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© 2019 Elsevier Ltd Bird eggs can become part of the archaeological record either accidentally or as a result of human activities but, in both instances, they can reveal important aspects of the environment at the site, the ways in which people chose to exploit it, and even the existence of subtle ecological balances between humans and other animals. This is the case for El Mirόn, one of the most important cave sites in Cantabrian Spain, with occupation levels spanning around 40,000 years, from the late Middle Palaeolithic to the Bronze Age. This mountainous area in Cantabria was an ideal environment for hunting medium-sized game and, as such, supported both human and non-human predators, including birds of prey. Here we use a combination of peptide mass fingerprinting (by MALDI-MS) and protein sequencing (by LC-MS/MS) in order to taxonomically identify ninety-five fragments of eggshells recovered from nineteen archaeological layers. We firmly identify these as diurnal birds of prey (Accipitridae) and suggest that the species might have been bearded vulture, based on previous taphonomic studies that highlighted its presence at the cave. The implication is that both species of diurnal predators, humans and birds, inhabited the cave and used the surrounding environment during different periods of the year.

Marine faunal remains from Grotta d’Oriente (Favignana Island, NW Sicily) offer invaluable snapshots of human-coastal environment interaction in the central Mediterranean from the Late Pleistocene to the Middle Holocene. The long-term shellfish and fish records reflect human exploitation of coastal environments undergoing considerable reorganizations during the postglacial sea level rise and the progressive isolation of Favignana from mainland Sicily. We detected an intensification of marine resource exploitation between ∼9.6 ka and ∼7.8 ka BP, which corresponds with the isolation of Favignana Island and, later on, with the introduction of early agro-pastoral economy in this region. We suggest that a higher investment in marine resource exploitation by late foragers and early farmers in NW Sicily was also supported by an increase in marine productivity in the south Tyrrhenian Sea in the Middle Holocene.

The level of glutamine (Gln) deamidation in bone collagen provides information on the diagenetic history of bone but, in order to accurately assess the extent of Gln deamidation, it is important to minimise the conditions that may induce deamidation during the sample preparation. Here we report the results of a preliminary investigation of the variability in glutamine deamidation levels in an archaeological bone due to: a) sampling location within a bone; b) localised diagenesis; and c) sample preparation methods. We then investigate the effects of pre-treatment on three bone samples: one modern, one Medieval and one Pleistocene. The treatment of bone with acidic solutions was found to both induce deamidation and break down the collagen fibril structure. This is particularly evident in the Pleistocene material (∼80,000 years BP) considered in this study. We show that ethylenediaminetetraacetic acid (EDTA), when used as an alternative to hydrochloric acid (HCl) demineralisation, induces minimal levels of deamidation and maintains the collagen fibril structure. Areas of bone exhibiting localised degradation are shown to be correlated with an increase in the levels of Gln deamidation. This indicates that the extent of Gln deamidation could provide a marker for diagenesis but that sampling is important, and that, whenever possible, subsamples should be taken from areas of the bone that are visually representative of the bone as a whole. Although validation of our observations will require analysis of a larger sample set, deamidation measurements could be a valuable screening tool to evaluate the suitability of bone for further destructive collagen analyses such as isotopic or DNA analysis, as well as assessing the overall preservation of bone material at a site. The measure of bone preservation may be useful to help conservators identify bones that may require special long-term storage conditions.

Intra-crystalline protein diagenesis (IcPD), a recent development of amino acid racemization dating (AAR), is now established as a reliable geochronological tool for the Quaternary. However, extending the method to new biominerals requires extensive testing in order to provide evidence for the closed-system behaviour of the intra-crystalline proteins and to assess the temporal span that can be covered.Here we present results from high-temperature experiments on the IcPD of the bivalve Pecten, demonstrating that a fraction of proteins can be isolated from a bleach-resistant mineral matrix, which effectively operates as a closed system under conditions of accelerated diagenesis in the laboratory. Analyses of Pecten from the well-dated terrace system of the Gulf of Corinth (Greece) provided a pilot test for the integrity of the intra-crystalline fraction in subfossil shells. The small sample sizes in this preliminary study preclude a full assessment of the aminostratigraphic power of Pecten IcPD, but a concordance is observed between the extent of IcPD and sites dating from between MIS 5 and MIS 11.We conclude that Pecten is a potentially good substrate for IcPD dating in the Mediterranean, and that the temporal limit of the technique in this area lies beyond MIS 11. © 2015 Published by Elsevier B.V.

In the North Sea basin the marine bivalve Macoma balthica first appears within the Early Pleistocene ‘Weybourne Crag’, which forms an important biostratigraphical datum. Here we review the fossil assemblages from sites of this age, prompted by new discoveries from Sidestrand, Norfolk, UK. The molluscan assemblages from this horizon are dominated by intertidal species with some colder/deeper water taxa and a few temperate non-marine species. A high boreal/low arctic marine environment with reduced salinities is indicated. An extensive assemblage of small mammals dominated by voles includes two species (Mimomys hordijki and Ungaromys dehmi) previously unknown from the British Pleistocene. The assemblage can be assigned to Tesakov’s Mammal Biozone MNR1 (=MN17, Middle Villafranchian), which according to current estimates corresponds to a date of ∼2.2-2.1 Ma (MIS 84-79). It matches another assemblage from -61 m to -65 m in the Zuurland-2 borehole in The Netherlands, and is similar to that from the Dutch Tiglian type site at Tegelen, although this has more temperate elements. A late Tiglian age is consistent with the co-occurrence of the marine bivalves Macoma balthica, Mya arenaria and the freshwater gastropod Viviparus glacialis in the Zuurland-2 borehole and in a North Sea borehole (BGS 52-02-472). A Macoma balthica – Mya arenaria Concurrent Range Zone is defined for this assemblage, which can be traced across the North Sea basin. Amino acid dating provides strong independent support for these correlations and indicates that the Baventian cold stage post-dates the Bramertonian (Norwich Crag). It also confirms that Early Pleistocene molluscan assemblages with M. balthica are younger than those without it. The correlation of this marine marker horizon with Mammal Biozone MNR1 provides a secure link between continental and marine sequences during the Early Pleistocene. It also provides a basis for dating events in the pre-glacial fluvial drainage history and linking it to the East European mammal zonation.

This study successfully isolates a fraction of intra-crystalline proteins from shells of the marine gastropod Patella vulgata and assesses the suitability of these proteins for IcPD (Intra-crystalline Protein Diagenesis) geochronology. We discuss the mineralogical composition of this gastropod, investigated for the first time by X-ray diffraction mapping, and use the results to inform our sampling strategy. The potential of the calcitic rim and of a bulk sample (containing both apex and rim) of the shell to act as stable repositories for the intra-crystalline proteins during diagenesis is examined. The composition and the diagenetic behaviour of the intra-crystalline proteins isolated from different locations within the shell are compared, highlighting the necessity of targeting consistent sampling positions.We induced artificial diagenesis of both intra-crystalline and whole-shell proteins by conducting high-temperature experiments in hydrous environment; this allowed us to quantify the loss of amino acids by leaching and therefore evaluate the open- or closed-system behaviour of the different fractions of proteins. The results obtained provide further confirmation that patterns of diagenesis vary according to the protein sequence, structure, and location within or outside the intra-crystalline fraction. As Patella is frequently found in the fossil record, both in archaeological and geological contexts, the application of IcPD geochronology to this biomineral opens up the possibility to obtain reliable age information from a range of sites in different areas of the world.

The Easington Raised Beach, in Shippersea Bay, County Durham, is the most northerly known interglacial beach deposit in England. It lies directly on Magnesian Limestone bedrock at 33 m O.D. and is covered by glacial sediments attributed to the Devensian. Detailed sedimentological analysis suggests that it is an interglacial beach, which is supported by the presence of pebbles bored by marine organisms and littoral, temperate-climate, marine macro- and micro-fossils. It comprises beds of unconsolidated, bedded, imbricated, well-rounded sands and gravels, overlain by similar, but calcreted, deposits. The gravel fraction is dominated by Magnesian and Carboniferous limestone, with orthoquartzite, flint, and porphyries also present; these are far-travelled erratics that must have derived from the erosion of older glacially transported sediments. Previous workers have described erratics derived from the Oslofjord region of Norway in the raised beach gravel, although rocks diagnostic of a Scandinavian origin have not been recovered as part of this study. The heavy-mineral suite is rich in epidote, dolomite, clinopyroxenes, garnet, tourmaline, and micas. The beach was dated previously by conventional amino acid analysis of the shells, which suggested a Marine Isotope Stage (MIS) 7 age, albeit with a reworked component from MIS 9. This has been confirmed by new optically stimulated luminescence (OSL) dates, which indicate that the beach formed between 240 and 200 ka BP. New amino acid racemisation analyses, using a modified technique, broadly support this interpretation but must await more comparative data before they can be assessed fully. The strong indication of an MIS 7 age for the formation of the beach has implications for the uplift history of northeastern England during the Pleistocene, and indicates an uplift rate of 0.19 mm a −1 . The stable isotope geochemistry indicates that the cementation occurred during an interglacial period, whilst U-Series dating of the cement indicates that cementation occurred mostly during the Holocene, and is genetically related to the overlying Devensian till. This work has formed part of a full re-appraisal of the glacial sequence in eastern County Durham, the results of which suggest that the Warren House Formation pre-dates the raised beach, and that the Devensian Horden Till overlies the raised beach.