenging when they are found in association with artistic historical objects. This is due to the inherent complex composition of lipids, their widespread occurrence, and the chemical alterations induced by ageing. The most common approach for lipid characterization in heritage objects entails profiling fatty acids by gas chromatography/mass spectrometry after saponification or transesterification. New developments in high‐performance liquid chromatography coupled with mass spectrometry (HPLC‐MS) for the characterization of acylglycerols, together with more efficient sample treatments, have fostered the introduction of liquid chromatography for characterizing the lipid profile in heritage objects. This review reports the latest developments and applications of HPLC‐MS for the characterization of lipid materials in the field of heritage science. We describe the various approaches for sample pretreatment and highlight the advantages and limitations of HPLC‐MS in the analysis of paint and archeological samples. © 2020 John Wiley & Sons Ltd. [ABSTRACT FROM AUTHOR]

Since the second half of the 19th century, the world of textile production was radically changed both in terms of esthetics and of the performances leading to industrial products whose chemical properties were totally unknown and unexplored. Stage costumes are typical examples of multi-material art objects where different natural and synthetic materials were used to fulfil specific purposes. This research was performed in the framework of a diagnostic and restoration campaign of dresses of two Federico Fellini's movies ("Il Casanova" and "Roma"). For the characterization of the textile fibers, Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR-FTIR) and Pyrolysis Gas Chromatography coupled with Mass Spectrometry (Py-GC/MS) were employed. The structure of the metallic threads was investigated by Scanning Electron Microscopy coupled with Energy-Dispersive X-ray Spectroscopy (SEM-EDX). Dye identification was carried out by High Performance Liquid Chromatography coupled with Diode Array Detector and mass spectrometry (HPLC-DAD, HPLC-ESI-Q-ToF). The analytical approach adopted allowed us to fully characterize the costumes composed of natural, synthetic and artificial fibers dyed with complex mixtures of last generation synthetic dyes. The results collected were fundamental to fine-tune an effective restoration aimed at minimizing the damages due to ageing, inaccurate home-made restoration interventions, or poor conservation conditions. [ABSTRACT FROM AUTHOR]

A comprehensive picture of the chemical composition and structure of the acyl-glycerides from ergot (fungi of the genus Claviceps ) sclerotia was carried out using liquid chromatography coupled with high resolution mass spectrometry (HPLC-ESI-Q-ToF) following microwave solvent extraction. The method allowed us to study the chemical structures of >70 compounds being most of these reported and characterized here for the first time in ergot sclerotia. Diglycerides, triglycerides and estolides were proper preliminary separated using reverse phase chromatography and the unambiguous chemical structure of each species was characterized using high resolution tandem mass spectrometry. Our data and results could be useful for anyone interested in detecting ergot contaminations in cereals and deriving products, as alternative to the identification of alkaloids, in better understanding the behavior of ergot fungi in biological contest and in evaluating the potential uses of ergot estolides in industrial applications. [ABSTRACT FROM AUTHOR]

We propose a new analytical method using reverse phase High performance liquid chromatography (HPLC) coupled through an electrospray source with a tandem quadrupole-time-of-flight (ESI-Q-ToF) mass spectrometric detector for the full characterization and quantitation of the different classes of fatty acids and acylglycerols in lipid samples in a single chromatographic run. In this work, we optimized the derivatization reaction for free fatty acids with 2-hydrazinoquinoline, which is a low-cost approach, using a full factorial design. This reaction does not involve transesterification, thus enabling the free fatty acids to be separated and successfully quantified in the presence of mono-, di- and triacylglycerols without altering the whole glyceride profile. This new analytical method provides a full profile of fatty acids, mono-, di- and triglycerides within a relatively short chromatographic run (less than 40 min), with low operating back-pressure (less than 110 bar). The derivatization of the free fatty acids allows their detection in positive mode, with limits of detection in the range of 0.2–1.9 ng/g, and a dynamic range of two orders of magnitude. The figures of merit of the procedure are competitive with respect to the literature. The method was validated by characterizing two different types of olive oils. Free fatty acid content was quantified, and the results are consistent with literature data. The method was applied to the characterization of cow milk and an infant formula, after the precipitation of proteins and phospholipids, and proved suitable for the detection of short chain fatty acids, free fatty acids and glycerides highlighting differences in the composition of the two milks. The proposed procedure improves the current methods for the analysis of acylglyceride based materials, such as olive oil, and proved promising for the characterization of lipids in complex matrices, such as milk. [ABSTRACT FROM AUTHOR]

Highlights: [•] We characterized commercial alkyd paints used in contemporary art. [•] We used a multi-analytical approach based on mass spectrometry. [•] We present the first application of TAGs profiling by HPLC–ESI-Q-ToF to alkyd paints. [•] FIA-ESI-Q-ToF was tested for the first time for the analysis of alkyd paints. [ABSTRACT FROM AUTHOR]

Highlights: [•] We describe a new chromatographic method for qualitative and quantitative analysis of triglycerides mixtures. [•] We developed and validated a new method using a Poroshell 120 EC-C18 column. [•] We used for the first time a core–shell column coupled with an ESI-Q-ToF mass spectrometer system. [•] Reproducible and resolved chromatograms for more than 40 TAGs were acquired in 25min. [•] The new method was applied to a set of 10 reference plant oils. [Copyright &y& Elsevier]

Microplastics (MPs) quantification in benthic marine sediments is typically performed by time-consuming and moderately accurate mechanical separation and microscopy detection. In this paper, we describe the results of our innovative Polymer Identification and Specific Analysis (PISA) of microplastic total mass, previously tested on either less complex sandy beach sediment or less demanding (because of the high MPs content) wastewater treatment plant sludges, applied to the analysis of benthic sediments from a sublittoral area north-west of Leghorn (Tuscany, Italy). Samples were collected from two shallow sites characterized by coarse debris in a mixed seabed of Posidonia oceanica, and by a very fine silty-organogenic sediment, respectively. After sieving at <2 mm the sediment was sequentially extracted with selective organic solvents and the two polymer classes polystyrene (PS) and polyolefins (PE and PP) were quantified by pyrolysis-gas chromatography-mass spectrometry (Pyr-GC/MS). A contamination in the 8–65 ppm range by PS could be accurately detected. Acid hydrolysis on the extracted residue to achieve total depolymerization of all natural and synthetic polyamides, tagging of all aminated species in the hydrolysate with a fluorophore, and reversed-phase high performance liquid chromatography (HPLC) (RP-HPLC) analysis, allowed the quantification within the 137–1523 ppm range of the individual mass of contaminating nylon 6 and nylon 6,6, based on the detected amounts of the respective monomeric amines 6-aminohexanoic acid (AHA) and hexamethylenediamine (HMDA). Finally, alkaline hydrolysis of the residue from acid hydrolysis followed by RP-HPLC analysis of the purified hydrolysate showed contamination by polyethylene terephthalate (PET) in the 12.1–2.7 ppm range, based on the content of its comonomer, terephthalic acid. [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]

This work is focused on the chemical characterization of the organic residues preserved in ceramic fragments that are suspected to have been used by the Basque whalers in the period from 16th to 17th Century to store whale oil. The lipid profiling along with the identification of biomolecular markers, makes possible to obtain information on the contents of the vessels and on the transformations undergone by the organic substances during the burial process. To achieve this goal, two complementary analytical techniques, High-Performance Liquid Chromatography - Electrospray Ionization - Quadrupole Time-of-Flight Mass Spectrometry (HPLC-ESI-QToF) and Gas Chromatography-Mass Spectrometry (GC–MS), were used not only to study the archaeological materials but also fresh whale oil products used as reference materials with the aim to detect potential diagnostic biomarkers. HPLC-ESI-QToF was used to identify triacylglycerols (TAGs) and study their distribution in the various samples, whereas GC–MS after suitable derivatization provided the fatty acid (FA) profile together with the detection of degradation compounds (dicarboxylic and dihydroxy fatty acids) and biomarkers related to marine commodities (isoprenoid acids). Samples of blubber from 5 different whale species belonging to the genus Balaenoptera (fin, sei and minke whale), Megaptera (Humpback whale) and Phocoena (harbour porpoise) were used as reference materials together with a sample of whale oil of unknown origin. The chemical results confirm the archaeological data regarding the vessels use as containers to store whale oil and indicate the whales from Balaenoptera genus as the most probable source of the oil. [ABSTRACT FROM AUTHOR]