The ORA (Organic residue analyses)

The biochemical and genetical approaches

Biochemical analyses (GC-MS) have been successfully implemented since the 1990s for the characterization of the organic residues from archaeological pottery, with numerous programs on the exploitation of honeybee products (Roffet-Salque 2015; Rageot et al. 2013, 2016), dairy products (Copley et al. 2005a; Evershed et al. 2008; Salque et al. 2012), resins, pitch and birch bark tar (Rageot et al. 2013, 2016, 2018), animal fats(Evershed et al. 2002; Copley et al. 2003; Copley et al. 2005b), on the contents and functions of specific types of vases (many cross-references, recently Steele & Stern 2017), on archaeological contexts (idem, recently Frère & Garnier 2017). The first analyses on specific “perfume” container forms (Archaic Greek aryballoi) came from W. R. Biers and his team. They were able to evidence the presence of fatty acids and terpenoids, suggesting a content of animal fats, oils, resins from coniferous trees, most likely cedar, and cypress and possibly camphor (Biers et al. 1994, 29). The “Minoans and Mycenaeans. Flavours of their time” program improved the integration of archaeology and biochemical analyses for the case of the Bronze Age in eastern Mediterranean. This has opened new routes of research that have been since applied to vessels in a peripheral area of the Greek Mycenaean world (Andreou et al. 2013) touching to scientific issues close to that of the Hercle project, albeit still in the Bronze Age. For the western Mediterranean, several chemical analyses have been concerned with flavours and perfumes, mainly for a Hellenistic ointment (Giachi et al. 2012), an Etruscan medicinal product (Giachi et al. 2013), food practices and ceramic functions in southern Italy (Notarstefano 2012), imported Etruscan amphorae and a limestone wine pressing platform in Lattara (Mc Govern et al. 2013b). 

Our team (programs Perhamo and Magi) has enabled to develop, for the first (Perhamo – Frère & Garnier 2012; Frère & Hugot 2012; Frère et al. 2013; Frère et al. 2015; Frère et al. 2016), the use of biochemical and DNA analyses and for the second (Magi – Coulié et al. 2018; Frère & Garnier 2016; Frère et al. 2018; Frère 2018; Pouzadoux & Frère 2019), the use of biochemical and archaeobotanical analyses (pollens and phytoliths, with the new pollen washes technique). With one exception (Argant et al. 2012), the genetic approach has failed to produce satisfactory results, mostly due to the problems of environmental contamination. So far, ancient DNA analyses have proved successful in one case only, some Greek amphorae retrieved from a shipwreck, yielding interesting results: olive, grape, Lamiaceae herbs, juniper, terebinth, mastic, pine… (Hansson et al. 2008; Foley et al. 2012). Michael Vickers (2010) asks the question: “Is there light at the end of the tunnel?” concerning the high scientific potential of the DNA molecules scraped from inside the internal walls of the amphorae. Yet, the DNA analysis applied to the archaeological organic residues is still in an infancy stage and this promising technique must be tried out with various kinds of archaeological containers in order to assess its relevance. More importantly, it is a complex and very expensive technique that can not yet be routinely used on sequence analyses.  Currently, the organic analyses still provide the best piece of evidence to uncover the contents of containers. We have thus uncovered GC-MS evidence of Citrus sp. skin (attested by a unique sequence of flavanones) in the content of a Sardinian Phoenician mushroom jug dated from the VIth c. BCE (Frère et al. 2016). Considering archaeobotanical and textual evidence in the Mediterranean, citron was proposed as the best specific candidate. Mixed with animal fat and other plant extracts (undetermined), this was being used for a funeral ritual, possibly for medicinal purpose. In another GC-MS analysis, some members of our team have assigned a piece of unburnt resin from a Carthaginian necropolis at Kerouane (eastern coast of Cape Bon, Tunisia) dated from the VIth-Vth c. BCE to labdanum, a resin produced by the Cistus genus (rock-rose), and were able to assign it to a western Mediterranean species (Garnier & Dodinet 2013). The analyses, thus, provided evidence that at an early date, the Carthaginians in their rituals had shifted to using a local species in lieu of what was considered to be an essentially eastern Mediterranean raw material. A Corinthian aryballos (a little perfume vase) in an archaic Etruscan tomb also revealed the biomarkers of Cistus ladanifer, a plant not represented in Italy, testifying of the adoption of a foreign flavoured material by northwestern Mediterranean societies (Frère et al. 2018).

Bibliography

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Argant J., Boucher C., Frère D., Garnier N., Gillet B., Hänni C., Lacroix S., Leroy- Langelin E. & Louis E. 2012- “De la fouille au laboratoire. Analyses et interprétations des contenus de céramiques et verres archéologiques”, Revue du Nord, 17, Hors Série Collection Art et Archéologie, 479-504.

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Copley M.S., Berstan R.S., Dudd N., Docherty G.,  Mukherjee A.J.,  Straker V.,  Payne S. & Evershed R.P. 2003- “Direct chemical evidence for widespread dairying in prehistoric Britain”, Proceedings of the National Academy of Sciences, 100, 4, 1524-1529.

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Copley M.S. Berstan R., Dudd S.N., Straker V., Payne S., Evershed R.P. 2005b- “Dairying in antiquity. I., Evidence from absorbed lipid residues dating to the British Iron Age”, Journal of Archaeological Science, 32, 4, 485-503.

Coulié A., Frère D., Garnier N. & Marton A. 2018- “Le tombeau A de Camiros : les vases archaïques et leurs contenus. L’apport de l’étude chronologique et des analyses chimiques des résidus”, Bulletin de Correspondance Hellénique, 141, 2017 (2018), 553-621.

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Frère D. 2018- “Les aryballes et alabastres archaïques: nature des contenus et modes d’échanges”, Mediterranea, XV

Frère D., Cygielman M. et al. 2015- “Les cruches askoïdes sardes en Etrurie : la problématique de leur contenu et de leur fonction”, Studi Etruschi, LXXVII, 2015, 253-291.

Frère D., Garnier N. & Dodinet E. 2016- “Archéologie des huiles parfumées et médicinales en Méditerranée nord-occidentale préromaine (VIIIe-VIe s. av. J.-C.)”, in Malet C. (ed.), Le corps, soins, rituels et symboles, Paris, 99-119.

Frère D., Hugot L. & Garnier N. 2018- “La Chambre des Chenets de Cerveteri. Les rituels parfumés d’après les analyses chimiques de contenus”, in Naso A. & Botto M. (eds.), Caere orientalizzante. Nuove ricerche su città e necropoli, Rome, 367-387.

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Frère D. & Garnier N. 2016- “Fonctions des vases, usages multiples et détournements”, SFECAG, Actes du Congrès d’Autun, Marseille, 269-274.

Frère D. & Garnier N. 2017- “Dairy Product and Wine in Funerary Rituals: The Case of a Hellenistic Etruscan Tomb”, Journal of Historical Archaeology & Anthropological Sciences, 1, 6, 222-227.

Frère D. & Hugot L. 2012- Les huiles parfumées en Méditerranée occidentale et en Gaule. VIIIe s. av.-VIIIe s. ap. J.-C., Rennes, Naples, 75-82.

Garnier N. & Dodinet E. 2013- “Une offrande de ciste dans une tombe carthaginoise (VIe-IVe s. av. J.-C.). Une approche interdisciplinaire alliant archéo-botanique et chimie organique analytique”, Archéosciences, revue d’archéométrie, 37, 51‑66

Giachi G., Ribechini E., Colombini M.P. & Garnier N. 2012- “A Multianalytical Approach in the Chemical Characterisation of the Etruscan Ointment of Thana Plecunia (Chiusi, Italy)”, in Frère D.& Hugot L. (eds.), Les huiles parfumées en Méditerranée occidentale et en Gaule. VIIIe s. av.-VIIIe s. ap. J.-C., Rennes, Naples, 75-82.

Giachi G., Pallecchi P., Romualdi A., Ribechini E., Lucejko J.-J., Perla Colombini M. & Mariotti Lippic M. 2013-“Ingredients of a 2,000-y-old medicine revealed by chemical, mineralogical, and botanical investigations”, Proceedings of the National Academy of Sciences of the United States of America, 110, 4, 1193–1196.

Hansson M.C. & Foley B.P. 2008- “Ancient DNA fragments inside Classical Greek amphoras reveal cargo of 2400-year-old shipwreck”, Journal of Archaeological Science 35, 1169-1176.

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NotNotarstefano F. 2012- Ceramica e alimentazione. L’analisi chimica dei residui organici nelle ceramiche applicata ai contesti archeologici, Bari.

Pouzadoux Cl. & Frère D. 2019- (eds.), Les produits biologiques en Italie et Gaule préromaines. Produits alimentaires, médicinaux, magico-religieux, cosmétiques, Naples, in press.

Roffet-Salque M., Regert M., Evershed R.P., Outram A.K. Cramp L.J. et al. 2015- “Widespread exploitation of the honeybee by early Neolithic farmers”, Nature, 527, 7577, 226-30.

Rageot M., Peche-Quilichini K. & Regert M. 2013- “Quand les Corses cherchaient du bouleau. Archéologie, histoire et chimie des colles autour de 1000 av. J.-C.”, Santari, 32, 32–37.

Rageot M, Pêche-Quilichini K., Py V., Filippi J.J., Fernandez X. & Regert M. 2016- “Exploitation of beehive products, plant exudates and tars in Corsica during the early Iron Age”, Archaeometry 58, 2, 315–332.

Salque M., Bogucki P.I., Pyzel J., Sobkowiak-Tabaka I., Grygiel R., Szmyt M. & Evershed R.P. 2012-  “Earliest evidence for cheese making in the sixth millennium BC in northern Europe”, Nature, 493, 7433, 522-525.

Steele V.J. & Stern B. 2017- “Red Lustrous Wheelmade ware: Analysis of organic residues in Late Bronze Age trade and storage vessels from the eastern Mediterranean”, Journal of Archaeological Science: Reports, 16, 641–657.

Vickers M. 2010- “Amphora Studies: is there light at the end of the tunnel ?”, in Patabs I. (ed.) Production and Trade of Amphorae in the Black Sea, Actes de la Table Ronde internationale de Batoumi et Trabzon, 27-29 avril 2006, Istanbul, 13-16.

Foodstuffs, Dairy products, Fermented beverages, Medicinal and Cosmetic products, Perfumes, Aromatic materials in the Mediterranean and West-European areas. This scientific notebook presents the bioarchaeology research programs of the Temos laboratory (CNRS, UMR 9016).

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