Search Results (286)

The ongoing substance use crisis in the United States involves a broad range of illicit and prescription drugs, including opioids, stimulants, sedatives, and various psychoactive and non-psychoactive compounds. Traditional surveillance methods rely on self-reported data, which could lead to bias and recall inconsistencies. Wastewater-based epidemiology has emerged as a powerful, non-invasive tool for monitoring community-level drug use, offering near real-time estimates and the potential to serve as an early warning system. However, challenges such as analyte degradation, wastewater variability, and matrix effects can affect data quality and comparability across regions. This study presents a standardized, practical workflow for multi-drug (n = 52) detection in wastewater, aiming to minimize analyte loss and improve reproducibility. Composite samples were collected from multiple U.S. cities, transported on ice, and extracted using solid-phase extraction. Extraction efficiencies were compared using Oasis Hydrophilic-Lipophilic-Balanced and Mixed-mode Cation-Exchange (MCX) cartridges, with the MCX sorbent providing complementary reversed-phase and cation-exchange interactions that enabled the retention of chemically diverse compounds across multiple drug classes. Analysis was performed with an Ultra-High-Performance Liquid Chromatography system coupled to a triple quadrupole mass spectrometer, in which the instrument parameters and critical methodological considerations, including sample handling, transport, column selection, and method validation, are detailed. This work contributes to the development of a robust, scalable protocol for multi-drug surveillance in wastewater, supporting timely, data-driven public health responses and informing national drug policy efforts. Full article

The increasing generation of organic and liquid wastes calls for sustainable strategies to convert residues into valuable energy resources. This study investigates waste Oxytree biomass (Paulownia Clon In Vitro 112^®) as a sorbent for producing impregnated solid fuels from selected liquid wastes, including used cooking oil, spent mineral oil, and pyrolysis condensate, targeting industrial energy applications. Oxytree biomass was selected due to its high and predictable yield, uniform composition, and favorable physical properties compared to conventional lignocellulosic residues such as pine sawdust. Biomass and liquid wastes were characterized in terms of fuel properties and elemental composition. Several empirical combinations of sorbent and liquid fractions were tested to optimize homogeneity and fuel quality, resulting in a final composition of sorbent:used cooking oil:used machine oil:pyrolytic condensate equal to 3:1:1:3. The temporal stability of this selected fuel was verified over 24 h, 3 days, and 1 week. The resulting fuels exhibited an energy value of approximately 15 MJ/kg, low ash content (<1%), and minimal concentrations of chlorine and sulfur (<0.08%). Overall, the findings demonstrate that Oxytree waste biomass can serve as an effective sorbent for integrating problematic liquid wastes into solid fuels, providing a practical route for waste valorization and supporting circular economy principles, and establishing a foundation for further research on sustainable energy applications of biomass and industrial residues. Full article

The efficient utilization of industrial waste (containing alkaline compounds, especially Ca-based species) for flue gas desulfurization (FGD) is of great importance for both environmental protection and resource recovery. In this study, paper industry white mud was modified with Ca(OH)₂ to develop a cost-effective sorbent with enhanced SO₂ removal performance. Optimization experiments identified the best preparation conditions as a 1:1 Ca(OH)₂/white mud ratio, 60 °C modification temperature, 6 h reaction time, and a liquid-to-solid ratio of 3:1. Under these conditions, the sorbent achieved nearly 100% SO₂ removal in the first 6 h and maintained >90% efficiency after 10 h, significantly outperforming raw white mud and Ca(OH)₂ alone. Characterization revealed that the superior performance originated from structural stability and abundant active sites. BET analysis showed a high surface area (24.8 m²·g⁻¹) and pore volume (0.160 cm³·g⁻¹), which were largely preserved after desulfurization, indicating resistance to pore blockage. SEM images confirmed a transition from porous aggregates to densified product layers, consistent with a shrinking-core/product-layer mechanism. XRD identified CaSO₄·2H₂O as the dominant product, while in situ FTIR demonstrated that O₂ promotes sulfite oxidation and H₂O accelerates hydrated sulfate formation, enhancing activity but causing faster pore blocking. The presence of NO extended sorbent durability by catalyzing continuous sulfite oxidation through NO/NO₂ redox cycling. Overall, Ca(OH)₂-modified white mud combines high reactivity, durability, and structural stability, offering a promising alternative to conventional sorbents. This work provides a viable route for the resource utilization of paper industry waste and practical insights for designing efficient and sustainable materials for industrial FGD systems. Full article

Zebrafish, as an emerging model organism, are widely used in in vivo pharmacodynamic and pharmacokinetic studies. Unlike direct chemical analyses that require no sample preparation, most biological samples must undergo preprocessing steps—procedures that profoundly affect analytical outcomes. This paper systematically summarizes the main methods and types of zebrafish sample pretreatment currently in use, aiming to provide a reference for future research in zebrafish sample analysis and preparation. A systematic search was conducted across PubMed, Web of Science, and CNKI for studies published between 2014 and 2024 focusing on liquid–liquid extraction (LLE), solid phase extraction (SPE), and related techniques for zebrafish drug analysis. The results indicate that traditional methods, including LLE and protein precipitation, remain prevalent due to their operational simplicity, but are limited by low enrichment efficiency and pronounced matrix effects (MEs). In contrast, advanced SPE techniques, particularly solid phase microextraction (SPME), are increasingly favored for complex biological sample processing, with key trends including technique hyphenation (e.g., SPME–high-performance liquid chromatography (SPME-HPLC), and micro-SPE–mass spectrometry (µSPE-MS)) and the development of novel sorbents. Despite these advances, current challenges persist, such as immature rapid on-site pretreatment protocols, the difficulty of balancing analytical efficiency with operational simplicity, and the lack of standardized procedures across studies. Overall, zebrafish sample pretreatment techniques are evolving toward higher efficiency, selectivity, and automation. Future research efforts should prioritize the development of intelligent, eco-friendly pretreatment methods and the establishment of unified standards to enhance the reproducibility and comparability of zebrafish-based pharmacological studies. Full article

Cyanotoxins, prevalent in eutrophic aquatic ecosystems, pose significant health risks via contaminated food, yet analytical methods for detecting multiple toxin classes in foodstuffs remain limited. In the current study, a method based on dispersive solid-phase extraction (dSPE) coupled with ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) was developed to simultaneously determine four common classes of cyanotoxins (i.e., microcystins, cylindrospermopsins, nodularins, and anatoxins) in aquatic products, vegetables and algal dietary supplements. Following initial extraction with 80% aqueous methanol, sample purification was performed using anhydrous sodium sulfate (400 mg) and C₁₈ sorbent (50 mg). For plant-based foods, additional graphitized carbon black (GCB, 15 mg) was also included. The method was successfully validated in eight different food matrices, demonstrating recoveries of 65–122% and relative standard deviations below 19%. The limits of detection and quantification across all matrices ranged from 0.1 to 3.4 μg/kg dry weight (dw) and 0.4 to 11.4 μg/kg dw, respectively. When applied to 96 food samples, this method detected multiple cyanotoxins in Tilapia and Spirulina-based dietary supplements. The proposed method provides a rapid, cost-effective, high-throughput, and sensitive analytical tool suitable for monitoring multiple cyanotoxins in various foodstuffs. Full article

The presence of antibiotics in aquatic systems presents significant ecological and health risks. Herein, Fe₃O₄/MgAl₂O₄ (MgFeAl-1), 2.5%NiO@Fe₃O₄/MgAl₂O₄ (MgFeAl-2), 5%NiO@Fe₃O₄/MgAl₂O₄ (MgFeAl-3), and 10%NiO@Fe₃O₄/MgAl₂O₄ (MgFeAl-4) were synthesized, selecting glucose as a capping agent, and 600 °C as calcination temperature. The TEM, EDX, BET, XRD, and FTIR techniques were employed to characterize the preidentified sorbents. The average size of MgFeAl-1, MgFeAl-2, MgFeAl-3, and MgFeAl-4 was about 6.53, 5.0, 7.61, and 10.52 nm, respectively, and they exhibited surface areas of 114.15, 154.02, 153.36, and 128.54 m² g⁻¹, respectively. The sorbents were tested for the removal of ciprofloxacin (CFCN) from aqueous solutions using the batch protocol. The MgFeAl-2 exhibited the highest performance, achieving an adsorption capacity of 99.45 mg g⁻¹, and the sorption equilibrium was reached within 60 min. The pseudo-second-order model best described CFCN sorption onto MgFeAl-2, and liquid-film diffusion influenced CFCN sorption. The CFCN adsorption onto MgFeAl-2 was well represented by the Langmuir isotherm model (R² = 0.93), indicating a monolayer adsorption. The thermodynamic results indicated a spontaneous, endothermic sorption process. A four-cycle MgFeAl-2 reusability study showed an average efficiency of 90%. Notably, MgFeAl-2 was effective in treating natural-water matrices, with a slight reduction in seawater due to ionic interference. The findings highlight the potential of MgFeAl-2 as an affordable and reusable adsorbent for removing antibiotics from contaminated water. Full article

In-tube solid-phase microextraction (IT-SPME) is an advanced microextraction technique in which a sample solution flows through a capillary containing an internal stationary phase, enabling efficient extraction and preconcentration of target analytes. The online coupling to liquid chromatography is a key advantage of this technique, enabling full automation and high analytical throughput, both of which are significant for food analysis. Recent advances have focused on developing novel sorbent materials that respond to external stimuli (e.g., magnetic, electrical, or thermal) and on integrating them into emerging chromatographic platforms. Moreover, key operational parameters, including sample volume, pH, phase thickness, and the capillary’s dimensions (length and inner diameter), must be optimized to achieve enhanced selectivity, speed, and sensitivity. Despite this, the literature still lacks updated reviews of SPME concepts and their innovations for versatile applications in food matrices. Hence, this review outlines the fundamental principles of IT-SPME while highlighting key parameters that affect analytical performance. Finally, we provide a literature review of SPME applications in food analysis over the past 6 years, while exploring current trends and future directions for SPME development and enhanced applications in food science. Full article

Background: Food waste contains abundant (+)-catechin, but its efficient recovery remains challenging. This study aimed to prepare ionic liquid (IL)-modified sorbents and establish an efficient method for (+)-catechin recovery from chocolate waste via solid-phase extraction (SPE). Methods: Three series of IL-modified sorbents (Sil-IL, ZIF67-IL, Sil@ZIF67-IL) were synthesized. Their adsorption performance was evaluated under different conditions; adsorption isotherm and kinetic data were fitted to Langmuir/Freundlich and pseudo-first/second-order models, respectively. Sorbent stability and (+)-catechin recovery from chocolate waste extracts were tested. Results: Sil@ZIF67-Hmim showed the highest adsorption capacity (154.4 mg/g) at 25 °C within 120 min. Adsorption followed the Langmuir model (R² = 0.99), indicating chemisorption. Sil@ZIF67-Hmim was subjected to repeated solid-phase extraction (SPE) for five consecutive days; the recovery rate ranged from 98.1% to 99.2%, and the relative standard deviation (RSD) was 3.2–4.4%. Conclusions: Sil@ZIF67-Hmim is a high-efficiency sorbent for (+)-catechin recovery from chocolate waste, providing a novel approach for food waste valorization and highlighting the application potential of IL-modified MOF-silica composites. Full article

The present contribution proposes a new design for adsorptive microextraction devices that promote a user-friendly and greener analytical approach. Novel Sorbent Strip Microextraction (SSμE) devices were made using a flexible adhesive film coated with convenient sorbents. Comparing the previous adsorptive microextraction devices, i.e., bar adsorptive microextraction and multi-sphere adsorptive microextraction, the main advantage of the sorbent strip device is its simple design and reduced device preparation time and waste. To demonstrate its applicability, three opioids (buprenorphine, tapentadol, and tramadol) and two local anesthetics (articaine and bupivacaine) were used as model compounds in urine matrices, followed by high-performance liquid chromatography with diode array detector (HPLC-DAD) analysis. Key parameters such as sorbent type, desorption conditions, and microextraction variables were systematically optimized by experimental designs. Under the final conditions, the method achieved recoveries ranging from 78% to 108%, trueness within ±7% and precision expressed by relative standard deviation below 13%. The technique demonstrated good linearity (r² ≥ 0.9922) across dynamic ranges of 5–500 ng/mL for local anesthetics and 50–5000 ng/mL for opioids. The validated SSμE/HPLC-DAD methodology was successfully applied to real urine samples, confirming its high precision and accuracy. The proposed microextraction technique offers a practical, eco-friendly, and effective alternative for routine drug screening in complex biological matrices and presents significant advantages over traditional and other microextraction-based methods. 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

Waste electrical and electronic equipment (WEEE) is a rapidly growing waste stream rich in precious metals, with gold in particular being concentrated in printed circuit boards and other high-value components. Historically, industrial recycling has relied on pyrometallurgy and non-selective hydrometallurgical leaching. These recovery routes have major drawbacks, including high energy demand, corrosion, the use of toxic reagents, and the complexity of pregnant leach solutions, which complicate downstream gold recovery. This review aims to synthesize recent advances in selective gold recovery from WEEE using a speciation-driven approach. Mechanical pretreatment and physical beneficiation methods are critically assessed as processes for concentrating gold and reducing the amount of material sent to downstream hydrometallurgical leaching. Different lixiviants, from conventional cyanide to halide-based, as well as greener chemistries such as thiosulfate and thiourea, are assessed for gold dissolution from the WEEE stream. Assessment of different extraction methods, including sorbents, ion exchange resins, solvent/ionic liquid, direct reduction/precipitation, and electrochemical recovery, is conducted. The review concludes with guidelines for potential process integration and highlights the need for scalable, reusable lixiviants and sorbent materials validated under realistic multi-metal conditions in real WEEE leachate. Full article

(1) Background: Energy-based transurethral resection of bladder tumor (TURBT) generates surgical smoke that may contain hazardous volatile organic compounds (VOCs), yet surgeon breathing-zone exposure during transurethral surgery remains insufficiently characterized. (2) Methods: We conducted a prospective paired-exposure study during 28 TURBT procedures over 10 operating days using personal sampling at the surgeon’s breathing zone and simultaneous intraoperative background sampling at three predefined locations (~1.5 m from the surgeon). VOCs were measured by active sampling onto Tenax TA sorbent tubes followed by thermal desorption Gas Chromatography–Mass Spectrometry (GC–MS), and formaldehyde was measured by 2,4-dinitrophenylhydrazine (DNPH) cartridges with high-performance liquid chromatography/ultraviolet detection (HPLC/UV). Breathing-zone versus background contrasts were summarized as paired geometric mean ratios (GMRs), and a dose index was calculated as concentration × operative time (µg·h/m³). (3) Results: Breathing-zone concentrations consistently exceeded background levels, including total VOCs (GMR 4.31; 95% CI 2.92–6.38), ΣBTEXS (sum of benzene, toluene, ethylbenzene, xylenes, and styrene; GMR 2.10; 1.69–2.60), and styrene (GMR 8.51; 6.25–11.60); formaldehyde showed a smaller but significant elevation (GMR 1.20; 1.07–1.35). ΣBTEXS dose increased with operative time (Spearman ρ = 0.80, p < 0.001) and resection mass where available (ρ = 0.62, p = 0.0038; n = 20) and scaled with operative time (β = 0.86; R² = 0.69; n = 28). (4) Conclusions: TURBT is associated with marked enrichment of aromatic VOCs in the surgeon’s breathing zone, supporting routine implementation of effective source-level smoke evacuation and filtration to reduce occupational exposure. Full article

The aim of this work is to develop structurally enhanced and highly hydrophobic polyurethane (PU) foams for the efficient remediation of liquid organic pollutants. For this purpose, PU foams were modified with renewable activated biochar derived from marine algae (AC) and a hydrophobic polydimethylsiloxane (PDMS) coating, producing four systems: pristine PU, PU-AC, PU/PDMS, and the hybrid PU-AC/PDMS composite. The study evaluates how AC incorporation and PDMS surface functionalization influence the microstructure, chemical composition, wettability, thermal stability, and sorption behavior of the foams. SEM images revealed progressive reductions in pore size from 420 ± 80 μm (PU) to 360 ± 85 μm (PU-AC/PDMS), with AC introducing heterogeneity while PDMS preserved open-cell morphology. FTIR confirmed the presence of urethane linkages, carbonaceous structures, and PDMS siloxane groups. Surface hydrophobicity increased markedly from 88.53° (PU) to 148.25° (PU-AC/PDMS). TGA results showed that PDMS improved thermal stability through silica-rich char formation, whereas AC slightly lowered degradation onset. Sorption tests using petroleum-derived oils and hydrophobic organic liquids demonstrated a consistent performance hierarchy (PU < PU/PDMS < PU-AC < PU-AC/PDMS). The ternary composite achieved the highest uptake capacities, reaching 44–56 g/g for oils and up to 35 g/g for hydrophobic solvents, while maintaining reusability. These findings demonstrate that combining activated biochar with PDMS significantly enhances the functional properties of PU foams, offering an efficient and sustainable material for oil–water separation and organic pollutant remediation. Full article

Ionic liquids (ILs) have attracted considerable attention for light olefin separation owing to their negligible vapor pressure, excellent thermal stability, and tunable molecular structures. However, their intrinsically high viscosity severely restricts gas diffusion, leading to poor mass-transfer efficiency and limited separation performance in bulk form. Herein, we report the develop a high-performance adsorbent by immobilizing a silver-functionalized ionic liquid within ordered mesoporous MCM-41 to overcome the diffusion limitations of bulk ILs. The IL@MCM-41 composites were prepared via an impregnation–evaporation strategy, and their mesostructural integrity and textural evolution were confirmed by XRD and N₂ sorption analyses. Their C₂H₄/C₂H₆ separation performance was subsequently evaluated. The composite with a 70 wt% IL loading achieves a high C₂H₄ uptake of 25.68 mg/g and a C₂H₄/C₂H₆ selectivity of 15.59 in breakthrough experiments (298 K, 100 kPa). X-ray photoelectron spectroscopy results are consistent with the presence of reversible Ag⁺–π interactions, which governs the selective adsorption of C₂H₄. Additionally, the composite exhibits excellent thermal stability (up to 570 K) and maintains stable separation performance over 10 adsorption–desorption cycles. These IL@MCM-41 composites have significant potential for designing sorbent materials for efficient olefin/paraffin separation applications. Full article

The increasing demand for clean and sustainable energy has driven significant research into hydrogen production from biomass-derived feedstocks. Unlike the gasification route, the pyrolysis of biomass followed by steam reforming of bio-oil (SRBO) offers several advantages, including the liquid nature of bio-oil and the operation at lower temperatures, which facilitate easier transportation and storage compared to raw biomass. The conventional SRBO process faces several limitations, mainly catalyst deactivation due to significant coke formation and metallic sintering, as well as low hydrogen yield and purity. Hence, the intensified sorption-enhanced steam reforming of bio-oil (SESRBO) is a promising strategy to overcome these drawbacks, to simultaneously produce high-purity hydrogen and capture carbon dioxide in situ from the reaction media. This critical review presents an in-depth comparative analysis of conventional and intensified steam reforming of bio-oil, with a focus on associated challenges. Special attention is given to recent developments in the design of bifunctional materials (BFMs), which integrate both catalyst and sorbent into a single particle, along with process optimization focusing on key parameters, i.e., reforming temperature and steam presence. Finally, the review highlights key research gaps and future directions to overcome existing challenges in achieving cost-effective and scalable hydrogen production. Full article