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Prehistoric wine-making at Dikili Tash (Northern Greece): Integrating residue analysis and archaeobotany

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... Although they demonstrated the effectiveness of pollen analyses in the identification and characterization of the nature and geographical origin of the transported wine, their methodologies have barely been followed and similar investigations are still rare. Even other types of organic materials, e.g., rope, caulking material, laces watercrafts, and organic coffin have been seldom investigated through pollen [12][13][14][15][16]. Archaeobotany has been often combined with other analytical disciplines to promote interdisciplinary approaches [17][18][19][20][21][22][23] but palynology is still barely associated to chemical analyses [11, [24][25][26]. At the same time, analytical methods are increasingly interested in using cutting edge techniques applied to archaeological materials. ...
... At the same time, analytical methods are increasingly interested in using cutting edge techniques applied to archaeological materials. Among them, liquid or gas chromatography coupled with mass spectrometry (GC-MS) dominate the field, due to highly sensitive and selective capacities to target molecules [21,25,[27][28][29]. Retention time and molecular fragmentation account for trustworthy molecular identifications [30]. ...
... Since acids were transesterified in the second step, molecules identification in 2LE-MW was restricted to grape derivatives markers (succinic, pyruvic, malic, tartaric and syringic acids). Considering the presence of diethyl or butyl ethyl grape acids reported by Garnier and Valamoti [21] in a Neolithic jar, similar reactions were controlled in our samples but no esters were observed. Such compounds would indeed be produced by esterification with the ethanol contained in the fermented beverage. ...
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We hereby investigate the pitch used for coating three Roman amphorae from San Felice Circeo (Italy) through a multidisciplinary study. The identification of molecular biomarkers by gas chromatography—mass spectrometry is combined with archaeobotanical evidence of pollen and plant tissues of Vitis flowers. Diterpenic chemical markers together with Pinus pollen and wood revealed Pinaceae tar coating. Aporate 3-zonocolpate pollen, identified as Vitis , together with tartaric, malic and pyruvic acids elucidate the grape-fermented nature of the content. Our conclusions open new consideration on the use of grape derivatives that cannot be supported by traditional analytical methods. Based on the finds of aporate Vitis pollen, found also in local modern and Middle Pleistocene samples, we hypothesize the use of autochthonous vines. The presence of a medicinal wine (historically reported as oenanthium ) is also considered. We interrogate Vitis pollen capacity to target grapevine domestication, thereby providing innovative tools to understand such an important process. We anticipate our study to encourage a more systematic multidisciplinary approach regarding the analyses of wine amphorae.
... Wine markers extraction. The extraction and analysis procedures of the wine-markers from the ceramic vessels followed Garnier and Valamoti (2016) [60]. 5.0 ml of boron trifluoride, butanol and cyclohexane (1:2:4, v:v) were added to each vial of the powder remaining from the TLE extraction. ...
... Wine markers extraction. The extraction and analysis procedures of the wine-markers from the ceramic vessels followed Garnier and Valamoti (2016) [60]. 5.0 ml of boron trifluoride, butanol and cyclohexane (1:2:4, v:v) were added to each vial of the powder remaining from the TLE extraction. ...
... isothermic hold). Peak assignments were based on comparisons with library spectra (NIST 17), spectra reported in the literature [24,60,61] and by comparison of retention times of reference standards. ...
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The article presents results of residue analysis, based on Gas Chromatograph Mass Spectrometer (GC-MS) measurements, conducted on 13 ceramic storage jars unearthed in the Babylonian destruction layer (586 BCE) in Jerusalem. Five of the jars bear rosette stamp impressions on their handles, indicating that their content was related to the kingdom of Judah's royal economy. The identification of the original contents remains is significant for the understanding of many aspects related to the nutrition, economy and international trade in the ancient Levant. The study shed light on the contents of the jars and the destruction process of the buildings in which they were found. The jars were used alternatively for storing wine and olive oil. The wine was flavored with vanilla. These results attest to the wine consumption habits of the Judahite elite and echo Jerusalem's involvement in the trans-regional South Arabian trade of spices and other lucrative commodities on the eve of its destruction by Nebuchadnezzar.
... The protocol aiming at butylating wine acid markers was adapted from Garnier and Valamoti [12]. It was firstly developed for tartaric acid before being extended to other standard molecules of maleic, succinic, fumaric, pyruvic, malic, syringic acids. ...
... Partially dissolving the ceramic clay, BF 3 , optimized the release of the organic compounds strongly bonded, or even polymerized [25,39]. Increasing the apolar character of the esterified acids, butylation favored their rapid extraction in cyclohexane, hence favoring the butylation of remaining acids by shifting the equilibrium [12]. From there, the extraction from the co-solvent is enhanced with DEE that has a low dielectric constant solvent. ...
... Starting from pure standard, quantitative analysis comparing the amount of tartaric acid recovered after extraction reported to identify 77% of the acid with butylation while it did not reach 0.1% with alkaline fusion [11]. Additionally, Garnier and Valamoti reported the detection of tartaric acid up to 10 ng/g shard with the acido-catalyzed protocol [12]. In conclusion, neither KOH fusion, nor the organic extraction with DCM-MeOH were suitable for the characterization of grape derivatives. ...
Article
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With the aim of addressing the impact of extractive protocols in molecular characterization of ceramic content, sixteen archaeological shards and waterproofing coatings of Roman amphorae were studied to compare the extractive capacities of protocols prevalently mentioned in wine amphorae analysis. A microwave-assisted protocol is developed in order to esterify grape-derivative markers from archaeological pitch and shard. Gas chromatography-mass spectrometry is used to highlight the great capacities of a two-step protocol that combines organic extraction with BF3-etherate complex butylation applied on archaeological shards. Instead, simultaneous alkaline fusion and direct-resin acid-catalyzed butylation are favored for the characterization of waterproofing material. The identification of tartaric acid, together with succinic, fumaric pyruvic and syringic acids provide valuable insights on the archaeological grape-derivative content, possibly wine. Diterpenic markers highlighted Pinus pitch and wood tar, originally used to waterproof the amphorae. Since markers are reliable tools in organic residue analyses, protocols exhibiting high extractive capacities are favored to avoid false conclusions drawn through the absence of markers.
... Understanding if these vessels contained wine can help us understand both the demand for these goods in the Eastern Mediterranean, as well as patterns of pottery use in antiquity. To this end, and in order to collect as much information as possible (presence of grapevine products, possible grape colour, possible additions of other substances), we have used an analytical protocol combining three complementary extraction methods, based on recent methodological developments (Drieu et al., 2020(Drieu et al., , 2021Garnier & Valamoti, 2016). In order to strengthen the interpretation and the identification of grapevine products by ruling out contamination, in each context we also analysed vessels that are not supposed to have been in contact with wine. ...
... The method was designed to analyse lipids (plant oils, aquatic products) and small organic acids (plant products, in particular grapes) separately. Following Garnier and Valamoti (2016), after the solvent extraction of lipids, we performed an acid butylation of small organic acids with a boron trifluoride-butanol/ hexane solution. We applied the same type of procedure by following the lipid extraction method with the small organic acid extraction method under alkaline conditions developed by Pecci et al. (2013). ...
... The ethyl acetate extraction was repeated twice and the resulting extracts were combined and dried under a stream of nitrogen. After Garnier and Valamoti (2016), the other part of the ceramic powder was treated for 2 h at 80 C with a boron trifluoride-butanol/hexane solution (BF 3 -BuOH/hexane, 1:2, v/v). After centrifugation, the solution was collected, neutralised with a saturated solution of sodium carbonate and extracted three times with DCM. ...
Article
Despite growing evidence to the contrary, wine remains the assumed content of many types of ancient pottery. Vessels from the Kyrenia and Mazotos shipwrecks, and Yeronisos island presumed to have contained wine were subjected to three different extraction protocols to test the assumption that these vessels were used to import and serve wine. Chemical extracts reveal grapevine products but also other fruit juice, beeswax and plant oil, sometimes mixed with grapevine products due to intentional mixing or reuse. Biomarkers detected in sediment samples from Mazotos and Yeronisos demonstrate why quantification is vital. Analyses show that even seemingly identical ceramics from the same shipwreck contained different commodities.
... The biomolecular research of Patrick McGovern has had a fundamental impact on the investigation of archaeological and chemical evidence of ancient wine (McGovern, 2004;McGovern et al. 2005;Michel et al. 1993). Later, more reliable techniques have been applied to identify wine biomarkers; in particular, Guash Jané et al. (2004) and Barnard et al. (2011) found wine residues in archaeological ceramics through the application of HPLC, while Garnier et al. (2003), Pecci et al. (2013aPecci et al. ( , 2013bPecci et al. ( , 2017a and Garnier and Valamoti (2016) applied gas chromatography-mass spectrometry (GC-MS) to several experimental and archaeological ceramics from the Mediterranean area. Recently, McGovern et al. (2013McGovern et al. ( , 2017 analysed samples from France and Georgia using LC-MS-MS. ...
... To identify wine (or other grape derivatives) residues, tartaric acid is considered the biomarker for grape (Garnier and Valamoti, 2016;Guasch Jané et al., 2004;McGovern, 2004McGovern, , 2019McGovern et al., 1996McGovern et al., , 20052013Pecci et al., 2013aPecci et al., , 2013bPecci, 2019a;Rageot et al., 2019). The methods currently applied to detect tartaric acid do not allow differentiating wine from vinegar (Pecci et al., 2013b) or other wine derivatives like must. ...
... As other fruits may also contain tartaric acid (Barnard et al., 2011;Singleton, 2005), to suggest the presence of wine in archaeological materials, chemical evidence needs to be referred to the archaeological context. This includes the archaeobotanical evidence of Vitis vinifera as branches/wood, pips or pollen in archaeological layers, the mentions of wine consumption in written documents or iconography, and the presence of archaeological tools for plant processing or to drink wine (Garnier and Valamoti, 2016;McGovern and Hall, 2016;Garnier et al., 2011;Pecci, in press). Long-lasting projects aimed at verifying the chemical absorption of wine in pottery and plasters (Pecci et al., 2013b;Garnier and Valamoti, 2016), and the ageing of experimentally enriched pottery and plaster through burial up to seven years and heating at 70 • C demonstrated thatat least in relatively short burial periodstartaric acid is preserved when trapped in the pores of pottery and is not washed away (Pecci et al., 2013b). ...
Article
The early consumption of wine or other grape derivatives (such as vinegar or must) is suggested from organic residues analysis conducted on Bronze Age pottery recovered from two sites in north-eastern Italy, Pilastri di Bondeno (Ferrara) and Canale Anfora (Aquileia, Udine). Pilastri is part of the Terramare culture of the Po plain, from which the archaeobotanical context has suggested that Vitis vinifera L. was known and used during the Middle Bronze Age. At Canale Anfora Vitis, macro-remains were found in earlier levels of the local stratigraphy. Organic residue analysis conducted by gas chromatography coupled to mass spectrometry allowed the identification of tartaric acid in twenty samples out of thirty-one recovered from different ceramic vessels (e.g., drinking cups, coarse ware pots, presumed storage vessels) found at the two archaeological sites and dated to the 15th-14th centuries BC. Based on integrated studies, we suggest that grape juice derivatives (including wine or vinegar) were likely consumed at the sites. This is the earliest direct evidence of grape derivatives consumption in this area. Combined with the botanical evidence, these findings contribute to our understanding of the emergence of wine consumption in the western Mediterranean.
... Recent chemical analysis of potsherds from Georgia (McGovern et al. 2017) claims to have pushed the antiquity of wine production back to the Early Neolithic period (around 6000-5800 BC), some 1000 years earlier than its previous earliest identification in a vessel from the Zagros Mountains (Iran, 5400-5000 BC; McGovern et al. 1996). Wine was also claimed to be identified in vessels from Northern Greece (around 4300 BC; Garnier and Valamoti 2016), Egypt (from 3000 BC; Guasch-Jané et al. 2004, 2006a, 2006b, Northern Italy (1500-1300 BC; Pecci et al. 2017), and in Southern France (around 500 BC; McGovern, Luley, et al., 2013), providing important insights into early establishment of the tradition throughout the Mediterranean. Analysis of Egyptian vessels has highlighted the role of wine in many aspects of political and religious life (Guasch-Jané et al. 2006a, 2006bMcGovern 1997). ...
... The polarity of tartaric acid and its salts makes it highly soluble in water and thus unlikely to be preserved in archaeological contexts (Barnard et al. 2011;Michel, McGovern, and Badler 1993;Singleton 1996), although tartrates are slightly less soluble in water than the acid. Fortunately, their polarity also offers a means of preservation by permitting binding to the ceramic matrix, through strong interactions between polar groups and Brønsted or Lewis sites of the ceramic paste, or hydrogen bonds with silicates (Garnier and Valamoti 2016;Michel, McGovern, and Badler 1993). Degradation experiments have shown that tartaric acid is better preserved in the ceramic matrix than other small acids (citric, malic, succinic, and fumaric acids) after seven years of burial in natural conditions (Pecci, Giorgi, Salvini, et al. 2013). ...
... To do this, alkaline solutions (e.g. NaOH or KOH) have been widely used (Table 1), but acid treatment has also been shown to be effective, probably as it promotes partial dissolution of the ceramic matrix (Correa-Ascencio and Evershed 2014; Garnier and Valamoti 2016). Methods involving only water or methanol extraction are ill suited, as they do not break these bonds. ...
Article
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Chemical analysis of archaeological artefacts is used with increasing regularity to understand how wine was produced, traded, and consumed in the past and to shed light on its antiquity. Based both on an extensive review of the published literature and on new analyses, here we critically evaluate the diverse range of methodological approaches that have been used for wine identification. Overall, we conclude that currently none of the proposed chemical‘biomarkers’ for wine provide unequivocal evidence. Nevertheless, valid interpretations may be offered if systematically supported by additional contextual data, such as archaeobotanical evidence. We found the extraction and detection method to be particularly crucial for successful identification. We urge the use of controls and quantification to rule out false positives. DNA sequencing offers potential for identifying wine and provides much higher taxonomic resolution, but work is needed to determine the limits of DNA survival on artefacts.
... Before the IV th millennium, remains of Pinaceae adhesives in the Mediterranean region are scarce. Only 10 pottery vessels out of 70 (14%) from Greece and the Balkans (Makriyalos, Toumba Kremastis Koliadas, Drenovac and Dikili Tash) (Garnier and Valamoti, 2016;Mitkidou et al., 2008;Urem-Kotsou et al., 2018) presented evidence of abietane diterprenoids. In the Pendimoun rock shelter (southern France), 16 vessels from a sample of 52 (30%) presented minimal amounts of diterpenoids which were not analysed further due to the absence of pine in the anthracological record from the site (Drieu et al., 2021). ...
... The study of the residues preserved in the ceramic matrix of Early Neolithic pottery in the northeast of the Iberian Peninsula has demonstrated the presence of multiple diterpenoids characteristic of aged Pinaceae resins in up to 31 ceramic vessels, representing 22% of the studied assemblage. This figure is in the range of the 30% of vases found at Pendimoun (Drieu et al., 2021), the 14% from studies in Greece and the Balkans (Garnier and Valamoti, 2016;Urem-Kotsou et al., 2018) and the 8% detected at Cueva del Toro (Tarifa-Mateo et al., 2019). Similar to the yields reported by Drieu et al (2021) and Hjulström et al. (2006), only small amounts of diterpenoids were recovered in the vessels, representing a maximum of 9% of the total lipid extract (CS11). ...
Article
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The use of resinous substances, certainly one of the earliest technologies developed by humans, was well-known by Holocene hunter-gatherers at the onset of the Neolithisation process across Europe. Recent research has revealed the use of birch bark tar in the central Mediterranean far from this taxon’s endemic regions both in the Paleolithic and Neolithic periods and shows that the first farmers from the Fertile Crescent hafted lithic tools and waterproofed artefacts using bitumen. The generalised absence of these natural products in south-western Europe may have thus forced a reformulation of Early Neolithic technologies by exploring and benefitting from existing knowledge in local European hunter-gatherer societies. However, information on resin use from the western Mediterranean is still scarce. Here, we report on the analysis of organic residues from 168 pottery sherds by gas chromatography and gas chromatography-mass spectrometry from 10 archaeological sites in this region dating from the second half of the VIth millennium to the first half of the Vth millennium cal BC. In a limited number of samples, minor amounts of several diterpenoids diagnostic of aged Pinaceae resins were detected as mixtures with fats. The presence of pine in the palynological and carpological record supports the human exploitation of this taxon, but its minimal incidence in the anthracological record suggests that other species were selected as fuelwood. This supports the hypothesis that Pinaceae resins were used in association with pottery sporadically but ubiquitously either as its contents, or as post-firing treatments to waterproof the vessels. This demonstrates the development of adhesive technologies and resin-involved labour processes specific to Early Neolithic societies.
... Most previous research objects were solid remains (including absorbed residues in pottery), while the study on liquid remains was rarely reported. Even though some were related to ancient wines [6][7][8][9][10], there is very little scientific analysis of the liquid remains. ...
... After a long burial process, liquor would be dried and some molecules might preserve inside pottery shards or in soil sediments within metal utensils. Organic residue analysis might be useful to identify the liquor remains and determine their type, and many attempts have been made [6][7][8][27][28][29][30][31][32]. Since 1990s, it has been thought that some organic acids could be used as markers of liquor residues, for that tartaric acid indicates wine [10] and oxalic acid indicates beer [33]. ...
Article
The analysis of solid residues and absorbed residues from archaeological contexts has developed rapidly, while the study of liquid residues is rarely reported. Liquid residues are often linked to liquor (alcohol drink) in China, but most of them have not been scientifically confirmed. Liquor has a nonnegligible influence on the history of human society, so it is important to characterize the liquor residue from the archaeological context. Moreover, it is generally believed that grain liquor has been mainly produced in East Asia for a long time, but grape wine did not appear until the Han Dynasty (2nd century BCE- CE 2nd century). In this study, a comprehensive analysis process of liquor residues with GC-MS and HPLC-MS/MS was designed and applied to liquids and silts unearthed at the Beibaie Cemetery (around 8th century BCE) in central China. The presence of volatile organic matter, organic acids, alcohols, esters and sugars show that these samples should be liquor remains. Then, this study discussed the limitations of organic acid criteria to judge the liquor type and emphasized the indicative significance of syringic acid to identify fruit wine. Thus, the general detection of syringic acid in the residues from Beibaie Cemetery indicate that they are the earliest known fruit wine remains in East Asia up to now, which advances the history of Chinese fruit wine-making by at least 500 years.
... The crushed forms indicate that the grapes were not simply cooked but were pressed to extract the juice for wine production. Such remains have been found in rich concentration at several sites in Europe, suggesting large-scale grape wine production (Figueiral et al., 2010;Garnier and Valamoti, 2016;Valamoti, 2015). ...
... While no single criterion is without problems, multiple strands of data provide the most reliable interpretations. For example, at the site of Dikili Tash in Northern Greece, chemical evidence of tartaric acid is corroborated by archaeobotanical remains of numerous crushed grape pips, providing strong evidence for wine production (Garnier and Valamoti, 2016). Similarly, in their analysis of pottery remains from Mijiaya in North China, archaeologists combined data from archaeobotanical remains, chemical evidence of oxalate, archaeological contexts, and ceramic typology to present a robust interpretation of beer making at the site (Wang et al., 2016). ...
Article
This special issue brings together recently developed theories and methodologies for understanding alcoholic beverages in the ancient world. While alcohol has continued to be a relatively overlooked research topic within anthropology/archaeology, the papers assembled for this special issue center the relationship between alcohol, rituals, and politics through novel archaeological fieldwork, analytical techniques, and theoretical concepts. In this introduction, we review established theoretical approaches to alcohol and drinking, explain the deep history of alcohol in human societies, and introduce papers in this special issue. We argue that alcohol production and consumption can be studied as a set of unique social phenomena that construct social identity, formulate political power, and precipitate historical transformations.
... Such foods make up 20 to 40% of the global food supply (Campbell-Platt, 1994). Although not all fermented foods contain ethanol, the majority of anthropological fermented food research to date targets ethanol as an indicator of fermentation (e.g., Dominy, 2015;Dudley, 2002;Garnier & Valamoti, 2016;Hayden et al., 2013;Kuijt, 2009;Liu et al., 2018;Milton, 2004;Ross et al., 2002;Smalley & Blake, 2003). ...
... Directed fermentation by humans has early origins. There is archaeological evidence that humans have engaged in directed fermentation of fruits and grains and stored the resulting ethanol in large quantities since 4300 B.C., although some suggest a date as early as 12,500 cal BP (Garnier & Valamoti, 2016;Hayden et al., 2013). Evolutionary changes in human genes for processing ethanol and for interacting with a major lineage of fermenting bacteria (Lactobacillales) are compatible with an even earlier association with fermented foods, dating back to the divergence of hominids from other primates at 10 ...
Article
Objectives Although fermented food use is ubiquitous in humans, the ecological and evolutionary factors contributing to its emergence are unclear. Here we investigated the ecological contexts surrounding the consumption of fruits in the late stages of fermentation by wild primates to provide insight into its adaptive function. We hypothesized that climate, socioecological traits, and habitat patch size would influence the occurrence of this behavior due to effects on the environmental prevalence of late‐stage fermented foods, the ability of primates to detect them, and potential nutritional benefits. Materials and methods We compiled data from field studies lasting at least 9 months to describe the contexts in which primates were observed consuming fruits in the late stages of fermentation. Using generalized linear mixed‐effects models, we assessed the effects of 18 predictor variables on the occurrence of fermented food use in primates. Results Late‐stage fermented foods were consumed by a wide taxonomic breadth of primates. However, they generally made up 0.01%–3% of the annual diet and were limited to a subset of fruit species, many of which are reported to have mechanical and chemical defenses against herbivores when not fermented. Additionally, late‐stage fermented food consumption was best predicted by climate and habitat patch size. It was more likely to occur in larger habitat patches with lower annual mean rainfall and higher annual mean maximum temperatures. Discussion We posit that primates capitalize on the natural fermentation of some fruits as part of a nutritional strategy to maximize periods of fruit exploitation and/or access a wider range of plant species. We speculate that these factors contributed to the evolutionary emergence of the human propensity for fermented foods.
... Even if precautions should be taken, notably to ensure the primacy of contextual information of the artefacts to be analyzed [1,2], this approach is restrictive since "absence of evidence is not evidence of absence". This is the example of tartaric acid, whose presence is systematically checked to prove the presence of wine/grape in a recipient, and numerous tailor-made analytical protocols were proposed for more than 25 years such as FT-IR spectroscopy, GC-MS and LC MS using different extraction procedures [3][4][5][6][7][8]. However, its absence is inconclusive since its longevity is not ensured due to its water solubility. ...
... As example, in amphorae forms known to have contained wine, most researchers focused on finding wine biomarkers such as organic acids and adapted an extraction procedure according to this purpose. To date, there are three of them, the approach proposed by McGovern et al. [5,6] and Garnier [8] with the same objective, ...
... Such foods make up 20 to 40% of the global food supply (Campbell-Platt, 1994). Although not all fermented foods contain ethanol, the majority of anthropological fermented food research to date targets ethanol as an indicator of fermentation (e.g., Dominy, 2015;Dudley, 2002;Garnier & Valamoti, 2016;Hayden et al., 2013;Kuijt, 2009;Liu et al., 2018;Milton, 2004;Ross et al., 2002;Smalley & Blake, 2003). ...
... Directed fermentation by humans has early origins. There is archaeological evidence that humans have engaged in directed fermentation of fruits and grains and stored the resulting ethanol in large quantities since 4300 B.C., although some suggest a date as early as 12,500 cal BP (Garnier & Valamoti, 2016;Hayden et al., 2013). Evolutionary changes in human genes for processing ethanol and for interacting with a major lineage of fermenting bacteria (Lactobacillales) are compatible with an even earlier association with fermented foods, dating back to the divergence of hominids from other primates at 10 ...
Article
Objectives Although fermented food use is ubiquitous in humans, the ecological and evolutionary factors contributing to its emergence are unclear. Here we investigated the ecological contexts surrounding the consumption of fruits in the late stages of fermentation by wild primates to provide insight into its adaptive function. We hypothesized that climate, socioecological traits, and habitat patch size would influence the occurrence of this behavior due to effects on the environmental prevalence of late‐stage fermented foods, the ability of primates to detect them, and potential nutritional benefits. Materials and methods We compiled data from field studies lasting at least 9 months to describe the contexts in which primates were observed consuming fruits in the late stages of fermentation. Using generalized linear mixed‐effects models, we assessed the effects of 18 predictor variables on the occurrence of fermented food use in primates. Results Late‐stage fermented foods were consumed by a wide taxonomic breadth of primates. However, they generally made up 0.01%–3% of the annual diet and were limited to a subset of fruit species, many of which are reported to have mechanical and chemical defenses against herbivores when not fermented. Additionally, late‐stage fermented food consumption was best predicted by climate and habitat patch size. It was more likely to occur in larger habitat patches with lower annual mean rainfall and higher annual mean maximum temperatures. Discussion We posit that primates capitalize on the natural fermentation of some fruits as part of a nutritional strategy to maximize periods of fruit exploitation and/or access a wider range of plant species. We speculate that these factors contributed to the evolutionary emergence of the human propensity for fermented foods.
... Such foods make up 20 to 40% of the global food supply (Campbell-Platt, 1994). Although not all fermented foods contain ethanol, the majority of anthropological fermented food research to date targets ethanol as an indicator of fermentation (e.g., Dominy, 2015;Dudley, 2002;Garnier & Valamoti, 2016;Hayden et al., 2013;Kuijt, 2009;Liu et al., 2018;Milton, 2004;Ross et al., 2002;Smalley & Blake, 2003). ...
... Directed fermentation by humans has early origins. There is archaeological evidence that humans have engaged in directed fermentation of fruits and grains and stored the resulting ethanol in large quantities since 4300 B.C., although some suggest a date as early as 12,500 cal BP (Garnier & Valamoti, 2016;Hayden et al., 2013). Evolutionary changes in human genes for processing ethanol and for interacting with a major lineage of fermenting bacteria (Lactobacillales) are compatible with an even earlier association with fermented foods, dating back to the divergence of hominids from other primates at 10 ...
Article
Objectives: Although fermented food use is ubiquitous in humans, the ecological and evolutionary factors contributing to its emergence are unclear. Here we investigated the ecological contexts surrounding fermented food use by wild primates to provide insight into its adaptive function. We hypothesized that climate, socio-ecological traits, and habitat size would influence the occurrence of this behavior due to effects on the environmental prevalence of fermented foods, the ability of primates to detect them, and potential nutritional benefits. Materials and Methods: We compiled data from field studies lasting at least nine months to describe the contexts in which primates were observed consuming fruits in the late stages of fermentation. Using generalized linear mixed-effects models, we assessed the effects of 18 predictor variables on the occurrence of fermented food use in primates. Results: Fermented foods were consumed by a wide taxonomic breadth of primates. However, they generally made up less than 3% of the annual diet and were limited to a subset of fruit species, many of which are reported to have mechanical and chemical defenses against herbivores when not fermented. Additionally, fermented food consumption was best predicted by climate and habitat size. It was more likely to occur in larger habitats with lower annual mean rainfall, higher annual mean maximum temperatures, and lower annual mean minimum temperatures. Discussion: We posit that primates capitalize on the natural fermentation of some fruits as part of a nutritional strategy to maximize periods of fruit exploitation and/or access a wider range of plant species. We speculate that these factors contributed to the evolutionary emergence of the human propensity for fermented foods.
... Other potsherds were buried for 12 mo in different environments in order to evaluate the degradation of wine molecules in Experimental Approach. Following the most recent publications in terms of identification of grapevine products (23,53), two successive extractions were used. Approximately 2 g ceramics were drilled into the inner walls of the potsherds, after removal of the outer surface (1 to 2 mm), to remove contamination from the surrounding sediments and from the handling. ...
... The mass spectrometer used was an Agilent 5977B, used in electron ionization mode (EI, 70 eV), with mass spectra acquisition between Chemical evidence for the persistence of wine production and trade in Early Medieval Islamic Sicily m/z 50 and 1,000. The presence of TA was identified from the mass spectrum of trimethylsilylated TA dibutyl ester (m/z 147, 276, and 391) (53). In some samples, a peak of trimethylsilylated TA methyl butyl ester (m/z 147, 234, 276, and 349), resulting from the reaction with residual methanol from the DCM/MeOH extraction, was also considered for quantification. ...
Article
Significance As a high-value luxury commodity, wine has been transported across the Mediterranean since the Bronze Age. The wine trade was potentially disrupted during political and religious change brought about by Islamization in the Early Medieval period; wine consumption is prohibited in Islamic scripture. Utilizing a quantitative criterion based on the relative amounts of two fruit acids in transport amphorae, we show that wine was exported from Sicily beyond the arrival of Islam in the ninth century, including to Christian regions of the central Mediterranean. This finding is significant for understanding how regime change affected trade in the Middle Ages. We also outline a robust analytical approach for detecting wine in archaeological ceramics that will be useful elucidating viniculture more broadly.
... On the other hand, grapevine management in northern Greece may be supposed as early as the 5th millennium BC, i.e. long before the emergence of the Mycenaean civilization in Southern Greece, according to the discovery of grape pips on several sites, in some places in large quantities and/or associated with grapevine charcoal (Renfrew 1995;Megaloudi 2006;Valamoti 2009Valamoti , 2015Valamoti et al., 2007Valamoti et al., , 2015Pagnoux 2019). The first evidence of wine making comes from Dikili Tash in northern Greece, dated to the Neolithic 4500-4000 BC (Valamoti et al., 2007Garnier and Valamoti 2016). Several lines of evidence raise therefore the question of the geographic origin of the domesticated grapevine in Greece and the question of the chronological origin and development of viticulture in relation to social, economic and cultural changes during prehistoric and historical times. ...
... Besides these first indications for grapevine cultivation in northern Greece dated to the Late Neolithic, evidence for juice extraction and wine making is provided by the large concentration of grape pips from Dikili Tash (Late Neolithic, 4500-4000 BC), where 2460 grape pips have been discovered, associated with other by-products of pressed grapes (pedicels and skin fragments) while tartaric and malic acids, present in grapes, as well as other acids characteristic of alcoholic fermentation were detected on sherds (Valamoti 2004(Valamoti , 2015Valamoti et al. 2007Valamoti et al. , 2015Garnier and Valamoti 2016). The joint discovery of these remains clearly testifies to wine making in Greece as early as the Late Neolithic. ...
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Grapevine (Vitis vinifera L.) is one of the emblematic crops of Greece. Despite evidence of early wine making in the Aegean since the Late Neolithic (ca 4500–4000 BC), the hypothesis of a local domestication of the grapevine in this area hasn't be thoroughly investigated. In order to date the first appearance of the domesticated grapevine and to explore the past cultivated diversity in the Aegean, morphometric analyses were performed on a large data set of 2223 archaeological grape pips from 11 sites located in various areas of Greece and dated to the Late Neolithic, Bronze Age and Archaic period (6th millennium BC - 7th century BC). All the grape pips from the Late Neolithic are morphologically wild. The shift from wild to domesticated shape occurred during the Middle Bronze Age (1900–1700 BC). From the Late Bronze Age (1500–1100 BC) onwards, domesticated types dominate almost all the assemblages. Possible indication of a local domestication process is provided by pips dated to the Early Bronze Age. Also still in the range of modern wild specimens, their shape is an intermediate between the Neolithic pips and those dated to later periods. A high morphological diversity characterizes the Late Bronze Age and Archaic assemblages. These grape pips are mostly allocated to modern varieties from the Balkans, Caucasus and South-West Asia. The geographical origin of the identified varieties may reflect introduction of cultivars from the eastern Mediterranean, but may also testify to an early stage of local domestication and grapevine diversification.
... The statement that wine was contained in the jars was not based solely on the presence of tartaric acid, which can be judged inconclusive (Stern et al. 2008;Barnard et al. 2011), but on the joint identification of a variety of organic compounds thought to be typical of grapes and/or wine. Tartaric, citric and malic acids can be found in large amounts in dark grapes, while succinic acid is regarded as a fermentation marker (Garnier and Valamoti 2016). The combination of these different biomarkers is probably the strongest evidence for ancient wine that can be obtained through chemical analysis. ...
... In Late Neolithic Dikili Tash, northern Greece, early wine making is suggested by the simultaneous presence of grape pressing residues (Valamoti 2015) and by chemical evidence of wine in associated vessels (Garnier and Valamoti 2016). The GMM study of these pips shows that only the wild morphotype was present (Valamoti et al. 2020) and therefore that this wine was produced from undomesticated grapes. ...
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The Near East and the Caucasus are commonly regarded as the original domestication centres of Vitis vinifera (grapevine), and the region continues to be home to a high diversity of wild and cultivated grapevines, particularly within Georgia. The earliest chemical evidence for wine making was recorded in Georgian Neolithic sites (6000–5800 bc) and grape pips, possibly of the domesticated morphotype, have been reported from several sites of about the same period. We performed geometric morphometric and palaeogenomic investigations of grape pip samples in order to identify the appearance of domesticated grapevine and explore the changes in cultivated diversity in relation to modern varieties. We systematically investigated charred and uncharred grape pip samples from Georgian archaeological sites. Their chronology was thoroughly assessed by direct radiocarbon dating. More than 500 grape pips from 14 sites from the Middle Bronze Age to modern times were selected for geometric morphometric studies. The shapes of the ancient pips were compared to hundreds of modern wild individuals and cultivated varieties. Degraded DNA was isolated from three pips from two sites, converted to Illumina libraries, sequenced at approximately 10,000 single nucleotide polymorphism (SNP) sites, and compared to a large public database of grapevine diversity. The most ancient pip dates from the Middle Bronze Age (1900–1500 cal bc) and the domesticated morphotype is identified from ca. 1000 bc onwards. A great diversity of domesticated shapes was regularly seen in the samples. Most are close to modern cultivars from the Caucasian, southwest Asian and Balkan areas, which suggests that the modern local vine diversity is deeply rooted in early viticulture. DNA was successfully recovered from historic pips and genome-wide analyses found close parental relationships to modern Georgian cultivars.
... Hexatriacontane (C36 n-alkane; 1 μg) was added to each of the samples prior to analysis for quantification purposes. Since wine was a possible product, each sample was re-extracted (BF 3 extraction) using established protocols (Garnier and Valamoti, 2016) to target shortchain carboxylic compounds present in fruit products. ...
... Due to the possible presence of wine in the vessels analysed, shortchain carboxylic compounds were targeted as part of the analysis. The identification of wine in archaeological contexts has generally been based on the presence of tartaric acid, due to its high composition in grapes (Barnard et al., 2011;Garnier and Valamoti, 2016;Pecci et al., 2013;Stern et al., 2008). In the Castelluccio samples, no tartaric acid and/or other associated markers were identified, except for malic acid, a dicarboxylic acid present in various fruits including grapes (Ribereau-Gayon et al., 2006), in sample CST-004. ...
Article
The study of vessel content can reveal important information about the dietary and culinary preferences of ancient communities. In this preliminary study, we analysed the absorbed lipid content of ten vessels from the settlement of Castelluccio in Sicily, dating to the Early Bronze Age (EBA). The vessels tested included a small selection of ceramic forms typically found in Bronze Age sites in Sicily, namely fine drinking wares and coarse ware vessels thought to have been used in food preparation and/or storage. All of the vessels tested were recovered from Hut 8. ORA results of this pilot project revealed challenging lipid preservation conditions known to occur in the Mediterranean region. Lipid analysis showed a possible animal contribution, although a plant input could not be excluded. Wine was not identified in the vessels tested.
... Wine was the earliest fermented beverage since, contrary to beer production, grapes only need to have their skins broken open to release the juice (Singleton 1996). Although exactly where wine was first made is still uncertain, early evidence of wine production is suggested by several research studies (McGovern et al. 2017;Valamoti et al. 2007;Garnier and Valamoti 2016). ...
... In a house at the Greek Neolithic village site of Dikili Tash (c. 4300 BC), a charred grapevine (Vitis vinifera) and jars containing grape pips with skins attached were found (Valamoti et al. 2007;Garnier and Valamoti 2016). The oldest winery was located in the Areni-1 cave in southern Armenia (c. ...
Chapter
The cultivation and domestication of the grape appear to have occurred between 7000 and 4000 BC. The archaeological and historical evidences suggest that the domestication of the grapevine took place in the Near East. Nevertheless, whether a single origin or secondary independent grapevine domestications occurred and where they happened remains so far unanswered. Wine has had an important role in religious rituals since antiquity. In mythology and theology, wine was symbolic of the power to revitalize and rebirth. In ancient Egypt, wine was daily served to the gods by the Pharaoh and the priests in ritual ceremonies in the Egyptian temples. In daily life, wine was an enjoyable drink consumed by the elite in festivals, banquets and funerals. Further, the grape was one of the most important fruits in the classical Mediterranean civilizations and grapevines and the wine were widely spread through trade sea routes. This chapter presents an overview of the archaeological evidence for wine culture in the ancient Near East, Egypt and the Mediterranean region. It also presents a discussion of the chemical and morphological research methods and paleogenomic analyses that have been applied to ancient grape and plant material.
... If this is the case, the fermentation of grape juice must have been underway when the house was destroyed by fire. A small number of grape pips and skins were reported from Building 3 as well (Valamoti 2004), suggesting that wine making may have been practiced by several households at the site, the earliest evidence to date for wine making in the Aegean and the Eastern Mediterranean (Garnier and Valamoti 2016;Valamoti 2015;Valamoti et al. 2007). The grape pips have been identified as morphologically wild (Mangafa and Kotsakis 1996), yet their cultivation or early management cannot be excluded (Valamoti 2015;Valamoti et al. 2007Valamoti et al. , 2015. ...
... At Yangjiaping, malic acid and citric acid appeared in Houlou. Both acids exist in a wide range of fruits (Pecci et al., 2013;Garnier and Valamoti, 2016;Drieu et al., 2020) and the results evidenced the presence of fruit drink in Houlou at a later stage of Han Dynasty. ...
Article
Ritual bronze vessels are the most important artefacts in the Chinese Bronze Age. Based on typological studies, different vessel types were linked with specific sacrificial offerings, for example meat, crop and alcohol, which further implied vessel functions and ritual traditions in early Chinese history. However, direct evidence of the original food and drink contents in the bronze vessels was largely missing and information was mostly inferred from casting inscriptions and historical records. To test the potentials of lipid residue analysis in ritual bronzes, we selected sediments associated with 17 bronzes from the Dahan Cemetery, Shandong Province, 11 bronzes from the Sujialong Cemetery and 1 from the Yangjiaping Cemetery, Hubei Province. Samples were collected from different positions of the vessels and characteristic types of bronzes to compare their lipid profiles. The results showed that solvent extraction yielded the highest concentrations of steroids at Dahan, while alkaline saponification recovered the most abundant lipid classes at Yangjiaping and Sujialong. Different extraction methods may be selected based on burial environments and research objectives. At Dahan, the lipid profiles from sediments attached to the interior bottom of the vessel which mixed with corrosion products displayed distinctive features in contrast to the lipids from environmental background, demonstrating their potentials in indicating original foodstuffs. The lipid results from Sujialong exhibited larger contributions from the burial environment. Sacrificial bronze vessels generally displayed different lipid compositions associated with their food and alcohol contents, showing the indicative significance of bronze residues. Long-chain fatty acids and plant steroids dominated the lipid profiles of Dui, Dou, Gui, Li and Fu, which have traditionally been considered as food containers, although the origins of plants cannot be confirmed. The presence of miliacin in the bronzes of Hu and Zunfou at Dahan points to the use of millets, probably as alcoholic beverage. At a later stage, fruit drink appeared in Houlou at Yangjiaping.
... BP), all of which is presumed to have relied on truly wild populations of grapes 26,48,66 . Clearer evidence for wine production, likely on a larger scale, dates to ca. 5000 BP in Anatolia 62 and northern Greece 36,67,68 . Other research suggests that the earliest domesticated grapes were present in the Caucasus by around 6000 BP 69 and the first cultivated morphotypes introduced to that region were still on a trajectory towards a more modern-looking domesticated form, some of these morphologically look more derived and others looking more plesiomorphic. ...
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The region of Transoxiana underwent an early agricultural-demographic transition leading to the earliest proto-urban centers in Central Asia. The agronomic details of this cultural shift are still poorly studied, especially regarding the role that long-generation perennials, such as grapes, played in the cultivation system. In this paper, we present directly dated remains of grape pips from the early urban centers of Sapalli and Djarkutan, in south Uzbekistan. We also present linear morphometric data, which illustrate a considerable range of variation under cultivation that we divide into four distinct morphotypes according to pip shape. While some of the pips in these two assemblages morphologically fall within the range of wild forms, others more closely resemble modern domesticated populations. Most of the specimens measure along a gradient between the two poles, showing a mixed combination of domesticated and wild features. We also point out that the seeds recovered from the Djarkutan temple were, on average, larger and contained more affinity towards domesticated forms than those from domestic contexts. The potential preference of morphotypes seems to suggest that there were recognized different varieties that local cultivators might aware and possibly propagating asexually.
... In addition, the search for polar molecules, such as fruit acids, with appropriate extraction methods (e.g. Garnier & Valamoti, 2016), should be implemented to determine whether it is possible to improve interpretations in terms of content (molecular profile) and function (absorption profiles along the vertical transect). ...
Article
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Investigating the organic content of archaeological pottery has largely focused on identifying food commodities, but their use and mode of processing still need to be thoroughly investigated. The present study aims to explore the diversity of organic residue absorption patterns, over a wider range of functions than previously studied by experimentation, by analysing ceramics still in use today. A field survey in Bedik Country, Senegal, where the use of pottery is still alive, was conducted to document the uses of ceramics and to interview potters and users of the vessels. As a preliminary study, nine ceramics whose use was recorded were investigated through 59 samples for their absorbed molecular profiles, lipid concentrations, and the preservation of triglycerides and C18 unsaturated fatty acids. The interpretations were first carried out as a blind test and then compared with the actual use. Lipid concentrations and molecular profiles indicated a diversity of contents, and the comparison of samples taken along the vertical transects of the vessels resulted in pottery function hypotheses that were broadly aligned with the actual uses. Cooking pots for fat-rich products were successfully identified, but the various documented patterns showed that lipid accumulation in ceramics is more complex than expected. Although caution is required to adopt this approach for archaeological pots, the vessel for fermenting plant products has been identified. Last, this work pointed out that ceramics can be used for a wider range of purposes than those usually considered for archaeological pottery, such as steaming or cooking non-food products.
... Organic residue analysis on pottery, a major class of archaeological artifact used for food processing, has enabled new understandings of the adoption and use of particular foodstuffs throughout space and time, such as dairy products (Evershed et al. 2008;Wilkin et al. 2020), fish (Courel et al. 2020;Lucquin et al. 2018), and plants (Hendy et al. 2018;Heron et al. 2016). A large body of research on organic residues has focused on detecting evidence of alcoholic beverages, such as beer and wine (Barnard et al. 2011;Garnier and Valamoti 2016;Guasch-Jané et al. 2006), with a search for "biomarkers" diagnostic of ferments (Guasch-Jané et al. 2004;Isaksson, Karlsson, and Eriksson 2010). However, the robustness of some biomolecular markers for these beverages has been called into question (Drieu et al. 2020). ...
Article
Recent discoveries on the importance of microbes for human biology, health, and culture, the rise of antimicrobial resistance, and developing technological advancements necessitate new dialogues about human relationships with microbes. Long perceptible only through their transformations—from epidemic disease to alcoholic beverages—it is now possible to more fully perceive the diversity of ways in which we influence and are influenced by microbes and to understand that human and microbial cultures are fundamentally intertwined. In the introduction to this supplement, we outline the current state of the art of an “anthropology of microbes” in three subfields of anthropology: biological anthropology, cultural anthropology, and archaeology. Moreover, as a result of dialogues borne out of the symposium associated with this issue, and now reflected in the articles themselves, we discuss the interactions between and within the subfields of anthropology. This supplement is committed to the development of a common language for an emerging anthropology of microbes, and in order to shape genuine transdisciplinarity we argue for the continued necessity of “trading zone” points of intersection— such as the Wenner-Gren Foundation’s symposium “Cultures of Fermentation.” © 2021 The Wenner-Gren Foundation for Anthropological Research. All rights reserved.
... Considering these caveats, the earliest evidence of wine production seems best supported for the Late Neolithic of Northern Greece (Garnier and Valamoti 2016), where the chemical evidence is supported by archeobotanical remains of crushed grape pips. For earlier claims (McGovern et al. 1996(McGovern et al. , 2004(McGovern et al. , 2017 where the archeobotanical evidence is less forthcoming, the chemical evidence needs to be treated more critically. ...
Article
Pottery production, like fermentation, is a highly skilled technology that requires the careful selection and transformation of raw ingredients under controlled conditions. Although the precise drivers for the invention and dispersal of ceramic containers are uncertain, it is clear that even the earliest pottery had a culinary role for processing foods. We now know from organic residue analysis that early pottery was used to process only a relatively limited range of the foodstuffs available, with biases, for example, toward fish among some hunter-gatherers or dairy products by early farmers. One reason for such selection might have been that pottery is well suited for the transformation of perishable fresh produce, such as milk and fish, to long(er)-life products that could be stored, exchanged, or accumulated. Such fermented products would be particularly useful for maximizing the return from seasonally abundant foods, thereby facilitating sedentism and greater investment in pottery production. Notwithstanding the fact that direct chemical evidence for fermentation is difficult to obtain, here it is proposed that the early uses of pottery and fermentation and the accumulation of storable surpluses are interrelated technologies that emerged in early sedentary or semi-sedentary societies during the final Pleistocene and start of the Holocene.
... Until relatively recently, our understanding of when humans began to utilize fermented foods was based heavily on the archaeological record, which commonly associates fermented food consumption with fermented food production as well as agriculture and/or domestication, tool use, and food storage. In this context, the earliest reliable evidence for fruit and grain fermentation is from Greece in about 4300 BC (although some suggest a date as early as 12,500 cal BP in the Middle East [Garnier and Valamoti 2016;Hayden, Canuel, and Shanse 2013]). Ceramics for use with dairy products found in Southeast Asia, southwestern Europe, and North Africa suggest fermentation of these foods by ca. ...
Article
Fermented foods are an important part of the human diet. While the types of fermented foods consumed as well as the processes used to create them vary regionally, the majority of human populations globally deliberately produce and consume fermented foods as a central part of their diets. This pattern is in contrast to that of other vertebrates, including nonhuman primates. However, it remains unclear when and why humans began to include high amounts of fermented foods in their diets. Here, we review existing knowledge regarding the timing and impetus for the emergence of fermented food use by humans and put forth a new hypothesis that fermented food use began as a “predigestion” strategy to increase nutrient availability in harsh, terrestrial environments with physically and chemically defended food resources. We explore support for this hypothesis in comparative behavioral and physiological data from extant nonhuman primates. Together the data presented in this paper suggest that food fermentation may have had an impact on human evolutionary trajectories via interactions with human biology and health. Future work should build on this foundation to interrogate these processes in more detail. © 2021 The Wenner-Gren Foundation for Anthropological Research. All rights reserved.
... This fact can be explained by the low solubility of tartaric acid in ethyl acetate [39] . Unlike acid treatment, the use of BF3 [46] accelerates the extraction of tartaric acid. In fact, Drieu et al. (2020) reported that 77% amount yield for standard pure tartaric acid was obtained in such conditions. ...
Article
Scientific analysis has provided new evidence in historical and archaeological studies in recent years. Archaeological samples are frequently contaminated because of conservation conditions and/or cleaning before restoration. Roman amphora, made of a material of great interest, is no exception. This study develops the chemical analysis of Dressel I amphorae coming from the Châteaumeillant oppidum in France, dating from the 2nd century-1st century BC. Traces of organic matter located on the internal surface of the amphorae were identified using a gas chromatography-mass spectrometry (GC–MS). This analytical technique notably allows markers of resinous matter (pitch) and wine to be detected. Analytical results showing the presence of syringic acid, along with other wine acids (benzoic, succinic and vanillic acids) in certain amphorae in the archaeological context, demonstrated that the vessels had contained wine. Moreover, two families of resins (Pinaceae and Cupressaceae) were observed. They were used for waterproofing or as an additive to resinated wine. In particular, the observation of sandarac resin (Cupressaceae) is rare in wine amphorae.
... The mineralogical composition of the paste (clay minerals and non-plastic inclusions) determines the type of interactions that are formed with organic matter (e.g. hydrogen bonds, dipole-dipole interactions, ion-dipole or electrostatic interactions; Correa-Ascencio Craig et al., 2004;Garnier & Valamoti, 2016;Goldenberg et al., 2014;Matlova et al., 2017) and the variable strength of these bonds influences the level of degradation of organic matter. It should be noted that the mineral composition may be slightly modified during the use of the vessel or due to taphonomic processes (addition of certain cations, for example, via cooking water or stream water; Correa-Ascencio & . ...
Article
Over the past thirty years, the study of the exploitation of natural substances by ancient societies has been a major focus of organic residue analysis in ceramics. However, the mechanisms controlling the absorption and preservation of organic matter within the walls of pottery at all stages of a vessel’s lifecycle are still very poorly understood. Organic and mineral composition of the paste, surface treatments, porosity, environmental conditions of disposal of the vessel are likely to influence the organic signal preserved over time. Storage conditions of the archaeo logical material can also affect the preservation of organic matter after excavation. Recent studies are beginning to address these issues, and the first results are already refining the interpretations of organic residue analysis and opening up new fields of investigation, particularly with regard to the study of the ceramic manufacturing chaîne opératoire, burial environments and potential contamination.
... Firstly, c. 1 mm of the surface was removed by a scalpel in order to avoid as much modern pollution as possible and then c. 100 mg of ceramic powder was scraped off more in-depth (around 1-2 mm). Lipids were extracted using the following double-step methodology (Garnier & Valamoti, 2016): a first lipid extraction was carried out following the classical method described by Charters et al. (1995), using a mixture of dichloromethane/ methanol (1:1, v/v) under ultrasonication for 30 min. The mixture was then centrifuged, and the upper organic phase collected, filtered through a silica gel column and evaporated to dryness, giving the first lipid extract labelled 1LE. ...
Article
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Two amphoras found at burials outside the ancient city of Thāj, Saudi Arabia, bear inscriptions mentioning wine. The chemical analysis of the content of one of them confirms the presence of wine and more precisely as red wine. Contextual information from one of the graves suggests that wine was consumed as part of burial rituals. One inscription is in Aramaic and the other is in South Arabian cursive or zabūr—in fact the first attestation for this particular script in the core region of the so‐called Hasaitic writing culture. Complementing the recent discoveries of zabūr inscriptions from Mleiha (Sharjah, UAE), this inscription buttresses our idea of the emergence of writing in East Arabia in the Hellenistic period.
... In antiquity, records of human use of domesticated grapes from archaeological remains go back to the Early Bronze Age in the Near East (see Miller 2008 for summary), with residue analysis pushing wine use back to the Neolithic in the Near East McGovern 2003) and Greece (Pagnoux et al. 2021). Archaeobotanical remains consisting of grape pressing is supporting it (Garnier and Valamoti 2016). Evidence for wild grape exploitation can be found even as far back as Palaeolithic deposits (Hansen and Renfrew 1978;Vaquer et al. 1986;Marinval 1997;Martinoli 2004;Weiss et al. 2004). ...
Article
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Grape (Vitis vinifera L. ssp. vinifera) has been identified as part of the Indus Civilization crop assemblage. As a non-native crop, with a wild ancestor that does not grow in the region, its presence in northern South Asia ca. 3200–1300 bc has thus been used to argue variously as evidence for crop diffusion, long distance trade, and the adoption of foreign agricultural strategies and foodways. Grape identification, particularly between wild and domesticated species, is complex. In this article the challenges of identifying ‘grape’ in South Asian antiquity are explored. The overreliance on length, breadth and thickness measurements, with limited description and a lack of standardisation are considered. Furthermore, an examination of the local flora demonstrates that there are multiple Vitaceae genera being possible ‘grape’ contenders in the region. Identification criteria for local Vitaceae need to be better developed to more understand the role of Indus grapes in order for the complicated social interpretations of ‘what grapes means in the Indus’ to be maintained.
... Viticulture is a complex agro-system: grapevine productivity, in addition profitability, depend on several factors such as soil management practices, soil fertility, breeding, propagation techniques, selection and constitution of new varieties, meteorology, climate, also in general from an intense interaction between humans and environment (Moriondo et al., 2015;Garnier and Valamoti, 2016). It is expected that the impact of climate change on viticulture will be significant (Scherrer et al., 2016), the future scenario will be characterized by a general reduction of the precipitation, higher temperatures, an increased tropical nights and more consecutive dry days' number (Santillàn et al., 2019). ...
Article
Climate change has an important impact on the phenological phases of the grapevine. The consequences are directly reflected in quantitative and qualitative characteristics of the grapes. In fact, there is a decrease in the skin-to-pulp ratio (therefore a decrease in production with an excess of alcohol) and a consequent reduction in the aromatic potential of white grapes (lowering of the quality of musts). Volatile tioles are important aromatic compounds found in various foods and drinks; in particular they contribute to forming the aroma of some types of white wines as they are characterized by extremely low perception thresholds. This work aimed to evaluate the effects of water stress on ecophysiology, technological maturity and on the thiol precursors of Vitis vinifera L. cv. Sauvignon Blanc vineyards in the Tuscan region (Italy) during two seasons. To this end, three treatments were established: WW (well watered), MW (medium watered), and WS (water stress with no irrigation). During the seasons, measurements were made of single-leaf gas exchange, pre-dawn and leaf midday water potential, leaf temperature, chlorophyll fluorescence, as well chlorophyll content. In addition, the parameters of plant yield, technological maturity (° Brix, acidity, pH and berries weight) and the precursors of 3-Mercaptohexanol (3MH) were analyzed: 3-S-cysteinylhexan-1-ol (Cys-3MH) and 3-S-glutathionylhexan-1-ol (GSH-3MH). Well watered treatments (WW) showed less negative water potential, a higher rate of photosynthesis, of stomatal conductance, a lower leaf temperature (°C). Furthermore, WW showed higher levels of precursors accumulation (Cys-3MH and GSH-3MH) than the other treatments during two seasons. Technological analyses (° Brix and acidity) showed significant differences between WW and WS treatments. The lower berry weight was found in the WS treatment. Finally as a result of climate change, precision irrigation has proved to be a good technique to rebalance the gap between technological and aromatic maturity in Sauvignon Blanc grapes.
... Thus, Guasch-Jané et al.'s extraction solvent is tailored to the mobile phases used in their successfully detecting tartaric acid/tartrate by liquid chromatography with tandem mass spectrometry (LC-MS/MS). By contrast, gas chromatography-mass spectrometry (GC-MS), which is the preferred method of Garnier and Valamoti (2016) and Drieu et al., need to follow a different extraction and detection route, especially since common derivatization agents cannot be used in conjunction with water that will cause hydrolysis of the targeted compounds, thereby limiting what can be tested for by this technique unless precautions are taken. Consequently, care must be taken when trying to adapt extraction techniques intended for LC-MS/ MS to another analytical platform such as GC-MS. ...
Article
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Comparable to Drieu et al.’s viewpoint, we argue that it is possible to identify ancient Eurasian grape wine by current biomolecular methods, but only in conjunction with the relevant archaeological, archaeobotanical, and other natural and social scientific data. Additionally, we advocate an inductive–deductive working hypothesis model, which is appropriate for the “historical science” of archaeology. We focus on two key deficiencies of Drieu et al.’s argumentation: (1) the assumption that Guasch-Jané et al. (2004) extracted their ancient samples with potassium hydroxide before testing for tartaric acid/tartrate, and (2) the supposition that 5000-year-old yeast DNA would not be preserved in the hot climate of Egypt but rather represents modern contamination.
... Viticulture is a complex agro-system: grapevine productivity, in addition profitability, depend on several factors such as soil management practices, soil fertility, breeding, propagation techniques, selection and constitution of new varieties, meteorology, climate, also in general from an intense interaction between humans and environment (Moriondo et al., 2015;Garnier and Valamoti, 2016). It is expected that the impact of climate change on viticulture will be significant (Scherrer et al., 2016), the future scenario will be characterized by a general reduction of the precipitation, higher temperatures, an increased tropical nights and more consecutive dry days' number (Santillàn et al., 2019). ...
... Archaeobotany and organic residues in ceramic vessels allowed investigating early cultivation and use of Vitis vinifera in Georgia [42,87], the Near East [88] and the eastern Mediterranean [89]. The most ancient proofs of wine production may be dated to the Neolithic (6000-5800 BC) without the possibility of distinguishing if the wine was produced from wild or domesticated Vitis vinifera both exploited in the South Caucasus [42]. ...
Article
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The recovery of inaperturate pollen from functionally female flowers in archaeological layers opens the question of a possible pollen-based discrimination between wild and domesticated Vitis vinifera in prehistoric times. Pollen analysis applied to archaeology has not routinely considered the existence of pollen dimorphism in Vitis, a well-known trait in the field of agrarian studies. Therefore, the inaperturate shape of grapevine pollen is ignored by studies on the archaeobotanical history of viticulture. In this paper we investigate pollen morphology of the domesticated and wild subspecies of V. vinifera, and report the first evidence of inaperturate Vitis pollen from an archaeological site. We studied exemplar cases of plants with hermaphroditic flowers, belonging to the subspecies vinifera with fully developed male and female organs, cases of dioecious plants with male or female flowers, belonging to the wild subspecies sylvestris and cases of V. vinifera subsp. vinifera with morphologically hermaphroditic but functionally female flowers. The pollen produced by hermaphroditic and male flowers is usually trizonocolporate; the pollen produced by female flowers is inaperturate. This paper reports on the inaperturate pollen of Vitis found in an archeological site of the Po Plain, Northern Italy. The site dated to the Bronze Age, which is known to have been a critical age for the use of this plant with a transition from wild to domesticated Vitis in central Mediterranean. Can the inaperturate Vitis pollen be a marker of wild Vitis vinifera in prehistoric times? Palynology suggests a possible new investigation strategy on the ancient history of the wild and cultivated grapevine. The pollen dimorphism also implies a different production and dispersal of pollen of the wild and the domesticated subspecies. Grapevine plants are palynologically different from the other Mediterranean "cultural trees". In fact, Olea, Juglans and Castanea which are included in the OJC index, have the same pollen morphology and the same pollen dispersal, in wild and domesticated plants. In contrast, the signal of Vitis pollen in past records may be different depending on the hermaphroditic or dioecious subspecies.
... Tartaric, succinic together with malic acid, are present in three of these samples (OL5, 6 and 10), suggesting that these amphorae were used to contain grape derivatives (Table 2). In fact, while other fruits may also contain tartaric acid (Barnard et al. 2011), this acid is particularly abundant in grape, and it is usually considered the marker of grape derivatives (Barnard et al. 2011;Drieu et al. 2020;Garnier and Valamoti 2016;Guash-Jané et al. 2004;Pecci 2018;Pecci, Cau Ontiveros, and Garnier 2013;Pecci et al. , 2017Pecci et al. , 2020Rageot et al. 2019). In particular, for the investigated period and region, it is possible to hypothesise that these amphorae contained wineor its derivatives. ...
Article
Amphorae are key materials in the investigation of the production and transport of goods in ancient times. For the Roman period, many typologies of amphorae are standardised and there are hypotheses concerning their uses and contents mainly based on the shape, provenance, tituli picti and, when preserved, the solid contents. However, there are still many amphora types that have to be investigated in order to better understand the economy of the regions where they were produced and filled. This is the case of the amphorae object of this paper: the so-called ovoid amphorae of Hispania Ulterior/Baetica. This paper presents new results of an interdisciplinary investigation aimed to discover the commodities contained in ovoid amphorae. This amphora type and its specific use have never been investigated, except for a preliminary test. Here, organic residues analysis of twenty-four amphorae produced in two different locations in Hispania Ulterior/Baetica (Bay of Cadiz and the Guadalquivir Valley) and excavated at the site of El Olivillo in Cadiz (Spain), are presented. The findings suggest that the majority of the amphorae were coated with abundant pitch derived from Pinaceae trees and that most of them contained grape derivatives, although other products were also identified. Not only is this documentation of Hispania Ulterior/Baetican wine production in the late Republican period important, but the use of ovoid amphorae for carrying wine is somewhat unexpected because it is usually thought that amphorae of this type in southern Italy and in the Corinthia probably carried olive oil.
... As discussed above, the uncertainties surrounding the origin of starch grain damage patterns are too great to constitute the only source of evidence for cooking or brewing. Supporting evidence should be obtained using other methods, which could include, among others, evidence for cooking or brewing from the analysis of macrobotanical remains (e.g., Bouby et al., 2011;Margaritis and Jones, 2006;Valamoti, 2011Valamoti, , 2018, microstructural evidence from macroscopic food and malting remains (e.g., González Carretero et al., 2017;Heiss et al., 2017Heiss et al., , 2020Samuel, 1996;Valamoti et al., 2008Valamoti et al., , 2019 and the analysis of microscopic remains (e.g., yeast and fungi) and chemical markers associated with the fermentation process (e.g., Garnier and Valamoti, 2016;Liu et al., 2019;Michel et al., 1993;Pecci et al., 2013;Wang et al., 2016). More indirect evidence could also be obtained from the analysis of stable isotopes from human remains, which might confirm whether a particular foodstuff identified in the starch assemblage was indeed part of the diet (e.g., Tao et al., 2020), and the presence of phytoliths showing evidence of heating in pottery vessels potentially used for cooking-although certain disagreement exists regarding the accuracy of the different methods developed to this end (see Devos et al., 2020 and references therein). ...
Article
The analysis of starch grains from food-related archaeological artefacts and human dental calculus has provided evidence for the consumption of plant resources worldwide. Recently, and based on experimental research, starch grain analysis has also been used as a proxy to reconstruct food transformation in the archaeological record through the analysis of the damage produced on starch grains by different food-processing techniques such as grinding, boiling and fermentation. The prospect of identifying food transformation through starch grain analysis opens exciting avenues for exploring the cultural factors underlying culinary practices. However, the structural integrity of starch grains may be affected by a variety of depositional and post-depositional processes, including but not limited to food processing, so that in order to identify damage produced by food processing one would first need to discard potential damage occurred at later stages (e.g., in the burial environment, during laboratory processing and analysis, etc.). The identification of food processing through the analysis of the damage produced on starch grains is further obscured by equifinality and multifinality, as exemplified by un-cooked modern reference material presented here showing damage patterns consistent with "boiling", "spouting" and "fermenting". Consequently, the identification of food transformation in the archaeological record through the analysis of the damage produced on starch grains needs to be supported by reliable contextual information, a representative number of samples and the existence of alternative sources of evidence (i.e., a multi-proxy approach).
... Also, the archaeobotanical evidence from this region has led to the suggestion that there was a transitional phase during which the grape pips were neither wild, nor domesticated in their entirety (Renfrew 1995;Valamoti et al. 2007;Valamoti et al. 2015). The finds from Dikili Tash (charred grape pips and wine pressings) represent the earliest evidence (secold half of the V th millennium BC) for the use of grape juice and/or wine in the Aegean and the eastern Mediterranean in general, during the Neolithic period (Valamoti et al. 2007;Valamoti et al. 2015;Garnier and Valamoti 2016). The answers that concerns the beginnings of winemaking and viticulture have to be sought in the history of the civilisations that populated the Earth a few millenia ago. ...
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This paper reviews the, so far available, paleorecords of Vitis sylvestris C.C. Gmel and Vitis vinifera L. from Romania. The study takes into consideration the presence of Vitis pollen from Holocene peat sediment sequences and archaeological context, but also the presence of macrorests from various archaeological sites that date from Neolithic, Chalcolithic, Bronze Age, and La Tène. Both paleobotanical arguments and archaeological discoveries support the theory that places the beggining of viticulture in Romania a few millenia ago, in Neolithic period. Also, written evidences (works of classical authors, epigraphical sources) confirm, indirectly, the presence of grapevine in La Tène period. Occurrences of Vitis vinifera and those of Vitis sylvestris manifest independently of the climate oscillations, being present both through colder and more humid episodes, as well as through drier and warmer events. Probably prehistoric communities have made a constant and deliberate effort, all along the Holocene, to maintain grapevine crops.
... If this is the case, the fermentation of grape juice must have been underway when the house was destroyed by fire. A small number of grape pips and skins were reported from Building 3 as well (Valamoti 2004), suggesting that wine making may have been practiced by several households at the site, the earliest evidence to date for wine making in the Aegean and the Eastern Mediterranean (Garnier and Valamoti 2016;Valamoti 2015;Valamoti et al. 2007). The grape pips have been identified as morphologically wild (Mangafa and Kotsakis 1996), yet their cultivation or early management cannot be excluded (Valamoti 2015;Valamoti et al. 2007Valamoti et al. , 2015. ...
... La découverte de charbons de bois est en effet un indice de l'utilisation de bois issu de la taille de ces fruitiers, et peut donc refléter leur entretien (Miller, 2008). Au Néolithique récent, les découvertes de grandes quantités de restes se multiplient, notamment à ArcheoSciences, revue d' archéométrie, 43(1), 2019, p. 27-52 Makri, en Thrace (Ntinou et Badal, 1998 ;Ntinou, 2002 ;Valamoti, 1998), et à Dikili Tash, en Macédoine, où plus de 2000 pépins ont été découverts associés à des restes de pressage (Valamoti et al., 2007, Valamoti, 2015Valamoti et al., 2015) et à des résidus de vin (Garnier et Valamoti, 2016). ...
... If archaeobotanical remains seem to point toward grape-growing in the Aegean since the fifth millennium bc (Renfrew, 1996), such an activity is likely linked to winemaking in light of the finds in House 1, ca. 4300 bc, of the Neolithic settlement of Dikili Tash, in Greek Eastern Macedonia. In association with ceramic containers there are thousands of grape pressings; moreover, residue analyses have yielded biomarkers of red wine in a big coarse jar, and in a small graphitepainted jug, the latter serving to pour liquids (Garnier & Valamoti, 2016). ...
Chapter
The taste for alcohol is not exclusive to humans, as some other animal species are attracted to ripe fruits and nectar due to the natural occurrence of ethanol. However, what makes Homo sapiens different is their capacity to produce alcoholic beverages. From the Neolithic, if not earlier, the production of alcoholic drinks is documented, and this production ensured the supply of alcohol. Consequently, alcohol consumption was no longer sporadic and occasional. This process ran in parallel to the development of specific alcohol-related equipment, and organized drinking patterns gradually became more and more formalized. Its use has depended not only on its effects, mainly its capacity to enhance sociability, but also on historical, economic, and religious factors. The aim of this chapter is to search for the origins of this dynamic in prehistoric Europe from an archaeological perspective in order to explore the foundations of the cultural construction of alcohol.
... The results of identification correspond to wine acids and fatty acids ( Table 3). The presence of wine markers such as tartaric and syringic acids (Stern et al., 2008;Garnier and Valamoti, 2016) was confirmed by the chromatogram in organic remains and in shards (Fig. 5, Table 3). In the other acids associated with wine, the amount of vanillic acid was high and subsequent acids were benzoic, succinic, glutaric and fumaric. ...
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This research work is focused on the chemical characterization of the substance present in the internal surfaces of Roman amphorae that made them waterproof and on the identification of their content. The samples come from the wreck of the Grand Congloué 2 that was studied in the Bay of Marseille by Commander Cousteau in 1952. The twenty studied amphorae are of type Dressel 1A and were provided by Cosa in Etruria (Tuscany, Italy). The FT-IR analysis indicated different bands concerning organic matter, as the chemical link O–H from carboxylic acid, C–H of the methylene group and C–O of the methyl ester. The study carried out by GC–MS showed nineteen diterpenoids, such as dehydroabietic acid and retene, which are chemical markers of Pinaceae family. Methyl ester by-products were also characterized and they revealed a pitch pyrogenically prepared from resinous wood (Pinus sp.). Principal Component Analysis allowed to group all of the twenty studied amphorae in two lots indicating two types of pitch. Concerning the content of these amphorae, the results from pitch as well as shards allowed to detect the presence of tartaric and syringic acids which are the main markers of the red wine. The comparison study between pitch and shard samples of same amphorae indicates that pitch analyses has permitted to obtain a high qualitative and quantitative proportion of wine markers.
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The purpose of this work is to present the archaeological and historical background of viticulture and winemaking from ancient times to the present day in the Mediterranean basin. According to recent archaeological, archaeochemical and archaeobotanical data, winemaking emerged during the Neolithic period (c. 7th–6th millennium BC) in the South Caucasus, situated between the basins of the Black and Caspian Seas, and subsequently reached the Iberian Peninsula and Western Europe during the local beginning of Iron Age (c. 8th century BC), following the main maritime civilizations. This review summarises the most relevant findings evidencing that the expansion of wine production, besides depending on adequate pedo-climatic conditions and wine-growing practices, also required the availability of pottery vessels to properly ferment, store and transport wine without deterioration. The domestication of wild grapevines enabled the selection of more productive varieties, further sustaining the development of wine trade. Other fermented beverages such as mead and beer gradually lost their relevance and soon wine became the most valorised. Together with grapes, it became an object and a system of value for religious rituals and social celebrations throughout successive ancient Western civilizations. Moreover, wine was used for medicinal purposes and linked to a wide variety of health benefits. In everyday life, wine was a pleasant drink consumed by the elite classes and commoner populations during jubilee years, festivals, and banquets, fulfilling the social function of easy communication. In the present work, emphasis is put on the technical interpretation of the selected archaeological and historical sources that may explain present viticultural and oenological practices. Hopefully, this review will contribute to nurturing mutual understanding between archaeologists and wine professionals.
Chapter
This chapter will provide an overview on the state of the art of the current practice and methodology of the analysis of the organic residues (ORA) in archaeology. By considering different materials and methods, we will focus in particular on those residues absorbed of and trapped in archaeological ceramic material and on the use of the technique of gas-chromatography coupled with mass spectrometry (GC-MS). We will integrate this overview with an evaluation of other techniques meaningfully integrating GC-MS analysis, like LC-MS and GC-IRMS, using also the isotopic signature of the detected substances. First, a critical bibliographic survey will aim at discussing potential and limits of the applied methods and results. Second, this chapter will focus in particular on the application of ORA to the study of the long-distance trade in foodstuff and of in-site consumption patterns in the historical periods, with a main emphasis on the contents of long distance transport containers (amphorae) and coarse/cooking wares of the Roman and Late Antique periods in the Mediterranean region. By doing so, this chapter addresses the question, whether and how the context-informed scientific analysis can contribute to fill gaps of the archaeological research and to reassess historical models by breaking down established certainties on containers function and contents.
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The POMEDOR project gave the opportunity to investigate the provenance and contents of some of the main types of Middle and Late Byzantine amphorae, for which we had very little information so far. This paper presents the first results obtained by residues analyses on amphorae of types Günsenin III and IV, which were widespread in the Mediterranean and the Black sea in the 12th-13th century AD, and are probably among the latest Mediterranean transport amphorae. We also studied another type of amphora, known only in the Levantine area in the Crusader period. The samples were analysed with gas chromatography-mass spectrometry. Different extraction methods were carried out in order to identify the residues preserved. The results of the analyses show wine was likely contained in almost all the amphorae. However, residues of plant oils were also present together with animal origin products and Pinaceae products probably used to coat the amphorae. In general, the results of the analyses seem to indicate that the analysed amphorae were often reused.
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The history of civilization is, in many ways, the history of wine. This book is the first comprehensive and up-to-date account of the earliest stages of vinicultural history and prehistory, which extends back into the Neolithic period and beyond. Elegantly written and richly illustrated, Ancient Wine opens up whole new chapters in the fascinating story of wine and the vine by drawing upon recent archaeological discoveries, molecular and DNA sleuthing, and the texts and art of long-forgotten peoples. Patrick McGovern takes us on a personal odyssey back to the beginnings of this consequential beverage when early hominids probably enjoyed a wild grape wine. We follow the course of human ingenuity in domesticating the Eurasian vine and learning how to make and preserve wine some 7,000 years ago. Early winemakers must have marveled at the seemingly miraculous process of fermentation. From success to success, viniculture stretched out its tentacles and entwined itself with one culture after another (whether Egyptian, Iranian, Israelite, or Greek) and laid the foundation for civilization itself. As medicine, social lubricant, mind-altering substance, and highly valued commodity, wine became the focus of religious cults, pharmacopoeias, cuisines, economies, and society. As an evocative symbol of blood, it was used in temple ceremonies and occupies the heart of the Eucharist. Kings celebrated their victories with wine and made certain that they had plenty for the afterlife. (Among the colorful examples in the book is McGovern's famous chemical reconstruction of the funerary feast--and mixed beverage--of "King Midas.") Some peoples truly became "wine cultures." When we sip a glass of wine today, we recapitulate this dynamic history in which a single grape species was harnessed to yield an almost infinite range of tastes and bouquets. Ancient Wine is a book that wine lovers and archaeological sleuths alike will raise their glasses to.
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The Handbook of Enology Volume 2: The Chemistry of Wine Stabilization and Treatments uniquely combines chemical theory with the descriptions of day-to-day work in the latter stages of winemaking from clarification and stabilization treatments to ageing processes in vats and barrels. The expert authors discuss: Compounds in wine, such as organic acids, carbohydrates, and alcohol. Stabilization and treatments The chemical processes taking effect in bottled wine The information provided helps to achieve better results in winemaking, providing an authoritative and complete reference manual for both the winemaker and the student. © 2006 John Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester. All Rights Reserved.
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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.
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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.
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Biologically produced compounds preserved in ancient ceramics can provide invaluable information on the vessel contents. Analysis and interpretation of these so-called archaeological “residues” is therefore important for understanding and reconstructing aspects of social and cultural behaviors of ancient societies. Based on the reaction of unsaturated compounds with iodine, we developed and apply two new methods. The first is a simple and relatively rapid method for assessing the amounts of unsaturated compounds in archaeological ceramics using X-ray fluorescence (XRF). We show that this method is a reliable indicator for assessing the general preservation state of the organic material and therefore a potential pre-screening method for identifying ceramic samples suitable for organic residue analysis. The second complementary approach, based on the same iodine reaction, makes it possible to map the unsaturated molecules on ceramic surfaces at a scale that enables to correlate organic matter distribution and the underlying mineral grains using a scanning electron microscope (SEM) equipped with an energy dispersive spectrometer (EDS) detector. With this method we show that the extent of adsorption of lipids onto ceramic surfaces varies with the surface properties of the different minerals in the ancient ceramic, with calcium containing minerals showing the highest affinity for compounds with unsaturated bonds. The ceramic substrate therefore influences the types of organic compounds bound and hence preserved in the ceramic. Fundamental information obtained using this method is essential for better interpreting molecular assemblages extracted from archaeological ceramics.
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Discriminant analyses using size variables and ratios were performed on populations consisting of modern wild and cultivated grape seeds before and after charring, and under various charring conditions. Four formulae were constructed, based on the charred population. The excellent predictive power of the models permits the identification of charred archaeological grape seeds to either subspecies. The formulae proposed were applied to archaeological populations from Greek prehistoric sites. (C) 1996 Academic Press Limited
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Ancient Egyptians were buried with the most precious food and drink as sustenance for their afterlife. One of these was Shedeh, the most valued and appreciated beverage in ancient Egypt. The botanic origin of Shedeh remains unclear as no mention of its raw material has survived. Some scholars have proposed that Shedeh was a pomegranate wine, while others, a grape wine. Presented here is the first ever analytical evidence of Shedeh's origin through the analysis of a sample of a residue from an extraordinarily well preserved Shedeh amphora from King Tutankhamun's collection. The previously developed LC/MS/MS wine markers method for archaeological samples was used and our results reveal Shedeh had a red grape origin.