Search Results (134)

Fruity natural flavors are widely used in food, cosmetics, and tobacco products, and their flavor profiles directly affect the sensory quality of the final products. However, the volatile organic compound systems in these flavors are highly complex, and severe co-elution among volatile components makes effective component resolution a persistent analytical challenge. In this study, comprehensive two-dimensional gas chromatography–olfactometry–time-of-flight mass spectrometry (GC×GC-O-TOF-MS) was employed to separate and identify volatile odor compounds in three natural fruit flavor extracts: plum, jujube, and grape. A total of 113, 103, and 85 volatile odor compounds were identified from the plum, jujube, and grape extracts, respectively. By progressively adjusting the split ratio, aroma extract dilution analysis was performed, leading to the screening of 14, 11, and 32 aroma-active compounds from the three extracts, respectively. Compounds with high flavor dilution factors were subjected to quantitative analysis, and their odor activity values were calculated. Subsequently, omission and recombination experiments were conducted to confirm the key aroma-active compounds in each extract. The results showed that octanal was a key aroma compound shared by the plum and jujube extracts, while ethyl cinnamate was common to both the plum and grape extracts. Through a molecular sensory science approach and utilizing GC×GC-O-TOF-MS chromatographic separation technology, this study provides a reliable analytical platform for aroma characterization in complex samples. It also establishes a critical theoretical and data foundation for precisely identifying key aroma-active components and implementing targeted aroma modulation to enhance the natural flavor quality of fruits. Full article

Chemical recycling of mixed plastic waste can recover hydrocarbon products, but additive-derived non-intentionally added substances (NIASs) and other volatile or extractable residues may affect product quality and safety. In this study, six polyolefin-rich waste streams (P1–P6) were analyzed by analytical pyrolysis coupled with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (Py–GC×GC–TOF–MS), while three additional consumer-grade plastics (P7–P9) were examined by headspace/solvent-extraction GC–MS and aqueous migration testing to profile volatile organic compounds (VOCs), semi-volatile organic compounds (SVOCs), and water migrants. Under rapid pyrolysis at 650 °C, the condensable products were dominated by C5–C30 aliphatic hydrocarbons. Polyethylene (PE)-rich feeds produced mainly n-paraffins and α-olefins, whereas polypropylene (PP)-rich feeds produced more branched olefins and modest mono-aromatics. Oxygenated compounds were negligible in non-oxidized feeds, but persisted at low levels in weathered high-density polyethylene (HDPE), consistent with pre-existing oxidation. Antioxidant-derived NIASs, including 2,4-di-tert-butylphenol and an Irganox 1010-related spiro-dione, were detected at trace to low area-fraction levels. VOC/SVOC and migration analyses revealed mainly low-intensity hydrocarbons, esters, antioxidant-related degradation products, caprolactam, and selected plasticizer-related compounds. These results show that relatively clean polyolefin streams can yield hydrocarbon-rich pyrolysates, but oxidized PE and additive-derived NIASs remain important quality-control targets. The GC-based methods used here characterize the volatile, condensable, and readily extractable fraction and do not represent the total contaminant load of the source waste. Full article

Inflammation is associated with metabolic alterations that can lead to the release of volatile organic compounds (VOCs) reflecting cellular biochemical activity. Profiling these volatile metabolites may provide insight into cellular responses to inflammatory stimuli, although their characterization in skin-derived cells remains limited. In this exploratory proof-of-concept study, we investigated the volatile metabolite profiles of human skin fibroblasts exposed to different inflammatory stimuli. Fibroblast cell lines were stimulated with polyinosinic:polycytidylic acid (Poly I:C), tumor necrosis factor-alpha (TNF-α), and lipopolysaccharide (LPS) to model viral-, cytokine-, and bacterial-associated stress conditions. Headspace solid-phase microextraction coupled with comprehensive two-dimensional gas chromatography and time-of-flight mass spectrometry (HS-SPME-GC×GC-TOFMS) was applied to analyze volatile metabolites released from the cell cultures, enabling exploratory profiling of the fibroblast volatilome. A data-processing workflow including pairwise comparisons between experimental groups and statistical filtering was implemented to identify volatile features associated with the different conditions. Several VOCs were tentatively identified, mainly belonging to alcohol, ester, and hydrocarbon classes, and showed differential abundance patterns between stimulated and control samples. Multivariate analysis indicated a separation between stimulated and non-stimulated groups, suggesting stimulus-associated differences in the volatile profiles of fibroblast cultures. While these observations may reflect metabolic responses occurring under inflammatory stimulation, the chemical identity and biochemical origins of several detected features remain to be confirmed. All in all, this study demonstrates the feasibility of applying HS-SPME-GC×GC-TOFMS-based volatilome profiling to investigate stimulus-associated changes in fibroblast cultures. The detected VOC patterns should therefore be considered preliminary observations requiring further chemical characterization and independent validation. Future studies including larger sample numbers, complementary biological verification of the inflammatory response, and more physiologically relevant experimental models will be necessary to further assess the robustness and potential relevance of these volatile signatures in the context of inflammatory processes. Full article

Rapid expansion of the plant-based milk market has increased the need to understand how the aroma profiles of these alternatives differ from that of dairy milk and how raw material selection and processing influence volatile formation. This study compared the volatile profiles of dairy milk, commercial plant-based milks, and laboratory-prepared cereal and pseudocereal milk prototypes to identify promising materials for plant-based milk development. Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) combined with chemometric analysis was used to characterize volatile compounds in bovine milk, four commercial plant milks, and five laboratory-prepared plant milks. Dairy milk was characterized by fatty acids, esters, and other lipid-derived volatiles, whereas plant-based samples were associated with hydrocarbons, pyrazines, ketones, and phenols. Within the plant-based group, volatile differences were influenced by raw material type and processing history. Commercial products showed more evident processing-related features, whereas laboratory-prepared cereal samples exhibited a simpler volatile background. Among them, barley milk displayed a distinctive toasted and cereal-like signature. Overall, the selected cereal and pseudocereal matrices showed distinct volatile characteristics, as well as relatively uniform raw material backgrounds, implying greater flexibility in aroma expression. These features make them promising candidates for dairy alternatives and may help guide future plant-based milk formulation. Full article

The genus Oncosiphon (Asteraceae), consisting of aromatic herbs, is indigenous to southern Africa. Oncosiphon species have been documented in Khoi-San ethnobotany as herbal remedies for typhoid fever, pneumonia, and as diuretics. Research on the biological properties and comprehensive phytochemical profiling of these important Oncosiphon species is currently limited. This study was therefore undertaken to address the knowledge void in chemical profiling, through the application of various analytical techniques to analyse the volatile and non-volatile constituents of three South African Oncosiphon species. The aerial parts of Oncosiphon suffruticosus (n = 28), O. grandiflorus (n = 16), and O. africanus (n = 4) were collected from various locations in the Western Cape Province of South Africa. The stems and leaves (SL) were separated from the flowers (F) and analysed as distinct samples. The methanol: chloroform (1:1, v/v) extracts were prepared and analysed using ultra–high–performance liquid chromatography quadrupole time-of-flight time–of–flight mass spectrometry (UHPLC–QToF–MS) and a semi–automated high–performance thin–layer chromatography (HPTLC) system. Multivariate data analysis was performed on the UHPLC–QToF–MS data to determine interspecies chemical variation. Two-dimensional (2D) gas chromatography (GCxGC–ToF–MS) was used to determine the headspace volatile profiles of the intact aerial parts. The results show that the non-volatile profiles of the Oncosiphon species are characterised by amino acids, phenolic acids, flavonoids, sesquiterpene lactones, and fatty acid derivatives. The HPTLC profiles of O. grandiflorus and O. africanus are chemically more closely related, and O. suffruticosus has a distinct profile, which is supported by the chemometrics results of the flowers. The major headspace volatile compounds in Oncosiphon flowers are α-pinene, α-ocimene, eucalyptol, o-cymene, and artemisia alcohol, whereas the stems and leaves mainly consist of α-ocimene, eucalyptol, and yomogi alcohol. Full article

Raisin syrup sourdough is a popular traditional leavening method in Japan, yet its specific impact on bread aroma evolution and shelf life stability remains scientifically underexplored. This study characterized the fermentation dynamics and volatile profiles of raisin syrup sourdough bread compared to a commercial yeast control over a 3-day shelf life, utilizing comprehensive two-dimensional gas chromatography–mass spectrometry (GC × GC-TOFMS) and primary metabolite profiling of sugars, amino acids, and organic acids. The analysis resolved over 760 volatiles and revealed a fundamental kinetic divergence. While the yeast control exhibited a 24 h metabolic lag, the raisin sourdough achieved rapid activation, establishing a higher initial volatile load immediately post-baking. Driven by lactic acid bacteria dominance and extensive proteolysis, the sourdough’s acidic environment facilitated the retention of fruity esters and malty branched-chain aldehydes while effectively suppressing lipid oxidation markers like 9,17-Octadecadienal. Key aromatic markers, including benzenepropanol and Octanoate <isopentyl->, were significantly elevated and stabilized in the sourdough group. These findings demonstrate that raisin syrup fermentation generates a superior, stable aromatic profile, providing a scientific basis for optimizing clean-label artisan bread production in the Japanese market. Full article

The recently introduced solid-state modulator (SSM) is a compact and relatively simple all-in-one solution to thermal modulation for use in comprehensive two-dimensional gas chromatography (GC×GC). In this work, we assess the performance of this modulator through a detailed assessment of its temperature stability and temperature programming capabilities, and corresponding retention time reproducibility. Through replicate analysis, ²D retention time standard deviation was determined to be 0.014 s (ranging from 0.000–0.023 s), corresponding to less than a single acquisition datapoint. Additionally, ¹D retention time repeatability in GC×GC was assessed using a ‘super-resolution method’ designed to predict ¹D retention based on the modulated peak distribution, and was determined to be comparable to that of conventional GC-MS analysis. A benchmarking framework was developed, which can be applied to future performance evaluations of thermal and other modulators, allowing for a more systematic comparison of modulation strategies. Full article

China is the world’s largest producer of acrylic fiber, and the wastewater generated from its production contains a significant amount of biologically refractory organic pollutants. However, comprehensive screening studies on organic compounds in such wastewater remain limited, which hampers effective wastewater treatment and ecological risk management to some extent. In this study, high-resolution mass spectrometry (HRMS) was combined with comprehensive two-dimensional gas chromatography (GC×GC) and ultra-performance liquid chromatography, along with multiple characterization techniques—including proton nuclear magnetic resonance spectroscopy, infrared spectroscopy, and fluorescence spectroscopy—to qualitatively analyze organic compounds present in wastewater from four stages of wet-spun acrylic fiber production: acrylonitrile mixed wastewater, polymerization wastewater, spinning wastewater, and final mixed wastewater. The results indicated that sulfonate esters, various other esters, alkanes, heterocyclic compounds, aromatic compounds, and substances containing multiple conjugated systems were commonly present across all four sample types, potentially contributing to the poor biodegradability of the wastewater. Additionally, a higher abundance of volatile organic compounds was detected in the mixed wastewater, while acrylonitrile appeared to be more concentrated in the spinning wastewater. The complementary use of spectral analysis, proton nuclear magnetic resonance, and HRMS provided a robust analytical foundation for identifying organic pollutants in acrylic fiber production wastewater. Full article

The aroma of wine is a defining quality attribute, determined mainly by volatile organic compounds (VOCs) originating from grape metabolism, fermentation, and maturation. This study aimed to characterize the VOC composition of young monovarietal red wines from the Alentejo region (Portugal), produced from Alicante Bouschet, Touriga Nacional, and Trincadeira across five consecutive vintages (2020–2024). Headspace solid-phase microextraction (HS-SPME) coupled with comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC×GC-ToFMS) was applied for VOC profiling, followed by multivariate statistical analyses. A strict identification and reproducibility criterion was applied to ensure longitudinal consistency over the five vintages. MANOVA analysis revealed significant effects (p < 0.001) of both grape variety and vintage on VOC distribution. Esters were the most abundant and discriminant group, while aldehydes and terpenes contributed markedly to varietal differentiation. Alicante Bouschet wines were associated with fruity ethyl esters, Touriga Nacional with monoterpenes (citronellol, terpinolene, α-farnesene) and aromatic alcohols, and Trincadeira with aldehydes and sesquiterpenes. Canonical discriminant analysis (CDA) achieved clear separation among varieties and vintages, with the first two canonical functions accounting for over 70% of the total variance. Heatmap analysis highlighted distinctive terpene and C13-norisoprenoid profiles across samples. These findings demonstrate the pivotal role of VOCs in defining Alentejo wine typicity and support their use as chemical markers for authenticity and PDO valorization. Full article

To characterize the key odorants and elucidate the flavor profiles of compound fermented beverages after fermentation, single-compound fermented beverages (GW, AW) and a compound fermented beverage (CW) were prepared using Italian Riesling grapes and SirPrize apples as raw materials. The flavor and metabolite profiles were systematically analyzed by integrating flavoromics (comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry, GC × GC–TOF MS) and metabolomics (LC–MS/MS). The results demonstrated that CW exhibited the most favorable acid/reducing sugars (2.18), imparting a drier taste and superior stability. Compounds with relative odor activity values (rOAV) greater than 1—including 3-methyl-1-butyl acetate, ethyl hexanoate, ethyl butanoate, and ethyl octanoate—collectively contributed prominent fruity, floral, and sweet aromas to all three wine types. Ethyl decanoate provided an additional distinctive traditional fruity note specifically to AW, while 1-octen-3-ol contributed a mushroom-like aroma to both GW and CW. Moreover, 3-methylbutanal, 4-ethyl-2-methoxyphenol, and ethyl 3-methylbutanoate added additional significant aroma contributions to CW, imparting floral, clove-like, and fruity notes, respectively. Notably, ethyl hexanoate (fruity aroma) exhibited a remarkably high rOAV of 27.43 in CW, significantly surpassing its levels in the single-substrate fermentations. Lipid metabolism and the phenylpropanoid pathway were significantly activated in CW, facilitating the coordinated synthesis of esters and phenolic compounds. Sensory attribute network analysis further confirmed that CW possessed more pronounced “sweet”, “fruity”, and “floral” characteristics. Correlation analysis revealed significant relationships between volatile organic compounds (VOCs) and total soluble solids (TS), titratable acidity (TA), the TA/TS ratio, and metabolite levels, underscoring the close connections among physicochemical properties, precursor/intermediate metabolites, and flavor formation. Comprehensive analysis of non-volatile metabolites and flavor-associated VOCs revealed variety-specific characteristics and compounding effects, providing valuable insights for enhancing the quality of compound fermented beverages. Full article

This study investigated the effects of three cooking methods—fragmenting process (FP), boiling treatment (BT), and high-pressure steam (HPS) treatment—on the structure and volatile compounds (VOCs) of fresh Lyophyllum decastes. The surface morphology and functional groups of L. decastes were analyzed by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The VOCs in L. decastes were analyzed by comprehensive two-dimensional gas chromatography–mass spectrometry (GC×GC-MS) and gas chromatography–ion mobility spectrometry (GC-IMS). SEM results showed that HPS resulted in the most pronounced structural disruption, forming a honeycomb-like porous surface, whereas FP yielded smaller fragments with smoother surfaces. FTIR spectra indicated that none of the treatments significantly altered the characteristic functional groups. A total of 73 VOCs were identified by GC×GC-MS, including 23 hydrocarbons, 14 alcohols, 10 ketones, seven aldehydes, six ethers, three esters, two terpenes, and eight other compounds. Additionally, 22 VOCs were identified by GC-IMS, including seven alcohols, six aldehydes, five esters, three ketones, and one other compound. The four compounds benzaldehyde, benzeneacetaldehyde, (E)-2-hexen-1-ol, and 1-hexanal were detected by both methods. Among the three methods, FP induced the least structural damage and better preserved the VOCs. These results offer theoretical insights and technical support for the flavor-oriented deep processing of L. decastes. Full article

Dietary intake is the major route of human exposure to fat-soluble and persistent chlorinated paraffins (CPs), which tend to accumulate in lipid-rich foods such as edible vegetable oils. This study investigated the levels of short-chain (SCCPs) and medium-chain chlorinated paraffins (MCCPs) in commercially available vegetable oils and assessed their potential health risks. The concentrations of SCCPs and MCCPs in 29 commercial edible vegetable oils were analyzed using comprehensive two-dimensional gas chromatography coupled with electron capture negative ionization mass spectrometry (GC × GC-ECNI-MS). Dietary exposure levels were estimated through probabilistic assessment integrating analytical results with dietary consumption data from the Chinese Total Diet Study (2017–2020). The margin of exposure (MOE) approach was employed for risk characterization. The average concentrations of SCCPs and MCCPs were 112 ng/g and 139 ng/g, respectively. The highest SCCP and MCCP concentration were found in sesame oil and peanut oil, respectively. Overall, MCCPs levels were generally higher than SCCPs. The estimated daily intakes (EDIs) of SCCPs and MCCPs were 56.06 and 73.63 ng/kg bw/d on average, with high consumers (P95) exposed to 180.91 and 230.49 ng/kg bw/d, respectively. Corresponding MOE at P95 were 1.27 × 10⁴ for SCCPs and 1.56 × 10⁵ for MCCPs. The current SCCPs and MCCPs dietary intake originated from edible vegetable oils did not pose a significant health risk. This study provides the first probabilistic exposure assessment of CPs in Chinese edible vegetable oils, offering current contamination profiles. Full article

This study examines the swelling behaviour of nitrile-butadiene rubber (NBR) when interacting with tyre pyrolysis oils (TPO), with a focus on the chemical composition of TPO and their interaction with rubber matrices. Initially, a comparative analysis with conventional diesel fuel (DF) was performed using advanced analytical techniques, including two-dimensional gas chromatography coupled to mass spectrometry (2D-GC/MS), infrared (IR) spectroscopy, and nuclear magnetic resonance (¹H-NMR) spectroscopy. The analysis revealed that TPO contains a significantly higher proportion of aromatic hydrocarbons than DF, along with unsaturated and oxygen-containing compounds not present in DF. Based on these compositional differences, blends of TPO and DF were formulated and evaluated for their suitability as liquid energy carriers according to the specifications of DF. In principle, blends with an addition of up to 5 vol% TPO in DF are technically suitable for use as fuel. Subsequently, the sorption behaviour of TPO, DF, and their blends in NBR was investigated. The swelling potential was determined based on mass, density, and volume, and the changes in the hardness and tensile strength of NBR were recorded. The results demonstrate that TPO induces pronounced swelling in NBR, as evidenced by a marked increase in mass uptake and volume expansion. A linear increase was observed between the degree of swelling and the increasing TPO content in the blends. Mechanical property assessments revealed a corresponding decrease in the hardness and tensile strength of NBR upon exposure to TPO, with the most severe effects associated with neat TPO. This work provides a comprehensive assessment of TPO as a potential blend component for DF. It highlights the need for careful consideration of material compatibility in practical applications. Full article

With the increasing consumption of mulberry fruits in commercial markets, flavor profiles have emerged as critical determinants of consumer preference and market acceptance. This investigation utilized four Morus laevigata (Morus L.) accessions exhibiting pronounced variations in fruit pigmentation and flavor characteristics as experimental materials. Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOF MS) was employed to identify key volatile aromatic compounds, while integrated untargeted metabolomics and transcriptomics approaches were applied to elucidate the underlying mechanisms of flavor biosynthesis. Analysis revealed that aldehydes, ketones, lactones, and heterocyclic compounds constitute the primary volatile organic compounds responsible for M. laevigata flavor complexity. The biosynthesis of these volatile aromatic compounds exhibits a direct correlation with lipid metabolite oxidation pathways. Concurrently, oxidative processes are modulated by M. laevigata flavonoid metabolites with antioxidant properties, which subsequently regulate both the compositional profile and quantitative distribution of volatile aromatic compounds. These findings offer novel insights into the metabolite–volatile compound interactions within mulberry systems, establishing a foundational framework for advancing fruit flavor research and cultivar development programs. Full article

Sperm membrane lipids play a crucial role in male fertility, influencing sperm motility, viability, and functional competence. This study comprehensively characterizes the phospholipid and sphingolipid composition in highly motile human spermatozoa obtained through the swim-up method, a widely used technique in assisted reproductive technology (ART). Using two-dimensional thin-layer chromatography and phosphorus analysis, we identified choline glycerophospholipids (CGP, 45%), ethanolamine glycerophospholipids (EGP, 26%), and sphingomyelin (SM, 17%) as predominant phospholipids, with minor components including cardiolipin, lysophospholipids, phosphatidylinositol, phosphatidylserine, phosphatidic acid, and neutral lipids. Gas chromatography analysis of glycerophospholipids (GPL) revealed a high long chain (C20–C22) polyunsaturated fatty acids (PUFA) content (46.3%), particularly docosahexaenoic acid (DHA, 22:6n-3), which was more abundant in CGP (46%) than EGP (26%). Sphingolipid analysis indicated that ceramide (Cer) and SM shared similar fatty acid profiles due to their metabolic relationship, with very-long-chain (VLC) PUFA (≥C26) being more prevalent in SM (10%) than in Cer (6%). Additionally, argentation chromatography identified highly unsaturated VLCPUFA species in Cer, including 28:3n-6, 28:4n-6, and 30:4n-6, which had not been previously quantified in motile human spermatozoa. Given the essential function of sphingolipid metabolism in spermatogenesis, capacitation, and acrosomal exocytosis, our findings suggest that the balance of VLCPUFA-containing SM and Cer could play a role in sperm performance and fertilization potential. This study provides novel insights into the lipid signature of human sperm and highlights the relevance of membrane lipid remodeling for male fertility and ART outcomes. Full article