Stable Carbon Isotope Analysis Research Articles

Comparative stable isotope analyses of green sturgeon (Acipenser medirostris) and white sturgeon (A. transmontanus) in the San Francisco estuary.

Green sturgeon (Acipenser medirostris) and white sturgeon (A. transmontanus) are closely related, sympatric species that inhabit the San Francisco estuary. Green sturgeon have a more marine life history but both species spawn in the Sacramento River and reside for some duration in San Francisco Bay. These sturgeons are of conservation concern, yet little is known about their dietary competition when they overlap in space and time. To examine evidence of dietary differentiation, we collected whole blood and blood plasma from 26 green sturgeon and 35 white sturgeon in San Francisco Bay. Using carbon and nitrogen stable isotope analyses, we compared their relative trophic levels and foraging locations along the freshwater to marine gradient. Sampling blood plasma and whole blood allowed comparison of dietary integration over shorter and longer time scales, respectively. Plasma and whole blood δ13 C values confirmed green sturgeon had more marine dietary sources than white sturgeon. Plasma δ15 N values revealed white sturgeon fed at lower trophic levels than green sturgeon recently, however, whole blood δ15 N values demonstrated the two species fed at the same trophic level over longer time scales. Larger individuals of both species had higher δ13 C values than smaller individuals, reflecting more marine food sources in adulthood. Length did not affect δ15 N values of either species. Isotope analyses supported the more marine life history of green than white sturgeon and potentially highlight a temporary trophic differentiation of diet between species during and preceding the overlapping life stage in San Francisco Bay.

Spatially resolved CO2 carbon stable isotope analyses at the microscale using Raman spectroscopy

Measuring the carbon stable isotope ratio (13C/12C, expressed as δ13CCO2) in geogenic CO2 fluids is a crucial geochemical tool for studying Earth's degassing. Carbon stable isotope analysis is traditionally performed by bulk mass spectrometry. Although Raman spectroscopy distinguishes 12CO2 and 13CO2 isotopologue bands in spectra, using this technique to determine CO2 isotopic signature has been challenging. Here, we report on in-situ non-destructive analyses of the C stable isotopic composition of CO2, applying a novel high-resolution Raman configuration on 42 high-density CO2 fluid inclusions in mantle rocks from the Lake Tana region (Ethiopia) and El Hierro (Canary Islands). We collected two sets of three spectra with different acquisition times at high spectral resolution in each fluid inclusion. Among the 84 sets of spectra, 58 were characterised by integrated 13CO2/12CO2 band area ratios with reproducibility better than 4‰. Our results demonstrate the determination of δ13CCO2 by Raman spectroscopy in individual fluid inclusions with an error better than 2.5 ‰, which satisfactorily matches bulk mass spectrometry analyses in the same rock samples, supporting the accuracy of the measurements. We thus show that Raman Spectroscopy can provide a fundamental methodology for non-destructive, site-specific, and spatially resolved carbon isotope labelling at the microscale.

Impact of Hydrocarbon Emissions from Oil and Gas Deposits on δ13C Variability in Pine Tree Rings from the Tatarstan Republic

Human-caused anthropogenic greenhouse emissions impact the climate globally. In this pilot study, we aim to reveal the influence of hydrocarbon emissions on pine forests by applying a stable carbon isotope analysis in pine tree rings (δ13Cptrw). Our study was conducted in an industrial giant oil field reservoir (UVRT) and natural reserve (Raifa) sites, the Tatarstan Republic, Russia. Our results show a decreasing δ13Cptrw at the UVRT site in 1943, when oil extraction started, and in 1970, when it reached maximum production. We found that the δ13Cptrw from UVRT indicates developing unfavourable drier conditions and a suppressed tree growth caused by both human-induced oil and deposit infrastructures and natural processes compared to the undisturbed Raifa site. A 5-year running correlation analysis showed a significant difference between the sites in 1965 over the period of 1930 to 2021. The δ13Cptrw values from Raifa are more negative compared to UVRT, which can be explained by a higher forest sensitivity to human-induced impacts. From an eco-physiological point of view, the decreasing of intercellular (ci)-to-ambient (ca) CO2 concentration ratios at the leaf level and the increasing of intrinsic water-use efficiency (iWUE) along with a decreasing of tree-ring widths at the UVRT site (1970–2021) indicate the development of drought conditions.

Predicting the potential implications of perch (Perca fluviatilis) introductions to a biodiversity-rich lake using stable isotope analysis

Biological invasions, particularly of fish species, significantly threaten aquatic ecosystems. Among these invaders, the introduction of the European perch (Perca fluviatilis) can have particularly detrimental effects on native communities, affecting both ecosystem functioning and human well-being. In this study, carbon and nitrogen stable isotope analysis was employed, using perch originating from five different ecosystems, to model the effects of their hypothetical introduction into İznik Lake, an economically and ecologically important, biodiversity-rich lake in northern Turkey, to ultimately assess their potential predation impact and competition with native predators. The results revealed that if perch were introduced to the community, they would – considering gape size limitations – primarily prey upon Vimba vimba and Rutilus rutilus, indicating a significant feeding pressure on these species. Furthermore, the study identified a potential overlap and competition for resources between commonly mesopredator perch and the European catfish Silurus glanis, the current top predator in the ecosystem. Both species would occupy top predatory positions, emphasizing the potential disruption of predator–prey dynamics. Our findings underscore the potential ecological repercussions of perch invasions. The selective predation on V. vimba and R. rutilus, with the latter being consumed to a lesser extent by perch, could lead to cascading effects throughout the food web, altering the community structure, and ecosystem dynamics. Additionally, the competition between perch and S. glanis raises concerns about effects on the stability and functioning of the fish community. These results highlight the need for proactive management strategies to mitigate the risk of perch introductions. Strict regulations on the movement and introduction of invasive species, along with comprehensive monitoring, are crucial for preserving native communities and maintaining the ecological integrity of freshwater ecosystems. Our study demonstrates the potential predation impact of perch on vulnerable fish species and the competition with the established apex predator, emphasizing the importance of considering the ecological consequences of perch invasions and informing management decisions to ensure the conservation and sustainability of aquatic ecosystems.

Tropical and temperate differences in the trophic structure and aquatic prey use of riparian predators.

The influence of aquatic resource-inputs on terrestrial communities is poorly understood, particularly in the tropics. We used stable isotope analysis of carbon and nitrogen to trace aquatic prey use and quantify the impact on trophic structure in 240 riparian arthropod communities in tropical and temperate forests. Riparian predators consumed more aquatic prey and were more trophically diverse in the tropics than temperate regions, indicating tropical riparian communities are both more reliant on and impacted by aquatic resources than temperate communities. This suggests they are more vulnerable to disruption of aquatic-terrestrial linkages. Although aquatic resource use declined strongly with distance from water, we observed no correlated change in trophic structure, suggesting trophic flexibility to changing resource availability within riparian predator communities in both tropical and temperate regions. Our findings highlight the importance of aquatic resources for riparian communities, especially in the tropics, but suggest distance from water is less important than resource diversity in maintaining terrestrial trophic structure.

Isotopic and proteomic evidence for communal stability at Pre-Pottery Neolithic Jericho in the Southern Levant

As one of the key, long-term occupied sites in the Southern Levant, Jericho was one of the most important early Neolithic centres to witness social and economic changes associated with the domestication of plants and animals. This study applies strontium (87Sr/86Sr), oxygen (δ18O) and carbon (δ13C) isotope analyses to the enamel of 52 human teeth from Pre-Pottery Neolithic (PPN) layers of Jericho to directly study human diet and mobility and investigate the degree of consolidation and the flexibility of social organization of Jericho society in the PPN period. The results indicate only two non-local individuals out of the 44 sampled inhabitants identified by strontium isotope analysis and are consistent with the presence of a largely sedentary community at PPN Jericho with no evidence for large-scale migration. We also construct strontium spatial baselines (87Sr/86Sr map) with local 87Sr/86Sr signatures for the sites across the Southern Levant based on systematic compilation and analysis of available data. In addition, we apply proteomic analysis of sex-specific amelogenin peptides in tooth enamel for sex estimation of the sampled individuals (n = 44), the results of which showed a sex-biased ratio (more male than female detected in this sample pool) in Jericho society during the PPN period, which may be due to the limited sample size or selective ritual practices like particular burial zones used for specific groups. We also pretreated a batch of human bone samples recovered from PPNB Jericho for stable carbon and nitrogen isotope analyses for dietary investigations. However, the extracted collagen showed poor preservation and no valid δ13C or δ15N data were obtained.

Evidence for a Temporary Positive Priming Effect in Aquatic Systems With Certain Substrates and Isotopic Discrimination of DOM Sources

AbstractThe “priming effect” (PE) is well documented in soils, but contradictory results have been reported in aquatic ecosystems. To investigate whether the presence of easily degradable labile dissolved organic matter (LDOM) changes the biodegradation rate of nonlabile DOM (NLDOM), incubations were performed with various sources of LDOM and NLDOM in microcosms amended with nutrients and a microbial inoculum. Stable carbon isotope analysis of DOM was used for the first time to estimate the PE. A significant positive PE (15%–34% of initial NLDOM) was measured, but only with mixed (glucose + amino acids) or complex (disaccharide) LDOM. Regardless of the LDOM, no PE was measured with more recalcitrant NLDOM (half‐life of 128 days here), when the LDOM/NLDOM ratio was low (0.3 versus 1), and when the NLDOM and microbial inoculum were from the same water (no mixing). The presence of sediments likely enhances microbial diversity and NLDOM degradation rate, but it did not increase the PE. Microbial use of LDOM produced new microbial NLDOM that should be discriminated (here by isotopes) from initial NLDOM for accurate PE measurements. The PE was temporary and lasted about 2 weeks after one LDOM addition. In areas with frequent additions of LDOM, a long‐lasting PE is expected and may significantly increase CO2 production. Exposing refractory DOM to new conditions and microbial community, such as during natural water mixing, seems to exert a strong control on its dynamics. Here, the addition of a new microbial inoculum had a stronger effect than adding LDOM or the PE.

Effects of lipid extraction on human bone collagen: Comparing stable carbon and nitrogen isotope values with and without lipid extraction

This study analyzes 24 human bone fragments to assess how lipid extraction affects stable carbon and nitrogen isotope ratios. Eighteen samples were archaeological bone and six were modern bone. Each bone was split into two pieces, producing 48 bone samples, and half underwent lipid extraction and half did not. This was done to assess whether the two techniques yielded statistically significant differences in δ13C and δ15N. The results are an important contribution for establishing standard stable isotope preparation protocols, which affect time and cost of laboratory procedures. Further, given that many dietary stable isotope studies compare original results to published material, this study addresses whether those comparisons are suitable if some samples undergo lipid extraction while others do not.We also examine 144 articles that report stable carbon and nitrogen isotope results to evaluate the proportion of studies that conduct lipid extraction versusthose that do not. We explore those outcomes by archaeological geographic region and by stable isotope laboratories. Findings show that 15% of the published studies do lipid extraction, and they tend to be grouped by researchers and laboratories who conduct research in specific global regions. The meta-analysis of the published articles and the findings that some laboratories conduct lipid extraction, while others do not, prompted the experimental portion of this study.Results of the experimental study show no significant differences in δ13C between samples prepared with and without lipid extraction and no significant differences in δ15N between samples prepared with and without lipid extraction. These results suggest that stable carbon and nitrogen isotope analysis of human bone collagen may not require lipid extraction for certain dietary reconstruction studies, specifically for non-coastal contexts (i.e., non-marine based diets). The isotope data was analyzed overall and among subgroups (e.g., archaeological bone, modern bone, mid-valley Peruvian ecological zones, and highland Peruvian ecological zones). In all cases, stable isotope ratios from samples prepared with and without lipid extraction were not significantly different.

Distribution of siphonophores in the Northwest Pacific Ocean and links to environmental conditions

Despite their abundance in marine ecosystems, studies on siphonophores are limited. In this study, 26 species of siphonophores in the Northwest Pacific Ocean were identified during multiple cruises of the R/V ISABU from 2018–2020, and various factors that may affect the occurrence of siphonophores, including water temperature, salinity, zooplankton biomass, and trophic niche were investigated. Statistical analysis revealed that the distribution of siphonophores and their biomass could be divided into two water mass groups, affected by the Kuroshio and Oyashio Currents. The species with high contributions to distinguishing the water mass groups (including Chelophyes contorta, Dimophyes arctica, Bassia bassensis, and Eudoxoides spiralis—mainly belonging to the Diphyidae) showed species-specific correlations with water temperature and salinity. This suggests that diphyids can be used as indicator species for currents and hydrological factors that influence water mass. The biomass of siphonophores exhibited a trend opposite to that of non-gelatinous zooplankton and showed no association with other gelatinous zooplankton. These results can be interpreted from an ecological niche perspective. Through nitrogen and carbon stable isotope analyses, the dietary sources of siphonophores could potentially overlap with those of chaetognaths or non-gelatinous zooplankton. Because the trophic position of siphonophores (2.4–3.2) also falls in the range of those of chaetognaths (2.8–3.4) and non-gelatinous zooplankton including copepods, euphausiids, and amphipods (2.4–3.5), diet competition with carnivorous mesozooplankton could be predicted. Considering that the diversity and biomass of most siphonophores are strongly positively correlated with water temperature and salinity, expansion of the Kuroshio Current is expected to lead to an increase in siphonophores in the Northwest Pacific in the future. The findings of this study are anticipated to provide novel insights into climate change prediction and response and enhance our understanding of siphonophore communities.

Occurrence and Genesis of Cold‐Seep Authigenic Carbonates from the South‐Eastern Mediterranean Sea

AbstractMethane‐derived authigenic seep carbonates occur globally along continental margins. These carbonates are important archives to identify seep dynamics, the source of the ascending methane‐enriched fluids together with their timing, and are an important carbon sequestration mechanism. Recently, seep carbonates were discovered in the Levant Basin in the south‐eastern Mediterranean Sea. To elucidate past seepage activity and dynamics across the basin, different seep carbonate morphologies (chimneys, crusts and pavements) retrieved from the Levant Basin were mapped based on remotely operating vehicle data and analysed using standard sediment petrographic techniques, X‐ray diffraction and stable carbon and oxygen isotope analyses. Carbonate chimneys consist of micrite (δ13CVPDB of −10‰ to +5‰) with dispersed baryte and dolomite crystals, fan‐shaped aragonite (δ13CVPDB of −52‰ to −30‰) and high‐magnesium calcite cements, with the latter often growing from low‐magnesium calcite spherules. Botryoidal low‐magnesium calcite cements are forming in small cavities. Carbonate crusts consist of micrite with low‐magnesium calcite breccias, high‐magnesium calcite nodules (δ13CVPDB of −35‰ to −20‰) and cements, and partially replaced fan‐shaped aragonite cements. Carbonate pavements consist of low‐magnesium calcite microsparite, micritic dolomite and high‐magnesium calcite. Fan‐shaped aragonite is locally present as pore‐lining cement. Iron oxides are often seen coating the low‐magnesium calcite, high‐magnesium calcite and dolomite cements. Chimneys and crusts, characterised by high amounts of high‐magnesium calcite and aragonite, are interpreted to have formed through advective methane fluxes. Pavements, with high quantities of dolomite, are explained as the product of diffusive methane flux. Sediment petrographic and geochemical analysis of the different carbonate morphologies and cement phases therein witness distinct modes of ascending fluid fluxes and their mixing with marine pore water and/or sea water during precipitation of the individual phases.

Development characteristics and genetic analysis of dense limestone reservoirs in the Taiyuan Formation of the Ordos Basin, China

Tight limestone reservoirs in the Permian Taiyuan Formation of the Ordos Basin have garnered increasing attention in recent years, emerging as a pivotal domain in the quest for natural gas exploration. This research delves into the comprehensive investigation of petrology, reservoir space, reservoir physical properties, and microscopic characteristics through the examination of field outcrops, core observations, thin section identification, scanning electron microscopy, stable carbon and oxygen isotope analysis, and testing. The systematic analysis focused on elucidating the development characteristics of these reservoirs and identifying the controlling factors governing favorable reservoir conditions. Based on our research analysis, the specific rock types with the potential to serve as excellent reservoirs, includes bioclastic silty limestone, bioclastic micrite limestone, and algal-rich limestone. The predominant reservoir spaces within these formations were found to consist of dissolved pores, residual bioclastic cavity pores, intercrystalline pores, and microfractures. These reservoirs exhibit an average porosity of 2.1%, and an average permeability of 0.22 × 10−3 μm2, indicating their classification as low porosity and low permeability reservoirs. The formation of favorable reservoirs in the Taiyuan Formation limestone was determined to be influenced by many factors; notably, the favorable sedimentary microfacies associated with bioclastic shoals and bioherms provided the foundational material basis for the formation of reservoirs, influencing the type of reservoir space and its extensive planar distribution. Penecontemporaneous karstification, guided by high-frequency cycles, was favorable for the formation of dissolution holes, effectively improving reservoir performance and facilitating the development of thick limestone reservoirs. Furthermore, fractures were identified as crucial agents in improving the seepage capacity of these tight limestone reservoirs. Drawing from our research results, this study offers valuable guidance for the future exploration of limestone formations in the Taiyuan Formation in the Ordos Basin. Additionally, these findings hold considerable significance as a reference point for research and exploration endeavors focused on bioclastic limestone reservoirs in the North China Platform.

Reconstruction of the Late Miocene to Pliocene continental succession of Samos Island: Palaeoenvironmental implications for the Eastern Aegean domain

AbstractOn the Island of Samos (East Aegean region, Greece), two sedimentary basins are filled by thick continental series dated to the Late Miocene to Early Pliocene. A multidisciplinary study has been performed including (1) the definition of 21 sedimentary facies, (2) a review of the biological components and (3) carbon, oxygen and strontium stable isotope analyses. The succession is characterised by various depositional settings and hydrochemical compositions. Five main stages of basin evolution have been identified: (1) The Late Serravallian is marked by the development of alluvial fans and fan delta; (2) during the Lower Tortonian, isolated shallow lakes with variable salinity, from fresh to brackish, developed under warm and relatively humid conditions; (3) the Middle to Upper Tortonian is marked by the development of a large and deep lake with saline and alkaline waters, under colder and drier conditions; (4) the Latest Tortonian to Messinian period is represented by an ephemeral alluvial system, developed under a dry climate; (5) during the Zanclean, a palustrine and paludal wetland system, dominated by tufa carbonates, developed under moderately humid conditions. This succession is of particular interest for the reconstruction of the palaeoenvironmental evolution of the transition zone between the Mediterranean domain, and the Paratethys and circum‐Paratethys areas. The geochemical data and the presence of flora (diatoms) and fauna (gastropods) of marine affinity suggest transient ingressions of marine‐related water or groundwater inflows as early as the Lower Tortonian. The Samos succession records the complex interaction between the regional geodynamics and climate. The extensional regime of the Eastern Aegean zone generates subsidence, interrupted in the mid‐Tortonian (9 Ma) by a brief compressive event and a major exposure of the basins. Furthermore, the Late Miocene progressive aridification, followed by a change to a more humid climate (Pliocene) is also a major driver of the sedimentation.

Neolithic herding practices in the Southern Caucasus: Animal management in the early 6th millennium BCE at Masis Blur in Armenia’s Ararat Valley

The Southern Caucasus is traditionally an important area of livestock production and a key region in the spread of herding from southwestern Asia to Eurasia’s western steppe. Neolithic settlements appeared across the Southern Caucasus in the early 6th millennium BCE. How these communities used the landscape and managed livestock in the context of mixed farming is not well understood. Stable carbon (δ13C) and nitrogen (δ15N) isotope analysis of bone collagen and stable carbon and oxygen (δ18O) isotope analysis of tooth enamel from faunal remains from Masis Blur, one of the earliest Neolithic sites in the Southern Caucasus, clarify how communities maintained herds in this topographically varied region. δ13C and δ15N values indicate hunting wild fauna in diverse environments. δ13C and δ18O values from sequentially sampled livestock teeth demonstrate markedly different strategies for managing cattle and caprines. Negative covariation in δ18O and δ13C values in most caprines suggest seasonal mobility to C3-dominated high elevation pastures in the summers, and/or winter foddering with water-stressed C3 or wild C4 plants. These seasonal strategies were in place in the earliest known phase of occupation at Masis Blur, indicating that Southern Caucasus Neolithic communities likely exploited a range of environments linking the lowland plains and mountainous zones.

Unprecedented shift in Canadian High Arctic polar bear food web unsettles four millennia of stability

Stable carbon (δ13C) and nitrogen (δ15N) isotope analysis was conducted on modern and archaeological polar bear bone collagen from the Canadian Arctic Archipelago to investigate potential changes in polar bear foraging ecology over four-millennia. Polar bear δ13C values showed a significant decline in the modern samples relative to all archaeological time-bins, indicating a disruption in the sources of production that support the food web, occurring after the Industrial Revolution. The trophic structure, indicated through δ15N, remained unaltered throughout all time periods. The lower δ13C observed in the modern samples indicates a change in the relative importance of pelagic (supported by open-water phytoplankton) over sympagic (supported by sea ice-associated algae) primary production. The consistency in polar bear δ13C through the late Holocene includes climatic shifts such as the Medieval Warm Period (MWP, A.D. 950-1250) and the early stages of the Little Ice Age (LIA, A.D. 1300-1850). These findings suggest that polar bears inhabit a food web that is more pelagic and less sympagic today than it was through the Late Holocene. We suggest that modern, anthropogenic warming has already affected food web structure in the Canadian Arctic Archipelago when modern data are contextualized with a deep time perspective.

Lipid Correction for Carbon Stable Isotope Analysis of Yellowfin Tuna

Carbon stable isotopes (δ13C) are widely used in ecological studies to understand diet, food web dynamics, and movements of marine fishes. Still, δ13C is influenced by lipid content and often requires chemical extraction or mathematical correction. Here, we developed a species-specific mathematical lipid correction for white muscle tissue of yellowfin tuna (Thunnus albacares), a highly migratory finfish of considerable economic and ecological value. Lipid extraction was conducted on yellowfin tuna white muscle tissue (C:N range: 2.96–6.49), and both linear and non-linear lipid correction models for δ13C were fitted and assessed. Lipid extraction increased δ13C, and to a lesser extent, δ15N values in yellowfin tuna white muscle tissue, but had no effect on δ34S. Both non-linear models provided better fits to the data than the linear model, suggesting an asymptotic relationship between C:N and ∆δ13C. Results support the growing body of evidence that C:N ratios can be used to predict lipid corrected δ13C and highlight the value of mathematical correction approaches. We provide species-specific parameter estimates that can be used for lipid correction of white muscle tissue for δ13C analysis in yellowfin tuna and similar species for which species-specific models have yet to be developed.

Sources of intraspecific variation in the isotopic niche of a semi-aquatic predator in a human-modified landscape.

Intraspecific variation modulates patterns of resource use by species, potentially affecting the structure and stability of food webs. In human-modified landscapes, habitat disturbance modifies trophic interactions and intraspecific niche variation, impacting population persistence. Here, we investigated the relationship of sex, ontogeny, and habitat factors with the trophic niche of Caiman crocodilus in an agricultural landscape. We evaluated temporal variation in the trophic niche parameters using carbon and nitrogen stable isotope analysis from different body tissues. We found that caimans exploit the same carbon and nitrogen pools through time, with low isotopic variability between seasons, partly due to the slow isotope turnover rates of tissues in crocodilians. Conversely, the trophic niche of caimans varied across habitats, but with no evidence of a difference between natural and anthropogenic habitats. It apparently results from the influence of habitat suitability, connectivity, and caiman movements during the foraging. Our findings highlight the broader niches of juvenile caimans relative to adults, possibly in response of territorialism and opportunistic foraging strategy. Although using similar resources, females had a larger niche than males, probably associated with foraging strategies during nesting. Considering the sex and body size categories, caimans occupied distinct isotopic regions in some habitats, indicating apparent niche segregation. Ontogenetic trophic shifts in the isotopes (δ13C and δ15N) depended on sex, leading to resource partitioning that can potentially reduce intraspecific competition. Decision-makers and stakeholders should consider the trophic dynamics of sex and body size groups for the sustainable management and conservation of caiman populations, which implies in the maintenance of wetland habitats and landscape heterogeneity in the Formoso River floodplain.

Pre-treatment methods for stable oxygen and carbon isotope analyses of structural carbonates of bones in marine teleost fishes.

Although the proportion of structural carbonates in vertebrate bones is low, the values of isotopes, namely stable oxygen (δ18 O) and carbon (δ13 C), in structural carbonates provide environmental and physiological information, which can be beneficial for estimating the palaeontological and ecological parameters of vertebrates. However, a few studies have analysed the isotopes of structural carbonates in modern teleost fishes, and a well-developed protocol for sample preparation is lacking. We examined different pre-treatment methods of preparing bone samples of three marine teleost fishes (Japanese flounder, Pacific bluefin tuna and yellowtail) and investigated the effects of the cleaning methods on the stable isotope values of structural carbonates among vertebrae in the same individual. Isotope values were analysed using isotope ratio mass spectrometry. Physical cleaning was the most promising pre-treatment method and resulted in δ18 O values that were comparable to those of otoliths. Chemical treatments with NaOH and H2 O2 changed the percentage of structural carbonates in the bone and affected δ18 O and δ13 C values. High-temperature treatments, such as boiling and roasting, altered δ18 O values due to the exchange of oxygen with environmental water or vapour. Our results suggest that chemical cleaning methods used to prepare bone phosphate or collagen samples for isotope analyses are not suitable for structural carbonates. Physical cleaning is the appropriate pre-treatment method for analysing the isotopes of structural carbonates. Also, we emphasise that standardising the vertebral number is necessary to make δ13 C values comparable between specimens in the same species.

The food culture of the Iron Age nomadic elite from the ‘Valley of the Kings’ in Tuva: radiocarbon dating, stable carbon and nitrogen analysis of the Chinge Tey barrows (Turan-Uyuk Basin, Russia)

Subsistence strategies of Eurasian pastoral populations have been broadly studied in the archaeological literature. The 'Valley of the Kings' in Tuva, Russia, has captivated archaeologists with its remarkable collection of large burial mounds, containing lavishly equipped tombs of nomadic kings, warlords, and aristocracy. These barrows bear witness to the ancestral connections between the deceased leaders, highlighting the alliances among prehistoric nomads in Central Asia. In this research, we present comprehensive radiocarbon dating and δ13C/δ15N isotopic data from the Chinge Tey barrows, which represent the burial sites of 12 high-ranking individuals. The chronological alignment of both Chinge Tey monuments with the Arzhan 1 and Arzhan 2 reference frames sheds light on their historical context. This study delves into intricate aspects of ecological adaptability, pastoral food practices, social hierarchies, and nomadic mortuary rituals. Analysis of carbon and nitrogen stable isotopes indicates potential connections between the barrows in the 'Valley of the Kings' and diverse nomadic cultures, suggesting that dietary habits among neighboring populations may have exhibited significant variation.

Using stable carbon isotope ratio analysis to detect adulteration in red yeast rice dietary supplements

Red yeast rice (RYR) is marketed as a dietary supplement because it contains natural 3-hydroxy-3-methylglutaryl coenzyme A reductase inhibitors (statins), including monacolin K. However, there is concern that some RYR supplements may be adulterated with the pharmaceutical drug lovastatin to enhance health claims. We have developed an optimized method to isolate monacolin K/lovastatin from complex RYR dietary supplement matrices to then test for adulteration in RYR supplements using stable carbon isotope (δ13C) analysis. Samples were initially screened for monacolin K/lovastatin using liquid chromatography with mass spectrometric detection (LC-MS). To ensure the extraction process did not affect the measured isotopic values (i.e., isotopic fractionation effects), neat lovastatin standards were spiked into two types of blank RYR matrices (powder and gel). The monacolin K/lovastatin peaks were detected using high performance liquid chromatography with ultraviolet detection (HPLC-UV) and isolated using fraction collection. Residual matrix components were removed from targeted fractions by solid phase extraction (SPE) using graphitized carbon black cartridges. The resulting isolates were then analyzed using elemental analyzer-isotope ratio mass spectrometry (EA-IRMS) to measure δ13C values. The δ13C values of the extracted lovastatin standards were compared to their respective neat lovastatin δ13C values and demonstrated negligible isotopic fractionation effects. Using this optimized clean up method and carbon isotope analysis, thirty-one samples were screened. Eight RYR dietary supplement samples had >0.8 mg/g of monacolin K/lovastatin, our minimum threshold for analyzing samples using this method. Four of these eight samples had δ13C values greater than −28.3‰, a previously proposed cutoff value for natural monacolin K, indicating likely adulteration. Additionally, five RYR powder samples were analyzed as part of a collaborative study using in-house methods from two laboratories and the data shows acceptable agreement in the δ13C values of monacolin K/lovastatin (differences ranging from ±0.02‰ to ±0.76‰). This optimized method represents a robust, reproducible procedure for detecting lovastatin adulteration in dietary supplements with minimal isotopic fractionation.

Weak seasonality in benthic food web structure within an Arctic inflow shelf region

The Arctic Ocean is characterized by pronounced seasonality in the quantity and quality of organic matter exported from the surface ocean. While it is well established that changes in food availability can alter the abundance, biomass and function of benthic organisms, the impact on food web structure is not well studied. We used bulk carbon and nitrogen stable isotope analysis to assess the quantity and quality of sediment organic matter and structure of the benthic food web in four seasons within the Northern Barents Sea (76°N − 82 °C). Despite a highly seasonal vertical flux, we found that the organic carbon and chlorophyll-a content of surface sediments was seasonally stable, suggesting a lack of seasonality in food availability at the seafloor. However, organic biomarkers indicate that the quality of sediment organic matter increased to a maximum in August and December, up to 6 months after the spring bloom. The seasonal stability of food quantity was mirrored in food-web structure (e.g., total isotopic range, number of trophic levels) which did not change significantly across sampling periods. We expected that suspension and deposit feeders would respond more readily to seasonal changes in food quality compared to predators. However, we observed no significant seasonal changes in the trophic levels or isotopic niche areas of benthic functional groups. The centroids of isotopic niches of all benthic functional groups shifted seasonally by <2 ‰ along the δ13C-axis, suggesting minimal shifts in carbon resource use. Because the northern Barents Sea experiences significant changes in seasonal sea ice cover, we expected that stable-isotope ratios of benthic organisms would show an increased consumption of sympagic-derived organic matter through less negative δ13C values in early spring and summer. However, only two taxa (the soft coral Gersemia spp. and bivalves in the family Yoldiidae) showed 13C-enrichment in spring or summer consistent with the assimilation of sympagic-derived organic matter, despite previous evidence suggesting widespread use of this carbon source. Overall, our results show that there is an apparent de-coupling in time between pelagic processes and benthic food-webs in which the accumulation and assimilation of high-quality organic matter occurs for benthos during the fall and early winter months when there is little to no fresh organic matter generated at the surface. This temporal mismatch highlights the importance of considering the timescales over which components of the marine ecosystem respond to short-term environmental changes and the methods employed to assess seasonality.