The analysis of residues collected from ceramics at the site of Dikili Tash (Kavala, Eastern Macedonia, Greece) suggests that wine was made in Europe as early as the 5th millennium B.C.
In addition to the tartaric acid found in the vessels, the joint Greek-French excavation team found carbonized grape pips and their skins in a Neolithic house dating to 4500 B.C. The grape pips and skins indicate that the grapes had been pressed. “The historical meaning of our discovery is important for the Aegean and the European prehistory, as it gives evidence of early developments of the agricultural and diet practices, affecting social processes,” said Dimitra Malamidou, co-director of the project.
NovoScriptorium: Now we shall present a number of relevant published papers, concluding with the one that actually proved that we are indeed talking about wine-making in the Greek peninsula during the Neolithic Age.
Abstract Northern Greece, one of the birthplaces of Dionysus in much later Greek mythology, provides evidence for the exploitation of the grape vine from the Neolithic through to the Bronze and Iron Age. The presentation discusses the archaeobotanical remains of Vitis vinifera in northern Greece and Dikili Tash in particular, exploring the potential uses of this plant, especially wine making. Archaeobotanical research at Dikili Tash, a multiperiod site in northern Greece, near the ancient city of Philippoi has yielded some unique so far remains of pressed grapes that were caught up in the flames of a fire that destroyed several Late Neolithic houses by the end of the 5th millennium BC. The archaeobotanical finds consist of numerous grape pips and grape pips surrounded by skins, found mainly in one of the houses, House 1. Excavation of this house in 2010 indicated that probably two such concentrations were present in the house, most likely in association with large, coarse-ware pots. It is possible that the pressings were placed in the pots together with grape juice for fermentation to take place, when fire broke out at the settlement destroying the house with its crops and ‘new’ wine. As grape pressings remain in grape juice for a limited number of days, it is possible that the fire episode took place in the autumn, a possibility corroborated by a house full of the summer (wheat, pulses) and autumn harvest (grapes, acorns). Yet, alternative possibilities, such as the storage of grape pressings for other uses need to be considered. The grape juice extracted at Dikili Tash could have been consumed as such or for the preparation of different sweets, or used for wine making or for the preparation of a syrup (e.g. petimezi/pekmez). The grape pips that have been associated with the grape-pressings from Dikili Tash have been attributed to morphologically wild grapes. Although wine can be made from the juice of wild grapes, it is also possible that the large quantities found at Dikili Tash belonged to plants in an incipient form of tending or cultivation that had not yet resulted in the morphological change of the grape-pips. Drinking cups, present at the site from the beginning of the Late Neolithic, might have contained some liquid with intoxicating effects. The finds from Dikili Tash are discussed within the context of prehistoric grape vine exploitation in northern Greece as evidenced from archaeobotanical remains from various sites. The possibility of a ‘tradition’ of grape juice extraction in the area is considered in light of other remains of grape pressings unearthed at sites dated to the Late Bronze and Iron Age. If wine was indeed produced at Dikili Tash, as the archaeobotanical and pottery evidence suggests, its qualities and etiquette of consumption may have evolved over time.
(Source: “An Archaeobotanical Investigation of Prehistoric Grape Vine Exploitation and Wine Making in Northern Greece: Recent Finds from Dikili Tash”, by Soultana Maria Valamoti, Pascal Darcque, Chaido Koukouli Chrysanthaki, Dimitria Malamidou, Zoi Tsirtsoni)
Abstract The relationship between farming communities in south-eastern Europe and wild plant resources, fruit and nut trees in particular, is explored in this paper, based on charred plant remains from House 1 at late Neolithic Dikili Tash in eastern Macedonia, northern Greece, retrieved between 2010 and 2012. Within the rubble of a burnt destruction level dated to the second half of the 5th millennium cal BC, a wide range of cultivated crops like cereals, pulses and flax were stored together with a variety of fruit and nuts, such as acorns, wild pears, grapes, including grape pips and grape pressings and possibly figs,too. These finds provide a rare opportunity to investigate the use of fruit as well as the origins and context of wine making and consumption in the Neolithic of south-eastern Europe. Human interference with natural vegetation in relation to use of wild trees is discussed in light of the archaeobotanical, palynological and charcoal evidence from the wider area of the site. It is suggested that the remains from Dikili Tash may be pointing towards some early form of arboriculture in the region. The interplay of wild and domesticated plant resources encountered at the site is discussed within the framework of established oppositions between ‘wild’ and ‘domesticated’ in archaeological discourse. It is suggested that fruit and nut use at Dikili Tash might correspond to old traditions dating back to the hunter-gatherers of south-eastern Europe while wine, for which there is evidence at the site, might have acted as a mediator between human communities, cultivated landscapes and wild vegetation, inducing altered states of consciousness and cultivated/wild boundary transitions.
(Source: “Harvesting the ‘wild’? Exploring the context of fruit and nutexploitation at Neolithic Dikili Tash, with special reference to wine”, by Soultana Maria Valamoti)
Abstract Houses burnt down at the Neolithic site of Dikili Tash in northern Greece preserved the remains of wild grapes and figs. The charred shapes showed that there was a pile of grape pips with skins – clear evidence for the extraction of juice. The authors argue that the juice was probably used to make wine – towards the end of the fifth millennium BC the earliest so far from the Aegean. The occupants of the houses also had two-handled cups, providing another clue to consumption of a special kind.
(Source: “Grape-pressings from northern Greece: the earliest wine in the Aegean?”, by S.M. Valamoti, M. Mangafa , Ch. Koukouli-Chrysanthaki & D. Malamidou)
Abstract A new two-step analytical protocol has permitted the reliable structural identification of red wine thanks to the presence of dark grape (tartaric, malic, syringic acids) and fermentation markers (succinic and pyruvic acids) in a smashed, large, coarse jar and a jug excavated inside a Neolithic house destroyed by fire around 4300 BCE at the site of Dikili Tash in northern Greece. This new method, which has also been tested successfully on other vessels, exploits the chemical break-down of the clay and the simultaneous liberation and derivatization of biomarkers. Since aldaric acids are not extracted by a simple solvent extraction, but only when submitted to the second acido-catalyzed extraction, their detection in the second extract indicates organic residues are more deeply impregnated and bound to the clay structure than previously thought. Chromatography coupled with mass spectrometry leads to the very sensitive detection and reliable identification of fermented grape biomarkers. Their identification in a Neolithic jar from Dikili Tash corroborates the finding of pressed grapes consisting of loose pips, skins, and pips still enclosed by skin in association with this jar. Our results demonstrate Neolithic wine-making in the northern Aegean, and provide the earliest solid evidence for the Eastern Mediterranean and Europe. This new method could be more widely used for detecting wine traces in all sorts of archaeological artefacts or structures. It constitutes an essential tool for a better understanding of wine-making and of contexts of consumption in ancient civilizations.
Introduction The origins of viticulture and wine making have been at the core of discussions concerning the emergence of social stratification among prehistoric societies of the Old World. Viticulture has been considered as a means to exploit soils less suited for crop cultivation thus contributing to the emergence of redistributive societies and Late Bronze Age Aegean palaces or a means to tie people to their land due to the large labour investment and late return of cultivating grape vines. Wine in turn holds a key role concerning the emergence of Bronze Age elites, among the Sumerians, Egyptians, Minoans and Mycenaeans. Textual evidence underlines the luxury nature of wine, its consumption in relation to rituals, funerary customs and feasting and its appropriation by Bronze Ageelites (Sumerian, Assyrian and Hittite states: Powell, 1995; Mycenaean Greece: Palmer, 1995). The origins of viticulture and winemaking could lie anywhere in the wider area of the distribution of the wild grape vine, Vitis vinifera sbsp. sylvestris (Gmelin) Hegi, which spreads from western Europe to the Trans-Caucasian zone and a large part of the Mediterranean basin and might have occurred several times rather than once. The available archaeobotanical evidence suggests that grape vine has been exploited and probably also cultivated in a wide region ranging from the Aegean to the eastern fringes of western Asia, including the Caucasus, since at least the 5th millennium BC. Despite this, a widespread scholarly position proposes that viticulture and/or grape domestication originated in a specific region from which it spread, e.g. Transcaucasia, the Levant or the eastern end of western Asia. For theAegean, Renfrew (1995), in a comprehensive review of the grape finds from the region, suggests that the cultivation of the grape vine is indicated by the 5th millennium BC with wild and domesticated forms being both present.
Winemaking does not necessarily require viticulture as a prerequisite: wine can be fermented from either wild or cultivated grapes. Wild grape wine may have been the first important alcoholic beverage due to the simple process required for fermentation: a rich harvest of wild grapes can result in fermentation and winemaking by simply crushing the fruit and allowing contact of the juice with the yeasts present on the skin (Singleton,1995; McGovern, 2003; Miller, 2008; Valamotietal., 2007).Various lines of evidence have been used to detect early winemaking in the archaeological record, including pottery typology, chemical residue analysis and archaeobotanical remains.
Pressed grapes found in archaeobotanical deposits are eloquent indicators of juice extraction from pressed fruits, which would ferment to different degrees, depending on the duration of the process. Charred finds of early grape pressings are reported from 5th millennium BC Dikili Tash in northern Greece (Valamoti et al.,2007), 3rd millennium BC Kurban Hoyük in Turkey (Miller, 2008), 3rd millennium BC Myrtos (Renfrew J.M.1972) and 2nd millennium BC Monastiraki on Crete (Sarpaki,2012). Although these finds per se
are not conclusive as to the specific use of the grape juice, wine is a very likely candidate, though alternative uses such as the preparation of grape syrup or vinegar cannot be ruled out.
Here, we attempt for the first time an integrated approach towards the detection of prehistoric wine that combines archaeobotanical remains of pressed grapes and a new two-step protocol for the detection of grape biomarkers, applied to an exceptional archaeological context from Neolithic Dikili Tash in northern Greece.
Context and archaeobotanical remains of Vitis from Dikili Tash The site of Dikili Tash is a large multi-layered settlement in Greek Eastern Macedonia (Kavala district), occupied during the Neolithic and Bronze Age periods (ca. 6400-1000 BCE) and systematically investigated over the last five decades.Among other remains, a group of very well preserved houses of the Late Neolithic II period, destroyed by fire around 4300 BCE, were unearthed during the 1989-1996 excavations. Inside one of them, House 1, hundreds of charred grape pips and skins were collected (Valamoti et al.,2007). They have been identified as grape pressings rather than whole grapes, raisins or grape mash, on the basis of comparison with experimentally charred plants (Mangafa et al., 2001). The pips, although morphologically wild (Mangafa and Kotsakis, 1996) could have originated from managed or cultivated grape vines with grape pip morphology remaining unaltered at the early stages of viticulture (cf Valamoti, 2015).
Excavations in the same building between 2008 and 2013 brought to light thousands more such remains, together with substantial quantities of other plant remains: domesticated (cereals, pulses) as well as fruits and acorns harvested from the wild (Valamoti, 2015). They were usually stored as pure concentrations, sometimes associated with ceramic containers.
Among them, a dense, pure concentration of loose grape pips, grape pips with skin attached, and a few stalks was found. So far more than 3000 pips have been counted. The finds, which suggest again the pressing of grapes for juice extraction, were uncovered in association with fragments of a smashed big coarse jar. Pips were also distributed in a wider area around the jar, represented in numerous archaeobotanical samples of mixed composition, together with other crops apparently stored inside House 1, in the vicinity of the jar with the grape finds (Valamoti, 2015). As the distribution of the grape finds covers a relatively large area (approximately 2m²) it is very likely that these spread, upon destruction, over a wide floor surface area. This could have been facilitated if the pips were contained in the jar together with a liquid that spilled as the vessel got smashed under the collapsed house rubble. Could that liquid have been grape juice extracted from the grapes mixed with grape marc in a process of fermentation? Alternatively, the grape finds could represent by-products of grape juice extraction, stored inside the house for later use as fodder or fertiliser.
Given the strong archaeological and botanical indications for an ancient winemaking process, two sherds were selected to test the developed analytical protocols in order to sustain the presence of grape and fermentation biomarkers. Two fragments of the smashed jar were selected, one from the 2010 excavation, the other from 2012. These were both body fragments, showing no visible residue on their inner wall. In the following seasons, further analyses were carried on a great number of vessels from House 1, and from later features/layers in the same area, as part of the broader archaeological project. The results of these works will be presented elsewhere. An exception is made forthe vessel inv. n° 6330-2 for it is relevant with the issue discussed here: this is a small graphite-painted jug found ca. 4 m away from the jar with the grape
finds. The jug lay intact on the house floor, with no particular botanical remains in or around it, and no visible residue either.
Methods The present methodology offers both a greater efficiency and sensitivity than the previous method developed for the identification of polyphenol markers of grape (Garnier et al., 2003). The method allows the detection of quantities lower than 10^6
mLeq.of actual must/wine adsorbed in 1 g of ceramic sherd. Since lipids are extracted during the first DCM/MeOH extraction, the two-step protocol presents the advantage to permit the easy identification of grape markers even if resins, pitch or lipid materials are present in greater amounts, and even in the absence of any visible residues on pottery surface. This sensitive method can be implemented on small ceramic fragments around 50-500 mg.
NovoScriptorium: The reader interested in the details is encouraged to study the whole ‘Methods‘ section of the paper.
The content of the Neolithic jar: winemaking at Dikili Tash
Application of the new two-step protocol to smashed jar 6288-001 from Dikili Tash, associated with grape pressings indicates, inspite of the strong presence of plastic contamination and restoration products on one of the fragments (#6183-2), a mixture of different biological materials: resin from conifer wood (dehydroabietic and 6-dehydro dehydroabietic acids) revealed by the first extraction, and then tartaric acid and traces of malic acid (identified by comparison with standard transbutylated malic acid and its characteristic peak, with respective concentrations of 3.15 and 0.21 m g/g sherd. Syringic acid was released only during the second extraction step, indicating that it necessarily comes from malvidin or its oxidised condensed forms (EsSafi et al., 2008) e.g. dark or
teinturier grapes, and not from any other source in which it is present as free extractible acid (Guash-Jane et al., 2006b). The association of these acids, together with the abundance of grape pips around and underneath the jar sherds, strongly suggests that grape juice had been placed together with pressings into the jar and allowed to ferment.
The fermentation process of grape is confirmed by the analysis of a second fragment from the same jar (#6323-2), leading to the identification of tartaric, malic and syringic acids as markers of dark or teinturier grapes, and pyruvic acid, glutaric acid, and succinic acid as fermentation markers. The presence of pyruvic acid could point to a spontaneous malolactic fermentation that would have followed the first alcoholic fermentation of the must.
The presence of syringic acid indicates a winemaking process conducive to red wine,
i.e. red winemaking: during the spontaneous fermentation of the crushed grapes with yeasts present on grape skin, the sugar from the fruit is converted into alcohol which, in turn, extracts the colour, mainly malvidin, from grape skins. The identified markers probably correspond to successive steps in the preparation and the use of the jar: it was initially water-proofed with a resinous material, then used to contain the grape juice and pressings for fermentation and ageing.
Conclusion The new analytical method presented here reveals that only a tiny fraction of organic markers is usually extracted by the classical approach using DCM/MeOH extraction; the use of strong Lewis acid allows the dissolution of insoluble or highly bound to the clay structure compounds, especially grape and fermentation markers. This method, consisting in two successive extractions and the separate GC-MS analysis of both extracts, opens up new pathways for future investigations of ancient wine ranging from the early stages of production to the multifaceted contexts of its consumption.
The methodology, successfully applied to Neolithic vessels from Dikili Tash, allowed the detection of grape juice and fermentation markers inside a jar that was associated with grape pressings. Thus, both lines of evidence, archaeobotanical finds and residue analysis of this specific archaeological context, clearly suggest that grape juice fermentation was in progress in the analysed vessel when House 1 collapsed, smashing it and spreading its contents. Winemaking and consumption of wine at late-5th millennium BC Dikili Tash involved pressing of grapes and crushing to break the grains, the use of fermentation, and then the use of serving and consumption vessels though no clear sign of social stratification is visible at the site. This find, millennia earlier than the Minoan or Mycenaean elites of southern Greece (2nd millennium BC) and other Bronze Age palatial societies (Egyptian, Sumerians, Hittites), calls for a reconsideration of the causal relationship assumed in the literature between wine and elites, and could challenge previous suggestions for a single origin of viticulture and winemaking. In light of our research, northern Greece, and more specifically present-day Eastern Macedonia (ancient Thrace), emerges as an area with a deep-rooted tradition in winemaking going back to theNeolithic, and seems to have played an active role preceding that of southern Greece, Crete, and maybe Cyprus, and predating the chronology of grape vine domestication. Perhaps this tradition led to identification of the area by ancient Greeks as one of the birthplaces of Dionysos.
(Source: “Prehistoric wine-making at Dikili Tash (Northern Greece): Integrating residue analysis and archaeobotany”, by Nicolas Garnier, Soultana Maria Valamoti)
Research-Selection for NovoScriptorium: Philaretus Homerides