Search Results (100)

In this study, weekly grab samples extracted by solid-phase extraction (SPE) and stir bar sorptive extraction (SBSE) were compared for the analysis of 230 pesticides in surface waters. Samples were collected from three different locations around Melbourne, Australia. Analysis was performed using Gas Chromatography Quadrupole Time of Flight High Resolution Mass Spectrometry (GC-QToF-HRMS). The two extraction techniques were compared, among others, for their limits of detection, recovery, extraction, and quantification efficiency of pesticides, as well as spatial and temporal differences in detected compounds. The target compounds screened were pesticides belonging mainly to the categories of fungicides, insecticides, and herbicides. Although SBSE extracted more pesticides at two out of three sites, SPE extracted total concentrations up to four times higher than SBSE over all sampling sites. The log K_OW of detected pesticides only partially explained the differences in detection, with SBSE performing better in the absorption of hydrophobic compounds. In addition, matrix effects, in particular turbidity, appeared to hinder extraction of contaminants, especially for SBSE. Spatially, SBSE detected 10 pesticides more than SPE at two locations, while the opposite was true at the third location, where turbidity was higher. The types of pesticides detected varied slightly between techniques and locations. The study highlights the complementarity of SBSE and SPE for monitoring pesticides in natural environments. SBSE is an easy-to-use technique and allows for extraction of a higher number of pesticides at trace level, but it might not be the preferred option for highly turbid waters. SPE requires more tedious and complex sample processing but allows for a more accurate quantification of a broader range of pesticides. Full article

This study investigated the changes in the physicochemical properties and metabolites of pickled purple radish during storage. Pickles of purple radish (‘Boraking’) prepared by the addition of acetic acid and sugar were stored in the dark at 4 °C for 60 days. The color of the pickled purple radish changed from purple to pink, while the pickling solution changed from pink to purple. During storage, sucrose content gradually decreased, while glucose and fructose levels increased. LC-ESI-QToF-MS metabolomic analysis indicated that metabolites, including organic acids, amino acids, sulfur-containing compounds, lysophosphatidylcholine, lysophosphatidylethanolamine, and anthocyanins, were identified. The antioxidant capacity and color meter of pickled purple radish may undergo changes due to the altered levels of non-volatile compounds (cyanidins, adenosine, and amino acids) during storage. Anthocyanins had negative correlations with the color of pickled purple radish. The radical scavenging activity and ferric-reducing antioxidant power of pickled purple radish declined during storage. These findings emphasized the need for further research to develop processing and storage methods that enhance the bioactivity and stability of pickled purple radish. Full article

Chaga (Inonotus obliquus) is an increasingly used natural product in botanical dietary supplements, valued for its bioactive compounds. However, inconsistent standardized analytical methods raise concerns over product authenticity, mislabeling, and quality control. This study employs a multi-analytical approach to differentiate wildcrafted chaga canker from North American chaga dietary supplements, particularly those containing mycelia fermented grain products. High-Performance Thin-Layer Chromatography (HPTLC), Liquid Chromatography with Evaporative Light Scattering Detection (LC-ELSD) or Photo/Diode Array Detection (LC-PDA/DAD), Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry (LC-QToF-MS), Nuclear Magnetic Resonance (NMR) spectroscopy, UV-Vis spectrophotometry, and iodine-starch assays were used to evaluate key markers, including triterpenoids, polysaccharides, and melanin. Whole chaga canker contained triterpenoids (inotodiol, trametenolic acid) and phenolics, like osmundacetone, while melanin absorbance at 500 nm differentiated it from fermented grain products. β-Glucan quantification and iodine-starch assays confirmed starch-rich composition in fermented grains and its absence in authentic chaga canker. NMR fingerprinting and LC-QToF-MS metabolomics demonstrated stark compositional deviations between wildcrafted chaga canker, I. obliquus mycelium, and fermented grain products. By integrating complementary techniques, we establish a framework that can reliably distinguish genuine chaga canker from misrepresented products, ensuring consumer safety and fostering trust in the functional mushroom, canker, and mycelium markets. Full article

This study characterizes the metabolomic profiles of three reference apricot cultivars (‘Bergeron’, ‘Currot’, and ‘Goldrich’) using ¹H NMR spectroscopy and untargeted UPLC-QToF MS/MS to support plant breeding by correlating metabolomic data with fruit phenotyping. The primary objective was to identify and quantify the key metabolites influencing fruit quality from a nutraceutical perspective. The analysis revealed significant differences in primary and secondary metabolites among the cultivars. ‘Bergeron’ and ‘Goldrich’ exhibited higher concentrations of organic acids (109 mg/g malate in ‘Bergeron’ and 202 mg/g citrate in ‘Goldrich’), flavonoids such as epicatechin (0.44 mg/g and 0.79 mg/g, respectively), and sucrose (464 mg/g and 546 mg/g), contributing to their acidity-to-sugar balance. Conversely, ‘Currot’ showed higher levels of amino acids (24.44 mg/g asparagine) and sugars, particularly fructose and glucose (79 mg/g and 180 mg/g), enhancing its characteristic sweetness. These findings suggest that metabolomic profiling can provide valuable insights into the biochemical pathways underlying apricot quality traits, aiding in the selection of cultivars with desirable characteristics. The integration of phenotyping data with ¹H NMR and UPLC-QToF MS/MS offers a comprehensive approach to understanding apricot metabolomic diversity, crucial for breeding high-quality, nutritionally enriched fruits that meet market demands. Full article

Lichens are an important source of diverse and unique secondary metabolites with recognized biological activities through experimental and computational procedures. The objective of this study is to investigate the metabolomic profile of the ethanolic extract of the Antarctic lichen Gondwania regalis and evaluate its antioxidant and antidiabetic activities with in vitro, in silico, and molecular dynamics simulations. Twenty-one compounds were tentatively identified for the first time using UHPLC/ESI/QToF/MS in negative mode. For antioxidant activity, the DPPH assay showed an IC₅₀ value of 2246.149 µg/mL; the total phenolic content was 31.9 mg GAE/g, the ORAC assay was 13.463 µmol Trolox/g, and the FRAP assay revealed 6.802 µmol Trolox/g. Regarding antidiabetic activity, enzyme inhibition yielded IC₅₀ values of 326.4513 µg/mL for pancreatic lipase, 19.49 µg/mL for α-glucosidase, and 585.216 µg/mL for α-amylase. Molecular docking identified sekikaic acid as the most promising compound, with strong binding affinities to catalytic sites, while molecular dynamics confirmed its stability and interactions. Toxicological and pharmacokinetic analyses supported its drug-like potential without significant risks. These findings suggest that the ethanolic extract of Gondwania regalis is a promising source of bioactive compounds for developing natural antioxidant and antidiabetic therapies. Full article

The rising demand for bioactive compounds from marine resources highlights the need for sustainable separation technologies. This study introduces an integrated process combining ultrasound-assisted extraction (USAE) and resin purification (RP) to isolate phlorotannins from Durvillaea incurvata, a brown seaweed with significant biomedical potential. Using a 32.5% ethanol–water solvent system for USAE followed by RP on Diaion HP-20 resin, phlorotannins were enriched 2.4-fold, with simultaneous removal of interfering compounds such as mannitol (~100%), which was demonstrated by FTIR and HPLC-IR analysis. Advanced characterization using UHPLC-QToF-MS/MS identified five novel phlorotannins with polymerization degrees of 3 to 8 phloroglucinol units in both USAE extracts and post-RP. Mass balance based on spectrophotometric measurements indicated a purification factor of ~2, confirming process effectiveness. RP streams showed distinct phlorotannin profiles, with one phlorotannin exceeding 70% relative abundance. However, MS/MS results showed significantly lower recoveries than spectrophotometric data, revealing a novel insight into RP purification. These findings highlight the critical role of comprehensive chemical characterization in optimizing sustainable phlorotannin extraction from seaweed. They propose a framework for scalable, eco-efficient technologies for achieving high-purity phlorotannin recovery. This approach facilitates the development of phlorotannin-based applications in the nutraceutical and pharmaceutical industries. Full article

Legumes, a dietary staple for centuries, have seen an influx of conventional and unconventional varieties to cater to human care conscious consumers. These legumes often undergo pretreatments like baking, soaking, or boiling to mitigate the presence of non-proteinogenic amino acids (NPAAs) and reduce associated health risks. The recent tara flour health scare, linked to the NPAA baikiain, emphasizes the need for robust analytical methods to ensure the safety and quality of both traditional and novel plant-based protein alternatives. While traditional techniques provide insights into protein and non-proteinogenic amino acid profiles, modern liquid chromatography-mass spectrometry (LC-MS) offers superior sensitivity and specificity for NPAA detection. This study employed an LC-QToF method with MS/MS analysis to comprehensively map the distribution of free NPAAs and proteinogenic amino acids (PAAs) in various legume samples. A total of 47 NPAAs and 20 PAAs were identified across the legume samples, with at least 7–14 NPAAs detected in each sample. Sulfur-containing NPAAs, such as S-methyl-L-cysteine, γ-glutamyl-S-methyl cysteine, and S-methyl homoglutathione, were predominantly found in Phaseolus and Vigna species. Cysteine and methionine were the sulfur-containing PAAs identified. Gel electrophoresis and soluble protein quantification were also conducted to understand legume protein composition holistically. This orthogonal approach provides a valuable tool for ensuring the overall quality of plant-based proteins and may aid in investigating food poisoning or outbreaks related to such products. Full article

Background: The use of illicit drugs and stimulants is a burgeoning socioeconomic problem, ultimately leading to an increase in street crimes and deteriorating human health. The persistent presence of CNS drugs in wastewater can also lead to downstream adverse effects on aquatic wildlife and humans. Objectives: In the present study, a method was developed for the solid-phase extraction and quantitative liquid chromatography coupled with tandem quadrupole/time-of-flight mass spectrometry (LC-QToF-MS) analysis of CNS stimulant drugs and their metabolites in municipal wastewater. The targeted species included amphetamine, methamphetamine, methylenedioxy-methamphetamine (MDMA), methylenedioxyethylamphetamine (MDEA), cocaine, and benzoylecgonine (BE). Methods: The method was validated and applied to analyzing wastewater samples collected at the University of Mississippi and the City of Oxford wastewater treatment plants (WWTPs) during weekends when the university hosted home college football games. Results: Our results indicate that while amphetamine, methamphetamine, MDMA, cocaine, and BE were all detected at quantifiable levels, amphetamine and BE were present in significantly higher concentrations in wastewater during football games. Conclusion: The insights from this study can be utilized to monitor long-term drug use trends, providing local law enforcement agencies with relevant data on consumption patterns over time. Full article

In this study, anthocyanin glycosides from nine cultivars of highbush blueberries grown in Korea were characterized using UPLC-DAD-QToF/MS and UPLC-Qtrap-MS/MS. A total of twenty-two derivatives were identified, consisting of mono-glycosides and acetyl-glycosides attached to aglycones, such as cyanidin, peonidin, delphinidin, petunidin, and malvidin. Among them, seven acetylated glycosides were tentatively determined by comparing the related authentic standards and previous reports and presented mass fragmentation, in which the acetyl group remained as the form attached to the sugar without de-esterification in positive ionization mode. The mid-season cultivar ‘New Hanover’ showed the highest total anthocyanin content (1011.7 mg/100 g dry weight) with predominant malvidin and delphinidin glycosides. Particularly, the ‘Patriot’ (early season) recorded the highest proportion of acetylated glycosides (19.7%). Multivariate analysis showed a distinct separation between early and mid-seasons with Draper. Especially, delphinidin 3-O-galactoside (VIP = 1.94) was identified as a marker for mid-season, and malvidin 3-O-glucoside (VIP = 1.79) was identified as a marker for early season. These comprehensive anthocyanin profiles of Korean blueberries will serve as fundamental data for breeding superior cultivars, evaluating and developing related products as well as clinical and metabolomic research. Full article

Green propolis, particularly from the unique flora of the Brazilian Caatinga biome, has gained significant interest due to its diverse chemical composition and biological activities. This study focuses on the chemical characterization and antimicrobial evaluation of Caatinga green propolis. Twelve compounds were isolated through different chromatographic techniques, including flavanones (naringenin, 7-O-methyleriodictyol, sakuranetin), flavones (hispidulin, cirsimaritin), flavonols (quercetin, quercetin-3-methyl ether, kaempferol, 6-methoxykaempferol, viscosine, penduletin), and one chalcone (kukulkanin B). Using liquid chromatography–quadrupole time-of-flight tandem mass spectrometry (LC-QToF-MS), a total of 55 compounds excluding reference standards were tentatively identified, which include flavonoids, phenolic acids derivatives, and alkaloids, with flavonols, flavanones, and flavones being predominant. Antimicrobial testing against pathogens revealed that the crude extract exhibited low inhibitory activity, against Gram-positive bacteria, including methicillin-resistant Staphylococcus aureus (MRSA) and vancomycin-resistant Enterococcus faecium (VRE) (IC₅₀: 148.4 and 120.98 µg/mL, respectively). Although the isolated compounds showed limited individual activity, a fraction containing sakuranetin and penduletin (Fraction 8) exhibited moderated activity against Cryptococcus neoformans (IC₅₀: 47.86 µg/mL), while a fraction containing quercetin and hispidulin showed moderated activity against VRE (IC₅₀: 16.99 µg/mL). These findings highlight the potential application of Caatinga green propolis as an antimicrobial agent, particularly against resistant bacterial strains, and underscore the importance of synergistic interactions between compounds in enhancing biological effects. Full article

Material planning is important in construction, for it affects procurement, cost, and schedule. Proper planning of material supply and logistics helps streamline the performance of all tasks through the avoidance of excessive or insufficient material supply. Material planning relies on quantity takeoff (QTO) and project schedules. Conventionally, quantity takeoff was a manual process based on 2D drawings and human interpretation and was error-prone. Presently, with the popularity of Building Information Modelling (BIM), in BIM-based projects, using inbuilt quantity takeoff functions, quantities of work can be generated automatically from BIM models to aid the quantity takeoff. However, if those inbuilt QTO solutions are object-based, then the quantities of works extracted may not meet the requirements of the users in selected cases, e.g., in zone-based construction projects. Also, for estimating daily material requirements, the accuracy of the quantities of work becomes more important, not only for the purpose of efficient planning but also for reducing construction waste. Since works using the same type of material can go overlapping, in addition to estimating the amount of material for each work, the total amount of material for a day must also be calculated. Thus, this research aims to develop a framework for automatic extraction of zone-based concrete volumes and formwork positions for cast-in-place concrete structures using the data in BIM models, followed by linking them with project schedules for estimating daily concrete and formwork requirements. This framework extends the body of knowledge by introducing an innovative algorithm for automatically calculating overlapped areas between concrete members and a rule for naming tasks in the schedule, followed by evaluating the formwork requirements without drawing formwork in a 3D model. A software tool will be developed to achieve the aim, and a case study will be used to validate the proposed framework. Full article

The flavoring of olive oils with aromatic plants is commonly used to enrich the oils with aromatic and antioxidant compounds. Origanum majorana L. was applied as a flavoring agent for extra virgin olive oil (EVOO), at concentrations of 20 g L⁻¹ and 40 g L⁻¹, via ultrasound-assisted maceration. The aim of this study was to evaluate the impact of flavoring on the EVOOs’ quality indices, oxidative stability, and antioxidant, antiradical and antifungal activities, as well as on the oils’ volatile and phenolic profile. The flavored EVOO maintained the quality indices (free fatty acids, peroxide value, extinction coefficients) below the maximum permitted levels, whereas the addition of marjoram enhanced the oxidative stability, the levels of chlorophyll and b-carotene and the total phenolic content. The incorporation of marjoram into the EVOO did not have a significant impact on the antioxidant and antiradical activities. Concerning the antifungal activity, no Zygosaccharomyces bailli cell growth was observed for two weeks in a mayonnaise prepared with the flavored EVOO at a 40 g L⁻¹ concentration. SPME-GC-MS analysis revealed the presence of 11 terpene compounds (hydrocarbon and oxygenated monoterpenes) that had migrated from marjoram in the flavored EVOO. Twenty-one phenolic compounds were tentatively characterized by LC-QToF-MS in the EVOO samples; however, hesperetin and p-coumaric acid, originating from marjoram, were only detected in the flavored EVOO. Full article

Dairy products are an important source of protein and other nutrients in the Mediterranean diet. In these countries, the most common sources of milk for producing dairy products are cow, goat, sheep, and buffalo. Andalusia is traditionally the largest producer of goat milk in Spain. Kefir is a fermented product made from bacteria and yeasts and has health benefits beyond its nutritional properties. There is a lack of knowledge about the molecular mechanisms and metabolites that bring about these benefits. In this work, the combination of analytical techniques (GC-FID, UHPLC-MS-QToF, GC-QqQ-MS, and GC-ToF-MS) resulted in the detection of 105 metabolites in kefir produced with goat milk from two different thermal treatments (raw and pasteurized) fermented at four time points (12, 24, 36, and 48 h, using 0 h as the control). Of these, 27 metabolites differed between kefir produced with raw and pasteurized milk. These changes could possibly be caused by the effect of pasteurization on the microbial population in the starting milk. Some interesting molecules were identified, such as shikimic acid, dehydroabietic acid, GABA, and tyramine, which could be related to antibacterial properties, strengthening of the immune system, and arterial pressure. Moreover, a viability assay of the NIRS technique was performed to evaluate its use in monitoring the fermentation and classification of samples, which resulted in a 90% accuracy in comparison to correctly classified samples according to their fermentation time. This study represents the most comprehensive metabolomic analysis of goat milk kefir so far, revealing the intricate changes in metabolites during fermentation and the impact of milk treatment. Full article

The Brassicaceae family, commonly referred to as cruciferous plants, is globally cultivated and consumed, with the Brassica genus being particularly renowned for its functional components. These vegetables are rich sources of nutrients and health-promoting phytochemicals, garnering increased attention in recent years. This study presents a comprehensive microscopic, chromatographic, and spectroscopic characterization of Brassica napus L. seeds from Kazakhstan aimed at elucidating their morphological features and chemical composition. Microscopic analysis revealed distinct localization of flavonoids, total lipids, and alkaloids. High-performance thin-layer chromatography (HPTLC) analysis of seed extracts demonstrated a complex chemical profile with significant quantities of non-polar compounds in the hexane extracts. Additionally, methanolic extracts revealed the presence of diverse chemical compounds, including alkaloids, flavonoids, and glucosinolates. The chemical composition exhibited varietal differences across different Brassica species, with B. napus L. seeds showing higher concentrations of bioactive compounds. Furthermore, liquid chromatography–quadrupole time-of-flight mass spectrometry (LC-QToF-MS) analysis provided insights into the chemical composition, with sinapine isomers, feruloyl, and sinapoyl choline derivatives as major compounds in the seeds. This study contributes to a better understanding of the chemical diversity and quality control methods’ approximations of B. napus L. seeds, highlighting their importance in functional food and nutraceutical applications. Full article

Nepeta nuda L., a notable medicinal species in the tradition of the Balkan region, is a rich source of bioactive iridoids and phenolics previously described as high-resolution taxonomical classifiers for the genus Nepeta. However, their potential in investigating intra-species differentiation is here described for the first time. The aim was to recognize the sources of natural chemical diversity and their association with the genetic variability both within and among N. nuda populations in the Central Balkans. Chemical diversity was assessed from methanol extracts and essential oils through untargeted and targeted metabolomics using state-of-the-art analytical tools, covering a broad spectrum of compounds that represent the N. nuda metabolome. We found that chemodiversity primarily resides within populations of N. nuda, and similar results were obtained at the DNA level using microsatellite markers. The low genetic and chemical differentiation of the studied N. nuda populations implies that their metabolomic profiles may be less influenced by geographic distance and variable environmental conditions within the Central Balkans, as they are under the pivotal control of their genetic backgrounds. Screening the distribution of the major bioactive compounds belonging to phenolics (phenolic acids and flavonoids) and iridoids (both aglycones and glycosylated forms), within and among N. nuda populations, is able to guarantee mass spectrometry-based tools for the selection of elite representative genotypes with practical importance. The knowledge acquired will allow us to delve deeper into the molecular background of N. nuda chemical diversity, which is the course of our further work. Full article