TY - JOUR

T1 - A comparative study of commercially available, minimally invasive, sampling methods on Early Neolithic humeri analysed via palaeoproteomics

AU - Hansen, Jakob

AU - Dekker, Joannes

AU - Troché, Gaudry

AU - Fagernäs, Zandra

AU - Olsen, Jesper V.

AU - Saña Seguí, Maria

AU - Welker, Frido

N1 - Funding Information: This project has received funding from the European Union's Horizon 2020 research and innovation programme under the Marie Sk\u0142odowska-Curie grant agreement No 956351 (ChemArch), the Horizon Europe MSCA Postdoctoral Fellowship grant agreement No 101106627 (PROMISE), and the European Research Council (ERC) grant agreement No. 948365 (PROSPER). This work also contributes to EarlyFoods (SGR-Cat-2021, 00527). Archaeological research at La Draga is made possible through the project \"Landscape modelization and resource management in the transition to farming in northeaster Iberia\u201D (PID2019-109254 GB-C21), funded by the Agencia Estatal de Investigaci\u00F3n (Spain), and \u201CLa Draga i la neolititzaci\u00F3 al NE de Catalunya, formaci\u00F3 i din\u00E0miques d'ocupaci\u00F3 del jaciment\u201D funded by Departament de Cultura de la Generalitat de Catalunya. Publisher Copyright: © 2024 The Authors

PY - 2024

Y1 - 2024

N2 - Due to methodological advances in the archaeological sciences, an increasing number of archaeological specimens undergo destructive sampling. However, the preservation of cultural heritage is a primary concern. This leads to a dilemma between accessing sample material and obtaining sufficient information for a meaningful analytical outcome. Ideally, sampling a specimen would preserve the object for further macro, micro, and molecular analyses. For palaeoproteomics, a number of minimally invasive sampling approaches have been proposed, representing different benefits and limitations. There have been studies comparing a selection of these protocols, however, these have focused on specimens from a homogenous preservation environment using Zooarchaeology by Mass Spectrometry (ZooMS). Here we expand on earlier work by extending the comparison to specimens from two highly different preservation environments through both ZooMS and liquid-chromatography tandem mass spectrometry (LC-MS/MS). We compare five sampling approaches and seven extraction protocols in total, on 10 Bos sp. humeri from the Early Neolithic site of La Draga, Spain, utilising MALDI-ToF MS and LC-MS/MS to generate proteomic output, while assessing protocol invasiveness using microscopy and 3D imaging. Five humeri originate from Sector A, which is mostly related to dry, terrestrial preservation conditions, while the other five humeri stem from Sector B, which is characterised by its phreatic/aquatic preservation conditions. We show that there is a significant difference in protein recovery and taxonomic specificity between the sampling techniques applied, as well as between burial conditions. Additionally, various surface modifications were observed depending on the specific sampling technique applied. It is therefore essential to assess protein preservation for each sedimentological context within an archaeological site before performing extensive sampling, as protein preservation can be highly inter- and intra-site-specific.

AB - Due to methodological advances in the archaeological sciences, an increasing number of archaeological specimens undergo destructive sampling. However, the preservation of cultural heritage is a primary concern. This leads to a dilemma between accessing sample material and obtaining sufficient information for a meaningful analytical outcome. Ideally, sampling a specimen would preserve the object for further macro, micro, and molecular analyses. For palaeoproteomics, a number of minimally invasive sampling approaches have been proposed, representing different benefits and limitations. There have been studies comparing a selection of these protocols, however, these have focused on specimens from a homogenous preservation environment using Zooarchaeology by Mass Spectrometry (ZooMS). Here we expand on earlier work by extending the comparison to specimens from two highly different preservation environments through both ZooMS and liquid-chromatography tandem mass spectrometry (LC-MS/MS). We compare five sampling approaches and seven extraction protocols in total, on 10 Bos sp. humeri from the Early Neolithic site of La Draga, Spain, utilising MALDI-ToF MS and LC-MS/MS to generate proteomic output, while assessing protocol invasiveness using microscopy and 3D imaging. Five humeri originate from Sector A, which is mostly related to dry, terrestrial preservation conditions, while the other five humeri stem from Sector B, which is characterised by its phreatic/aquatic preservation conditions. We show that there is a significant difference in protein recovery and taxonomic specificity between the sampling techniques applied, as well as between burial conditions. Additionally, various surface modifications were observed depending on the specific sampling technique applied. It is therefore essential to assess protein preservation for each sedimentological context within an archaeological site before performing extensive sampling, as protein preservation can be highly inter- and intra-site-specific.

KW - 3D scanning

KW - LC-MS/MS

KW - Microscopy

KW - Minimally invasive sampling

KW - Palaeoproteomics

KW - ZooMS

U2 - 10.1016/j.jas.2024.106002

DO - 10.1016/j.jas.2024.106002

M3 - Journal article

AN - SCOPUS:85193568996

VL - 167

JO - Journal of Archaeological Science

JF - Journal of Archaeological Science

SN - 0305-4403

M1 - 106002

ER -