Abstract:

Residues from ancient artifacts can help identify which plant species were used for their psychoactive properties, providing important information regarding the deep-time co-evolutionary relationship between plants and humans. However, relying on the presence or absence of one or several biomarkers has limited the ability to confidently connect residues to particular plants. We describe a comprehensive metabolomics-based approach that can distinguish closely related species and provide greater confidence in species use determinations. An ~1430-year-old pipe from central Washington State not only contained nicotine, but also had strong evidence for the smoking of Nicotiana quadrivalvis and Rhus glabra, as opposed to several other species in this pre-contact pipe. Analysis of a post-contact pipe suggested use of different plants, including the introduced trade tobacco, Nicotiana rustica. Ancient residue metabolomics provides a new frontier in archaeo-chemistry, with greater precision to investigate the evolution of drug use and similar plant-human co-evolutionary dynamics.

Keywords: ancient residue metabolomics; archaeology; caffeine; nicotine; pre-contact pipe; psychoactive compound; smooth sumac; tobacco.

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An Ancient Residue Metabolomics-Based Method to Distinguish Use of Closely Related Plant Species in Ancient Pipes

^{Institute of Biological Chemistry, Washington State University, Pullman, WA, United States}

^{Department of Anthropology, Washington State University, Pullman, WA, United States}

^{Department of Civil and Environmental Engineering, Washington State University, Pullman, WA, United States}

Edited by: Robert David Hall, Wageningen University and Research, Netherlands

Reviewed by: Takayuki Tohge, Nara Institute of Science and Technology (NAIST), Japan; Lena Fragner, University of Vienna, Austria

*Correspondence: Shannon Tushingham ude.usw@mahgnihsut.nonnahs

David R. Gang ude.usw@dgnag

This article was submitted to Metabolomics, a section of the journal Frontiers in Molecular Biosciences

†Present address: Korey J. Brownstein, Department of Molecular Genetics and Cell Biology, The University of Chicago, Chicago, IL, United States

Edited by: Robert David Hall, Wageningen University and Research, Netherlands

Reviewed by: Takayuki Tohge, Nara Institute of Science and Technology (NAIST), Japan; Lena Fragner, University of Vienna, Austria

Received 2020 Feb 20; Accepted 2020 Jun 4.

This is an open-access article distributed under the terms of the Creative Commons Attribution License (CC BY). The use, distribution or reproduction in other forums is permitted, provided the original author(s) and the copyright owner(s) are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. No use, distribution or reproduction is permitted which does not comply with these terms.

Abstract

Residues from ancient artifacts can help identify which plant species were used for their psychoactive properties, providing important information regarding the deep-time co-evolutionary relationship between plants and humans. However, relying on the presence or absence of one or several biomarkers has limited the ability to confidently connect residues to particular plants. We describe a comprehensive metabolomics-based approach that can distinguish closely related species and provide greater confidence in species use determinations. An ~1430-year-old pipe from central Washington State not only contained nicotine, but also had strong evidence for the smoking of Nicotiana quadrivalvis and Rhus glabra, as opposed to several other species in this pre-contact pipe. Analysis of a post-contact pipe suggested use of different plants, including the introduced trade tobacco, Nicotiana rustica. Ancient residue metabolomics provides a new frontier in archaeo-chemistry, with greater precision to investigate the evolution of drug use and similar plant-human co-evolutionary dynamics.

Keywords: ancient residue metabolomics, archaeology, caffeine, nicotine, pre-contact pipe, psychoactive compound, smooth sumac, tobacco

Acknowledgments

We would like to thank Mario Zimmermann for assisting with the experimental pipes; Anna Berim and Jeong-Jin Park for assistance with operation of the GC- and LC-MS instruments used in this investigation; Todd Coffey for statistical assistance; Amy Hetrick, Julie Thayer, Devon Thrasher, and Susan Vogtman for growth chamber and greenhouse assistance; and the USDA ARS National Plant Germplasm System for providing the Nicotiana seeds.

Footnotes

Funding. This research was supported by the National Science Foundation under Grant #1419506. We also acknowledge support from the National Science Foundation Graduate Research Fellowship Program (NSF GRFP), Achievement Rewards for College Scientists (ARCS) Foundation, Seattle ARCS Chapter, and Anne and Russ Fuller Fellowship for Interdisciplinary Research to KB. This work was also supported, in part, by the USDA National Institute of Food and Agriculture, Hatch project 227700.

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