Micro-contextual identification of archaeological lipid biomarkers using resin-impregnated sediment slabs

Caterina Rodríguez de Vera; Antonio V. Herrera-Herrera; Margarita Jambrina-Enríquez; Santiago Sossa-Ríos; Jesús González-Urquijo; Talia Lazuen; Marine Vanlandeghem; Claire Alix; Gilliane Monnier; Goran Pajović; Gilbert Tostevin; Carolina Mallol

doi:10.1038/s41598-020-77257-x

Micro-contextual identification of archaeological lipid biomarkers using resin-impregnated sediment slabs

Caterina Rodríguez de Vera, Antonio V. Herrera-Herrera, Margarita Jambrina-Enríquez, Santiago Sossa-Ríos, Jesús González-Urquijo, Talia Lazuen, Marine Vanlandeghem, Claire Alix, Gilliane Monnier, Goran Pajović, Gilbert Tostevin, Carolina Mallol

Anthropology (Twin Cities)

Research output: Contribution to journal › Article › peer-review

14 Scopus citations

Abstract

Characterizing organic matter preserved in archaeological sediment is crucial to behavioral and paleoenvironmental investigations. This task becomes particularly challenging when considering microstratigraphic complexity. Most of the current analytical methods rely on loose sediment samples lacking spatial and temporal resolution at a microstratigraphic scale, adding uncertainty to the results. Here, we explore the potential of targeted molecular and isotopic biomarker analysis on polyester resin-impregnated sediment slabs from archaeological micromorphology, a technique that provides microstratigraphic control. We performed gas chromatography–mass spectrometry (GC–MS) and gas chromatography–isotope ratio mass spectromety (GC–IRMS) analyses on a set of samples including drill dust from resin-impregnated experimental and archaeological samples, loose samples from the same locations and resin control samples to assess the degree of interference of polyester resin in the GC–MS and Carbon-IRMS signals of different lipid fractions (n-alkanes, aromatics, n-ketones, alcohols, fatty acids and other high polarity lipids). The results show that biomarkers within the n-alkane, aromatic, n-ketone, and alcohol fractions can be identified. Further work is needed to expand the range of identifiable lipid biomarkers. This study represents the first micro-contextual approach to archaeological lipid biomarkers and contributes to the advance of archaeological science by adding a new method to obtain behavioral or paleoenvironmental proxies.

Original language	English (US)
Article number	20574
Journal	Scientific reports
Volume	10
Issue number	1
DOIs	https://doi.org/10.1038/s41598-020-77257-x
State	Published - Dec 2020

Bibliographical note

Funding Information:
This study has been funded by an ERC-Paleochar Consolidator Grant Project (ERC-2014-CoG-648871-PALEO-CHAR). Archaeological research at El Salt is currently funded by the Spanish Ministry of Science and Innovation (Project PID2019-107113RB-I00) and was funded by the Spanish Ministry of Economy, Industry and Competitiveness (Project HAR2015-68321-P) when sampling for this study took place. Additional financial support for El Salt fieldwork is from the Cultural Heritage Department of the Valencia Government and the Archaeological Museum Camil Visedo Moltó of Alcoy. Research at the Axlor site is funded by the Spanish Ministry of Science and Innovation (Project PID2019-107260GB-I00, PID2019-107113RB-I00). Research at Crvena Stijena is funded by the Montenegrin Ministry of Culture, the Montenegrin Academy of Sciences, the United States National Science Foundation (NSF-BCS 1758285), and the University of Minnesota’s Office of the Vice President of Research Grant-in-Aid program. Research at Cape Esperberg is funded by a collaborative grant from the US National Science Foundation (ARC-1523160, ARC-1523205, ARC-1523059, ARC-1523079) and from the Archeology Commission of the French Ministry of Foreign Affairs.

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© 2020, The Author(s).

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Rodríguez de Vera, C., Herrera-Herrera, A. V., Jambrina-Enríquez, M., Sossa-Ríos, S., González-Urquijo, J., Lazuen, T., Vanlandeghem, M., Alix, C., Monnier, G., Pajović, G., Tostevin, G., & Mallol, C. (2020). Micro-contextual identification of archaeological lipid biomarkers using resin-impregnated sediment slabs. Scientific reports, 10(1), Article 20574. https://doi.org/10.1038/s41598-020-77257-x

Rodríguez de Vera, C, Herrera-Herrera, AV, Jambrina-Enríquez, M, Sossa-Ríos, S, González-Urquijo, J, Lazuen, T, Vanlandeghem, M, Alix, C, Monnier, G, Pajović, G, Tostevin, G & Mallol, C 2020, 'Micro-contextual identification of archaeological lipid biomarkers using resin-impregnated sediment slabs', Scientific reports, vol. 10, no. 1, 20574. https://doi.org/10.1038/s41598-020-77257-x

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abstract = "Characterizing organic matter preserved in archaeological sediment is crucial to behavioral and paleoenvironmental investigations. This task becomes particularly challenging when considering microstratigraphic complexity. Most of the current analytical methods rely on loose sediment samples lacking spatial and temporal resolution at a microstratigraphic scale, adding uncertainty to the results. Here, we explore the potential of targeted molecular and isotopic biomarker analysis on polyester resin-impregnated sediment slabs from archaeological micromorphology, a technique that provides microstratigraphic control. We performed gas chromatography–mass spectrometry (GC–MS) and gas chromatography–isotope ratio mass spectromety (GC–IRMS) analyses on a set of samples including drill dust from resin-impregnated experimental and archaeological samples, loose samples from the same locations and resin control samples to assess the degree of interference of polyester resin in the GC–MS and Carbon-IRMS signals of different lipid fractions (n-alkanes, aromatics, n-ketones, alcohols, fatty acids and other high polarity lipids). The results show that biomarkers within the n-alkane, aromatic, n-ketone, and alcohol fractions can be identified. Further work is needed to expand the range of identifiable lipid biomarkers. This study represents the first micro-contextual approach to archaeological lipid biomarkers and contributes to the advance of archaeological science by adding a new method to obtain behavioral or paleoenvironmental proxies.",

author = "{Rodr{\'i}guez de Vera}, Caterina and Herrera-Herrera, {Antonio V.} and Margarita Jambrina-Enr{\'i}quez and Santiago Sossa-R{\'i}os and Jes{\'u}s Gonz{\'a}lez-Urquijo and Talia Lazuen and Marine Vanlandeghem and Claire Alix and Gilliane Monnier and Goran Pajovi{\'c} and Gilbert Tostevin and Carolina Mallol",

note = "Funding Information: This study has been funded by an ERC-Paleochar Consolidator Grant Project (ERC-2014-CoG-648871-PALEO-CHAR). Archaeological research at El Salt is currently funded by the Spanish Ministry of Science and Innovation (Project PID2019-107113RB-I00) and was funded by the Spanish Ministry of Economy, Industry and Competitiveness (Project HAR2015-68321-P) when sampling for this study took place. Additional financial support for El Salt fieldwork is from the Cultural Heritage Department of the Valencia Government and the Archaeological Museum Camil Visedo Molt{\'o} of Alcoy. Research at the Axlor site is funded by the Spanish Ministry of Science and Innovation (Project PID2019-107260GB-I00, PID2019-107113RB-I00). Research at Crvena Stijena is funded by the Montenegrin Ministry of Culture, the Montenegrin Academy of Sciences, the United States National Science Foundation (NSF-BCS 1758285), and the University of Minnesota{\textquoteright}s Office of the Vice President of Research Grant-in-Aid program. Research at Cape Esperberg is funded by a collaborative grant from the US National Science Foundation (ARC-1523160, ARC-1523205, ARC-1523059, ARC-1523079) and from the Archeology Commission of the French Ministry of Foreign Affairs. Publisher Copyright: {\textcopyright} 2020, The Author(s).",

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AU - Sossa-Ríos, Santiago

AU - González-Urquijo, Jesús

AU - Lazuen, Talia

AU - Vanlandeghem, Marine

AU - Alix, Claire

AU - Monnier, Gilliane

AU - Pajović, Goran

AU - Tostevin, Gilbert

AU - Mallol, Carolina

N1 - Funding Information: This study has been funded by an ERC-Paleochar Consolidator Grant Project (ERC-2014-CoG-648871-PALEO-CHAR). Archaeological research at El Salt is currently funded by the Spanish Ministry of Science and Innovation (Project PID2019-107113RB-I00) and was funded by the Spanish Ministry of Economy, Industry and Competitiveness (Project HAR2015-68321-P) when sampling for this study took place. Additional financial support for El Salt fieldwork is from the Cultural Heritage Department of the Valencia Government and the Archaeological Museum Camil Visedo Moltó of Alcoy. Research at the Axlor site is funded by the Spanish Ministry of Science and Innovation (Project PID2019-107260GB-I00, PID2019-107113RB-I00). Research at Crvena Stijena is funded by the Montenegrin Ministry of Culture, the Montenegrin Academy of Sciences, the United States National Science Foundation (NSF-BCS 1758285), and the University of Minnesota’s Office of the Vice President of Research Grant-in-Aid program. Research at Cape Esperberg is funded by a collaborative grant from the US National Science Foundation (ARC-1523160, ARC-1523205, ARC-1523059, ARC-1523079) and from the Archeology Commission of the French Ministry of Foreign Affairs. Publisher Copyright: © 2020, The Author(s).

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N2 - Characterizing organic matter preserved in archaeological sediment is crucial to behavioral and paleoenvironmental investigations. This task becomes particularly challenging when considering microstratigraphic complexity. Most of the current analytical methods rely on loose sediment samples lacking spatial and temporal resolution at a microstratigraphic scale, adding uncertainty to the results. Here, we explore the potential of targeted molecular and isotopic biomarker analysis on polyester resin-impregnated sediment slabs from archaeological micromorphology, a technique that provides microstratigraphic control. We performed gas chromatography–mass spectrometry (GC–MS) and gas chromatography–isotope ratio mass spectromety (GC–IRMS) analyses on a set of samples including drill dust from resin-impregnated experimental and archaeological samples, loose samples from the same locations and resin control samples to assess the degree of interference of polyester resin in the GC–MS and Carbon-IRMS signals of different lipid fractions (n-alkanes, aromatics, n-ketones, alcohols, fatty acids and other high polarity lipids). The results show that biomarkers within the n-alkane, aromatic, n-ketone, and alcohol fractions can be identified. Further work is needed to expand the range of identifiable lipid biomarkers. This study represents the first micro-contextual approach to archaeological lipid biomarkers and contributes to the advance of archaeological science by adding a new method to obtain behavioral or paleoenvironmental proxies.

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Micro-contextual identification of archaeological lipid biomarkers using resin-impregnated sediment slabs

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