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Cosmetic has a long history in China while its origin has remained unclear. It potentially originated in the Spring and Autumn period (770‐476 BC) but little is known about its early manufacture and use. The Liujiawa Site, located at the southern edge of the Loess Plateau in northern China, was the late capital of the Rui State in the early to middle Spring and Autumn Period. During the excavation, a sealed small and exquisite container with suspected cosmetic use was unearthed from tomb M49 belonging to a male associated with the aristocratic class. Here, we report the multidisciplinary application of ATR‐FTIR, XRD, SEM, stable isotope analysis, GC/MS, and GC‐C‐IRMS analysis of the residue inside the container, demonstrating that the residue, made of ruminant adipose fat mixed with monohydrocalcite coming from cave moonmilk, was likely used as cosmetic face cream by the nobleman of ancient Rui State. This work provides an early example of cosmetic production in China and, together with the prevalence of similar cosmetic containers during this period, suggests the rise of an incipient cosmetics industry. Furthermore, the exploitation of moonmilk, a special stalactite in some limestone caves, reflects the link between early Taoist School and cosmetic production encouraged by the aristocratic class. 1. Introduction 2. Materials and Methods 2.1 Site and sample background 2.2 FTIR analysis 2.3 XRD analysis 2.4 SEM analysis 2.5 Inorganic carbon and oxygen isotope analysis 2.6 GC/MS analysis 2.7 GC-C-IRMS analysis 3. Results 3.1 The source of inorganic mineral 3.2 The origin of fat matrix 4. Discussion 4.1 The origin of the animal lipids 4.2 The exploitation of stalactites along with the Taoist School Cave Cultus 4.3 The earliest face cream in China 4.4 The rise of the cosmetic industry in the early period of Spring and Autumn

International audience; The origin of Tibetan papermaking is poorly documented. Up to now, only the Tibetan paper fragments from Endere and Dunhuang sites have been scientifically studied outlining the basic knowledge about plant fiber uses and artwork manufacturing procedures. In order to deepen the knowledge on the unique ancient Tibetan papermaking, we report here the analysis of a set of paper fragments from the Samye Monastery in south Tibet, China. Multidisciplinary scientific investigations utilizing 14C radiocarbon dating, microscopic observation, scanning electron microscopy (SEM), pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), pyrolysis-comprehensive gas chromatography/mass spectrometry (Py-GCxGC/MS), and proteomic analysis have been applied to these ancient paper fragments. The results show that the fragments were dated to the 12th~13th century AD and made from fibers of the Thymelaeaceae family plant Stellera Chamaejasme L of which the fiber’s chemical profiles have been firstly studied. The presence of starch granules from Triticum spp wheat and proteins from bovine milk (more likely assigned to native yak), offers the first indication that a unique sizing technique using starch-milk sizing had been employed in early Tibetan papermaking, compared to using alum-animal glue sizing agent which is more popular in contemporary Central China. The combined use of organic material (unaltered starch grains) and inorganic material (calcium carbonate) as paper fillers is also firstly revealed in Tibetan papermaking. The application of Py-GC/MS, Py-GCxGC/MS and proteomic analysis revealed more detailed profiles of early Tibetan hand papermaking, indicating that these methods have great potential to explore the production technology of ancient handmade papers.

The analysis of organic residues in pottery can provide abundant information on the lives of ancient people, including the natural resources consumed, the techniques applied, the functions of pottery, and so on. In this paper, a variety of methods, including FT-IR (Fourier transform infrared spectroscopy), GC–MS (gas chromatography-mass spectrometry), SEM (scanning electron microscopy) and SR-μCT (synchrotron radiation micro-computed tomography), have been employed to characterize the carbonized residues from an amphora, unearthed from the Changning site, Qinghai Province, Northwest China. The pottery residues were identified as birch bark tar, so ancient people in China could have used the particular local plant resources, birch bark, to produce tar as early as the Qijia cultural period (c. 4,000–3,500 bp). The birch bark tar could have been used to make composite tools discovered at the Changning site, and the amphora has probably been used for tar production. This, to our knowledge so far, is the earliest evidence for the use of birch bark tar in China. Due to the special geographical location of the Gansu-Qinghai Region, and the transition of subsistence strategy during the Qijia cultural period, the production and utilization of birch bark tar could not rule out the possibility of western influence, which needs further evidence.

The archaeological culture found in Xiaohe Cemetery (1980–1450 BC) is one of the early Bronze Age cultures in Xinjiang, northwestern China. The material assemblages from Xiaohe culture display features with both eastern and western influences. These east-west cultural and dietary interactions may be observed via the diet of the Xiaohe population. This paper examined the stable carbon and nitrogen isotopes of human and animal bones and human hairs from the Xiaohe Cemetery and compared with those of human bones from the Gumugou Cemetery, another Xiaohe culture site. The results indicate that the diets of the peoples from the Xiaohe culture varied significantly over different periods. The unified diets of the earlier periods reflect that an admixed population first settled in the Lop Nur region and primarily engaged in animal husbandry. In the later periods, the transformations in the human diets in this region reflect that new immigrants constantly relocated here and promoted population complexity over time. Moreover, this population occasionally produced small quantities of domesticated wheat and millet. The complex population and diversified economy of the Xiaohe culture were due to the expansion of the coeval cultures in the Eurasian steppe and eastern immigrants. Additionally, the millet cereal was probably mainly used for ritual practices rather than for staple food in the later periods.

The spotted hyena (Crocuta crocuta) is the only extant species of the genus Crocuta, which once occupied a much wider range during the Pliocene and Pleistocene. However, its origin and evolutionary history is somewhat contentious due to discordances between morphological, nuclear, and mitochondrial data. Due to the limited molecular data from east Asian Crocuta, also known as cave hyena, and the difficulty of extracting ancient DNA from this area, here we present proteomic analysis of cave hyenas from three locations in northern China. This marks the first proteomic data generated from cave hyenas, adding new molecular data to the east Asian populations. Phylogenetic analysis based on these protein sequences reveals two different groups of cave hyenas in east Asia, one of which could not be distinguished from modern spotted hyenas from northern Africa, tentatively the result of previously suggested gene flow between these lineages. With developments of instrumentation and analytical methods, proteomics holds promising potential for molecular phylogenetic reconstructions of ancient fauna previously thought to be unreachable using ancient DNA.

Fourier transform infrared spectroscopy (FTIR) and gas chromatography mass spectrometry (GC/MS) were conducted to identify a birch bark quiver from Ergonghe Reservoir Cemetery (the Tang Dynasty, A.D. 618–907) in Xinjiang, Northwest China. White substance on the bark surface was identified as gypsum (CaSO4·2H2O) by FTIR and X-ray diffraction analysis (XRD). The gypsum was probably residual white pigment of colored painting on the birch bark quiver. This is the first time that birch bark has been scientifically identified in China and it also provides the earliest evidence of colored painting on a birch bark artifact in ancient China. The minimally destructive methods are informative and promising for the analysis of ancient samples. Birch species are widely distributed in North China and ancient nomadic people put the bark to use in many aspects of their lives, reflecting the considerable importance of birch exploitation in their local life.

Some bright black beads with dense surface and poor light transmittance are generally considered as jet artifacts in China. However, little scientific investigation has been applied to support this judgment. This study focuses on the nondestructive identification of a jet bead, unearthed from the Changle Cemetery, Han Dynasty (202 BC-AD 220), Ningxia, China through multi nondestructive approach. The results of Gas Chromatography-Mass Spectrometry (GC/MS) analysis indicate that the bead belongs to coal products, based on the typical coal biomarkers including n-alkanes, acyclic isoprenoids and terpenoids. FTIR analysis further confirms that the bead is made of jet in comparison with modern jet samples in China. The bead is also scanned with Synchrotron Radiation Micro-computed Tomography (SR-μCT) to obtain the structure and drilling technology information, which suggests that the bead is uniform and was drilled from both sides. The nondestructive identification of ancient jet artifacts is first reported in China up to date, which not only reveals the varied utilizations of coal products in ancient society but also suggests that the popularization of jet in the Han Dynasty might be related to the first large-scale exploitation of coal, and offers an effective method suitable for archaeological jet samples.

Archaeological dental calculus has emerged as a rich source of ancient biomolecules, including proteins. Previous analyses of proteins extracted from ancient dental calculus revealed the presence of the dietary milk protein β-lactoglobulin, providing direct evidence of dairy consumption in the archaeological record. However, the potential for calculus to preserve other food-related proteins has not yet been systematically explored. Here we analyse shotgun metaproteomic data from 100 archaeological dental calculus samples ranging from the Iron Age to the post-medieval period (eighth century BC to nineteenth century AD) in England, as well as 14 dental calculus samples from contemporary dental patients and recently deceased individuals, to characterize the range and extent of dietary proteins preserved in dental calculus. In addition to milk proteins, we detect proteomic evidence of foodstuffs such as cereals and plant products, as well as the digestive enzyme salivary amylase. We discuss the importance of optimized protein extraction methods, data analysis approaches and authentication strategies in the identification of dietary proteins from archaeological dental calculus. This study demonstrates that proteomic approaches can robustly identify foodstuffs in the archaeological record that are typically under-represented due to their poor macroscopic preservation.

Detailed description of methods, supplementary tables and figures

Mortars are the layers paved on the surface of timber, earth or stone before painting and drawing. The analysis of their material composition and manufacture technology is necessary for revealing old technological approaches, selecting a suitable technological process in restoration and protection, and guiding the development of traditional technology of Chinese painting and colored drawings. According to ancient literature, crop flour and blood have been used as binders in the mortars of Chinese wooden buildings. However, little work is published on their scientific identification, and the reported methods could not determine their precise origins, which is important to understanding ancient mortar technology. In this study, Fourier Transform Infrared Spectroscopy (FTIR), Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) and starch grain analysis were employed to analyze the three mortars taken from the Old Summer Palace (18th and early 19th centuries), the Eastern Royal Tombs of the Qing Dynasty (middle 17th to early 20th centuries) and the Taiyuan Confucius Temple (late 19th century), respectively. FTIR analysis indicated the presence of proteins, and then different organic additives, namely, wheaten flour, cattle blood and pig blood, were identified respectively in the three mortars by LC/MS/MS analysis. Starch grain analysis also confirmed the proteomic results. Thus, proteomic analysis is highly effective for identifying the nature and origin of organic additives in the mortars of ancient painting.

With the emergence and progress of composite tools in the Middle Stone Age, the adhesive became one of the most widely used materials by early human societies. However, the precise composition identification of adhesive in archaeological remains is a real analytical challenge, because the adhesive mainly consists of organic materials that are susceptible to decay during burial process. Of particular interest is to know which animal/plant species were being exploited for glue manufacturing other than for food. The arid climate of the Xiaohe Cemetery, located in Taklamakan Desert, northwestern China, provides favorable conditions for the preservation of organic residues. A bone sculpture-inlaid wooden artifact was collected from the Xiaohe Cemetery, with some semi-transparent yellowish adhesive exposed due to the detachment of an inlaid bone sculpture. In this paper, micro samples of the adhesive were scraped for FTIR (Fourier Transform Infrared Spectroscopy, primary examination) and subsequent proteomic analysis to determine the proteinous component(s) and precise origin(s). The identified tryptic peptides match most closely to known bovine collagen markers, suggesting that this adhesive was an animal glue made from cattle. These results reveal the diverse utilizations of cattle in the Xiaohe Cemetery, which provided not only meat, milk, hides, sinews and dung, but also leftover parts for manufacturing adhesive. This is the earliest evidence of adhesive identified in China up to our knowledge, which sheds light on adhesive development around 3500 years ago.

We analyzed the best light intensity for callus induction and maintenance in Vitis vinifera and explored the mechanism of grape callus browning. Tender stem segments of grape cultivar "gold finger" were used to study the effects of different light intensities (0, 500, 1 000, 1 500, 2 000, 2 500, 3 000 and 4 000 Lx) on the induction rate, browning rate and associated enzyme activity and gene expression during Vitis vinifera callus formation. The callus induction rate under 0, 500, 1 000 and 1 500 Lx was more than 92%, significantly higher than in other treatments (P0.05). A lower browning rate and better callus growth were also observed during subculture under 1 000 and 1 500 Lx treatments. We found that chlorogenic acid, caffeic acid, p-hydroxybenzoic acid and coumaric acid contents were correlated with the browning rate of callus, among which chlorogenic acid content was positively correlated with the browning rate (P0.05). Peroxidase (POD) and polyphenol oxidase (PPO) activities were negatively correlated with the browning rate of callus (P0.01). The POD, PPO and phenylalanine ammonialyase (PAL) expression levels were positively correlated with the browning rate at P0.05 or P0.01. An appropriate light intensity for the tissue culture of Vitis vinifera was 1 000-1 500 Lx, higher or lower light intensities significantly impaired normal callus growth.

Phytoliths and biomolecular components extracted from ancient plant remains from Chang’an (Xi’an, the city where the Silk Road begins) and Ngari (Ali) in western Tibet, China, show that the tea was grown 2100 years ago to cater for the drinking habits of the Western Han Dynasty (207BCE-9CE) and then carried toward central Asia by ca.200CE, several hundred years earlier than previously recorded. The earliest physical evidence of tea from both the Chang’an and Ngari regions suggests that a branch of the Silk Road across the Tibetan Plateau, was established by the second to third century CE.