Biomolecular characterization of 3500-year-old ancient Egyptian mummification balms from the Valley of the Kings

Ancient Egyptian mummification was practiced for nearly 4000 years as a key feature of some of the most complex mortuary practices documented in the archaeological record. Embalming, the preservation of the body and organs of the deceased for the afterlife, was a central component of the Egyptian mummification process. Here, we combine GC-MS, HT-GC-MS, and LC-MS/MS analyses to examine mummification balms excavated more than a century ago by Howard Carter from Tomb KV42 in the Valley of the Kings. Balm residues were scraped from now empty canopic jars that once contained the mummified organs of the noble lady Senetnay, dating to the 18th dynasty, ca. 1450 BCE. Our analysis revealed balms consisting of beeswax, plant oil, fats, bitumen, Pinaceae resins, a balsamic substance, and dammar or Pistacia tree resin. These are the richest, most complex balms yet identified for this early time period and they shed light on balm ingredients for which there is limited information in Egyptian textual sources. They highlight both the exceptional status of Senetnay and the myriad trade connections of the Egyptians in the 2nd millennium BCE. They further illustrate the excellent preservation possible even for organic remains long removed from their original archaeological context

Genetic insights into the social organization of Neanderthals

Genomic analyses of Neanderthals have previously provided insights into their population history and relationship to modern humans1–8, but the social organization of Neanderthal communities remains poorly understood. Here we present genetic data for 13 Neanderthals from two Middle Palaeolithic sites in the Altai Mountains of southern Siberia: 11 from Chagyrskaya Cave9,10 and 2 from Okladnikov Cave11—making this one of the largest genetic studies of a Neanderthal population to date. We used hybridization capture to obtain genome-wide nuclear data, as well as mitochondrial and Y-chromosome sequences. Some Chagyrskaya individuals were closely related, including a father–daughter pair and a pair of second-degree relatives, indicating that at least some of the individuals lived at the same time. Up to one-third of these individuals’ genomes had long segments of homozygosity, suggesting that the Chagyrskaya Neanderthals were part of a small community. In addition, the Y-chromosome diversity is an order of magnitude lower than the mitochondrial diversity, a pattern that we found is best explained by female migration between communities. Thus, the genetic data presented here provide a detailed documentation of the social organization of an isolated Neanderthal community at the easternmost extent of their known range

Preparative HPLC separation of underivatized amino acids for isotopic analysis

Single-compound analysis of stable or radioactive isotopes has found application in a number of fields ranging from archaeology to forensics. Often, the most difficult part of these analyses is the development of a method for isolating the compound(s) of interest, which can derive from a wide range of sample types including the hair, nails, and bone. Here we describe three complementary preparative HPLC techniques suitable for separating and isolating amino acids from bone collagen and hair keratin. Using preparative reversed-phase, ion-pair, or mixed-mode chromatography in aqueous carbon-free mobile phases, or those from which carbon can easily be removed, underivatized single amino acids can be isolated and further analyzed using mass spectrometric techniques.</p

Preparative HPLC separation of underivatized amino acids for isotopic analysis

Single-compound analysis of stable or radioactive isotopes has found application in a number of fields ranging from archaeology to forensics. Often, the most difficult part of these analyses is the development of a method for isolating the compound(s) of interest, which can derive from a wide range of sample types including the hair, nails, and bone. Here we describe three complementary preparative HPLC techniques suitable for separating and isolating amino acids from bone collagen and hair keratin. Using preparative reversed-phase, ion-pair, or mixed-mode chromatography in aqueous carbon-free mobile phases, or those from which carbon can easily be removed, underivatized single amino acids can be isolated and further analyzed using mass spectrometric techniques

Les résines végétales de type copal et encens : caractérisation, exploitation et circuits commerciaux

Les résines végétales de type copal et encens : caractérisation, exploitation et circuits commerciau

TGMS analysis of archaeological bone from burials of the late Roman period

The use of thermogravimetric analysis-mass spectrometry (TGMS) to study the state of preservation of archaeological bones has been investigated. As part of a collaborative multi-analytical study, bones exhumed from graves of the late Roman period in France and Italy were examined. A decrease in organic matter for the archaeological bones compared to that for new bone was confirmed, demonstrating that diagenesis of aged bones can be detected using TGMS. Different amounts of collagen were determined for bones from different graves and could, for the majority of specimens, be correlated with the visually observed preservation states. © 2009 Akadémiai Kiadó, Budapest, Hungary

Single amino acid radiocarbon dating of two Neanderthals found at Šal’a (Slovakia)

Human remains from the (late) Middle Paleolithic remain rare. Improving our understanding of their spatio-temporal distribution is essential for obtaining insights into human evolution and the dynamics between Neanderthals and early Anatomically Modern Humans (AMHs). We present the single-amino-acid radiocarbon dating and ancient DNA results from the only Neanderthal skeletal remains known in Slovakia (Šal’a I and Šal’a II). As they were found without archaeological context and in secondary deposition, recontextualization is important. By employing the hydroxyproline radiocarbon dating method, we were able to successfully counteract contamination issues and circumvent problems caused by highly degraded collagen. By contrast, DNA analysis did not detect any endogenous DNA at the limits of our resolution. We conclude that the radiocarbon ages of >44,800 BP (OxA-X-2731-16) and >45,100 (OxA-X-2731-15) firmly place the two individuals in the Middle Paleolithic, and before the arrival of AMHs to the region. Furthermore, indirect evidence based on morphology and possibly related faunal remains suggest ages younger than 100 ka. This time frame coincides with a period in which Neanderthal populations were highly dispersed in Europe, yet in decline

New data for the Early Upper Paleolithic of Kostenki (Russia)

Several questions remain regarding the timing and nature of the Neanderthal-anatomically modern human (AMH) transition in Europe. The situation in Eastern Europe is generally less clear due to the relatively few sites and a dearth of reliable radiocarbon dates. Claims have been made for both notably early AMH and notably late Neanderthal presence, as well as for early AMH (Aurignacian) dispersal into the region from Central/Western Europe. The Kostenki-Borshchevo complex (European Russia) of Early Upper Paleolithic (EUP) sites offers high-quality data to address these questions. Here we revise the chronology and cultural status of the key sites of Kostenki 17 and Kostenki 14. The Kostenki 17/II lithic assemblage shares important features with Proto-Aurignacian material, strengthening an association with AMHs. New radiocarbon dates for Kostenki 17/II of ∼41–40 ka cal BP agree with new dates for the recently excavated Kostenki 14/IVw, which shows some similarities to Kostenki 17/II. Dates of ≥41 ka cal BP from other Kostenki sites cannot be linked to diagnostic archaeological material, and therefore cannot be argued to date AMH occupation. Kostenki 14's Layer in Volcanic Ash assemblage, on the other hand, compares to Early Aurignacian material. New radiocarbon dates targeting diagnostic lithics date to 39–37 ka cal BP. Overall, Kostenki's early EUP is in good agreement with the archaeological record further west. Our results are therefore consistent with models predicting interregional penecontemporaneity of diagnostic EUP assemblages. Most importantly, our work highlights ongoing challenges for reliably radiocarbon dating the period. Dates for Kostenki 14 agreed with the samples' chronostratigraphic positions, but standard pre-treatment methods consistently produced incorrect ages for Kostenki 17/II. Extraction of hydroxyproline from bone collagen using preparative high-performance liquid chromatography, however, yielded results consistent with the samples' chronostratigraphic position and with the layer's archaeological contents. This suggests that for some sites compound-specific techniques are required to build reliable radiocarbon chronologies

A multi-analytical approach using FTIR, GC/MS and Py-GC/MS revealed early evidence of embalming practices in Roman catacombs

© 2017 Elsevier B.V. During the second-third century, cremation was progressively abandoned for inhumation in the Roman Empire and was accompanied by new funeral practices. Recent archaeological excavations in the catacombs of Saints Peter and Marcellinus in Rome revealed thousands of formerly undiscovered skeletons of individuals plastered and methodically stacked in previously unknown and inaccessible rooms. By setting up and applying a multi-analytical approach to characterize chemically all amorphous materials surrounding the skeletons, we investigated this important cultural change regarding the treatment of death. Chemical characterization of the amorphous samples was achieved using FTIR spectroscopy and gas chromatography/mass spectrometry (Py-GC/MS and GC/MS) and by comparison with reference samples from known origin. This allowed for the unambiguous identification of precious and exotic resinous substances involved in the embalming process of the bodies. Amber, sandarac and frankincense, which were sourced from widespread locations, were used as part of the funerary treatment. This first evidence of such highly prized commodities in burial process provides us with new insight into funerary practices as well as commercial networks in the Roman Empire during the first centuries A.D

Increasing accuracy for the radiocarbon dating of sites occupied by the first Americans

Genetic analysis of Paleoamerican human remains suggests that people first entered the Americas sometime between ∼14,000 and ∼16,000 years ago. Evaluation of these data requires unequivocal archaeological evidence in a solid geological context that is well dated. Accurately determining the age of late Pleistocene sites is thus crucial in explaining when and how humans colonized the Americas. There are, however, significant challenges to dating reliability, especially when vertebrate fossils (i.e. bones, teeth and ivory) are often the only datable materials preserved at sites. We re-dated vertebrate fossils associated with the North American butchering sites of Wally's Beach (Canada), La Prele [also known as Fetterman (Wyoming)], Lindsay (Montana), and Dent (Colorado). Our work illustrates the crucial importance of sample chemical preparation in completely removing contaminants derived from sediments or museum curation. Specifically, our work demonstrates that chromatographic methods, e.g. preparative High Performance Liquid Chromatography and column chromatography using XAD resins, are currently the only efficient methods for removing environmental and museum-derived contaminants. These advanced techniques yield demonstrably more accurate AMS 14C measurements that refine the ages of these four sites and thereby contribute to advancing our understanding of human dispersals across North America during the late Pleistocene