Search Results (828)

Mass spectrometry-based lipidomics has created new opportunities to investigate the role of lipids in coffee quality formation and stability across the production chain. Coffee lipids contribute to flavor precursor formation, aroma release, mouthfeel, and storage behavior, but their molecular remodeling during maturation, processing, roasting, and storage remains insufficiently integrated. This review summarizes recent progress in lipidomics methodologies relevant to coffee research, with emphasis on sample preparation, mass spectrometry platforms, data analysis, and the strengths and limitations of current lipid annotation strategies. It further examines how lipid profiles change during bean maturation, how they differ among coffee species and varieties, and how they are reshaped by postharvest processing, roasting, and storage. However, it is important to note that most of these associations are currently correlational rather than causal; direct evidence linking specific lipid species to particular sensory attributes remains limited. Existing studies suggest that lipid composition, rather than total lipid content alone, is more informative for understanding coffee quality differences and for identifying candidate markers associated with origin, processing method, roasting degree, and storage conditions. In particular, alterations in glycerolipids, glycerophospholipids, fatty acids, diterpenes, and other minor lipid constituents are increasingly associated with lipid oxidation, thermal degradation, and flavor-related transformations in coffee. However, current evidence is still limited by incomplete structural annotation, isomeric ambiguity, platform dependence, and the frequent gap between statistical discrimination and mechanistic validation. Future work integrating high-resolution mass spectrometry, ion mobility, targeted quantification, stable isotope tracing, sensory analysis, and multi-omics approaches will be essential to improve marker reliability and to clarify the functional roles of coffee lipids. Overall, lipidomics provides a promising framework for linking molecular composition with coffee quality control, traceability, and process optimization, although substantial work is still needed to establish mechanistic links to flavor formation. Full article

The Mega-Tsunami of March 2011 in eastern Japan caused severe damage in the coastal black pine (Pinus thunbergii) forests along the Pacific coast. To evaluate post-disturbance forest recovery, tree-ring samples from 30 trees at Ishinomaki coastal forest were analyzed for the period 2006–2020 using tree-ring indices and stable carbon isotope discrimination (Δ¹³C). The results revealed a strong decline in radial growth immediately after the tsunami, indicating severe growth suppression during the years 2011–2014. Simultaneously, Δ¹³C values decreased, suggesting reduced stomatal conductance and acute physiological stress associated with the initial salinity effect at the root zone. Although isotopic signals indicated gradual physiological adjustment in subsequent years, radial growth recovery occurred more slowly. Most trees returned to pre-disturbance growth levels within approximately 3–5 years and later exceeded pre-disturbance growth levels, likely due to reduced competition following the mortality of nearly 40% of trees after the tsunami. However, recovery trajectories differed markedly among individual trees, with some trees showing prolonged growth suppression beyond 6 years. This variability may reflect highly localized or tree-level factors, including intrinsic differences in individual resilience, while spatial autocorrelation analysis did not indicate significant clustering of recovery time across the stand. We conclude that black pine coastal forests show a high degree of resilience, showing physiological recovery in a short period (3–4 years). Although growth recovery took longer, initial tree mortality promoted the growth of the surviving trees beyond pre-disturbance values. Full article

Freshwater mussels (Bivalvia, Unionidae) are now among the world’s most imperiled taxonomic groups, and their diversity is under serious threat. The metamorphosis of glochidia parasitizing on a host fish into juveniles is undoubtedly the most unique and critical stage in the life cycle of freshwater mussels, but the underlying mechanisms remain unclear. Here, we integrated microscopic observation, stable isotope (δ¹³C and δ¹⁵N) tracing, and transcriptomic analysis to investigate this process in the globally distributed freshwater mussel Sinanodonta woodiana on yellow catfish (Pelteobagrus fulvidraco). Compared with glochidia, juveniles exhibited byssus abandonment and the formation of a foot, visceral mass, and new shell. The shell length (0.34 ± 0.02 mm) and height (0.31 ± 0.01 mm) of the juveniles were both larger than those of the glochidia (0.26 ± 0.01 mm and 0.30 ± 0.01 mm, respectively) (p < 0.05); however, this growth likely occurred after excystment from the host fish rather than during the parasitic phase. Juveniles showed significantly higher δ¹³C (−17.70 ± 0.26‰) and δ¹⁵N (9.80 ± 0.90‰) than glochidia (δ¹³C: −23.58 ± 0.63‰; δ¹⁵N: 6.18 ± 0.37‰) (p < 0.05), with juvenile δ¹⁵N comparable to host fish tissues. Metamorphosis generated 12,584 differentially expressed genes, mainly enriched in upregulated neuroactive ligand–receptor interaction, Ras signaling, and calcium signaling pathways. This study reveals the mechanisms of S. woodiana metamorphosis, providing valuable insights for improving breeding and thus supporting the diversity conservation of freshwater mussels. Full article

Microplastic (MP) pollution is an emerging environmental stressor in marine ecosystems, yet its relationship with trophic ecology remains poorly understood in deep-sea environments. This study investigated MP ingestion in relation to trophic ecology in three deep-sea fish species (Chlorophthalmus agassizi, Hoplostethus mediterraneus, and Coelorinchus caelorhincus) from the central Tyrrhenian Sea (Western Mediterranean). Stable isotope analysis (δ¹³C and δ¹⁵N) was combined with detailed characterisation of ingested MPs to assess trophic niches, trophic position, and species-specific ingestion patterns. The three species showed distinct isotopic signatures, with C. agassizi occupying a lower trophic position, while H. mediterraneus and C. caelorhincus overlapped at higher trophic levels. MPs were detected in all species, with an overall frequency of occurrence of 34.4%, and no significant interspecific differences in occurrence or abundance were observed. However, significant differences emerged in MP characteristics. C. caelorhincus, which exhibited the widest isotopic niche, ingested larger and more diverse particles, whereas C. agassizi showed lower occurrence but higher particle loads in affected individuals. These results suggest that trophic ecology is not clearly associated with MP ingestion rates but may influence the size and diversity of ingested particles, highlighting ecological drivers of exposure in deep-sea ecosystems. Full article

The geographical origin fraud of tea is a serious challenge faced by the global tea market. This review systematically sorts out the full chain technical system from analysis and detection to data analysis in the field of tea origin traceability, reviews the traceability mechanism and application boundaries of four core technologies including stable isotopes, mineral element fingerprints, spectroscopy and mass spectrometry metabolomics, and emerging sensors, reveals the differential masking effect of the processing techniques of the six major tea types on chemical fingerprints, and systematically analyzes the methodological evolution of chemometrics and machine learning in origin discrimination. This article provides a systematic reference for understanding the overall pattern of the tea origin traceability technology system and the selection of differentiated traceability strategies for different tea types. Full article

Marginal lacustrine systems are highly sensitive archives of hydrological fluctuations, climatic variability, and changes in sediment supply in continental basins. The Alagöz Formation (Late Miocene–Pliocene) exposed in the Haymana–Polatlı Basin, Central Anatolia, was investigated through integrated sedimentological, mineralogical, geochemical, and stable isotope analyses to constrain provenance, weathering history, and lacustrine hydrological variability. Facies analysis reveals a transition from alluvial–fluvial systems to a shallow marginal lacustrine environment subjected to short-term hydrological fluctuations. Mineralogical and geochemical data indicate that sedimentation occurred within a mixed carbonate–siliciclastic lacustrine system controlled by variable lake-water chemistry. Detrital mineral assemblages indicate contributions from metamorphic source rocks. Trace-element and REE signatures suggest derivation mainly from felsic-to-intermediate continental sources. Reworked carbonate fragments and fossil debris indicate recycling of older carbonate units. The occurrence of calcite, dolomite, and protodolomite reflects variable Mg/Ca ratios, whereas clay mineral assemblages record shifts between detrital input during relatively humid phases and chemically concentrated conditions. Palygorskite occurrence indicates localized and episodic alkaline conditions associated with short-lived evaporative concentration. Weathering indices (CIA, CIW, PIA, and ICV) suggest low-to-moderate chemical weathering and compositionally immature sediments, consistent with transitional humid to semi-arid climatic conditions. Trace-element systematics also indicate a minor mafic contribution to the detrital source. Stable isotope values (δ¹³C: −7.05‰ to +2.82‰; δ¹⁸O: −8.60‰ to −2.94‰ VPDB) and their weak correlation (r = 0.34) support a shallow, hydrologically dynamic lacustrine system dominated by freshwater input but episodically influenced by evaporative concentration. Taken together, the Alagöz Formation records a sensitive marginal lacustrine system shaped by short-term hydrological fluctuations. These findings provide a useful analog for understanding hydrologically sensitive marginal lacustrine systems developed in post-collisional continental basins under fluctuating semi-arid climatic conditions. Full article

As part of a fundamental and comprehensive monitoring and conservation of the tomb of Emperor Otto the Great in the cathedral of Magdeburg, the question of the provenance of the marble cover slab of the sarcophagus was investigated. Within the restoration activities, two samples of the slab were taken for scientific provenance analyses, one sample of the white marble and another of the irregular grey bands. The following investigations were used for this purpose: analysis of the stable isotopes of O and C, and chemical analysis of a large number of trace elements, resulting in a large number of variables. For the simultaneous evaluation of these numerical results, statistical multivariate analysis was used for comparing the results with our database of approximately 7000 samples from ancient marble quarries and the data being referenced in this investigation are published and listed here. The results obtained clearly identify the quarries of Prokonnesos in the Sea of Marmara as the most probable source of the examined slab. This is in perfect agreement with petrographic analyses carried out on these samples. Full article

High-fluoride (F⁻) groundwater is a widespread environmental problem that poses significant risks to human health in many regions worldwide. Understanding the origin, circulation, and evolution of fluoride-rich groundwater is therefore essential for effective groundwater management and mitigation strategies. In recent years, stable isotope techniques have helped to address key gaps in understanding the hydrogeochemical processes governing F⁻ enrichment, particularly regarding the source identification and water-rock interaction mechanisms that remain poorly constrained. This study reviews the applications of hydrogen–oxygen, strontium–calcium, and lithium–boron isotopes in research on high-F⁻ groundwater systems. Hydrogen and oxygen isotopes (δ²H and δ¹⁸O) are widely used to identify groundwater recharge sources, mixing processes, and evaporative effects, thereby providing key constraints on the origin of fluoride-rich groundwater. Strontium and calcium isotopes (⁸⁷Sr/⁸⁶Sr and δ^44/40Ca) serve as effective tracers of water-rock interactions and associated hydrogeochemical processes, including mineral weathering and dissolution, cation exchange, and secondary mineral precipitation, which play critical roles in fluoride mobilization and enrichment. In addition, lithium, and boron isotopes (δ⁷Li and δ¹¹B) provide valuable insights into the influence of geothermal fluids and deep hydrothermal processes on fluoride accumulation in groundwater systems. Overall, the integrated application of these stable isotope systems offers a robust framework for elucidating the formation mechanisms and evolutionary pathways of high-F⁻ groundwater. Moving beyond qualitative source identification, future research should prioritize the development of Bayesian isotope mixing models that explicitly quantify uncertainty in fluoride source apportionment and utilize sensitivity analysis to test competing hydrogeochemical mechanisms. Full article

Ophicarbonates provide an important natural record of mineral carbonation during serpentinization of ultramafic rocks and therefore offer insight into the mechanisms and limits of CO₂ fixation in low-temperature geological environments. This paper presents a synthesis and process-oriented reinterpretation of stable-isotope published and previously unpublished data, petrographic, and mineralogical evidence for carbonate formation under fluid-limited serpentinization conditions. Using mineralogical constraints together with a compiled δ¹³C–δ¹⁸O dataset that includes legacy measurements from the 1980s–1990s, we evaluate how multi-stage carbonate precipitation reflects evolving water–rock ratio, redox state, transport limitation, and deformation-controlled permeability. Particular attention is given to systematic differences between vein-hosted carbonates and dispersed intergranular or scattered-grain ophicarbonates, as these textural–isotopic relationships help identify fluid flux, carbon source, and reaction progress in ultramafic systems. The analysis shows that carbonation does not proceed uniformly but is restricted to overlapping reactive windows controlled by fluid availability, nucleation kinetics, and permeability evolution. These constraints help explain why carbonation may either intensify or stall during progressive serpentinization. The Author further discuss why kinetic barriers and Mg–Ca partitioning may redirect carbonate mineralogy toward calcite or metastable Mg-rich phases even where dolomite or magnesite may be thermodynamically favored. The results highlight the importance of coupling isotopic signatures with petrographic context in reconstructing carbonation pathways and provide a broader framework for understanding natural mineral sequestration of carbon in heterogeneous serpentinite systems. Full article

The Idrija mercury deposit represents one of the largest mercury formations globally, ranking second only to the Almadén deposit in Spain. The deposit has been exploited for more than five centuries and represents one of the most historically significant and extensively studied mercury mines worldwide. The Karoli orebody is characterized by a high abundance of pyrite (50 to 90 vol.% of the rock) and exceptionally rich cinnabar mineralization, with contents reaching up to 78 wt.% Hg locally. This study investigates the trace-element composition of Py3 pyrite from the Karoli orebody using LA-ICP-MS analysis to examine variations within Py3 pyrite, revealing insights into ore-forming processes and mineralization characteristics. Trace-element analysis of pyrite was performed and complemented by microscopic examination of thin sections. Three different pyrite types were identified: fine-grained framboidal Py1, subhedral to euhedral Py2, and larger, well-developed euhedral Py3. LA-ICP-MS analysis of Py3 pyrite grain revealed low trace-element contents, with maximum values remaining below 100 ppm. These observations, combined with published sulfur and mercury isotope data, suggest that Py3 pyrite crystallized under stable growth conditions from mercury-rich, low-salinity hydrothermal fluids. Our research provides insights into Py3 pyrite formation and the characteristics of the hydrothermal fluids in the Karoli orebody, serving as a solid foundation for further studies. Future research is envisioned to include the analysis of Py2 grains to complement the current dataset, with further investigations of fluid composition, salinity, and fluid inclusions. Full article

8-Hydroxy-dihydroergotamine is the major human metabolite of the anti-migraine drug dihydroergotamine and is required, along with a stable isotope-labelled derivative, to aid metabolic studies. An efficient, scalable synthesis of the unlabelled compound is described via the coupling of dihydrolysergic acid to the tricyclic amino compound (2R,5S,8R,10aS,10bS)-2-amino-5-benzyl-10b-hydroxy-8-methoxy-2-methyltetrahydro-8H-oxazolo[3,2-a]pyrrolo[2,1-c]pyrazine-3,6(2H,5H)-dione. The tricycle was obtained by a convergent synthesis combining precursors from suitably protected L-glutamic acid and L-phenylalanine, and 2-bromo-2-methylmalonic acid. For the labelled molecule, the tricyclic precursor contained a pentadeutero benzyl group derived from [2,3,4,5,6-²H₅]L-phenylalanine. Considerable experimentation was required to achieve optimal activation of dihydrolysergic acid for efficient amide formation with the tricycle’s amino function affording 8-methoxy-dihydroergotamine. The stereochemical integrity of an intermediate in this synthesis, ethyl (2R,5S,8R,10aS)-5-benzyl-10b-hydroxy-8-methoxy-2-methyl-3,6-dioxooctahydro-8H-oxazolo[3,2-a]pyrrolo[2,1-c]pyrazine-2-carboxylate, was validated by crystal structure analysis. Acid-catalysed hydrolysis of 8-methoxy-dihydroergotamine gave 8-hydroxy-dihydroergotamine. Pentadeuterated 8-hydroxy-dihydroergotamine was obtained in an analogous manner from [2,3,4,5,6-²H₅]L-phenylalanine. Both 8-hydroxy-dihydroergotamine and its ²H₅-derivative were obtained as an equilibrating mixture of C-8 epimers (diastereomers), with the major isomer having (R)-configuration according to ¹H NMR analysis. The syntheses described enable the routine synthesis of 50–100 mg quantities of each target molecule. Full article

Stable oxygen isotopes (δ¹⁸O) in wood provide integrative records of plant water use and regional hydroclimatic processes, offering a powerful framework for spatial ecological analysis in tropical forests. Here, we present the first regional-scale δ¹⁸O isoscapes for Amazonian wood based on 387 trees sampled across 25 sites. After α-cellulose extraction, δ¹⁸O values were modeled using multiple linear regression (MLR) and Random Forest (RF) approaches. A Moran’s I test revealed no significant spatial autocorrelation (p = 0.73), indicating that geostatistical interpolation methods such as kriging were not appropriate for this dataset. The MLR model based on site-average data achieved an R² of 0.70, with a mean absolute error (MAE) of 0.56‰ and root mean square error (RMSE) of 0.68‰. The RF model showed comparable performance (R² = 0.67; MAE = 0.64‰; RMSE = 0.77‰). Both approaches reproduced a coherent southeast-to-northwest gradient, with lower δ¹⁸O values in the western Amazon and higher values in the east, consistent with regional patterns in precipitation isotopic composition and evapotranspiration. These findings demonstrate that climate-driven statistical modeling effectively captures large-scale isotopic structure across the Amazon basin, providing a robust spatial representation of δ¹⁸O variability in tropical forest wood. Full article

Background/Objectives: Oral squamous cell carcinoma (OSCC) exhibits substantial biological heterogeneity, and current clinicopathological risk stratification incompletely reflects tumor metabolic behavior. Stable isotope ratio mass spectrometry enables the quantitative assessment of carbon and nitrogen isotopic composition, potentially capturing cumulative metabolic reprogramming associated with tumor aggressiveness. This study evaluated whether isotopic signatures of tumor tissue and surgical margins are associated with lymph node metastasis and survival outcomes in OSCC. Methods: In this prospective study, 54 consecutive patients undergoing primary surgical treatment for OSCC were enrolled. Paired samples derived from tumor tissue and surgical margins were analyzed using isotope ratio mass spectrometry to determine the relative abundance of nitrogen-15 and carbon-13 isotopes. The primary endpoint was pathological lymph node metastasis. Secondary endpoints included disease-free survival and overall survival. Paired comparisons were performed using Wilcoxon signed-rank tests with false discovery rate correction. Logistic regression models for nodal metastasis were constructed using Firth penalization with bootstrap internal validation, while survival outcomes were evaluated using Cox proportional hazards models with model complexity restricted according to the number of events. Results: Tumor tissues demonstrated significantly lower δ¹³C and δ¹⁵N values and higher nitrogen-to-carbon ratios compared with surgical margins (all adjusted p < 0.05). In multivariable analysis, tumor δ¹⁵N was independently associated with lymph node metastasis and modestly improved model discrimination. However, it was not independently associated with disease-free or overall survival. Exploratory analyses indicated that higher δ¹³C values in surgical margins were independently associated with shorter disease-free survival. Conclusions: These findings suggest that isotope ratio mass spectrometry-based isotopic profiling identifies reproducible metabolic differences between tumor and margin tissues in OSCC. Tumor δ¹⁵N is associated with lymph node metastasis, whereas margin δ¹³C may reflect recurrence risk and potentially capture metabolic field effects. These findings are hypothesis-generating and warrant validation in larger, independent cohorts. Full article

Natural mineral waters hosted in volcanic terrains are globally significant, but the co-enrichment mechanisms of metasilicate and strontium remain poorly understood. Here we investigate a Jurassic volcanic-hosted mineral water source in eastern China using hydrochemical analysis, ¹⁴C dating, stable isotopes, and structural analysis. The groundwater is of Ca–Mg–HCO₃ type with slightly alkaline pH (7.44–7.63). Metasilicate (26.4–32.9 mg/L) and strontium (0.40–0.83 mg/L) co-enrichment is governed by plagioclase weathering in a bicarbonate-dominated, weakly alkaline environment where ${\mathrm{S}\mathrm{r}\mathrm{H}\mathrm{C}\mathrm{O}}_3^{+}$ ion pairs enhance strontium mobility. Pearson-corrected ¹⁴C ages of 3900–4900 years reveal that millennial-scale residence time is critical for sufficient water-rock interaction and attainment of regulatory thresholds. A conduit-barrier system formed by NW-trending extensional-shear and NNE-trending compressional-shear faults controls groundwater flow paths and residence times, leading to systematic inter-well hydrochemical differentiation. These findings provide a theoretical basis for the genetic identification, potential evaluation, and sustainable management of high-quality mineral water resources in volcanic terrains. Full article

Groundwater-dependent communities such as De Aar require a better understanding of groundwater systems to ensure sustainable allocation. This study aims to trace recharge sources in unconfined and confined aquifers and identify processes controlling groundwater quality using hydrogeochemistry and environmental tracers. It argues that aquifer delineation and hydraulic parameters alone cannot fully identify recharge sources or geochemical processes; integrating them with hydrogeochemistry and environmental tracers provides stronger evidence to support groundwater allocation. To validate the argument, the study integrated hydrogeochemical analysis, stable isotopes, tritium, radon-222, and statistical methods supported by depth-specific groundwater sampling. The results, interpreted using Piper and Gibbs diagrams, PHREEQC modelling, and scatter plots, show that groundwater evolution is mainly controlled by rock–water interaction, ion exchange, evaporation, and mixing processes. Ca–HCO₃ water indicates recent recharge, while Na–Cl water reflects evaporation effects in both unconfined and confined aquifers, with halite dissolution contributing to Na and Cl enrichment. Isotope results indicate that unconfined aquifer water is isotopically enriched and linked to recent recharge, whereas confined aquifer and spring waters are depleted, suggesting recharge from higher elevations through fractured zones. Tritium dating reveals young (<30 years), intermediate (30–50 years), and old groundwater (60–109 years), while radon results indicate active groundwater flow path, particularly along fractures. These findings demonstrate that groundwater recharge is derived from both local meteoric sources and regional contributions, resulting in predominantly fresh groundwater; however, localized quality concerns should be considered for improved water allocation. Full article