Search Results (2,375)

Benzo[a]pyrene (BaP), a potent carcinogenic polycyclic aromatic hydrocarbon, is a critical food contaminant originating from environmental deposition and thermal processing, posing a significant threat to public health and driving stringent global regulations. This review critically examines recent advancements in analytical methodologies for BaP determination, giving particular emphasis to sample preparation and detection techniques. The discussion covers the evolution from conventional methods, such as solid-phase extraction, towards more efficient and sustainable approaches, including magnetic, dispersive, and molecularly imprinted solid-phase extraction, as well as microextraction techniques and gel permeation chromatography. For detection, the performance of established chromatographic methods, such as gas chromatography–mass spectrometry (GC-MS) and high-performance liquid chromatography with fluorescence detection (HPLC-FLD), is evaluated against emerging rapid techniques such as sensors, immunoassays, and spectroscopic methods. The analysis reveals that while significant progress has been made in improving sensitivity, selectivity, and throughput, challenges remain in balancing speed with accuracy, managing matrix effects, and translating novel materials from research to routine application. The review concludes by underscoring the necessity for future development to focus on the integration of smart materials, automation, and advanced data science to achieve robust, on-site, and holistic monitoring solutions for ensuring food safety against BaP contamination. Full article

In this preliminary study, chitosan-based molecularly imprinted polymers crosslinked with glutaraldehyde were synthesized and evaluated for the selective removal of m-cresol, a volatile phenol associated with the sensory defect known as smoke taint in wine. Three formulations of chitosan-based molecularly imprinted polymers (MIP-Gs) were synthesized using glutaraldehyde as a crosslinker and m-cresol as a template. Non-imprinted polymers (NIP-Gs) served as controls. The polymers were characterized by Fourier-transform infrared spectroscopy, thermogravimetric analysis, and scanning electron microscopy, which confirmed successful crosslinking and structural differences between MIPs and NIPs. Adsorption performance was evaluated using solid-phase extraction cartridges packed with the synthesized polymers, employing a Cabernet Sauvignon wine. The MIPs exhibited higher adsorption efficiency and selectivity toward m-cresol compared to NIPs, achieving removal rates of 15% to 40%, depending on polymer formulation and analyte concentration. Molecular dynamics simulations were used to investigate polymer–analyte interactions at the molecular level, providing mechanistic insight into the preferential binding of m-cresol within the imprinted cavities. Physicochemical analyses of red wine showed that m-cresol removal occurred with minimal impact on key phenolic parameters, supporting the functional selectivity of MIPs. These results demonstrate that chitosan-based MIPs constitute a promising class of materials for selective adsorption applications in complex liquid systems. Full article

Niobium and tantalum are critical metals that are important for technological development. Their main applications are in the production of alloys for the civil construction, electronics, nuclear, and aerospace industries, and in catalysis. Tin reduction slag is a possible secondary source of niobium and tantalum, containing 3.7% and 0.5% of Nb and Ta, respectively. The slag matrix is mainly composed of calcium silicate, a low-reactivity material that prevents contact between the leaching solution and the metals to be extracted; therefore, it is necessary to previously react the material with molten NaOH. This reaction converts calcium silicates into sodium silicates, which are more reactive and water-soluble, and converts the metals into oxyanions, niobates, and tantalates, which are more reactive species. After treatment with molten hydroxide, the material is then solubilized in water; this reaction removes part of the soluble materials and also fragments the silicate matrix. Nb and Ta remain in the solid phase during the water washing step and then undergo acid leaching, where, after the parameters are evaluated, Nb extraction of 96% and Ta leaching of less than 3% are achieved, using a concentration of 10 mol/L H₂SO₄, a time of 2 h, a temperature of 90 °C, and a liquid–solid ratio of 50. Full article

The rapid growth and diversification of the cosmetic industry have led to increasingly complex formulations containing numerous bioactive ingredients, excipients, and synthetic additives, often delivered through advanced nanostructured systems. Ensuring product safety, efficacy, and regulatory compliance requires analytical approaches capable of accurately detecting both declared components and hazardous contaminants such as heavy metals, phthalates, nitrosamines, and banned preservatives or dyes. Traditional sample preparation methods are often solvent-intensive, time-consuming, and environmentally burdensome, prompting a shift toward green microextraction strategies aligned with the principles of green analytical chemistry. Techniques including solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), and dispersive liquid–liquid microextraction (DLLME) offer miniaturized, solvent-efficient workflows with improved selectivity and sensitivity for complex cosmetic matrices. This review summarizes advances from the past five years in green microextraction methods for the determination of organic and inorganic species in cosmetic products. Emphasis is placed on their integration with separation techniques and applicability across product categories. Emerging trends, analytical challenges, and future directions toward more sustainable cosmetic safety assessment are also highlighted. Full article

Background: Caloric restriction (CR) is a dietary intervention based on limiting calories relative to the basic energy needs of the organism, which changes the intensity of metabolism, causes changes in the functioning of the endocrine and sympathetic systems, and influences the expression of genes in muscle, heart, and brain cells. During the use of CR, there is a transition from carbohydrate supply to increased fat metabolism. Fatty acids are more or less susceptible to free radicals, depending on their molecular structure. Oxidation (peroxidation) contributes to the production of metabolites (including hydroxyeicosatetraenoic acid and hydroxyoctadecadienoic acid), some of which are involved in inflammation. Methods: The aim of this study was to evaluate the effects of long-term caloric restriction on the tissue levels of selected fatty acids and fatty acid-derived lipid mediators with pro-inflammatory or anti-inflammatory properties in skeletal muscle and intestinal tissues. The study was carried out on C57BL/6 mice. During the 8-month experiment, the mice in the study group were fed a 30% calorie restricted diet—according to the Every-Other-Day Diet concept. Analyses were performed on intestinal and muscle tissues collected from animals. Fatty acid derivatives were isolated using solid-phase extraction (C-18 columns) columns, and isolation of fatty acids was performed using a modified Folch method. The compounds were analyzed by liquid and gas chromatography. Results: CR induced detectable alterations in both fatty acid profiles and lipid mediator concentrations in a tissue-specific manner. However, most of these changes did not remain statistically significant after multiple testing correction. Conclusions: These findings suggest potential effects of long-term CR on lipid signaling pathways, although the current dataset lacks the statistical power required to draw definitive conclusions. This study highlights the need for further research using larger sample sizes and integrated multiomic approaches to elucidate the molecular mechanisms underlying lipidomic adaptations to prolonged caloric restriction. Full article

Pesticide contamination poses significant threats to both humans and the environment, with residues frequently detected in surface waters worldwide. This study compares the effectiveness of passive samplers (POCIS and Chemcatcher) and grab sampling coupled with Stir-Bar Sorptive Extraction (SBSE) and Solid-Phase Extraction (SPE) for monitoring pesticides in surface waters. The comparative study was conducted at three sites in Victoria, Australia, representing different land uses. A total of 230 pesticides were screened, with 79 different pesticides detected overall. SBSE extracted the highest number of pesticides from grab samples, followed by SPE and passive samplers. The study highlights the complementarity of different sampling and extraction techniques in detecting a wide range of pesticides. The study also explores the suitability of these techniques for citizen science applications, emphasizing the importance of selecting appropriate methods based on specific research objectives and available resources. The findings underscore the need for a tiered approach, combining passive samplers for initial screening and grab sampling for quantitative analysis, to develop a robust monitoring strategy for protecting water quality. Full article

Exogenous toxic compounds in foods, arising from agricultural practices, environmental contamination, industrial processing, and packaging migration, remain a major global concern for food safety. These contaminants include mycotoxins, veterinary drug residues, antibiotics, pesticides, per- and polyfluoroalkyl substances, heterocyclic aromatic amines, and polycyclic aromatic hydrocarbons, which have multiple adverse effects on human and animal health. The continued presence of these substances highlights the need for reliable exposure assessment, strengthened regulatory frameworks, and advanced analytical methodologies. Food matrices introduce variability in analytical performance, making sample preparation a critical and often limiting step. Conventional extraction techniques such as solid-phase extraction, liquid–liquid extraction, and Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) are still widely applied. Moreover, recent advances have highlighted sustainable alternatives aligned with the principles of green analytical chemistry. In this context, this review provides a comprehensive overview of recent advances (2020–2025) in environmentally friendly extraction techniques for determining exogenous toxic compounds in food samples analyzed by liquid chromatography coupled with mass spectrometry (LC–MS), including their sustainability. Special attention is given to the chemical nature and toxicological relevance of major exogenous organic contaminant families (specialized categories such as hormones and packaging-derived bisphenols were excluded due to distinct migration and metabolic pathways; however, these topics exceed the scope of this manuscript), the analytical challenges associated with different food matrices, and the evolution of extraction and cleanup techniques. Overall, this review integrates analytical robustness, matrix effects, and green metrics to support the development of reliable and more sustainable sample preparation strategies. Full article

Herbicides are widely used agrochemicals and are increasingly recognised as contaminants of emerging concern in aquatic environments due to their extensive application, environmental persistence, and potential ecological and human health impacts. Their determination in water presents significant analytical challenges, as these compounds occur at trace to ultra-trace levels and encompass a wide range of chemical properties, including highly polar and ionic species as well as transformation products. This review provides a critical overview of recent advances in separation technologies for the analysis of herbicides in water, based on peer-reviewed studies published between 2020 and 2025 retrieved from the PubMed and Scopus databases. The discussion focuses on developments in sample preparation, extraction strategies, chromatographic separation, and detection techniques, with particular attention to analytical performance and sustainability. The reviewed studies demonstrate that solid-phase extraction remains central to achieving the lowest detection limits, while miniaturised and greener extraction approaches are increasingly adopted to reduce solvent consumption and simplify workflows. Advances in chromatographic separation and detection, especially liquid chromatography coupled to tandem mass spectrometry, have further enhanced sensitivity and selectivity for a broad range of herbicides. Overall, this review highlights current analytical capabilities and emerging trends, outlining future directions for reliable and sustainable monitoring of herbicides in aquatic environments. Full article

Ciprofloxacin, being a widely used antibiotic agent, has sparked growing interest in the field of molecularly imprinted polymers (MIP) for its selective recognition and removal. This review provides a comprehensive analysis of the recent advances in the synthesis and applications of ciprofloxacin-imprinted polymers. The examination of synthesis compositions for the preparation of these polymers includes thorough discussions on functional monomers, crosslinkers, initiators, and solid supports. Various imprinting techniques, including bulk, precipitation, co-precipitation, and surface polymerization, have been assessed for the fabrication of the imprinted polymers. Furthermore, the advancing imprinting techniques, encompassing nano-scale imprinting, multi-functional monomers, multi-template imprinting, and electrochemical imprinting, are also highlighted. Additionally, an extensive exploration of the diverse applications of these polymers is also presented. These applications encompass selective separation and removal of ciprofloxacin from environmental samples, visual and electrochemical detection in complex matrices, their use as a stationary phase for HPLC, drug release, and photocatalysis. This review offers valuable insights into the current advancements and potential future directions in the development of ciprofloxacin-imprinted polymers, emphasizing their importance in diverse analytical and environmental applications. Full article

Bongkrekic acid (BKA), a highly lethal toxin, has been implicated in frequent poisoning incidents in recent years, posing a serious threat to global food safety and creating an urgent need for rapid and sensitive detection methods. This review provides a systematic analysis of the entire BKA detection technologies, covering sample pretreatment techniques, instrumental analysis, immunoassays, and biosensing methods. It assesses the merits of key methods and also explores the strategic cross-application of detection paradigms developed for analogous toxins. This review delivers a comprehensive and critical evaluation of BKA detection technologies. First, it discusses sample pretreatment strategies, notably solid-phase extraction (SPE) and QuEChERS. Subsequently, it analyzes the principles, performance, and applications of core detection methods, including high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS), high-resolution mass spectrometry (HRMS), time-resolved fluorescence immunoassay (TRFIA), dual-mode immunosensors and nanomaterial-based sensors. Instrumental methods (e.g., HRMS) offer unmatched sensitivity [with a limit of detection (LOD) as low as 0.01 μg/kg], yet remain costly and laboratory-dependent. Immunoassay and biosensor approaches (TRFIA and dual-mode sensors) enable rapid on-site detection with high sensitivity (ng/mL to pg/mL), though challenges in stability and specificity remain. Looking forward, the development of next-generation BKA detection could be accelerated by cross-applying cutting-edge strategies proven for toxins—such as Fumonisin B1 (FB1), Ochratoxin A (OTA), and Aflatoxin B1 (AFB1)—including nanobody technology, CRISPR-Cas-mediated signal amplification, and multimodal integrated platforms. To translate this potential into practical tools, future research should prioritize the synthesis of high-specificity recognition elements, innovative signal amplification strategies, and integrated portable devices, aiming to establish end-to-end biosensing systems capable of on-site rapid detection through multitechnology integration. Full article

Monitoring trace nitrophenol pollutants in water has garnered considerable attention. A porous organic polymer-modified cellulose nanofiber membrane (COP-99@DCA) was fabricated via in situ growth of a porous organic polymer on an electrospun cellulose nanofiber membrane. The resulting brown COP-99@DCA composite possessed abundant functional groups, including C-F, C-O, and hydroxyl groups, and exhibited excellent thermal and chemical stability. Furthermore, when employed as a sorbent in dispersive solid-phase microextraction (d-SPME), COP-99@DCA efficiently enriched trace nitrophenols in water. Under optimal enrichment and desorption conditions, the enrichment efficiencies for five nitrophenol congeners ranged from 97.24% to 102.46%. Mechanistic investigations revealed that the efficient enrichment of trace nitrophenols by COP-99@DCA was primarily governed by hydrogen bonding, π-π stacking, and hydrophobic interactions. Coupled with solid-phase extraction (SPE) pre-treatment, high-performance liquid chromatography (HPLC) enabled the sensitive detection of trace nitrophenols. The established calibration curves exhibited favorable linearity, with low limits of quantitation (LOQs) ranging from 0.5 to 1 μg/L and low limits of detection (LODs) between 0.08 and 0.1 μg/L. Moreover, practical applications in real water samples confirmed the outstanding enrichment performance of COP-99@DCA. At spiked concentrations of 5 and 10 μg/L, the recovery rates were 85.35–113.55% and 92.17–110.46%, respectively. These results demonstrate the great potential of COP-99@DCA for practical water sample analysis. Collectively, these findings provide a novel strategy for the design of pre-treatment materials for the analysis of trace organic pollutants. Full article

Background/Objectives: Gentamicin (GEN) is an aminoglycoside antibiotic used in veterinary medicine to treat infections caused mainly by Gram-negative bacteria. GEN is a mixture of pharmacologically active components, known as isoforms. The objective was to develop and validate a sensitive, accurate, and precise Ultra-Performance Liquid Chromatography with triple quadrupole mass detector (UPLC-MS/MS) method to quantify the different GEN isoforms in pig plasma and feces using streptomycin as an internal standard. Methods: Solid-phase extraction (SPE) was carried out. A high-strength silica (50 × 2.1 mm, 1.8 µm) column was used for chromatographic separation and a mobile phase of 0.26% HFBA in water (A) and acetonitrile (B) was delivered in a gradient with a flow rate of 0.5 mL/min. The column temperature was 40 °C and the sample injection volume was 30 µL. Results: The method showed good selectivity and specificity, with no interfering peaks. Calibration curves were linear in the range from 0.05 to 0.3 µg/mL for all isoforms in both matrices. Within- and between-run precision and accuracy were satisfactory for the lower limit of quantification (LLOQ), with coefficients of variation (CV) ≤ 13.4% and deviations ≤ 116.5% in plasma and CV ≤ 12.3% with deviations ≤ 101.7% in feces. No carry-over was observed, and analyte stability was confirmed under different storage conditions. Conclusions: The method development fulfilled all validation criteria established by the European Medicine Agency Guideline (EMA/CHMP/ICH/172948/2019). Moreover, the applicability of the method in clinical practice was demonstrated by the quantification of GEN in plasma and feces samples from pigs. Full article

The widespread use of antibiotics has taken a heavy toll on the environment, which cannot be ignored. Tetracycline antibiotics (TCs), as representative pharmaceutical contaminants, have emerged as a growing environmental concern due to their persistence and potential ecological risks. This study utilized 1,3,5-benzenetricarboxylic acid (BTC) as a functionalizing reagent to synthesize magnetic nanoparticles NiFe₂O₄-COOH. These were then combined with Zr-MOF to create the magnetic adsorbent designated as NCF@Zr-MOF (where NCF represents carboxyl-functionalized nickel ferrite). Magnetic solid-phase extraction (MSPE) technology was employed to remove two representative tetracycline antibiotics, tetracycline (TC) and chlortetracycline (CTC) from the environment. The Langmuir model fitting revealed maximum adsorption reached 190.85 and 196.32 mg/g for TC and CTC, respectively, both of which conformed to the pseudo-second-order model during the adsorption process with spontaneous, heat-absorbing and entropy-increasing properties. Furthermore, following five cycles of adsorption and desorption, the removal rate for TCs was found to have decreased by 30%, yet the removal of CTCs remained at 95.32%. This adsorbent enables rapid separation via an external magnetic field. With its excellent stability and reusability, NCF@Zr-MOF shows great potential for removing antibiotics from water. Full article

Electronic waste (e-waste) is a growing solid waste stream with largely undisclosed and poorly characterized fluorinated constituents. We evaluated per- and polyfluoroalkyl substances (PFAS) leachability from four e-waste components (phone screens, phone plastics, capacitors, and Lithium-ion batteries) using a 30-day deionized water leaching test. PFAS were extracted by solid-phase extraction using weak anion exchange (WAX) cartridges and analyzed with a liquid chromatography triple-quadrupole mass spectrometer. In addition, the PFAS chemical profiles of e-waste components were characterized by non-targeted analysis. Leachable sums of detected PFAS (∑PFAS) were highest in phone screens (1739–1932 ng·kg⁻¹) and phone plastics (1575–2197 ng·kg⁻¹) and an order of magnitude lower in Lithium-ion batteries (148–158 ng·kg⁻¹) and capacitors (147–243 ng·kg⁻¹). Short-chain perfluoroalkyl acids (PFAAs) (e.g., PFBA, PFHxA) and legacy acids (e.g., PFOA, PFNA) were more prevalent in phone screens/plastics, whereas capacitors and batteries showed mixed sulfonate/carboxylate patterns (PFOS, PFHxS, and 6:2 FTS). Although capacitors and Lithium-ion batteries contained essential PFAS with high hazard potential at trace levels, phone screens and phone plastics pose a greater risk per mass due to higher ∑PFAS levels and larger volumes. Non-targeted analysis using Orbitrap Astral revealed CF₂/CF₂O homologous trends (confidence levels 2–3) with corroborating targeted findings. These findings highlight the need for PFAS-free alternatives, the disclosure of fluorinated additives, and stronger end-of-life management strategies to prevent PFAS releases from e-waste. Full article

Large outcrops of ophiolites from exposed land surfaces can potentially impact the geochemistry of much greater areas through transport and weathering. Derived soil and sediments contain significant concentrations of heavy metals, including chromium and nickel. In the context of environmental risk analysis, there is a necessity to obtain more information about the distribution of Cr and Ni in serpentine rocks and their derived associated geological matrices, and about how easily Cr could be released and then oxidized in the environment, causing pollution of groundwater. The aim of this study was to evaluate the distribution of Cr and Ni in the geochemical fractions containing Fe and Mn and the role of Fe and Mn oxides (crystalline and non-crystalline) in redox processes leading to the formation of Cr(VI) during serpentine soil weathering. Through the combination of chemical selective sequential extraction (SSE) and X-ray diffraction, solid samples belonging to ophiolitic rocks and their derived soils and sediments in southern Tuscany were investigated. The applied SSE method followed the established extraction scheme commonly used in sequential selective extraction procedures. The extraction was accomplished in seven successive steps, using appropriate reagents to destroy the binding agents between the target metal and the specific soil fraction to release the heavy metals selectively from their structural context. The results indicated significant differences in the availability and mobility of Cr and Ni in soils, with Cr concentrations ranging from 200 to 950 μg/g and Ni from 274 to 665 μg/g in reactive fractions. Cr is tightly bound to well-crystallized Fe-oxides and primary rock-derived phases, whereas Ni is substantially more mobile, being mainly controlled by Mn-oxides and amorphous Fe-oxides. Weakly acidic solutions or systems with high redox potential increase Cr and Ni mobility in the environment due to Fe/Mn hydroxides produced by the weathering of serpentinites. An ORP higher than 1000 mV leads to the formation of Cr(VI) by oxidation of Cr(III), increasing the mobility of Cr in groundwater and the hazard for human health. The analytical activity carried out in this research can be used to identify the potential risk of Cr(VI) release in groundwater from serpentine and derived geomaterials. Full article