Museum collections are extremely valuable sources of material for ongoing research, although the conservation history of some objects is not always recorded, which can be problematic for chemical analyses. While most contamination is removed using the acid-base-acid treatment, this may not be the case for cross-linked contamination. The XAD resin protocol was implemented at the radiocarbon (14C) laboratory in the Muséum national d’Histoire naturelle, and the setup was tested using known age bone samples and a consolidated Palaeolithic bone. Known age samples were consolidated with shellac or Paraloid, aged for a month, treated with or without the XAD resin and 14C dated. Bone blank results showed that XAD resin was able to remove shellac, which was not the case for the ABA-only method. Results from VIRI I were more variable and VIRI F was possibly too young to show the effects of the consolidants. Two 14C dates on the Palaeolithic bone after XAD treatment are statistically the same, while a sample without XAD treatment was significantly older, suggesting that the contaminant was not fully removed by the ABA-only treatment. This study demonstrates the potential of the XAD treatment to clean heritage bone samples stored in museums prior to geochemical analyses.

During the last glacial period, rapidly changing environments posed substantial challenges to Neanderthal populations in Europe. Southern continental regions, such as Iberia, have been proposed as important climatic “buffer” zones during glacial phases. Contextualising the climatic and ecological conditions Neanderthals faced is relevant to interpreting their resilience. However, records of the environments and ecosystems they exploited across Iberia exhibit temporal and spatial gaps in coverage. Here we provide new evidence for palaeotemperatures, vegetation structure, and prey herbivore ecology during the late Pleistocene (MIS 5–3) in northern Spain, by applying multiple stable isotope tracers (δ18O, δ13C, δ15N, δ34S) to herbivore skeletal remains associated with Neanderthal occupations at Axlor Cave, Bizkaia. The results show little change over time and indicate stable climatic conditions and ecosystems across different occupations. Large within-layer isotopic variability in nitrogen and sulphur suggests the presence of a mosaic environment and a variety of isotopic ecotones that were exploited by Neanderthals and their prey. We implement a combination of carbonate and phosphate δ18O measurements to estimate palaeotemperatures using a cost-effective workflow. We show that the targeted use of phosphate δ18O measurements to anchor summer peak and winter trough areas enables high-precision seasonal palaeoclimatic reconstructions.

In the last decade, the identification of bone fragments by peptide mass fingerprinting or zooarchaeology by mass spectrometry is developing as a powerful tool in Quaternary palaeontology. The sequence of amino acids that make up the bone collagen molecule shows slight variations between taxa, which can be studied by mass spectrometry for taxonomic purposes. This requires reference databases that allow peptide identification. Although the cave bear (Ursus spelaeus Rosenmüller, 1794) is a common component in many European Pleistocene cave sites, no peptide fingerprint taxonomic study has paid special attention to this species up to now. For peptide markers in Ursidae, the most recent proposal is based on collagen obtained from a modern brown bear sample. In this work we attempt to cover this gap by studying bone collagen of cave and brown bear samples from different origins and different chronology, applying matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI TOF). We also performed an in-silico study of ursid bone collagen sequences published in databases. In our results we detected some discrepancies between the peptides obtained from both in silico and MALDI TOF analysis of fossil collagen and those published in the literature, in which we conclude that there are some misidentified peptides. The identification of skeletal remains by means of their peptide fingerprint is proving to be a powerful tool in palaeontology, which will bear greater fruit once the limitations of a technique that is in its initial stages have been overcome.

Human burials from the cemetery at the Rounala church, northern Sweden, were radiocarbon (14C) dated to shed light on the use of the cemetery. Carbon, nitrogen and sulfur stable isotope analysis of bone collagen from 19 distinct individuals indicated that these individuals had a mixed diet consisting of freshwater, marine and terrestrial resources. Dietary modeling using FRUITS was employed to calculate the contributions of the different resources for each individual. These data were then used to calculate individual ΔR values, taking into account freshwater and multiple marine reservoir effects, the latter caused by Baltic and Atlantic marine dietary inputs, respectively. 14C dating of tissues from modern freshwater fish species demonstrate a lack of a freshwater reservoir effect in the area. Two OxCal models were used to provide endpoint age estimates. The calibrated data suggest that the site’s cemetery was most likely in use already from the 14th century, and perhaps until at least the late 18th century.

Higher δ15N values in bone collagen of mammoth (Mammuthus primigenius) compared with coeval large herbivores is a classic trait of the mammoth steppe. An exception applies to the Epigravettian site of Mezhyrich (ca. 18–17.4 ka cal BP) in the central East European plains, where mammoth bones have δ15N values equivalent to or in a lower range than those of horse specimens (Equus sp.). We expanded our preliminary dataset to a larger sampling size of mammoth, other large herbivores, and carnivores from contemporaneous and nearby sites of Buzhanka 2, Eliseevichi, and Yudinovo. The unusual low mammoth δ15N values were confirmed at Buzhanka 2 and for some specimens from Eliseevichi, while most individuals from Yudinovo displayed the expected high δ15N values, meaning similar to those of the large canids. The possibility of a contrast in migration pattern is not supported since the δ34S values, a marker of mobility, do not correlate with the δ15N values of mammoth bone collagen. No clear chronological tendency could be revealed, at least not at the scale of radiocarbon dating. The low range in δ15N values is likely to reflect a change in the specific niche of the mammoth in the southern part of its distribution.

High elevation plant and animal communities are considered extremely sensitive to environmental change. We investigated an exceptional fossil record of yellow-bellied marmot (Marmota flaviventris) specimens that was recovered from Cement Creek Cave (elev. 2860 m) and ranged in age from radiocarbon background circa 49.8 cal ka BP to ~ 1 cal ka BP. We coupled isotopic and radiocarbon measurements (δ18O, δD, δ15N, δ13C, and 14C) of bone collagen from individually-AMS dated specimens of marmots to assess ecological responses by this species to environmental change over time in a high elevation basin in the Rocky Mountains of southwestern Colorado, USA. We find little change in all four isotope ratios over time, demonstrating considerable environmental stability during periods when the marmots were present. The stable ecology and the apparent persistence of the small mammal community in the cave fauna throughout the late Quaternary are in marked contrast to the changes that occurred in the large mammal community, including local extirpation and extinction, at the end of the Pleistocene.

Climatic and ecological conditions during Marine Oxygen Isotope Stage (MIS) 3 are complex and the impact of cold spells on the ecosystems in Central Europe still needs to be investigated thoroughly. Ziegeleigrube Coenen (ZC) is a late Pleistocene MIS 3 locality in the Lower Rhine Embayment of Germany, radiocarbon-dated to > 34 14C ka BP. The site yielded a broad spectrum of mammal species. We investigated the carbon (δ13C), nitrogen (δ15N) and sulfur (δ34S) isotope signatures of bone collagen, since these are valuable tools in characterizing ecological niches, environmental conditions and aspects of climate and mobility. By comparison with pre- and post-Last Glacial Maximum (LGM) sites in Central Europe we show that ZC belongs in a cold event of MIS 3 and was climatically more similar to post-LGM sites than to pre-LGM sites. However, the trophic structure resembled that of typical pre-LGM sites in Belgium. This cold event in MIS 3 changed the bottom of the foodweb, but do not seem to have had a direct impact on the occurrence of the mammalian species and their ecological distribution. Apparently the (mega-) faunal community could adapt also to harsher environmental conditions during MIS 3.

The diets of laboratory rats were isotopically and nutritionally manipulated using purifiedC3 and/or C4 macronutrients to investigate the routing of dietary carbonto bone collagen biosynthesis. Diets were formulated with purified proteins, carbohydrates andlipids of defined composition and natural abundance stable isotope ratios. Bulk protein and constituent amino acid δ13C values determined for whole diet and bone collagen provided the basis for assessing isotopic fractionation and estimating the degree of routing versus synthesis de novo of essential, non-essential and conditionally indispensable amino acids. Essential and conditionally indispensable amino acids were shown to be routed from diet to collagen with little isotopic fractionation whereas non-essential amino acids differed by up to 20‰. Mathematical modelling of the relationships between macronutrient and tissue δ13C values provided qualitative and quantitative insights into the metabolic and energetic controls on bone collagen biosynthesis. Essential amino acids comprise 21·7% of the carbon in collagen, defining the minimum amount of dietary carbon routing. Estimates of 42 and 28% routing were shown for the non-essential amino acids, glycine and aspartate, respectively. In total, the routing of non-essential and conditionally indispensable amino acids was estimated to equal 29·6% of the carbon in collagen. When the contribution of carbon from the essential amino acids is also considered, we arrive at an overall minimum estimate of 51·3% routing of dietary amino acid carbon into bone collagen.

Stable isotopes are commonly used in ecological studies to infer food resources (Ambrose & DeNiro 1986, Bocherens et al. 1990,1991,1994;Yoshinaga et al. 1991) since isotopic composition is conserved during the feeding process. Moreover,for herbivorous (sensu lato) species, it is often possible to identify the main resource because different photosynthetic pathways generate different values of carbon isotope ratios (Park & Epstein 1961, Sternberg et al. 1984). This allows the characterization of broad biota such as savannas or forest and discrimination of grazers from sympatric folivorous species (DeNiro & Epstein 1978).