Search Results (355)

Knowledge about the composition (volatile and non-volatile) and functionality of natural extracts from Mediterranean plants serves as a basis for their further application. In this study, five selected plants were used for the extraction of plant metabolites. Leaves and flowers of Critmum maritimum, Rosmarinus officinalis, Olea europea, Phylliera latifolia and Mellisa officinalis were collected, and a total of 12 extracts were prepared. Extractions were performed under microwave-assisted conditions, with two solvent types: water (W) and a hydroalcoholic (ethanolic) solution (HA). Detailed extract analysis was conducted. Phenolics were analyzed by detecting individual bioactive compounds using high-performance liquid chromatography and by calculating total phenolic and total flavonoid content through spectrophotometric analysis. Higher concentrations of total phenolics and total flavonoids were obtained in the hydroalcoholic extracts, with the significantly highest total phenolic and flavonoid values in the rosemary hydroalcoholic extract (3321.21 mg_GAE/L) and sea fennel flower extract (1794.63 mg_QE/L), respectively; and the lowest phenolics in the water extract of olive leaves (204.55 mg_GAE/L) and flavonoids in the water extracts of sea fennel leaves, rosemary, olive and mock privet (around 100 mg_QE/L). Volatile organic compounds (VOC) were detected using HS-SPME/GC–MS (Headspace Solid-Phase Microextraction coupled with Gas Chromatography-Mass Spectrometry), and antioxidant capacity was estimated using DPPH (2,2-diphenyl-1-picrylhydrazyl assay) and FRAP (Ferric Reducing Antioxidant Power) methods. HS-SPME/GC–MS analysis of samples revealed that sea fennel had more versatile profile, with the presence of 66 and 36 VOCs in W and HA sea fennel leaf extracts, 52 and 25 in W and HA sea fennel flower extracts, 57 in rosemary W and 40 in HA, 20 in olive leaf W and 9 in HA, 27 in W mock privet and 11 in HA, and 35 in lemon balm W and 10 in HA extract. The lowest values of chlorophyll a were observed in sea fennel leaves (2.52 mg/L) and rosemary (2.21 mg/L), and chlorophyll b was lowest in sea fennel leaf and flower (2.47 and 2.25 mg/L, respectively), while the highest was determined in olive (6.62 mg/L). Highest values for antioxidant activity, determined via the FRAP method, were obtained in the HA plant extracts (up to 11,216 mg_AAE/L for lemon balm), excluding the sea fennel leaf (2758 mg_AAE/L) and rosemary (2616 mg_AAE/L). Considering the application of these plants for fresh fish preservation, antimicrobial activity of water extracts was assessed against Vibrio fischeri JCM 18803, Vibrio alginolyticus 3050, Aeromonas hydrophila JCM 1027, Moraxella lacunata JCM 20914 and Yersinia ruckeri JCM 15110. No activity was observed against Y. ruckeri and P. aeruginosa, while the sea fennel leaf showed inhibition against V. fisheri (inhibition zone of 24 mm); sea fennel flower was active against M. lacunata (inhibition zone of 14.5 mm) and A. hydrophila (inhibition zone of 20 mm); and rosemary and lemon balm showed inhibition only against V. fisheri (inhibition zone from 18 to 30 mm). This study supports the preparation of natural extracts from Mediterranean plants using green technology, resulting in extracts rich in polyphenolics with strong antioxidant potential, but with no clear significant antimicrobial efficiency at the tested concentrations. Full article

Tomatoes are globally esteemed not only for their nutritional value but also for their complex and appealing aroma, a key determinant of consumer preference. The present study aimed to comprehensively characterise the volatilomic fingerprints of three tomato species—Solanum lycopersicum L., S. lycopersicum var. cerasiforme, and S. betaceum—encompassing six distinct varieties, through the application of headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS). A total of 55 volatile organic compounds (VOCs) spanning multiple chemical classes were identified, of which only 28 were ubiquitously present across all varieties examined. Carbonyl compounds constituted the predominant chemical family, with hexanal and (E)-2-hexenal emerging as putative key contributors to the characteristic green and fresh olfactory notes. Notably, esters were found to dominate the unique volatile fingerprint of cherry tomatoes, particularly methyl 2-hydroxybenzoate, while Kumato and Roma varieties exhibited elevated levels of furanic compounds. Multivariate statistical analyses, including principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA), demonstrated clear varietal discrimination and identified potential aroma-associated biomarkers such as phenylethyl alcohol, 3-methyl-1-butanol, hexanal, (E)-2-octenal, (E)-2-nonenal, and heptanal. Collectively, these findings underscore the utility of volatilomic fingerprint as a robust tool for varietal identification and quality control within the food industry. Full article

The garden Nasturtium (Tropaeolum majus L.) is increasingly consumed worldwide due to its culinary appeal and perceived health benefits. However, the chemical markers underlying its functional properties remain insufficiently characterized. Building on evidence from a recent human pilot study confirming both high acceptability and dietary safety, we conducted a comprehensive volatilomic and phytochemical analysis of T. majus flowers and their juice. Headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS) was employed to establish the volatilomic fingerprint of floral tissues and juice. Our analysis revealed a striking dominance of benzyl isothiocyanate and benzonitrile, which together accounted for 88% of the total volatile organic metabolites (VOMs) in the juice, 67% and 21%, respectively. In the floral tissues, benzyl isothiocyanate was even more prevalent, representing 95% of the total volatile profile. Complementary in vitro assays confirmed a substantial total phenolic content and strong antioxidant activity in the flowers. These findings provide a robust chemical rationale for the potential health-promoting attributes of T. majus, while identifying key volatilomic markers that could support future functional and safety claims. In parallel, a benefit–risk assessment framework is discussed in accordance with the European Food Safety Authority (EFSA) guidelines for the Qualified Presumption of Safety (QPS) of edible flowers. Given that both benzyl isothiocyanate and benzonitrile are classified as Cramer Class III substances, a conservative intake threshold of 1.5 μg/kg body weight per day is proposed. To enable quantitative exposure modeling and support the derivation of a tolerable daily intake (TDI), future studies should integrate organic solvent-based extraction methodologies to estimate the total volatile load per gram of floral biomass. This would align risk–benefit assessments with the EFSA’s evolving framework for novel foods and functional ingredients. Full article

Clove essential oil (Eugenia caryophyllata essential oil, ECEO) is known for its high eugenol content and notable antimicrobial properties. However, the volatility and instability of its active compounds hinder broader pharmaceutical applications. Methods: This study characterised the chemical composition of ECEO and comparatively evaluated four β-cyclodextrin (β-CD) encapsulation methods: kneading, co-precipitation, lyophilisation, and co-precipitation–lyophilisation for eugenol, eucalyptol, and ECEO. Encapsulation efficiency, physicochemical properties, and antimicrobial potential were assessed. Analytical techniques included Gas Chromatography–Mass Spectrometry (GC-MS), Headspace GC-MS (HS-GC-MS), Differential Scanning Calorimetry (DSC), Job’s method, and Dynamic Light Scattering (DLS). Results: GC-MS identified eugenol (90.67%), eugenyl acetate (4.77%), and (E)–β-caryophyllene (3.98%) as major components of ECEO, while HS-GC-MS indicated a slightly reduced eugenol content (86.46%). The kneading method yielded the highest encapsulation efficiency for eugenol, whereas the co-precipitation–lyophilisation method was optimal for eucalyptol. DSC thermograms confirmed complex formation, and DLS analysis revealed nanostructures averaging 186.4 nm in diameter (PDI = 0.298). Antimicrobial assays showed MIC values ranging from 0.039 mg/mL to 10,000 mg/mL. Notably, ECEO and its β-CD complex displayed enhanced efficacy against Escherichia coli (0.039 mg/mL), surpassing the reference antibiotic gentamicin (0.049 mg/mL). Conclusions: β-Cyclodextrin encapsulation significantly enhances the stability and bioactivity of volatile antimicrobial compounds, thereby supporting their potential integration into advanced essential oil-based pharmaceutical formulations. Full article

Wuyi Shuixian tea, a premium oolong tea known for its complex floral-fruity aroma, exhibits significant quality variations across different grades. This study systematically analyzed the aroma characteristics and key fragrant compounds of four grades (Grand Prize SA, First Prize SB, Outstanding Award SC, and Non-award SD) using headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS), odor activity value (OAV) analysis, and multivariate statistical methods. A total of 159 volatile compounds were identified, with similar compound categories but distinct concentration gradients between grades. OAV-splitting analysis (based on OAV ≥ 1 as the threshold for aroma activity) identified β-ionone (fruity), octanal (fatty), and linalool (floral) as core aroma-active contributors, as their OAV values significantly exceeded 10 in awarded grades (SA, SB, SC), indicating dominant roles in sensory perception. Notably, linalool, a floral marker, showed a concentration gradient (SA > SB > SC) and was absent in SD, serving as a critical determinant of grade differentiation. Orthogonal partial least squares-discriminant analysis (OPLS-DA) further distinguished awarded grades (SA, SB, SC) by balanced fruity, floral, and woody notes, while SD lacked floral traits and exhibited burnt aromas. This classification was supported by hierarchical clustering analysis (HCA) of volatile profiles and principal component analysis (PCA). Electronic nose data validated these findings, showing strong correlations between sensor responses (W5S/W2W) and key compounds like hexanal and β-ionone. This study elucidates the molecular basis of aroma-driven quality grading in Wuyi Shuixian tea, providing a scientific framework for optimizing processing techniques and enhancing quality evaluation standards. The integration of chemical profiling with sensory attributes advances precision in tea industry practices, bridging traditional grading with objective analytical metrics. Full article

Hemp essential oils are rich in bioactive compounds, including terpenes and cannabinoids, yet standardized analytical methods for their simultaneous quality control are limited. This study aimed to (i) validate a static headspace gas chromatography–mass spectrometry (SHS-GC-MS) method for simultaneous quantification of 20 terpenes and 2 cannabinoids and (ii) apply it to fingerprint essential oils from four hemp strains, including local (HRDI2, HRDI5) and internationally cultivated (Charlotte’s Angel, Cherry Wine) varieties. The method met AOAC validation criteria, with detection limits of 0.025–0.5 µg/mL for terpenes and 1 µg/mL for cannabinoids. Quantitation limits ranged from 0.1–1 µg/mL for terpenes and 5 µg/mL for cannabinoids. Intraday precision (%RSD) ranged from 0.27–11.00%, while interday precision ranged from 3.14–13.89%. The method recoveries ranged from 85.12–115.47%. Precision and recovery confirmed the method’s reliability. Multivariate statistical analysis identified 82 metabolites, revealing distinct chemical fingerprints among strains, and emerged as newly identified chemotype markers, supporting chemotype classification. This work demonstrates, for the first time, a solvent-free, automatable SHS-GC-MS approach for simultaneous terpene and cannabinoid profiling in hemp essential oils, enabling both qualitative and quantitative characterization and supporting regulatory compliance for the development of standardized phytopharmaceutical products. Full article

The exploitation of underutilised resources is critical for achieving a sustainable society, and non-edible seaweeds are promising candidates. This study focused on the red alga Portieria hornemannii from Okinawa, Japan, a seaweed with a distinctive aroma, and determined its volatile organic compounds (VOCs) and halogenated secondary metabolites using headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC-MS) at various extraction temperatures. HS-SPME-GC-MS analysis revealed 52 VOCs in Okinawan P. hornemannii, including predominant compounds α-pinenyl bromide (IUPAC name: 2-bromomethyl-6,6-dimethylbicyclo [3.1.1]hept-2-ene; halogenated monoterpene), myrcene disulfide (3-(6-methyl-2-methylidenehept-5-enylidene)dithiirane), and 5,6-dimethyl-1H-benzimidazole, the content of which in the extract increased with increasing extraction temperature from 30 to 60 °C. On the other hand, the β-myrcene (7-methyl-3-methyleneocta-1,6-diene) content, which likely contributes majorly to the distinct fresh odour of the algae, declined as the temperature increased. Furthermore, the proportion of β-myrcene obtained using SPME was significantly higher than that extracted using solvent liquid extraction (SLE) (7.20% in SPME at 30 °C vs. 0.09%, respectively). However, SLE-GC-MS provided a different P. hornemannii volatile profile, allowing for the acquisition of more furan-, alcohol-, ester-, and carboxylic acid-containing compounds. These data provide valuable information, such as a systematic analytical framework for volatiles profiling in the marine macroalgae P. hornemannii, with potential applicability in the development of food and fragrance products. Full article

The evaluation of region-specific aroma characteristics in green tea remains critical for quality control. This study systematically analyzed eight Tongcheng Xiaohua tea samples (standard and premium batches) originating from four distinct regions using sensory analysis, electronic nose (E-nose), headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC-MS), and chemometrics. The E-nose results demonstrated that the volatile characteristics of Tongcheng Xiaohua tea exhibit distinct geographical signatures, confirming the regional specificity of its aroma. HS-SPME-GC-MS identified 66 volatile metabolites across samples, with 18 key odorants (OAV > 1) including linalool, geraniol, (Z)-jasmone, and β-ionone driving aroma profiles. The partial least squares–discriminant analysis (PLS-DA) model, combined with variable importance in projection (VIP) scores and OAV, identified seven compounds that effectively differentiate the origins, among which α-pinene and β-cyclocitral emerged as novel markers imparting unique regional characteristics. Further comparative analysis between standard and premium grades revealed 2-methyl butanal, 3-methyl butanal, and dimethyl sulfide as main differential metabolites. Notably, the influence of geographical origin on metabolite profiles was found to be more significant than batch effects. These findings establish a robust analytical framework for origin traceability, quality standardization, and flavor optimization in tea production, providing valuable insights for the tea industry. Full article

The increasing scarcity of traditional nectar sources due to climate change has led beekeepers to explore alternative floral sources. This study investigates the volatile profile, sensory characteristics, and consumer acceptability of monofloral honey derived from Capparis spinosa L., a drought-resistant Mediterranean plant. Honey samples produced by Apis mellifera ssp. sicula on Aeolian Islands (Sicily, Italy) were analyzed. Volatile organic compounds (VOCs) were extracted using headspace solid–phase microextraction (HS-SPME) and identified by gas chromatography–mass spectrometry (GC–MS), revealing 59 compounds, with dimethyl sulfide being the predominant one. Sensory evaluation using quantitative descriptive analysis (QDA) and Time Intensity (TI) analysis identified distinctive descriptors such as sweet-caramel, cabbage/cauliflower, and pungent notes. Statistical analyses confirmed correlations between specific VOCs and sensory perceptions. A consumer acceptability test involving 80 participants showed lower preference scores for caper honey in terms of aroma and overall acceptability compared to commercial multifloral honey, with differences observed across age groups. The unique aromatic profile and consumer feedback suggest that caper honey has strong potential as a niche, high-quality product, particularly within the context of climate-resilient beekeeping, offering valuable opportunities for innovation and diversification in sustainable apiculture. Full article

The development of sensitive, non-invasive methods is essential for the preservation and study of heritage books, allowing insights into their historical production processes and conservation needs. Volatile organic compound (VOC) analysis provides a valuable, non-destructive approach to assess paper composition and degradation in historical volumes. In this study, we analyzed VOC emissions from two books preserved at the Biblioteca Capitolare of Busto Arsizio, Italy: a 16th-century Latin grammar book and a 19th-century mathematics handbook for measurement conversions. Using headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC-MS), VOCs were sampled after 24 h of storage at room temperature. The results revealed distinct degradation markers: Straight-chain aldehydes, indicative of lipid oxidation, were more prevalent in the 16th-century book, reflecting the higher quality and durability of its rag-based paper. In contrast, elevated furfural levels in the 19th-century book suggest accelerated cellulose hydrolysis typical of wood pulp paper. Additionally, the presence of menthol and anethole in both volumes points to the use of bacteriostatic agents for preservation. These findings not only highlight differences in material composition but also underscore the importance of tailored conservation approaches for historical documents from different eras. Full article

This study investigates the impact of using Lactiplantibacillus plantarum and Saccharomyces cerevisiae, either individually or in co-culture, on the fermentation of rose beverage. We comprehensively analyzed the resulting changes in quality characteristics and volatile compound profiles. Fermentation significantly altered the physicochemical properties, appearance, color, and free amino acid/organic acid content. Both microbial strains significantly increased total polyphenols and flavonoid content, with co-fermentation exhibiting a more pronounced effect compared to single-strain fermentations. Furthermore, the volatile compounds in rose beverages fermented with different microorganisms were characterized by an electronic nose (E-nose) and headspace–solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS). E-nose analysis demonstrated distinct volatile profiles distinguishing the four fermentation samples. HS-SPME/GC-MS identified a total of 245 volatile compounds, among which alcohols constituted the most abundant class. Integrating GC-MS data with odor activity value (OAV ≥ 1) analysis pinpointed 34 key aroma compounds. Partial least-squares discriminant analysis (PLS-DA) based on variable importance in projection (VIP) identified eight key volatile markers: eugenol, phenylethyl alcohol, (E)-3,7-dimethyl-2,6-octadienoic acid, methyleugenol, ethyl octanoate, citronellol, D-citronellol, and 2,4-bis(1,1-dimethylethyl)phenol. These findings provide valuable insights into the microbial influence on rose beverage quality and offer a theoretical basis for optimizing industrial fermentation processes. Full article

The quality of persimmon wine is closely related to various compounds, including polysaccharides. Polysaccharides are an essential class of macromolecules that modulate the wine’s chemical and physical characteristics by influencing the colloidal state or interacting with other compounds through non-covalent bonds. Polyphenols, on the other hand, exhibit antioxidant properties and effectively neutralize free radicals. This study employed Luotian sweet persimmons and Brassica napus (rapeseed) as core ingredients for producing functional fermented wine. Using GC-MS, rapeseed polysaccharides were subjected to trifluoroacetic acid hydrolysis and then derivatized via silylation for qualitative analysis of their monosaccharide composition. Molecular docking and molecular dynamics simulations were performed to provide molecular-level insights into the interactions between D-glucopyranose from rapeseed polysaccharides and quercetin, a polyphenol present in persimmon wine. The objective was to explore the binding mechanisms of these compounds during fermentation and to assess how these molecular interactions in-fluence the wine’s flavor and stability. In addition, volatile flavor compounds in two types of persimmon wine (pure persimmon wine and oleoresin-enriched persimmon wine) were qualitatively and quantitatively analyzed using headspace solid-phase microextraction (SPME) combined with gas chromatography–mass spectrometry (GC-MS). The results reveal that D-glucopyranose forms hydrogen bonds with quercetin, modulating its redox behavior and thereby enhancing the antioxidant capacity of persimmon wine. The results from four in vitro antioxidant assays, including DPPH, ABTS, FRAP, and vitamin C analysis, demonstrate that the addition of rapeseed flowers improved the antioxidant activity of persimmon wine. HS-SPME-GC-MS analysis revealed that esters, alcohols, and aldehydes were the primary components contributing to the aroma of persimmon wine. Persimmon wines with varying levels of oleoresin addition exhibited significant differences in the contents of key compounds, which subsequently influenced the aroma complexity and flavor balance. In conclusion, these findings provide reliable data and a theoretical foundation for understanding the role of rapeseed flower in regulating the aroma profile of persimmon wine. These findings also offer theoretical support for a deeper understanding of the fermentation mechanisms of persimmon wine while providing practical guidance to optimize production processes, ultimately improving both product flavor and stability. This study fills a critical academic gap in understanding microscopic molecular interactions during fermentation and offers a novel perspective for innovation in the fermented food industry. Full article

Unguentaria are ancient vessels for oils, perfumes, ointments, or balms. Glass unguentaria are typically small in size and have long narrow necks to limit the loss of precious contents through spills and evaporation. The vessels may have single or double barrels. This study includes both double and single unguentaria from unprovenanced archaeological contexts. Residues found inside the vessels may reveal the original contents. Gas chromatography-mass spectrometry (GC-MS) and direct analysis in real time-mass spectrometry (DART-MS) were used to identify organic components of the residues, while headspace solid-phase microextraction (HS-SPME) gas chromatography mass spectrometry provided a method to target specifically the volatile aroma compounds. Inorganic compounds in the unguentaria residues were identified by scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS). The results are consistent with a plant oil base, but few volatile perfume components could be characterized. While the collection of unguentaria may have contained perfumes, these results do not rule out the possibility of other unguents such as cosmetics. Full article

Butyriboletus roseoflavus is a rare wild edible mushroom. Yet, the relationship between its chemical composition and quality, as well as the influence of geographic origin on its flavor profile, remains unclear. In this study, ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) and headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC-MS) were used to investigate flavor differences and influencing factors among samples from different regions. Seventeen key volatile compounds (OAV > 1) were identified, with α-pinene, styrene, octanal, 1,3,5-trithiane, and 2,4-undecadienal being the primary aroma contributors. Six characteristic taste-active compounds (TAV > 1) were detected, among which Glu, Ala, and His played dominant roles. Differential metabolites were mainly enriched in nucleotides and their derivatives, suggesting their importance in environmental adaptation and quality formation. Correlation analysis revealed that the abundance of key metabolites was closely related to geographic origin: temperature, humidity, light intensity, and CO₂ concentration mainly influenced aroma variation, while taste differences were associated with soil electrical conductivity and microclimatic changes mediated by altitude. These findings provide a comprehensive understanding of the flavor characteristics of B. roseoflavus and offer a theoretical basis for its future processing and utilization. Full article

The Oddy test is an accelerated metal corrosion test used extensively by cultural institutions to determine the suitability of a material for use in museums. Alternatively, the use of gas chromatography-mass spectrometry (GC-MS) to directly identify volatile organic compounds (VOCs) from construction materials is growing in popularity because of its comprehensiveness and speed. Interpreting the reactivity of these potential pollutants, however, relies on ‘chemical intuition’ based on observed functional groups since the reactivity of only a handful of common VOCs has been studied intensively with regard to artworks. While short chain organic acids are known to be deleterious to some metals, polymers, and other culturally relevant materials, the common observation of lower volatility acids as well as their complementary aldehydes and esters in these offgassing experiments do not have clear indicators of their potential for artwork damage. In this work, the lead coupon, known to be a sensitive indicator of damaging organic acids, was exposed to known concentrations of a homologous series of organic acids, aldehydes, and esters from C2 to C18. Analysis of the coupon surface by infrared and Raman spectroscopies, and of the headspace within an Oddy jar by GC-MS, provides insights into the corrosion processes of these potential pollutants. Humidity was identified as a necessary component for corrosion to occur, and very volatile and semi-volatile compounds up to C9 created the corresponding lead carboxylate on the coupon surface in addition to lead carbonate. For higher order acids, and to a far lesser extent the esters and aldehydes, a high concentration of the VOC was necessary to induce small amounts of corrosion. In some instances, the gas phase chemistry of the reactor was particularly complex, suggesting mixtures of pollutants may prove more problematic to artist materials than single offgassed species. Full article