Search Results (134)

Sewage sludge (SS) is commonly applied as a soil amendment. This practice has raised concern about the dissemination of emerging pollutants (EPs). EPs include compounds such as flame retardants, plasticizers, pharmaceuticals, and personal care products, among others, which may pose risks to human health and ecosystems. The complexity of the SS matrix, combined to the absence of an international legislation framework, makes it necessary to evaluate the techniques available for detecting these contaminants. Detection is typically performed using sensitive analytical techniques; however, the extraction strategy selected remains a crucial step. This review aims to compile different methodologies for the determination of EPs in SS, focusing on extraction strategies reported between 2010 and 2025. Ultrasound-assisted extraction (UAE), pressurized liquid extraction (PLE), and microwave-assisted extraction (MAE) are the most widely used strategies for EPs. UAE is considered the most preferable option, as it enables the extraction of a wide range of compounds without the need for expensive equipment. Among novel techniques, the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method is especially promising, as it is applicable to multiple target compounds. This review provides up-to-date information that can support the development of routine and standardized methodologies for the characterization of EPs in SS. Full article

Detecting pharmaceuticals in environmental matrices, particularly in wastewater, is crucial due to their potential environmental occurrence and unpredictable ecological and health-related consequences. These substances, often present in trace amounts, require highly sensitive and selective analytical methods for effective monitoring. A modified version of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was evaluated to evaluate 18 pharmaceuticals and 2 metabolites in wastewater samples using liquid chromatography with tandem mass spectrometry (LC-MS/MS). The method’s performance was assessed using linearity, recovery, precision, limits of quantification (LOQ) and detection (LOD), and the matrix effect (ME). The final method was based on acetonitrile, Na₂EDTA, citrate buffer, and graphene oxide (GO). Finally, the calibration curves prepared in acetonitrile and the matrix extract showed a correlation coefficient of 0.99. Most of the compounds had LOQ values lower than 0.5 μg⋅mL⁻¹. Recoveries were achieved in the 70–98% range, with RSD lower than 13%. GO allowed the elimination of the ME, which occurred in the range of −11% to 15%. The results indicate that a low-cost and straightforward method is suitable for routinely monitoring pharmaceuticals in wastewater, which is crucial for minimizing the impact of pollutants on aquatic ecosystems. Full article

The soil phytomonitoring and phytostabilization potential of Syringa vulgaris and Ficus carica was evaluated regarding 16 priority polycyclic aromatic hydrocarbons (PAHs) using a chemometric approach and the calculation of bioconcentration factors (BCFs) for each individual PAH in plants’ roots from each selected location in the Bor region. PAHs in roots and the corresponding soils were analyzed using the QuEChERS (Quick, Effective, Cheap, Easy, Rugged, Safe) method with some new modifications, gas chromatography/mass spectrometry, Pearson’s correlation study, hierarchical cluster analysis, and BCFs. Several central conclusions are as follows: Each plant species developed its own specific capability for PAH management, and root concentrations ranged from not detected (for several compounds) to 5592 μg/kg (for fluorene in S. vulgaris). In some cases, especially regarding benzo(a)pyrene and chrysene, both plants had a similar tactic—the total avoidance of assimilation (probably due to their high toxicity). Both plants retained significant quantities of different PAHs in their roots (many calculated BCFs were higher than 1 or were even extremely high), which recommends them for PAH phytostabilization (especially fluorene, benzo(b)fluoranthene, and benzo(k)fluoranthene). In soil monitoring, neither of the plants are helpful because their roots do not reflect the actual situation found in soil. Finally, the analysis of the corresponding soils provided useful monitoring information. Full article

Glyphosate (GLYP) is an effective and low-cost broad-spectrum herbicide. However, this herbicide and its primary degradation product, aminomethylphosphonic acid (AMPA), have been linked with adverse human health effects. The global use of glyphosate has significantly increased in recent years, resulting in more direct and indirect human exposure. In this context, GLYP and AMPA are often detected in fresh and processed foods for adults and infants, as well as in drinking water worldwide. Diverse extraction and quantification methods for GLYP and AMPA from foods have been developed. Solid-phase extraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are the most frequently employed cleanup strategies, while LC-MS/MS is one of the most sensitive and selective techniques for detecting GLYP and AMPA in food products. Although most studies show that GLYP and AMPA concentrations in foods remain within established maximum residue limits, occasionally they exceed legal limits. Thus, the widespread presence of GLYP and AMPA in foodstuffs is a public concern that may lead to consumers exceeding the acceptable daily intake due to prolonged dietary exposure, even if levels remain within thresholds. Therefore, this review explores the different approaches and techniques used in the extraction, detection, and quantification of GLYP and AMPA in foods. Full article

This study aims to develop a simultaneous analytical method for detecting 19 pesticides, including 4,4′-DDD, in fishery products using gas chromatography with micro-electron capture detection (GC-μECD) and gas chromatography–tandem mass spectrometry (GC-MS/MS). A new analytical method was developed to measure pesticide residues in fishery products based on the modified Association of Official Analytical Chemists protocol combining quick, easy, cheap, effective, rugged, and safe (QuEChERS) and the Pesticide Analytical Manual for extraction and purification. Extraction was performed using acetonitrile containing 0.1% acetic acid, and purification was conducted with Florisil cartridges. The Florisil cartridges were more effective than QuEChERS in removing impurities and pigments during purification and also resulted in a reduced matrix effect. The validation followed Codex guidelines (CAC/GL 40). The limit of detection ranged from 2 to 3 ng/g, and the limit of quantification (LOQ) from 7 to 10 ng/g. Matrix-matched calibration curves exhibited linearity with coefficients of determination exceeding 0.99 for all target analytes. Accuracy was assessed based on recovery rates, while precision was evaluated using relative standard deviations (RSD) at three spiking levels (LOQ, 10×LOQ, and 50×LOQ). The recovery rates ranged from 62.6 to 119.1%, with RSDs of 0.4 to 19.5%, conforming to Codex guidelines. Full article

Nucleoside reverse transcriptase inhibitors (NRTIs) and platinum-based chemotherapeutics are widely utilized in cancer treatment. Evidence suggests that drug plasma concentrations are closely linked to both therapeutic efficacy and the risk of adverse effects. Consequently, developing therapeutic drug monitoring (TDM) methods is essential. Here, an effective procedure utilizing QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) techniques for preparing samples and UPLC-MS/MS for simultaneously measuring eight NRTIs and platinum-based drugs in human plasma is described. Chromatographic separation was conducted with an Agilent Eclipse Plus C18 column (4.6 × 100 mm, 3.5 μm) with acetonitrile with 0.1% formic acid as Phase A and 0.1% formic acid in water as Phase B, achieving complete separation within 10 min. The target analytes—lamivudine, telbivudine, emtricitabine, entecavir, tenofovir, nedaplatin, oxaliplatin, and adefovir dipivoxil—exhibited strong linearity within the 10–1000 ng/mL and 1–100 ng/mL ranges, showing correlations (r²) ≥ 0.9962. The method demonstrated excellent accuracy (−6.72% to 7.82%) and selectivity (84.53%–110.49%), as well as satisfactory recovery and stability. Overall, this analytical approach can be used to detect the combination of eight NRTIs and platinum-based drugs in human plasma. This method enables plasma drug-level monitoring in real time, with applications for individualized treatment approaches. Full article

A high-throughput method for the determination of a variety of chemical hazards in poultry muscle and egg samples was established via ultra-performance liquid chromatography–tandem triple quadrupole mass spectrometry (UPLC–QqQ-MS). The sample preparation procedure was developed based on this quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and validated for 280 chemical hazards potentially present in poultry products. The target compounds in poultry samples were extracted with a 1% formic acid–acetonitrile solution (15:85, v/v), and the metal ions in the matrix were chelated by adding ethylenediaminetetraacetic acid disodium salt (Na₂EDTA). The supernatant was purified using Enhanced Matrix Removal (EMR) lipid sorbent. Chromatographic gradient separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with multiple reaction monitoring (MRM) under both negative- and positive-ion mode. Internal standard calibration or matrix-matched calibration was used for the quantitation. The results showed that good linearity was achieved for each target compound with correlation coefficients (R²) ≥ 0.99. The limits of detection (LODs) ranged from 0.05 to 10 µg/kg, and the acceptable limits of quantification (LOQs) were determined to be 0.1–20 µg/kg for all 280 compounds. Approximately 90% of the target compounds exhibited mean recoveries ranging from 60% to 120%, with relative standard deviations (RSDs) within 16.2%. This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs due to its easy operation and high accuracy. It was applied in real sample detection, and 43 chemicals including metronidazole were found in 211 poultry samples, with a concentration range of 0.11–638 μg/kg. Full article

Veterinary drugs are extensively employed in livestock, poultry, and aquaculture, playing a crucial role in preventing and treating animal diseases, facilitating growth, and enhancing feed conversion rates. Nevertheless, veterinary drug residues in animal-derived foods pose a direct or potential threat to human life and health. Precise detection of these residues in animal-derived foods to ensure their safety has become an important mission. In this review, we sum up the current progress of applied pretreatment methods and detection techniques for veterinary drug residues in animal-derived foods. At present, sample pretreatment methods mainly consist of the following: liquid–liquid extraction; solid-phase extraction; immunoaffinity chromatography; Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method; and molecular imprinting technology. Detection techniques mainly involve chromatographic techniques, immunoassay techniques, fluorescence polarization immunoassay, and surface-enhanced Raman scattering. We also discussed the advantages and limitations of these technologies. Moreover, we point out the development direction and tendency of detection techniques in the future, providing references for the detection of veterinary drug residues in animal-derived foods. Full article

The current status of multi-mycotoxin contamination in edible and medicinal plants demands urgent development of high-throughput analytical methods for mycotoxin detection. In this study, a reliable and sensitive method for the simultaneous analysis of 73 mycotoxins was established and successfully applied to detect mycotoxins in 260 samples of four dual-purpose plants (lotus seed, coix seed, licorice root, and dried tangerine peel). Sample preparation involved optimized QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction combined with liquid–liquid extraction purification, and an enhanced ion pair library was established to reduce matrix interference and improve the method’s universality. Method validation demonstrated recovery rates ranging from 61.6% to 118.6% for all compounds, with relative standard deviations (RSDs) below 15%. The limits of detection (LODs) and quantification (LOQs) ranged from 0.25–12.25 μg/kg and 0.5–25 μg/kg, respectively. Based on the contamination analysis and health risk assessment using Margin of Exposure (MOE) and Hazard Index (HI) methods, we found that multi-mycotoxin contamination is highly prevalent in edible and medicinal plants, with different components being susceptible to invasion by distinct fungal genera. Seed-type plants showed high susceptibility to Aspergillus (53.3%) and Fusarium (22.2%) contamination, with MOE values below 10,000 for aflatoxins indicating potential health risks. Physical state and good storage conditions significantly influenced contamination levels, with fragmented samples showing substantially higher mycotoxin levels. Additionally, mycotoxins with associated biosynthetic metabolic pathways were frequently detected simultaneously in highly contaminated samples. Based on these findings, we recommend implementing strict moisture control during storage, maintaining intact product form where possible, and establishing comprehensive supplier qualification systems. This study provides valuable reference for monitoring mycotoxin contamination in similar plants. Full article

The bioaccumulation of pesticides in honeybee products (HBPs) should be studied for a number of reasons. The presence of pesticides in HBPs can provide new data on the risk related to the use of pesticides and their role in bee colony losses. Moreover, the degree of contamination of HBPs can lower their quality, weaken their beneficial properties, and, in consequence, may endanger human health. The aim of this study was to quantify a broad range of pesticide residues in three different HBPs—bee pollen, propolis, and royal jelly. Samples were collected in the years 2017–2019 from the apiary in west-central Poland. Bee products were analyzed for the presence of over 550 pesticides using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method. Twenty-nine of the contaminants were quantified at least in one of the samples. Nine of them exceeded the maximum residue levels for honey. It should be noted that any dose of pesticides can cause a health hazard due to toxicity, since these substances may act synergistically. This current study revealed the high need for the pesticide monitoring of HBPs and proved that there is a need to expand the European Union Pesticides Database to include more HBPs. Full article

The growing prevalence of pharmaceutical compounds in the environment raises significant concerns due to their potential impacts on ecological and human health. This present manuscript focuses on the methods used to extract and determine these pharmaceuticals in water samples. It provides a comprehensive analysis of the extraction techniques and analytical approaches employed for the identification and quantification of pharmaceuticals in environmental water. Due to their chemical properties and widespread use, pharmaceuticals persist in the environment and contaminate water bodies, soil, and sediments. The presence of pharmaceuticals in the aquatic environment has been linked to several adverse effects on aquatic organisms, including the disruption of physiological processes and reproductive impairment. Furthermore, pharmaceuticals in the environment can affect human health through food and drinking water contamination and contribute to antibiotic resistance. The analysis of pharmaceutical contaminants in water samples presents several challenges due to the complex matrix and low concentrations of target substances. Various sample preparation techniques and protocols, including solid-phase extraction (more than 76% of the studied literature) and QuEChERS (quick, easy, cheap, effective, rugged, and safe), coupled with liquid chromatography–tandem-mass spectrometry, are commonly used for their determination. These methods offer high sensitivity, selectivity, and efficiency in identifying and quantifying pharmaceuticals in environmental samples. It is, therefore, essential that ongoing research is conducted in order to develop more efficient analytical methods and mitigation strategies to address pharmaceutical contamination in the environmental water effectively. It is also crucial that increased awareness and regulatory measures are put in place in order to minimize the environmental and human health risks associated with pharmaceutical pollutants. Full article

Polycyclic aromatic hydrocarbons are considered to be potentially genotoxic and carcinogenic to humans. For non-smoking populations, food is the main source of polycyclic aromatic hydrocarbons exposure. Due to their lipophilic nature, oils and fats rank among the food items with the highest polycyclic aromatic hydrocarbon content. Consequently, the detection of polycyclic aromatic hydrocarbons in edible oils is critical for the promotion of human health. This paper reviews sample pretreatment methods, such as liquid-phase-based extraction methods, adsorbent-based extraction methods, and the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, combined with detection techniques like mass spectrometry and chromatography-based techniques for accurate quantification of polycyclic aromatic hydrocarbons in edible oils since 2010. An overview on the advances of the methods discussed herein, along with a commentary addition of current challenges and prospects, will guide researchers to focus on developing more effective detection methods and control measures to reduce the potential risks and hazards posed by polycyclic aromatic hydrocarbons. Full article

A facile procedure for extracting and determining seven neonicotinoids was developed. Water was the only extraction solvent without phase separation and cleanup steps. The method was validated according to European Union standards, and the values obtained were compared with the criteria. The accuracy values were between 99.8% (thiamethoxam) and 106.8% (clothianidin) at the spiking levels of 0.01, 0.1, and 1 mg/kg in the tested matrices. The precision as pooled RSD values was ≤6.1% (intra-day) and ≤6.9% (inter-day). The limit of quantification was set and tested at 0.01 mg/kg. The matrix effect was evaluated, and all matrices had a suppressive effect. The matrix of the cucumber was the most effective, with −20.9% for dinotefuran and an average of −9.8% for all compounds, while the tomato matrix had the slightest effect. Real marketed samples were analyzed using the developed and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methods; the results were not significantly different. A supervised field trial was conducted in the open field to study the dissipation patterns of imidacloprid and dinotefuran in tomatoes. The dissipation of both compounds followed first-order kinetics. The half-life (T_½) values were 3.4 and 2.5 days, with dissipation rates k of 0.2013 and 0.2781 days, respectively. Following the EU-MRL database, the calculated pre-harvest interval (PHI) values were 7 and 14 days for imidacloprid and dinotefuran, respectively, and 3 days for both compounds following Codex Alimentarius regulations. The risk of imidacloprid and dinotefuran residues was estimated from chronic and acute perspectives. The risk factors of dinotefuran were lower than those of imidacloprid. Nonetheless, the highest expected residues of both compounds were below the tolerance limits. Full article

Per- and polyfluorinated alkyl substances (PFASs) are a group of anthropogenic chemicals used in a range of industrial processes and consumer products. Recently, their ubiquitous presence in the environment as well as their toxicological effects in humans have gained relevant attention. Although the occurrence of PFASs is widely investigated in scientific community, the standardization of analytical method for all matrices still remains an important issue. In this review, we discussed extraction and detection methods in depth to evaluate the best procedures of PFAS identification in terms of analytical parameters (e.g., limits of detection (LODs), limits of quantification (LOQs), recoveries). Extraction approaches based on liquid–liquid extraction (LLE), alkaline digestion, and solid phase extraction (SPE), followed by liquid chromatography–mass spectrometry (LC-MS) and gas chromatography–mass spectrometry (GC-MS) analysis are the main analytical methods applied in the literature. The results showed detectable recoveries of PFOA and PFOS in meat, milk, vegetables, eggs products (90.6–101.2% and of 89.2–98.4%), and fish (96–108%). Furthermore, the low LOD and LOQ values obtained for meat (0.00592–0.01907 ng g⁻¹; 0.050 ng g⁻¹), milk (0.003–0.009 ng g⁻¹; 0.010–0.027 ng g⁻¹), fruit (0.002–0.009 ng g⁻¹; 0.006–0.024 ng g⁻¹), and fish (0.00369–0.017.33 ng g⁻¹; 0.05 ng g⁻¹) also confirmed the effectiveness of the recent quick, easy, cheap, effective, rugged, and safe method (QuEChERS) for simple, speedy, and sensitive ultra-trace PFAS analysis. Full article

Commercial viticulture necessitates regular pesticide applications to manage diseases and pests, raising significant concerns regarding pesticide residues among stakeholders. Due to health risks associated with these residues in Turkish vine leaves, the European Commission has increased the frequency of official control from 20% to 50%. Thus, the aim of this study was to determine multi-class pesticide residues in brined vine leaves from Turkey. A total of 766 samples of vine leaves were collected between May 2022 and June 2023. More than 500 residues were analyzed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, followed by liquid chromatography-tandem mass spectrometry. In-house validation data demonstrated that the analytical method exhibits fit-for-purpose performance in terms of linearity, accuracy, precision, and measurement uncertainty. Out of 766 samples analyzed, 180 samples (23.5%) contained one (131, 17.1%) or multiple (49, 6.4%) pesticides. Both the frequencies of occurrence and the rate of maximum residue level (MRL) exceedance increased in 2023 compared to 2022, with the MRL exceedance rate rising from 9.5% to 25.2%. Forty-three different residues were found in quantifiable concentrations and eight of them were non-approved. Among the residues, the non-systemic pyrethroid insecticides, lambda-cyhalothrin (8.0%) and cypermethrin (7.2%), were the two most frequently detected, with concentrations ranging from 0.010 to 0.248 mg kg⁻¹ and from 0.011 to 0.533 mg kg⁻¹, respectively. Turkey is a major exporter of vine leaves and these results provide crucial information regarding pesticide occurrence and quality assessment of vine leaves. The significant increase in both pesticide occurrence and MRL exceedance rates between 2022 and 2023 underscores the urgency for regulatory bodies to reassess current pesticide usage and monitoring practices. The findings emphasize the importance of implementing more stringent rules and improving enforcement methods in order to reduce the spread of unapproved pesticides and ensure adherence to global food safety standards. Full article