Anika Lokker, Pierre‐Hugues Stefanuto, Dries Cnuts, V. Rots, J.-F. Focant
{"title":"Optimization of Dynamic Headspace Sampling Conditions for the Identification of Paleolithic Adhesives","authors":"Anika Lokker, Pierre‐Hugues Stefanuto, Dries Cnuts, V. Rots, J.-F. Focant","doi":"10.1002/sscp.202400085","DOIUrl":null,"url":null,"abstract":"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.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.3000,"publicationDate":"2024-07-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"SEPARATION SCIENCE PLUS","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1002/sscp.202400085","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0
Abstract
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.