Explore the vast range of titles available.

Dating the quaternary The British Quaternary, spanning roughly the past 2.6 million years, is unmatched for the biodiversity and abundance of its fossil localities and its record of climatic contrasts. However, with all but the most recent deposits beyond radiocarbon range, and with no readily datable volcanic rocks, it has been difficult to get accurate dates for many British Pleistocene deposits. Penkman et al . have developed new analytical methods based on the intra-crystalline proteins of stable biominerals (in the 'opercula' shell closure of the freshwater gastropod Bithynia ), common in Quaternary deposits. They obtain confident assignments for various strata to global marine isotope stages, securely placing Britain's rich record of faunal and archaeological change into a broader context. Marine and ice-core records show that the Earth has experienced a succession of glacials and interglacials during the Quaternary (last ∼2.6 million years), although it is often difficult to correlate fragmentary terrestrial records with specific cycles. Aminostratigraphy is a method potentially able to link terrestrial sequences to the marine isotope stages (MIS) of the deep-sea record 1 , 2 . We have used new methods of extraction and analysis of amino acids, preserved within the calcitic opercula of the freshwater gastropod Bithynia , to provide the most comprehensive data set for the British Pleistocene based on a single dating technique. A total of 470 opercula from 74 sites spanning the entire Quaternary are ranked in order of relative age based on the extent of protein degradation, using aspartic acid/asparagine (Asx), glutamic acid/glutamine (Glx), serine (Ser), alanine (Ala) and valine (Val). This new aminostratigraphy is consistent with the stratigraphical relationships of stratotypes, sites with independent geochronology, biostratigraphy and terrace stratigraphy 3 , 4 , 5 , 6 . The method corroborates the existence of four interglacial stages between the Anglian (MIS 12) and the Holocene in the terrestrial succession. It establishes human occupation of Britain in most interglacial stages after MIS 15, but supports the notion of human absence during the Last Interglacial (MIS 5e) 7 . Suspicions that the treeless ‘optimum of the Upton Warren interstadial’ at Isleworth pre-dates MIS 3 are confirmed. This new aminostratigraphy provides a robust framework against which climatic, biostratigraphical and archaeological models can be tested.

We investigate the origin of archaeological wool textiles preserved by anoxic waterlogging from seven medieval archaeological deposits in north-western Europe (c. 700-1600 AD), using geospatial patterning in carbon (δ13C), nitrogen (δ15N) and non-exchangeable hydrogen (δ2H) composition of modern and ancient sheep proteins. δ13C, δ15N and δ2H values from archaeological wool keratin (n = 83) and bone collagen (n = 59) from four sites were interpreted with reference to the composition of modern sheep wool from the same regions. The isotopic composition of wool and bone collagen samples clustered strongly by settlement; inter-regional relationships were largely parallel in modern and ancient samples, though landscape change was also significant. Degradation in archaeological wool samples, examined by elemental and amino acid composition, was greater in samples from Iceland (Reykholt) than in samples from north-east England (York, Newcastle) or northern Germany (Hessens). A nominal assignment approach was used to classify textiles into local/non-local at each site, based on maximal estimates of isotopic variability in modern sheep wool. Light element stable isotope analysis provided new insights into the origins of wool textiles, and demonstrates that isotopic provenancing of keratin preserved in anoxic waterlogged contexts is feasible. We also demonstrate the utility of δ2H analysis to understand the location of origin of archaeological protein samples.

The straight-tusked elephants Palaeoloxodon spp. were widespread across Eurasia during the Pleistocene. Phylogenetic reconstructions using morphological traits have grouped them with Asian elephants (Elephas maximus), and many paleontologists place Palaeoloxodon within Elephas. Here, we report the recovery of full mitochondrial genomes from four and partial nuclear genomes from two P. antiquus fossils. These fossils were collected at two sites in Germany, Neumark-Nord and Weimar-Ehringsdorf, and likely date to interglacial periods ~120 and ~244 thousand years ago, respectively. Unexpectedly, nuclear and mitochondrial DNA analyses suggest that P. antiquus was a close relative of extant African forest elephants (Loxodonta cyclotis). Species previously referred to Palaeoloxodon are thus most parsimoniously explained as having diverged from the lineage of Loxodonta, indicating that Loxodonta has not been constrained to Africa. Our results demonstrate that the current picture of elephant evolution is in need of substantial revision. Understanding how extinct species are related to each other or to their living relatives is often a difficult task. Many extinct species have been identified only from incomplete fragments of some of their bones. However, even if complete skeletons have been found, determining the relationships between species can be tricky because researchers often have to rely solely on the shapes of the bones. It is sometimes possible to retrieve DNA sequences from fossil bones. This is easier with younger fossils and those that have been recovered from cold environments. Ancient DNA sequences have been retrieved from only a few fossils older than 100,000 years, but such DNA sequences can be tremendously useful in determining how different species are related to each other. Today there are three living elephant species: the African forest elephant, the African savanna elephant and the Asian elephant. However, there are many extinct elephant species. For example, the European straight-tusked elephant went extinct at least 30,000 years ago, although most of the fossils that have been discovered are at least 100,000 years old. Straight-tusked elephants are generally assumed to be closely related to the Asian elephant, but this conclusion had been based solely on reconstructing skeletons. Meyer et al. have now obtained DNA sequences from fossils of four straight-tusked elephants ranging from around 120,000 to 240,000 years in age. These sequences were analysed to determine how straight-tusked elephants are related to the three living elephant species and the extinct mammoth, the DNA sequences for which can be found in public databases. The analyses revealed that straight-tusked elephants are in fact most closely related to the African forest elephant, not the Asian elephant as previously thought. This result completely changes our picture of elephant evolution and suggests that it is extremely difficult to determine elephant relationships based on the shape of their skeleton alone. It also shows that the African elephant lineage was not restricted to the African continent (the place where all elephant lineages originated), but that it also left Africa. Overall, the results presented by Meyer et al. confirm that DNA sequences are of critical importance for understanding the evolution of animals. Future research should include obtaining DNA sequences from additional extinct elephant species as well as careful re-evaluation of skeletal measurements for reconstructing elephant evolution.

Waterlogged archaeological wood can present management challenges due to its vulnerability to chemical and biological decay, both during burial and post-excavation. Decay processes also often leave it severely weakened and therefore susceptible to mechanical damage. Quantifying preservation and understanding active decay mechanisms is therefore critical in informing the management of this unique cultural resource. It is critical that assessments of preservation are robust, and sensitive enough to allow changes over time to be detected. A wide range of analytical methods can be applied to assess the state of preservation of waterlogged archaeological wood, and determining which of these is most appropriate to the circumstances can be challenging. This review summarises some of the most commonly reported methods suitable for the analysis of waterlogged archaeological wood, ranging from widely used ‘low-tech’ methods, to assessment using advanced analytical instrumentation. Methods are evaluated in terms of the information gained weighed up against their cost, logistical considerations, and time investments, with the aim of supporting the development of an analytical strategy. We conclude that although an analytical strategy must be informed by the aims of assessment as well as any external restrictions, the best available analytical techniques should be employed in order to supply an accurate baseline against which future change can be measured. Critically, a multi-analytical approach is vital in obtaining a clear picture of the present state of decay, as no single technique gives the best assessment.

Written in stone A collection of stone tools from East Anglia has been dated at around 700,000 years old, making them the the earliest signs of human activity in northern Europe by about 200,000 years. Humans were present in sunnier southern Europe before 750,000 years ago, but until now there were no traces of human activity north of the Alps before half a million years ago. The flint artefacts found at Pakefield, near Lowestoft, extend human activity in Britain and the entire northern European landmass back to an antiquity we're more used to from southern Europe. The tools are from the well known Cromer Forest-bed Formation, which has yielded Ice Age fossils for over a century. But this find was notable as the 32 worked flints, including the scraper shown on the cover, were in a clearly datable stratigraphic context. Go to tinyurl.com/d2zko for video clips of the press conference announcing this discovery. The colonization of Eurasia by early humans is a key event after their spread out of Africa, but the nature, timing and ecological context of the earliest human occupation of northwest Europe is uncertain and has been the subject of intense debate 1 . The southern Caucasus was occupied about 1.8 million years (Myr) ago 2 , whereas human remains from Atapuerca-TD6, Spain (more than 780 kyr ago) 3 and Ceprano, Italy (about 800 kyr ago) 4 show that early Homo had dispersed to the Mediterranean hinterland before the Brunhes–Matuyama magnetic polarity reversal (780 kyr ago). Until now, the earliest uncontested artefacts from northern Europe were much younger, suggesting that humans were unable to colonize northern latitudes until about 500 kyr ago 5 , 6 . Here we report flint artefacts from the Cromer Forest-bed Formation at Pakefield (52° N), Suffolk, UK, from an interglacial sequence yielding a diverse range of plant and animal fossils. Event and lithostratigraphy, palaeomagnetism, amino acid geochronology and biostratigraphy indicate that the artefacts date to the early part of the Brunhes Chron (about 700 kyr ago) and thus represent the earliest unequivocal evidence for human presence north of the Alps.

The thermal behaviour of the animal by-product meat and bone meal (MBM) has been investigated in order to assess how it is affected structurally and chemically by incineration. Initially composed of intergrown collagen and hydroxyapatite (HAP), combustion of the organic component is complete by 650 °C, with most mass loss (50–55%) occurring by 500 °C. No original proteins were detected in samples heated at 400 °C or above. Combustion of collagen is accompanied by an increase in HAP mean crystallite size at temperatures greater than 400 °C, from 10 nm to a constant value of 120 nm at 800 °C or more. Newly formed crystalline phases appear beyond 400 °C, and include β-tricalcium phosphate, NaCaPO4, halite (NaCl) and sylvite (KCl). Crystallite thickness as judged by small angle X-ray scattering (SAXS) increases from 2 nm (25–400 °C) to 8–9 nm very rapidly at 550 °C, and then gradually increases to approximately 10 nm. The original texture of HAP within a collagen matrix is progressively lost, producing a porous HAP dominated solid at 700 °C, and a very low porosity sintered HAP product at 900 °C.

Background Many biominerals form from amorphous calcium carbonate (ACC), but this phase is highly unstable when synthesised in its pure form inorganically. Several species of earthworm secrete calcium carbonate granules which contain highly stable ACC. We analysed the milky fluid from which granules form and solid granules for amino acid (by liquid chromatography) and functional group (by Fourier transform infrared (FTIR) spectroscopy) compositions. Granule elemental composition was determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES) and electron microprobe analysis (EMPA). Mass of ACC present in solid granules was quantified using FTIR and compared to granule elemental and amino acid compositions. Bulk analysis of granules was of powdered bulk material. Spatially resolved analysis was of thin sections of granules using synchrotron-based μ-FTIR and EMPA electron microprobe analysis. Results The milky fluid from which granules form is amino acid-rich (≤ 136 ± 3 nmol mg −1 (n = 3; ± std dev) per individual amino acid); the CaCO 3 phase present is ACC. Even four years after production, granules contain ACC. No correlation exists between mass of ACC present and granule elemental composition. Granule amino acid concentrations correlate well with ACC content (r ≥ 0.7, p ≤ 0.05) consistent with a role for amino acids (or the proteins they make up) in ACC stabilisation. Intra-granule variation in ACC (RSD = 16%) and amino acid concentration (RSD = 22–35%) was high for granules produced by the same earthworm. Maps of ACC distribution produced using synchrotron-based μ-FTIR mapping of granule thin sections and the relative intensity of the ν 2 : ν 4 peak ratio, cluster analysis and component regression using ACC and calcite standards showed similar spatial distributions of likely ACC-rich and calcite-rich areas. We could not identify organic peaks in the μ-FTIR spectra and thus could not determine whether ACC-rich domains also had relatively high amino acid concentrations. No correlation exists between ACC distribution and elemental concentrations determined by EMPA. Conclusions ACC present in earthworm CaCO 3 granules is highly stable. Our results suggest a role for amino acids (or proteins) in this stability. We see no evidence for stabilisation of ACC by incorporation of inorganic components. Graphical abstract Synchrotron-based μ-FTIR mapping was used to determine the spatial distribution of amorphous calcium carbonate in earthworm-produced CaCO 3 granules.

Many rare and valuable ancient specimens now carry the scars of ancient DNA research, as questions of population genetics and phylogeography require larger sample sets. This fuels the demand for reliable techniques to screen for DNA preservation prior to destructive sampling. Only one such technique has been widely adopted: the extent of aspartic acid racemization (AAR). The kinetics of AAR are believed to be similar to the rate of DNA depurination and therefore a good measure of the likelihood of DNA survival. Moreover, AAR analysis is only minimally destructive. We report the first comprehensive test of AAR using 91 bone and teeth samples from temperate and high-latitude sites that were analysed for DNA. While the AAR range of all specimens was low (0.02-0.17), no correlation was found between the extent of AAR and DNA amplification success. Additional heating experiments and surveys of the literature indicated that d/l Asx is low in bones until almost all the collagen is lost. This is because aspartic acid is retained in the bone within the constrained environment of the collagen triple helix, where it cannot racemize for steric reasons. Only if the helix denatures to soluble gelatin can Asx racemize readily, but this soluble gelatine is readily lost in most burial environments. We conclude that Asx d/l is not a useful screening technique for ancient DNA from bone.

Fossils were thought to lack original organic molecules, but chemical analyses show that some can survive. Dinosaur bone has been proposed to preserve collagen, osteocytes, and blood vessels. However, proteins and labile lipids are diagenetically unstable, and bone is a porous open system, allowing microbial/molecular flux. These ‘soft tissues’ have been reinterpreted as biofilms. Organic preservation versus contamination of dinosaur bone was examined by freshly excavating, with aseptic protocols, fossils and sedimentary matrix, and chemically/biologically analyzing them. Fossil ‘soft tissues’ differed from collagen chemically and structurally; while degradation would be expected, the patterns observed did not support this. 16S rRNA amplicon sequencing revealed that dinosaur bone hosted an abundant microbial community different from lesser abundant communities of surrounding sediment. Subsurface dinosaur bone is a relatively fertile habitat, attracting microbes that likely utilize inorganic nutrients and complicate identification of original organic material. There exists potential post-burial taphonomic roles for subsurface microorganisms. The chances of establishing a real-world Jurassic Park are slim. During the fossilization process, biological tissues degrade over millions of years, with some types of molecules breaking down faster than others. However, traces of biological material have been found inside some fossils. While some researchers believe these could be the remains of ancient proteins, blood vessels, and cells, traditionally thought to be among the least stable components of bone, others think that they have more recent sources. One hypothesis is that they are in fact biofilms formed by bacteria. To investigate the source of the biological material in fossil bone, Saitta et al. performed a range of analyses on the fossilized bones of a horned dinosaur called Centrosaurus. The bones were carefully excavated in a manner to reduce contamination, and the sediment the bones had been embedded in was also tested for comparison. Saitta et al. found no evidence of ancient dinosaur proteins. However, the fossils contained more organic carbon, DNA, and certain amino acids than the sediment surrounding them. Most of these appeared to have a very recent source. Sequencing the genetic material revealed that the fossil had become a habitat for an unusual community of microbes that is not found in the surrounding sediment or above ground. These buried microbes may have evolved unique ways to thrive inside fossils. Future work could investigate how these unusual organisms live and whether the communities vary in different parts of the world.

The extensive use of mollusc shell as a versatile raw material is testament to its importance in prehistoric times. The consistent choice of certain species for different purposes, including the making of ornaments, is a direct representation of how humans viewed and exploited their environment. The necessary taxonomic information, however, is often impossible to obtain from objects that are small, heavily worked or degraded. Here we propose a novel biogeochemical approach to track the biological origin of prehistoric mollusc shell. We conducted an in-depth study of archaeological ornaments using microstructural, geochemical and biomolecular analyses, including ‘palaeoshellomics’, the first application of palaeoproteomics to mollusc shells (and indeed to any invertebrate calcified tissue). We reveal the consistent use of locally-sourced freshwater mother-of-pearl for the standardized manufacture of ‘double-buttons’. This craft is found throughout Europe between 4200–3800 BCE, highlighting the ornament-makers’ profound knowledge of the biogeosphere and the existence of cross-cultural traditions. Just like people do today, prehistoric humans liked to adorn themselves with beautiful objects. Shells, from creatures like clams and snails, were used to decorate clothing or worn as jewelry at least as far back as 100,000 years ago. Later people used shells as the raw materials to make beads or bracelets. Learning where the shells came from may help scientists understand why prehistoric people chose certain shells and not others. It may also offer clues about how they used natural resources and the cultural significance of these objects. But identifying the shells is difficult because they lose many of their original distinctive features when worked into ornaments. New tools that use DNA or proteins to identify the raw materials used to craft ancient artifacts have emerged that may help. So far, scientists have mostly used these genomic and proteomic tools to identify the source of materials made from animal hide, ivory or bone – where collagen is the most abundant protein molecule. Yet it is more challenging to extract and characterize proteins or genetic material from mollusc shells. This is partly because the amount of proteins in shells is at least 300 times lower than in bone, and also because the makeup of proteins in shells is not as well-known as in collagen. Sakalauskaite et al. have now overcome these issues by combining the analytical tools used to study the proteins and mineral content of modern shells with those of ancient protein research. They then used this approach, which they named palaeoshellomics, to extract proteins from seven “double-buttons” – pearl-like ornaments crafted by prehistoric people in Europe. The double-buttons were made between 4200 and 3800 BC and found at archeological sites in Denmark, Germany and Romania. Comparing the extracted proteins to those from various mollusc shells showed that the double-buttons were made from freshwater mussels belonging to a group known as the Unionoida. The discovery helps settle a decade-long debate in archeology about the origin of the shells used to make double-buttons in prehistoric Europe. Ancient people often crafted ornaments from marine shells, because they were exotic and considered more prestigious. But the results on the double-buttons suggest instead that mother-of-pearl from fresh water shells was valued and used by groups throughout Europe, even those living in coastal areas. The palaeoshellomics technique used by Sakalauskaite et al. may now help identify the origins of shells from archeological and palaeontological sites.