Industrial alkyd resins: characterization of pentaerythritol and phthalic acid esters using integrated mass spectrometry

Nasa, Jacopo La; Degano, Ilaria; Modugno, Francesca; Colombini, Maria Perla

doi:10.1002/rcm.7099

Cited by 25 publications

(11 citation statements)

References 26 publications

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“…The mass spectrometry system conditions were adapted from previous published works 16 , 18 , 29 , 30 , and the data elaboration was performed using MassHunter Workstation Software (B.04.00). The structures of all the identified species were interpreted by their MS 2 spectra 29 , 32 .…”

Section: Methodsmentioning

confidence: 99%

Long-lasting ergot lipids as new biomarkers for assessing the presence of cereals and cereal products in archaeological vessels

Łucejko

Nasa

Porta

et al. 2018

Sci Rep

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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.

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Section: Methodsmentioning

confidence: 99%

Long-lasting ergot lipids as new biomarkers for assessing the presence of cereals and cereal products in archaeological vessels

Łucejko

Nasa

Porta

et al. 2018

Sci Rep

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“…HPLC‐MS has been applied for the characterization and ageing study of the lipid profile of these resins (La Nasa et al, 2013b, 2014, 2015b). In detail, the alkyd paints were submitted to extraction in an ultrasonic bath at 60°C for 5 min.…”

Section: Analysis Of Paint Samplesmentioning

confidence: 99%

“…HR‐MS/MS mass spectrum (collision cell voltage set at 50 V) and fragmentation pattern of the [M + Na] + ion relative to LGlyPhGlyLn. Reprinted from La Nasa et al (2015b, 2020) with permission from Elsevier. HR‐MS/MS, high‐resolution tandem mass spectrometry.…”

Section: Analysis Of Paint Samplesmentioning

confidence: 99%

Liquid chromatography and mass spectrometry for the analysis of acylglycerols in art and archeology

Nasa

Modugno

Degano

2020

Mass Spectrometry Reviews

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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.

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“…This indicates the presence, in both samples, of metal carboxylates of fatty acids (palmitic and stearic mainly) and of diacids (suberic, azelaic and sebacic acid), and also of abietic and pimaric acids. The relatively high amount of dicarboxylic acids suggests the presence of a lipid material together with the resin: the application of this new approach does not allow to identify the precise origin of the materials and other approaches must be used for this purpose [34][35][36][37][38][39][40]. The Pinaceae resin shows different molecular patterns in the two samples.…”

Section: Characterization Of Free Aliphatic and Abietane Acids And Frmentioning

confidence: 99%

Two-step analytical procedure for the characterization and quantification of metal soaps and resinates in paint samples

et al. 2018

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Metal soaps and resinates are known to be spontaneously formed in artistic paintings, as a product of the reaction between aliphatic and terpenoid acids released by hydrolysis and oxidation of the organic media and certain cations contained in some inorganic pigments. In this paper we present an optimization and the validation of a GC/MS method for the qualitative and quantitative analysis of mixtures of terpenoid acids and aliphatic mono and dicarboxylic acids and metal carboxylates of terpenoid and aliphatic mono and dicarboxylic acids in the same paint microsample. This is based on a two-step analytical approach entailing the subsequent use of two silylating agents, N,O-bis(trimethylsilyl)trifluoroacetamide for the analysis of free acids and metal carboxylates, and 1,1,1,3,3,3-hexamethyldisilazane for the analysis of free acids. The application of this approach is possible because of the good stability at room temperature of the TMS derivatives of aliphatic and terpenoid species, characterized by high boiling points and relatively low vapour pressures. The method was then applied to the characterization of samples collected from two reference paint layers aged for 20 years, a paint sample taken from a pulpit, and sample of the varnish coating of a wooden writing desk, both from the second half of the seventeenth century.

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Industrial alkyd resins: characterization of pentaerythritol and phthalic acid esters using integrated mass spectrometry

Cited by 25 publications

References 26 publications

Long-lasting ergot lipids as new biomarkers for assessing the presence of cereals and cereal products in archaeological vessels

Long-lasting ergot lipids as new biomarkers for assessing the presence of cereals and cereal products in archaeological vessels

Liquid chromatography and mass spectrometry for the analysis of acylglycerols in art and archeology

Two-step analytical procedure for the characterization and quantification of metal soaps and resinates in paint samples

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