Optimization of Dynamic Headspace Sampling Conditions for the Identification of Paleolithic Adhesives

GC × GC–MS; headspace; natural substances; optimization; prehistory; Dynamic headspace; Dynamic headspace sampling; Gaschromatography-mass spectrometry; GC × gas chromatography–mass spectrometry; Headspaces; Identification method; Natural substance; Optimisations; Pine resin; Prehistory; Analytical Chemistry; Filtration and Separation

Abstract :

[en] The characterization of Paleolithic adhesives holds great potential for understanding human behavior and its evolution. Gas chromatography–mass spectrometry (GC–MS) is the most accurate identification method; unfortunately, it is destructive and requires a large sample size. Hence, most Paleolithic adhesives are not characterized with GC–MS. Here, a new nondestructive identification method is introduced; dynamic headspace (DHS) with two-dimensional GC coupled to a time-of-flight MS. The DHS extraction is optimized with an experimental design approach. Four parameters were selected, and the optimized values were as follows: incubation temperature: 50°C, incubation time: 20 min, purge volume: 450 mL, and purge flow: 22.5 mL min−1, pine resin was chosen as a proxy for Paleolithic adhesives. Subsequently, DHS was also tested on hide glue, which has less volatile than pine resin, and the universality of the extraction was tested. With untargeted techniques, a distinction between hide glue and pine resin could be made based on their chromatographic profiles. Lastly, DHS was tested against an existing HS-solid-phase microextraction method. DHS showed a higher response in the total area of the chemical groups of interest. Thus, DHS has a higher sensitivity for prehistoric adhesives than solid-phase microextraction, which is desired for minimal samples.

Disciplines :

Chemistry

Author, co-author :

Lokker, Anika ; Université de Liège - ULiège > Molecular Systems (MolSys)

Stefanuto, Pierre-Hugues ; Université de Liège - ULiège > Département de chimie (sciences)

Cnuts, Dries ; Université de Liège - ULiège > Unités de recherche interfacultaires > Art, Archéologie et Patrimoine (AAP)

Rots, Veerle ; Université de Liège - ULiège > Département des sciences historiques ; F.R.S-FNRS, Brussels, Belgium

Focant, Jean-François ; Université de Liège - ULiège > Département de chimie (sciences) > Chimie analytique, organique et biologique

Language :

English

Title :

Optimization of Dynamic Headspace Sampling Conditions for the Identification of Paleolithic Adhesives

Publication date :

15 July 2024

Journal title :

Separation Science Plus

eISSN :

2573-1815

Publisher :

John Wiley and Sons Inc

Peer reviewed :

Peer Reviewed verified by ORBi

Funding text :

This research was funded by the ARC\u2010project GLUE (PI: V. Rots) and the University of Li\u00E8ge through the collaborative research actions (Actions de Recherche Concert\u00E9e). V. Rots is also indebted to the F.R.S\u2010FNRS. Funding:

Available on ORBi :

since 07 August 2024

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