Search Results (639)

As rapidly developing consumer products, cosmetics confront challenges regarding safety, especially hazardous ingredients, like sex hormones. Prolonged exposure to trace sex hormones in cosmetics can inflict immeasurable damage to human health. To accurately detect the trace amounts of sex hormones in cosmetics, a reliable method was developed and validated using ultra-high performance liquid chromatography–mass spectrometry (UHPLC-MS/MS) with magnetic solid-phase extraction (MSPE) and isotope-labeled internal standards (IL-ISs). The conditions of sample pretreatment, chromatography, and mass parameters were systemically investigated. In the MSPE procedure, the commercial Fe₃O₄@HLB magnetic material was employed for sample pretreatment, which was beneficial for operation, as well as sample purification and analyte enrichment. The utilization of IL-ISs compensated for potential matrix effects and losses during sample preparation, thereby improving precision and accuracy. Based on the proposed MSPE technology, UHPLC-MS/MS can address the qualitative and quantitative analysis needs for target analytes in complex cosmetic matrices. At three fortification levels, recoveries were in the range of 71.7–116.2%, with a relative standard deviation (RSD) ranging from 1.6% to 8.3%. Furthermore, based on the method proposed here, a total of 116 batches of cosmetics were analyzed, and trace progestins and estrogens were discovered in 10 samples. The MSPE method, coupled with UHPLC-MS/MS using IL-ISs, was convenient, efficient, and feasible for detecting trace amounts of sex hormones in cosmetics. The method scored 0.66 (out of 1) on the AGREE metric, confirming its green profile. Based on the detected concentrations, a preliminary safety evaluation was performed to assess the potential health risks of residual progesterone in hair loss prevention cosmetics by calculating the margin of safety (MoS). Full article

Aflatoxin M1 (AFM1), a hydroxylated metabolite of aflatoxin B1, is a persistent food safety hazard in the dairy production chain. This study investigated AFM1 occurrence in fermented dairy products collected from the Croatian market in spring 2025 and assessed associated dietary exposure risks. A total of 81 samples were analyzed using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) following immunoaffinity column clean-up. AFM1 was detected in 48.1% of samples, with a mean concentration of 0.015 µg/kg. Products with thermophilic and probiotic bacterial cultures showed the lowest incidence rates, at 33.3% and 40.0%, respectively. Significantly higher AFM1 occurrence was found in Croatian samples than in imported ones (p < 0.05). Exposure assessment, based on estimated daily intake (EDI), hazard index (HI), and margin of exposure (MOE), identified toddlers and children as the most at-risk groups, with EDI ranging from 0.21 to 0.93 ng/kg bw/day, depending on AFM1 concentration. HI exceeded 1 even at mean AFM1 levels, while MOE fell below the safety threshold of 10,000 in worst-case scenarios, indicating potential health concerns. These findings underscore the need for continuous monitoring and targeted risk mitigation strategies for vulnerable populations, and support expanding regulatory limits to include processed dairy products. Full article

Evaluating the potential chronic health risks posed by pesticides to consumers is essential for ensuring food safety and protecting public health. An ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method coupled with modified QuEChERS extraction was developed to simultaneously determine 26 pesticide residues in wheat grain and bran. Samples were extracted with acetonitrile with 2% (v/v) acetic acid and cleaned up using C₁₈ sorbent. Method validation demonstrated excellent linearity, accuracy, and precision. When applied to 48 wheat grain and 24 bran samples collected from major wheat-growing regions in China, 12 and 21 pesticides were detected at concentrations ranging from <0.005 to 1.785 mg kg⁻¹ and <0.01 to 2.188 mg kg⁻¹, respectively. Chronic hazard quotients (HQc) and acute hazard quotients (HQa) for all pesticides for grain and bran were far below the safety threshold of 100%. These results indicate that pesticide residues in wheat grain and bran present negligible chronic dietary risks to consumers across all age groups. Full article

The aim of this study is to investigate the occurrence of melamine and cyanuric acid in milk, baby food, and protein supplements collected in Croatia. A total of 56 samples were collected during 2022 and 2023 from retail stores in Zagreb, Croatia. Sample preparation involved acetonitrile extraction, followed by analysis using ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). Cyanuric acid concentrations above the limit of quantification (LOQ) were found in five milk samples (33.3% detection frequency), with a range from 0.26 to 0.39 mg/kg and a mean concentration of 0.31 mg/kg. In protein supplements, melamine was detected above the LOQ in six samples (23% detection frequency), with a mean concentration of 0.30 mg/kg and concentrations ranging from 0.20 to 0.57 mg/kg. No concentrations above the LOQ were found in baby food samples. All detected values were below the EU maximum limits (2.5 mg/kg for general food and 1.0 mg/kg for baby food). The accuracy and reliability of the method were verified using certified reference material. This is the first study to confirm the presence of melamine and cyanuric acid in protein supplements and milk on the Croatian market. The detected levels do not indicate a potential health risk to consumers. Full article

Background/Objectives: Land management practices strongly influence soil biochemical processes, yet conventional soil measurements often overlook dynamic small-molecule variation underlying nutrient cycling and microbial activity. This study aimed to evaluate whether MS¹-based untargeted metabolomics can resolve meaningful biochemical differences among soil systems under distinct land management practices. Methods: Soils from six land-use types—conventional cultivation, organic cultivation, pasture, white pine, tulip poplar, and hardwood forest—were analyzed using ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS). Multivariate analyses, including PLS-DA, were performed to evaluate metabolic variation across systems. Both identified metabolites and unknown spectral features (MSI Level 4) were assessed, and biosynthetic class assignment of unknown features was performed using NPClassifier. Results: Metabolic features revealed clear separation between land management systems, demonstrating distinct chemical fingerprints across ecosystems. While conventional elemental ratios (e.g., C/N) showed minimal differentiation, phosphorus-related stoichiometric ratios (C/P and N/P) displayed strong land-use-dependent differences. NPClassifier superclasses highlighted unique chemical patterns, with forest soils enriched in diverse secondary metabolites, cultivated soils characterized by simplified profiles, and pasture soils dominated by microbial membrane lipids and alkaloids. Conclusions: Untargeted MS¹-based metabolomics effectively distinguished soil systems under different land-use practices and revealed ecologically meaningful variation even without complete structural identification. This study demonstrates that an MS¹-only workflow leveraging unknown spectral features can robustly distinguish soil systems, underscoring their value in untargeted metabolomics analyses. Full article

Background/Objectives: Ergot alkaloids are mycotoxins produced mainly by fungi of the genus Claviceps, infecting a wide variety of plants, especially cereals. These toxins usually manifest as black, hardened sclerotia (ergots), though they may also be invisible when dispersed in grain. They pose a significant risk to animals and humans when present in contaminated cereals. They can cause ergotism, with vasoconstriction, ischemia, hallucinations, and in severe cases gangrene. This study was carried out in response to the European legislative actions which determine the permissible levels of ergot alkaloids in cereals. Historically, consumers manually removed visible sclerotia from grain, and farmers applied fertilizers or timed harvests to specific periods to mitigate contamination. However, these traditional methods have proven insufficient. We therefore explored advanced techniques for detecting and quantifying ergot-contaminated cereals, as well as methods for reducing ergot alkaloid concentrations. Methods: Searches were conducted in scientific databases including Google Scholar, PubMed, and Scopus to identify research articles, reviews, and experimental studies published mainly between 2012 and August 2025, including accepted or in-press manuscripts, with special attention to works from 2021 onward to capture the most recent advancements. Results/Conclusions: Ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) is the reference method for confirmatory, epimer-aware quantification of ergot alkaloids, and is already standardized. Recent QuEChERS-UHPLC-MS/MS workflows in cereal matrices, including oat-based products, routinely achieve limits of quantification of about 0.5–1.0 µg/kg with single-run analysis times of about 5–15 min. Rapid screening options complement, rather than replace, confirmatory mass spectrometry: magnetic bead-based immunoassays that use magnetic separation and a smartphone-linked potentiostat provide sub-hour turnaround and field portability for trained quality-assurance staff, although external validation and calibration traceable to LC-MS/MS remain prerequisites for routine use. In practice, operators are adopting tiered, orthogonal workflows (e.g., immunoassay or electronic-nose triage at intake followed by DNA-based checks on grain washings and LC–MS/MS confirmation, or hydrazinolysis “sum parameter” screening followed by targeted MS speciation). Such combinations reduce turnaround time while preserving analytical rigor. Biotechnology also offers potential solutions for reducing ergot alkaloid concentrations at the source. Finally, to enhance consumer safety, artificial intelligence and blockchain-based food traceability appear highly effective. These systems can connect all stakeholders from producers to consumers, allowing for real-time updates on food safety and rapid responses to contamination issues. This review primarily synthesizes advances in analytical detection of ergot alkaloids, while mitigation strategies and supply chain traceability are covered concisely as supporting context for decision making. Full article

Lichens are complex symbiotic systems known for synthesizing diverse secondary metabolites with documented antimicrobial, antioxidant, and antiproliferative activities. The present study focused on Pseudevernia furfuracea, a species widely distributed across Moroccan habitats. Two hydrodistillation-derived extracts (HE1 and HE2) were analyzed through ultra-high-Performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) to characterize their metabolite composition, and their effects were evaluated on Jurkat cells, a representative human cell line of the immune system. As the results of the characterization, the main compounds identified were Caprolactam, N,N-Diethylaniline, Erucamide, and 4-Isopropylaniline. Cytotoxicity assessment revealed that both HE1 and HE2 decreased the viability of Jurkat cells in a concentration-dependent manner. The mean effective concentrations (EC₅₀) after 24 h of treatment were 53.79 ± 2.92 µg/mL for HE1 and 59.76 ± 2.01 µg/mL for HE2. Cell death mechanisms were further examined by flow cytometry, revealing that apoptosis predominated after 24 h of treatment, progressing mainly to late apoptotic stages after 48 h. In parallel, the expression levels of key cytokine genes, including IL-2, TNF-α, and IFN-γ, were quantified at the mRNA level to evaluate potential immunomodulatory effects. Up-regulation was observed in IL-2 after exposure to both extracts for 24 and 48 h, and in the case of IFN-γ after exposure to HE2 for 24 h; in contrast, HE1 and HE2 produced down-regulation in TNF-α at 24 h. These findings suggest that HE1 and HE2 have immunomodulatory activity in Jurkat cells. Further investigations are needed to elucidate the underlying mechanisms and to clarify how HE1 and HE2 influence immune responses in human systems. Full article

In the context of the ten-year fishing ban on the Yangtze River, illegal poaching for profit persists. To support the enforcement of this ban and protect the river’s ecosystem, an efficient and precise method for distinguishing between wild and farmed common carp is essential. This study utilized ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) combined with metabolomics technology to analyze and compare the metabolic differences between wild and farmed common carp. Principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) revealed a clear separation between the two groups, which was further verified by metabolic fingerprint profiles. Moreover, 16 metabolites with high discriminatory potential were identified from 491 differentially metabolites, such as phytosphingosine, succinic acid and threonine. In addition, a cluster analysis of the differential metabolites classified them into four classes: peptides, fatty acyls, steroids and steroid derivatives, and glycerophospholipids. Furthermore, candidate biomarkers, including 3-hydroxybutyrylcarnitine, 3-hydroxyhexanoylcarnitine and jasminoside were identified to potential distinguish wild populations. To our knowledge, this is the first study to apply metabolomics technology to differentiate wild from farmed common carp, providing a new theoretical basis for ecological restoration efforts in the context of the Yangtze River fishing ban. Full article

Unrefined vegetable oils are an important source of bioactive compounds with beneficial effects on health. Therefore, confirming the biological identity of oils is important for ethical and economic reasons. In this study, a method was developed for discriminating vegetable oils based on the phenolic compounds profile obtained by ultrahigh-performance liquid chromatography-mass spectrometry (UHPLC-MS/MS). It was found that extra virgin olive oil has a cinnamic acid content of 2.2 mg/kg (mean value), a much higher value compared to other oils (not detected—0.4 mg/kg), thus being a representative phenolic marker for this oil. From the phenolic compounds profile of different vegetable oils, it can be stated that extra virgin olive oil has a specific phenolic content. However, walnut, sunflower, and corn oils have some similarities regarding the phenolic compounds content (for instance, ellagic acid) and, therefore, these oils can be used as adulterants of extra virgin olive oil. Data analysis, including principal component analysis, hierarchical cluster analysis, and partial least-squares discriminant analysis, demonstrated the discrimination of olive oils from other vegetable oils. Data analysis also allowed the discrimination and classification of olive oil samples adulterated with corn oil when the percentage of adulterant was 1%, with an accuracy of more than 90%. Full article

Background/Objectives: Phytochemicals from Chaenomeles japonica (CJ) (Thunb.) Lindl. ex Spach, a plant belonging to the Rosaceae family, are recognized for their potential to inhibit enzymes associated with diabetes, obesity, neurodegeneration, and inflammation. However, the influence of constituents from different plant parts on cytokine secretion has not yet been explored or comparatively analyzed. Methods: This study aimed to evaluate the anti-inflammatory potential of CJ by assessing its effects on chemokine and cytokine secretion, including interleukin (IL)-8, IL-1β, TNF-α, IL-6, and IL-10. Extracts from various plant parts (fruit, seed, flower, and leaf) were examined for their ability to modulate cytokine production in human neutrophils (PMNs). Among them, the aqueous fruit extract exhibited the strongest activity and was subsequently tested on peripheral blood mononuclear cells (PBMCs) and the human intestinal epithelial cell line Caco-2. The extract was also subjected to in vitro gastrointestinal digestion to assess the stability and bioactivity of its metabolites. The phytochemical composition of CJ preparations was characterized by ultra-high-performance liquid chromatography coupled with diode-array detection and tandem mass spectrometry (UHPLC-DAD-MS/MS). Results: The aqueous fruit extract significantly reduced the secretion of pro-inflammatory cytokines across all tested models. Fractions obtained after in vitro digestion also inhibited IL-8 release in Caco-2 cells. Conclusions: The most active fractions were rich in flavan-3-ols and proanthocyanidins. These findings indicate that CJ fruit possesses notable anti-cytokine properties and may serve as a promising natural source for developing functional food. Full article

Gastrodiae Rhizoma (GR) is known to have a medicinal and food-based homology. It is used to treat infantile convulsion, epilepsy, spasm, tetanus, and vertigo. In this study, an ultra-high performance liquid chromatography/tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated to quantify fourteen components (p-hydroxybenzyl alcohol, gastrodin, parishin E, p-hydroxybenzoic acid, parishin C, parishin A, parishin B, nicotinamide, p-hydroxybenzaldehyde, adenosine, 3,4-dihydroxybenzaldehyde, syringaldehyde, dauricine, and nobiletin) of GR in rat plasma. Methanol precipitation was used to prepare the samples with astragalin, serving as the internal standard. In multiple reaction monitoring (MRM) mode, the fourteen components were separated by gradient elution on a Waters ACQUITY UPLC^® HSS T3 column. Under these conditions, all fourteen analytes’ calibration curves demonstrated strong linearity within wide concentration ranges (r > 0.9941). Accuracy for the intra-day and inter-day assessments ranged from −13.74% to 12.76%, and the precision for all analytes remained below 8.88%. The analytes’ extraction recoveries ranged from 66.78% to 114.2%, accompanied by matrix effects ranging from 63.65% to 117.61%. Under the evaluated conditions, stability tests confirmed that the compounds remained stable, with relative standard deviations below 13.83%. Consequently, the UHPLC-MS/MS method was effectively used to determine the pharmacokinetics of fourteen components in rat plasma after oral administration of GR extract. This study provides supportive data for rational application of GR. Full article

Phenolic compounds are widely known for their beneficial effects on human health. However, it is essential to understand which low molecular weight metabolites are produced by the gut microbiota, when non-absorbed compounds reach the colon, and whether these metabolites are more biologically active than their precursors. In this context, this study aims to explore the gut microbiota metabolites of relevant phenolic compounds commonly found in the human diet. Therefore, ellagic acid, naringenin, and phloroglucinol were incubated with human feces for 48 h, and the ensuing metabolites were analyzed by ultra-high-performance liquid chromatography with diode array detector coupled to ion trap mass spectrometry (UHPLC-DAD-MSⁿ) and gas chromatography–mass spectrometry (GC-MS). Ellagic acid metabolism by the gut microbiota produced a diversity of urolithins, with 8-hydroxyurolithin being identified for the first time. Isomers of 4-hydroxybenzoic, 3,4-dihydroxybenozic, and p-coumaric acids were identified for the first time as naringenin metabolites, while phloroglucinic, 2-hydroxy-3-phenylpropanoic, 3-phenylpropanoic, and 2-phenylacetic acids are reported for the first time as phloroglucinol metabolites. These findings contribute to a more comprehensive understanding of the beneficial health effects of these metabolites through the evaluation of their biological activities in conjunction with their effects on the gut microbiota, thus providing the basis for the development of food supplements, novel probiotics or functional foods. Full article

The quality and flavor of chicken meat are fundamentally determined by muscle metabolite composition, which reflects the regulatory effects of genetic background on metabolic pathways and muscle development. In this study, we profiled the meat quality of breast muscle across 3 crossbreeding combinations (D×HD, HD×D, and D×LD) between the Yunong D line and Houdan chickens to elucidate the metabolic mechanisms underlying flavor variation. Eighteen representative breast muscle samples were analyzed using common physicochemical indexes, untargeted metabolomics based on Gas Chromatography-Time-of-Flight Mass Spectrometry (GC-TOF-MS) and Ultra-High-Performance Liquid Chromatography coupled with Quadrupole Exactive Mass Spectrometry (UHPLC-QE-MS). Differential metabolites were identified through Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA). Multivariate analysis revealed distinct metabolic signatures among crossbreeding combinations, with HD×D exhibiting the most favorable tenderness, color, and water-holding capacity. A total of nine differential metabolites (5 upregulated and 4 downregulated) were identified between D×HD and HD×D, and thirty-eight metabolites (18 upregulated and 27 downregulated) between D×HD and D×LD. The identified metabolites were predominantly associated with amino acid metabolism, lipid biosynthesis, nucleotide turnover, and energy metabolism. Among these, arachidonic acid, taurine, L-alanine, and citric acid exhibited marked intergroup differences. Enrichment analysis based on the Kyoto Encyclopedia of Genes and Genomes (KEGG) indicated significant involvement of pathways such as amino acid biosynthesis, taurine and hypotaurine metabolism, and ABC transporters in flavor formation. Hierarchical clustering and Pearson correlation analyses further delineated synergistic or antagonistic interactions among key metabolites, suggesting the existence of intricate regulatory mechanisms. These findings reveal critical metabolites and metabolic pathways associated with flavor attributes, offering both a theoretical framework and potential molecular targets for enhancing poultry meat quality through breeding strategies. Full article

Carotenoid pigments are widely distributed in nature and play a crucial role in protecting organisms from photodynamic damage. However, the characterization of carotenoid production in clinically relevant mycobacteria has been limited due to the low sensitivity of conventional detection methods. We present a descriptive analysis of carotenoid production in seven mycobacterial isolates from the scotochromogenic, photochromogenic, and non-chromogenic groups. To achieve this, we used a combination of High-performance liquid chromatography with diode-array detection (HPLC-DAD) and Ultra-high performance liquid chromatography–mass spectrometry (UHPLC-MS) to detect carotenoids pigments. Mycobacterium tuberculosis (MTB) and Mycobacterium bovis (MB) (non-chromogenic mycobacteria) produced β-carotene when cultured in the absence of light, at levels comparable to those of photochromogenic mycobacteria such as M. marinum (MM) and M. kansasii (MK). The highest levels of carotenoids were found in scotochromogenic species M. avium (MAV) and M. gordonae (MGOR). Conversely, M. abscessus (MABS), a non-chromogenic species in which no β-carotene was detected, served as a negative control for matrix effects. As expected, the use of highly sensitive analytical techniques such as HPLC-DAD and UHPLC-MS significantly enhanced the detection of β-carotene compared to visual pigment assessment. These methods allowed the detection of basal β-carotene levels even in mycobacteria classified as non-chromogenic. The proposed analytical approach provides a robust research tool to understand the effects of different stimulus that may alter the cell physiology in terms of pigment production. Full article

Background: To investigate the endogenous metabolites in Polygonatum odoratum (Mill.) Druce from different geographical origins within Guizhou Province, the metabolic profiles of samples from 12 regions were analyzed using ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Methods: Multivariate statistical methods including principal component analysis (PCA), hierarchical clustering analysis (HCA), and Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway enrichment analysis were employed to explore the influence of geographical origin on the metabolic composition of P. odoratum. Results: PCA revealed significant differences among samples from different regions which showed clear clustering patterns in our study, indicating that the growing environment considerably affects the metabolite profiles of P. odoratum. A total of 6055 potential metabolites were detected in both positive and negative ion modes. Significantly differential metabolites were then screened based on a fold change (FC) ≥ 2 or ≤0.5 and p < 0.05. Comparative analysis was conducted on representative samples from three clustered regions: As, ZYMT, and XY−1. The results indicated that alcohols, nucleotides and their derivatives were the major differential metabolites between AS and ZYMT, and alcohols were the key differential metabolites between AS and XY−1, while ketones and sphingolipids were the most significant differential metabolites between ZYMT and XY−1. KEGG enrichment analysis revealed that the pathways of nucleotide metabolism, amino acid biosynthesis, and aminoacyl-tRNA biosynthesis were notably disturbed, suggesting their crucial roles in the synthesis of differential metabolites in P. odoratum. Conclusions: These findings demonstrated the notable differences in the metabolite composition of P. odoratum from different regions of Guizhou province. Full article