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The pressures on honeybee (Apis mellifera) populations, resulting from threats by modern pesticides, parasites, predators and diseases, have raised awareness of the economic importance and critical role this insect plays in agricultural... more
The pressures on honeybee (Apis mellifera) populations, resulting from threats by modern pesticides, parasites, predators and diseases, have raised awareness of the economic importance and critical role this insect plays in agricultural societies across the globe. However, the association of humans with A. mellifera predates post-industrial-revolution agriculture, as evidenced by the widespread presence of ancient Egyptian bee iconography dating to the Old Kingdom (approximately 2400 BC). There are also indications of Stone Age people harvesting bee products; for example, honey hunting is
interpreted from rock art in a prehistoric Holocene context and
a beeswax find in a pre-agriculturalist site. However, when and
where the regular association of A. mellifera with agriculturalists emerged is unknown. One of the major products of A. mellifera is beeswax, which is composed of a complex suite of lipids including n-alkanes, n-alkanoic acids and fatty acyl wax esters. The composition is highly constant as it is determined genetically through the insect’s biochemistry. Thus, the chemical ‘fingerprint’ of beeswax provides a reliable basis for detecting this commodity in organic residues preserved at archaeological sites, which we now use to trace the exploitation by humans of A. mellifera temporally and spatially. Here we present secure identifications of beeswax in lipid residues preserved in pottery vessels of Neolithic Old World farmers. The geographical range of bee product exploitation is traced in Neolithic Europe, the Near East and North Africa, providing the palaeoecological range of honeybees during prehistory. Temporally, we demonstrate that bee products were
exploited continuously, and probably extensively in some regions, at least from the seventh millennium cal BC, likely fulfilling a variety of technological and cultural functions. The close association of A. mellifera with Neolithic farming communities dates to the early onset of agriculture and may provide evidence for the beginnings of a domestication process.

Authors: Roffet-Salque, M., Regert, M., Evershed, R. P., Outram, A. K., Cramp, L. J. E., Decavallas, O., Dunne, J., Gerbault, P., Mileto, S., Mirabaud, S., Pääkkönen, M., Smyth, J., Šoberl, L., Whelton, H. L., Alday-Ruiz, A., Asplund, H., Bartkowiak, M., Bayer-Niemeier, E., Belhouchet, L., Bernardini, F., Budja, M., Cooney, G., Cubas, M., Danaher, E. M., Diniz, M., Domboróczki, L., Fabbri, C., González-Urquijo, J. E., Guilaine, J., Hachi, S., Hartwell, B. N., Hofmann, D., Hohle, I., Ibáñez, J. J., Karul, N., Kherbouche, F., Kiely, J., Kotsakis, K., Lueth, F., Mallory, J. P., Manen, C., Marciniak, A., Maurice-Chabard, B., Mc Gonigle, M. A., Mulazzani, S., Özdoğan, M., Perić, O. S., Perić, S. R., Petrasch, J., Pétrequin, A.-M., Pétrequin, P., Poensgen, U., Pollard, C. J., Poplin, F., Radi, G., Stadler, P., Stäuble, H., Tasić, N., Urem-Kotsou, D., Vuković, J. B., Walsh, F., Whittle, A., Wolfram, S., Zapata-Peña, L. and Zoughlami, J.
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A new multistep analytical methodology is described in this paper for the precise identification of triacylglycerols, which are biomarkers of dairy products and subcutaneous fats, that may be chemically identified in archaeological... more
A new multistep analytical methodology is described in this paper for the precise identification of triacylglycerols, which are biomarkers of dairy products and subcutaneous fats, that may be chemically identified in archaeological pottery. It consists of the analysis of the total lipid extract from different kinds of fats by high-temperature gas chromatography, performed in order to select the ceramic vessels in which animal fats are well preserved, followed by nanoelectrospray QqTOF mass spectrometry that allows for distinguishing the specific origins of the lipids detected (namely, cow, sheep, or goat). The analysis of model samples, cow and goat dairy products and cow and sheep adipose fats, was successfully achieved. The fatty acid composition of each triacylglycerol was identified, which allowed for the discrimination of subcutaneous fats and dairy fats and distinguishing between cow and goat milk. This methodology was then applied to archaeological samples, and the presence of goat milk, cow milk, and possibly sheep subcutaneous fat was assessed based on the discriminating criteria found on modern fats.
The pressures on honeybee (Apis mellifera) populations, resulting from threats by modern pesticides, parasites, predators and diseases, have raised awareness of the economic importance and critical role this insect plays in agricultural... more
The pressures on honeybee (Apis mellifera) populations, resulting from threats by modern pesticides, parasites, predators and diseases, have raised awareness of the economic importance and critical role this insect plays in agricultural societies across the globe. However, the association of humans with A. mellifera predates post-industrial-revolution agriculture, as evidenced by the widespread presence of ancient Egyptian bee iconography dating to the Old Kingdom (approximately 2400 BC). There are also indications of Stone Age people harvesting bee products; for example, honey hunting is interpreted from rock art in a prehistoric Holocene context and a beeswax find in a pre-agriculturalist site. However, when and where the regular association of A. mellifera with agriculturalists emerged is unknown. One of the major products of A. mellifera is beeswax, which is composed of a complex suite of lipids including n-alkanes, n-alkanoic acids and fatty acyl wax esters. The composition is highly constant as it is determined genetically through the insect's biochemistry. Thus, the chemical 'fingerprint' of beeswax provides a reliable basis for detecting this commodity in organic residues preserved at archaeological sites, which we now use to trace the exploitation by humans of A. mellifera temporally and spatially. Here we present secure identifications of beeswax in lipid residues preserved in pottery vessels of Neolithic Old World farmers. The geographical range of bee product exploitation is traced in Neolithic Europe, the Near East and North Africa, providing the palaeoecological range of honeybees during prehistory. Temporally, we demonstrate that bee products were exploited continuously, and probably extensively in some regions, at least from the seventh millennium cal BC, likely fulfilling a variety of technological and cultural functions. The close association of A. mellifera with Neolithic farming communities dates to the early onset of agriculture and may provide evidence for the beginnings of a domestication process.
An art historian, a paintings conservator, and a chemist jointly conducted this study of a group of 15th- to 18th-century Ethiopian icons from the museum of the Institute of Ethiopian Studies in Addis-Ababa. The study pertains to the... more
An art historian, a paintings conservator, and a chemist jointly conducted this study of a group of 15th- to 18th-century Ethiopian icons from the museum of the Institute of Ethiopian Studies in Addis-Ababa. The study pertains to the sampling and analysis of the constitutive material, pigments, binder, and varnish, a sanitary and esthetic assessment of the works, as well as a historical study. The results presented mainly concern the characterization of the pigments and varnishes and how they were used for the four icons dated and attributed to two painters, Feré Seyon and Brancaleon (15th century to the early 16th century). The results showed that similar techniques were used, specifically an identical selection of pigments and the presence of oil varnish, while each also had its unique characteristics.
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A new multistep analytical methodology is described in this paper for the precise identification of triacylglycerols, which are biomarkers of dairy products and subcutaneous fats, that may be chemically identified in archaeological... more
A new multistep analytical methodology is described in this paper for the precise identification of triacylglycerols, which are biomarkers of dairy products and subcutaneous fats, that may be chemically identified in archaeological pottery. It consists of the analysis of the total lipid extract from different kinds of fats by high-temperature gas chromatography, performed in order to select the ceramic vessels in which animal fats are well preserved, followed by nanoelectrospray QqTOF mass spectrometry that allows for distinguishing the specific origins of the lipids detected (namely, cow, sheep, or goat). The analysis of model samples, cow and goat dairy products and cow and sheep adipose fats, was successfully achieved. The fatty acid composition of each triacylglycerol was identified, which allowed for the discrimination of subcutaneous fats and dairy fats and distinguishing between cow and goat milk. This methodology was then applied to archaeological samples, and the presence of goat milk, cow milk, and possibly sheep subcutaneous fat was assessed based on the discriminating criteria found on modern fats.
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Traditionally, pottery use has been discussed through morphotypological characteristics and mechanic properties of the vessels (Rice 1987) but amorphous organic residues analysis has also greatly contributed to understand exploitation of... more
Traditionally, pottery use has been discussed through morphotypological characteristics and mechanic properties of the vessels (Rice 1987) but amorphous organic residues analysis has also greatly contributed to understand exploitation of natural resources during the Holocene (Evershed 2008). Nevertheless these methodologies are rarely combined due to the high fragmentation of pottery and to the impossibility to link ceramic content with specific shape. At the site of Clairvaux XIV (Middle Neolithic, NMB - 39e-37e century BC), the large and diversified corpus of ceramic vessels (377 vessels with restituted profiles) combined to anoxic condition favoring lipids preservation offers a unique opportunity to investigate the use of pottery to better understand lake dwelling Neolithic society (Pétrequin et Pétrequin 2015).

The corpus was first classified based on morphological and morphometric criteria. Chemical analysis of the lipids preserved into pottery walls or into carbonized surface residues were then carried out using an analytical strategy combining chromatographic (HT GC), spectrometric (HT GC-MS, NanoESI MS and MS/MS – Mirabaud et al. 2007) and isotopic (GC-C-IRMS) techniques.

The data obtained on 95 pottery conducted to: (i) the identification of a broad diversity of commodities processed in the vessels, mainly from animal origin; (ii) the establishment of clear relationships between content, traces of cooking, shape and volumes of the vessels.

This study highlights some characteristic consumption pattern of the Neolithic people living at Clairvaux XIV in the first half of 4th millennium BC. First, a clear difference is observed between cooking pots and serving vessels. Dairy substances were significantly used in all category of ceramics but small individual vessels seem to be especially dedicated to the consumption or transformation of these high value products. The surprising low representation of fish and vegetable products may be due to the low fat-content of cereals and to the fact that lake resources were prepared and consumed without using ceramics (grilled, dried etc.). Non-food products as beeswax and birch bark tar were also detected in some pottery.

From the results of our work, we suggest that (i) depending on the commodity, it existed a large variety of transformation and consumption usages on this site, and (ii) dairy products possessed a particular status. These complex culinary customs carried out at Clairvaux XIV and highlighted by our integrative approach will be compared with data from other archaeological sites in order to build an overview of food practices in lacustrine Middle Neolithic societies.

Evershed, R. P. (2008). "Organic residue analysis in archaeology: the archaeological biomarker revolution." Archaeometry 50: 895-924.

Mirabaud, S., et al. (2007). "Molecular criteria for discriminating adipose fat and milk from different species by NanoESl MS and MS/MS of their triacylglycerols: Application to archaeological remains." Analytical Chemistry 79(16): 6182-6192.

Pétrequin P. & Pétrequin A.M. (ed.), 2015.- Clairvaux et le « Néolithique Moyen Bourguignon ». Cahiers de la MSHE C.N. Ledoux, Besançon, Presses Universitaires de Franche-Comté et Centre de Recherche Archéologique de la Vallée de l’Ain, 2 vol., 1430 p.

Rice, P. M. (1987). Vessel function: Form, Technology, and use. Pottery Function, a source book: 207-243