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1.
PLoS One ; 19(5): e0301341, 2024.
Article En | MEDLINE | ID: mdl-38753666

The deficiency of clinically specific biomarkers has made it difficult to achieve an accurate diagnosis of temporomandibular joint osteoarthritis (TMJ-OA) and the insufficient comprehension of the pathogenesis of the pathogenesis of TMJ-OA has posed challenges in advancing therapeutic measures. The combined use of metabolomics and transcriptomics technologies presents a highly effective method for identifying vital metabolic pathways and key genes in TMJ-OA patients. In this study, an analysis of synovial fluid untargeted metabolomics of 6 TMJ-OA groups and 6 temporomandibular joint reducible anterior disc displacement (TMJ-DD) groups was conducted using liquid and gas chromatography mass spectrometry (LC/GC-MS). The differential metabolites (DMs) between TMJ-OA and TMJ-DD groups were analyzed through multivariate analysis. Meanwhile, a transcriptomic dataset (GSE205389) was obtained from the GEO database to analyze the differential metabolism-related genes (DE-MTGs) between TMJ-OA and TMJ-DD groups. Finally, an integrated analysis of DMs and DE-MTGs was carried out to investigate the molecular mechanisms associated with TMJ-OA. The analysis revealed significant differences in the levels of 46 DMs between TMJ-OA and TMJ-DD groups, of which 3 metabolites (L-carnitine, taurine, and adenosine) were identified as potential biomarkers for TMJ-OA. Collectively, differential expression analysis identified 20 DE-MTGs. Furthermore, the integration of metabolomics and transcriptomics analysis revealed that the tricarboxylic acid (TCA) cycle, alanine, aspartate and glutamate metabolism, ferroptosis were significantly enriched. This study provides valuable insights into the metabolic abnormalities and associated pathogenic mechanisms, improving our understanding of TMJOA etiopathogenesis and facilitating potential target screening for therapeutic intervention.


Metabolomics , Osteoarthritis , Temporomandibular Joint Disorders , Transcriptome , Humans , Osteoarthritis/metabolism , Osteoarthritis/genetics , Metabolomics/methods , Male , Female , Temporomandibular Joint Disorders/metabolism , Temporomandibular Joint Disorders/genetics , Adult , Temporomandibular Joint/metabolism , Temporomandibular Joint/pathology , Gene Expression Profiling , Biomarkers/metabolism , Synovial Fluid/metabolism , Gas Chromatography-Mass Spectrometry , Middle Aged
2.
Food Res Int ; 183: 114240, 2024 May.
Article En | MEDLINE | ID: mdl-38760119

Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic organic pollutants found in various environments, notably aquatic ecosystems and the food chain, posing significant health risks. Traditional methods for detecting PAHs in food involve complex processes and considerable reagent usage, raising environmental concerns. This study explores eco-friendly approaches suing solid phases derived from natural sources in matrix solid phase dispersion. We aimed to develop, optimize, and validate a sample preparation technique for seafood, employing natural materials for PAH analysis. Ten natural phases were compared with a commercial reference phase. The methodology involved matrix solid phase dispersion and pressurized liquid extraction, followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Three solid phases (perlite, sweet manioc starch, and barley) showed superior performance in LC-MS/MS and were further evaluated with gas chromatography-tandem mass spectrometry (GC-MS/MS), confirming perlite as the most effective phase. Validation followed Brazilian regulatory guidelines and European Community Regulation 2021/808/EC. The resulting method offered advantages in cost-effectiveness, reduced environmental impact, cleaner extracts, and enhanced analytical performance compared to the reference solid phase and LC-MS/MS. Proficiency analysis confirmed method reliability, with over 50% alignment with green analytical chemistry principles. In conclusion, this study developed an environmentally sustainable sample preparation technique for seafood analysis using natural solid phases, particularly perlite, for PAH determination.


Food Contamination , Gas Chromatography-Mass Spectrometry , Polycyclic Aromatic Hydrocarbons , Seafood , Tandem Mass Spectrometry , Polycyclic Aromatic Hydrocarbons/analysis , Seafood/analysis , Tandem Mass Spectrometry/methods , Gas Chromatography-Mass Spectrometry/methods , Chromatography, Liquid/methods , Food Contamination/analysis , Solid Phase Extraction/methods , Reproducibility of Results , Brazil , Green Chemistry Technology/methods
3.
Food Res Int ; 183: 114183, 2024 May.
Article En | MEDLINE | ID: mdl-38760123

A large number of volatile compounds are formed during the baking of foods by reactions such as caramelization and Maillard reactions. Elucidating the reaction mechanisms may be useful to predict and control food quality. Ten reaction volatile markers were extracted during baking of solid model cakes implemented with known amounts of precursors (glucose with or without leucine) and then quantified by Thermal desorption-Gas chromatography-Mass spectrometry. The kinetic data showed that the level of air convection in the oven had no significant influence on the reaction rates. In contrast, increasing baking temperatures had a nonlinear accelerating impact on the generation of newly formed volatile compounds with a bell-shaped kinetic curve found for most of the markers at 200 °C. The presence of leucine triggered the activation of the Maillard and Strecker routes with a specific and very rapid formation of 3-Methylbutanal and pyrazines. A dynamic model was developed, combining evaporation flow rate and kinetic formation and consumption of reaction markers. It can be used to describe, for two furanic compounds of different volatilities, the vapor concentrations in the oven from the concentrations measured in the model cakes.


Cooking , Gas Chromatography-Mass Spectrometry , Glucose , Hot Temperature , Leucine , Maillard Reaction , Volatile Organic Compounds , Kinetics , Volatile Organic Compounds/analysis , Volatile Organic Compounds/chemistry , Cooking/methods , Glucose/chemistry , Glucose/analysis , Leucine/chemistry , Aldehydes/analysis , Aldehydes/chemistry , Pyrazines/analysis , Pyrazines/chemistry
4.
Food Res Int ; 183: 114180, 2024 May.
Article En | MEDLINE | ID: mdl-38760124

Platostoma palustre (Mesona chinensis Benth or Hsian-tsao, also known as "Xiancao" in China), is an edible and medicinal plant native to India, Myanmar, and Indo-China. It is the main ingredient in the popular desserts Hsian-tsao tea, herbal jelly, and sweet herbal jelly soup. P. palustre is found abundantly in nutrient-rich substances and possesses unique aroma compounds. Variations in the contents of volatile compounds among different germplasms significantly affect the quality and flavor of P. palustre, causing contradiction in demand. This study investigates the variation in the volatile compound profiles of distinct ploidy germplasms of P. palustre by utilising headspace gas chromatography-mass spectrometry (HS-GC-MS) and an electronic nose (e-nose). The results showed significant differences in the aroma characteristics of stem and leaf samples in diverse P. palustre germplasms. A total of sixty-seven volatile compounds have been identified and divided into ten classes. Six volatile compounds (caryophyllene, α-bisabolol, benzaldehyde, ß-selinene, ß-elemene and acetic acid) were screened as potential marker volatile compounds to discriminate stems and leaves of P. palustre. In this study, leaves of P. palustre showed one odor pattern and stems showed two odor patterns under the influence of α-bisabolol, acetic acid, and butyrolactone. In addition, a correlation analysis was conducted on the main volatile compounds identified by HS-GC-MS and e-nose. This analysis provided additional insight into the variations among samples resulting from diverse germplasms. The present study provides a valuable volatilome, and flavor, and quality evaluation for P. palustre, as well as new insights and scientific basis for the development and use of P. palustre germplasm resources.


Electronic Nose , Gas Chromatography-Mass Spectrometry , Odorants , Volatile Organic Compounds , Volatile Organic Compounds/analysis , Odorants/analysis , Plant Leaves/chemistry , Taste , Plant Stems/chemistry
5.
Food Res Int ; 183: 114211, 2024 May.
Article En | MEDLINE | ID: mdl-38760139

The wheat grains that are cultivated in saline-alkali soil exhibit a richer "wheat aroma" compared to their counterparts. This study characterized the composition and content of volatiles in five wheat kernel varieties, harvested from two fields with varying pH levels and total salt content in the soil. The wheat grown in soil with high pH and total salt content had significantly lower levels (p < 0.05) of ethyl 3-methylbutanoate and 1-octen-3-one and significantly higher levels (p < 0.05) of 1-butanol and 1-octen-3-ol. Among all factors, plant site contributed the highest F-value contribution rate (more than 77 %) for these four volatile compounds. Six e-nose sensors responsive to these four compounds exhibited consistent trends. Therefore, the lower of ethyl 3-methylbutanoate and 1-octen-3-one, the higher of 1-butanol and 1-octen-3-ol in wheat, grown on saline-alkali soil, served as characteristic markers for "wheat aroma".


Odorants , Soil , Triticum , Volatile Organic Compounds , Triticum/chemistry , Volatile Organic Compounds/analysis , Soil/chemistry , Odorants/analysis , Hydrogen-Ion Concentration , Alkalies/chemistry , Gas Chromatography-Mass Spectrometry , Electronic Nose
6.
J Tradit Chin Med ; 44(3): 515-523, 2024 Jun.
Article En | MEDLINE | ID: mdl-38767635

OBJECTIVE: To explore the material basis of the difference of efficacy of Dahuang (Radix Et Rhizoma Rhei Palmati)-Taoren (Semen Persicae) (DT) drugs with different proportions. METHODS: Samples of different ratios of Dahuang (Radix et Rhizoma Rhei Palnati, DH) to Taoren (Semen Persicae, TR) (Group A 1:1, B 2:3, C 3:2) were analyzed based on gas chromatography time-of-flight mass spectrometry untargeted metabolomics technique. RESULTS: A total of 240 primary metabolites were detected. Forty-one differential metabolites involved nine differential metabolic pathways, of which four were closely related to the efficacy of DT in the treatment of heat and blood stasis syndrome. These pathways included the biosynthesis of amino acid (phenylalanine tyrosine and tryptophan), flavonoids, unsaturated fatty acids, and the glycolysis/glycogenesis pathway. CONCLUSION: There are significant differences in the efficacy of different ratios of DT drugs, and their optimal ratio for the treatment of heat and blood stasis syndrome should be 1:1.


Drugs, Chinese Herbal , Metabolomics , Humans , Male , Gas Chromatography-Mass Spectrometry , Animals
7.
Food Res Int ; 187: 114316, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763629

This study investigates the dynamic changes in the aroma profile of Tuo tea during long-term storage, a process not well understood yet critical to the formation of aged tea's unique characteristics. Aroma profiling of Tuo tea samples stored for 2 to 25 years was conducted using sensory evaluation and the HS-SPME/GC × GC-QTOFMS technique, revealing a progressive transition from fresh, fruity, and floral scents to more stale, woody, and herbal notes. Among 275 identified volatiles, 55 were correlated with storage duration (|r| > 0.8, p < 0.05), and 49 differential compounds (VIP > 1, FC > 1.2, FC < 0.833, p < 0.05) were identified across three storage stages (2-4, 5-10, and 13-25 years). Furthermore, theaspirane, eucalyptol, o-xylene, and 1-ethylidene-1H-indene were selected as potential markers of Tuo tea aging, incorporating the implementation of a Random Forest (RF) model. Additionally, our model exhibited high accuracy in predicting the age of Tuo tea within a prediction error range of -2.51 to 2.84 years. This research contributes to a comprehensive understanding of the impact of storage time on tea aroma and aids in the precise identification of tea age.


Food Storage , Gas Chromatography-Mass Spectrometry , Odorants , Tea , Volatile Organic Compounds , Odorants/analysis , Tea/chemistry , Volatile Organic Compounds/analysis , Food Storage/methods , Time Factors , Humans , Camellia sinensis/chemistry , Solid Phase Microextraction
8.
Food Res Int ; 187: 114330, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763633

Processing technology plays a crucial role in the formation of tea aroma. The dynamic variations in volatile metabolites across different processing stages of fresh scent green tea (FSGT) were meticulously tracked utilizing advanced analytical techniques such as GC-E-Nose, GC-MS, and GC × GC-TOFMS. A total of 244 volatile metabolites were identified by GC-MS and GC × GC-TOFMS, among which 37 volatile compounds were concurrently detected by both methods. Spreading and fixation stages were deemed as pivotal processes for shaping the volatile profiles in FSGT. Notably, linalool, heptanal, 2-pentylfuran, nonanal, ß-myrcene, hexanal, 2-heptanone, pentanal, 1-octen-3-ol, and 1-octanol were highlighted as primary contributors to the aroma profiles of FSGT by combining odor activity value assessment. Furthermore, lipid degradation and glycoside hydrolysis were the main pathways for aroma formation of FSGT. The results not only elucidate the intricate variations in volatile metabolites but also offer valuable insights into enhancing the processing techniques for improved aroma quality of green tea.


Food Handling , Gas Chromatography-Mass Spectrometry , Odorants , Tea , Volatile Organic Compounds , Volatile Organic Compounds/analysis , Volatile Organic Compounds/metabolism , Gas Chromatography-Mass Spectrometry/methods , Odorants/analysis , Tea/chemistry , Food Handling/methods , Electronic Nose , Aldehydes/analysis , Aldehydes/metabolism , Acyclic Monoterpenes/metabolism , Acyclic Monoterpenes/analysis , Camellia sinensis/chemistry , Camellia sinensis/metabolism , Ketones/analysis , Ketones/metabolism , Octanols
9.
Food Res Int ; 187: 114366, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763646

In recent years, numerous studies have demonstrated the significant potential of non-Saccharomyces yeasts in aroma generation during fermentation. In this study, 134 strains of yeast were isolated from traditional fermented foods. Subsequently, through primary and tertiary screening, 28 strains of aroma-producing non-Saccharomyces yeast were selected for beer brewing. Headspace-solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) and chemometrics were employed to analyze the volatile flavor substances in beer samples fermented using these strains. Chemometric analysis revealed that distinct species of non-Saccharomyces yeast had a unique influence on beer aroma, with strains from the same genus producing more similar flavor profiles. Accordingly, 2,6-nonadienal, 1-pentanol, phenyl ethanol, isoamyl acetate, ethyl caprate, butyl butyrate, ethyl propionate, furfuryl alcohol, phenethyl acetate, ethyl butyrate, ethyl laurate, acetic acid, and 3-methyl-4 heptanone were identified as the key aroma compounds for distinguishing among different non-Saccharomyces yeast species. This work provides useful insights into the aroma-producing characteristics of different non-Saccharomyces yeasts to reference the targeted improvement of beer aroma.


Beer , Fermentation , Fermented Foods , Gas Chromatography-Mass Spectrometry , Odorants , Solid Phase Microextraction , Volatile Organic Compounds , Yeasts , Beer/analysis , Beer/microbiology , Odorants/analysis , Volatile Organic Compounds/analysis , Fermented Foods/microbiology , Fermented Foods/analysis , Yeasts/isolation & purification , Yeasts/metabolism , Food Microbiology
10.
Food Res Int ; 187: 114359, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763643

Chinese Xiaokeng green tea (XKGT) possesses elegant and fascinating aroma characteristics, but its key odorants are still unknown. In this study, 124 volatile compounds in the XKGT infusion were identified by headspace-solid phase microextraction (HS-SPME), stir bar sorptive extraction (SBSE), and solvent extraction-solid phase extraction (SE-SPE) combined with gas chromatography-mass spectrometry (GC-MS). Comparing these three pretreatments, we found HS-SPME was more efficient for headspace compounds while SE-SPE was more efficient for volatiles with higher boiling points. Furthermore, SBSE showed more sensitive to capture ketones then was effective to the application of pretreatment of aroma analysis in green tea. The aroma intensities (AIs) were further identified by gas chromatography-olfactometry (GC-O). According to the AI and relative odor activity value (rOAV), 27 compounds were identified as aroma-active compounds. Quantitative descriptive analysis (QDA) showed that the characteristic aroma attributes of XKGT were chestnut-like, corn-like, fresh, and so on. The results of network analysis showed that (E, Z)-2,6-nonadienal, nonanal, octanal and nerolidol were responsible for the fresh aroma. Similarly, dimethyl sulfide, (E, E)-2,4-heptadienal, (E)-2-octenal and ß-cyclocitral contributed to the corn-like aroma. Furthermore, indole was responsible for the chestnut-like and soybean-like aroma. This study contributes to a better understanding of the molecular mechanism of the aroma characteristics of XKGT.


Gas Chromatography-Mass Spectrometry , Odorants , Olfactometry , Solid Phase Microextraction , Tea , Volatile Organic Compounds , Odorants/analysis , Tea/chemistry , Volatile Organic Compounds/analysis , Solid Phase Microextraction/methods , Humans , Camellia sinensis/chemistry , Solid Phase Extraction/methods
11.
Food Res Int ; 187: 114398, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763656

Nowadays, it is important to monitor the freshness of meat during storage to protect consumers' health. Volatile organic compounds (VOCs) are responsible for odour and taste of food, and they give an indication about meat quality and freshness. This study had the aim to seek and select potential new markers of meat spoilage through a semi-quantitative analysis in five types of meat (beef, raw and baked ham, pork sausage and chicken) and then to develop a new quantitative analytical method to detect and quantify potential markers on five types of meat simultaneously. Firstly, a new headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method was developed to evaluate the volatile profile of five types of meat, preserved at 4 °C for 5 days. Among the 40 compounds identified, 15 were chosen and selected as potential shelf-life markers on the basis of their presence in most of meat samples or/and for their constant increasing/decreasing trend within the sample. Afterwards, a quantitative HS-SPME-GC-MS analytical method was developed to confirm which VOCs can be considered markers of shelf-life for these meat products, stored at 4 °C for 12 days. Some of the compounds analyzed attracted attention as they can be considered markers of shelf-life for at least 4 types of meat: 1-butanol, 3-methylbutanol, 1-hexanol, 2-nonanone, nonanal, 1-octen-3-ol and linalool. In conclusion, in this study a new quantitative HS-SPME-GC-MS analytical method to quantity 15 VOCs in five types of meat was developed and it was demonstrated that some of the compounds quantified can be considered markers of shelf-life for some of the meat products analyzed.


Food Storage , Gas Chromatography-Mass Spectrometry , Meat Products , Solid Phase Microextraction , Volatile Organic Compounds , Volatile Organic Compounds/analysis , Gas Chromatography-Mass Spectrometry/methods , Solid Phase Microextraction/methods , Meat Products/analysis , Animals , Swine , Odorants/analysis , Cattle , Aldehydes/analysis , Chickens , Ketones/analysis , Pentanols/analysis , Acyclic Monoterpenes/analysis , Octanols
12.
Food Res Int ; 187: 114424, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763675

This study aimed to investigate the changes in flavor quality of roasted duck during repetitive freeze-thawing (FT, -20 ℃ for 24 h, then at 4 ℃ for 24 h for five cycles) of raw duck preforms. HS-SPME/GC-MS analysis showed that more than thirty volatile flavor compounds identified in roasted ducks fluctuated with freeze-thawing of raw duck preforms, while hexanal, nonanal, 1-octen-3-ol, and acetone could as potential flavor markers. Compared with the unfrozen raw duck preforms (FT-0), repetitive freeze-thawing increased the protein/lipid oxidation and cross-linking of raw duck preforms by maintaining the higher carbonyl contents (1.40 âˆ¼ 3.30 nmol/mg), 2-thiobarbituric acid reactive substances (0.25 âˆ¼ 0.51 mg/kg), schiff bases and disulfide bond (19.65 âˆ¼ 30.65 µmol/g), but lower total sulfhydryl (73.37 âˆ¼ 88.94 µmol/g) and tryptophan fluorescence intensity. Moreover, A lower protein band intensity and a transformation from α-helixes to ß-sheets and random coils were observed in FT-3 âˆ¼ FT-5. The obtained results indicated that multiple freeze-thawing (more than two cycles) of raw duck preforms could be detrimental to the flavor quality of the roasted duck due to excessive oxidation and degradation.


Cooking , Ducks , Freezing , Gas Chromatography-Mass Spectrometry , Taste , Volatile Organic Compounds , Animals , Volatile Organic Compounds/analysis , Food Handling/methods , Oxidation-Reduction , Food Quality , Thiobarbituric Acid Reactive Substances/analysis
13.
Food Res Int ; 187: 114438, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763685

Early changes in sensory quality of phenols-rich virgin olive oil (VOO) and their relationship with the chemical changes are less studied in the literature. Therefore, the objective of this study was to propose a predictive model of dynamics of sensory changes based on specific chemical markers. The evolution of the sensory quality of phenol-rich VOOs from Tuscan cultivars stored under optimal storage conditions (i.e., absence of light, no O2 exposure, low temperature) was investigated using a multi-step methodological approach combining sensory (official sensory analysis (so-called Panel Test), Descriptive Analysis and Temporal Dominance of Sensation) and chemical measurements. The sensory map from descriptive data was related to the phenolic and volatile profiles, measured using HPLC-DAD and HS-SPME-GC-MS, respectively. A predictive model of the sensory changes over storage based on chemical compounds was developed. Results showed that very early changes involving phenolic and volatile compounds profiles occur in VOOs stored under optimal storage conditions, which turn in changes in sensory properties evaluated by the official panel test, the descriptive analysis and the temporal dominance of sensation. Furthermore, a chemical marker of sensory dynamics of oils during storage was identified as the ratio between two groups of secoiridoids. The proposed model, supported by the mentioned chemical marker, has the potential of improving the control of sensory changes in phenols-rich virgin olive oils during storage in optimal conditions.


Food Storage , Olive Oil , Phenols , Volatile Organic Compounds , Olive Oil/chemistry , Phenols/analysis , Food Storage/methods , Volatile Organic Compounds/analysis , Humans , Taste , Chromatography, High Pressure Liquid , Gas Chromatography-Mass Spectrometry , Male , Female , Adult , Biomarkers/analysis , Iridoids/analysis
14.
Molecules ; 29(9)2024 Apr 24.
Article En | MEDLINE | ID: mdl-38731439

The production of peanut oil in the industrial sector necessitates the utilization of diverse raw materials to generate consistent batches with stable flavor profiles, thereby leading to an increased focus on understanding the correlation between raw materials and flavor characteristics. In this study, sensory evaluations, headspace solid-phase micro-extraction gas chromatography mass spectrometry (HS-SPME-GC-MS), odor activity value (OAV) calculations, and correlation analysis were employed to investigate the flavors and main contributing amino acids of hot-pressed oils derived from different peanut varieties. The results confirmed that the levels of alcohols, aldehydes, and heterocyclic compounds in peanut oil varied among nine different peanut varieties under identical processing conditions. The OAVs of 25 key aroma compounds, such as methylthiol, 3-ethyl-2,5-dimethylpyrazine, and 2,3-glutarone, exceeded a value of 1. The sensory evaluations and flavor content analysis demonstrated that pyrazines significantly influenced the flavor profile of the peanut oil. The concentrations of 11 amino acids showed a strong correlation with the levels of pyrazines. Notably, phenylalanine, lysine, glutamic acid, arginine, and isoleucine demonstrated significant associations with both pyrazine and nut flavors. These findings will provide valuable insights for enhancing the sensory attributes of peanut oil and selecting optimal raw peanuts for its production.


Amino Acids , Arachis , Gas Chromatography-Mass Spectrometry , Odorants , Peanut Oil , Amino Acids/analysis , Amino Acids/chemistry , Arachis/chemistry , Odorants/analysis , Peanut Oil/chemistry , Volatile Organic Compounds/analysis , Volatile Organic Compounds/chemistry , Flavoring Agents/chemistry , Flavoring Agents/analysis , Pyrazines/chemistry , Pyrazines/analysis , Solid Phase Microextraction , Taste , Hot Temperature
15.
Molecules ; 29(9)2024 Apr 25.
Article En | MEDLINE | ID: mdl-38731460

Tanacetum parthenium L. (Asteraceae) is a perennial herbaceous plant with a long-standing historical use in traditional medicine. Recently Tanacetum parthenium L. essential oil has been associated with a promising potential for future applications in the pharmaceutical industry, in the cosmetics industry, and in agriculture. Investigations on the essential oil (EO) have indicated antimicrobial, antioxidant, and repellent activity. The present study aimed to evaluate the chemical composition of Bulgarian T. parthenium essential oil from two different regions, to compare the results to those reported previously in the literature, and to point out some of its future applications. The essential oils of the air-dried flowering aerial parts were obtained by hydrodistillation using a Clevenger-type apparatus. The chemical composition was evaluated using gas chromatography with mass spectrometry (GC-MS). It was established that the oxygenated monoterpenes were the predominant terpene class, followed by the monoterpene hydrocarbons. Significant qualitative and quantitative differences between both samples were revealed. Camphor (50.90%), camphene (16.12%), and bornyl acetate (6.05%) were the major constituents in the feverfew EO from the western Rhodope Mountains, while in the EO from the central Balkan mountains camphor (45.54%), trans-chrysanthenyl acetate (13.87%), and camphene (13.03%) were the most abundant components.


Gas Chromatography-Mass Spectrometry , Oils, Volatile , Tanacetum parthenium , Oils, Volatile/chemistry , Bulgaria , Tanacetum parthenium/chemistry , Terpenes/chemistry , Terpenes/analysis , Camphor/chemistry , Camphor/analysis , Plant Oils/chemistry , Bicyclic Monoterpenes
16.
Molecules ; 29(9)2024 Apr 25.
Article En | MEDLINE | ID: mdl-38731461

This present study aims to characterize the essential oil compositions of the aerial parts of M. spicata L. and endemic M. longifolia ssp. cyprica (Heinr. Braun) Harley by using GC-FID and GC/MS analyses simultaneously. In addition, it aims to perform multivariate statistical analysis by comparing with the existing literature, emphasizing the literature published within the last two decades, conducted on both species growing within the Mediterranean Basin. The major essential oil components of M. spicata were determined as carvone (67.8%) and limonene (10.6%), while the major compounds of M. longifolia ssp. cyprica essential oil were pulegone (64.8%) and 1,8-cineole (10.0%). As a result of statistical analysis, three clades were determined for M. spicata: a carvone-rich chemotype, a carvone/trans-carveol chemotype, and a pulegone/menthone chemotype, with the present study result belonging to the carvone-rich chemotype. Carvone was a primary determinant of chemotype, along with menthone, pulegone, and trans-carveol. In M. longifolia, the primary determinants of chemotype were identified as pulegone and menthone, with three chemotype clades being pulegone-rich, combined menthone/pulegone, and combined menthone/pulegone with caryophyllene enrichment. The primary determinants of chemotype were menthone, pulegone, and caryophyllene. The present study result belongs to pulegone-rich chemotype.


Gas Chromatography-Mass Spectrometry , Mentha spicata , Mentha , Oils, Volatile , Oils, Volatile/chemistry , Mentha/chemistry , Mentha spicata/chemistry , Multivariate Analysis , Mediterranean Region , Cyclohexane Monoterpenes/chemistry , Cyclohexane Monoterpenes/analysis , Monoterpenes/chemistry , Monoterpenes/analysis , Limonene/chemistry , Terpenes/chemistry , Terpenes/analysis , Menthol
17.
Molecules ; 29(9)2024 Apr 29.
Article En | MEDLINE | ID: mdl-38731554

BACKGROUND: Fatty acids are essential for human health. Currently, there is a search for alternative sources of fatty acids that could supplement such sources as staple crops or fishes. Turions of aquatic plants accumulate a variety of substances such as starch, free sugars, amino acids, reserve proteins and lipids. Our aim is to see if turions can be a valuable source of fatty acids. METHODS: Overwintering shoots and turions of aquatic carnivorous plants were collected. The plant material was extracted with hexane. The oils were analyzed using a gas chromatograph with mass spectrometer. RESULTS: The dominant compound in all samples was linolenic acid. The oil content was different in turions and shoots. The oil content of the shoots was higher than that of the turions, but the proportion of fatty acids in the oils from the shoots was low in contrast to the oils from the turions. The turions of Utricularia species were shown to be composed of about 50% fatty acids. CONCLUSIONS: The turions of Utricularia species can be used to obtain oil with unsaturated fatty acids. In addition, the high fatty acid content of turions may explain their ability to survive at low temperatures.


Fatty Acids , Plant Shoots , Fatty Acids/analysis , Plant Shoots/chemistry , Gas Chromatography-Mass Spectrometry , alpha-Linolenic Acid/analysis , Plant Oils/chemistry , Plant Oils/analysis
18.
Molecules ; 29(9)2024 Apr 30.
Article En | MEDLINE | ID: mdl-38731560

2, 6-diisopropylaniline (2, 6-DIPA) is a crucial non-intentionally organic additive that allows the assessment of the production processes, formulation qualities, and performance variations in biodegradable mulching film. Moreover, its release into the environment may have certain effects on human health. Hence, this study developed simultaneous heating hydrolysis-extraction and amine switchable hydrophilic solvent vortex-assisted homogeneous liquid-liquid microextraction for the gas chromatography-mass spectrometry analysis of the 2, 6-DIPA additive and its corresponding isocyanates in poly(butylene adipate-co-terephthalate) (PBAT) biodegradable agricultural mulching films. The heating hydrolysis-extraction conditions and factors influencing the efficiency of homogeneous liquid-liquid microextraction, such as the type and volume of amine, homogeneous-phase and phase separation transition pH, and extraction time were investigated and optimized. The optimum heating hydrolysis-extraction conditions were found to be a H2SO4 concentration of 2.5 M, heating temperature of 87.8 °C, and hydrolysis-extraction time of 3.0 h. As a switchable hydrophilic solvent, dipropylamine does not require a dispersant. Vortex assistance is helpful to speed up the extraction. Under the optimum experimental conditions, this method exhibits a better linearity (0.0144~7.200 µg mL-1 with R = 0.9986), low limit of detection and quantification (0.0033 µg g-1 and 0.0103 µg g-1), high extraction recovery (92.5~105.4%), desirable intra- and inter-day precision (relative standard deviation less than 4.1% and 4.7%), and high enrichment factor (90.9). Finally, this method was successfully applied to detect the content of the additive 2, 6-DIPA in PBAT biodegradable agricultural mulching films, thus facilitating production process monitoring or safety assessments.


Amines , Aniline Compounds , Gas Chromatography-Mass Spectrometry , Hydrophobic and Hydrophilic Interactions , Liquid Phase Microextraction , Solvents , Liquid Phase Microextraction/methods , Gas Chromatography-Mass Spectrometry/methods , Solvents/chemistry , Amines/chemistry , Amines/analysis , Aniline Compounds/chemistry , Hydrolysis , Polyesters/chemistry
19.
Molecules ; 29(9)2024 Apr 30.
Article En | MEDLINE | ID: mdl-38731568

Cancer is one of the major causes of death, and its negative impact continues to rise globally. Chemotherapy, which is the most common therapy, has several limitations due to its tremendous side effects. Therefore, developing an alternate therapeutic agent with high biocompatibility is indeed needed. The anti-oxidative effects and bioactivities of several different crude extracts of marine algae have been evaluated both in vitro and in vivo. In the present study, we synthesized the aqueous extract (HA) from the marine algae Amphiroa anceps, and then, a liposome was formulated for that extract (NHA). The extracts were characterized using different photophysical tools like dynamic light scattering, UV-visible spectroscopy, FTIR, scanning electron microscopy, and GC-MS analysis. The SEM image revealed a size range of 112-185 nm for NHA and the GC-MS results showed the presence of octadecanoic acid and n-Hexadecanoic acid in the majority. The anticancer activity was studied using A549 cells, and the NHA inhibited the cancer cells dose-dependently, with the highest killing of 92% at 100 µg/mL. The in vivo studies in the zebrafish model showed that neither the HA nor NHA of Amphiroa anceps showed any teratogenic effect. The outcome of our study showed that NHA can be a potential drug candidate for inhibiting cancer with good biocompatibility up to a dose of 100 µg/mL.


Antineoplastic Agents , Rhodophyta , Zebrafish , Rhodophyta/chemistry , Humans , Animals , Antineoplastic Agents/pharmacology , Antineoplastic Agents/chemistry , A549 Cells , Neoplasms/drug therapy , Neoplasms/pathology , Plant Extracts/chemistry , Plant Extracts/pharmacology , Liposomes/chemistry , Gas Chromatography-Mass Spectrometry , Nanoparticles/chemistry , Cell Line, Tumor
20.
Molecules ; 29(9)2024 May 03.
Article En | MEDLINE | ID: mdl-38731605

The aim of this study is to develop a rapid and accurate method for simultaneous analysis of multi-residue pesticides and conduct pesticide monitoring in agricultural products produced by the production and distribution stage in Korea. The representative agricultural products were selected as brown rice, soybean, potato, mandarin, and green pepper and developed using gas chromatography with tandem mass (GC-MS/MS) for the analysis of 272 pesticide residues. The experimental samples were extracted by the QuEChERS-EN method and then cleaned up by using d-SPE, including MgSO4 and primary secondary amine (PSA) sorbents. The established method was validated in accordance with Codex CAC-GL/40, and the limit of quantitation (LOQ) was determined to be 0.01 mg/kg. A total of 243 pesticides satisfied the guidelines in five samples at three levels with values of 60 to 120% (recovery) and ≤45% (coefficient of variation, CV). The remaining 29 pesticides did not satisfy the guidelines, and these pesticides are expected to be used as a screening method for the routine inspection of agricultural products. As a result of analyzing 223 agricultural products in South Korea by applying the simultaneous analysis method, none of the detected levels in the samples exceeded the standard values based on maximum residue limits (MRLs). The developed method in this study will be used to inspect residual pesticides in agricultural products, and it is anticipated to contribute to the distribution of safe agricultural products to consumers.


Gas Chromatography-Mass Spectrometry , Pesticide Residues , Tandem Mass Spectrometry , Tandem Mass Spectrometry/methods , Pesticide Residues/analysis , Gas Chromatography-Mass Spectrometry/methods , Pesticides/analysis , Crops, Agricultural/chemistry , Republic of Korea , Food Contamination/analysis , Limit of Detection , Solid Phase Extraction/methods
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